Binder UNT

Juan A. Caballero, Eng.
, PhD
Research Council Officer
Information and Communication Technologies
National Research Council Canada
DISEÑO Y ANALISIS DE
EXPERIMENTOS CON MINITAB
 El diseño de experimentos (DOE) es una técnica estadística que se
basa en organizar y diseñar una serie de experimentos de forma que
con el mínimo número de pruebas se consiga extraer información
útil para obtener conclusiones que permitan optimizar la
configuración de un proceso o producto
Diseño y Analisis de Experimentos - UNT 2015 2

 Determinar si utilizar un determinado tratamiento produce una mejora en el
proceso  Confiabilidad  Rendimiento  Optimización de la calidad del
Producto
El DOE, por lo general, se desarrolla en 4 fases: Planificación, screening,

optimización, y verificación

 Definir el problema  Se indentifica la
preguntas que se debe responder
 Definir el objetivo  cuál es el objetivo
del experimento?
 Desarrollar un plan experimental
capáz de proporcionar información
significativa  experiencia,
conocimientos del proceso, principos
teóricos, identificación de factores o
condiciones, etc.
 Asegúrese que el proceso y
mediciones puedan ser controladas 
Proceso de control estadístico (SPC) y
variavilidad en las mediciones

Cernido (Screening) Optimización
 Plan experimental donde se  Se determina los valores óptimos
encuentra los “pocos” factores más para los factores experimentales.
importantes de una lista de “muchos Estos dependen de los objetivos del
posibles” experimento
 El objetivo principal es identificar los  Los métodos disponibles en Minitab
efectos principales significativos. son:
La identificación de los efectos de  Diseños general-factorial completos
interacción es menos importante  Diseño de superficie respuesta –
 Los Métodos mas usados en la incluye diseños compuestos
etapa de screening son: centrales y diseños Box-Behnken
 Diseños factorial completos o  Diseños mezcla – incluye diseños
fraccionales de 2-niveles (del tipo III centroide simple, cuadrícula simple
& IV) y de vértice extremo
 Diseños factorial Plackett-Burman  Diseños Taguchi (matrices
ortogonales)
 Diseños general-factorial completos
(más de 2 niveles)

 Se realizan corridas experimentales
para confirmar la validéz del diseño
óptimo. Se usa la “mejor”
configuración, y se obtiene el
intervalo de confidencia para la
respuesta media

 Unidad experimental
 Bloquear
 Objetos, individuos, intervalos de
 Division de las unidades
espacio o tiempo sobre los que se
experimentales en grupos de unidades
experimenta similares
 Variable de interés (respuesta)  Observación experimental
 Variable que se desea estudiar y  Es cada medición de la variable
controlar su variabilidad respuesta
 Factor  Matriz de Diseño
 Variable independiente que puede  Conjunto de factores y niveles de un
influir en la variabilidad de la variable diseño experimental
de interés  Aleatorización
 Nivel  Secuencia de experimentos y/o
 Valor de un factor que se esta asignación de especímenes a los
examinando en el experimento tratamientos diferentes
 Tratamiento  Replicación
 Combinación específica de los  Repetición de una observación o
niveles de los factores de estudio medida en las mismas condiciones
experimentales

 Cuando se estima un parámetro
poblacional, un intervalo de confianza
(CI) es una rango de valores calculado en
el cual se encuentra el verdadero valor
del parámetro, con una probabilidad
determinada
 La probabilidad de que el verdadero
0.95
valor se encuentre en el intervalo
calculado se denomina nivel de
confianza: 1-α
0.025 0.025
 La probabilidad de equivocarnos se
llama nivel de significancia: α
 Generalmente se construyen intervalos
con confianza 1-α = 95% (o significancia
α = 5%)

 La hipótesis nula es la hipótesis sobre la cual se debe de tomar una
decisión y se simboliza por Ho. Esta se contrasta con otra hipótesis
llamada Hipótesis alterna H1
 La decisión de aceptar Ho implica rechazar H1
 Para efectos prácticos, habitualmente la hipótesis nula es la que el
experimentador espera rechazar
 Ho es el reverso de la hipótesis de investigación
Cuando
Z-score > 1.96
o
Z-score < -1.96
Se rechaza Ho
Distribución normal

Z= (𝑋𝑋 − 𝜇𝜇)/𝜎𝜎
X = valor experimental; μ = Promedio Z-score = 2.5, P-value = 0.006 is
σ= standard deviation graphically represented
Para (1-α) de 5%, el valor crítico de Z =

1.96  Ho se rechaza. Esto se deben a
que las observaciones distan mucho de
aquellos correspondientes a una muestra
aleatoria. El valor-p es la probabilidad
de obtener este tipo de resultados.
• En DOE, el valor-p se utiliza para determinar si los resultados son

estadísticamente significativos
• Se usa para tomar decisiones: Se “rechaza” o “no rechaza” una hipótesis nula (Ho)
• El valor-p representa la probabilidad de rechazar INCORRECTAMENTE una
hipótesis nula que en realidad es verdadera

 El valor p se compara con el
nivel de significancia (α) para
decidir si debe rechazar la
hipótesis nula (H0). Si el valor
p es menor que el nivel de
significancia (α), rechace H0
 Si el valor p es mayor que el
nivel de significancia (α),
usted no puede rechazar H0.
 Para el nivel de significancia
(α) suele utilizarse un valor de
0.05, entonces, si el valor p es
menor que 0.05, rechace H0.

 Permite el estudio simultáneo de los efectos de varios factores en un proceso  Variación
simultánea de los niveles de los factores
 Estima efficientemente el efecto de cada factor en la “respuesta”
 Revela y estima las interacciones entre los factores
 Ahorro de tiempo y costos
Diseño de 2 factores Diseño de 3 factores

• 2 niveles para factor A • 2 niveles para cada factor
• 3 niveles para factor B
Cuales son la variables con mayor influencia en la respuesta?

Cual es la configuración de factores que optimizan la Respuesta?
K = número de factores; 2  dos niveles (-1 ,+1)
 Numero de corridas = 2K
 En un diseño factorial completo de 2
niveles, cada factor experimental tiene
solo dos niveles
 Las corridas experimentales incluyen
todas las combinaciones de los niveles
de los factores
 Identifican tendencias importantes, por
sirven de base para experimentación
adicional  convertir a diseño central
compuesto  encontrar un
configuración óptima
Problema: El número de corridas crece exponencialmente al aumentar los factores

 Son una alternativa a los diseños factoriales completos cuando el número de factores
se incrementa  Ventaja: Menor costo y tiempo
 Utilizan una fracción seleccionada de un factorial completo para obtener información
sobre los efectos principales y las interacciones de orden inferior
 Sirven para identificar los factores más importantes que afectan a la respuesta
 Desventaja: Las interacciones de varios efectos se confunden entre sí o a veces con
efectos principales  El grado de confusión es la resolución del diseño
Contiene 2k-p corridas y se conoce

como fracción 1/2p del diseño
factorial 2k
Estos diseños requieren “p”
generadores independientes

 Design generator (Generador de Diseño):
 Se utiliza para generar un diseño factorial fraccional. Permite determinar la relación
de definición
 Defining Relation (Relación de definición)
 Es la colección total de generadores de diseño, incluyendo los productos de los
generadores
 Confounding (Confundido):
 Cuando los términos son indistinguibles de uno a otro. Los efectos no pueden
estimarse independientemente
 Alias Structure (Estructuras Aliadas):
 Describe el patrón de confusión que ocurre en el diseño. Los términos confundidos
esta aliados
 Resolución:
 La extensión a la que las interacciones en un diseño están aliadas con otros factores
e interacciones

Si p = 1, the DOE contiene 23-1 corridas y se
conoce como fracción 1/21 del diseño factorial 23
+c
C b
+
-
(1) - B
A +a-
Design Generator: C = AB
Or C = -AB
Defining Relation:
I = ABC or I = -ABC

Factors: 5 Base Design: 5, 16 Resolution: V
Runs: 16 Replicates: 1 Fraction: 1/2
Blocks: 1 Center pts (total): 0
 Resolución III: Design Generators: E = ABCD
 Los efectos principales forman Defining Relation: I = ABCDE
estructuras de alias con las Alias Structure

interacciones de 2 factores I + ABCDE
 Resolución IV:
 Algunas interacciones de 2 factores A + BCDE
forman estructuras de alias con B + ACDE
otras interacciones de 2 factores y C + ABDE
los efectos principales forman
estructuras de alias con las D + ABCE
interacciones de 3 factores E + ABCD
 Resolución V: AB + CDE
Las interacciones de 2 factores

AC + BDE

forman estructuras de alias con las AD + BCE
interacciones de 3 factores y los AE + BCD

efectos principales forman BC + ADE
estructuras de alias con las BD + ACE
interacciones de 4 factores.
BE + ACD
CD + ABE
CE + ABD
DE + ABC

Modelo empírico que se ajusta a datos experimentales de 2K
Ejemplo: Modelo para tres factores y dos niveles
Y = β0+ β1X1+β2X2+ β3X3+β12X1X2 + β13X1X3+ β23X2X3 + β123X1X2X3+ ε
Y: Respuesta
X1, X2, X3: Factores
β0, β1, β2, β3, β12, β13, β23, β123: Coeficientes lineales a determinar con los
datos
ε: Error experimental

Y = β0+ β1X1+ β2X2+ β3X3 + β12X1X2+β13X1X3+
β23X2X3+ β123X1X2X3 + ε
• Efectos principales
• Efectos debido a los factores X’s
• Interacciones
• Efectos debido al conjunto de dos o más factores
actuando simultáneamente

Analysis of Variance
Source DF Adj SS Adj MS F-Value P-Value

Model 3 0.98432 0.32811 24.06 0.000
Linear 2 0.96931 0.48466 35.54 0.000
Presión 1 0.07156 0.07156 5.25 0.041
Tipo_Base 1 0.89776 0.89776 65.84 0.000
2-Way Interactions 1 0.01501 0.01501 1.10 0.315
Presión*Tipo_Base 1 0.01501 0.01501 1.10 0.315
Error 12 0.16362 0.01364
Total 15 1.14794
Model Summary
S R-sq R-sq(adj) R-sq(pred)
0.116771 85.75% 82.18% 74.66%
 R-cuadrado (R-sq)
 R2 es el % de la variación en la respuesta explicada por el modelo. Cuanto mayor sea R2 mejor
el modelo se ajusta a los datos
 El valor F (F-value)
 Es una prueba estadística que se utiliza para determinar si el término está asociado con la
respuesta
 S es la Desviación Standard

 Se agregan puntos centrales al DOE por 2 razones:
 Medir estabilidad del proceso
 Determinar si hay o no curvatura en superficie de respuesta

Y = β0+ β1X1+β2X2+ β3X3+β12X1X2 + β13X1X3+ β23X2X3 + β11(X1)2 + β22(X2)2 + ε

α = Distancia de los ‘punto estrellas” al punto central
CCF
CCI
CCC
CCC: Circumscribed; CCF: Faced centered; CCI: Inscribed

• Es un tipo de diseño de superficie respuesta que no tiene un diseño factorial o
factorial fraccionado incrustado
• Tienen combinaciones de tratamiento que están en los puntos medios de los
bordes del espacio experimental y requieren al menos tres factores continuos
• Estiman eficientemente los coeficientes de 1er y 2nd orden
• Como tienen menos puntos de diseño, pueden ser menos costosos de realizar
que los diseños centrales compuestos con el mismo número de factores
• No son adecuados para los experimentos secuenciales
• Pueden ser útiles si se conoce la zona de operación segura de su proceso

• Diseños Box-Behnken
requieren menos corridas
• Requiere mas conocimiento
del proceso estudiado

 Taguchi recomienda el uso de
arreglos ortogonales para hacer
matrices que contengan los
controles y factores de ruido en
DOE
 Pueden aplicarse a DOEs
involucrando un gran numero de
Arreglo Ortogonal L12 y Razón S/R
factores
 Estiman la contribución de los
factores individuales en la calidad
 “Gana” las mejores condiciones para
un proceso
 Desventaja: Solo se aplican en la
etapa inicial del diseño del sistema
del producto o proceso

“ Fabricante usa un primer (base) para mejorar la adhesión de pintura de carro”
Pregunta: ¿ que tipo de base y nivel presión de spray maximiza la adhesión?
Diseño Factorial completo: 2 factores; 2 niveles; 4 réplicas

Factores: Pressure : (310, 380 kPa)
Primer type: One, Two
Adhesion Fuerza para despegar la pintura de la base metálica
Ingrese los siguientes mediciones (respuestas) a la filas 1-16 de C7 (Adhesion)

4.52 4.55 5.05 4.88 4.48 4.37 4.89 4.75 4.29 4.43 5.14 4.91 4.60 4.25 4.95 4.71
Nota: asegúrese que su diseño esta en “standard order”

• Pequeñas ruedas plásticas son producidas por proceso de moldeo por injección
• Se diseña un experimento con el objetivo de maximizar la resistencia de la piezas
Factores Niveles
-1 +1
A: Mold Temp (°C) 130 170
B: Nozzle Temp (°C) 350 375
C: Shot Size (Oz) 6.7 10
D: Injection Press (psi) 700 900
Los Ingenieros sospechan la existencia de interacciones AxB y AxD;

descartando otro tipo de interacciones

 Un diseño factorial completo permitiría la evaluación de los 4 factores y todas
las interacciones, al costo de 16 corridas (runs)
 Si el criterio de los ingenieros es correcta (solo 2 tipos de interacciones
probablemente existan) entonces una resolución IV será suficiente y solo 8
corridas será suficiente
Fractional Factorial Design
Factors: 4 Base Design: 4, 8 Resolution: IV

Runs: 8 Replicates: 1 Fraction: 1/2
Blocks: 1 Center pts (total): 0
Design Generators: D = ABC
Alias Structure
I + ABCD
A + BCD
B + ACD
C + ABD
D + ABC
AB + CD
AC + BD
AD + BC

Se ejecutarón 2 corridas “replicates” por cada combinación
A B C D
Std Run Nozzle Injection Replicates
Mold Temp Shot Size
Order Order Temp Press Data1 Data2
1 1 -1 -1 -1 -1 63 59
2 2 1 -1 -1 1 60 65
3 3 -1 1 -1 1 77 85
4 4 1 1 -1 -1 60 62
5 5 -1 -1 1 1 68 70
6 6 1 -1 1 -1 35 39
7 7 -1 1 1 -1 35 36
8 8 1 1 1 1 47 45

Diseño de un DOE Factorial Completo para evaluar Indice de Refracción de
Películas delgadas de Oxinitruro de Silicio Analizar curvatura  Si hay
curvatura agregar puntos experimentales para convertirla en Diseño Central
Compuesta

# de Factores = 4; Niveles = 2; # de puntos centrales = 3
Realizar el experimento de forma aleatoria
 SiON Films:
 SiH4 Flow = (14) sccm
 N2O Flow = (300, 1700) sccm
 Síntesis de películas delgadas de
 NH3 Flow = (50, 90) sccm
Oxinitruro de Silicio por PECVD
 N2 Flow = (500) sccm
• Producir Películas con un Indice  Power = (40, 80) Watts
de refracción (RI) a 1300nm =  Pressure = (700,1100) mTorr
1.51 – 1.52  Platen/SH Temp. = 300oC/250oC

(Ref. O. Celep, E.Y. Yazici)
 El mineral es refractario y se necesita molienda ultra-fina para extraer

Plata por cianuración
 El efecto del diámetro de las bolas (2 – 4.5mm), velocidad de agitación
(200 – 800 rpm) y ratio bolas/carga (50% - 80%) es analizado usando el
diseño Box-Behnken
Nivel de significancia α = 0.05)
 Resultados sugieren que la velocidad de agitación y ratio bolas/carga son

relevantes estadísticamente
 Se determinó un modelo de regresión con un R2 = 0.96
 El producto más fino con un d80 de 2.73um se obtuvo con bolas de 2mm,
velocidad de agitación de 800 rpm y ratio bolas/carga de 80%

Modelo de regresión cuadrática de segundo orden:
Y = 6.52 +1.28x1 -4.27x2 -1.52 x3 -1.07(x1) 2 +

2.81(x2)2 +0.88(x3)2 - 0.45x1x2 + 0.08x1x3 + 1.11x2x3

Research Article
Friction Performance of Al-10%SiCp Reinforced Metal Matrix
Composites Using Taguchi Method
Shouvik Ghosh, Prasanta Sahoo, and Goutam Sutradhar
 Material structural  Propiedades: livianos y alta dureza

 This is an Al metal matrix composite (MMC) reinforced with SiC particles –
Liquid metallurgy route using LM6 Aluminum and SiC particles (size ~ 37um)
by varying the weight fraction of SiC in the range of 5% - 10%
 Material is synthesized by stir casting process in an electric melting furnace
 Materials were subject to wear testing in a multitribotester using block on
roller configuration

 DOE based on L27 Taguchi Orthogonal array to acquire wear data
 Analysis of variance is employed to investigate the influence of four
controlling parameters:
 Normal load, Sliding speed, and Sliding time on the dry sliding wear of
the composite
 What are the most significant effects? What is the most optimal
combination? What is the nature of surface wearing?

Agregar interacciones: LxS, LxT y xT

Interaction Plot for SN ratios
Data Means
1 2 3
11.0 Load
1
2
9.5 Load 3
8.0
11.0 Speed
1
2
Speed 9.5 3
8.0
11.0 Time
1
2
9.5 Time 3
8.0
1 2 3 1 2 3
Signal-to-noise: Smaller is better
Combination for minimum friction is found to be L3S1T1, that is, the highest level of
normal load and lowest levels of speed and time. All the factors applied load (𝐿𝐿𝐿𝐿), speed (
𝑆𝑆𝑆𝑆), and time (𝑇𝑇𝑇𝑇) are found to affect the friction significantly. But the factor load (𝐿𝐿𝐿𝐿) is
the most important factor with a contribution of 63.20%. The interaction between load
and speed (𝐿𝐿𝐿𝐿 𝐿𝐿 𝐿𝐿𝐿𝐿) is found to be the most significant interaction.

SEM image of worn surface of Al-10%SiCp composite

Response Surface Design
Design Type: Box-Behnken
EXN03 Minitab - Relaves de Plata
See discussions, stats, and author profiles for this publication at: http://www.researchgate.net/publication/259500882
Ultra-fine Grinding of Silver Plant Tailings of a

Refractory Ore Using a Vertical Stirred Media
Mill
ARTICLE in TRANSACTIONS OF NONFERROUS METALS SOCIETY OF CHINA · NOVEMBER 2013

Impact Factor: 1.18 · DOI: 10.1016/S1003-6326(13)62882-4
CITATIONS READS
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2 AUTHORS:
Oktay Celep Ersin Y Yazici

Karadeniz Technical University Karadeniz Technical University
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Available from: Oktay Celep

Retrieved on: 01 October 2015
Trans. Nonferrous Met. Soc. China 23(2013) 34123420
Ultra fine grinding of silver plant tailings of

refractory ore using vertical stirred media mill
O. CELEP, E. Y. YAZICI
UFG Group, Division of Mineral & Coal Processing, Department of Mining Engineering,
Karadeniz Technical University, Trabzon 61080, Turkiye
Received 21 March 2013; accepted 25 April 2013
Abstract: Ultra fine grinding of the plant tailings of a refractory silver ore was studied using a laboratory type vertical stirred media
mill. Preliminary tests confirmed that ultra fine grinding substantially improves the extraction of silver from the tailings in cyanide
leaching (i.e. 36% Ag extraction rate from the as-received tailings with d80 of 100 μm, c.f. 84% extraction rate after ultra fine
grinding of the tailings with d80 of 1.2 μm). In the ultra fine grinding tests, the effects of ball diameter (24.5 mm), stirring speed
(200800 r/min) and ball charge ratio (50%80%) on the fineness of grind (d80, Pm) were investigated through a BoxBehnken
design. Increasing stirrer speed and ball charge ratio decreased fineness of grind while larger balls resulted in the coarser products.
The tests demonstrated that a fineness of grind less than 5 Pm can be achieved under suitable conditions. Analysis of stress intensity
indicated an optimum range of stress intensity of (0.82)×103 N·m for all power inputs.
Key words: refractory ore tailings; stirred media mill; ultra fine grinding; experimental design; BoxBehnken design; stress intensity
Stirred Media Detritor (SMD®) and ISAMill® have been

1 Introduction the most commonly used stirred media mills in mineral
processing. The various types (e.g. glass, steel, ceramic,
Refractory ores yield low extractions rates (i.e. pebble etc.) and sizes (usually between 200 and 4000 μm)
<80%) of gold and silver in cyanide leaching even after of grinding media were used depending on the feed size
grinding the ore down to 75 Pm. These ores need a and feed material [11,12].
suitable pretreatment to achieve high gold and silver Various process parameters including stirrer speed,
extractions rates during cyanidation [1]. Roasting [2], ball diameter, ball charge ratio and media density as well
pressure oxidation [3], biooxidation [4,5] and ultra fine as mineral type affect the performance of a grinding
grinding [6] have been commercially practiced to process [11,1318]. Many studies have been carried out
enhance the gold/silver recoveries from refractory ores. to examine the operating parameters affecting the
The most common cause of refractoriness in gold and grinding performance of stirred media mills [15,16,19].
silver ores is the encapsulation of fine gold and silver One classical factor at a time approach may fail in
particles within the mineral matrix in which these determining main and interaction effects together and
particles are not accessible to the lixiviating action of optimising grinding parameters [20]. In this respect, the
cyanide and oxygen [7]. If the encapsulated gold is 12 statistical experimental design methods can be suitably
μm to approximately 20 μm in size, a desired degree of utilized to assess the main/interaction effects of
liberation can be suitably achieved by ultra fine grinding parameters. Response surface methodology (RSM) is
(UFG) without the need for costly and environmentally widely used since it combines mathematical and
unfavorable chemical pretreatments [6,8]. statistical methods [8,2124]. Stress intensity analysis of
In the last 20 years, the stirred media mills have grinding media based on grinding parameters such as
been widely used for ultra fine grinding in different stirrer speed, ball diameter and media height as well as
industrial fields such as mineral processing, plastic, slurry density, can be used to identify the optimum
ceramics, paint, food and cosmetic [9,10]. Vertimill®, conditions at a given energy consumption [9,11].
Corresponding author: O. CELEP; Tel: +90-462-377-4118; Fax: +90-462-325-7405; E-mail: ocelep@ktu.edu.tr

DOI: 10.1016/S1003-6326(13)62882-4
O. CELEP, et al/Trans. Nonferrous Met. Soc. China 23(2013) 34123420 3413
Recently, application of ultra fine grinding using mill designed by the authors (Fig. 1) within a batch mode
stirred media mills for the treatment of refractory gold of operation. The technical features of the stirred media
and platinum ores prior to leaching, has been increased mill were described earlier by CELEP et al [8]. Energy
dramatically to improve the metal recoveries [25,26]. consumptions in the grinding tests were measured using
Old plant tailings, which were produced by conventional an electrical counter connected to the stirrer rotor.
comminution circuits, may also contain substantial Micro-grinding ceramic beads (alumina-based zirconia
amount of precious metals. Chemical pretreatment of toughened, DMM AZ 2000®) with different sizes (mean
such tailings may fail to improve the extraction of diameters of 2, 3.5 and 4.5 mm) were kindly provided by
precious metals [27]. Ultra fine grinding as a Dakot Milling Media (Pty) Ltd. (South Africa) and used
pretreatment step can be exploited as a potentially new as the grinding media. The beads had Al2O3 content of
approach for reprocessing of such plant tailings to 80%, specific gravity (SG) of 3.753.80 and Vickers
recover contained metal/mineral values, which would hardness (HV) of 1314 m. Utilization of inert ceramic
also contribute to the conservation of natural resources. grinding media would avoid/limit adverse effects of steel
In this study, the ultra fine grinding of the plant media during leaching through formation and subsequent
tailings of a refractory silver ore was studied to recover coating of iron oxide on mineral surfaces [29]. In the
the contained silver in subsequent cyanidation. The tests, the pulp density was kept at 24% (w/v). Analysis of
effects of ball diameter (24.5 mm), stirring speed particle size of the samples was carried out by the laser
(200800 r/min) and ball charge ratio (50%80%) on the diffraction method using a Malvern Mastersizer 2000
ultra fine grinding process were investigated using a MU. Particle size analysis was performed in four
laboratory type vertical stirred media mill. Response replicates (RSD: 0.71%) and the mean values were
surface methodology, a three-level BoxBehnken design, present in the results.
was adopted to assess the effect of parameters on the
response, i.e. particle size (d80) of the product. Grinding
efficiency in terms of stress number and intensity
concept was also evaluated.
2 Materials and methods
2.1 Tailing sample and preliminary cyanidation tests

