Está en la página 1de 18

WANDER L.

VASCONCELOS

IIM Review No. 9

Characterization of microstructures
A. M, Gokhalc

ABSTRACT
Various stereological techniques for characterization of microstructures are presented.
The
methods for
the
estimation of
volume fraction, surface area, total curvature, length of lineal features,
and topological properties are described.
Emphasis is
placed on the underlying assumptions, limitations and applicability of the stereological equations.
Important derived properties are
described and their limitations and utility are discussed.
Techniques for the estimation of particle size distributions are presented.

INTRODUCTION

A microstructure is an arrangement of points, lines,


surfaces and volumes.
Thus, it can be characterized by
estimating some important geometrical properties of these
four basic, features,
Proper characterization of microstructures is of central importance in any microstructureproperty correlation study.
If the quantitative characterization of microstructures is not rigorous enough, then
significant differences in the physical properties may
result from the apparently subtle differences in
the
microstructures. It must be mentioned that any naturally
evolved microstructure has infinite geometrical properties
.and it is impossible to measure or mention all of them.
However, fortunately enough, most of the mechanical
and physical properties are sensitive to only those microstructural parameters which have a rigorous geometrical
and physical meaning, and can be estimated by stereological techniques.
The science of quantitative characterization of microstructures is called
"Quantitative
Microscopy" or
"Stereology". Direct observation of a three dimensional
microstructure is extremely difficult. An image of a
flat specimen surface observed in a reflection type optical
microscope is actually a two dimentional section through
the three dimensional microstructure contained in the
sample. An image observed by transmission microscopy
is the projection of the three dimensional microstructure.
It follows that, in order to estimate the geometrical
properties of three dimensional microstructures, it is
essential to develop proper relationships between the
geometrical properties of microstructures and some
appropriate measurements made on two dimensional

sections or projected images. In some cases this has


been successfully done by applying the principles of
geometrical probabilities ' . li is desired that the relationship between the quantity measured on two dimensional section or projected image and the corresponding
property of the three dimensional microstructure satisfy
the following requirements :
1

(1)

It must be
distribution.

(2)

T h e measured quantity must be an unbiased


estimator of the corresponding geometrical property of microstructure.

valid

for

any

shape

and

size

The geometrical properties


of microstructures,
for
which the relationships satisfying the above requirements
have been foun '., arc called the " g l o b a l " properties. The
global geometrical properties can be divided into two
categories, namely, metric and topological. The metric
geometrical properties can be unambiguously estimated
from the measurements made on a two dimensional section,
whereas the topological properties cannot be
estimated from such measurements. Estimation of t o p o logical properties require the measurements on a projected image or serial sectioning of the structure. There
are some geometrical properties of microstructures which
can be estimated from combinations of two or more
global properties.
These are called
the
"derived"
geometrical properties. However, it must be mentioned
that the derived proper!ics are sensitive to s h a p e . This
limitation of the derived properties is many times overlooked and it has led to sciious errors in the interpretation of stereological data.

The author, formerly of Department of Metallurgical Engineering. Indian Inaiilute of Technology,


Research a n d Development Center, -Hindustan Brown Boveri Ltd., Baroda.
Original manuscript received at 11. O. on 30. 8. 19S0.

Kanpur,

is

now

with the

Transactions of T h e Indian Institute of Metals, Vol. 34, N o . i, February 19S1

71

72 Ochtstle : Charaetizaiion of microslructures


Particle size distributions give detailed information
about the geometrical state of simple microstructures.
Precise information regarding the evolution process can
be obtained if the particle size distribution is measured
at different times duiing its evolution. However, the
techniques for estimation of size distributions make
restrictive assumptions regarding the particle shape and
fairly complex calculations are needed for estimating
particle size distributions.
The next section of this paper deals with the estimation of metric properties. The subsequent sections
deal with the topological properties, derived properties
and size distributions.

"
2

METRIC

PROPERTIES

Area of the microstrcturai f i e l d = L


Each three, two and one dimensional feature in a
microstructure
has associated with it, a "numerical
extent" which can be unambiguously estimated from
the measurements made on a two dimensional section.
The volume fraction of each phase, surface area per
unit volume of each type of internal surface and length
per unit volume of each type of lineal feature can be
estimated. In addition to their surface area per unit
volume, it is also possible to estimate the total
curvature per unit volume of each type of interface
present in the structure. Let us first consider the
techniques for estimation of the numerical extents of the
"various features.

Area occupied by p Phase = S As


i-1

Aj is i\\e area of i P loop


A s S Aj I ; A is the expected
GjA '"
V = A
t h

fl

value

Fig. 1

fl

Estimation of volume fraction by areal


analysis.

12

Rosiwal showed that if a test line is


the three dimensional microstructure or on
of polish, then the average value of the
the test line length, Lj,, contained in a
phase is equal to its volume fraction ( s e e
T h u s , one can write,

placed in
the plane
fraction of
particular
Figure 2 ).

V L*

A. Volume fraction

...2

In 1848 Delesse showed that the average value or


the expected value of the area fraction A of a phase
in the plane of polish ( i.e., two dimensional section )
is equal to its volume fraction V in the microstructure
( see Figure 1 ).
A

V =A~
T

... 1

The volume fraction analysis performed by measuring


the length fraction is called "lineal analysis." Equation
(2) can be derived in several different w a y s . A
derivation of this equation is also given by Milliard
and U n d e r w o o d . It is not necessary to randomize
the test line with respect to its angular orientation.
The relationship is statistically exact and it is valid
for any shape and size. However, L must be measured
on the representative microsections. The lineal analysis
is more convenient than area fraction measurement if
the interparticle distance is large. Semi-automatic and
automatic devices are available for measuring lineal
fraction.
6 - 8

10

The above
equation has been re-derived by several
other
research workers . It is not necessary to
randomize the sectioning plane with respect to the
spatial
orientation for the estimation
of volume
fraction .
The above equation is valid for any particle
shape and size distribution and it is statistically exact.
However, the area fraction must be measured ou a
T h e volume fraction can also be estimated by
representative two dimensional section. The statistical " p o i n t counting" method. This simple technique was
error involved in the estimation of volume fraction developed by T h o m s o n and Glagolev . If a number
can be kept as small as desired by increasing the -.of test points are placed at r a n d o m on a plane of
n u m b e r of observations.
polish or in the three dimensional microstructure, then
L

11

18

14

15

Transactions of The Indian Institute of Metals, Vol. 34, No. 1, Febru, ry 19S1

10

Gokhel:

Characterization oj"microsmiptvrcs

where

.73

' .

t a foil thickness
S = surface area of the phase of interest per unit
volume Equation (4) is applicable u n d e r t h e following
v

conditions :

T.L. T e s t

(2)

Foil thickness must be less t h a n the


particle, size.
v

must be k n o w n to

estimate the

fraction is mainly determined by the surface area


of phase of interest per unit volume.
The estimation

of S and t

average

volume fraction from the projected


area fraction. If
the foil thickness is large, then the projected area

Total length of the t e s t


lines =31 ; Test line l e n g t h
contained in P P h a s e = S L ^
L =SLf/3L I L i s a n average
value' of L ; V = L
Fig. 2

All t h e particles must be convex.

T h e values

line

(1)

of volume

fraction, from a

projected

image

obtained

from a thick
distribution .

An example of lineal analysis.

the average value of the fraction of test points P


contained in a particular phase is equal to its volume
fraction ( see Figure 3 ).
P

V =P
v

slice,

requires estimation of particle size

40

... 3

E q u a t i o n (3) is valid for a n o n - r a n d o m array of test


points ( e.g., intersections of a s q u a r e lattice ) provided
the grid is placed at r a n d o m . If a grid of test points
is used in point counting then it is called "Systematic
P o i n t C o u n t i n g . " The point counting is a very convenient method for estimating the volume fraction of
finely dispersed particles. In general, systematic point
counting involves less effort than area! analysis or lineal
analysis for a given a c c u r a c y . T h e point counting can
be performed by using cross hairs in the m i c r o s c o p e *
or by inserting a grid in the eye piece of a m i c r o s c o p e , .
It can also be p e r f o r m e d - b y superimposing a grid on a
p h o t o m i c r o g r a p h . Automatic and mechanical divices
are available for performing point c o u n t i n g . .

