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Trabajo Microdureza
Trabajo Microdureza
MICRODUREZA
1. RESUMEN:
A travs del tiempo, la ciencia ha visto la necesidad de medir y clasificar las propiedades
mecnicas de diferentes tipos de materiales, principalmente su dureza y mdulo elstico, a travs
de ensayos estticos los cuales se realizan por medio de distintos mtodos los cuales son: Brinell,
vickers y knoop, o dependiendo de su medida de profundidad de identacin por medio del ensayo
Rockwell. Esto ha favorecido el desarrollo de instrumentos de nanoidentacion o microdureza
capaces de clasificar las propiedades mecnicas de las superficies de capas finas, cables
microscpicos o materiales masivos. Los parmetros ms habituales de medir son: la dureza
(deformacin plstica) y el modulo elstico (mdulo de Young). Dichos parmetros son medidos a
travs de ensayos, los cuales se realizan rigindose por las normas ASTM.
Es posible trabajar con muestras diminutas y extremadamente delgadas, a su vez se realizan
medidas aplicando cargas muy pequeas al material de estudio (esta tcnica no es destructiva).
Tiene aplicaciones en el campo de los metales, cristales inicos, cermicas y recientemente en
polmeros.
2. INTRODUCCION:
3. MICRODUREZA:
Figura1: microdureza
hallar
4. METODOS
(
4.1 Brinell:
P = carga utilizada.
D = dimetro (mm).
d = dimetro de la huella (mm).
El esclermetro o durmetro (figura3) es una
maquina la cual sirve para la medicin de la
dureza de Brinell este aparato posee un
microscopio integrado de 0,001 mm y la rige
la norma ASTM E10.
4.1.1TIPO DE PROBETAS:
Segn el ASTM E 10 las probetas deben tener
un espesor 10 veces ms que la profundidad
de identacin. Adems la superficie debe ser
lijada y pulida de manera que se observen
con claridad los bordes de la huella en el
momento de la medicin con la precisin
necesaria.
4.2 VICKERS:
Es una prueba de dureza por penetracin
con el fin de obtener la dureza Vickers de la
superficie de un material.
El mtodo consiste en presionar contra la
probeta un indentador piramidal (figura 4)
de diamante con ngulo entre sus caras de
= 136. La pirmide o identador se mantiene
algn tiempo bajo la carga P. Luego de
retirada la carga se miden las dos diagonales
de la impronta dejada, con ayuda de un
microscopio. El valor medio de las diagonales
(d) y el valor de la carga se sustituyen en la
frmula de trabajo para obtener el valor de
la dureza Vickers. En las mismas condiciones
se realizan varias indentaciones ms con el
fin de tener un promedio y obtener
mediciones mucho ms exactas.
4.1.2TIPO DE IDENTADORES:
La bola debe tener 10mm de dimetro con
una desviacin no mayor a 0,005mm, y las
bolas ms pequeas tienen diferente
tolerancia como se muestra en la tabla.1.
4.3 KNOOP:
Este mtodo es similar a los anteriores
ensayos nombrados ya que consiste en
presionar un identador con una punta de
diamante y una base en forma de rombo, sus
diagonales guardan una relacin 7:1 y la
profundidad es de solo 1/30 de la diagonal
mayor (figura 5); sobre la superficie pulida
del material a ensayar con una fuerza
conocida, durante un tiempo de empuje
determinado. Las diagonales de la huella
resultante se miden usando un microscopio.
Ecuacin 5:
recuperada.
base
de
impresin
no
P = carga aplicada.
L = longitud de la diagonal mayor en mm.
La longitud de la diagonal l puede variar de 5
a 1000 segn la carga y la dureza del
material.
4.4 ROCKWELL:
Es el mtodo de dureza ms usado para
medir la dureza de un material, puesto que
no se necesita tener conocimientos
especiales.
La prueba consiste en penetrar en dos
tiempos las capas superficial del material y
medir la huella dejada por el identador,
inmediatamente en la pantalla del
durmetro nos aparecer el valor de la
dureza.
Ecuacin 7:
diamante.
Para
identador
cono
de
5 Aplicaciones:
Segn el ASTM 14-74 las aplicaciones en el
campo de la microdureza
Comparacin De Materiales Al medir la
dureza de diferentes materiales usamos
diferentes escalas de dureza, la ms
Materiales
muy
frgiles
o
quebradizos (indentador de Knoop), como
silicio, germanio, vidrio, esmalte de dientes.
