Refractory Metals and Hard Materials 10 (1991) 61 81

Microstructural Characterization of Cemented

Carbides Using SEM Based Automatic Image
Analysis
Anders Nordgren
Swedish Institute for Metals Research, Drottning Kristinas Vfig 48, S-114 28 Stockholm, Sweden

Abstract: Methods for SEM based automatic image analysis of cemented carbide
microstructure were developed. Two different categories of hard metal were
investigated: WC-Co grades and WC ~ C o grades, i.e. cemented carbides
containing cubic carbides (7-phase) as well as tungsten carbide WC. The materials
represented a wide range in grain size, chemical composition and structure
complexity.
Automatic object detection and evaluation of carbide grain size, carbide contiguity
and volume fractions were possible through the combination of optimized
specimen preparation, high resolution microscopy and image processing in a
software oriented image analyzer. The importance of careful specimen preparation
in order to obtain maximum contrast and structure definition was emphasized.
High spatial resolution in SEM was achieved by working at low accelerating
voltages. Two different back scattered electron contrast modes were utilized:
atomic number (Z) contrast and channelling contrast.
Mean values of WC and cubic carbide (y-phase) grain size in the range 0.6-2/~m
were measured; values which were considerably lower than values obtained
according to conventional methods. The difference was explained by the low
detection limit in the SEM based analysis, enabling detection of fine carbide grain
populations. Binder mean free path increased and carbide contiguity decreased
with increasing binder volume and with increasing carbide grain size in the
WC-Co alloys.
The results of the automatic measurements were of fully sufficient accuracy for a
wide range of hard metals. In cases of very weak contrast, limited manual editing
was sufficient to obtain results close to actual values. It was concluded that
automatic methods can be successfully applied to the characterization of complex
cemented carbide microstructures.

1 INTRODUCTION microscope (LOM) is sufficient for coarse grained

Conventional microstructural characterization of
cemented carbides in terms of carbide grain size and
volume fractions of different phases is usually
synonymous with semi-automatic analysis of struc-
ture micrographs. 1'2 In such a case the object
detection is made by the operator who marks grain
boundaries and phases, e.g. using a stylus and a
digitizer tablet. Data are transferred to a computer
for processing and parameter evaluation. Different
types of microscopes are available for imaging the
microstructure. The resolution of the light optical
61
Refractory Metals and Hard Materials 02634368/91 $3.50 © 1991 Elsevier Science Publishers Ltd, England. Printed in Great Britain.
material and LOM is in addition frequently used for
defect control such as the measurement of pores
and free graphite. However, modern hard metals
are often fine grained with a complex microstructure
requiring higher resolution than that offered by
LOM. In early works plastic replicas and trans-
mission electron microscopes (TEM) were used, 3
but nowadays the scanning electron microscope
(SEM) is the most widely used instrument? 6 The
SEM offers a unique combination of qualities such
as high spatial resolution, high image contrast
between different structure constituents and the
62 Anders Nordgren

possibility of chemical characterization through the SEM instruments equipped with efficient BSE
detection of emitted characteristic X-rays. In ad- detectors.
dition, the photo-emission electron microscope Due to the rapid developments in semiconductor
(PhEEM) should be mentioned. PhEEM gives high technology, the performance of modern software
material contrast and a true surface image of the oriented image analyzers has increased tremen-
specimen due to negligible penetration of the ultra- dously during the last decade. 1°'11 However,
violet light emitting electrons from the specimen although very advanced image analysis systems
surface. 7'8 PhEEM is, however, not a routine have been available for several years the semi-
technique to the same extent as SEM. automatic procedures still play an important role in
Image formation in SEM is possible utilizing structure analysis of cemented carbide. The main
different modes of electron detection. Most suitable reasons are the very high demands on image
for quantitative geometrical characterization of contrast and structure definition in order to permit
planar cross sections are the back scattered electrons a fully automatic and reliable object detection of,
(BSEs). These are high energetic electrons leaving e.g. grain boundaries, and thereby take full ad-
the specimen surface with energies relatively close vantage of the advanced analyzers with their high
to the incident electron energy. The BSE intensity is speed of analysis and possibilities to accumulate
characterized by a strong material or atomic large data volumes and thus improving the stat-
number contrast. BSE contrast is discussed further istical quality of the results. The developments in
in the present work. The incident electrons in SEM the more hardware oriented fields of microscopy
penetrate into the specimen surface and the image is and specimen preparation have not been quite that
thereby representative for a surface volume rather dramatic as for the image analyzers.
than being a true surface image. The electron However, both high performance microscopy
penetration depends on the energy of the incoming and careful specimen preparation are of vital
electrons and on the specimen properties. The importance in the quantitative metallography of
limitations in lateral and depth resolution of BSE in hard metals.
SEM when working at high accelerating voltages The aim of the present research was to investigate
(20-35 kV) have been pointed out. r However, the the possibilities to apply modern SEM based
electron penetration can be decreased to very low automatic image analysis to the microstructural
values by working at low accelerating voltages. The characterization of cemented carbides. The ap-
lateral resolution in BSE mode when imaging proach has been a combination of
tungsten carbides (WC) at 6 kV accelerating voltage
can be estimated to better than 0-05/zm, 9 a value --optimized specimen preparation techniques in
considerably lower than the carbide grain size in order to maximize image contrast and structure
most commercial cemented carbide grades. Hence, definition;
suitable SEM conditions for stereologcial analysis --high resolution SEM utilizing low accelerating
of hard metal are BSE detection and low acceler- voltage and high efficient BSE detection; and
ating voltage. It should be emphasized that these - - a combination of favourable BSE contrast
demands are generally only fulfilled in modern modes and image processing in the image