It is m o r e convenient to estimate the volume fraction


from the measurements m a d e on a two dimensional
section. If the volume fraction is t o o small or the
particle size is very fine, then scanning electron microscopy may be used to get high magnification. F o r the
specimens with flat surfaces, the average values of the
area fraction, lineal fraction and point fraction estimated from S E M images are equal to the true volume
fraction .
However, in most of the cases, it is necessary
to m a k e some correction for the fore-shortening of the
S E M image when the specimen is tilted with respect
to the optical axis.
27

8,17

13

18,19

20

21

22

0
"

23

Let us consider the technique for estimating volume fraction from the measurements m a d e on a projected image.
The projected area fraction is usually larger than the
area fraction observed in a two dimensional section. This
difference between the projected and true areal fraction is
called " H o l m e s effect" . Calm and N u t t i n g have given
the following relation between volume fraction and the
average value of the projected area fraction, ^ A Jproj-"
21

25

\ y
7

ft

0
Test Points are the i n t e r s e c t i o n
Points of the g r i d . T o t a l number
of test Points = 9 ; number of test
Poits in ? Phase = 3 .". P = 0 33
P is an average value of P
P

S -t
v

(A )pr jA

'

Fig. 3

Point counting procedura for the estimation of volume fraction,

Transections of The Indian Institute of Metals, Vol. 34, No I, February 19SI

OoUuik -. Characterization of mkrostructun

74

89

Billiard -* and Calm and Hilliard have analyzed


the errors involved in the various methods for estimation
of volume fraction. Their conclusions are as follows :
(1)

(2)

The statistical error is basically determined by


the number of observations. The n a t u r e of
observation ( e . g., area fraction measurement,
point counting, etc. ) is of secondary importance.
The observations should be spread out at a lowdensity over many fields of view. High sampling densities are inefficient due to resulting
redundancy in the d a t a .

of this test line With the traces of a particular type


of interface in the plane of polish per unit length of
test line. Suppose the experiment - is. repeated with the
various orientations of the test line and the various
orientations of the plane of polish.
Let Rx, be the
average value of N obtained from all these experiments.
It can be shown that the surface area per unit volume S
of a given type of interface is related to the corresponding
value of Nx, by the following equation :
L

S = 2N
v

Figure 4 demonstrates an application of this result. This


equation was derived independently by Saltykov , Smith
a n d G u t t m a n and Duffin, Meussner and R h i n c s " . The
above equation has been re-derived by several other
research w o r k e r s . . It is a statistically exact equation
and it is valid for surface elements of any arbitrary
curvature. The test line need not be a straight line.
H i l l i a r d suggests that it is advantageous to use a circular
test line so that the averaging is automatically done over
all the orientations in the plane of polish. It is necessary
to randomize the test line with respect to its spatial orientation in order to estimate S . However, if the microstructure is isotropic ( i. e., no preferred orientation ) a n d
homogeneous ( i. e., no segregation ) then it is not
necessary to randomize the test line.
6

(3)

(4)

The choice of a technique should be based on


the a m o u n t of effort necessary to get the
required accuracy. This is because the statistical error can be kept as small as desired by
increasing the n u m b e r of observations, and
this is true for all the three techniques ( i.e..
areal analysis, lineal analysis and point counting ).
Equally spaced traverses give an appreciably
lower variance than the random traverses for
the same number of observations. This conclusion is supported by an experimental evidence .
30

(5)

(6)

The variances of the areal and lineal analysis


not only depend on the number of observation,
but also on the size and shape distribution
of the areas of the phase of interest in two
dimensional sections.

31

10

37

38

There is another method for estimating the surface


area per unit volume. Let L be the length of the traces
A

For point counting, the optimum efficiency is


obtained if there is approximately ore test point
per particle or area of phase of interest in the
plane of polish. If this'condition is satisfied, then
the systematic point counting has a smaller variance than either areal or lineal analysis with the
same number of observations. Furthermore, in
such a case, the variance of systematic point counting is independent of the shape and size distribution of the phase of interest.

0
T.L.I

T.L.2

I\

.L.3

. i

Thus, the systematic point counting is the most efficient method, provided t h a t there is approximately one
test point per feature of the phase of interest.

T . L . : T e s t line ; X : I n t e r s e c t i o n s
of the

t e s t lines w i t h <p b o u n d a r i e s

N = 15/L ; U
L

B.

Surface area per unit volume

Suppose a test line is placed at random on the


plane of polish.
Let N be the number of intersections
L

Transactions of The Indian Institute of Metals, Vol. 34, N o . 1, February 1981

of N

is an a v e r a g e

yahie

S = 2N
V

Fig. 4

An example of line intercept counting.

Gokhale : Charactrization of microstructures 75


of a particular type of interface with the unit area of the
plane of polish. It can be shown t h a t ' :
8

3 1

La =

... 6

The result is valid for the curved test lines as well as


straight test lines. It is necessary to obtain N from the
measurements made with the various test line orientations. Combining equations (5; and (6) gives :
t

t r i p l e point
1-L

... 7

IT

However, in equation (7) L must be interpreted as the


average value obtained from the measurements made with
the various orientations of the plane of polish.
Equations (5) and (7) are statistically exact and the statistical
error involved in the estimation cf S can be kept as
small as desired by increasing the number of observations.
The statistical error involved in the estimation of S can
be evaluated from the standard deviation of either N or
L . The line intercept count ( i. e., N measurement ) is
more efficient than L measurement for a given amount
of effort if the measurements are performed manually.
A

FA=14/[_
v a l u e of P

; ^ i s a n average
A

L =2P

Fig. 5

Triple point count for the, estimation


of L .
v

Equation (8) was derived independently by Saltykov


and Smith and G u t t m a n . It is applicable to any type
of lineal feature in space. If the orientation of the lineal
features of interest is r a n d o m , then the value of P
obtained from a single plane of polish can give a reliable
estimate of L . If the lineal features have a preferred
orientation, then, the value of P will depend on the
orientation of the plane of polish. H i l l i a r d ' has
given a general mathematical treatment for a system of
oriented lines in space.
81

The value of N will change systematically with the test


line orientation if the elements of the interface of interest
have a preferred orientation. This principle has been
utilized by Milliard '
in the analysis of oriented
structures. Spektor has also given a mathematical treatment of oriented surfaces in space, however, his analysis
is restricted to symmetrical structures.
L

39

40

41

C.

39

40

Length per unit volume

The quantity L can be estimated from the measurev

Lineal features exist in almost every microstructure.


A statistically exact relationship is available for the estimation of the length of a given type of lineal feature ( e . g . ,
dislocation lines, grain edges, etc. ) per unit volume of
the structure. In a two dimensional section ( i.e., plane
of polish ) a lineal feature usually appears as a point.
Let P be the number of intersections of the lineal feature
of interest with the unit area of the plane of polish.

ments m a d e on a projected image.


of r a n d o m l y oriented

Consider a system

lines in space.

Let L '

ted image.

4 2

It can be shown t h a t '


T

4 3

.. 9
L ' i s related t o N b y equation (6).
equations (6) and (9) g i v e s !

L = 2NJt
A

be the

length of these lines observed per unit area of the projec-

Let p be the corresponding average value obtained from


a large number of measurements performed on the various
orientations of the plane of polish. The length of the
lineal feature of interest per unit volume L is related
to the corresponding value of p by the following equation :

Thus,

combining

... 10

L = 2 P
v

Figure 5 demonstrates

... 8

an

application of this

result.

where t i s the foil thickness. However, N must b e


obtained from the line intercept count performed on a
projected image. F u r t h e r m o r e , equation (10) is valid
only if the lineal features of interest are oriented in a
r a n d o m fashion.
l

Transactions of The Indian Institute or Metals, Vol. 34, No. 1, February 19SI

76
D.

Gokhale ;

Characterization of microstruclurcs

T h e total curvature per unit volume is given by : <

Total curvature per unit volume

Consider a small surface element dS. This surface


element may have any arbitrary curvature. If such a
surface element is intersected by a plane, the intersection
gives a line element. The curvature of this line element
depends on the curvature of the surface clement and the
orientation of the sectioning plane with respect to the
surfa.ee element. The curvature of the line element has a
minimum and maximum value for two specific orientations of the sectioning plane. These maximum and
minimum values of the curvature ire called the principal
normal c u r v a t u r e s
and they are denoted by Kj and K ,
respectively ( see Figure 6. ) For any surface element K,
and K have unique values. The mean curvature IT of
the surface element dS is denned as follows :
44

H=(K +K ) 2
1

T h e total curvature

d\I

... 11

of the surface element dS

is

defined as follows :
dM

The total curvature of a particular type

dS

... 12

of interface

per

unit volume M is then given- by :


v

M =
v

JJ
H.dS
unit volume

... 13

O M r a r u c c . n ^ r w - J M(R) n ( R ) d R - 4TT J R n ( R ) d R
v

o
.
o
... 15
where R is the size of the largest particle. The integral
on the right hand side of equation (15) is the first moment
of the particle size distribution function.
DeHoftf
has
shown that for a tubule network, M is proportional to
the length of the network per unit volume. The total
curvature is expected to be a very important microstructural parameter for the processes driven by surface
tension.
For example, the rates of grain g r o w t h
and
particle coarsening .
depend significantly on the ratio
of the total curvature to surface area. The total curvature may be an important geometrical parameter in the
kinetics of the spherodization process.
Experimental
measurements of total curvature have been carried out
only in few c a s e s . .
m