Materiales
translcidos.
opacos,
Superficies plateadas.
Metales en polvo.
Para
investigar
individuales de un material.
claros
constituyentes
Referencias
http://www.utp.edu.co/~gcalle/DUREZABRIN
ELL.pdf
http://www.cyti.com.mx/dureza_microdurez
a.asp
http://www.kansert.es/Shore.swf
https://www.youtube.com/watch?v=ZEeIcJQ
pero
http://www3.ucn.cl/FacultadesInstitutos/lab
oratorio/durezam4.htm
http://www2.ictp.csic.es/qf/ppcontrol/biblio
grafia/D22-MH-2011.pdf
Knoop,
ANNALSofFacultyEngineeringHunedoara
InternationalJournalofEngineering
TomeXII[2014]Fascicule3[August]
ISSN:15842673[CDRom,online]
afreeaccessmultidisciplinarypublication
oftheFacultyofEngineeringHunedoara
JozefPETRK,2.PeterBELLA,3.AnnaGUZANOV,4.IvetaSINAIOV
1.
THEAUTOMATICTESTERSINMICROHARDNESS
MEASUREMENTANDISEEFFECT
TechnicalUniversityofKoice,FacultyofMetallurgy,Koice,SLOVAKIA
TechnicalUniversityofKoice,FacultyofMechanicalEngineering,Koice,SLOVAKIA
4.InstituteofMaterialResearch,SlovakAcademyofSciences,Koice,SLOVAKIA
12.
3.
Abstract: The measurement of microhardness with applied loads 0.09807 N, 0.24518 N, 0.49035 N and
0.9807Nhasbeencarriedoutbyfiveautomaticmicrohardnesstesters.Eachappraiserobtainedreadingsof
the tester which she/he normally operates.The influence of applied load and equipment on the measured
valueofmicrohardnessandthenatureandthesizeofISEphenomenonwasevaluatedbyMeyersindexn.
Thedifferencebetweenvaluesobtainedbyparticulartestersisstatisticallysignificant.
Keywords:Automatictester,microhardnesstest,microindentation,CRM
1.INTRODUCTION
Measurement of microhardness can be carried out in a similar manner to the Vickers macro
indentation tests with diamond pyramid. However, the most important and intractable
problemassociated with low loads (the deep of indentation is less than 10 m as a rule) is that
concerned with change in indentation size [1, 2]. The microhardness of solids depends on the
appliedload.Thestudyofrelationshipbetweenmicrohardnessandloadhasbeencarriedoutnot
only for metallic materials, but also forsemiconductors, glass, slag, ceramics and organic crystals
[38].Thedependenceofmeasuredvaluesof themicrohardnessofsolidsontheappliedloadis
knownastheindentationsizeeffect(ISE).Itincreasestheuncertaintyofthemeasurementresult
andmayresultinunreliableconclusions,particularlyiflowloads(lessthan0.294or0.392Nasa
rule)areused.Lowloadisrequiredwhenmeasuringthehardnessofsmallsamples,coatings,thin
layers or phases in metallography [9]. When low load is used, the measured microhardness is
usually high; with an increase in test load it decreases. Such a phenomenon is referred to as
normalISE.Itmaybecausedbythetestingequipment[10,11]orbyintrinsicstructuralfactors
of the material: work hardening during indentation, load to initiate plastic deformation, elastic
resistance and mixed elastic/plastic deformation response of material [9, 10, 12], the effect of
indenter/specimen friction resistance, the effect of machininginduced residually stressed
measured surface [10, 913]. In the literature, there are many examples, which reveal that the
normalISEoccursinbrittlematerialsincludingglass[10].IncontrasttonormalISE,areverse
(inverse) ISE (RISE), where the apparent microhardness increases with increasing load, is also
known. The reverse ISE essentially takes place in materials in which plastic deformation is
predominant.Thepurposeofthispaperistoevaluatetheinfluenceoftheloadandequipmenton
thevaluesofmicrohardness,usingMeyersandPSRmethods.