The plant tailings after cyanide leaching (d80=100
μm) of a refractory silver ore were used in this work. The
chemical composition of the ore sample was determined
by wet chemical analysis method using ICPAES
(inductively coupled plasmaatomic emission
spectroscopy), NAA (neutron activation analysis) after
hot digestion in aqua regia for AuAg analysis and XRF
analysis for major oxides. The tailing sample consisted
Fig. 1 Section drawing of stirred mill used in ultrafine grinding
of 50.7% SiO2, 9.80% BaO, 7.30% Al2O3, 6.76% CaO
tests [8] (1üMotor for moving of grinding chamber; 2üMotor
and 5.72% Fe2O3. The sample was determined to be rich
of stirring shaft; 3üConnection of motor and shaft; 4üStirring
in silver containing 83 g/t Ag and 1.5 g/t Au. Earlier
pins; 5 ü Grinding chamber; 6 ü Moving table of stirred
mineralogical studies on the tailings have shown that
grinding chamber; 7üStability table; 8üControl panel)
silver is present mainly in the form of native silver,
pyrargyrite, tetrahedrite, argentite and proustite, which
2.3 Experimental design
are closely associated with and/or encapsulated in other
Response surface methodology (RSM) involves the
mineral phases, i.e. mainly barite, quartz, dolomite and
utilization of mathematical and statistical techniques and
feldspar [27]. Earlier studies have confirmed poor
allows the evaluation of contribution of several
extraction of silver even after various chemical
independent parameters (variables) on the response. A
pretreatments of the tailings [27]. Details of the
BoxBehnken design (BBD), essentially a type of RSM,
procedure for cyanide leaching and chemical analysis
has three levels, low (1), center (0) and high (+1) as
can be found elsewhere [28].
coded levels, with equally spaced intervals among these
levels. Actual levels can be calculated by [30]
2.2 Ultra fine grinding tests
Ultra fine grinding experiments were performed X high X low
X center (1)
using a laboratory scale pin-type vertical stirred media 2
3414 O. CELEP, et al/Trans. Nonferrous Met. Soc. China 23(2013) 34123420
The relationship between the coded and actual events of each product particle and affects product
(uncoded) values can be obtained by fineness for a given stress intensity and expressed as
[14,33]
X actual X center
xcoded (2)
X center X min N c Ps
Ns (5)
Np
where xcoded is coded value; Xactual, Xcenter and Xmin are
corresponding actual value, actual value in the center and where Nc, Ps and Np are the number of media contacts,
minimum (low) actual value, respectively. The number the probability of stressing of a particle at a media
of experiments (N) required for a Box–Behnken design contact and the number of product particles inside the
can be calculated as mill, respectively. In the case of grinding of crystalline
N=n2+n+cp (3) materials, the following proportionality is derived [14].
where n and cp are the number of parameters and MGM (1 H ) nt

Ns v (6)
replicates in the central point, respectively [21,30]. [1 MGM (1 H )]cv d GM
2
Accordingly, 15 experiments are needed for a three-

where n is the number of revolutions of the stirrer per
variable design (n=3) with three replicate experiments
unit time, t is the grinding time, MGM is the filling ratio of
(cp=3) in the central point. A second-order mathematical
the grinding media, H is the porosity of the bulk of
model can be built to estimate the response (Y) based on
grinding media, dGM is the diameter of the grinding
the experimental data.
media, and cv is the volume concentration of the pulp.
E 0 E1 x1 E 2 x2 E 3 x3 E11 x12 E 22 x22 E 33 x32 Stress intensity describes the energy involved in a
E12 x1 x2 E13 x1 x3 E 23 x2 x3 (4) breakage event. There is an optimal range for this energy
required to break a particle. When the stress intensity
where Y is the predicted response; 0 is the model
produced is smaller than the required level, the number
constant; x1, x2, x3 and x4 are independent variables; 1, 2,
of stress events should be increased to break a particle,
3 and 4 are linear coefficients; 12, 13 and 23 are
i.e. low breakage rate. The stress intensity beyond the
interaction coefficients; 11, 22 and 33 are the quadratic
optimum range will lead to the excessive consumption of
coefficients [20,30].
energy [11]. Stress intensity analysis was primarily
In the current study, BBD was adopted to assess the
developed for high-speed horizontal stirred media mills
effect of the parameters (i.e. ball diameter, stirrer speed
and ball charge ratio) on the particle size (d80) of the in which grinding event is governed mainly by
ground material over 15 min of grinding. Selected centrifugal forces. In low-speed vertical stirred media
variables and their corresponding levels in the ultra fine mills, gravity forces also take action [11,34]. Centrifugal
grinding tests are presented in Table 1. Minitab [31] and forces become more important at high stirring speeds (i.e.
DesignExpert [32] software were used to perform the a tip speed of >3 m/s) in a pin type vertical mill while the
statistical analysis of the experimental data. gravitational forces are more dominant at low stirring
speeds (<3 m/s), particularly for industrial applications
Table 1 Parameters and their corresponding coded and actual where media height is up to 2 m [34]. The gravitational
levels (Igm) and centrifugal stress intensities (Ism where the
Symbol Coded level modulus of elasticity of the feed material is smaller than
Parameter that of grinding media) can be expressed by Eq. (7) and
Low Center High
Actual Coded
(1) (0) (+1)
Eq. (8), respectively [11,35].
Ball diameter/mm a X1 x1 2 3.5 4.5 I gm v Dm2 ( U m U ) gh (7)

Stirring
X2 x2 200 b 500 c 800 d I sm v Dm3 ( U m U )Q t2 (8)
speed/(r·min1)
Ball charge ratio/% X3 x3 50 65 80 where Igm and Ism are gravitational and centrifugal stress
a
Due to practical reasons, selected ball diameters do not match precisely intensities of the grinding media, respectively; Dm is the
with BBD's experimental layout; b 0.77 m/s; c 1.92 m/s; d 3.07 m/s. grinding media size; Um is the grinding media density; U
is the slurry density; g is the gravitational constant; h is
2.4 Stress number and intensity of grinding media the media height; Qt is the stirrer tip speed.
In stirred media mills, comminution process is It can be seen from Eqs. (7) and (8) that in a vertical
controlled intimately by the number (Ns) and intensity (Is) stirred media mill, stress intensity reflects the combined
of the stress generated within the grinding environment. effects of stirring speed (or media height), media size and
Stress number is referred as the average number of stress density as well as slurry density [34,35]. In this respect,
the performance of a stirred mill as a function of those
grinding parameters can be evaluated by analysis of
stress intensity [35]. In this study, the stress number and
intensity were calculated using the data obtained and
plotted as a function of product particle size (d80).
3 Results and discussion
3.1 Preliminary cyanidation tests

Ultra fine grinding of the tailings can substantially
enhance the cyanide leaching of silver, i.e. 84% silver
extraction rate after ultra fine grinding (d80=1.2 μm) even
at 1 h, while only 36% extraction rate for the as-received
tailings (d80=100 μm) (Fig. 2). This suggests that ultra
fine grinding is a suitable pretreatment method for the
tailings. Therefore, ultra fine grinding of the tailings was
studied and the effects of grinding parameters were
evaluated using BoxBehnken design as well as stress
intensity/number approach.
Fig. 2 Effect of particle size on extraction of silver in cyanide

solutions (1.5 g/L NaCN; pH 10.5; temperature: (25r3) qC;
flow rate of air: 0.3 L/min; pulp density: 24% (w/v))
3.2 Effect of grinding time

Fineness of grind (expressed as d80) obtained for
Fig. 3 Effect of grinding time on particle size (d80) with
different grinding periods (i.e. 1, 4 and 15 min) was used
different parameters: (a) Stirring speed (3.5 mm ball diameter,
to assess the effect of grinding time under the different 80% ball charge ratio); (b) Ball diameter (800 r/min stirring
conditions of stirring speeds, ball diameters and ball speed, 80% ball charge ratio); (c) Ball charge ratio (2 mm ball
charge ratios (Fig. 3). The increase in grinding time from diameter, 500 r/min stirring speed)
1 to 15 min had an important effect on the fineness of the
product (Fig. 3). Longer periods (>4 min) were needed to the relative contribution of these parameters to the
achieve d80<5 Pm. Accordingly, a constant grinding time fineness of product was further evaluated by the
of 15 min was taken for the design of grinding tests. BoxBehnken design below.
Figure 3 also reflects the effect of stirring speed, ball
diameter and ball charge ratio on d80 of the product as a 3.3 Evaluation of experimental data
function of grinding time. It can be concluded that The experimental layout produced by BoxBehnken
increasing stirring speed and ball charge ratio or using design for 15 experiments is shown in Table 2. Parameter
small balls leads to the finer products. Furthermore, combinations with coded/actual values for each
experiment and observed/predicted results (d80) are also probability that the test statistic will take on a value that
included in Table 2. The predicted values were estimated is at least as extreme as the observed value of the statistic
by the regression model described in Section 3.3.1. The when the null hypothesis (H0) holds true. Simply, a P
relative standard deviation (RSD) of the data was value <0.05 suggests that the null hypothesis is rejectd).
calculated as 2.31%. If the P value is lower than the confidence level in the
3.3.1 Modelling and statistical analysis significance test, it is statistically significant according to
The observed experimental results (d80) (Table 2) the selected confidence level. For example, if P=0.04
were employed to establish a second-order regression <=0.05, it shows the significance of a parameter at a
model. An unknown response (Y in d80) can be estimated confidence level of 95% (=0.05) [21]. In this respect,
for any coded level of ball diameter (x1), stirrer speed (x2) the P value (0.001) of the regression model confirms
and ball charge ratio (x3). the adequacy of the model, i.e. statistically significant
even at 99.5% (=0.005) confidence level (Table 3). The
Y 6.52 1.28 x1 4.27 x2 1.52 x3 1.07 x12 linear (main) and square (quadratic) contributions were
2.81x 22 0.88 x32 0.45 x1 x2 0.08 x1 x3 1.11 x2 x3 also found to be significant at 95% (=0.05) and
(9) interactions were found to be insignificant.
The analysis of variance (ANOVA) for the Table 4 shows the estimated regression coefficients
regression model and linear/square/interaction used to construct the model with their statistical
contributions is presented in Table 3. P values were significance test. It was also confirmed that all the linear
used for the significance test. The P value shows the (main) and square (quadratic) effects were significant at
Table 2 Box-Behnken design layout with coded and actual values with observed results (d80)
Level of parameter d80/Pm
Experimental No. Coded Actual
Observed Predicted
x1 x2 x3 X1/mm X2/(r·min1) X3/%
1 1 1 0 2 200 65 9.72 10.80
2 +1 1 0 4.5 200 65 13.8 14.25
3 1 +1 0 2 800 65 3.64 3.16
4 +1 +1 0 4.5 800 65 5.90 4.82
5 1 0 1 2 500 50 6.34 6.64
6 +1 0 1 4.5 500 50 8.15 9.05
7 1 0 +1 2 500 80 4.35 3.45
8 +1 0 +1 4.5 500 80 6.46 6.16
9 0 1 1 3.5 200 50 18.5 17.11
10 0 +1 1 3.5 800 50 6.18 6.35
11 0 1 +1 3.5 200 80 12.0 11.85
12 0 +1 +1 3.5 800 80 4.15 5.53
13 0 0 0 3.5 500 65 6.42 6.52
14 0 0 0 3.5 500 65 6.69 6.52
15 0 0 0 3.5 500 65 6.45 6.52
Table 3 Analysis of variance (ANOVA) for regression model

Source Degree of freedom Sum of square Adjusted sum of square Adjusted mean square P value Contribution/%
Regression
9 220.514 220.514 24.5016 0.004 96.3
model
Linear 3 177.309 177.309 59.1031 0.001 77.4
Square 3 37.447 37.447 12.4822 0.028 16.4
Interaction 3 5.759 5.759 1.9195 0.420 2.51
Residual error 5 8.474 8.474 1.6949 3.70
Total 14 228.989 100
Table 4 Estimated regression coefficients and test of statistical
significance for analysis of model terms
Regression Standard error
Item Symbol P value
coefficient of coefficient
Constant 0 6.52067 0.7516 0.000
Ball diameter 1 1.27888 0.4603 0.039
Stirring speed 2 4.26800 0.4603 0.000
Ball charge
3 1.52062 0.4603 0.021
ratio
Ball diameter
11 1.07258 0.6775 0.174
ball diameter
Stirring speed
22 2.80967 0.6775 0.009
stirring speed
Ball charge
ratioball 33 0.87942 0.6775 0.251 Fig. 4 Correlation between observed and predicted d80
charge ratio
Ball diameter 3.3.2 Response surface plots of parameters
12 0.44875 0.6509 0.521
stirring speed Regression equations can be used to derive response
Ball diameter surface plots for couples of variables. These plots are
ball charge 13 0.07500 0.6509 0.913 practical in terms of simultaneous observation of the
ratio
effects of dual variables on the response. In the current
Stirrer speed study, three surface plots were produced by showing the
ball charge 23 1.11025 0.6509 0.149
simultaneous effects of two parameters on the particle
ratio
size (d80) while the third parameter was held at the center
level (Fig. 5).
95% (=0.05) with the exception of quadratic effect of
Figure 5(a) shows that the increase in stirring speed
ball diameter, i.e. P>0.05. The contributions show the
resulted in a finer product at all levels of ball diameter
relative impact of linear, square and interaction effects
while larger balls led to a coarser product. As also
with the linear effects being the most dominant (77.4%)
confirmed by the statistical analysis (Table 4), stirring
(Table 3). It can be inferred from the absolute values of
speed had a greater effect than the ball diameter.
the regression coefficients (Table 4) that the order of
Increasing the stirring speed from 200 to 800 r/min (i.e.
significance of linear (main) effects was stirring
the 9th and 10th runs, 3.5 mm ball diameter, 50% ball
speed>ball charge ratio>ball diameter. The mode and
charge ratio) produced one third finer material. CELEP et
magnitude of effects can be observed from the response
al [8] also reported that when the stirring speed was
surface plots (see Section 3.3.2). The coefficient of
increased from 250 to 750 r/min, the product particle size
multiple determinations (R2) for the regression model
(d80) decreased from 9 μm to 4 μm when using 1 mm
was found to be 0.96 (Fig. 4).
Further grinding tests apart from BoxBehnken balls in diameter. In contrast to the findings in the current
design were also performed to test/verify the regression study (Figs. 5(a) and (c)), previous researchers [10,18,
model. Parameter combinations for the tests with the 36] reported that high speeds (up to 1350 r/min) resulted
observed and the predicted results are presented in Table in an increase in the mean particle size with a reduction
5. It can be noted that, in the 16th run the finest particle in the energy efficiency. This adverse effect of stirring
size (d80=2.73 Pm) was obtained (Table 5) under the speed at high levels can be attributed to the occurrence of
conditions of 2 mm ball diameter, 800 r/min stirring central vortex during grinding which increased energy
speed and 80% ball charge ratio. consumption dramatically [14,36].
Table 5 Verification experiments with observed/predicted d80

d80/Pm
Experimental No. Ball diameter level Stirring speed level Ball charge ratio level
Observed Predicted
16 1 (2 mm) +1 (800 r/min) +1 (80%) 2.73 3.55
17 +1 (4.5 mm) +1 (800 r/min) +1 (80%) 4.91 5.36
18 1 (2 mm) 0 (500 r/min) 0 (65%) 5.26 4.17
related with the reduction in grinding efficiency as the
ball charge ratio declines. In stirred media mill
applications, higher ball charge ratios (typically up to
85%) than the conventional grinding systems (40%
50%) were employed [37,39]. The findings in the current
study (Figs. 5(b) and (c)) also confirmed that using high
ball charge ratios is necessary to achieve finer particle
sizes. However, it should be noted that increasing ball
charge ratio will cause an increase in power draw of the
mill [8,37].
Simultaneous effect of ball charge ratio and stirring
speed on particle size is shown in Fig. 5(c). The large
magnitude of effect of stirring speed was observed at all
the ball charge ratios tested. The contribution of ball
charge ratio was apparent particularly at low stirring
speeds.
Figure 6 presents the effects of stirring speed, ball
diameter and ball charge ratio on energy consumption
over 15 min grinding period. Energy consumption was
determined to increase by 40183 kW·h/t with increasing
stirring speed, ball diameter and ball charge ratio.
Fig. 5 Surface plots reflecting simultaneous effect of dual

variables on particle size d80 (Three variables are held at centre
level): (a) Ball diameter and stirring speed; (b) Ball diameter
and ball charge ratio; (c) Ball charge ratio and stirring speed Fig. 6 Relationship of energy consumption depending on
stirring speed (2 mm ball diameter, 65% ball charge ratio), ball
Selection of ball diameter is also of importance diameter (800 r/min stirring speed, 80% ball charge ratio) and
regarding stirred milling efficiency and energy ball charge ratio (2 mm ball diameter, 500 r/min stirring speed)
consumption [37]. Smaller media are required to obtain with 15 min grinding time
finer products, namely, the decrease in ball diameter
from 4.5 to 2 mm (the 5th and 6th runs, 500 r/min 3.4 Evaluation of grinding efficiency using stress
stirring speed, 50% ball charge ratio) reduced the particle number and intensity analysis
size (d80) from 8.15 to 6.34 Pm. It was suggested that Figure 7 illustrates the product particle size (d80) as
optimum ball-to-particle size ratio should be selected as a function of stress number at a ball charge ratio of 80%.
20:1 for the maximum breakage rate [38]. However, the Particle size had a tendency to decrease with the increase
ratio may vary from 7:1 to 20:1 depending on the in stress number (Fig. 7). Smaller balls (2 mm) allowed
content/quantity of minerals in the ore and type of the production of higher stress number and, hence, finer
grinding media [15]. In the current study, the material. KWADE and SCHWEDES [33] reported
ball-to-particle size ratio varied between 8:1 and 18:1. similar findings for the comminution of limestone in a
Figure 5(b) confirms the beneficial effect of decreasing stirred media mill. However, they also observed no
ball diameter on the fineness of the product. decrease in the product fineness below a critical ball
It can be also seen from Fig. 5(b) that finer products diameter (d399 Pm). These researchers claimed that this
can be obtained at higher ball charge ratios. This can be adverse effect is due to the fact that in the initial stages of
grinding, small balls cannot generate sufficient stress
intensity. 4 Conclusions
Figure 8 demonstrates the effect of centrifugal stress
intensity on product particle size (d80) and corresponding Application of ultra fine grinding to cyanidation
stress number at energy consumption levels of 260 and plant tailings as a potential treatment method for the
920 kW·h/t. The optimal stress intensity was identified recovery of silver contained was studied. The effects of
within the range of (0.82)×103 N·m while finer ball diameter (24.5 mm), stirring speed (200800 r/min)
material was produced at a high energy consumption, and ball charge ratio (50%80%) on ultra-fine grinding
920 kW·h/t. Outside of this optimal range of stress of the tailings were demonstrated at three levels using a
intensity, coarser material was obtained even at high BoxBehnken design. The findings showed that stirring
stress intensities (>2×103 N·m). Figure 8 also shows that speed, media size and ball charge ratio were statistically
in the optimal range of stress intensity ((0.82)×103 significant parameters regarding their contributions to
N·m), the stress number was also maximized. A similar the fineness of the product. A regression model with a
trend was also observed for gravitational stress intensity coefficient of determination (R2) of 0.96 was derived. It
(data not shown). This also confirmed that media height was shown that a product finer than 5 Pm can be
(i.e. ball charge ratio) is of practical importance for produced under the suitable conditions using ceramic
grinding efficiency. These findings confirmed that stress beads. The finest product with d80 of 2.73 Pm was
intensity analysis can be suitably used to determine the obtained under the conditions of ball diameter of 2 mm,
optimum conditions of grinding parameters to achieve stirring speed of 800 r/min and ball charge ratio of 80%
the desired product fineness. over 15 min. Energy consumption was increased with
increasing the level of each grinding parameter tested.
The grinding process was controlled closely by the stress
intensity, which had an optimal range of (0.82)×103
N·m to obtain a finer product.
Acknowledgements
The authors would like to express their sincere
thanks and appreciation to Dr. brahim Alp and Yildizlar
Holding for kindly providing the tailings sample, to Dr.
Haci Deveci for proof reading the article and to Dakot
Milling Media (Pty) Ltd (South Africa) for kindly
providing the ceramic micro-grinding beads (DMM AZ
2000®).
Fig. 7 Dependency of product particle size (d80) on stress References

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ゟᓣ᧙ᢠ㒚⺼䲒໘⧚䫊ॖሒⷓ
O. CELEP, E. Y. YAZICI
UFG Group, Division of Mineral & Coal Processing, Department of Mining Engineering,
Karadeniz Technical University, Trabzon 61080, Turkiye
ᨬ㽕˖䞛⫼ᅲ偠ᅸൟゟᓣ᧙ᢠ⺼ᴎᇚ䫊ॖሒⷓ䖯㸠䍙㒚⺼⹢Ǆ䆩偠䆕ᯢˈᇚሒⷓ䍙㒚⺼⹢㛑໻ᐙᑺᦤ催ሒⷓ∄
࣪⍌ߎ䫊ⱘᦤপ⥛ˈҢ㒚⺼ࠡሒⷓ(d80 Ў 100 μm)Ё䫊ⱘ⍌ߎ⥛ 36%ᦤ催ࠄ㒚⺼ৢ(d80 Ў 1.2 μm)ⱘ 84%Ǆ೼䍙㒚
⺼䆩偠Ёˈ䗮䖛 Box–Behnken 䆒䅵ˈⷨおњ⺼⧗Ⳉᕘ(2~4.5 mm)ǃ᧙ᢠ䗳ᑺ(200~800 min/min)੠⧗᭭↨(50%~80%)
ᇍⷨ⺼㒚ᑺⱘᕅડǄ㒧ᵰ㸼ᯢˈᦤ催᧙ᢠ䗳ᑺ੠⧗᭭↨䰡Ԣњ⺼᭭㒚ᑺˈՓ⫼䕗໻ⱘ⺼⧗Ӯᕫࠄ䕗㉫໻ⱘѻકǄ
೼䗖ᔧⱘᴵӊϟˈৃҹᕫࠄ㒚ᑺᇣѢ 5 μm ⱘ⺼᭭Ǆᑨ࡯ᔎᑺߚᵤ㸼ᯢˈᑨ࡯ᔎᑺ㣗ೈ(0.8~2)×103 N·m ᰃড়䗖ⱘǄ
݇䬂䆡˖䲒໘⧚ሒⷓ˗᧙ᢠ⺼˗䍙㒚⺼˗ᅲ偠䆒䅵˗Box–Behnken 䆒䅵˗ᑨ࡯ᔎᑺ
(Edited by Xiang-qun LI)
Hindawi Publishing Corporation
ISRN Tribology
Volume 2013, Article ID 386861, 9 pages
http://dx.doi.org/10.5402/2013/386861
Research Article
Friction Performance of Al-10%SiCp Reinforced Metal Matrix
Shouvik Ghosh, Prasanta Sahoo, and Goutam Sutradhar