46

48

46

47

47

35

Total curvature can be estimated by performing the


area tangent count devised by R h i n e s . The measurement consists of counting the n u m b e r of tangents formed
by a random sweeping test line with the traces of a particular type of interface on the plane of polish as the test
line sweeps the plane of polish. D c H o f f
has shown
that :
49

51

F o r a microstructure consisting of geometrically similar


discrete particles in a matrix, the total curvature per unit
volume M of the particle matrix interface is directly
proportional to the first m o m e n t of the partic le size
distribution function.
For example, let us consider the
particles of spherical shape distributed in a matrix.
Let
n (R) be the size distribution function and let M ( R ) be
the total curvature of a sphere of radius, R.
v

M = 7 7 . (T )
V

... 16

n c l

where
(T )n.==((T )+-(T )_)
A

...17

The quantity ( T ) is the average number of tangents per


unit area of sweep, formed by test line, with the traces of
interface elements which are convex with respect to the
phase of interest. ( T ) _ is the average number of
tangents per unit area formed by sweeping test line with
the traces of interface elements which are concave with
respect to the phase of interest. An element of a trace
of an in :ei face is convex if the line joining two adjacent
points on the trace lies inside the phase of interest. An
element of a trace of an interface is concave if the line
joining two adjacent points on the trace lies in some other
phase. Figure 7 illustrates the area tangent count
procedure.
A

... 14

5 0

H =(hV*K )/
2

C a h n has given the following


estimation of the total curvature :

equation

for

the

dM= HdS
Fig. 6 Definition of local mean curvature.
Transactions of The Indian Institute of Metals, Vol. 34, N o . 1, February 1981

M =2n(N )
T

... 18

M t

(NAW=(N ) -(NJ_
A

... 19

Gokhale :

Characterization of microstructure

77

introduced due to the area loop outlines

which truncate

on the edges of the frame of observation.

Such truncated

area loops may be counted

as

1/2.

This

problem

of

truncated area loops does net cause a serious eiror in the


( T ) , measurement.
A

n c

If the interface contains edges, then its total curvature


consists of two

contributions ;

surface elements
elements ( M ) .
v

(M -)
v

Gehl and DcHoff


;

~23/L

T; = J / L

T , = T;-T;
An

T,

A|K t

= T T ^

52

... 20

53

and DeHoff .

54

have shown

the
...21

The integral on the right hand side of equation (21) has to

be carried out over all the

volume

of
53

54

the

edge

structure.

elements

Gehl

DeHoff ,

loops per unit area of plane of polish

can be estimated by applying the area

which enclose

( N ) _ is the average

the

number

closed area loops per unit area of plane of polish

of

have shown that the total

in

the

unit

and

The quantity ( N ) + is the average n u m b e r of closed area


phase of interest and

that

where X is the local dihedral angle of the edge element dl.

not

V
NCT
An example of area tangent count.

Fig. 7

edge

( M ) = i { X . di
v

smooth
the

T , is an a v e r a g e value of

the

total curvature of a collection of edges is given by :

=16/l

from

One car, write :

M = (M ) + (M )
v

one

and the other from

DeHoff *

and

curvature of edges
tangent

count

49

separately to edges

which

(Ma=^

(T )
A

22

enclose the phases other than the phase of interest ( see


where ( T ) is the average n u m b e r of tangents ( or more
A

Figure 8 ).

precisely
N o t e that

equations (16)

and

(18)

are

statistically

exact and they are valid for any type of interface.

The

of

first points

sweep

by

of contact ) formed
sweeping

edge elements ( or m o r e precisely

test

line

per unit area


with

the

with the triple points

interface may be of the discrete particles or of a connected


structure.

The total curvature may be estimated to any

desired accuracy,; by increasing the number of observations.

If the value of ( T

A rii

. oi ( N )
t

J X

n e ;

is very small or

near to zero, then the number of measurements


to get a particular accuracy may be very large.
involved in the measurement of ( T )
A

required
The error

or ( N ) , is the

N E L

n c

sum o f the errors involved, ( T ) + and ( T ) _ o r ( N ) +


A

and ( N ) _ .

Thus,

if ( t )
A

( N ) _ are large numbers,


A

error involved

and

if these are small

and

although t h e relative statistical

n e t

or ( N ) i may be quite large,


A

n e

numbers.

It is necessary to randomize the


to its spatial

C N ) t are

in their estimation may be small, the rela-

tive error involved in ( T )

respect

(T )j_ or ( N )

orientation

the average

possible orientations.

values

plane of polish with


because

obtained

(T ) ,
A

from

0 e

all

and

However, if the microstructurc is

on a single plane of polish may give a reliable estimate of


y

In

the ( N )
A

n e t

measurement some

error

may

N>3|L

the

isotropic and homogeneous, then the measurements m a d e


M .

N;=H/L ;
N

"net

is an average value of . N .
_

A ,
(

e t

be
Transactions of The
Institute
Metals,
34, N o , 1 of
February
19S1
F i g Indian
. 8 Area
loop of
count
for Vol.
the estimation
My

73 Gokhale Characterization of microstructiircs


formed by intersection of the edge elements with the
plane of polish ).
TOPOLOGICAL P R O P E R T I E S

An unambiguous estimation of topological properties


requires measurements made on a projected image or
serial sectioning of microstructure. Barrett and Y u s t
have given a general review of the topological properties which may be used to characterize microstructures.
T h e topological properties provide the information
about the basic '-skeleton"' of microstructure .
Unambiguous experimental estimation of topological properties has been carried out in few cases - "" . The two
important topological properties of interest are " n u m b e r "
and "connectivity." 'Let us first consider the technique
for estimation of number per unit volume.

65

61

48

A.

61

should be 0.1 r to 0.3 r.


should be about 50 to 100.

The total

number of sections

If the features of interest are of convex shape, then


the number per unit volume can be estimated from the
measurements made on a projected image. Let ( N )
be the number of features observed per unit area of the
projected image. It can be shown that :
A

'

"' ^ T T ( N ) - M
v

tr

2 4

T h e above . equation is valid only if the foil thickness t,


is less than the average feature size.

63

Number per unit volume

B.

Connectivity

. T h e choice of a parameter which describes the connectivity of a microstructural feature depends upon the
dimensionality of the feature. The connectivity of a
network can be described by its first Betti n u m b e r .
The first Betti number Pj is defined as follows :
66

The number of particular type of features ( e , g . ,


particles, grains, grain faces, grain edges, etc. ) per
u n i t volume can be unambiguously estimated only by
serial sectioning if the features are multiply connected.
T h e serial sectioning procedure is described in detail
by Aigehinger . An algorithm for analyzing the serial
sectioning data is given by DeHoff, Aigeltinger and
Craig .

1 = =

bn-r-P

... 25

where
b = number of branches in the network

62

n = number of nodes in the network


P

61

In order to perform a serial sectioning analysis it


is necessary to photograph a particular location in
the plane of polish, re-polish the sample a little bit
and re-photograph the same location. The procedure
is repeated until 50 to 100 serial section photographs
are obtained. Let E be the total n u m b e r of sections
obtained and let d be the average spacing between the
two consecutive sections. Let A be the area of each
section. The volume of the sample observed in E
sections is ( E . A . d ) . One can count the number of
particular type of features N in this volume either by
reconstructing the three dimensional microstructure or
by observing the appearance and disappearance of
features in the successive sections. T h e number per
unit volume N is then given by :
T

N,

E.A.d

..23

If the average feature size is r, then the area of sections


should be about 50 r ~ in order to get a good statistical
accuracy. The spacing between the consecutive sections
s

= n u m b e r of separate parts of network

The parameter P is also called Zeroth Betti number.


The topology of the network of lineal features ( e. g.,
grain edge network ) can be characterized by parameters
P and P . If the network is completely connected,
then P is equal to one. One can write the following
equation for the average values of the topological properties of networks.
0

C =B -K -|-N
V

... 2 6

where
C

= connectivity of network per unit volume

B number of branches per unit volume


v

= number of nodes per unit volume

= number o f separate parts per unit volume

T h e connectivity per unit volume, C , represents the magnitude of the first Betti number per unit volume. T h e
quantity C represents the number of branches per unit
volume, which may be removed from the network without
creating any new separate parts and thus it is a measure

Transactions of l h e Indian Institute of Metals, Vol. 34, No. 1, February I9SI

Gokhite Characterization of inicivsinic: lires 79


of the multiple connectedness of network.