2.EXPERIMENTALMATERIALSANDPROCEDURES
Fivetypes of automatic microhardness testers (marked as AE) were used as equipments. The
hardnessreferenceblock(certifiedreferencematerialCRM)forindirectcalibrationwithspecified
copyrightFacultyofEngineeringHunedoara,UniversityPOLITEHNICATimisoara
239 | Fascicule 3
m icrohardness HV
hardnessHc=195HV0.05andstandarduncertaintyuCRM=4.0HV0.05wasthesample.Theapplied
loadsPwere0.09807N,0.24518N,0.49035Nand0.9807N.Eachappraiserobtainedreadingsofthe
tester which she/he normally operates. An appraiser performed five indentations (trials) at each
load. The result was the file of 20 indentations. The load duration time was 15 seconds, and the
ambient temperature was in accord with thestandard [14, 15]. Average values of particular files
(HV)areintab.1(HV).ThestatisticaloutliersweredetectedbyGrubbstest(significancelevel=
0.05). Their presence would testify that the process is out of statistical control. No outlier was
found.Absenceofoutlierssuggeststhatthemeasurementprocesshasavoidedthegrosserrors.
The normality (determined by Freeware Process
260
240
CapabilityCalculatorsoftware(AndersonDarling
220
A
test,p 0.05fornormaldistribution)wasconfirmed
200
B
forallfiles,table1.Thevaluesofthemicrohardness
C
180
D
160
obtained at the load 0.49035 N was used for the
E
140
calibrationofthetesterinaccordwiththestandard
120
[14].
100
0
0,2
0,4
0,6
0,8
1
1,2
Average values of microhardness, measured at
load P (N)
isgivenbyKicksLaw.However,n<2indicated
Figure2.Theboxplot,resultsofparticulartesters
normal ISE behavior, and the measured
microhardness decreases with applied load. When n >2, there is the reverse ISE behavior,
measuredmicrohardnessincreaseswithincreasingoftheload.
3.2PSR(ProportionalSpecimenResistancemodel)andmodifiedPSR
Severalauthors[9,11]haveproposedthatISEbehaviormaybedescribedbytheEq.(2):
P=c1d+c2d2(2)
Gong et al. [9, 11] used an energy balance approach to examine the ISE and rearranged Eq. (2)
intomodifiedformofthePSR:
P=c0+c1d+c2d2(3)
Thevaluesofconstantsc0 (N),c1(Nmm1)andc2 (Nmm2)ofEq.(3),obtainedfromthequadratic
polynomial regressions of P/d (N mm1)against d (mm) are given in tab. 2. The parameter
c1characterisestheloaddependenceofmicrohardness(elasticproperties).Itconsistsoftheelastic
resistanceofthetestspecimenandthefrictionresistancedevelopedattheindenterfacet/specimen
interface [16]. The parameter c2 is the measure of the loadindependent microhardness (plastic
properties).Theratioc1/c2 maybetreatedapproximatelyasameasureoftheresidualstressdueto
machiningandpolishing[11,17].
240 | Fascicule 3
3.3HaysKendallapproach
HaysandKendallproposedthatthereexistsaminimumloadW(N)necessarillytoinitiateplastic
deformation and below which only elastic deformation occurs. Then the load dependence of
hardnessisexpressedbyEq.(4),whereA1(Nmm2)isaconstantindependentofload.
P=W+A1d2(4)
The values of W and A1 may be obtained from the regressions of P (N)against d2 (mm)[10] and
theirmeasuredvaluesaregivenintab.2.Theloadtoinitiateplasticdeformation(tocreatevisible
indentation)variesintherange0.0140.062N.TheconstantA1canbeusedforcalculationoftrue
hardness;HPSRA1=0.1891A1.
Table1.Theaveragemicrohardnessvalueofparticularfiles(HV),thenormality(pvalue),micro
hardnessHV0.05,relativerepeatabilityrrel(%),maximalrelativeerrorErel(%)andrelativeexpanded
uncertaintyofcalibrationUrel(%)oftheresultsobtainedbyparticulartesters.
tester
HV
normality HV0.05
rrel
Erel
Urel
A
192
0.4297
195
4.1 0.1
5.6
B
219
0.5950
215
1.8 10.0 14.5
C
172
0.6311
188
4.7 3.5
9.9
D
178
0.4107
189
7.0 1.1
8.8
E
176
0.0700
176
2.2 4.4
9.1
Table2.ThevaluesofMeyersindexnandindicesAln,c0,c1,c2,W,A1andtruehardnessHPSRA1.