Department of Mechanical Engineering, Jadavpur University, Kolkata 700032, India
Correspondence should be addressed to Prasanta Sahoo; psjume@gmail.com
Received 27 April 2012; Accepted 25 June 2012
Academic Editors: J. Antunes and J. Wang
Copyright © 2013 Shouvik Ghosh et al. is is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
e present paper considers the friction performance of Al-10%SiCp reinforced metal matrix composites against steel for varying
tribological test parameters. e composite is prepared by stir-casting process using aluminium alloy LM6 being mixed with
10% silicon carbide by weight. e tribological tests are performed by varying applied load, sliding speed, and time. e friction
performance is studied using plate-on-roller con�guration in a multitribotester and optimized using Taguchi L27 orthogonal array.
Analysis of variance (AN�VA) is performed to observe the signi�cance of test parameters and their interactions on friction
performance. It is observed that normal load and the interaction between normal load and speed in�uence the friction behaviour,
signi�cantly. e wear tracks are analyzed with the help of scanning electron microscopy.
1. Introduction e increasing use of composite materials in the automo-

bile and aeronautics �elds is due to good friction and wear
Particle reinforced composites are recognized as a light properties. In aeronautics, it is used for manufacturing of
weight material having enhanced mechanical and tribolog- rotor blades due to increased creep resistance. e aluminium
ical properties than the constituent materials. e MMC composites exhibit lower friction coefficient than their base
(metal matrix composite) materials attain the toughness of alloys [8, 9]. Iwai et al. [6] conducted the study with 2024
the alloy matrix and hardness, stiffness, and strength of Al alloy reinforced with 10% vol SiC. e friction study
the reinforcement. Researchers [1–3] have used different showed that initially the friction coefficient value is around
types of aluminium alloys for synthesis of the composites. 0.6 for both 2024 Al alloy and 2024Al-10%SiC and then
Also, different types of silicon carbide reinforcement such gradually decreases to 0.4. Martin et al. [9] conducted the
as particle, whisker, and �bre reinforcement are used by study on 2618Al alloy with 15% vol SiC reinforcement.
researchers. Mainly reinforcement volume fraction is varied e materials are tested at different temperatures ranging
by most researchers. Ahlatci et al. [4] carried out tribological from 0 to 200∘ C. e friction coefficient value of reinforced
experiments by mixing reinforcement in the volume fraction material is less than the alloy. e friction coefficient value
range from 0 to 60%. But most researchers [5–7] used volume increases from 0.5 to 1.5 with increase in temperature for
fraction ranging from 1 to 20% for their study. e compos- both cases. Bai et al. [10] found that friction coefficient
ites, synthesised by mixing the base metal and reinforcement, value increased with increase in sliding time. e variation
have greater strength, improved stiffness, improved corrosion is higher for high applied load. Chen et al. [5] carried out
resistance, and improved wear resistance. However, the tribological study with volume fraction range of 0–10%. From
relatively poor seizure resistance of aluminium alloy has this study, it was concluded that friction coefficient value
restricted to uses in some engineering applications. ese increases with increase in volume fraction at lower load
materials are good alternative to the traditional materials due and values range from 0.3 to 0.8 with gradual increase in
to the improved properties. % vol. But at higher load the friction coefficient value of
2 ISRN Tribology
all the material ranges from 0.3 to 0.4. Murthy et al. [11] insensitive (robust) to variation in uncontrolled or noise fac-
investigated the abrasive wear behaviour of Al-SiC whisker tors. Taguchi recommends that this can be done by the proper
reinforcement of volume fraction ranging from 10 to 40%. design of parameters during the “parameter design” phase
e study showed that friction coefficient value increased of offline quality control. He designed certain standard OAs
gradually with an increase in volume fraction, but decreased by which simultaneous and independent valuation of two or
with increase in sliding distance. Chen et al. [3] carried out more parameters for their ability to affect the variability of a
another study on the fretting wear behaviour and found particular product or process characteristic can be done in a
that friction coefficient value increased from 0.16 to 0.45 minimum number of tests. Using OA, the Taguchi method
for change in normal load from 5 N to 20 N and from 0.25 explores the entire design space through a small number of
to 0.45 for heat treated-materials. It was also concluded experiments in order to determine all of the parameter effects
that friction coefficient varies for pre-and post-heat-treated and several of the interactions. ese data are then used to
materials at lower load whereas no variation is found at predict the optimum combination of the design parameters
higher load. Rodríguez et al. [12] conducted the study on that will minimize the objective function and satisfy all
Al/Li alloy reinforced with SiC and found that the friction the constraints. In addition to locating a near optimum
coefficient value of reinforced materials is higher than the objective function, the Taguchi method provides information
alloy. Ma et al. [13] found from his experimentation that on parameter trends and noise sensitivities thereby enabling
friction coefficient value increased with increase in volume a robust design. e parameter design phase of the Taguchi
fraction. A350 Al alloy showed lower coefficient value than method generally includes the following steps: (1) identifying
50% SiC reinforced material. Yalcin and Akbulut [14] found the objective of the experiment; (2) identifying the quality
that friction coefficient value decreased with increase in characteristic (performance measure) and its measurement
volume fraction and applied load. Hassan et al. [7] concluded systems; (3) identifying the factors that may in�uence the
from their study of Al-4 wt%Mg-5 wt%SiC and Al-4 wt%Mg- quality characteristic, their levels, and possible interactions;
10 wt%SiC that the friction coefficient value is higher for (4) select the appropriate OA and assign the factors at
both cases than the alloy metal. e composite with 10% their levels to the OA; (5) conducting the test described by
SiC exhibits higher friction coefficient value. Tang et al. [15] the trials in the OA; (6) analysing the experimental data
found that monolithic SiC showed higher value of friction using the signal-to- noise (S/N) ratio, factor effects, and
coefficient than the composite. the analysing variance (ANOVA) to see which factors are
For the present experimental study LM6 aluminium alloy statistically signi�cant and to �nd the optimum levels of fac-
is used as base metal and silicon carbide particle (SiCp) tors; (7) verifying of the optimal design parameters through
is used as reinforcement (10% by weight). e composite con�rmation experiment. e OA requires a set of well-
is prepared by stir-casting process in an electric melting balanced (minimum experimental runs) experiments. e
furnace. e tribological tests are carried out on Al-10%SiCp Taguchi method uses a statistical measure of performance
for testing the friction property of the material. e result data called (S/N) ratios, which are logarithmic functions of desired
are analyzed by Taguchi method. Furthermore, a statistical output to serve as objective functions for optimization. e
analysis of variance (ANOVA) is performed to �nd the S/N ratio takes both the mean and the variability into account
statistical signi�cance of tribological test parameters. Finally, and is de�ned as the ratio of the mean (signal) to the
a con�rmation test is carried out to verify the optimal standard deviation (noise). e ratio depends on the quality
process parameters obtained from the parameter design. e characteristics of the product/process to be optimized. e
microstructure study is done with the help of SEM to judge three categories of S/N ratios are used: lower the better (LB),
the wear mode of the material. higher the better (HB), and nominal the best (NB). e
parameter level combination that maximizes the appropriate
S/N ratio is the optimal setting. For the case of minimization
of friction, LB characteristic needs to be used. Furthermore, a
2. Taguchi Method statistical analysis of variance (ANOVA) is performed to �nd
which process parameters are statistically signi�cant. �ith
e Taguchi method [16–18] is a powerful tool for design- the S/N ratio and ANOVA analyses, the optimal combination
ing high-quality systems based on orthogonal array (OA) of the process parameters can be predicted. Finally, a con�r-
experiments that provide much reduced variance for the mation experiment is conducted to verify the optimal process
experiments with an optimum setting of process control parameters obtained from the parameter design.
parameters. It introduces an integrated approach that is sim-
ple and efficient to �nd the best range of designs for quality,
performance, and computational cost. is method achieves 3. Experimental Details
the integration of design of experiments (DOE) with the
parametric optimization of the process yielding the desired 3.1. Fabrication Process. For the fabrication of the composite,
results. e traditional experimental design procedures focus aluminium alloy, that is, LM6, is used as matrix metal that
on the average process performance characteristics. But the has been reinforced with 10 wt% of SiC particles of 400
Taguchi method concentrates on the effect of variation on mesh size. e chemical composition of the matrix material
the process quality characteristics rather than on its averages. (LM6) is given in Table 1. e material is fabricated by
at is, the Taguchi approach makes the process performance liquid metal stir-casting process. is process is chosen for
ISRN Tribology 3
T 1: Chemical composition of LM6.
Elements Si Cu Mg Fe Mn Ni Zn Pb Sb Ti Al
Percentage (%) 10–13.0 0.1 0.1 0.6 0.5 0.1 0.1 0.1 0.05 0.2 Remaining
T 2: Design factors with levels L27 OA which has 27 rows corresponding to the number of
tests and 26 degrees of freedom (DOFs) with 13 columns at
Levels three levels is chosen. To check the DOFs in the experimental
Design factors Unit
1 2 3 design, for the three level test, the three main factors take
Load (𝐿𝐿) N 50 75i 100 6 [3 × (3 − 1)] DOFs. e DOF for three second-order
Speed (𝑆𝑆) RPM 180 200i 220 interactions (𝐿𝐿 𝐿𝐿𝐿, 𝐿𝐿 𝐿𝐿𝐿, 𝑆𝑆 𝑆𝑆𝑆) is 12 [3 × (3 − 1) × (3 − 1)] and
Time (𝑇𝑇) MIN 20 30i 40 the total DOFs required is 18. As per the Taguchi method,
i: initial condition. the total DOFs of selected OA must be greater than or equal
to the total DOFs required for the experiment and hence the
L27 OA has been selected. As per the requirements of the L27
the fabrication of the composite as it is both simple and less OA, the 1st column is assigned to applied load (𝐿𝐿), the 2nd
expensive. e small ingots of LM6 are melted in clay graphite column is assigned to sliding speed (𝑆𝑆), the 5th column is
crucible using an electric resistance furnace and 3 wt.% Mg assigned to Time (𝑇𝑇), and six columns are assigned to the two-
is added with the liquid metal in order to achieve a strong way interactions of the �rst three factors while the remaining
bonding by decreasing the surface energy (wetting angle) three columns are assigned for error terms. Table 3 shows the
between the matrix alloy and the reinforcement particles. e OA with design factors and their interactions assigned. Here,
addition of pure magnesium also enhances the �uidity of each column represents a speci�c factor, each row represents
the molten metal. Before mixing, the silicon carbide particles an experimental run, and the cell values indicate the factor
are preheated at 900∘ C for 2-3 hours to make their surface settings for the run. e cell values in the main factor columns
oxidized. e melt is mechanically stirred by using a mild (i.e., 𝐿𝐿, 𝑆𝑆, and 𝑇𝑇) indicate their levels (1, 2 or 3) while the same
steel impeller and then the preheated silicon carbide particles in interaction columns (two-cell �elds in two columns for a
are added with the stirred liquid metal. e processing of the particular interaction) indicate the combination of the levels
composite is carried out at a temperature of 720∘ C with a of the main factors concerned. For example, the interaction
stirring speed of 400–500 rpm. e melt is then poured at 𝐿𝐿 𝐿𝐿𝐿 occupies columns 3 and 4, and for trial no. 1, the cell
a temperature of 690∘ C into a green silica sand mould. e �elds show 1 in column 3 and 1 in column 4. us 𝐿𝐿 𝐿𝐿𝐿 has
material is then cooled and samples for tribological testing the value 11 which means, it is the combination of level 1 of
are prepared. 𝐴𝐴 and level 1 of 𝑆𝑆. Similarly, there are 9 such combinations
(11, 22, 33, 12, 21, 23, 32, 13, and 31) for 𝐿𝐿 𝐿𝐿𝐿 interaction
3.2. Design of Experiments. Design of experiments (DOE) in columns 3 and 4. A similar procedure applies to other
technique introduced by Fisher [19] is a powerful tool which interaction terms as well. However, the experimental run is
allows us to carry out modelling and analysis of the in�uence controlled by the settings of the controllable design factors,
of process variables on the response variables. e response that is, 𝐿𝐿, 𝑆𝑆, and 𝑇𝑇, and not by the interactions. e cell
variables are the unknown functions of the process variables values in interaction columns and error columns are used in
also known as design factors. ere are a number of control ANOVA for determination of their percentage contribution
factors that can affect friction behaviour of Al-10%SiCp. But to the total effect. In this case, if the full factorial design
literature review reveals that load, speed, and time are the was used, it would have 33 = 27 runs for consideration
most widespread among the researchers. Table 2 shows the of even the three main factors only. e L27 OA requires
design factors with their levels used in the present study. By only 27 runs—a fraction of the full factorial design—for
selecting three levels, the curvature or nonlinearity effects consideration of main factors along with the interactions.
could be studied. e friction characteristic of Al-10%SiCp is is array is orthogonal; factor levels are weighted equally
studied with coefficient of friction as the response variable. across the entire design.
e tribological test parameters are optimized with the
objective of minimizing the friction coefficient. 3.3. Tribological Test. e tribological tests are carried out in
DOE basically refers to the process of planning, design- a plate on roller multitribotester TR25 (Ducom, India) (Fig-
ing, and analyzing the experiment so that valid and objective ure 1). It is used to measure the friction of Al-10%SiCp under
conclusion can be drawn effectively and efficiently. Based on dry nonlubricated condition and at ambient temperature
Taguchi method an orthogonal array (OA) is considered to (28∘ C) and relative humidity of about 85%. e Al-10%SiC
reduce the number of experiments required to determine the samples (size 20 mm × 20 mm × 8 mm) are pressed against a
optimal friction for Al-10%SiCp metal matrix composite. An rotating steel roller (diameter 50 mm, thickness 50 mm, and
OA provides the shortest possible matrix of combinations material EN8 steel) of hardness 55 HRc. e setup is placed in
in which all the parameters are varied to consider their such a way that the rotating roller serves as the counter face
direct effect as well as interactions simultaneously Taguchi material and stationary plate serves as the test specimen. A
has tabulated several standard OAs. In this investigation, a 1 : 5 ratio loading lever is used to apply normal load on top
4 ISRN Tribology
T 3: L27 orthogonal array with design factors.
Column
1 2 3 4 5 6 7 8 9 10 11 12 13
Trial no.
(𝐿𝐿) (𝑆𝑆) (𝐿𝐿 𝐿 𝐿𝐿) (𝐿𝐿 𝐿 𝐿𝐿) (𝑇𝑇) (𝐿𝐿 𝐿 𝐿𝐿) (𝐿𝐿 𝐿 𝐿𝐿) (𝑆𝑆 𝑆𝑆𝑆) — — (𝑆𝑆 𝑆𝑆𝑆) — —
1 1 1 1 1 1 1 1 1 1 1 1 1 1
2 1 1 1 1 2 2 2 2 2 2 2 2 2
3 1 1 1 1 3 3 3 3 3 3 3 3 3
4 1 2 2 2 1 1 1 2 2 2 3 3 3
5 1 2 2 2 2 2 2 3 3 3 1 1 1
6 1 2 2 2 3 3 3 1 1 1 2 2 2
7 1 3 3 3 1 1 1 3 3 3 2 2 2
8 1 3 3 3 2 2 2 1 1 1 3 3 3
9 1 3 3 3 3 3 3 2 2 2 1 1 1
10 2 1 2 3 1 2 3 1 2 3 1 2 3
11 2 1 2 3 2 3 1 2 3 1 2 3 1
12 2 1 2 3 3 1 2 3 1 2 3 1 2
13 2 2 3 1 1 2 3 2 3 1 3 1 2
14 2 2 3 1 2 3 1 3 1 2 1 2 3
15 2 2 3 1 3 1 2 1 2 3 2 3 1
16 2 3 1 2 1 2 3 3 1 2 2 3 1
17 2 3 1 2 2 3 1 1 2 3 3 1 2
18 2 3 1 2 3 1 2 2 3 1 1 2 3
19 3 1 3 2 1 3 2 1 3 2 1 3 2
20 3 1 3 2 2 1 3 2 1 3 2 1 3
21 3 1 3 2 3 2 1 3 2 1 3 2 1
22 3 2 1 3 1 3 2 2 1 3 3 2 1
23 3 2 1 3 2 1 3 3 2 1 1 3 2
24 3 2 1 3 3 2 1 1 3 2 2 1 3
25 3 3 2 1 1 3 2 3 2 1 2 1 3
26 3 3 2 1 2 1 3 1 3 2 3 2 1
27 3 3 2 1 3 2 1 2 1 3 1 3 2
specimen. e loading lever is pivoted near the normal load behaviour of Al-10%SiCp is studied. Since the study is related
sensor and carries a counter weight at one end while at the to friction, coefficient of friction is taken as system response.
other end a loading pan is suspended for placing the dead Accordingly, the effect of the tribo-testing conditions on the
weights. e frictional force is measured by a frictional force friction behaviour of Al-10% SiCp is studied.
sensor that uses a beam type load cell of capacity 1000 N. e
friction tests are carried out at different load and speed for 4.1. Analysis of Signal-to-Noise Ratio. e desirable factor
different interval of time as mentioned in Table 2. levels are calculated by simple average of the results. is
traditional method is not able to capture the variability of
3.4. Microstructure Study. Aer friction tests, scanning elec- the results within the trial condition. us the 𝑆𝑆𝑆𝑆𝑆 ratio
tron microscopy (SEM) is used to evaluate the microstructure analysis is done in this study with the friction coefficient as
of the specimens. e microstructure study is conducted to the performance index. e 𝑆𝑆𝑆𝑆𝑆 ratio for friction coefficient
know the nature of the wear tracks. A scanning electron is calculated using LB criterion and the same is given by
microscope (JEOL, JSM-6360) is used for the microstructure
1
study of the material. S/N = −10 log 󵠈󵠈 󵠈󵠈2 , (1)
𝑛𝑛
4. Results and Discussion where 𝑦𝑦 is the observed data and 𝑛𝑛 is the number of
observations. Table 4 shows the experimental results for
e aim of the present study is to minimize friction of Al- friction coefficient and the corresponding S/N ratio. e
10%SiCp by optimizing the tribo-testing parameters with orthogonal experimental design enables it to separate out the
the help of Taguchi method. e in�uence of tribological effect of each tribological parameter at different levels. For
testing parameters like applied load, sliding speed, and sliding example, the mean S/N ratio for factor 𝐿𝐿 (Load) at levels
duration together with their interactions on the friction 1, 2, and 3 can be calculated by averaging the S/N ratios
ISRN Tribology 5
Friction Wear
PC monitor
Load RPM
Friction wear
measuring unit
Wear sensor
Counter weight Loading lever
Normal load sensor
Friction force sensor
Pivot
Specimen holder
Plate specimen
Steel roller
Loading pan
Drive unit
F 1: Schematic diagram of Multitribotester.
Main effects plot S/N ratio 2 and 3, respectively. e signi�cance of each parameter is
Load Speed Time determined from the inclination of the main effects plot. A
10.5 parameter for which the line has the highest inclination will
Mean of S/N ratio
10 have the most signi�cant effect. It is very much clear from the
9.5 main effects plot that parameter 𝐿𝐿 (applied load) is the most
9 signi�cant parameter while parameter 𝑆𝑆 (sliding speed) also
8.5 has some signi�cant effect. To study an interaction plot means
1 2 3 1 2 3 1 2 3 to determine the nonparallelism of parameter effects. If the
lines of an interaction plot are not parallel, it suggests that
F 2: Main effects plot. there is nominal interaction occurred and if the lines intersect
each other, then strong interactions occurred between the
parameters. Figure 3 shows that there is strong interaction
between the parameters 𝐿𝐿 and 𝑆𝑆 while there is moderate
for the experiments 1–9, 10–18, and 19–27, respectively. e interaction between the parameters 𝐿𝐿 and 𝑇𝑇 and between 𝑆𝑆
mean S/N ratio for each level of the other factors can be and 𝑇𝑇. us from the present analysis, it is clear that the
computed in the similar manner. e mean S/N ratio for applied load (𝐿𝐿) is the most in�uencing parameter for friction
each level of the factors 𝐿𝐿, 𝑆𝑆, and 𝑇𝑇 is summarized and characteristics of Al-10%SiCp metal matrix composites. e
called the response table for friction coefficient (Table 5). In optimal process parameter combination is the one that yields
addition, the total mean S/N ratio for the 27 experiments maximum mean S/N ratio and thus, the same for minimum
is also calculated and listed in Table 5. All the calculations friction coefficient is found to be L3S1T1, that is, the highest
are performed using Minitab [20]. e response table shows level of normal load and lowest levels of speed and time.
the average of the selected characteristic for each level of the
factors. e response table includes ranks based on Delta
statistics, which compares the relative magnitude of effects. 4.2. Analysis of Variance (ANOVA). ANOVA is a statistical
e Delta statistic is the highest average for each factor minus technique which can provide some important conclusions
the lowest average for the same. Ranks are assigned based based on analysis of the experimental data. is method
on Delta values; rank 1 is assigned to the highest Delta is very useful for revealing the level of signi�cance of the
value, rank 2 to the second highest Delta value, and so on. in�uence of factor(s) or interaction of factors on a particular
e corresponding main effects and interaction effects plots response. It separates the total variability of the response
between the process parameters are also shown in Figures into contributions of each of the factors and the error.
6 ISRN Tribology
Interaction plot for load versus speed Interaction plot for load versus time
11 11.5
10.5 11
10 10.5
Mean of S/N ratio

Mean of S/N ratio
9.5 10
9 9.5
8.5 9
8 8.5
1 2 3 1 2 3
Speed Time
Load Load
1 1
2 2
3 3
(a) (b)
Interaction plot for speed versus time
10.4
10.2
10
Mean of S/N ratio
9.8
9.6
9.4
9.2
1 2 3
Time
Speed
1
2
3
(c)
F 3: Interaction plots: (a) load versus speed, (b) load versus time, and (c) speed versus time.
ISRN Tribology 7
T 4: Friction test results.

Trial no. COF S/N ratio
1 0.353 9.0445
2 0.356 8.9710
3 0.344 9.2688
4 0.392 8.1343
5 0.371 8.6125
6 0.383 8.3360
7 0.350 9.1186
8 0.369 8.6595
9 0.394 8.0901
10 0.314 10.061
11 0.322 9.8429
12 0.328 9.6825
13 0.331 9.6034
14 0.348 9.1684
15 0.366 8.7304
16 0.399 7.9805 F 4: SEM image of worn surface of Al-10%SiCp composite.
17 0.386 8.2683
18 0.395 8.0681
19 0.258 11.768 the signi�cance of the parameter also increases. e ANOVA
20 0.318 9.9515 table shows the percentage contribution of each parameter.
21 0.333 9.5511 It is seen that parameter 𝐿𝐿, that is, applied load has the most
22 0.271 11.341 signi�cant in�uence on friction coefficient at the con�dence
23 0.320 9.8970 level of 99% while parameters 𝑆𝑆 (sliding speed) and 𝑇𝑇 (Time)
is signi�cant only at a 90% con�dence level within the speci�c
24 0.284 10.934
test range. Similarly, the interaction of parameters 𝐿𝐿 𝐿 𝐿𝐿 has
25 0.275 11.213
strong in�uence on friction property of the composite.
26 0.308 10.229
27 0.284 10.934
4.�. �o��r��tio� �est. Aer the optimal level of testing
parameters have been found, it is necessary that veri�cation
T 5: Response table for friction coefficient. tests are carried out in order to evaluate the accuracy of
the analysis and to validate the experimental results. e
Level Load Speed Time estimated S/N ratio 𝜂𝜂,
󵰁󵰁 using the optimal level of the testing
1 8.693 9.793 9.807 parameters can be calculated as
2 9.045 9.417 9.289
𝑜𝑜
3 10.646 9.173 9.288
𝜂𝜂󵰁󵰁 𝜂 𝜂𝜂𝑚𝑚 + 󵠈󵠈 󶀡󶀡𝜂𝜂𝑖𝑖 − 𝜂𝜂𝑚𝑚 󶀱󶀱 , (2)
Rank 1 2 3 𝑖𝑖𝑖𝑖
Delta 1.954 0.620 0.519
Total mean S/N ratio = 9.461 dB. where, 𝜂𝜂𝑚𝑚 is the total mean S/N ratio, 𝜂𝜂𝑖𝑖 is the mean S/N ratio
at the optimal testing parameter level, and 𝑜𝑜 is the number of
main design process parameters that signi�cantly affect the
Using Minitab [20], ANOVA is performed to determine friction performance of Al-10%SiCp.
which parameter and interaction signi�cantly affect the Table 7 shows the comparison of the estimated friction
performance characteristics. Table 6 shows the ANOVA result coefficient with the actual friction coefficient using the
for friction coefficient of Al-10%SiCp. ANOVA calculates optimal condition. Good agreement seems to take place
the 𝐹𝐹-ratio, which is the ratio between the regression mean between the estimated and actual friction coefficient. e
square and the mean square error. e 𝐹𝐹-ratio, also called improvement of S/N ratio from initial to optimal condition is
the variance ratio, is the ratio of variance due to the effect 2.5992 dB which means there is a reduction of 28% in friction
of a factor and variance due to the error term. is ratio is coefficient of Al-SiCp MMC.
used to measure the signi�cance of the parameters under
investigation with respect to the variance of all the terms 4.4. Microstructure Study. Figure 4 shows the SEM micro-
included in the error term at the desired signi�cance level, graph of the wear surface of the Al-10%SiCp composite. e
𝛼𝛼. If the calculated value of the 𝐹𝐹-ratio is higher than the SEM micrograph exhibits longitudinal grooves and partial
tabulated value of the 𝐹𝐹-ratio, then the factor is signi�cant irregular pits which indicates adhesive wear. e presence
at a desired 𝛼𝛼 level. In general, when the 𝐹𝐹 value increases, of grooves indicates the microcutting and microploughing
8 ISRN Tribology
T 6: ANOVA table for coefficient of friction.