The quantities

B , K and N can b e measured b y a serial sectioning


analysis. The details of serial sectioning analysis are
v

= *_(TAT
1v

.. 29

where ( T ) is the average n u m b e r of tangents formed


by a sweeping test line with the lineal feature as the
A

81

given by Aigeltinger, DeHoff and C r a i g .


The connectivity of a closed surface can be described
in terms of " g e n u s . " The genus of a closed surface
is defined as the number of fundamental cuts which can
be made upon the surface without breaking into two
parts.
It can be shown that the genus of a closed surface
is numerically equal to the first Betti number of its
deformation retract . For a system of closed surfaces
in a microstructure, the genus per unit volume, G ,
gives the measure of the connectivity of the surfaces.
The exact estimation of G is not practically feasible,
but the upper and lower bounds on G can be estimated
by the serial sectioning analysis .
65

test line sweeps through the unit area of


image.

a projected

The tangent and normal vectors to a space curve


define a plane called "osculating p l a n e . " T h e local
44

torsion, T,

of a space curve reports the rate at which the

osculating plane changes direction as the curve twists


through s p a c e , . The total torsion per unit volume,
44

53

T , is given by :
v

01

30

The integration must be carried out


element

The topological parameters ( other than number )


associated with the three dimensional volumes bounded
by surfaces may exist, however, their description requires
the introduction of the fourth dimension .
This is
beyond the scope of the present article.

dl

dl

of interest in

DeHoff and G e h l

52

the

over

all

the

line

unit volume of material.


53

and DeHoff .

54

have shown that :

JA

31

08

C. Total torsion and total curvature of lineal features

0 =lO.d\

eatures of a given type in the


-vtructure.

The quantity

out

Tv

Strictly speaking, total torsion and total curvature


of lineal features are not topological properties. They
are included in this section because they can be estimated
only from the measurements on a projected image or by
a serial sectioning analysis. The local cui vature 9 of a
line element, dl, reports the rate at which the tangent
to the line element changes direction. The total curvature of lineal feature per unit volume 6 is given by
the following equation :

The integration must be carried

where I is the average number of the inflection points


of the lineal features of interest in a unit area of a
projected image. In principle,
can also be estimated by a serial sectioning analysis. Since t h e torsion is
a measure of the "out-of-planeness" of a space curve,

...27

over all the lineal

unit volume of micro-

can be estimated by utilizing

he following equation given by DeHoff and Gehf

52

the estimation of of a dislocation array m a y provide a


quantitative measure of the a m o u n t of cross slip
experienced by the s t r u c t u r e .
rv

53

DERIVED ROPErTT.ES

Some geometrical properties of microstructure which


may be locally defined in the structure, a n d hence vary
with the position, possess meaningful average values.
These average values are obtained from a combination
of the global properties and they are called the " d e r i v e d "
geometrical properties. Some of the derived properties
appear as parameters in some theoretical models for
solid state t r a n s f o r m a t i o n s '
and some others a p p e a r
in the structure-property c o r r e l a t i o n s . T h e i m p o r t a n t
derived properties are as follows.
70

0 =7rT
v

vhere x

is

...28

the

average

ormed by a sweeping
is

the

test plane

flicrostructure. T

test

number

of

tangents

be

78

plane with lineal features

sweeps through a unit


can

per-

71

measured by

volume of

serial

A,

Average mean curvature

section-

ig analysis or by performing an area tangent count on


projected image. If the measurements are made on
projected image, then one can write :

The average mean curvature, H, of a given type of


interface in a microstructure is defined by the following
equation . .
50

51

Transactions of The Indian Institute of Metals, Vol. 34, No i, February 1931

so

Gokhale .- Characterization of microstructures

H = J J H dS/JJ d s

. _

...32

curvature of the

surface

where H is

the local m e a n

element dS.

F r o m the definition of the total curvature

it follows that :

Thus, the average mean curvature

is

just

given

by

... 36

Mean free patli

... 3 3

S<fi
v
C.

H=M,/S

The

mean free path is the

surface

to

surface

distance

average

uninterrupted

between

the

particles

the ration of the total curvature and surface area.


T h e average mean curvature is a very important

through the matrix.


For a system of discrete particles
in a matrix, F u l l m a n '
has shown that the mean free

parameter in the kinetics of the

by

p a t h , a , is given by :

surface energy. G i b b s
has shown that the chemical
potential of fine particles is linearly related to
their

= 4(1-V )/S,

processes driven

70

77

60

mean curvature. In some theories of particle coarseni n g ' , the critical particle size is given by the recipro-

37

where V and

are

the

volume fraction

and

surface

particle-

area per unit volume of the particulate phase. T h e


m e a n free path in a r a n d o m two dimensional section

matrix interface.

is the same as that

B.

particles in a

structure. The mean free path appears as a p a r a m e t e r


in the precipitation hardening t h e o r i e s
particle coarsening t h e o r y and in the theory of grain growth of t w o
phase structures .

70

cal

71

of the average mean

curvature

of

the

through

the

three

dimensional

73

Mean intercept length

70

The

mean

intercept

7 of

isolated

matrix is given by the following e q u a t i o n


-

4V

71

D.

Contiguity ratio

.. 34
where V, and S are the volume fraction and surface
area of the particulate phase. The mean tntercept
value in the three dimensional structure is the same
v

as that in a r a n d o m two dimensional section. F o r


the space filling cells or grains, the mean intercept is
siven bv :
(=2/S =l/N
v

70

35

Equation (35) is often used to estimate the grain size


of single phase materials. According to S c h u c k e r f
should be regarded as t h e best practical definition of
grain size.
However, according to R h i n e s and Rhines
and C r a i g , ( 1 / N )
is the most appropriate measure
of grain size of the single phase materials.

T h e contiguity ratio gives the measure of the extent


of interparticle contacts in a microstructure consisting
of particles and matrix.
Gurland
has given the
following definition of the contiguity ratio :
81

C,

Sy/(Sy)ti

38

where Sy is the interparticle contact area per unit


volume and ( S )
is the total interfacial area of
particles per unit volume.
v

t o t M

55

E.

Average nearest neighbor distance

18

The

average

nearest

neighbor

distance,

A,

for

1 / 3

82

r a n d o m l y distributed point particles is given by


0.554 ( N v )-"1 / 3
1

74

84

:
39

75

El-Soudani has analyzed the applicability of


equation (34) to the system of discrete particles or
interconnected phases truncated at the external surface
of the sample. He has shown that in equation (34),
the term S must exclude those surface portions of the
phases which coincide with the boundaries of the external
surface.
T

where N is the
n u m b e r of point particles per unit
volume. Bansal and A r d e l l have derived the following
expression for the average nearest neighbor distance,
A for the randomly distributed monodispersed spherical particles :
T

88

8V

R . e v

80

Gurland
has shown that for a system of partially
contiguous phase ( say < ) in a matrix ( s a y / ? ) , the
mean intercept of a phase is given by :

y '
V v ) 1

dy

... 40

8V

where R is the radius of the impenetrable monodispersed spherical particles. Equation (40) is not valid for

Transactions of The Indian Institute of Metals, Vol, 34 No. 1 February 198J

Cokhale-: - Clumiclerizatlon of mtcrestructurcs 81


80

large volume fractions. A r d e l l has utilized the parameter, A to predict the effect of volume fraction of
precipitates on the rate of precipitate coarsening.
K

The growth rate averaged mean curvature H


defined by the following e q u a t i o n

J J Hvds

He
F.

Mean area intercept

This parameter gives the average value of the areas


of all the possible planer sections through a particular
phase. The mean area intercept A is given by :
A =

... 41

- ^

M,

... 45

97

*dv

... 46
v

Similarly, one can define the growth rate


Gaussian curvature, k , a s follows * :

89

Average dihedral angle

90

... 47

94

Dihedral angle affects the morphology of grain


boundary phases.
H a r k e r and P a r k e r analyzed the
problem -of estimation of dihedral angle from the
measurements made on planar section. They concluded
that the probabilities of the section angular values are
such that the most frequently observed section angles
correspond to true dihedral angles. G u r l a n d has carried out experimental measurement of the dihedral angles
in a microstructure consisting of cemented carbides.
Gehl and DeHoff have given the following expression
for the estimation of the average dihedral angle, x.

fj K.v.ds
7 1 v-ds

where K is the local Gaussian curvature of the surface


element d S . D e H o f f , has shown that :
-

G.

averaged

93

8 8

v is the
It can be

60

82

Jeffrie's m e t h o d
of grain size determination utilizes
(A) ' as the measure of grain size. The ASTM grain
size number is also related to A . Recently, G o k h a l e
has shown that for single phase materials, a is related
to the grain edge length per unit volume.

is

vds

where II is the local mean curvature and


local velocity of the surface element d S .
shown t h a t :
U

88

d M
dV7
v

.. 48

50

C a l m has pointed out that if H < H then a large


positive curvature decreases the local growth rate and
the reverse is true if H > Ft.
If H = H, then the
growth rate does not depend on the particle size.
Thus,
the dynamical curvature averages give some insight into
the process of microstructural evolution.
G

91

52

^ 2 ( M ) e
v

... 42

Lv

PARTICLE S I Z E DISTRIBUTION

An experimental estimation of particle size distribution


and its evolution is desired in the study of many metallurgical processes. A useful information regarding the nucleation rate a n d local growth of particles can be obtained
if the size distribution is k n o w n at various times during
the evolution process * . It is possible to deduce the
rate controlling mechanism of a coarsening process if
the precipitate size distribution attains a quasi-stationary
form > . Estimation of size distribution is desirable
to study the effect of inclusions on the mechanical
properties. It is observed that inclusions are deleterious to mechanical properties only if they are larger
than a certain critical s i z e * .
94

H.