Table 1. N o m i n a l chemical c o m p o s i t i o n a n d c a r b i d e g r a i n size ( g r a d e d a t a a c c o r d i n g to S a n d v i k C o r o m a n t A B a n d Seco T o o l s AB,

Sweden)

WC TiC ( TaNb)C Co Grain size

Grade (% vol.) (% vol.) (% vol.) (% vol.) (~m)

WC-Co grades
31C 69 -- -- 31 3
18C 82 -- -- 18 3"5
18F 82 -- -- 18 1"9
10F1 90 -- -- 10 2"4
10F2 90 -- -- 10 2

W C 7-Co grades
7C 49'5 27'5 11 12 2-3
7F 57 11 17"5 14.5 1-2
 Microstructural characterization of cemented carbides
Fig. 1. Microstructure of the WC-Co grades.
analyzer in order to automatically detect
objects and evaluate structural parameters.
A wide range of cemented carbide micro-
structures have been investigated. The efforts have
g li R M I0
63
Fig. 2. Microstructure of the WC-7-Co grades (WC, white ; 7'-
phase, gray; Co, black).
been concentrated on developing metallographic
techniques rather than obtaining high statistical
accuracy. Most of the quantitative microstructural
information available in the literature has been
evaluated for W C - C o grades. Quantitative data for
the cubic phase (y-phase) present in steel cutting
grades are very rare. A prime objective was thus to
develop metallographic techniques for revealing the
grain boundary network of y-phase.
2 CEMENTED CARBIDES
Two different categories of cemented carbide were
investigated: W C - C o and WC 7' Co grades. The
materials represented a wide range in chemical
composition and grain size.
Nominal chemical composition and carbide grain
size for the investigated materials are given in Table
1 and overview SEM micrographs are shown in
Figs 1 and 2. Five different WC Co grades were
investigated, with a nominal binder content of
10-31 v / o and nominal carbide grain size in the
range of 1.9-3.5/tm. Two coarse grained W C - C o
alloys were studied: grade 31C and 18C. The figure
in the grade label refers to the nominal Co fraction
while C and F indicate a coarse and a fine grained
material respectively. Grade 18C appears from the
micrographs to be considerably more coarse grained
than 31C. The frequency of fine carbides ( < 2/~m)
is higher in 31C. Three fine grained alloys were
studied: 18F, 10F1 and 10F2. Grade 18F and 10F1
appears to be rather close in grain size distribution,
64 Anders Nordgren