Source DF SS MS 𝐹𝐹 Contribution (%)
𝐿𝐿 2 19.51 9.76 39.61# 63.20
𝑆𝑆 2 1.76 0.86 3.56∗ 5.69
𝑇𝑇 2 1.61 0.81 3.28∗ 5.23
𝐿𝐿 𝐿𝐿𝐿 4 4.01 1.01 4.06∧ 12.96
𝐿𝐿 𝐿𝐿𝐿 4 1.83 0.46 1.86 5.94
𝑆𝑆 𝑆𝑆𝑆 4 0.19 0.05 0.19 0.60
Error 8 1.98 0.25 6.38
Total 26 30.89 100
Signi�cant parameters and interactions (# 𝐹𝐹0.01, 2, 8 = 8.65; ∗ 𝐹𝐹0.10, 2, 8 = 3.11; ∧ 𝐹𝐹0.05, 4, 8 = 3.84).
T 7: Con�rmation result table. References

Optimal parameter [1] M. Bai, Q. Xue, X. Wang, Y. Wan, and W. Liu, “Wear mech-
Initial parameter
Predicted Experimental anism of SiC whisker-reinforced 2024 aluminum alloy matrix
Level L2S2T2 L3S1T1 L3S1T1 composites in oscillating sliding wear tests,” Wear, vol. 185, no.
COF 0.348 0.258 1-2, pp. 197–202, 1995.
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silicon carbide particulate reinforced aluminium-copper alloy
Improvement of S/N ratio = 2.5992 dB. matrix composites produced by direct squeeze casting method,”
Journal of Alloys and Compounds, vol. 489, no. 1, pp. 119–124,
2010.
effect of the counterface while pits or prows are indicative [3] R. Chen, A. Iwabuchi, and T. Shimizu, “e effect of a T6 heat
of adhesive failure of Al-10%SiCp composite. e adhesion treatment on the fretting wear of a SiC particle-reinforced A356
occurs under the experimental conditions used that induced aluminum alloy matrix composite,” Wear, vol. 238, no. 2, pp.
a substantial attractive force between the mating surfaces 110–119, 2000.
leading to a high mutual solubility of aluminium and iron. [4] H. Ahlatci, E. Candan, and H. Cimenoglu, “Abrasive wear
Hence, the wear phenomenon encountered in case of Al-SiCp behavior and mechanical properties of Al-Si/SiC composites,”
Wear, vol. 257, no. 5-6, pp. 625–632, 2004.
composite is both abrasive and adhesive.
In the present study, the in�uence of three factors, at [5] R. Chen, A. Iwabuchi, T. Shimizu, H. S. Shin, and H. Mifune,
“e sliding wear resistance behavior of NiAl and SiC particles
is, applied load, sliding speed and time on the friction
reinforced aluminum alloy matrix composites,” Wear, vol. 213,
behaviour of Al-SiCp composite is studied. Some other no. 1-2, pp. 175–184, 1997.
factors like heat treatment, temperature, volume fraction of [6] Y. Iwai, H. Yoneda, and T. Honda, “Sliding wear behavior of SiC
reinforcement, and so forth are considered to be constant in whisker-reinforced aluminum composite,” Wear, vol. 181–183,
this investigation. In future studies,an attempt will be made to no. 2, pp. 594–602, 1995.
evaluate the effect of these factors on the friction behaviour [7] A. M. Hassan, A. Alrashdan, M. T. Hayajneh, and A. T. Mayyas,
of the composite. “Wear behavior of Al-Mg-Cu-based composites containing SiC
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5. Conclusions [8] F. Akhlaghi and A. �are-Bidaki, “In�uence of graphite content
e friction performance of Al-10%SiCp reinforced metal on the dry sliding and oil impregnated sliding wear behavior
of Al 2024-graphite composites produced by in situ powder
matrix composites against steel is studied for varying tri-
metallurgy method,” Wear, vol. 266, no. 1-2, pp. 37–45, 2009.
bological test parameters. e optimal tribological testing
[9] A. Martín, M. A. Martínez, and J. Llorca, “Wear of SiC-
combination for minimum friction is found to be L3S1T1, reinforced Al-matrix composites in the temperature range
that is, the highest level of normal load and lowest levels of 20 − −2000∘ C,” Wear, vol. 193, no. 2, pp. 169–179, 1996.
speed and time. All the factors applied load (𝐿𝐿), speed (𝑆𝑆), [10] M. Bai, Q. Xue, and Q. Ge, “Wear of 2024 Al-Mo-SiC composites
and time (𝑇𝑇) are found to affect the friction signi�cantly. under lubrication,” Wear, vol. 195, no. 1-2, pp. 100–105, 1996.
But the factor load (𝐿𝐿) is the most important factor with a [11] V. S. R. Murthy, K. Srikanth, and C. B. Raju, “Abrasive wear
contribution of 63.20%. e interaction between load and behaviour of SiC whisker-reinforced silicate matrix compos-
speed (𝐿𝐿 𝐿 𝐿𝐿) is found to be the most signi�cant interaction. ites,” Wear, vol. 223, no. 1-2, pp. 79–92, 1998.
From the con�rmation test, it is found that the improvement [12] J. Rodríguez, P. Poza, M. A. Garrido, and A. Rico, “Dry sliding
of S/N ratio from initial to optimal testing condition for opti- wear behaviour of aluminium-lithium alloys reinforced with
mization of coefficient of friction is 2.5992 dB, which means SiC particles,” Wear, vol. 262, no. 3-4, pp. 292–300, 2007.
there is a decrease of 28% for coefficient of friction. From the [13] T. Ma, H. Yamaura, D. A. Koss, and R. C. Voigt, “Dry sliding
microstructure study of the wear tracks, it is observed that wear behavior of cast SiC-reinforced Al MMCs,” Materials
both abrasive and adhesive wear are encountered. Science and Engineering A, vol. 360, no. 1-2, pp. 116–125, 2003.
ISRN Tribology 9
[14] Y. Yalcin and H. Akbulut, “Dry wear properties of A356-SiC

particle reinforced MMCs produced by two melting routes,”
Materials and Design, vol. 27, no. 10, pp. 872–881, 2006.
[15] H. Tang, X. Zeng, X. Xiong, L. Li, and J. Zou, “Mechanical and
tribological properties of short-�ber-reinforced SiC compos-
ites,” Tribology International, vol. 42, no. 6, pp. 823–827, 2009.
[16] G. Taguchi, Introduction to Quality Engineering, Asian Produc-
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[17] P. J. Ross, Taguchi Technique for Quality Engineering, McGraw-
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[18] R. K. Roy, A Primer on Taguchi Method, Van Nostraid Reinhold,
New York, NY, USA, 1990.
[19] R. A. Fisher, Design of Experiments, Oliver & Boyd, Edinburgh,
UK, 1951.
[20] Minitab User Manual (Release 13.2), Making Data Analysis
Easier, MINITAB, State College, Pa, USA, 2001.
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Trial # COF S/N Ratio
1 0.353 9.0445
2 0.356 8.971
3 0.344 9.2688
4 0.392 8.1343
5 0.371 8.6125
6 0.383 8.336
7 0.35 9.1186
8 0.369 8.6595
9 0.394 8.0901
10 0.314 10.061
11 0.322 9.8429
12 0.328 9.6825
13 0.331 9.6034
14 0.348 9.1684
15 0.366 8.7304
16 0.399 7.9805
17 0.386 8.2683
18 0.395 8.0681
19 0.258 11.768
20 0.318 9.9515
21 0.333 9.5511
22 0.271 11.341
23 0.32 9.897
24 0.284 10.934
25 0.275 11.213
26 0.308 10.229
27 0.284 10.934
The Scientific World Journal
Volume 2012, Article ID 758719, 8 pages
doi:10.1100/2012/758719
The cientificWorldJOURNAL
Research Article
Statistical Evaluation and Optimization of Factors Affecting
the Leaching Performance of Copper Flotation Waste
Semra Çoruh,1 Sermin Elevli,2 and Feza Geyikçi3

1 Department of Environmental Engineering, Ondokuz Mayıs University, 55139 Samsun, Turkey
2 Department of Industrial Engineering, Ondokuz Mayıs University, 55139 Samsun, Turkey
3 Department of Chemical Engineering, Ondokuz Mayıs University, 55139 Samsun, Turkey
Correspondence should be addressed to Sermin Elevli, sermin.elevli@omu.edu.tr
Received 11 October 2011; Accepted 19 December 2011
Academic Editor: Sushil R. Kanel
Copyright © 2012 Semra Çoruh et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copper flotation waste is an industrial by-product material produced from the process of manufacturing copper. The main concern
with respect to landfilling of copper flotation waste is the release of elements (e.g., salts and heavy metals) when in contact with
water, that is, leaching. Copper flotation waste generally contains a significant amount of Cu together with trace elements of other
toxic metals, such as Zn, Co, and Pb. The release of heavy metals into the environment has resulted in a number of environmental
problems. The aim of this study is to investigate the leaching characteristics of copper flotation waste by use of the Box-Behnken
experimental design approach. In order to obtain the optimized condition of leachability, a second-order model was examined.
The best leaching conditions achieved were as follows: pH = 9, stirring time = 5 min, and temperature = 41.5◦ C.
1. Introduction to refine concentrated copper. Pyrometallurgy, or smelting,

is used on ore with copper sulfide and iron sulfide minerals.
Waste materials coming from municipal and industrial The concentrate is dried and fed into a furnace. The minerals
processes in Turkey are increasing, just as they are in many are partially oxidized and melted, resulting in segregated
other countries. The release of large quantities of heavy layers. The matte layer refers to the iron-copper-sulfide
metals into the natural environment due to hazardous waste mixture that sinks to the bottom. The slag, which refers
leaching has resulted in a number of environmental problems to the remaining impurities, floats on top of the matte.
[1, 2]. These waste materials may contain metals such as The copper flotation waste (slag) generated from the copper
copper, lead, zinc, arsenic, cobalt, nickel, and chromium. For industry is a by-product from the copper smelting industry
every tonne of blister copper production, about 2.2 tonnes of [5–8]. The toxicity of the waste is determined by leaching
flotation waste are generated. In this regard, landfill disposal tests and depending on the characteristics of the waste; the
of copper flotation waste from copper flash smelting plant spent abrasive must be disposed of as solid or hazardous
is not feasible since a few hundred tons are produced per waste. Owing to the environmental impact of the process
year; leaching of heavy metals into groundwater is of concern and waste management challenges faced for safe disposal
[3]. The disposal of industrial waste materials is becoming of the wastes, the United States Environmental Protection
more expensive each year due to large land areas needed for Agency (US EPA) encourages industries, businesses, and
its disposal. The best way to solve the disposal problem of institutions to consider all pollution prevention options
waste materials is to decrease the quantity for disposal with to aid environmentally preferable purchasing (EPP). EPP
utilization of waste materials in the industry [4]. will result in resource and energy conservation, waste
Copper is mined in open pits and below ground. The ore minimization, and extension of landfill capacity [3, 9].
usually contains less than 1% copper and is often associated The Black Sea Copper Works is situated in the metropoli-
with sulfide minerals. One of two processing methods is used tan city center of Samsun, Turkey. About 1.5–2 million
2 The Scientific World Journal
Table 1: Chemical composition (wt. %) of copper flotation waste. Table 2: The levels of experimental factors for the full factorial
design.
Copper flotation waste
SiO2 24.87 Factors Symbols Low level (−1) High level (+1)
Fe2 O3 67.68 pH X1 3 9
Al2 O3 0.92 Stirring time (minutes) X2 5 150
TiO2 0.08
Temperature (◦ C) X3 20 60
CaO 0.69
CuO 0.98
ZnO 2.78
PbO 0.21 It can be assumed that the material to be leached is
Cr2 O3 0.12
known, although its physical and chemical/mineralogical
SO3 2.18
K2 O 0.48
properties will affect the final result.
MgO 0.36 Leaching is one of the central unit operations in the
BaO 0.10 hydrometallurgical processes. A recent survey of the litera-
CoO 0.21 ture identified more than 100 leaching methods to remove
MnO 0.12 soluble components from a solid matrix. Several of these
are regulatory methods, mandated to characterize materials;
others are approved by organizations for establishing com-
tonnes of copper flotation waste arising from the factory pliance to particular specifications. Many were developed
are disposed of on the flood plain of the Yeşilırmak River, for application to municipal solid waste or industrial wastes
without any environmental pollution control [10]. The toxic prior to use or disposal. Some are intended to mimic
metals present in the copper flotation waste, such as Cu, Zn, natural conditions, while the intent of others is to obtain
Co, and Pb, affect rich groundwater resources and surface information about the nature of the extractable material
waters by leaching due to rain water, which is very high in within a particular solid. The methods vary in the amount
this region. and particle size of the leached sample, the type and volume
The aim of the present study is to investigate whether of leachant solution(s), and the leachant delivery method
or to what extent pH, stirring time, and temperature and time. Although some methods have been developed for
have an effect, either individually and/or jointly, on the specific types of materials, most leaching methods have been
leaching of copper flotation waste. The main effects and applied to a variety of materials [9, 11, 12].
the interactions of these factors were studied at three levels Batch leaching studies were used to evaluate the leaching
using a Box-Behnken experimental design, which provides a and pollution potentials of pollutants in copper flotation
second-order mathematical model, more information from waste samples. Effects of the pH, stirring time, and tem-
fewer experiments, and optimum values of the experimental perature on leaching behaviors of the pollutants in the
factors. copper flotation waste were investigated in the batch leaching
experiments. These experiments were carried out in the
batch reactors containing liquid/solid (L/S) mass ratio of
2. Materials and Experimental Procedure 10 (10 g solid for 100 mL of deionized water) and different
2.1. Materials. Copper flotation waste has a black color and pH, stirring time, and temperature. At the end of each
a glassy appearance. The specific gravity of copper flotation experiment, the mixtures were filtered. The leachates were
waste under investigation is 3100 kg/m3 . The absorption maintained to be highly acidic by adding nitric acid to
capacity of the waste material is typically very low (0.13%). prevent the metal ion precipitation. The samples were
The chemical composition of the flotation waste was deter- refrigerated at 4◦ C until analysis by atomic absorption
mined by using an X-ray fluorescence spectrometer (Rigaku, spectrometry (AAS) was carried out. A UNICAM 929 model
Rix-2000). The chemical composition of the waste, labeled Atomic Absorption Spectrophotometer with air-acetylene
as CFW in Table 1, shows iron oxides (67.68%) and silica flame was used for the determination of copper. The hallow
(24.87%), together with some hazardous oxides, as ZnO, cathode lamp for copper was operated at 6 mA and the
CuO, PbO, Cr2 O3 , and CoO. In previous studies, X-ray wavelength was set at 327.4 nm using a slit-width of 1.0 nm.
diffractometry (XRD) and scanning electron microscopy Detection limit of copper is 0.041 mg/L.
(SEM) spectra results show that copper flotation waste
mainly consisted of magnetite (FeO·Fe2 O3 ) and fayalite 3. Experimental Design
(2FeO·SiO2 ) [10].
In an experiment, one or more factors are deliberately
2.2. Experimental Procedure. Leaching is a method to remove changed in order to observe the effect of the changes on one
soluble components from a solid matrix. We can describe or more response variables. When too many factors or factor
leaching by a very simple equation: levels need to be considered to produce sufficient data, there
will be a huge number of repetitive experiments that need
to be conducted. This would be prohibitive in practice from
material (leachee) + leachant −→ leachate. (1) a time and cost viewpoint. Additionally, univariate methods
The Scientific World Journal 3
Table 3: Design matrix of the 23 full factorial design.
Average concentration of leached

Run no. pH Stirring time (min) Temperature (◦ C)
copper (mg/L)
1 3 (−1) 5 (−1) 20 (−1) 221.00
2 9 (+1) 5 (−1) 20 (−1) 146.95
3 3 (−1) 150 (+1) 20 (−1) 209.90
4 9 (+1) 150 (+1) 20 (−1) 132.20
5 3 (−1) 5 (−1) 60 (+1) 191.00
6 9 (+1) 5 (−1) 60 (+1) 133.70
7 3 (−1) 150 (+1) 60 (+1) 228.75
8 9 (+1) 150 (+1) 60 (+1) 216.4
9 6 (0) 77.5 (0) 40 (0) 129.00
10 6 (0) 77.5 (0) 40 (0) 180.00
11 6 (0) 77.5 (0) 40 (0) 145.00
Table 4: Analysis of variance for concentration of leached copper.
Source DF Seq SS Adj SS Adj MS F P

Main effects 3 15385.8 15385.8 5128.6 33.71 0.000
pH 1 12254.5 12254.5 12254.5 80.54 0.000
Stirring time 1 2237.3 2237.3 2237.3 14.70 0.003
Temperature 1 894.0 894.0 894.0 5.88 0.036
(2) Way interactions 3 7462.4 7462.4 2487.5 16.35 0.000
pH∗stirring time 1 426.4 426.4 426.4 2.80 0.125
pH∗temperature 1 1685.1 1685.1 1685.1 11.07 0.008
Stirring time∗temperature 1 5350.9 5350.9 5350.9 35.17 0.000
(3) Way interactions 1 590.5 590.5 590.5 3.88 0.077
pH∗stirring time∗temperature 1 590.5 590.5 590.5 3.88 0.077
Curvature 1 2861.3 2861.3 2861.3 18.81 0.001
Residual error 10 1521.6 1521.6 152.2
Pure error 10 1521.6 1521.6 152.2
Total 18 27821.6
do not take interactive effects between factors into account. p is the number of factors, is a special case of factorial design
Therefore, an efficient method of experimental planning and allows the experimenter to study several factors with two
is critical to produce credible data by concise experiment levels simultaneously.
design. The Box-Behnken design is an independent quadratic
The statistical design of experiments (DOE) is an design in that it does not contain an embedded factorial or
efficient procedure for planning experiments so that the fractional factorial design; the treatment combinations are at
data obtained can be analyzed to yield valid and objective the midpoints of edges of the process space and at the center.
conclusions. The two main applications of experimental
design are screening, in which the factors that influence 3.1. Full Factorial Design. The metal mobility depends on
the experiment are identified, and optimization, in which the pH, stirring time, and temperature, as they influence
the optimal settings or conditions for an experiment can the speciation and association of the metals in the waste
be found [13, 14]. The usual approach is to start with material [15]. In order to obtain optimized conditions for
a screening design by including all possible experimental the leachability of copper, a 23 full factorial experimental
factors, to select the significant factors, to identify whether design was used to evaluate the preliminary significance of
or not linearity assumption is violated, and then to continue the variables, as well as the interactions between them. The
with an experimental optimization design, such as Box- experimental variables, which are pH, stirring time, and
Behnken design. temperature, were evaluated at two levels, low (denoted as
Factorial experiments are experiments that investigate −1) and high (denoted as +1), as shown in Table 2. The level
the effects of two or more factors or input parameters on the selection for each factor was carried out on the basis of the
output response of a process. 2 p factorial experiment, where preliminary trials and previous publishing results.
Normal probability plot Versus fits

99 60
90 30
Residual
0
50
(%)
−30
10
−60
1
−70 −45 −20 5 30 55 80 100 150 200 250
Residual Fitted value
(a) (b)
Histogram Versus order
60
10
30
8
Residual
Frequency
0
6
4 −30
2 −60
0
−60 −30 0 30 60 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Residual Observation order
(c) (d)
Figure 1: Residual plots for concentration of leached copper.
Stirring time∗ pH Temperature∗ pH

150 60
240 150
210 120
50
100 225
40 105
180
50
195 30 150
135
165 165
20
3 4 5 6 7 8 9 3 4 5 6 7 8 9
Temperature∗stirring time
60
180 210 225
50 Hold values
150 pH 3
40 Stirring time 5
Temperature 20
30 210
165
195 225
20
25 50 75 100 125 150
Figure 2: Contour plots of concentration of leached copper.

Table 5: Estimated effects and coefficients for concentration of leached copper.
Term Effect Coef. SE Coef. T P

Constant 184.99 3.084 59.99 0.000
pH −55.35 −27.67 3.084 −8.97 0.000
Stirring time 23.65 11.83 3.084 3.83 0.003
Temperature 14.95 7.47 3.084 2.42 0.036
pH∗stirring time 10.33 5.16 3.084 1.67 0.125
pH∗temperature 20.52 10.26 3.084 3.33 0.008
Stirring time∗temperature 36.57 18.29 3.084 5.93 0.000
pH∗stirring time∗temperature 12.15 6.07 3.084 1.97 0.077
Ct Pt −33.65 7.761 −4.34 0.001
S = 12.3351, PRESS = 6057.65, R-Sq = 94.53%, R-Sq (pred) = 78.23%, and R-Sq (adj) = 90.16%.
Table 6: The levels of experimental factors for the Box-Behnken experimental design.
Factors Symbols Low level (−1) Center Level (0) High level (+1)
pH X1 3 6 9
Stirring time (minutes) X2 5 77.5 150
Temperature (◦ C) X3 20 40 60
For 2k factorial designs, it is assumed that the response contribution of precipitation at the high pH levels causes
is close to linear over the range of the factor levels. However, this relationship. According to the determination coefficient
linearity assumption is often violated in practice. In this case, (R2 -adj = 0.9016), which shows the explanatory power of
it is necessary to include one or more runs where all factors model, only 9.84% of total variation was not explained.
are set at their midpoint. The addition of center points to
design allows the researcher to check whether the linearity of 3.2. Box-Behnken Design. 23 factorial design was used to
the effects is a reasonable assumption or whether quadratic identify whether or not the selected experimental factors
terms should be added to the model. The results of the two- are significant and whether or not curvature exists. Since
level statistical design for three-independent variables with curvature in fitted data was detected, the assumption of
two replicates and three center points (pH = 6, stirring time = linear effects is not reasonable. Thus, a second-order model
75.5 minutes, and temperature = 40◦ C) are shown in Table 3. should be examined next, instead of a first-order model with
interaction, in order to obtain an optimized condition of
The data was processed using the Minitab 16 statistical leachability.
computer program. The null hypothesis stating that the main Response surface methodology (RSM) is an experimental
effects, interactions, and the curvature equal to zero was technique invented to find the optimal response within the
tested by using F-test (Table 4). The small P values (<0.05) specified ranges of the factors. These designs are capable
mean that not all the main effects and interactions are zero at of fitting a second-order prediction equation ( y = β0 +
the 5% significance level. In other words, there is reasonably k k
2
strong evidence that at least some of the main effects and i=1 βi xi + i=1 βii xi + i< j βi j xi x j ) for the response. The
interactions are not equal to zero. Curvature term with P quadratic terms in these equations model the curvature in
value lower than 0.05 indicates that there is curvature in the the true response function. The two most common designs
fitted data, and the response at the center point will be either generally used in response surface modeling are central
higher or lower than the fitted value of the factorial (corner) composite and Box-Behnken designs (BBDs). In this study,
points. BBD has been used for the purpose of finding optimal
The estimated effects and coefficients are summarized settings. Table 6 gives the levels of experimental factors. The
in Table 5. It is clearly seen that the chosen experimental factors were varied at three levels: high, central, and low.
parameters are significant at the 5% level. Since experimental The BBD is not directly based on a full factorial design, as
factors were found as significant in this step, they can it uses middle points instead of corner points. The number of
be used in the optimization step. From examining the experiments (n) required for the BBD is computed by using
magnitude of the effects, pH is dominant, followed by the following equation:
the interaction of BC (stirring time and temperature). All n = 2k(k − 1) + Co , (2)
the main and interaction effects, except pH, have positive
effects on leachability. According to the coefficients, it can where k is the number of factors and Co is the number of
be concluded that one unit increase in pH will result in a central points. Table 7 shows the mean results of 15 trials
27.67 unit decrease in concentration of leached copper. The with two replicates (k = 3, Co = 3).
250
175
200 150
C C
150 160 125 60
120
re
100 100
tu
80 40
im
ra
3 4 5
gt
3 4 5 40
pe
6 7 8 6 7 8
in
0 20
m
9
ir r
9
Te
(pH)
St
(pH)
250 Hold values

200 pH 3
C Stirring time 5
150 60
Temperature 20
re
100 40
tu
ra
0 40
80 120 20 pe
m
160
Te
Stirring time
Figure 3: Surface plots of concentration of leached copper.
Table 7: Design matrix of the Box-Behnken design.
Run no. pH Stirring time (min) Temperature (◦ C) Concentration of leached copper (mg/L)
1 3 (−1) 5 (−1) 40 (0) 121.80
2 9 (+1) 5 (−1) 40 (0) 79.90
3 3 (−1) 150 (+1) 40 (0) 224.85
4 9 (+1) 150 (+1) 40 (0) 191.00
5 3 (−1) 77.5 (0) 20 (−1) 213.30
6 9 (+1) 77.5 (0) 20 (−1) 208.40
7 3 (−1) 77.5 (0) 60 (+1) 201.40
8 9 (+1) 77.5 (0) 60 (+1) 168.00
9 6 (0) 5 (−1) 20 (−1) 162.45
10 6 (0) 150 (+1) 20 (−1) 162.50
11 6 (0) 5 (−1) 60 (+1) 165.90
12 6 (0) 150 (+1) 60 (+1) 212.20
13 6 (0) 77.5 (0) 40 (0) 129.00
14 6 (0) 77.5 (0) 40 (0) 180.00
15 6 (0) 77.5 (0) 40 (0) 145.00
Table 8: Estimated regression coefficients for concentration of leached copper.
Term Coef. SE Coef. T P

Constant 438.141 77.8093 5.631 0.000
pH −36.180 16.1679 −2.238 0.037
Stirring time 0.538 0.5119 1.052 0.305
Temperature −9.494 2.4252 −3.915 0.001
pH∗pH 2.087 1.1702 1.783 0.090
Stirring time∗stirring time −0.003 0.0020 −1.493 0.151
Temperature∗temperature 0.100 0.0263 3.813 0.001
pH∗stirring time 0.009 0.0465 0.199 0.844
pH∗temperature 0.090 0.1686 0.531 0.601
Stirring time∗temperature 0.008 0.0070 1.143 0.267
Table 9: Estimated regression coefficients for concentration of leached copper (reduced).
Term Coef. SE Coef. T P

Constant 331.331 44.6537 7.420 0.000
pH −6.835 2.5007 −2.733 0.011
Stirring time (ST) 0.449 0.1035 4.340 0.000
Temperature (T) −8.295 2.2282 −3.723 0.001
Temperature∗temperature
0.100 0.0275 3.637 0.001
(T 2 )
Table 10: Analysis of variance for concentration of leached copper.