Average torsion and average cursature of lineal features


53

Gehl and DeHoff


torsion, , and average
features are given by :
T

have shown that the average


curvature, o, of the lineal

T = T /Ly
T

... 4 3

71

95

9G

87

0 '= 0 / L
V

I.

98

... 44

Dynamical curvature averages

In an evolving microstructure, some derived properties related to the path of microstructural change can
be defined. These derived properties may give important information regarding the evolution process.

T h e problem of estimation of size distribution from the


measurements m a d e on two dimensional sections is quite
complex. A general solution to the problem does not
exist. It is necessary to make simplifying assumptions
regarding the particle shape. Even when a simple particle
shape is assumed ( e.g., sphere ), it is necessary to go
through fairly complex numerical calculations for size

Transactions of The Indian Institute of Metals, Vol. 34, N o . \, February 981

Gokhale r Characterization of microstructures


distribution.
The following assumptions are
to all the techniques to be discussed :

common

(1)

Particles are uniformly distributed in a matrix

(2)

All the particles have a convex shape

Most of the techniques, with a few notable except i o n s ' , assume that all the particles have a geometrically similar shape ( e . g . . ellipsoids of same axial
r a t i o ) and they differ only in size. The assumptions
regarding the particle shape are not generally verified
when the experimental measurements are carried out.
F o r example, if most of the sections are circular,
it is taken for granted that the particle shape is spherical. However, such a conclusion may be quite misl e a d i n g ' ' . For example, if the precipitate phase
consists of a tubule network along the grain edges of
matrix, most of the precipitate sections in the plane
of polish would be discrete and convex .
59

t h a n or equal to r. Lot 6 ( r, R ) be a function such


t h a t , <j> ( r, R ) dR gives the n u m b e r of circular sections
of sizes larger than or equal to r obtained from spheres
whose sizes are between R and ( R-j-dR ). Thus,
N.,> (r) - J <f> (r, R) d R / |

49

100

55

101

where f is the total area of the plane of polish. T h e


sphere of size R will give sections of size larger than or
equal to r only if its center is at a distance less than, or
equal to ( R r ) from the plane of polish.
Thus, all
the spherical particles whose size is between R and
( R + dR ), contained in the volume 2. ( R r )
will
give sections of size larger than or equal to r.
2

i a

1 / 2

102

0 ( r, R ) d R = 2 { ( R - r )

1 , a

n (R) dR

... 50

Combining equations (49) and (50) gives :

55

N
The techniques for detailed estimation of particle
size distribution ( henceforth denoted, by P S D ) require
a measurement of the distribution of some geometrical
variable ( e . g . , section sizes, linear intercepts, etc. ) on
the plane of polish. This measured distribution function
is then transformed into P S D by applying the principles
of geometrical probabilities .
3

A >

( r ) = 2 | (R r ) / n ( R ) dR
r

... 51

Operating on this equation by d/dr gives


, ,
"

( r )

~ ?> n ( R ) d R
/ (R*-r)i'
v

2 r

5 2

Equation (52) can be converted into a standard Abelian


integral equation and then it can be solved for n (R).
The result is as follows.
v

A.

Estimation of PSD from section size distribution


c

d
Consider a system of polydispersed spherical particles distributed uniformly in a matrix.
Let n ( R ) be
the particle size distribution function such that n ( R )
dR gives the number of spheres per unit volume whose
radii are between R and ( R + d P . ) . A two dimensional
section through such a microstructure consists of circles
of various radii distributed uniformly in the two dimensional matrix. Let the variable r represent the radii of
the circular particle sections. Let n ( r) be the section
size distribution ( henceforth denoted by SSD ) such
that n ( r ) dr gives the number of circles per unit area
of plane of polish whose radii are between r and ( r + d r ).
The SSD n ( r ) can be measured from the plane of
polish.
The problem is to estimate n ( R ) front n ( r ).
Let us define

n (R)

(r)
2

- 2TT
- dR
- t Hk (r R ) /

dr

... 53

108

Equation (53) was first derived by W i c k s e l l . However,


the derivation given here may be different from that given
by Wicksell . It is possible to estimate the moments of
P S D directly from the moments of S S D . Let us define :
103

m. = l (r) " A (r) dr


o

... 54

Mj = J (R)' n (R) dR

... 55

and

10

It can be shown that *

rn

- Pt

+ 1

M,

... 56

where,
N > (r) = J n (r) dr
A

... 48

T h u s , N a > ( r ) gives the number of circular sections


per unit area of plane of polish whose radii arc larger
Transactions of The Indian Institute of Metals, Vol. 34, No. 1, February 1981

+1

.. 57

Uukhalc

where,

S3

unless the nucleation and growth behavior is such as to


produce the P S D having the assumed functional form.

r(o+i)orf)
r(i/2)=v^;r(i)=i

... 58

Wickscll's analysis for estimation of PSD has the


ing limitations :
(1)

Characterization of mkfoitrwtures

It is necessary to have an analytical


for n (r) to estimate n (R).
A

follow-

expression

If no information is available regarding the analytical


functional form of n (R) or n (r), then it is necessary
to
approximate equation (51) by a set of linear
equations in order to estimate P S D . This procedure is
called "unfolding a particle size distribution." Such
numerical procedures have been developed for spherical
particles by S c h c i l , ' ,
Schwartz
a n d Saltykov .
Saltykov's m e t h o d is more convenient and involves less
computational error. T h e basic algorithm is as follows.
v

110

(2)

One has to calculate a numerical derivative.

(3)

The total number of particles per unit volume N


is given by :

11

118

CO

Nv=2- \ - ^ - d r

... 5 9

It is necessary to calculate mj moment of SSD to


estimate N . This is a very insecure estimate because
m _ ! is most sensitive to the behavior of n (r) at small
section sizes where the error involved in the measured
SSD is the largest.
v

Some of the above drawbacks can be eliminated if


some .information is available regarding the functional
form of n ( R ) . If n (R) can be represented by a two
parameter gamma distribution, then the two unknown
parameters can be easily estimated from the moments of
S S D . In this context, log-normal form of P S D is
important and it has been verified in some c a s e s , " . In
many cases the experimental P S D appears to have a
log-normal f o r m
. It can be shown that if the
particles follow certain specific growth laws during the
evolution of PSD, then n (R) has a
log-normal
form
. Simpson and S t a n d i s h , have given some
justifications for assuming a log-normal form for n (R)
and they have given an algorithm to calculate the
unknown parameters of log-normal P S D
from
the
moment of SSD. DeHoff has shown that if the P S D
can be adequately represented by a two parameter
log-normal form, then these two parameters can be
estimated from the measured values of volume fraction,
surface area and total curvature. There is no need to
estimate the SSD. Furthermore, DeHoff's analysis
is
applicable to particles of any shape, as long as the particle
shape is known. It must be emphasized that the P S D is
determined by the nucleation rate and local growth rate of
particles during the evolution process" .
Thus,
the
assumption of particular functional form for n (R) ( e. g.,
log-normal form ) may be quite misleading and erroneous
v

104

105

10

(1) The size distribution is divided into K classes


( K may be any integer between 7 a n d 15 ). The size
class interval A is given by :
A =D /K

...60

where D is the diameter of the largest sphere and


hence the diameter of the largest circular section.
m

(2) N

V j

, N

number

of

per unit volume whose diameters are

A,

V |

spheres

... N

... N

V j

represent

Vfc

the

2 A , j A , k A , respectively.
(3) n

A i

, n

, ... n

A j

, ... n . represent the n u m b e r of sec-

A [

tions per unit area whose section diameters are in the


range, 0 to

A, A to 2 A , ( i - T )

to

i A ,

( k I ) A t o k A , respectively.
(4) N

T j

N . , ... N
v

, ... N ,

V j

can be calculated from

1 0 7 - 1 0 9

"AJ , % . A , , A

by using the following

);

equation :