while grade 10F2 contains a lower frequency of 3.1 Z contrast

coarse carbides > 5/~m.
The second group of cemented carbides contains
a 7-phase, i.e. an additional carbide phase with a
cubic crystal structure. The main constituents in the
y-phase are usually TiC, TaC and NbC. The
composition of the y-phase of the materials in this
work varies considerably due to different nominal
compositions, but also due to a different degree of
dissolution of WC into the ~,-phase. A consequence
was that the etching response of the y-phase varied
between different alloys. Hence, the etching of the 7-
phase had to be adapted for each specific grade.
Two homogeneous WC-7-Co grades--one fine
grained (TF) and one coarse grained (yC)-- were
studied. Grade 7C contains a relatively high
nominal volume of TiC while 7F is rich in (Ta,
Nb)C. The two phase structure of the coarse 7
grains in grade 7C (Fig. 2) is due to the inward
diffusion of W, Ta and Nb towards a TiC rich core.
Both carbide populations WC and 7 are coarser in
7C compared to yF. 7F contains a higher volume
fraction of WC in the sintered state. It is apparent
that the 7 grains in both grades have a much more
rounded shape than the prismatic WC grains.
Hence, the seven grades represent an increasing
degree of complexity from the relatively simple
coarse grained, high-Co W C - C o grades to the fine
grained WC-7-Co alloy 7F. For each category of
hard metal, specimen preparation and etching
techniques were developed, conditions for high
resolution imaging of fine structure constituents in
SEM were defined and procedures for automatic
object detection and parameter evaluation were
determined.
3 ATOMIC NUMBER (Z) AND
CHANNELLING CONTRAST IN SEM
The SEM is necessary in order to image fine carbide
grains and thin binder ligaments, thus enabling
In the case of Z contrast, the intensity of the back
scattered electrons increases with increasing atomic
number, i.e. the back scatter power for WC is
higher than for Co due to higher mean atomic
number, Zwc = 70 and Zoo = 27. Thus, WC appears
brighter than Co in the micrograph. The mean
atomic number for the ~,-phase varies with chemical
composition but generally the y-phase gray level is
somewhere in between the WC and Co levels. By
expanding the contrast and adjusting the black level
it is possible to obtain a white WC, grey y-phase and
black Co on the micrographs. Furthermore, the
phases often have a well defined composition and
structure and the intensity is therefore practically
constant within each phase, a fact of great value in
image analysis.
Detection of back scattered electrons is also
attractive due to the low contribution from topo-
graphic effects to the image contrast. Small devia-
tions from a perfect planar section is allowed
without drastic changes in contrast. The grooves in
an etched grain boundary network represent a
topographic variation in the surface. The absorp-
tion of incoming primary electrons is higher in the
grain boundary grooves and the BSE intensity is
thus lower. Grain boundary grooves appear darker
than the grains. Figure 3 shows schematically BSE
contrast due to different mean atomic numbers and
due to grain boundary grooves.
3.2 Channelling contrast
The channelling contrast can be qualitatively ex-
plained as different electron absorption for different
ATOMICNUMBERCONTRASTAT HIGH ACCELERATINGVOLTAGE
I=
Line
Incident I scan
etectrons I Backscctftered
J. / etectrons

~
Etched •
parameter evaluation of the main part of the qmin boundary I I Unetd)ed Co Polishedsurface
X . . . . . . . . . . . . . . . . .
microstructure. The resolution limit due to the finite Efched groin surface
depth of electron penetration can be decreased to
low values by working at a low accelerating voltage. BSE
intensif,
Especially, the detection of high energetic, back
scattered electrons offers useful possibilities. Con- vhife WC
trast in BSE mode is due to different mechanisms.
c ~ phase ~ ~ " y
Two different mechanisms were utilized in the
present work, atomic number (Z) contrast and
channelling contrast. Co boundaries Co
Fig. 3. Schematic view of atomic number (Z) contrast in an
etched WC 7~Co grade.
 Microstructural characterization of cemented carbides 65

MIXTURE OF CHANNELLING CONTRAST AND ATOMIC Table 2. SEM conditions

NUMBER CONTRAST AT LOW ACCELERATING VOLTAGE

Accelerating voltage
Line scan
) ~tched specimens for grain size 6kVand 12kV
measurements
Incident
e{ecfpons
II ,
I
I t Bocksco.ffered --polished specimensfor volume 6 kV
fraction measurements
x
ti
] [
t / '""
[ I
y
Y_
....
4.,.~.Specimen
Beam current 2 nA
Electron detection BSE
Working distance 9 mm
Tilt angle 0°

BSE pendence on accelerating voltage is shown in Fig. 5

infensi~
for etched surfaces of grade 18C and 10F2. At a
whlte
high voltage (12 kV) the intensity is approximately
equal for all WC grains. Image contrast is due to the
black y difference in Z between Co (black) and WC (bright)
Dark WC grain Bright WC gram with an increased absorption in the grain boundary
due t~ electron
channelling mong grooves (dark). At a low voltage (6 kV) the gray
crystal planes