Regression 4 36208.1 36208 9052.0 10.05 0.000
Linear 3 24297.1 36174 12057.9 13.39 0.000
pH 1 6728.1 6728 6728.1 7.47 0.011
Stirring time 1 16965.1 16965 16965.1 18.84 0.000
Temperature 1 603.9 12481 12480.7 13.86 0.001
Square 1 11911.0 11911 11911.0 13.23 0.001
Temperature∗temperature 1 11911.0 11911 11911.0 13.23 0.001
Residual error 25 22512.5 22513 900.5
Lack-of-fit 8 19249.3 19249 2406.2 12.53 0.000
Pure error 17 3263.3 3263 192.0
Total 29 58720.6
Estimated regression coefficients and related statistical are other experimental factors, such as liquid/solid ratio
terms are shown in Table 8. The effects are statistically and particle size that need to be considered. Based on the
significant when P value, defined as the smallest level of coefficients given in Table 8, the second-order prediction
significance leading to rejection of null hypothesis, is less equation can be written as follows:
than 0.05.
Based on Table 8, the terms, which seem insignificant y = 331.331 − 6.835 · pH + 0.449 · ST
(3)
compared to other effects, were neglected one by one, and − 8.295 · T + 0.100 · T 2 ,
the related statistics were then recalculated with remaining
variables. Table 9 shows the results of the reduced model. where y = concentration of leached copper (mg/L), ST =
The ANOVA results in Table 10 indicate the relative stirring time (min.), T = temperature (◦ C).
importance of the first-order and second-order sources According to (3), only temperature has the second-order
with respect to the sum of squares. The order of factors term. Thus, optimum value for temperature can be found as
from high to low contribution on concentration of leached follows:
copper is stirring time, temperature∗temperature, pH, and ∂y
temperature. = −8.295 + 0.2 · T = 0 =⇒ Topt = 41.475◦ C. (4)
∂T
The design of experimental analysis assumes that the
residuals are normally and independently distributed with A contour plot provides a two-dimensional view where all
the same variance in each treatment or factor level. Depar- points that have the same response are connected to produce
tures from this assumption mean that the residuals contain contour lines of constant responses. Figure 2 shows the
structure that is not accounted for in the model. Residual relationship between concentration of leached copper and
plots given in Figure 1 were used to check the assumption. experimental variables. The variables not displayed in the
Since the residuals lie approximately along a straight line graphs were held constant at low levels. From these figures, it
and any pattern, such as sequences of positive and negative is possible to determine the values of experimental factors for
residuals, is not observed, it was concluded that the residuals a specified concentration. For example, for a concentration
are normally and independently distributed. of leached copper lower than 105 mg/L, it is necessary to set
R Square given in Table 8 means that 55.53% of the total pH at 8.5–9 and temperature at 35–45◦ C, while stirring time
variation in the concentration of leached copper from copper is held constant at 5 minutes.
flotation waste can be attributed to the studied experimental The surface plot is used to see a graphic representation of
factors. This value is lower than expected. That is, there how two factors at one time affect the output (concentration)
together. Since there are more than two factors, the factors [9] USEPA, Applicability of the Toxicity Characteristic Leaching
not displayed in graphs are held constant. From Figure 3, it Procedure to Mineral Processing Wastes, Office of Solid Waste,
is observed that surface plots, including temperature, have a Washington, DC, USA, 1995.
concavity characteristic due to optimum value. The lowest [10] S. Çoruh, “Immobilization of copper flotation waste using red
concentrations were found with pH at 9, stirring time at 5 mud and clinoptilolite,” Waste Management and Research, vol.
minutes, and temperature at 41.5◦ C. 26, no. 5, pp. 409–418, 2008.
[11] E. E. Chang, P. C. Chiang, P. H. Lu, and Y. W. Ko, “Com-
parisons of metal leachability for various wastes by extraction
4. Conclusion and leaching methods,” Chemosphere, vol. 45, no. 1, pp. 91–99,
2001.
The copper flotation waste generated from the copper [12] F. Vegliò, M. Trifoni, and L. Toro, “Leaching of manganiferous
industry is classified as “hazardous waste” according to ores by glucose in a sulfuric acid solution: kinetic modeling
literature. In this study, a series of experiments varying the and related statistical analysis,” Industrial and Engineering
pH, stirring time, and temperature were performed to study Chemistry Research, vol. 40, no. 18, pp. 3895–3902, 2001.
heavy metal release from copper flotation waste. Despite [13] L. J. Lozano Blanco, V. F. Meseguer Zapata, and D. De Juan
the fact that leaching studies have been extensively used Garcı́a, “Statistical analysis of laboratory results of Zn wastes
for the waste material, the leaching characteristics of the leaching,” Hydrometallurgy, vol. 54, no. 1, pp. 41–48, 1999.
copper flotation waste have not been investigated before by [14] G. Hanrahan and K. Lu, “Application of factorial and response
using experimental design approach in literature. This study surface methodology in modern experimental design and
has given a regression equation for prediction and showed optimization,” Critical Reviews in Analytical Chemistry, vol.
36, no. 3-4, pp. 141–151, 2006.
the effects of experimental factors and their interactions on
[15] S. R. Al-Abed, P. L. Hageman, G. Jegadeesan, N. Madhavan,
concentration of leached copper.
and D. Allen, “Comparative evaluation of short-term leach
According to the experimental results and statistical tests for heavy metal release from mineral processing waste,”
analysis, heavy metal release is strongly influenced by the pH. Science of the Total Environment, vol. 364, no. 1–3, pp. 14–23,
Under the experimental condition of this study, the solution 2006.
of prediction equation for pH = 9, ST = 5 min, and T =
41.5◦ C gives the minimum concentration of leached copper,
which is 100 mg/L. This value is still considerably higher than
the allowed Turkish limit (Cu: 3 mg/L). Because of this, it is
suggested to apply immobilization methods to decrease the
concentration.
References
[1] W. Hogland and J. Stenis, “Assessment and system analysis
of industrial waste management,” Waste Management, vol. 20,
no. 7, pp. 537–543, 2000.
[2] K. S. Al-Jabri, R. A. Taha, A. Al-Hashmi, and A. S. Al-Harthy,
“Effect of copper slag and cement by-pass dust addition on
mechanical properties of concrete,” Construction and Building
Materials, vol. 20, no. 5, pp. 322–331, 2006.
[3] K. Kambham, S. Sangameswaran, S. R. Datar, and B. Kura,
“Copper slag: optimization of productivity and consumption
for cleaner production in dry abrasive blasting,” Journal of
Cleaner Production, vol. 15, no. 5, pp. 465–473, 2007.
[4] E. Cokca and Z. Yilmaz, “Use of rubber and bentonite added
fly ash as a liner material,” Waste Management, vol. 24, no. 2,
pp. 153–164, 2004.
[5] M. Singh, “Treating waste phosphogypsum for cement and
plaster manufacture,” Cement and Concrete Research, vol. 32,
no. 7, pp. 1033–1038, 2002.
[6] B. Gorai, R. K. Jana, and Premchand, “Characteristics and
utilisation of copper slag—a review,” Resources, Conservation
and Recycling, vol. 39, no. 4, pp. 299–313, 2003.
[7] K. Hietala and O. Varien, “HydroCopper—a new technology
for copper production,” in Proceedings of the Alta Copper
Conference, Perth, Australia, 2003.
[8] M. F. M. Zain, M. N. Islam, S. S. Radin, and S. G. Yap,
“Cement-based solidification for the safe disposal of blasted
copper slag,” Cement and Concrete Composites, vol. 26, no. 7,
pp. 845–851, 2004.
OPTIMIZATION OF SHAKING TABLE AND DRY MAGNETIC SEPARATION ON
RECOVERY OF EGYPTIAN PLACER CASSITERITE USING EXPERIMENTAL DESIGN
TECHNIQUE
M. A. Youssef 1, M.K. Abd El-Rahman 1, N.H. Helal 2, M. M. El- Rabiei 2, S. R. Elsaidy 1

1Central Metallurgical Research of Development Institute, P.O. Box :87, Helwan, Cairo, Egypt
2 Faculty of Science, Fayoum University
ABSTRACT: Experimental design technique is applied to optimize shaking table and dry high intensity magnetic
separation processes on recovery of cassiterite from Igla Placer ore of Eastern Desert of Egypt. It could
investigate the effects of individual operating parameters and their interactions for both shaking table and dry
high intensity magnetic separation processes. Applying the optimum conditions for both separation techniques
showed that in case of shaking table separation concentrate containing 13.2% SnO2 and recovery of 86.2% by
weight SnO2 was obtained from a feed containing about 0.048 % SnO2. Cleaning of this concentrate by using dry
high intensity magnetic separation a final concentrate with 90.67% SnO2 and operational recovery of 96.7% SnO2
by weight was obtained.
Keywords: Cassiterite, shaking table, dry high intensity magnetic separation, Box-Behnken design, statistical experimental design
1. INTRODUCTION ore of 0.12 % tin is concentrated by three-stage

jigging, spiral concentration, and tabling to give a
Cassiterite (SnO2) is known as tinstone, stannic high-grade concentrate of 63% tin with a recovery of
oxide, tin (IV) oxide. It has many different industrial 80% of the tin [17]. Induced-roll magnetic separator
applications such as ceramics, coating cans, pigments has been successfully used in cassiterite recovery and
[1], sensors of combustible gases [2], high voltage series of experiments have been performed on
varistors [3-4], and as electrode. It has a high specific cassiterite/wolframite separations [18]. A comparison
gravity (6.8 - 7.1) and a Moh’s scale hardness of the performance of the Bartles Crossbelt
of 6 to 7. There are two types of cassiterite, alluvial performance with a standard slimes table, treating a
placer and lode cassiterite. Alluvial placer cassiterite is feed of 0.7% Sn grade and 97% -40 um, showed a
the major source of tin concentrate [5]. Tin placers similar overall recovery of just 55% but the Crossbelt
contain recoverable amounts of other heavy minerals produced a grade of 32% Sn compared with just 13%
such as columbite-tantalite, wolframite, ilmenite, and Sn for the slime table [19].
monazite [6-10]. About 70% of total world tin
In Egypt most cassiterite placers present in the
production is produced from placer deposits [11].
Eastern Desert. The most common localities are
About 35 countries mine tin throughout the world.
Igla, Mueilha, Abu Dabab, and Nuweibi [20-22].
China, Indonesia, Peru, Bolivia and Brazil accounted
for about 95% of the world tin production [12].
2. MATERIAL AND METHODS
Gravity technique is more recommended for
recovery of cassiterite due to the large difference in 2.1 Material
specific gravity between cassiterite (6.8-7.1) and the
A representative sample of Igla placer ore from Igla
gangue silicate minerals (2.6) [13-16]. Cassiterite
locality about two tons was used in this study.
could be upgraded by washing, tabling, and magnetic
Complete chemical analysis, using “type” X-ray
or electrostatic separation. The final product is
fluorescence and for phase analysis using X- ray
virtually pure cassiterite. On the other hand lode
diffractometer model “PW 1010” was conducted.
cassiterite deposit is reduced to the necessary size by
conventional crushing and grinding. The prepared 2.2. Experimental Methods
feed is concentrated by gravity methods that involve
screening, classification, jigging, and tabling. The 2.2.1. Processing of Igla Placer Cassiterite
concentrate is usually a lower grade than placer
concentrate owing to associated sulfide minerals [5]. A representative sample was crushed using the jaw
The unit operation to prepare primary cassiterite crusher to prepare a feed about 3.36 mm for the
concentrate in Malaysia and Thailand is the sluice grinding process. The grinding process is carried out
box used on alluvial deposits known as palongs. The for in closed circuit using “Denver” pilot rod mill
concentrate contains about 15 to 30 % tin and the and sieve size 125 micron. The ground product from
recovery efficiency can be up to 80 % [13]. At Iscor's 125 to 80 micron was used as a feed for shaking table
Uis Mine in South West Africa, a very low-grade tin separation.
2 Volume 11 - Issue 22
2.2.2. Separation Techniques for Igla Placer Cassiterite

The separation techniques involve a pilot
“Wilfley” shaking table gravity separator and
“Ereiz” dry high intensity rare earth magnetic
roll separator.
2.2.3. Shaking Table Separation Experiments

The feed is introduced onto an inclined plane and
reciprocated deck and moves in the direction of
motion while simultaneously being washed by a
water film, which moves it also at right angles to the Figure 1. “Eriez” three stage rare earth magnetic roll
motion of the deck. The feed enters at the top of the separator
table, and collects within the valleys formed by the
Table 1. List of symbols
narrow cleats, or riffles, which taper in height from
Symbol Definition Unit
right to left. Under the effect of the reciprocating Symbols used for Shaking Table Separation
action, the particles stratify with the heavier particles Inclination angle degree
α
on the bottom, and they move from right to left. Stroke length cm
β
Owing to decreasing taper of the riffles, the exposed
γ Feed rate gm/min
upper surface of the stratified material is acted upon λ Water flow rate l/ min
by crosscurrents of water and by the inclination of
ρ Grade % by weight
the deck, as indicated by the arrow, and is moved
η Recovery % by weight
downhill. A “Wilfley” shaking table was used in this Symbols used for DryHigh Intensity Magnetic
study, figure 1. Shaking table technique is applied on Separation
feed -0.125 + 0.080 mm size fraction, and four ε Splitter inclination degree
parameters are studied. The parameters are namely; δ Belt speed rpm
inclination angle, stroke length, feed rate and water ϕ Feed rate gm/min
flow rate. μ Grade % by weight
σ Recovery % by weight
Σ Sum of squares
Φ DF
Ψ Mean square
χ F Value
τ Prope > F
2.2.5. Applying Box-Behnken Design (BBD) for Both

Figure 1. Wilfley shaking table unit Shaking Table and Dry Magnetic Separation
1: Sample feeding box, 2: Washing water feeding box, 3: Washing water, The Box-Behnken Design (BBD) was conducted for
4: Heavy products reservoirs, 5: Light products reservoirs
both shaking table and dry high intensity magnetic
separation to determine the most important variables
2.2.4. Dry High Intensity Magnetic Separation Experiments and the interactions between different variables and
Dry high intensity magnetic separation was carried to identify the optimum conditions. According to
out on the concentrate obtained from shaking table this design, the optimal conditions were estimated
process using “Eriez” three stage rare earth magnetic using a second order polynomial function by which a
roll separator with permanent field intensity about1.5 correlation between studied factors and response
tesla, figure 2. Three parameters are studied which (mean diameter) was generated. The general form of
are splitter inclination, belt speed, and feed rate. this equation is:
Where: is the predicted response, s are studied

variables; and are the regression
parameters. Software package, Design-Expert 6.0.5,
Stat-Ease, Inc., Minneapolis, USA, was used for
regression analysis of experimental data and to plot
M. A. Youssef, M.K. Abd El-Rahman, N.H. Helal, M. M. El- Rabiei, S. R. Elsaidy / The Journal of ORE DRESSING ® 2009 3
response surface [23]. Analysis of variance separation processes. Table 3 illustrates the factorial
(ANOVA) was used to estimate the statistical design, recovery and grade of cassiterite for both
parameters. The extent of fitting the experimental shaking table and magnetic separation processes.
results to the polynomial model equation was
expressed by the determination coefficient, R2. F-test Table 2. Test levels of parameters for both shaking
was used to estimate the significance of all terms in table and dry high intensity magnetic separation
the polynomial equation within 95% confidence Dry High Intensity Magnetic
Shaking Table Separation
interval. "Adeq Precision" measures the signal to Separation
noise ratio, a ratio greater than 4 is desirable and Symbol (-) (0) (+) Symbol (-) (0) (+)
indicates an adequate signal. α 3 4 5 ε 70 75 80
β 2 2.5 3 δ 50 75 100
Table 2 represents the operating parameters for both γ 100 250 400 ϕ 500 750 1000
shaking table and dry high intensity magnetic λ 15 20 25
Table 3. Factorial design for shaking table and dry magnetic separation
Run Shaking Table Separation Dry Magnetic Separation
α β γ λ ρ η ε δ ϕ μ σ
1 4 3 400 20 7.37 81.4 75 75 750 90.6 96.7
2 5 2.5 400 20 6.87 84 80 75 500 62.5 96.4
3 4 2 100 20 10.6 76.8 80 100 750 58.7 95.6
4 4 2.5 100 25 8.94 82 75 100 1000 77.1 91.2
5 4 3 100 20 5.7 80 75 75 750 90.6 96.7
6 4 3 250 25 7.95 83 75 50 500 81.3 94.6
7 5 2.5 100 20 6.2 81.9 70 50 750 74.6 87.6
8 4 3 250 15 7.46 79.8 70 75 1000 73.2 88.1
9 3 3 250 20 5.79 79.2 75 75 750 90.6 96.7
10 4 2.5 400 25 12.47 83.4 75 75 750 90.6 96.7
11 3 2.5 400 20 9 82.6 80 50 750 61.3 95.7
12 4 2.5 100 15 8.5 81 75 50 1000 79 92.3
13 5 2 250 20 4 74.5 80 75 1000 64.2 96.1
14 3 2.5 100 20 8.2 81.4 75 75 750 90.6 96.7
15 3 2.5 250 15 7.95 80.8 70 100 750 78.6 85.8
16 4 2.5 250 20 13.2 84.9 70 75 500 72.4 89.3
17 4 2.5 250 20 13.2 84.9 75 100 500 78.2 91.7
18 4 2.5 250 20 13.19 84.9
19 5 2.5 250 15 4.5 76.4
20 3 2 250 20 8.8 80.4
21 5 3 250 20 3.4 77.5
22 4 2.5 400 15 9.4 79.4
23 4 2.5 250 20 13.21 84.9
24 4 2 400 20 11.5 77.9
25 4 2 250 25 11.9 80
26 3 2.5 250 25 10 82
27 4 2.5 250 20 13.2 84.9
28 4 2 250 15 9.4 78.4
29 5 2.5 250 25 8.7 88.6
3. RESULTS AND DISCUSSIONS
3.1.Chemical and Mineralogical analyses of Igla

Placer Cassiterite
The results of complete chemical analysis of the
representative sample of Igla placer cassiterite ore
using X-ray fluorescence are given in table 4. It has
been shown that it contains about 0.048% SnO2.
Figure 3 represents the X-ray diffraction of the Igla
placer tin ore. It is noticed that it involves quartz,
feldspar, actinolite, and mica respectively.
Figure 3. X-ray diffraction of Igla original placer tin
ore
Table 4. Complete chemical analysis of Igla original 3.2. Size Analysis of Original Igla Placer
placer tin ore Cassiterite Ore
Constituent Assay %
Figure 4 shows the grain size analysis of the
SnO2 0.048 cassiterite ore. It is shown that the ore passed 100 %
SiO2 58.6 from 22 mm sieve size. The d80 and d50 of the ore are
Al2 O3 12.01 14 mm and 6.8 mm respectively. It is seen that the
SnO2 % increases with decreasing the size. The
MgO 8.26 distribution percentage of the SnO2 reaches its
CaO 4.90 maximum at size less than 11.3 mm. It is noticed that
Na2O 4.05 the size fraction larger than 11.3 mm represents
K2O 1.79 about 30 % by weight from the cassiterite ore and
contains only about 0.017 % SnO2. Therefore the ore
TiO2 0.53
is screened on the sieve 11.3 mm for preparing a feed
Fe2O3 6.16 for the recovery process. The oversize is discarded
ZrSO4 0.01 and the undersize fraction is used for the recovery
Cl 0.20 process. Table 5 represents the size analysis and
P 2O5 0.11 distribution percentage of SnO2 of the undersize of
the sieve 11.3 mm. The size fraction from 11.3 mm
SO3 0.046 to 0.125 mm represents about 95 % by weight with
L .O. I 3.00 0.061 SnO2 % and 95 % distribution of cassiteriate.
It was crushed and grinding using rod mill in closed
circuit with screen 0.125 mm to prepare a feed for
shaking table.
18 100 0.10
Cum. Wt% passing
16
SnO2 % ( ±0.0005)
14 80 SnO2 Distribution % 0.08
Cumulative Weight % Passing
SnO2 Distribution %
12
60 0.06
SnO2 %
10
8
40 0.04
6
4 20 0.02
2
0 0 0.00
10 100 1000 10000
Size, micron
Figure 4. The relation between the size (micron) of the original sample and cumulative weight %, SnO2 %, and
distribution percentage of the SnO2
Table 5. Size analysis and distribution of the
fine fraction less than 80 micron was taken for falcon
undersize fraction of sieve 11.3 mm separation technique.
Weight SnO2 % Distribution
Size, mm Table 6. Grinding and screening
% (±0.0005) %
-11.3 + 0.9 81.52 0.061 80.80 Size fraction, Weight SnO2 % Distribution
-0.9 + 0.4 7.39 0.060 7.17 (mm) % (±0.0005) %
-0.4 + 0.125 6.60 0.064 6.83 -0.125 + 0.080 45 0.0580 42.08
-11.3 to 0.125 95.51 0.0611 94.8 - 0.080 55 0.0653 57.92
-0.125 + 0.08 1.88 0.060 1.82 Total 100 0.062 100
-0.08 2.61 0.080 3.37
Total 100.00 0.062 100.00 3.4. Relation between Recovery of Cassiterite and
Different Experimental Parameters
3.3. Preparation of Feed for Shaking Table The Design-Expert 6.0 software program was used
The results of grinding and screening of size fraction to analyze each response to the regression model of
less than 11.3 mm are presented in table 6. It has the parameters listed in table 3. Table 3 represents
been noticed that the size fraction -0.125 +0.08 mm groups of experimental data and it could establish the
represent about 45 % by weight with 0.058 % SnO2 multinomial model of the relation between recovery
and 42 distribution percentage of cassiterite . The of cassiterite and the operating parameters. It can be
expressed as equations 2 and 3 for both shaking table separation (λ, α2, β2, αλ) are more significant terms
separation and dry high intensity magnetic and the terms in case dry magnetic separation
separation. The analysis of variance of the ( ε,δ,ϕ,ε2, δ2, ϕ2) are more significant terms. The
multinomial model is given in tables 7 and 8. The values greater than 0.1000 indicate model terms are
model F-value (χ) for both shaking table separation not significant. Table 8 represents the “ANOVA”
and dry magnetic separation represents 5.26 and statistical analysis for both shaking table and dry high
100.79 respectively and it indicates that the model is intensity magnetic separation. The values in that table
significant. There is only 0.19 % and 0.01 % chance indicate the will fitting of the experimental results to
for shaking table and dry magnetic separation that a the polynomial model equations for both shaking
"Model F-Value" this large could occur due to noise. table and dry magnetic separation and hence accuracy
Values of "Prob > F" less than 0.0500 indicate model of these models.
terms are significant. The terms in case shaking table
η Recovery = _7.43 _ 2.48 * α + 77.38 * β + 7.76 * γ _ 0.68 * λ _1.8 * α2 _ 17.42 * β2 _ 6.63* γ2 _ 0.045* λ 2 + 2.1* αβ +
1.5* αγ + 0.55* αλ + 1.0* βγ + 0.16* β λ + 1.0* γλ (2)
σ Recovery = -585.05 +16.94* ε + 0.33* δ + 0.014* ϕ - 0.11* ε2 - 4.44* δ2 - 2.36* ϕ2 + 3.40 * εδ + 1.80* εϕ + 7.20*
δϕ (3)
Table 7. ANOVA for response surface 2FI model analysis of variance

Source Σ Φ Ψ χ τ
Model 231.41 14 16.53 5.26 0.0019
α 1.02 1 1.02 0.32 0.5778
β 13.87 1 13.87 4.41 0.0543
γ 2.61 1 2.61 0.83 0.3773
λ 44.85 1 44.85 14.27 0.0020
α
2 21.11 1 21.11 6.72 0.0213
β
2 122.98 1 122.98 39.12 < 0.0001
γ
2 14.43 1 14.43 4.59 0.0502
λ2 8.09 1 8.09 2.57 0.1310
αβ 4.41 1 4.41 1.40 0.2559
αγ 0.20 1 0.20 0.064 0.8033
αλ 30.25 1 30.25 9.62 0.0078
βγ 0.022 1 0.022 7.158E-003 0.9338
βλ 0.64 1 0.64 0.20 0.6587
γλ 2.25 1 2.25 0.72 0.4117
Residual 44.01 14 3.14
Lack of Fit 44.01 10 4.40
Pure Error 0.00 4 0.00
Cor Total 275.42 28
Dry High Intensity Magnetic Separation
Model 225.81 9 25.09 100.79 < 0.0001
ε 136.13 1 136.13 546.84 < 0.0001
δ 4.35 1 4.35 17.48 0.0041
ϕ 2.31 1 2.31 9.28 0.0187
ε
2 31.84 1 31.84 127.92 < 0.0001
δ
2 32.42 1 32.42 130.25 < 0.0001
ϕ
2 9.16 1 9.16 36.80 0.0005
εδ 0.72 1 0.72 2.90 0.1322
εϕ 0.20 1 0.20 0.81 0.3971
δϕ 0.81 1 0.81 3.25 0.1142
Residual 1.74 7 0.25
Lack of Fit 1.74 3 0.58
Pure Error 0.00 4 0.00
Cor Total 227.55 16
Table 8. ANOVA for response surface quadratic model for the shaking table separation and dry high intensity
magnetic separation
Shaking Table Separation Dry Magnetic Separation
The statistical parameters ρ (Grade %) η (Recovery % μ (Grade %) σ (Recovery %
The standard deviation 0.85 1.77 2.24 0.50
R-squared 0.9575 0.8402 0.9820 0.9923
Adequate precision 15.631 7.879 18.017 28.811
Table 9 summarizes the obtained optimum