1 1 0 - 1 1 2

113

114

115

116

1
=--

p (j, i) n

... 61

i=j
where |8 (j, i) are the Saltykov's coefficients, and these
are tabulated by Saltykov and DeHoff .
0

119

The p r o b l e m of unfolding P S D is analyzed by


Nicholson and M e r c k x
on the basis of estimation
theory.
They have also given the method for error
analysis. W a t s o n
has discussed the numerical procedures for estimation of P S D . N i c h o l s o n has given
a technique for the estimation of the moments of
P S D for particles of any shape.
120

1 2 2

122

Let us consider the techniques for estimation of


P S D of ellipsoidal particles. W i c k s e l l " has given
integral equations similar to equation (53). His analysis

Transactions of The Indian Institute of Metals. Vol. 34, N o . 1, February 1981

84

Gakhale

Charactization

of

microstructures

is applicable.'even, if the. system consists-of ellipsoids


of different axial ratios, p r o v i d e d - t h a t all the ellipsoids
are either prolate or oblate. However, an analytical
functional form is needed for SSD to estimate the
P S D . D c H o f f has given a technique, similar to Saltykov's technique, for estimation of PSD of geometrically
similar ellipsoids of revolution.
DeHoff
gives the
following equation.

..area

distribution.

Saltykov's

method

is more flexible

and convenient. The basic steps involved in the Saltykov


m e t h o d are as follows.
(1) Size of a section is specified by A / A where A is
the area of circular section and A is the area of
m

119

the largest circle on the plane of polish.

110

(2) The section area distribution described in terms


of the variable A / A is divided into K size
m

*S - A.KCQj

!/CJ,i)N

...62

where K(Q) is a shape factor and it depends on the


axial

ratio,

Q, of the ellipsoids.

prolate ellipsoids,
axes

of

the

then n

of

polish.
used

major
The

other

notations

123

0.613

is the distribu-

represent the number of circu-

A (

per unit area of plane of polish whose

The N

V j

values can

the problem exists only if all the ellipsoids are either


oblate or prolate. The input information required is
a bivariant distribution of major and minor axes of
ellipses on the plane of polish. This bivariant section
size distribution is related to the corresponding bivariant
P S D through a double} Abelian integral equation.
121

Myers
has given a technique for estimation of
P S D of cubic particles. The input information required
is the measurement of altitudes of the four-sided sections
on the plane of polish. He has shown that the altitude
of a four-sided section is closely related to the edge
length of the cube, and furthermore, the four-sided sections form a fixed fraction of the section shapes observed.
Estimation of P S D of polyhedral particles is considered
by Scheil and W u r s t , Hull and H o u k
and P a l a u s .
The experimental work of White and
Van V l a c k
indicates that the pentagonal dodecahedran
is an adequate
model shape for the estimation of
cell size distribution.
120

be calculated

0.0079 N

0.0038 N

A
A

0.001 N

A ]

- 0.0003 N

0.0018 N

A l
A

j5

A j

- 0.0002 N

A j

A Q

]7

A j

...63

have any integer value

twelve, and N

J4

A
A

JS

0.0002 N _ . ]
where j can

j 3

j2

up to and including

N _ , , N _ , , etc., are zero.


A

13

Lewis, Walters and J o h n s o n * have generalised the


Saltykov m e t h o d
for convex particles of any shape.
The particles need to be of the same shape only within
a size class interval. If the particle shape is a direct
function of its size ( as it would happen in the case of
one dimensional or two dimensional growth ), then Lewis,
Walters and Johnson's m e t h o d
is ideal for estimating
PSD. Myers and S i n n o t i
have carried out a computer
simulation for deducing the section area distribution of
polyhedral particles.
131

132

133

C. Estimation of PSD from linear intercept distribution

1 5 8

127

129

B. Estimation of PSD from section area distribution

the P S D

A a

131

Saltykov

to 0.613 A ,

t o 0.398 A , 0.398 A t o 0.251 A , etc.,

= ~ [1.6461 N
- 0.451 N,
,
j
Dj
j
*J-i
0.1162 N
0.0415 N
0.0173 N ,

100

to estimate

... N .

are the same as those

The problem is also analyzed

However, his analysis is similar to that

and

respectively.

Recently, C r u z - O r i v e
has given a method for
estimation of size and shape distribution of ellipsoidal
particles.
He has shown that a unique solution to

130

A 2

from the following equation :

given by Wicksell".

Johnson

, N

section areas arc in the range A

If the

axes of the ellipses on the plane of

in equation (61).

by T a l u s

A 1

The size class interval is equal to 1 0 ~ .

lar sections

is the distribution of minor

particles are oblate ellipsoids, then n


tion

(3) N

If the particles are

ellipses on the plane of polish.

0 3

classes.

have developed methods

of spherical particles from section

Consider a set of test lines placed at random in the


three dimensional microstructure or on the plane of
polish. These test lines will intersect the particles
present in the microstructure, this producing the intercepts of various lengths.
Let n (i) be the distribution
of the intercepts obtained from intersections of test lines
with various particles. T h u s , n (/) d/ gives the number
of intercepts per unit length of test line whose lengths

Transactions of The Indian Institute of Metals, Vol. 34, N o . l , Fi-brui y.mi

Cokhalc Characterization -of micro structures' 85


14

are between 1 and (7 + d/). I t o h


and Exner ~and
L u c a s have given the following relationship between n
(/) and n (R).
135

on

(0

2 1

11

(R)

y (,/R) d R
... 64

a (R) . n (R) d R
v

148

151

image is analyzed ' by H i l l i a r d ' and o t h e r s - ' : '


The analysis becomes extremely complicated due to the
overlap and truncation effects. It is possible to solve
the problem only for some simple particle shapes and
even then some additional assumptions are necessary.
It is relatively easier to estimate P S D of second phase
particles from extraction replica. Eshby and E b c l i n g
have analyzed this problem. Stumpf and S e l l a r s
have carried out experimental measurements of P S D
from the measurement made on extraction replicas.
162

103

where <l> (l/R) intercept


particle of size R, and.
a (R) = C . R"

length

distribution

of one

c is the shape factor. F o r convex particles, a (R) is onefourth of the total surface area of the particle.
F o r spherical particles, it can be shown t h a t
V 0/R) =

i
2R

1 3 6 - 1 3 8

... 65

and

Another interesting problem is the estimation of P S D


from the measurements made cn the field ion micrographs. An image produced by field ion microscope
is a plane projection of a curved surface. In such a case
it is not possible to estimate the true size distribution
directly from the observed size distribution.
However, if
the true size distribution is known, then the observed size
distribution can be calculated. S c h w a r t z and Schwartz
and R a l p h
have given and algorithm to calculate the
observed size distribution for a given true size distribution.
153

o (R) = v R"

... 66

1 5 1

Substituting equations (65) and (66) into


gives :
n

(/) -

equation (64)

(/))

dl

6 7

/
136

This result was first given by S p e k t o r


and Calm
and P u l l m a n . Lord and W i l l i s
have given a
graphical procedure to calculate the size distribution
from n ( ; ) . Their m d h o d is based on a numerical
solution to equation (67). The problem of estimation
of the size distribution of spherical particles from their
linear intercept distribution is also analyzed by Stjenberg ,
Bookstiegel and Henlser .
187

139

140

141

142

143

DeHoff and B o u s q u e t
have given the following
result for the geometrically similar triaxial ellipsoids.

where K is a shape factor and it depends on


axial ratios of the triaxial ellipsoids.
1 3 4

1 4 4

the

DISCUSSION

The eight independent global properties, namely,


Vy, Sv, M v , Ly. N , Cv, T and 9y can be unambiguously estimated for any homogeneous ( i . e., no segregation ) microstructure. Estimation of these stereological
parameters does not require any information or assumption
regarding the shape and size of the features. F o r a
microstructure consisting cf only two j hases, one can
estimate m o r e than twenty independent global properties.
To the best knowledge of the author, such a rigorous
characterization of microstructure ( i. e., estimation of
all the global properties ) has never been carried out
and may not even be needed for most of the applications.
However, depending on the evolution process of interest or
the physical property to be correlated, a particular subset
of the global properties may be estimated to study the
evolution process or microstructure-property correlations.
v

1 4 6

Itoh
and
Coleman '
have considered the
intercept distribution of cubic particles. I t o h
has
derived
an analytical expression for the intercept
distribution of a cube of unit edge length. W a r r e n
has
experimentally verified I t o l r s f o r m u l a for cubic particles.
1 3 4

146

134

The above description gives the techniques for


estimation of P S D from the measurements made on
a two dimensional section. The problem of estimation
of P S D from the measurements m a d e on a projected

The ultimate limitation on the information which can


be obtained from the measurements m a d e on plane
sections or projected images is not known. Some
measurements, which can be carried out on plane
sections, have n o t yet been related to any global property.
F o r example, one can count the inflection points in the
traces of interfaces on the plane sections. However, the
relationship between this quantity and any global property
has not yet been developed.