tester
n
Aln
c0
c1
c2
c1/c2
W
A1 HPSRA1
A
2.0280 7.0326 0.041 4.91 892 0.0055 0.004 1007 190
B
1.8439 6.4091 0.002 2.21 999 0.0022 0.019 1054 199
C
2.1275 7.4092 0.040 6.91 1241 0.0056 0.023 1076 203
D
2.0888 7.2608 0.003 1.79 1095 0.0016 0.014 1052 199
E
2.2596 7.7786 0.067 13.17 1365 0.0097 0.062 1064 201
4.TOTALDISPERSIONZONE
ThevalueoftheTotalDispersionZoneSMcalculatedforaparticularloadevaluatestheabilityofthe
testers achieve the same values of the microhardness. It is necessary to calculate the average
valuesHVA,HVBHVEandtocalculatetheirstandarddeviationss A,s Bs Eof5trialsofparticular
testeratparticularload[18].TotalscatterzoneSMwillbecalculatedbyEq.(5)and(6)asarelative
value:
15,5
SM
15
.100 (5)(6)
T
14,5
s
2
14
S M%
S M = 6 s + s v 2 S M % =
13,5
13
12,5
12
11,5
0,098
0,245
0,49
load P (N)
(8)
0,98
Figure3.TheValuesSM%
svisastandarddeviationof5averagevaluesHVA,HVB...,HVEmeasuredunderthesameload.
The sign tolerance T = 39 HV in Eq. (6), the same for all test loads,was calculated pursuant to
maximal permissible error (10 % of 195 HV 0.05) according to standard[14]. We regard SM % as
follows:0to20%good,21to30%limitedusableandmorethan30%unacceptable.Ascanbe
seeninFig.3,thevaluesofSM%aregoodforallfourappliedloads.Thedifferencesbetweenthe
resultsofhardnessobtainedbyparticulartesterarenotsignificantunderthismethod.Thisfactis
notingoodaccordwiththeresultsofANOVA.ItseemsthatthemethodofTotalDispersionZone
isnotsensitiveenoughforthistypeofmeasurement.
5.DISCUSION
The influence of the appraiser on the result is marginal with respect to automatic function of
testers. High variability of the measured values was observed despite the same sample and
automatic measurement system. The sample was standard hardness block with expected high
241 | Fascicule 3
homogeneityofmicrohardnessandwithuniformresidualstressduetomachiningandpolishing
of its surface. Both equipments and test loads have statistically significant effect on the micro
hardness.TheresultisthatthesamesampleshowssimultaneouslynormalandreverseISE.In
the literature, there are many examples, which reveal that the normal ISE occurs in brittle
materials as nonmetals, semiconductors or glass. Just normal ISE was detected by the tester
withamaximalerrorErelandmaximaluncertaintyUrel(thetesterB).
Asitwasusedthesamesample,theISEobviouslymaybecausedbythetestingequipment.The
experimental errors resulting from the measurement of indentation diagonals as a result of the
limitations of the resolution of the objective lens, inadequate measurement capability of small
areasofindentationsanddeterminationoftheappliedloadaretypicalcausesofnormalISE[10,
11,12].Asforthetester,reverseISEcanbeexplainedbyeffectsofvibrationandindenterbluntness
at low loads [9].Vickers method allows calibration in relatively broad interval of temperatures
(23C5C)[14].Inthisinterval,thetemperaturewasfoundtoinfluencethevalueoftheindexn
[19]. A variability of the nature (normal and reverse) of ISE were observed on the same block
measuredmanuallybyHanemanntester.Thevalueofnvariedbetween1.874and2.360[19].High
variability of n was observed also in repeated measurements of more hard (up to 392 HV0.05)
referenceblocks,forexample[20].
6.CONCLUSIONS
The variability of measured values of the microhardness values and parameters ISE is high
despite the use of automatic hardness testers with practically excluding the impact of the
researcher. The influence of the type of the tester is statistically significant. The results of testers
withhighuncertaintyshowextremevaluesofMeyersindex.
ACKNOWLEDGEMENTS
ThisworkwassupportedbytheSlovakGrantAgencyforScienceVEGA1/0173/14.
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