3.5. Response Surfaces for the Relation of
parameters for both separation techniques. The
Recovery of Cassiterite with Different Parameters
results of applying the optimum parameters obtained
Figure 5 (a & b) represents the response surfaces for (Table 9) for shaking table separation and dry high
the shaking table cassiterite concentrate product intensity magnetic separation for concentrate
recovery at different values of studied parameters. In obtained from shaking table are shown in table 10. It
figure 4a it is noticed that with increasing both is shown that a shaking table concentrate with 13.2
inclination angle and stroke length the recovery value % SnO2 and 86.2 % recovery is obtained. In case of
increases and reaches to the maximum value which is dry high intensity magnetic separation a non
84.97 % at inclination angle 3.95 degree, and stroke magnetic fraction concentrate with 90.67 % SnO2
length 2.56 cm. On the other hand increasing and 83.36% recovery is obtained. Figures (8 and 9)
inclination angle and stroke length more than 3.95 represent the X-ray diffraction of both shaking table
degree and 2.56 cm respectively lead to a slight concentrate and non magnetic fraction of dry
decrease in the recovery value. In figure 4b it is magnetic separation. The X -ray diffraction of
noticed that with increasing both water flow rate and shaking table concentrate showed that it contains
feed rate the recovery value increases and reaches its ilmenite, cassiterite, hematite, and zircon respectively.
maximum value about 86 % at feed rate 311.15 Meanwhile the X-ray diffraction of the non magnetic
gm/min, and water flow rate 24.76 l/min. On the concentrate showed that it involves cassiterite, with
other hand increasing both feed rate and water flow little content of zircon.
rate more than 311.15 gm/min and 24.76 l/min
respectively leads to a slight decrease in the recovery
value.
Figure 6 (a & b) illustrates the response surfaces for 84.9646
the cleaning of shaking table concentrate using dry 82.8047

high intensity magnetic separation. It represents the 80.6448
recovery of cassiterite in non magnetic fraction at
R e co ve ry %
78.4849
different values of the studied factors. In figure 5a it
is noticed that with increasing both splitter 76.325
inclination and belt speed the recovery value

increases and reaches its maximum value about 97%
at splitter inclination 78.48 degree and belt speed
71.29 rpm. On the other hand increasing both 3.00
splitter inclination and belt speed more than 78.48 2.75
5.00
degree and 71.29 rpm respectively leads to a very 4.50
slight decrease in the recovery value. In figure 5b it is 2.50

4.00
noticed that with increasing both splitter inclination Stroke length (cm) 2.25 3.50
Inclination angle (degree)
and belt speed the recovery value increases and 2.00 3.00
reaches to the maximum value which is 98 % at
splitter inclination 78.62 degree and belt speed 73.89
rpm. On the other hand increasing splitter inclination Figure 5a. Response surfaces for the shaking table
concentrate recovery as a function of different factors
and belt speed more than 78.62 degree and 73.89 (water flow rate 20 l/min and feed rate 250gm/min.)
rpm respectively lead to a very slight decrease in the
recovery value.
3.6. Optimization of the Experimental

Parameters
Figure 7 (a & b) shows the optimum parameters that
give both maximum recovery and grade for shaking
table separation and dry high intensity magnetic.
3.00
Desirability
0.295 0.417
0.417 0.540
85.9647 0.540
84.4923
83.0198 2.75
Recovery %
81.5474
Stroke length (cm)

80.075
Predicti 0.91
2.50
25.00
400.00
22.50
325.00
2.25 0.786
20.00
250.00
water flow rate (l/min) 17.50 175.00
Feed rate (gm/min) 0.540
15.00 100.00 0.540
0.663
0.417
Figure 5b. Response surfaces for the shaking table 2.00
concentrate recovery as a function of different factors 3.00 3.50 4.00 4.50 5.00
(inclination angle 4 degree and stroke length 2.5 cm)

Inclination angle (degree)
(a)
97.212
100.00
Desirability
94.0903 0.381
0.381
90.9685
Recovery %
87.8468
87.50
0.536
84.725
0.536
Belt speed (rpm)
0.690 0.690
75.00
Predicti 1.00
100.00
80.00
87.50
77.50
75.00
75.00 62.50
Belt speed (rpm) 62.50 72.50
Splitter inclination (degree)
50.00 70.00
50.00
Figure 6a. Response surfaces for the dry magnetic 70.00 72.50 75.00 77.50 80.00
separation concentrate recovery as a function of (feed
rate 500gm/min.) Splitter inclination (degree)
(b)
Figure 7. Optimum parameters for shaking table and
98.2563 dry high ıntensity magnetic separation
95.1641
92.0719 Table 9. Optimum parameters for both shaking table

and dry high ıntensity magnetic separation
Recovery %
88.9797
Dry High Intensity Magnetic

85.8875
Separation
Inclination Splitter 74.95
α angle 4.13 ε inclination
100.00 (degree) (degree)
80.00
Stroke Belt speed 73
β length (cm) 2.50 δ
87.50
77.50
75.00
75.00
(rpm)
Feed rate Feed rate 742
Belt speed (rpm) 62.50 72.50
Splitter inclination (degree) γ (gm/min)
307.6 ϕ
(gm/min)
50.00 70.00
Water flow
λ 24.22
Figure 6. Response surfaces for the dry magnetic rate (l/min)
separation concentrate recovery as a function of (feed
rate 750gm/min)
Table 10. Shaking table and dry high ıntensity magnetic separation cassiterite concentrates at optimum
parameters
Fraction Weight % SnO2 % Recovery %
Concentrate 0.314 13.2 86.2
tail 99.686 0.0066 13.8
Total 100 0.048 100
Cleaning of Shaking Table Concentrate using Dry High Intensity Magnetic Separation
Fraction Weight % SnO2 % Recovery %
Operational Overall Operational Overall
Non magnetic 14.5 0.046 90.67 96.7 83.36
Magnetic 85.5 0.268 0.51 3.3 2.84
Total 100 0.314 13.2 100 86.20
Figure 8. X-ray diffraction for the shaking table concentrate
Figure 9. X-ray diffraction for the non magnetic concentrate
was successfully achieved. A statistical design using

4. CONCLUSIONS
the Box-Behnken design of experiments was
conducted on both shaking table separation and dry
Recovery of cassiterite from Igla Placer ore of
magnetic separation experiments to investigate the
Eastern Desert of Egypt using shaking table gravity
effect of main combination parameters. A
separation and high intensity dry magnetic separation
mathematical model for calculation of recovery and
grade for both shaking table and dry magnetic accumulations in the ESCAP region, Berlin,
separation is suggested according to the statistical Springer-Verlag, 3 (1988) 718.
experimental design. The best combination desirable
[10] B.L. Reed, Tin resources. In: Carr, D.D. and
experimental conditions obtained in case of shaking
Herz, N. eds, Concise encyclopedia of mineral
table separation are inclination angle (4.13 degree),
resources, Oxford, Pergamon Press., (1989)
Stroke length (2.5 cm), feed rate (307.6 gm/min), and
426.
water flow rate (24.22 l/min) and in case of using dry
high intensity magnetic separation are splitter [11] C.L. Sainsbury, Tin resources of the world, U.S.
inclination (74.9 degree), belt speed (73 rpm), and Geological Survey, Bulletin 1301 (1969) 1.
feed rate (742 gm/min). A shaking table concentrate
[12] J.F., Jr. Carlin, Tin, U.S. Geological Survey,
containing 13.2 % SnO2 and recovery of 86.2 % by
Mineral Commodity Summaries, (2008) 176.
weight SnO2 was obtained from a feed containing
about 0.061 % SnO2 at the best desirable condition [13] L.M. Falcon, The gravity recovery of cassiterite,
obtained. Cleaning of this concentrate by using dry Journal of the South African institute of mining
high intensity magnetic separation a final concentrate and metallurgy, 82 (1982)112.
with 90.67% SnO2 and recovery of 96.7% SnO2 by [14] A. Gupta and D.S. Yan, Mineral processing
weight was obtained. design and operation, Gravity separation,
(2006) 494.
REFERENCES
[15] Inc. Carpco, Expanding leadership in
[1] A. F. Holleman, E. Wiberg, Inorganic separation technology, Bulletin No. 929 (1992).
Chemistry, San Diego: Academic Press, (2001).
[16] Barry A Wills’ and Tim Napier-Munn, Wills'
[2] Joseph Watson, The stannic oxide Mineral processing technology (Seventh
semiconductor gas sensor in The Electrical Edition), Gravity concentration, (2005) 225.
engineering Handbook 3d Edition; Sensors
[17] H. C. Voges, Heavy-medium and gravity
Nanoscience Biomedical Engineering and
separation at Iscor's tin-ore and iron-ore mines,
Instruments ed R.C Dorf CRC Press Taylor
Journal of the South African institute of mining
and Francis, (2006).
and metallurgy, 82 (1982)186.
[3] Wang, Chun-Ming; Wang, Jin-Feng; Su, Wen-
[18] A. D. Read, A. Whitehead and T. J. N.
Bin, Microstructural morphology and electrical
Grainger-Allen, Pre-treatment of feed for dry
properties of copper- and niobium-doped tin
magnetic separation of fine materials,
dioxide polycrystalline varistors, Journal of the
International Journal of Mineral Processing, 3
American Ceramic Society 89 (2006) 2502.
(1976) 343.
[4] A. Dibb, M. Cilense, P.R. Bueno, Y. Maniette,
[19] R.O. Burt, International Journal of Mineral
J.A. Varela, and E. Longo, Evaluation of rare
Processing, 2 (1975) 219.
earth oxides doping SnO2.(Co0.25,Mn0.75)O-
based varistor System, Materials Research, 9 [20] M.S. Amin, A tin-tungsten deposits in Egypt,
(2006) 339. Econ. Geol., 42 (1947) 637.
[5] J.F., Jr. Carlin, Tin recycling in the United [21] Report of the Egyptian mineral resources
States in 1998, U.S.Geological Survey, circular authority, Investment chance in Egyptian
1196 (2003)1. mining sector, (2007).
(http://purl.access.gpo.gov/GPO/LPS50041). [22] A.H. Sabet, V.B. Tsogoev, S.P. Shibanin, M.B.
[6] R.G. Taylor, Geology of tin deposits, in El kait, and S. Awad, The placer tin deposits of
Developments in economic geology, no.11: Abu dabbab, Igla, and Nuweibi, Annals of the
New York, NY, Elsevier Scientific Publishing Geological Survey of Egypt, 6 (1976)169.
Company, (1979) 543. [23] G.E.P. Box, D.W. Behnken, Some new three
[7] C.S. Hutchison, Economic deposits and their level designs for the study of quantitative
tectonic setting. London, The Macmillan Press, variables, Technometrics, 2 (1960) 455.
(1983)365.
[8] K.F.G. Hosking, Mineral concentrations and
hydrocarbon accumulations in the ESCAP
region, Berlin, Springer-Verlag, 3 (1988)18.
[9] W.D. Menzie, B.L. Reed, and D.A. Singer,
Mineral concentrations and hydrocarbon
World Academy of Science, Engineering and Technology
Vol:2 2008-02-24
Performance Evaluation of Powder Metallurgy

Electrode in Electrical Discharge Machining of
AISI D2 Steel Using Taguchi Method
Naveen Beri, S. Maheshwari, C. Sharma, Anil Kumar
The recent developments in the field of EDM have
Abstract—In this paper an attempt has been made to correlate progressed due to the growing application of EDM process
the usefulness of electrodes made through powder metallurgy (PM) and the challenges being faced by the modern manufacturing
in comparison with conventional copper electrode during electric industries, from the development of new materials that are
discharge machining. Experimental results are presented on electric hard and difficult-to-machine such as tool steels, composites,
discharge machining of AISI D2 steel in kerosene with copper
ceramics, super alloys, hastalloy, nitralloy, waspalloy,
tungsten (30% Cu and 70% W) tool electrode made through powder
metallurgy (PM) technique and Cu electrode. An L18 (21 37)
nemonics, carbides, stainless steels, heat resistant steel, etc.
orthogonal array of Taguchi methodology was used to identify the Typically, the major cost and time components in die and
effect of process input factors (viz. current, duty cycle and flushing mould machining by EDM are in the electrode fabrication,
pressure) on the output factors {viz. material removal rate (MRR) which can account for over 50% of the total machining cost
[3]. Typical materials, used as EDM electrodes include
International Science Index Vol:2, No:2, 2008 waset.org/Publication/40
and surface roughness (SR)}. It was found that CuW electrode (made
through PM) gives high surface finish where as the Cu electrode is copper, brass, chromium, tungsten, steel, copper-tungsten and
better for higher material removal rate. copper chromium alloys [4,5,6]. Conventional methods of
fabricating the electrodes include stamping, coining, grinding,
Keywords—Electrical discharge machining (EDM), Powder extrusion, drawing, and more commonly, turning, milling,
Metallurgy (PM), Taguchi method, Material Removal Rate (MRR), incurring long processing time and material wastage
Surface Roughness (SR).
especially if a complex geometry or profile is required [4].
EDM research has concentrated on achieving faster and
I. INTRODUCTION
more efficient metal removal rate coupled with a reduction in
E LECTRICAL DISCHARGE MACHINING is a thermo-electrical

material removal process, in which tool electrode shape is
reproduced mirror wise into a work material, with the
tool wear and improved surface characteristics [7, 8, 9]. The
majority of work has been done using mechanically formed
tool electrodes and the present EDM user is compelled to
shape of the electrode defining the area in which the spark search for alternative tooling such as powder metallurgy (PM)
erosion will occur [1]. It has been widely used to produce method of electrode fabrication which is more economic and
dies, molds, aerospace, automotive industry and surgical faster to manufacture. A complex electrode made by
components [2]. It is also useful for machining brittle conventional method can cost around 100 times more than a
materials, as there is virtually no contact between the tool and simple square electrode. However, in the PM route a large
work-piece. number of tool electrodes can be made from a single die and
In EDM, the material is removed primarily through the punch assembly, resulting in an overall reduction of EDM
conversion of electrical energy into thermal energy through a tooling cost. Therefore, PM turns out to be a viable alternative
series of successive sparks between the electrode and the work to produce tool electrode in which the desirable properties of
piece in a dielectric fluid. The thermal energy is consumed in different materials can be combined. Moreover, the thermal,
generating high temperature plasma, eroding the work piece electrical, mechanical and micro structural properties of PM
material. Moreover there is no direct contact between the tool electrodes can be effectively controlled by the process
electrode and the work piece which eliminates mechanical variables such as compacting pressure and sintering
stresses chatter and vibration problems during machining. temperature. These will affect density and pore shape. An
example is an alloy of CuW made through PM where tungsten
particles are uniformly embedded in highly conductive copper
Naveen Beri is with Department of Mechanical Engineering, Beant College matrix. The electrodes made by using powder metallurgy
of Engineering & Technology, Gurdaspur, Punjab, India. (e-mail: technology from special powders have been used to modify
nav_beri74@yahoo.co.in).
S. Maheshwari, is with Division of Manufacturing Process & Automation
EDM surfaces in recent years, to improve wear and corrosion
Engineering, Netaji Subash Institute of Technology, Dwarka, New Delhi, resistance.
India. (e-mail: ssaacchhiinn@gmail.com). Gangadhar e.t. al. [10] reported surface deposition by EDM
C. Sharma is with Department of Mechanical and Automation Engineering, in a liquid dielectric using PM compact tool electrode.
IGIT, Kashmiri Gate, Delhi, India. (e-mail: chitrabisht@rediffmail.com).
Deposition of tungsten carbide on flank and rake of a HSS toll
Anil Kumar is with Department of Mechanical Engineering, Beant College
of Engineering & Technology, Gurdaspur, Punjab, India. (phone: +91- using PM electrode containing 40%WC and 60% Fe (zinc
9417286270 ; fax: +911874-221463; e-mail: ak_101968@yahoo.com). sterate as lubricant) with reverse polarity and kerosene as
dielectric resulted in low variation in cutting forces. Soni and
Chakraverti [11] found that appreciable amount of elements
International Scholarly and Scientific Research & Innovation 2(2) 2008 497
Vol:2 2008-02-24
has migrated from the tool electrode to work piece and vice freedom based upon number of parameters and their levels.
versa and got alloyed in the resolidified layer causing a The non-linear behavior of the process parameters, if exists,
change in chemical composition and significant increase in can only be revealed if more than two levels of the parameters
surface hardness of the work piece during electro-discharge are investigated. Therefore, parameter A was analyzed at two
machining of high carbon high chromium die steel (hardened) levels and parameter B, C & D were analyzed at three levels.
with rotating copper-tungsten tool electrode. EDMing of Experimental parameters and their levels selected for the
hardened steel (BS 970817M40, 53Rc) work material of Cu study are tabulated in Table 1 and all other parameters are
electrode made through PM and paraffin as dielectric has been kept constant.
reported by Samual et al. [12]. Wang, et al. [13] described a
new method of surface modification by EDM. By using an TABLE I
MACHINING PARAMETERS LEVELS
ordinary EDM machine tool and kerosene fluid, a hard
ceramic layer can be created on the work piece surface with a Factor Parameter Level 1 Level 2 Level 3
Ti or other compressed powder electrode in a certain symbol
condition. It was observed that a compact TiC ceramic layer A Electrode Material Copper Copper ---
(Cu) Tungsten
can be created on the surface of the metal work piece. (CuW)
Blending of copper powders containing resin with chromium B Current I (amp) 4.5 7.5 10.5
powders to form tool electrode has been investigated by Tsai C Duty Cycle 0.5 0.66 0.78
et al. [14]. Lee et .al [15] investigated the small area EDM D Flushing Pressure 0.3 0.5 0.7
Fp (Kg/cm2)
process using a copper–tungsten electrode on AISI 1045
carbon steel and has reported that the values of the MRR, SR
increase for higher values of pulse current. Ferreira [16]

observed that copper-tungsten electrodes with negative It was decided to study the two factor interaction effects and
polarity are suitable for the planetary EDM surface micro- the selected interactions were: (i) between current and duty
finishing of die steel (AISI H13) with good geometry cycle (B×C) and (ii) between current and flushing pressure
accuracy and sharp details. Chen et .al [17] has investigated (B×D) and other interactions are neglected. There are 7 degree
how machining characteristics and surface modifications of freedom owing to one two level parameter and three three
affect low-carbon steel (S15C) during electrical discharge level parameters and the degree of freedom of interactions
machining (EDM) processes with semi-sintered electrodes. It selected is 8. The total degree of freedom is 7+8 = 15. A
was found that the composition of the semi-sintered electrodes mixed orthogonal array L18 (21 37) was used for
was transferred onto the machined surface efficiently and experimentation as it has degree of freedom 17 which is more
effectively during the EDM process and that the process is than degree of freedom of selected machining parameters and
feasible and can easily form a modified layer on the machined interactions (7+8=15).
surface. To obtain optimal machining performance, the maximum
From the above reviewed literature it is observed that PM MRR and the minimum SR are desired. Therefore, the lower-
tool electrodes have a significant role in metal removal the-better SR and the higher-the-better MRR criteria was
process in addition to their contribution in surface selected.
treatment/modification applications and a need is felt to The loss function Lij of the lower-the-better performance
correlate the usefulness of CuW electrode made through characteristic can be expressed as
n
powder metallurgy (PM) with a view to optimize the process 1 1
parameters [10,18,19,20]. L if
n
¦k 1
2
y ijk
The present experimental work is focused on the electrical (1)
discharge machining of AISI D2 steel with CuW (30% Cu and
70% W) electrode made through PM technique in comparison where Lij is the loss function of the ith performance
with convention Cu electrode and an attempt has been made to characteristic in the jth experiment, n the number of tests, and
obtain optimal setting of the process input parameters for yijk is the experimental value of the ith performance
optimum MRR and SR with kerosene as dielectric fluid. characteristic in the jth experiment at the kth test.
Taguchi methodology has been applied to plan and analyze The loss function of the higher-the-better performance
the experiments. characteristic can be expressed as
n
1
II. EXPERIMENTAL WORK L if
n
k 1
¦ 2
y ijk
(2)
A. Experimental Planning (Taguchi Method) The loss function is further transformed into an S/N ratio. In
Taguchi method uses special design of orthogonal array to the Taguchi method, the S/N ratio is used to determine the
study the entire parameters space with only a small number of deviation of the performance characteristic from the desired
experiments. In selecting an appropriate OA, the pre- value [21]. The S/N ratio Zij for the ith performance
requisites are (i) selection of process parameters and interac- characteristic in the jth experiment can be expressed as
tions to be evaluated (ii) selection of number of levels for the n ij 10 log Lij
selected parameters, and (iii) evaluation of total degree of (3)
Vol:2 2008-02-24
material, current, duty cycle and flushing pressure effect the

multiple performance characteristics.
B. Experimental Procedures and Parameters
The experiments were carried out on a standard EDM TABLE III
machine; model SPARKMAN (S-10) of Sparkonix with ANOVA FOR MRR
straight polarity. AISI D2 Steel (specimens 85mm X 25mm X
3mm) hardened to 55-58 HRC was used as work piece Source DF Seq SS Adj SS Adj MS F P
material with commercial grade kerosene as the dielectric A 1 189.420 189.420 189.420 57.39 0.017
fluid. Cylindrical Cu electrodes (I 8mm) and CuW electrodes B 2 479.116 479.116 239.558 72.58 0.014
C 2 12.549 13.440 6.720 2.04 0.329
made through powder metallurgy (Cu30%, W70%, I 8mm) D 2 8.230 5.865 2.932 0.89 0.530
were used for the experimentation. BXC 4 1.231 2.075 0.519 0.16 0.943
BXD 4 2.663 2.663 0.666 0.20 0.917
Work piece was weighed on digital balance (accuracy 1 Residual
mg) to get the initial weight before machining. Then erosion Error 2 6.601 6.601 3.301
was switched on for a depth of cut of 1mm and time taken to Total 17 699.810
complete the operation was noted and the work piece was
weighed again. The surface roughness (Ra value in microns)
was measured on Surfcoder (model SE 1200, make Kosaka It is clear from fig. 1 that MRR is maximum at the 1st level
Laboratory Ltd., Japan). Two sets of 18 experiments (as of parameter A, 3rd level of parameter B, 2nd level of
depicted in coded form in Table 2) were performed as per L18 parameter C and 3rd level of parameter D. The S/N ratio
(21×37) Taguchi design and average value of each output analysis suggests the same levels of the parameters (A1, B3, C2
and D3) as the best levels for maximum MRR
parameter were statistically analyzed using Minitab 14.1

software.
Main Effects Plot (data means) for SN ratios
TABLE II A B
1 7 30
EXPERIMENTAL LAYOUT USING MIXED ORTHOGONAL ARRAY L18 (2 ×3 )
25
Exp. No. Electrode Current Duty Cycle Flushing Pr.
material (I) (amp) (DC) (P) (Kg/cm2) 20
Mean of SN ratios
(A) (B) (C) (D) 15

1 1 1 1 1 1 2 4.5 7.5 10.5
2 1 1 2 2 C D
30
3 1 1 3 3
4 1 2 1 1 25
5 1 2 2 2 20
6 1 2 3 3
7 1 3 1 2 15
0.50 0.66 0.78 0.3 0.5 0.7
8 1 3 2 3
Signal-to-noise: Larger is better
9 1 3 3 1
10 2 1 1 3
11 2 1 2 1
12 2 1 3 2 Fig. 1 Mean effect plot for S/N ratios for material removal rate
13 2 2 1 2 (MRR)
14 2 2 2 3
15 2 2 3 1 The interaction graph (Fig. 3) also reveals that B3 , C2 and
16 2 3 1 3
D3 is the best treatment combination to give maximum MRR.
17 2 3 2 1
18 2 3 3 2 These graphs show significant influence of current on the
output parameters. MRR increases with the increase in current
for both the electrodes but it is less with CuW electrode as
III. RESULTS AND DISCUSSIONS compared with Cu electrode this can be attributed to the
deposition of material from CuW electrode on the work piece
The mean effects plots of the S/N ratios for the output
and its lower conductivity.
measures are obtained using Minitab 14.1 software. Plots with
the steeper slope along with longer lines shows that the factor
B. Analysis of Surface Roughness (SR)
has significant impact on the output parameter.
The average values of S/N ratios for SR at different levels
A. Analysis of Material Removal Rate (MRR) are plotted in Fig. 3 keeping the objective as “smaller is
The average values of S/N ratios for MRR at different levels better”. In order to study the significance of the parameters in
are plotted in Fig. 1 keeping the objective as “larger is better”. affecting the quality characteristic of interest i.e. SR ANOVA
In order to study the significance of the parameters in was performed. The S/N ANOVA for SR is given in Table 3.
effecting the quality characteristic of interest i.e. MRR The result of ANOVA indicates that electrode material,
ANOVA was performed. The S/N ANOVA for MRR is given current, duty cycle and flushing pressure effect the multiple
in Table 3. The result of ANOVA indicates that electrode performance characteristics.
Vol:2 2008-02-24
Interaction Plot (data means) for SN ratios Interaction Plot (data means) for SN ratios
0.50 0.66 0.78
0.50 0.66 0.78
30
B -5 B
4.5
24 4.5
7.5
B 10.5 -10 7.5
18
B 10.5
-15
30
C
0.50 -5 C
24 0.66 0.50
C 0.78 0.66
-10
18 C 0.78
30 -15
D
0.3
24 -5 D
0.5
D 0.7 0.3
18 -10 0.5
D 0.7
4.5 7.5 10.5 0.3 0.5 0.7 -15
S ignal-to-noise: Larger is better