Transactions of The Indian Institute of Metals Vol. 34, N o . 1, February 19S1

36

Gofchale : Characterization oj mtcrosiruciures


There

are

many unsolved

problems

in

stereology.

21.

a. T. Howard and M. Cohen, Trans. Met, Soc. ALME, 172


(1947), 413.

22.

J. Swift and Sons Ltd., London : "Swift Automatic Point


Counter",

Characterization of microstructurcs from the m e a u r c m e n t s


made

on

fractured

projections

of

investigation.
estimation

surfaces,

curved
Several

curved

surfaces

need

questions

surfaces,
a

plane

of further
the

'23.

H o w many n u m b e r of

24.

arise

of size distributions.

lot

regarding

size classes should be chosen to unfold a size distribution ?


How

do

the

distribution

errors involved in the measured section size


propagate

performed

to

ment

stereology

of

estimate

when
size

is

not

complex

calculations

distribution ?
yet

are

T h e develop-

complete and

further

research may bring answers to these questions.

A. H. Holmes, Portographie Methods


Murby and Co., London, (1927).

and

Calculations,

25. J. W. Cahn and J. Nutting. Trans. Met. Soc. AI ME, 215


(1959), 526.
26.

J. E. Billiard, Trans. Met. Soc. ALME, 224 (1962), 90 6.

27.

J. E. Hilliard, J, Microscopy, 95 (1972), 45.

28. J. E. Milliard, Reervstaltizalion, Grain Growth and Textures,


ASM Publication, Metals Park, Ohio, (1966), 267.

REFERENCES
1.

R. T. DeHoff, Quantitative Microscopy, ed. R. T DeHofT and


F. N. Rhincs, McGraw-Hill, New York, NY, (1968), 32-43.

2.

M. G. Kendall and P. A P. Moran, Geometrical Probability,


Griffins Statistical Monographs, C. Griffin, London, (1963),
No. i 0 .

3.

F. N. Rhines, Met. Trans., 8A (1977), 127.

4.

A. Delesse, Ann. Mines. IV, 13 (1848), 379.

5.

F. Chaves, Pertographic Model Analysis, John Willey, New


York, (1956), 16.

6.

S. A. Saltykov. Stereometric
Metallurgizdat, Moscow, (1958).

7.

E. R. Weibel, Morphometry of Human Lung, Springer-Verlag,


Berlin, (1963), 12.

8.

J. E. Milliard, "Volume Fraction Analysis by Quantitative


Metallography," Rep. N o . 61 RL 2652 M, General Electric
Research Lab., (1961).

Metallography,

I. H. Ford, J. Sei. Instr., 31 (1954), 164,

29.

J. E. Milliard and J. W. Cahn, Trans. Met. So. AIME, 221


( 1961), 344.

30.

J. G. Osborne, J. Am. Stat. Soc., 37 (1942), 256.

31. C. S. Smith and L. G u t t m a n , Trans. Met. Soc. AIME, 197


(1953), 81.
32.

R. J. Duffin. R. A. Meussner and F. N. Rhines Carnegie


tust. Tech , Tech. Rep. N o . 32, AF-33 (616), (1953), 294.

33. E. Horikawa, Tetsu to Hagane, 40 (1954), 991.

2nd

ed.,

9. J. E. Milliard, Quantitative Microscopy, ed. R. T. DeHoff and


F. N. Rhines, McGraw-Hill, New York, (1968), 45-74.
10. E E. Underwood, Quantitative Stereology, Addison-Wesley,
New York, (1970), 110.

34.

H. Campbell and S. I. Tomkeicff, Nature, 179 (1952), 117.

35. S. Corrsin, Quart. Appl. Math., 12 (1954), 404.


36.

A. Hennig, Mikroskopie, 11 (1956), 1.

37.

E. E. Underwood, Quantitative Microscopy, ed. R. T. DeHoff


and F . N . Rhines, McGraw-Hill, New York, (1968), 77-123.

38.

J. E. Hilliard, Proceedings of Symposium on Statistical and


Probabilistic Problems in Metallurgy, ed. \V. L. Nicholson, A
Special Supplement to Advances in Applied Probability,
Applied Probability Trust, (1972), 92-106.

39.

J. E. Hilliard, Trans. Met. Soc. A I M E , 224 (1962), 1201.

40

J. E. Hilliard, Stereology, ed., H. Elias, Springer-Verlag,


New York, (1967), 219-225.

41. A. G. Spektor, Zavod. Lab., 20 (1954), 5.

11. D. McLean, Grain Boundaries in Metals, Oxford University


Press, London, (1957), 110.

42.

J. E. Bailey and P. B. Hirsch, Phil. Mag.. 5 (1960). 485.

12.

A. Rosiwal and K. K. Geal, Reich. Wien.,5-6 (1898), 143.

43.

E. E. Underwood, Quantitative Stereologv, Addison-Wesley,


New York, (1970), 148-157.

13.

H. F. Fischmeister, Quantitative Microscopy, ed. R. T.


DeHoff and F. N. Rhines, McGraw-Hill, New York, (1968),
336-371.

44.

D. J. Struik, Lectures in Classical


Addison-Wesley, New York, (1950).

14. C. Fisher, Microscope, 19 (1971), 1.

45.

R. T. DeHoff, private communication.

15.

46.

R. T. DeHoff, Dynamics of Microstructural Change, N S F


Grant No. 16371, Annual Report, (1970).

47.

R . M . D i w a n , Ph.D. Dissertation, University


(1974).

48.

K. R Craig and F. N. Rhincs, Met. Trans., 5 (1974) 413.

49.

F. N. Rhines, R. T. DeHoff and R. A. Rummel, Topological


Models for S intering Process, AEC Contract No. AT-(4001)2851, Annual Report, (1962).

50.

J. W. Cahn. Trans. Met. Soc. AIME. 239 (1967), 610

E. Thomson, J. Geol., 38 (1930), 193.

Differential Geometry,

16. A. A. Glagolev, Eng. Min. J., 135 (1934), 399.


17. J. E. Hilliard and J. W. Cahn, Trans. Met. Soc. A1ME, 221
(1961), 344.

of

Florida,

18. A. Chayes, Amer. Min., 34 (1949), 1.


19.

H. F. Fischmeister, Stereology, ed. 1-1. Elias, Springer-Verlag,


New York, (1967), 263-273.

20.

A Hennig, Zeiss Werkzeitschrift, 30 (1958), 3.

Transactions of The Indian Institute of Metals, Vol. 34, No. 1, Febr

1981

Gokliale :
-.82.

51. R T. DeHoff, Trans. Met. Soc. AIME, 239 (19G7), 617.


52.

S. M. Gehl and R. T. DeHoff. Proceedings of Fourth


International Conference for Stereology, e d . , E . E. Underwood,
N. B. S. Publication, (1976), 29.

53. R. T. DeHoff, Quantitative Determination of the StructureProperty Correlationshlps in


Nuclear
Fuel
Element
Materials, AEC Contract N o . AT-(40-l)-4212, Final Report,
(1975).

56.

C. Fisher. Practical Metallography, 6 (1969), 659.

57.

G. A. Ratz, Metal Prog., (1968), 45.

Mod.

Phy., 15 (1943), 86.

84.

P. Hertz, Math. Ann., 57 (1909), 387.

85.

P. P. BansaJ and A. J. Ardcll, Metallography, 5 (1972), 97.

86. A. J. Ardcll, Acta. Met., 20 (1972), 61.

R. T. DeHoff, to be published in J. Microscopy.

55. A. M. Gokliale, Ph D. Dissertation, University of Florida,


(1976).

S. Chandrasekhar, Rev.

87

83. F. Forscher, J. Franklin I n s t , 259 (1955), 107.

87.
54.

Characterization oj micro'siruciures

Z. Jeffries, A. H. Kline and E. B. Zimmer, T r a n s . Met.


A I M E , 57 (1916), 596.

Soc.

88. L. L. Wymen, ASTM Bull., (1956), 59.


89.

A. M. Gokhalc, to be published.

90.

D. Harker and E. R. Parker, Trans. ASM, 34 (1945), 156.

91. J. Gurland, Metallography, 10 (1977.), 461.


58. A Strang, J, Sei. Instr., 2 (1969), 45.
59.

E. R. Weibel, Stereology, ed. H. Elias,


New York, (1967), 330.