4.5 7.5 10.5 0.3 0.5 0.7
Fig. 2 Interaction plot for S/N ratios for material removal rate (MRR)
Fig. 4 Interaction plot for S/N ratios for surface roughness (SR)
TABLE IV
ANOVA FOR SR Confirmation experiment was performed at A1, B3, C2 and
D3 levels of the parameters for maximum MRR as suggested
by the mean effect plot of MRR and MRR obtained is 43.0211
A 1 15.213 15.213 15.213 4.98 0.155 mg/min. Another confirmation experiment was performed at
B 2 349.624 349.624 174.812 57.28 0.017 A2, B1, C1 and D1 levels of the parameters for maximum SR as
C 2 6.037 4.062 2.031 0.67 0.600
suggested by the mean effect plot of SR and the SR obtained
D 2 0.606 0.015 0.008 0.00 0.998
BXC 4 3.058 2.361 0.590 0.19 0.922 is 1.38 microns.
BXD 4 0.143 0.143 0.036 0.01 0.999
Residual IV. CONCLUSIONS
Error 2 6.104 6.104 3.052
Total 17 380.784 The Taguchi approach employed enabled the identification
of significant factors and their associated levels on specific
output measures. Selection of appropriate operating values
Main Effects Plot (data means) for SN ratios from these data enabled preferred work piece characteristics to
-5.0
A B be achieved. During EDMing of AISID2 steel it is found that
-7.5 electrode material, current and duty cycle has significant
-10.0 effect on both the performance parameters. Best parameter
-12.5
selection with in the experiment range for maximum MRR is
Mean of SN ratios
-15.0
with copper electrode at 10.5 A current, 0.66 duty cycle and
1 2 4.5 7.5 10.5
0.7 Kg/cm2 flushing pressure i.e. A1B3C2D3 and for minimum
C D
-5.0 surface roughness is with copper tungsten electrode at 4.5 A
-7.5
current, 0.50 duty cycle and 0.3 Kg/cm2 flushing pressure i.e.
-10.0
-12.5
A2B1C1D1. From above it is obtained that Cu electrode is
-15.0 better for higher MRR and CuW electrode gives minimum
0.50 0.66 0.78 0.3 0.5 0.7
surface roughness. So if the requirement is to have high MRR
Signal-to-noise: Smaller is better then it is recommended to use Cu electrode and if the
requirement is to have better surface finish only on the
Fig. 3 Mean effect plot for S/N ratios for surface roughness (SR) machined surface of AISI D2 steel then it is recommended to
use CuW electrode made through PM.
It is clear that SR is minimum at the 2nd level of parameter
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Proceedings of the International Conference on Mining, Material and Metallurgical Engineering
Prague, Czech Republic, August 11-12, 2014
Paper No. 113
Flotation of Nickel-Copper Sulphide Ore: Optimisation of

Process Parameters Using Taguchi Method
Trust T. Masiya
University of Zimbabwe, Institute of Mining Research
P.O. Box MP167, Mount Pleasant, Harare, Zimbabwe
tmasiya@science.uz.ac.zw
Willie Nheta
University of Johannesburg, Department of Metallurgy
Faculty of Engineering & Built Environment,
South Africa, PO Box 526, Wits 2050, South Africa
wnheta@uj.ac.za
Abstract -Froth flotation is widely used for concentration of base metal sulphide minerals in complex ores. One of
the major challenges faced by flotation of these ores is the ever varying grade and mineralogy. This therefore calls
for a continual characterisation and optimisation of flotation parameters such that concentrator performance as a
whole is always maintained. In this study, the robust Taguchi experimental design method was used to determine the
optimum conditions for the flotation of nickel, copper and cobalt from a nickel-copper sulphide ore. The parameters
investigated include collector dosage, percentage solids, depressant dosage and pH. The effects of these parameters
at three different levels on the recovery of Ni, Cu and Co were investigated using an L9 Taguchi orthogonal array.
The optimum conditions for the recovery of the base metals are collector dosage, 80g/t; pH, 10.15; %solids, 25; and
depressant dosage, 100g/t. Relative significance of flotation parameters (based on difference between max and min.
values) indicates that pH has the most significant effect on the recovery of nickel, copper and cobalt during flotation.
Analysis of variance showed that pH and depressant dosage were the most significant parameters affecting the
recovery of Ni, while collector dosage and percentage solids were insignificant. None of the tested parameters
significantly affected copper recovery whilst pH was found to also significantly affect cobalt recovery.
Keywords: flotation, process optimization, Taguchi orthogonal array, ANOVA.
1. Introduction
Froth flotation is widely used for separating base metal sulphide minerals in complex ores. One of
the major challenges faced by the flotation of these ores is the ever varying grade and mineralogy as the
ore is exploited (Kabuda et. al., 2011). As in any mineral processing operation the efficiency of the
flotation separation is highly dependent on changes in feed characteristics all of which may influence
product grade and recovery (Nashwa, 2007). There is therefore need to continually characterise such ores
and optimise their flotation parameters such that concentrator performance as a whole is always
maintained. Flotation efficiency depends on a number of parameters which include particle size, pulp
density, water quality, pH and reagent dosage (Pérez-Garibay et. al., 2014; Muzenda, 2010; Saleh, et. al.,
2008; Shuhua, 2006; Göktepe, 2002). Therefore, in order to achieve maximum recoveries and grades
these parameters should be delicately balanced and optimised collectively (Muzenda et. al., 2011).
The Taguchi experimental design method has been shown to be an effective means for the
improvement of quality and productivity in research and development (IIyas, 2010). It is a well-accepted
technique that has been widely used for product design and process optimization in manufacturing and
engineering worldwide [Kamaruddin et. al., 2004; Gopalsamy et. al., 2009; Rama and Padmanabhan,
2012; Sapakal and Telsang, 2012]. In recent years, its use has extended to include the metallurgical
113-1
industry [Ilyas et. al., 2010; Haghi et.al. 2009; Temur et. al., 2009; Abali et al., 2006]. It provides a
simplified systematic and efficient methodology for process optimisation (Bagchi, 1993). The greatest
advantage of this method is the saving of effort in conducting experiments; saving experimental time,
reducing the cost, and discovering significant factors quickly. The number of experiments that need to be
done is greatly reduced compared to that required by other classical statistical methods such as factorial
design.
The Taguchi method was therefore, selected to determine the optimum conditions for maximising
the flotation recovery of Ni, Cu and Co from a nickel-copper sulphide ore. The effect on flotation
performance of various parameters such as pH, collector dosage, % solids and depressant dosage at
different levels was investigated. Therefore, the main objective of the study was to optimize the process
parameters for the flotation of base metals from a nickel-copper sulphide ore.
2. Materials and Methods

2. 1. Materials
The nickel-copper sulphide ore used in this study was supplied by Trojan Nickel Mine located in
Bindura, Zimbabwe. From the X-ray diffraction analysis, the main phases present in the ore were
pentlandite (49.4%), pyrrhotite (41.2%) and quartz (4.6%), Fig.1. The ore which was supplied in lumpy
form was subjected to crushing and grinding. The ore was ground to 70% passing 75 microns. Chemical
analysis of this ore is shown in Table 1. 1% solutions of all flotation reagents i.e. collector (SIPX- sodium
isopropyl xanthate) and depressant (Betamin 300) were used for the investigations and 10% solutions of
both analytical grade sulphuric acid and sodium hydroxide were used as pH modifiers. For each test
freshly prepared reagent solutions were used. Distilled water was used in all flotation experiments.
Fig.1. X-ray diffraction pattern of the nickel-copper sulphide ore sample
Table. 1. Chemical composition of the nickel-copper sulphide ore (mass fraction, %).
Component Ni Cu Co Fe MgO SiO2 SG

% 12.61 0.71 0.17 47.04 0.13 10.60 4.38
2.2 Experimental Plan

Based on previous studies and literature, collector dosage, pH, percentage solids and the depressant
dosage were chosen as the four main parameters to be investigated. According to the Taguchi design
methodology, three levels were chosen for each parameter as illustrated in Table 2. Considering the four
parameters and the relevant three levels, a Taguchi Orthogonal array (L9) was established to execute the
experiment. Nine experiments were therefore conducted as shown in Table 3. One (1) to three (3) levels
appearing in Table 3 are the relative levels of the parameters indicated in Table 2. In this study
interactions between parameters were not taken into consideration.
113-2
Table. 2. Experimental parameters and their relative levels.
Levels
Code Parameter 1 2 3
A pH 6.15 8.15 10.15
B Collector Dosage (g/t) 40 60 80
C Depressant dosage (g/t) 80 100 150
D %Solids 20 25 30
Table. 3. Taguchi Orthogonal array (L9;34) for influencing factors and their levels coded with actual values in
brackets.
Experiment No. pH Collector Dosage (g/t) %Solids Depressant dosage (g/t)

1 1 (6.15) 1 (40) 1 (20) 1 (80)
2 1 (6.15) 2 (60) 2 (25) 2 (100)
3 1 (6.15) 3 (80) 3 (30) 3 (150)
4 2 (8.15) 1 (40) 2 (25) 3 (150)
5 2 (8.15) 2 (60) 3 (30) 1 (80)
6 2 (8.15) 3 (80) 1 (20) 2 (100)
7 3 (10.15) 1 (40) 3 (30) 2 (100)
8 3 (10.15) 2 (60) 1 (20) 3 (150)
9 3 (10.15) 3 (80) 2 (25) 1 (80)
In experiments based on the Taguchi design the use of signal-to-noise (SN) ratios is recommended
for the optimisation of process parameters. In the Taguchi method the term signal represents the desirable
value (mean) for the output characteristics and the term noise represents the undesirable values (standard
deviation) for the output characteristic. The SN ratios can then be calculated based on the required
response characteristics i.e. ‘larger is better’, ‘smaller is better’ and ‘nominal is better’. In this
investigation the aim is to increase the amount of the base metal recovered to the concentrate, therefore
SN ratios for “larger is better” were selected and calculated using response values i.e. percentage metal
(Ni, Cu or Co) recovered. The SN ratio for this scenario was determined using:
SN = -10 [ ∑ ( )] (1)
Where n is the number of repetition of experiments, and yi is the response value (recovery) of the ith
experiment.
2. 2. Flotation Procedure
All the flotation test-work was done using the Denver laboratory machine with a 1.5l stainless steel
flotation cell. The required mass of nickel-copper sulphide ore material ground to 70% passing 75 µm
was weighed and placed in the flotation cell. This was followed by the addition of distilled water to about
60% of the cell volume before the required volumes of 1% solutions of the collector; SIPX (sodium
isopropyl xanthate) and depressant were added. The additions of the reagents solution were done using
small (2-5ml) barrel medical syringes. More water was added to the cell to about 90% cell volume (about
10mm below the froth overflow lip). pH was then adjusted to the required set value using either sulphuric
acid or sodium hydroxide. Two drops of the frother were then added before conditioning with the air
valve closed for 4 minutes at 750rpm agitation. Following conditioning, the air valve was opened to
113-3
maximum to allow aeration. After 3 minutes the froth was allowed to overflow and the float was kept at
constant level mark (10mm below overflow lip) using distilled water from a wash bottle. Samples of the
froth concentrate were collected after every 5minutes for 20 minutes. The collected samples were then
sun-dried, weighed and assayed for nickel, cobalt and copper. The same drying procedure was also
followed for the tailings. The experimental runs as described in Table 3 were run randomly and were done
in duplicate. A total of 18 batch flotation test-works were done for this study.
The amount of metal (Ni, Cu or Co) recovered was calculated using equation (2) which is based on
assays alone of the feed (f), tailings (t) and concentrate (c).
( )
%Metal Recovery = 100( ) ( )
(2)
2. 2. Analysis of Variance
Analysis of variance (ANOVA) is a standard statistical tool that can be used to interpret
experimental data. A statistical test called an F-test, named after Fisher, is then used to see which
process parameters have a significant effect on recovery. The contribution percentage of various
parameters to the response can also be estimated by ANOVA. This identifies the parameter with
the highest influence on metal recovery. The equations involved in the analysis of variance are
presented in this section.
The total sum of squared deviations, SST was calculated based on the following formula:
(∑ )
SST = ∑ ( ) - (3)
Where,
N is the total number of observations or experiments,
Yi is the metal recovery for the ith experiment
The total sum of squared deviations is composed of two sources: the sum of squared deviations,
SSP due to each process parameter and the sum of squared error, SSE.
(∑ ) (∑ )
SSP = ∑ - (4)
Where p is one of the parameter of the experiment and j the level number of this parameter p
The sum of squared error is therefore calculated as:
SSE = SST - ∑ (5)
The variance (VP), mean of squared deviations for each parameter p was computed using the
following equation:
VP = ( )
(6)
Where NK is the number of levels for each parameter (3 in this case) and NK-1 = fP is therefore the
degrees of freedom for parameter, p. The total degrees of freedom of the result (fT) are equal to the total
number of experiments (9 in this case) minus one. The degrees of freedom for the experimental error (fE)
is then given by:
113-4
fE = fT - ∑ (7)
This is followed by the calculation of the variance ratio (Fcalc) for each parameter, which is defined by
Fcalc = (8)
Where VE is the mean square (variance) of the error.
This is used in the evaluation of significance of the parameters on the response. The percentage
contribution of each parameter to the response is then determined as:
%PC= *100 (9)
where PSSp is the pure sum of squares of each factor and is given by;
PSSP = SSp – fiVE (10)
3. Results and Discussions

This section gives a summary of the findings for the flotation performance of nickel, copper and
cobalt in the supplied sulphide ores. It is also dedicated to the analysis of data and identification of the
optimal levels for all control parameters. Minitab 15.0 was used for statistical data analysis.
3.1 Base Metal Recovery

The average recovery of metals (nickel, copper and cobalt) by flotation for the various
combinations of process parameters and levels is shown in Table 4. The highest recovery of nickel of
81% into the concentrate occurred in the 7th experiment run (pH = 10.15; collector dosage = 40g/t; %
solids = 30; depressant dosage = 100g/t) and the lowest (38.3%) was recorded in the 5 th experiment run
(pH=8.15; collector dosage=60g/t; %solids=30; depressant dosage=80g/t). For copper the maximum
recovery was 91.1% achieved in the 9th experimental run whilst lowest (25%) was recorded in the 1 st
experimental run. The maximum cobalt recovery (70.6%) was achieved in the 9th experimental run.
Table. 4. Experimental results for metal (Ni, Cu, Co) recovery.
Ave. Ave. % Ave.

Exp. Collector Depressant
pH %Solids %Ni Cu %Co
No. Dosage (g/t) dosage (g/t)
Recovery Recovery Recovery
1 1 (6.15) 1 (40) 1 (20) 1 (80) 56.4 25.0 27.8
2 1 (6.15) 2 (60) 2 (25) 2 (100) 75.6 64.0 26.4
3 1 (6.15) 3 (80) 3 (30) 3 (150) 64.7 50.8 25.7
4 2 (8.15) 1 (40) 2 (25) 3 (150) 40.7 51.8 7.7
5 2 (8.15) 2 (60) 3 (30) 1 (80) 38.3 54.4 10.8
6 2 (8.15) 3 (80) 1 (20) 2 (100) 61.5 67.3 21.5
7 3 (10.15) 1 (40) 3 (30) 2 (100) 81.0 78.7 63.6
8 3 (10.15) 2 (60) 1 (20) 3 (150) 48.3 85.7 41.8
9 3 (10.15) 3 (80) 2 (25) 1 (80) 70.0 91.1 70.6
113-5
To determine the effect each parameter has on the response, the signal-to-noise ratio (SN) was
calculated for each experiment. The SN ratio, based on ‘larger is better’ (Eqn.1), for the base metal
recoveries for all the experimental runs are shown in Table 5.
Table. 5. SN ratios for metal recovery based on ‘larger is better’.
Exp. Collector Depressant SN ratio SN ratio SN ratio

pH %Solids
No. Dosage (g/t) dosage (g/t) for Ni for Cu for Co
1 1 (6.15) 1 (40) 1 (20) 1 (80) 35.03 27.96 28.88
2 1 (6.15) 2 (60) 2 (25) 2 (100) 37.57 36.12 28.43
3 1 (6.15) 3 (80) 3 (30) 3 (150) 36.22 34.12 28.20
4 2 (8.15) 1 (40) 2 (25) 3 (150) 32.19 34.29 17.73
5 2 (8.15) 2 (60) 3 (30) 1 (80) 31.66 34.71 20.67
6 2 (8.15) 3 (80) 1 (20) 2 (100) 35.78 36.56 26.65
7 3 (10.15) 1 (40) 3 (30) 2 (100) 38.17 37.92 36.07
8 3 (10.15) 2 (60) 1 (20) 3 (150) 33.68 38.66 32.42
9 3 (10.15) 3 (80) 2 (25) 1 (80) 36.90 39.19 36.98
Using data in Table 5, the average SN ratios of each level of the four parameters for the flotation of
nickel were calculated and listed in Table 6. Delta values, which show the relative significance of the
factors, were also calculated as the difference between the maximum and minimum average values. Based
on this, depressant dosage followed by pH under the experimental conditions tested were the most
influencing factors affecting the flotation behaviour of nickel from the sulphide ore. Percentage solids had
the least influence on flotability of the nickel.
Table. 6. Average SN values for nickel flotation at three levels of parameters and delta statics.
Code Flotation parameter Level 1 Level 2 Level 3 Delta(max-min) Rank

̅ pH 36.28* 33.21 36.25 3.06 2
̅ Collector dosage 35.13 34.30 36.30* 2.00 3
̅ %Solids 34.83 35.55* 35.35 0.72 4
̅ Depressant dosage 34.53 37.17* 34.03 3.14 1
*
Optimum condition
The level of a parameter with highest average SN ratio corresponds to a better performance and
gives the best combination level. Therefore, the optimal levels of flotation parameters are the ones with
the greatest average SN ratio. The optimum levels of parameters for recovery of nickel are pH, 6.15
(Level 1); collector dosage, 80g/t (Level 3); %solids, 25 (Level 2); and depressant dosage, 100g/t (Level
2), asterixed figures in Table 6. A plot of the graph of the parameter against its response on each level is
referred to as the main effect and it indicates the general trend of influence of each parameter. Fig.2
shows the effect of the process parameters on flotation recovery of nickel.
113-6
Fig.2. Main effect of process parameter on nickel recovery.
Delta values in Table 7 show that pH has the most relative significance on the flotation behaviour
of copper and is followed by collector dosage, which is ranked second. Percentage solids show the least
relative significance. The optimum levels for copper recovery are pH, 10.15 (level 3); collector dosage,
80g/t (level 3); percentage solids, 25 (level 2); and depressant dosage, 100g/t (level 2).
Table. 7. Average SN values for copper flotation at three levels of parameters and delta statics.
Flotation parameter Level 1 Level 2 Level 3 Delta (max-min) Rank

̅ pH 32.73 35.19 38.59* 5.86 1
̅ %Solids 34.39 36.53* 35.58 2.14 4
*
Optimum condition
Fig.3 shows the main effects of process parameters on copper flotation.
Fig.3. Main effect of process parameter on copper recovery
113-7
Delta values for cobalt in Table 8 also show pH as the most influencing parameter and percentage
solids as the least influencing parameter affecting its flotation behaviour. The asterixed values in Table 8,
i.e. pH level of 3 (10.15), collector dosage level 3 (80g/t), percentage solids level 1 (20%) and depressant
dosage level 2 (100) gives the optimum recovery of cobalt into the concentrate.
Table. 8. Average SN values for cobalt flotation at three levels of parameters and delta statics.
Code Flotation parameter Level 1 Level 2 Level 3 Delta (max-min) Rank

̅ pH 28.50 21.68 35.16* 13.48 1
̅ %Solids 29.32* 27.71 28.31 1.61 4
*
Optimum condition
The change in response performance with change in process parameter is shown in Fig.4.
Fig.4. Main effect of process parameters on cobalt recovery.
3.2 Analysis of Variance (ANOVA)

The parameters which significantly affected the base metal recovery were investigated using the
analysis of variance (ANOVA). The contribution percentage of different parameters on nickel, copper and
cobalt recovery as obtained by ANOVA are presented in Table 6, 7 and 8, respectively. These percentage
values also confirm the relative importance of each parameter. For example, it can be seen from Table 6
that the pH (A), collector dosage (B) and depressant dosage (D) affect nickel recovery by 41.84%,
12.26% and 38.25% in the flotation of nickel-copper sulphide ore respectively. Since the degree of
freedom for the error term is zero, it was necessary to pool the parameter having less influence (%solids
in this case) for the results to be interpreted.
Based on ANOVA and at 95% confidence level, pH has significant effect on the flotation recovery
of both nickel and cobalt from the sulphide ore whilst depressant dosage has significant effect only on
nickel recovery. None of the tested parameters significantly affected the recovery of copper at the tested
same confidence level.
113-8
Table. 9. ANOVA table for nickel recovery after pooling (at 95% confidence level).
Code Parameter Degree of Sum of Mean Fcalc ratio P-Value Pure Sum %PC
freedom squares Squares, Vi of Squares
A pH 2 18.64677 9.323383 22.89789 0.0418 17.83242 41.84
B Collector Dosage 2 6.038956 3.019478 7.415726 0.1188 5.224611 12.26
C %Solids 2 0.834956 0.417478 - -
D Depressant dosage 2 17.11776 8.558878 21.02029 0.0454 16.30341 38.25
Error 0 0 - - -
(Pooled Error) (2) (0.814344) (0.40717) 3.257378 (7.64)
Total 8 42.61782
Table. 10. ANOVA table for copper recovery after pooling (at 95% confidence interval).
Code Parameter Degree of Sum of Mean Fcalc P-Value Pure Sum %PC
freedom squares Squares ratio of Squares
A pH 2 51.90207 25.95103 7.524001 0.1173 45.00387 49.02

C %Solids 2 6.8982 3.4491 - -
D Depressant dosage 2 12.88807 6.444033 1.868323 0.3486 5.989867 6.52
Error 0 0
Pooled Error (2) (6.8982) (3.4491) 0(27.5928) (30.06)
Total 8 91.8102
Table. 11. ANOVA table for cobalt recovery after pooling (at 95% confidence interval).
Code Parameter Degree of Sum of Mean Fcalc P- Pure Sum %PC

freedom squares Squares ratio Value of Squares
A pH 2 272.31000 136.15500 69.16062 0.0143 268.3726 82.44
C %Solids 2 3.937356 1.968678 - - - -
D Depressant 2 28.01076 14.00538 7.114104 0.1232 24.0734 7.40
dosage
Error 0 0
Pooled Error (2) (3.937356) (1.968678) 0(15.74942) (4.84)
Total 8 325.5208
3.3 Prediction of the Optimum Performance

Once the optimum parameters have been determined, the optimum performance of the response at
these parameters can be predicted. The predicted SN ratio (SNopt) of recovery of the metal (Ni, Cu &Co)
at optimum condition was calculated by adding the mean performance to the contribution of each
parameter at the optimum level using the following equation.
SNopt = + (̅ ) + (̅ ) + (̅ ) + (̅ ) (11)
where,
SNT : grand total of average SN ratio for each experiment,
N : total number of experiments,
̅ : average SN ratio for parameter A at its optimum level,
̅ : average SN ratio for parameter B at its optimum level,
̅ : average SN ratio for parameter C at its optimum level, and
113-9
̅ : average SN ratio for parameter D at its optimum level.
Since the sum of squares due to the parameter C is small as well as used to estimate the error variance,
this term is not included in the prediction of the optimum recovery. Table 12 shows the optimum level of
each parameter to achieve the highest Ni recovery and the corresponding recoveries of Cu and Co; highest
Cu recovery and corresponding recoveries of Ni and Co; and the highest Co recovery and corresponding
Ni and Co recoveries.
Table. 12. Predicted SN and metal recoveries at optimum conditions.
Target A B C D Predicted value for Ni Predicted value for Cu Predicted value for Co
SN Recovery SN Recovery SN Recovery
Ni recovery- 6.15 80 - 100 39.27 91.94 35.22 57.68 32.59 42.61
max
Cu recovery- 10.15 80 - 100 39.24 91.62 41.08 100 39.25 91.73
max
Co recovery- 10.15 80 - 100 39.24 91.62 41.08 100 39.25 91.73
max
4. Conclusion
The following conclusions are drawn from the present study within the levels of process parameters
selected:
 The optimum conditions for maximum Ni recovery are: collector dosage, 80g/t; pH, 6.15; %solids,
25; and depressant dosage, 100g/t. For maximum Cu recovery the optimum conditions are:
collector dosage, 80g/t; pH, 10.15; %solids, 25; and depressant dosage, 100g/t whilst for Co
recovery they are: collector dosage, 80g/t; pH, 10.15; %solids, 25; and depressant dosage, 100g/t.
 The optimal levels of parameters for the maximum recovery of all the three base metals is achieved
with a pH, 10.15; collector dosage, 80g/t; percentage solids, 25% and depressant dosage of 100g/t.
 Relative significance of flotation parameters (based on difference between max and min. average
values) indicates that pH has the most significant effect on the recovery of nickel, copper and
cobalt during flotation.
 Based on ANOVA and at 95% confidence level, pH has significant effect on the flotation recovery
of both nickel and cobalt from the sulphide ore whilst depressant dosage has significant effect only
on nickel recovery. None of the factors significantly affect the recovery of copper at the tested
confidence level of 95%.
 pH has the major contribution in controlling the flotation of the base metals (Ni, Cu and Co) from
the nickel-copper sulphide ore. Depressant dosage also plays a significant effect in controlling the
flotability of nickel (~40% contribution to overall nickel recovery). The range of percentage solids
considered for this study had the least contribution on recovery of base metals.
Acknowledgements
The authors would like to acknowledge Trojan Nickel Mine for supplying the ore material used
for this study.
113-10
References
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Bagchi, T.P. (1993). Taguchi methods explained: Practical steps to robust design, Prentice-Hall of India
Private Limited, New Delhi
Göktepe, F. (2002). Effect of pH on pulp potential and sulphide mineral flotation, Turkish J. Eng. Sci. 26,
pp. 309-318
Gopalsamy, B.A., Mondal, B. and Ghosh,S. (2009). Taguchi method and ANOVA: An approach for
process parameters optimization of hard machining while machining hardened steel, Journal of
scientific and Industrial Research, Vol. 68, pp. 686-695
Haghi, H., Ghadyani, A., Biranvand, B., and Shafaei, S.Z. (2009). Optimization of Apatite flotation using
Taguchi method, 7th industrial Minerals Symposium and Exhibition, 25-27 February, Turkey
IIyas, S., Bhatti, H.N., Bhatti, I.A., Sheikh, M.A., and Ghauri, M.A. (2010). Bioleaching of metal ions
from low grade sulphide ore: Process optimization by using orthogonal experimental array design,
African Journal of Biotechnology, Vol. 9(19), pp. 2801-2810
Kabuba, J., Muzenda, E., and Ntuli, F. (2011). Examination of flotation reagents suitable for nickel
concentrator plant, 2nd International Conference on Chemistry and Chemical engineering, IPCBEE,
Vol.14, Singapore, pp. 65-69
Kamaruddin, S., Khan,Z.A., and Wan, K.S. (2004). The use of the Taguchi method in determining the
optimum plastic injection moulding parameters for the production of a consumer product, Jurnal
Mekanikal, Bil.18, pp. 98-110
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Academy of Science, Engineering and Technology 45, pp. 237-241
Muzenda, E., Afolabi, A.S., Abdulkareem, A.S. and Ntuli, F. (2011). Effect of pH on the Recovery and
grade of base metal sulphides (PGMs) by flotation, Proceedings of the World Congress on
engineering and Computer Science 2011 Vol II, WCECS 2011, October 19-21, San Francisco, USA
Nashwa, V.M. (2007). The flotation of high talc-containing ore from the Great Dyke of Zimbabwe, MSc
Thesis, University of Pretoria
Pérez-Garibay, R., Ramírez-Aguilera, N., Bouchard, J., and Rubio, J. (2014). Froth flotation of sphalerite:
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Saleh, A-H.M., Ramadan, A.M., and Moharam, M.R. (2008). Beneficiation of Egyptian Abu-Swayel
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International Symposium on Sustainable Development, June 9-10, Sarajevo
113-11
Available online at www.sciencedirect.com
ScienceDirect
Procedia Materials Science 6 (2014) 503 – 511
3rd International Conference on Materials Processing and Characterisation (ICMPC 2014)
Optimization of Wear Performance of Aa 5083/10 Wt. % Sicp

Ravindra Singh Ranaa, Rajesh Purohitb, Anil kumar Sharmac, Saraswati Ranad
a,
Assistant Professor, Mechanical department Manit, Bhopal and 462052 , India
b,
Associate Professor, Mechanical department Manit, Bhopal and 462052 , India
c,
Professor, Civil department Manit, Bhopal and 462052 , India
d,
Research Scholar, Chemical department Manit, Bhopal and 462052 , India
Abstract
Aluminium metal matrix composite is a relatively new material that has proved its position in automobile, aerospace and other
engineering design applications due to its wear resistance and substantial hardness. Need for improved tribological performance
has led to the design and selection of newer variants of the composite. The present investigation deals with the study of dry
sliding wear performance of Al5083-10 wt. % SiC composites fabricated by Ultrasonic assisted stir casting process. Dry sliding
wear tests have been carried out by using Pin-on-Disk wear test rate with normal loads of 10N, 20N, 30N, sliding distance 754 m,
1131 m, 1508 m and sliding velocity 0.42 m/s, 0.63 m/s, 0.84 m/s at constant time 30 minutes. Experiments were conducted
based on the plan of experiments generated through Taguchi‟s technique. A L9 Orthogonal array was selected for analysis of the
output. Investigation to find the influence of applied load, sliding speed and sliding distance on wear rate, during wearing process
was carried out using ANOVA and regression equation were developed for 10% SiC reinforced Al-5083 AMMCs. Objective of
the model was chosen as “smaller the better‟ characteristics to analyse the dry sliding wear resistance. In this research it is
observed that applied load has the highest influence followed by sliding distance and sliding speed. Finally, the experimental
results were validated by the confirmation tests.
© 2014
© 2014Elsevier
The Authors. Published
Ltd. This byaccess
is an open Elsevier Ltd.under the CC BY-NC-ND license
article
Selection and peer-review under responsibility of the Gokaraju Rangaraju Institute of Engineering and Technology (GRIET).
(http://creativecommons.org/licenses/by-nc-nd/3.0/).
Selection and peer review under responsibility of the Gokaraju Rangaraju Institute of Engineering and Technology (GRIET)
Keywords- AMMCs- Metal Matrix Composites, Ultrasonic assisted Stir casting, Taguchi‟s techniques, Analysis of variance, and wear behaviour
1. Introduction
Conventional monolithic materials have limitations in achieving optimum levels of strength, stiffness, density,
toughness and wear resistance. To overcome these shortcomings, discontinuously reinforced aluminium metal
matrix composites (DRAMMCs) are gaining importance due to their high specific strength, high stiffness, low
Corresponding author. Tel: +91-8989096856,

E-mail address:ravindrarana74@gmail.com
2211-8128 © 2014 Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/3.0/).
Selection and peer review under responsibility of the Gokaraju Rangaraju Institute of Engineering and Technology (GRIET)
doi:10.1016/j.mspro.2014.07.064
504 Ravindra Singh Rana et al. / Procedia Materials Science 6 (2014) 503 – 511
density and good wear resistance and they have the potential to replace their monolithic counterparts primarily in
automotive, aerospace and energy applications as reported by Rohatgi, P.K.et al.(1986)and Mahendra, K.V. etl
al.(2007).
Fabrication of MMCs has several challenges like porosity formation, poor wettability and improper distribution of
reinforcement. Achieving uniform distribution of reinforcement is the foremost important work. A new technique of
fabricating cast Aluminium matrix composite has been proposed to improve the wettability between alloy and
reinforcement. The application of ultrasonic vibration on the composite during melting not only refined the grain
microstructure of the matrix, but also improved the mechanical and tribological properties of composites. Wear
performances of particulate reinforced aluminium matrix composites reinforced with SiC and Al2O3 were compared
by Hosking FM et. al.(1982) found that SiC particles was more effective than Al2O3 particles for the improvement
of wear resistance of Al matrix composites due to the high hardness. Lee CS et al.(1992) stated that SiC particles
reinforced composites have better wear resistance than that of Al2O3 reinforced composites. The tribological
parameters that control the friction and wear performance of DRAMMCs like load, sliding velocity, sliding distance,
reinforcement size and reinforcement volume fraction have been reviewed in detail by Sannino and Rack (1995), In
present study dry sliding wear test has been carried out on Al5083-10 wt.% SiC composites by using Pin-on-Disk
wear test rate with normal loads of 10-30N, sliding distance 754 m, 1131 m, 1508 m, 1885 m and sliding velocity
0.42 m/s, 0.63 m/s, 0.84 m/s and 1.04 m/s at constant time 30 minutes to find the influence of applied load, sliding
speed and sliding distance on wear rate, Scanning Electron Microscope were done on wear surfaces.
2. Design Of Experiments (DOE)

Design of Experiment is one of the important and powerful statistical techniques to study the effect of multiple
variables simultaneously and involves a series of steps which must follow a certain sequence for the experiment to
yield an improved understanding of process performance as reported by Taguchi G (1990). All designed
experiments require a certain number of combinations of factors and levels be tested in order to observe the results
of those test conditions. The DOE process is made up of three main phases: the planning phase, the conducting
phase, and the analysis phase. A major step in the DOE process is the determination of the combination of factors
and levels which will provide the desired information reported by Fisher R.A.(1951).Taguchi techniques have been
used widely in engineering design. This method is useful for studying the interactions between the parameters, and
also it is a powerful design of experiments tool, which provides a simple, efficient and systematic approach to
determine optimal process parameters. Compared to the conventional approach of experimentation, this method
reduces drastically the number of experiments that are required to model the response functions.Taguchi has used
Signal–Noise (S/N) ratio as the quality characteristic of choice. The plan of experiments is generated in Taguchi
method by the use of standard orthogonal arrays. The experimental results are then analyzed by using analysis of
mean and analysis of variance (ANOVA) of the influencing factors reported by taguchi G et. al.(1987) and taguchi
G (1993).
3. Experimental procedure
3.1. Materials
AA 5083 Aluminum alloy was used as the matrix material in the present investigation and has the chemical
composition as shown in Table 1. The aluminium alloy was reinforced with 10 wt.% SiC to synthesise the
composite through Ultrasonic assisted stir casting
Ravindra Singh Rana et al. / Procedia Materials Science 6 (2014) 503 – 511 505
Table 1 Composition of AA 5083 Al alloy
Elements Percentage (%)
Zn 0.03
Fe 0.173
Ti 0.04
Cu 0.0181
Si 0.16
Pb 0.0140
Mn 0.526
Mg 5.13
Cr 0.097
Al Balance
SEM analysis of the SiC particles are shown in the fig.1.The SiC particles size was 400 mesh and average
particles size was 35 μm SiC (99% Pure) .
Fig.1: SEM analysis of Micron size SiC particles
3.2. Synthesis of Al-SiC composites

Ultrasonic assisted stir casting was used to synthesise the micron composite. The matrix alloy AA 5083 was first
superheated above its melting temperature 7600C. A vortex was created in the melt due to continuous stirring by a
stainless steel mechanical stirrer with a rotational speed of 450 rpm. At this stage, the preheated (400 0C) 10 wt. %
micron SiC particles were introduced into the melt. Stirring was continued for about 5 minutes until the interface
between the particle and the matrix promoted wetting and the particles were uniformly dispersed. Then the
ultrasonic probe (1200 watt, 21.22 khz frequency and amplitude of vibration 40 micron) was inserted into the melt
for 5 minutes for the uniform distribution of SiC particles in the melt. Composite melt was degassed using Nitrogen
gas.. The melt was then superheated above the liquidus temperature and solidified in a mild steel permanent mould
to obtain cylindrical samples. Sliding wear test specimens were machined from as-cast samples, to obtain cylindrical
pins of diameter 09 mm and length 30 mm. The specimen faces were then metallographically polished.
3.3. Experimental set up and procedure

Dry sliding wear tests has been carried out using a computerized Pin-on-Disc wear testing apparatus (Model: TR20-
LE, Wear and Friction Monitor, Ducom, Bangalore, India) .The dry sliding wear tests were conducted as per ASTM
G99-04 standards. The pin was cleaned with acetone and its initial mass was measured using a digital electronic
balance. In these tests, a cylindrical sample alloy and composites of 09 mm in diameter and 30 mm in length is hold
against a rotating disc made of EN-31 steel and a required normal load was applied through a lever mechanism. The
hardness of disc was 64 HRC and surface roughness was 0.1 microns. The surface of the pins and the disc are
ground using 200 grit emery paper prior to test. Care has been taken that the specimens under test are continuously
cleaned with woollen cloth to avoid the entrapment of wear debris and to achieve uniformly in experiential
procedure. The difference between the initial and final mass of the pin gave the mass loss due to sliding wear. The
volume loss due to wear was calculated by the use of corresponding density values of the pin. The wear rate of the
composite pins was then calculated (ratio of volume loss to sliding distance). After the tests, the worn out surface
(tribosurface) of test specimens were observed by scanning electron microscope (SEM) to study the wear
mechanisms.
Fig. 2 pin-on-disc sliding wear testing apparatus

3.4. Plan of experiments
The experimental plan was formulated considering three parameters (variables) and three levels based on the
Taguchi technique. The levels of these variables chosen for experimentation are given in Table 2.
Table 2: Parameters and their levels
Level Load, L (N) Sliding speed, V (m/s) Sliding distance, S (m)
1 10 0.42 754
2 20 0.63 1131
3 30 0.84 1508
Dry sliding wear test was performed with three parameters: applied load, sliding speed, and sliding distance and
varying them for three levels. According to the rule that degree of freedom for an orthogonal array should be greater
than or equal to sum of those wear parameters reported by Roy K R(1990) and Paulo Davim, J.(2000) a L9
Orthogonal array which has 9 rows and 3 columns was selected as shown below:
Table 3 Orthogonal array L9 of Taguchi
Experiment No. Column 1 Column 2 Column 3
1 1 1 1
2 1 2 2
3 1 3 3
4 2 1 2
5 2 2 3
6 2 3 1
7 3 1 3
8 3 2 1
9 3 3 2
A set of experiments were performed based on the run order generated by the Taguchi model. The response for the
model is wear rate. In Orthogonal array, first column is assigned to applied load (L), second column is assigned to
sliding speed (V) and third column is assigned to sliding distance (S) and the remaining columns are assigned to
their interactions.The response variable to be studied was wear rate. The Signal to Noise (S/N) ratio, which
condenses the multiple data points within a trial, depends on the type of characteristic being evaluated. In this study,
“smaller the better” characteristics were chosen to analyse the dry sliding wear resistance. The S/N ratio for wear
rate “smaller the better” characteristic given by Taguchi, is logarithmic transformation of the loss function, is given
as:
S/N = -10 log [1/n (Σy2)] (1)
Where y is the observed data (wear rate) and n is the number of observations. The above S/N ratio transformation is
suitable for minimization of wear rate. The response table for signal to noise ratios show the average of selected
characteristics for each level of the factor. This table includes the ranks based on the delta statistics, which compares
the relative value of the effects. S/N ratio is a response which consolidates repetitions and the effect of noise levels
into one data point. Analysis of variance of the S/N ratio is performed to identify the statistically significant
parameters.
4. Results and discussion

The aim of this paper is to find the important factors influence on wear process to achieve the minimum wear rate.
4.1 Results for Statistically analysis of wear rate

The experiments were conducted as per orthogonal array and the wear rate; S/N ratio results obtained for various
combinations of parameters are shown in Table 4. The experimental values were transformed into S/N ratios for
measuring the quality characteristics using MINITAB 15.
Table 4: Results of L9 Orthogonal array for AA 5083 / 10% SiC Composites
S.No. L (N) V (m/s) S (m) Wear rate S/N ratio

(mm3/ m) wear rate
1 10 0.42 754 0.00205 53.7649

2 10 0.63 1131 0.00216 53.3109
3 10 0.84 1508 0.00224 52.9950
4 20 0.42 1131 0.00249 52.0760
5 20 0.63 1508 0.00258 51.7676
6 20 0.84 754 0.00240 52.3958
7 30 0.42 1508 0.00349 49.1435
8 30 0.63 754 0.00276 51.1818
9 30 0.84 1131 0.00284 50.9336
The Influence of control process parameters such as load, sliding speed and sliding distance on wear has been
analysed. The ranking of process parameter using signal to noise ratios obtained for different parameter levels for
wear are given in the table 5 and table 6.
Table 5 Responses table for Means wear
Level Load Sliding velocity Sliding distance
1 0.002150 0.002677 0.002403

2 0.002490 0.002500 0.002497
3 0.003030 0.002493 0.002770
Delta(∆) 0.000880 0.000183 0.000367
Rank 1 3 2
Table 6. Responses table for S/N ratio for wear
Level Load Sliding velocity Sliding distance
1 53.36 51.66 52.45

2 52.08 52.09 52.11
3 50.42 52.11 51.30
Delta(∆) 2.94 0.45 1.15
Rank 1 3 2
The control factors are statistically significant in the signal to noise ratio and it is observed that applied load is the
dominant parameter on the wear rate followed by sliding distance and sliding speed.
The main effect plot for mean, S/N ratio for the wear and interaction effects plots between the process parameters
are also shown in the Fig. 3(a), 3(b) and Fig. 4.The significance of each parameter is determined from the inclination
of the mail effects plot. A parameter for which the line has the higher inclination will have the most significant. It is
very much clear from the main effect plot for wear from Fig. 3(a) and main effect plot for S/N ratio from Fig. 3(b)
that parameter L (applied load) is most significant parameter while parameter S (sliding distance) also has some
significant effect. To study an interaction plot means to determine the nonparallelism of parameter effects. If the
lines of an interaction plot are not parallel, it suggests that there is nominal interaction occurred and if the lines
interact each other, then strong interaction occurred between the parameters. Fig. 4 shows that there is strong
interaction between the parameter load (L) and sliding distance (S) while there is moderate interaction between the
parameters L and V and between V and S. Thus from the present analysis, it is clear that the applied load (L) is most
influencing parameter for wear characteristic of Al-10% SiCp composites.
Main Effects Plot (data means) for SN ratios

Load Speed
53
52
Mean of SN ratios 51
50
10 20 30 0.42 0.63 0.84
Distance
53
52
51
a b
50
754 1131 1508
Fig.3 Main effects for plot for (a) Means Wear Rate (b) S/N Ratio –Wear Rate
Interaction Plot (data means) for W

0.42 0.63 0.84
0.0036
L
10
0.0030 20
L 30
0.0024
0.0036
V
0.42
0.0030 0.63
V 0.84
0.0024
0.0036
S
754
0.0030 1131
S 1508
0.0024
10 20 30 754 1131 1508
Fig. 4: Interaction effect of process parameters on wear rate

4.2 Analysis of variance for wear rate

The experimental results were analysed by analysis of variance (ANOVA) which is used to investigate the influence
the wear parameters like applied load, sliding distance and sliding speed. By performing the analysis of variance, it
can be decided which factor dominate over the other and the percentage contribution of that particular independent
variable. Table 7 shows the analysis of variance results for the wear rate for three factors varied at three levels and
interactions of those factors. This analysis were carried out for the confidence level 95%.Sources with a P value less
than 0.05 were considered to have a statistically significant contribution to the performance measures.
Table 7: Analysis of Variance for S/N ratios
Source DF Seq SS Adj SS AdjMS F P
Load 2 13.0151 13.0151 6.5075 25.33 0.038
Speed 2 0.3809 0.3809 0.1904 0.74 0.574
Distance 2 2.0758 2.0758 1.03379 4.04 0.198
Residual 2 0.5138 0.5138 0.2569

Error
Total 8 15.9856
It can be observed that for aluminium 10% SiC Metal Matrix Composites, from the Table 7, that the sliding distance
has the highest influence on wear rate. Hence sliding load is an important control factor to be taken into
consideration during wear process followed by sliding distance & sliding speed respectively. The interaction terms
has little or no effect on wear rat. It is inferred that the applied load has the highest contribution on wear rate
followed by sliding distance & sliding speed.
5. Multiple linear regression model
A multiple linear regression model is developed using statistical software “MINITAB 15”. This model gives the
relationship between an independent / predicted variable & a response variable by fitting a linear equation to
observe data. Regression equation thus generated establishes correlation between the significant terms obtained from
ANOVA analysis namely applied load, sliding speed & sliding distance.
The regression equation developed for Al / (10%) SiC MMCs wear rate is as follows
Wear Rate (mm3/ m) = 0.00140 + 0.000012 S (m) - 0.000437 V (m/s) + 0.000044 L (N) (2)
From Esq. (1), it is observed that applied load play a major role on wear rate and it is highly influenced by load
followed by sliding distance.
VII. CONFIRMATION TEST

A confirmation test is the final step in design of experiment process. Dry sliding test were conducted using specific
set of parameters to validate the statistical analysis. After getting the optimum label of process parameter it is
necessary to carried out the verification test to evaluate the accuracy of tests and to validate the experimental results.
Table 8: Confirmation test for wear rate
Experiments Load (N) Sliding distance(m/s) Sliding speed (m)
1 15 800 0.45
2 25 1300 0.73
Table 9: Result of confirmation test and comparison with regression result
S. No. Experiment wear rate Predicted Wear rate % error

(mm3/m) (mm3/m)
1 0.011932 0.011464 3.9
2 0.018906 0.017781 5.8
6. Conclusions
Following are the conclusions drawn from the study on dry sliding wear test using Taguchi technique.
1. Applied load has the highest influence on wear rate followed by sliding distance and sliding speed for Al-
5083/10% SiC composites.
2. Regression equation generated for the 10% SiC metal matrix composites is used to predict the wear rate of
above composite for intermediate condition with reasonable accuracy.
3. Confirmation experiment was carried out and made comparison between experimental values showing an
error associated with dry sliding wear are 3.9 % and 5.8 %. Thus design of experiments by taguchi method
was successfully used to predict the tribological behaviour of composites.
References
Aluminum Composites: Review and Discussion, Wear, 189, pp. 1-19.
Fisher R. A. 1951. Design of Experiments, Oliver & Boyd, Edinburgh, UK
Hosking FM, Folgar Portillo F, Wonderlin R, Mehrabian R. 1982.Composite of aluminium alloys: fabrication and wear behaviour. Journal
Material Science, 17 pp.477–98
Lee CS, Kim YH, Han KS, Lim T. 1992.Wear behaviour of aluminium matrix composite materials. Journal Material Science, 27, pp793–800.
Mahendra, K.V. and Radhakrishna, K., 2007, “Castable Composites and their Application in Automobiles”, Proceedings of the Institution of
Mechanical Engineers, Part D: Journal of Automobile Engineering, 221, pp. 135-140.
Paulo Davim, J. 2000. An experimental study of Tribological Behaviour of the Brass/Steel pair, Journal of Materials Processing Technology, 100,
pp. 273-277.
Rohatgi, P.K., Asthana, R. and Das, S., 1986, Solidification, Structures, and Properties of Cast Metal-Ceramic Particle Composites, International
Metals Reviews, 31, pp. 115-139.
Roy, K. R., 1990.A Primer on the Taguchi method, Van Nostrand Reinhold, New York, NY.
Sannino, A.P. and Rack, H.J. 1995. Dry Sliding Wear of Discontinuously Reinforced
Taguchi G. 1990. Introduction to quality engineering, Asian productivity organization.
Taguchi, G., Konishi, S., 1987, Taguchi Methods Orthogonal Arrays and Linear Graphs: Tools for Quality Engineering, American Supplier
Institute, Dearborn.
Taguchi, G. 1993. Taguchi on Robust Technology Development: Bringing Quality Engineering Upstream, ASME press, New York, NY.

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Diseño y Analisis de Experimentos - UNT 2015 2

El DOE, por lo general, se desarrolla en 4 fases: Planificación, screening,

Diseño y Analisis de Experimentos - UNT 2015 3

Diseño y Analisis de Experimentos - UNT 2015 4

Diseño y Analisis de Experimentos - UNT 2015 5

Diseño y Analisis de Experimentos - UNT 2015 6

Diseño y Analisis de Experimentos - UNT 2015 7

Diseño y Analisis de Experimentos - UNT 2015 8

Diseño y Analisis de Experimentos - UNT 2015 9

Para (1-α) de 5%, el valor crítico de Z =

• En DOE, el valor-p se utiliza para determinar si los resultados son

Diseño y Analisis de Experimentos - UNT 2015 10

Diseño y Analisis de Experimentos - UNT 2015 11

Diseño de 2 factores Diseño de 3 factores

Cuales son la variables con mayor influencia en la respuesta?

Problema: El número de corridas crece exponencialmente al aumentar los factores

Diseño y Analisis de Experimentos - UNT 2015 13

Contiene 2k-p corridas y se conoce

Diseño y Analisis de Experimentos - UNT 2015 14

Diseño y Analisis de Experimentos - UNT 2015 15

Diseño y Analisis de Experimentos - UNT 2015 16

 Resolución III: Design Generators: E = ABCD

 Los efectos principales forman Defining Relation: I = ABCDE

estructuras de alias con las Alias Structure

interacciones de 3 factores E + ABCD

Las interacciones de 2 factores

interacciones de 3 factores y los AE + BCD

Diseño y Analisis de Experimentos - UNT 2015 17

Ejemplo: Modelo para tres factores y dos niveles

Y = β0+ β1X1+β2X2+ β3X3+β12X1X2 + β13X1X3+ β23X2X3 + β123X1X2X3+ ε

Diseño y Analisis de Experimentos - UNT 2015 18

Diseño y Analisis de Experimentos - UNT 2015 19

Source DF Adj SS Adj MS F-Value P-Value

Diseño y Analisis de Experimentos - UNT 2015 20

Diseño y Analisis de Experimentos - UNT 2015 21

Diseño y Analisis de Experimentos - UNT 2015 23

CCC: Circumscribed; CCF: Faced centered; CCI: Inscribed

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Pregunta: ¿ que tipo de base y nivel presión de spray maximiza la adhesión?

Diseño Factorial completo: 2 factores; 2 niveles; 4 réplicas

Ingrese los siguientes mediciones (respuestas) a la filas 1-16 de C7 (Adhesion)

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Los Ingenieros sospechan la existencia de interacciones AxB y AxD;

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Fractional Factorial Design

Factors: 4 Base Design: 4, 8 Resolution: IV

Design Generators: D = ABC

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 El mineral es refractario y se necesita molienda ultra-fina para extraer

 Resultados sugieren que la velocidad de agitación y ratio bolas/carga son

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Y = 6.52 +1.28x1 -4.27x2 -1.52 x3 -1.07(x1) 2 +

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 Material structural  Propiedades: livianos y alta dureza

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where n and cp are the number of parameters and MGM (1 H ) nt

Ball diameter/mm a X1 x1 2 3.5 4.5 I gm v Dm2 ( U m U ) gh (7)