Springer-Verlag,

92. R. T. DeHoff, Proceedings of the Symposium on Statistical


and Probabilistic Problems in Metallurgy, ed., \V. L.
Nicholson, A Special Supplement to Advances in Applied
Probability, Applied Probability Trust, (1972), 188-197.

60. H. F. Fischmeister, Stereology ed. I I . Elias, Springer-Verlag,


New York, (1967), 263.

93.

61. R. T. DeHoff, E. H. Aigeltingcr


J. Microscopy, 95 (1972), 69.

R. T. DeHoff, Treatise on Materials Science,


Academic Press, New York, (1972).

94.

R. T. DeHoff, Met. Trans., 2 (1970), 521.

and

K.

R.

Craig,

62. E. H. Aigeltinger, Ph. D. Dissertation, University of Florida,


(1969).
63. J. H. Steele, Ph. D. Dissertation, University of Florida,
(1967).
64. F. N. Rhines, R. T. DeHoff and J. Kronsbein, A Topological
Study of Sintering Process, AEC Contract No. AT-(40-l)2581, Final Report, (1969).
65.

L. K. Barrett and C. S. Yust, Metallography, 3 (1970). 1.

66.

S, S. Crains, Introductory Topology. Ronald Press, New York,


(1961).

67. P. S. Aleksandrov, Combinatorial Topology, Graylock Press,


Rochester. New York, (1956), Vol. 1.
68. E. H. Patterson, Topology, Olivei and Bovd Ltd., L o n d o n , '
(1963), 12-20.
69.

J. W. Gibbs, The Scientific Papers of J. Wiiard


Vol. 1., Dover Publications. Inc., New York, (1961).

Gibbs,

70.

R. T. DeHoff, private communication.

It,

C. Wagner, Z. Elektrochimie, 65 (1961), 243.

72.

F. Schuckhcr, Quantitative Microscopy, ed., R. T. DeHoff


and F. N. Rhines, McGraw-Hill, New York, (1968), 201-251.

S. M. El-Soudani, Metallography, 10 (1977), 27.

75.

S. M. El-Soudani, Metallography, 8 (1975), 297.

76.

R.

L.

Fullman, Trans. Met.

77.

R.

L.

Fullman, Trans. Met. Soc. A I M E , 197(1953), 1267.

78.

E.

Orovvan,

Soc. AIME, 197 (1953), 447.

Symposium on Internal Stresses Institute of

Metals, London, (1947), 451.


79.

M. Hillert, Acta. Met., 12 (1965), 227.

80.

1, Gurland, Trans. Met. Soc. AIME, 236 (1966), 642.

81

J. Gurland. Trans. Met.

1,

95. J. W. Wooohcad, Metallography, 1 (1968), 35.


96.

I. M. Liftshitz and V. V. Slyozov, J. Phys. Chcm. Solids. 19


(1961), 35.

97.

R. Keissling, Jernkont. Ann., 153 (1969), 79.

98.

3 . 1 . Kievcbring, E. Borger and R. Mahrs, Met. Trans., 6A


(1975), 319.

99.

S. D. Wicksell, Biometrika, 18 (1926), 151,

100.

Cruz-Orive, to be published in the J. Appl. Phys.

101. R. T. DeHoff, Metallography, 8 (1975), 71.


102. L, K. Barrett and C. S. Yust, Trans. Met. Soc. A I M E , 239
(1967), 1172.
103. S. D. Wicksell, Biometrika, 17 (1925), 84.
104.

P. A. P. Moran, Proceedings of the Symposium on Statistical


and Probabilistic Problems in Metallurgy, ed., VV. L,
Nicholson, A Special Supplement to Advances in Applied
Probability, Applied Probability Trust, (1972), 76-83.

105. S. Drapal and V. Haralek, Acta. Tech., 4 (1959), 474.


106.

W. M. Wojick, R. M. Raybcck and E. J. Poliwoda, J. Metals,


19 (1967), 36.

107.

W. M. Swift, Met. Trans., 4 (1973), 153.

73. F. N. Rhines and K. R. Craig, Met. Trans., 5 (.1974), 413.


74.

Vol.

108

W. E. Stumpf and C. M. Sellars, Metallography, 1 (1968), 25.

109.

P. F. F o o t n c r and C. B. Alcock, Met. Trans., 3 (1972), 2633.

110.

F. ICottlcr, J. Franklin Inst., 250 (1950), 339.

111. S. D. Wicksell, Ark. Mat. Atr. Fys., 12 (1917), 1.


112.

J. Aitchison and J. A. C. Brown, The


Distribution, Cambridge University Press,
(1966). 20.

Log-Normal
Cambridge,

113. I . M . S i m p s o n and S. Standish, Metallography, 10 (1977),


149.

Soc. A I M E , 212 (1958), 452.

Transa ions of The Indian Institute of Metals, Vol. 34, N o . 1, February 1981

88
114.

Gokhale :

Characterization of microslrnctures

I. M. Simpson and S. Standish, Metallography, 10 (1977),


433.

115. R. T. DeHoff, Trans. Met. Soc. A I M E , 233 (1965), 25.


116.

E. Scheil, Z. Anorg Allgeni. Chem., 201 (1931), 259.

117.

E Scheil, Z. Metallic.., 27 (1935), 199.

118.

11. A. Schwartz, Metal Alloys, 5 (1934), 139.

119. R. T. DeHoff, Trans. Met. Soc. AIME, 224 (1962), 474.


120.

W. L. Nicholson and K. R. Merckx, Technometrics,


(1969), 707.

12!.

G. S. Watson, Biometrika, 58 (1971), 483.

11

134.

II. Hh, Metallography, i (1970), 404.

135.

II. E. Exner and II. L. Lucas, Metallography, 4 (1971), 325.

136.

A. G. Spektor, Zavod. Lab., 16 (1950), 173.

137.

J. W. Calm and R. L. Fullman, Trans. Mot. Soc. AIME, 206


(1956), 610.

138.

II. E. Exner, Z. Metallk., 57 (1966), 755.

139.

G. W. Lord and T. F, Willis, ASTM Bulletin, 17 (1951), 56.

140.

K. G. Stjenberg, Metallography, 2 (1969), 161.

141. G. Bockstiegel, Z. Metallk., 57 (1966), 647.


142.

122. W. L. Nicholson, Biometrika, 57 (1970), 273.

J. H. Hcnslcr, J. Inst. Metals, 96 (1968), 190.

143. R. T. DeHoff and P. Bousquet, J. Microscopy, 92 (1970), 119.

123.

G. M. Talus, Biometrics, 26 (1970),.S7.

124.

E. J. Myers, Stereoiogy, ed., H. Elias, Springer-Verlag, New


York, C1967), 187-190.

125. E. Scheil and H. Wurst, Z. Metallk., 28 (1936), 340.

144.

R. Coleman, J. Appf. Probability, 6 (1969), 411,

145. R. Coleman, Metallography, 6 (1973), 103.


146. R. Warren, Metallography, 4 (1971), 56!.

126.

M. Palaus, Me'taux, Corrosion-Industries, 37 (1962), 448.

127.

M. Palaus, Me'taux, Corrosion-Industries, 38 (1963), 449.

12S.

F. C. Hull and W. H. Houk, Trans. Met. Soc. AIME, 197


(1953), 505.

129.

P. L. White and L. H. Van Clack, Metallography, 3


241.

147. J. E. Hilliard, Trans. Met. Soc. A I M E , 224 (1962), 906.

130.

J. W. Philips, Bri, J. Appl. Pays. Supp!., 3 (1954), 133.

149.

P. C. W. Hawksey, Bri. J. Appl. Phys. Suppl., 3 (1954), 125.

150.

P. L. Goldsmith, Bri. J. Appl. Phys. Suppl., 18 (1967), 813.

(1970),

W. A. Jhonson, Metal. Prog., 49 (1946), 87.

131. S.A. Saltykov, Stereology, ed., H. Elias, Springer-Verlag,


New York, (1967).
132.

148.

H. D. Lewis, K. L. Walters and K. A. Jhonson, Metallography, 6(1973), 93.

133. E. J. Myers and M. J. Sinnott, Computer Applications in


Metallurgical Engineering, A. S. M. Publication, Metals Park,
Ohio, (1964), 17-22.

151. J. M. G. Crompton, R. M. Waghorne and


Bri. J. Appl. Phys., 17 (1966). 1301.
152.

Transaction of The Indian Institute of Metal, Vol, 34, No. 1, February 981

Brook,

M. F. Ashby end R. Ebeling, Trans. Met. Soc. AIME, 236


(1966), 1396.

153. D. M. Schwartz, Ph. D.


Cambridge, (1968).
154.

G. B.

Dissertation.

University

D. M. Schartz and B. Ralph. Phil. Mag., 9 (1969), 1061.

of

También podría gustarte