Fig. 4. Schematic view of channelling contrast in a WC-Co
grade.
18C 12kV
Fig. 5. Different contrast for low and high accelerating volt-
age. High (12 kV) mainly Z contrast; low (6 kV)--mixture
of Z and channelling contrast.
grain orientations. The phenomenon is schematic-
ally shown in Fig. 4. The BSE intensity is low for
grains with high electron absorption and such
grains appear dark on the micrograph. Thus, even
though the mean atomic number is equal for all
grains, contrast can be obtained between different
grains. The channelling contrast depends on chemi-
cal composition, SEM conditions and specimen
surface conditions.
The channelling contrast increases with increas-
ing atomic number and is relatively strong for WC
but generally unsignificant for the 7-phase. Fur-
thermore, the channelling contrast increases with
decreasing accelerating voltage in SEM. The de-
level of the individual WC grains varies from dark
to bright. Image contrast is a mixture of Z contrast
and channelling contrast. The change in image
IOF2 contrast with accelerating voltage can be taken
advantage of in image analysis for automatic
detection of the complete grain boundary network.
Grain boundaries which have not been etched and
thus appear without contrast at a high accelerating
voltage (12 kV) can often be identified in the 6 kV
image, due to differences in gray level between the
adjacent grains. Thus, by combining the two types
of images, a more complete network can be
detected. It should be emphasized that due to low
channelling contrast for the y-phase the detection of
boundaries between 7 grains is dependent on the
etching of the grain boundaries.
Finally, the surface conditions are of major
importance for the channelling contrast. A dis-
tortion of the grain surface, e.g. by careless specimen
preparation, will completely mask the channelling
contrast. Thus, the preparation of a planar section
without distortion in the outermost surface layer is
an irremissible demand for channelling contrast at
low accelerating voltage in SEM.
The cemented carbide surfaces were examined in
a SEM JEOL 6400. Electron optical and geo-
metrical conditions are given in Table 2. An
important feature of the SEM is a high performance
BSE detector with high atomic number resolution.
4 S P E C I M E N P R E P A R A T I O N FOR CARBIDE
GRAIN SIZE M E A S U R E M E N T S
The mechanical polishing and subsequent etching
of the carbide grains is probably the most important
8-2
66 Anders Nordgren
single step in the automatic measurement of carbide
grain size in cemented carbide. There are three
major and somewhat contradictory demands on the
specimen surface.
(1) A surface practically free from grinding and
polishing marks and free from distortion due
to deformation in the outermost layer of the
grains during polishing.
(2) Revealed grain boundary network, of special
importance when detecting the 7-phase grain
boundaries.
(3) Minimum in surface topography and de-
viation from a planar cross section.
Polishing marks appear as randomly orientated
straight lines across the field of view. Such lines will
be detected in the automatic image analysis and
linked into the grain boundary network, thus
creating artificial grains. However, even if the
surface is free from such a line pattern from the
mechanical polishing, there will still be a thin layer
of disturbed material in the grain surface due to the
action of the diamond abrasive in the polishing
cloth. Such a disturbed layer has to be removed in
order to obtain maximum contrast between dif-
ferent carbide grains. This is achieved by a very
light etching of the carbides.
Secondly, etching of the carbide phase is generally
necessary in order to reveal the grain boundaries,
which in most cases are attacked more rapidly than
the grain surfaces. Hence, with increasing time of
etching, the amount of disturbed material in the
grain surface decreases and the grain boundary
attack increases. These desirable effects are counter-
acted by the increase in surface topography. The
Table 3. Scheme for mechanical polishing
Step 1: Grinding
Fine grinding with diamond grinding disc
Step 2: Alternating mechanical polishing and deep etch of carbide phases
Polishing Cloth
(1) Coarse Pellon PAN-W
(2) Medium Pellon PAN-W
(3) Fine LAMPLAN 410
(4) Deep etch in 20 % Murakami
(5) Repeat step 2~4 one or two times with decreasing time of deep etch
(e.g. 1 min, 30 s)
Step 3: Final polishing
(1) Fine LAMPLAN 410
(2) Fine LAMPLAN 410
Struers DP suspension.
measurements should, if possible, be made on a
perfectly planar section through the material.
Increased surface topography due to prolonged
etching will not only result in errors in apparent
grain size but, in addition, the definition and
contrast in the microstructure will be lost and it will
not be possible to apply an automatic measuring
procedure.
Hence, the etching of the carbide phases will in
practice be a compromise between, on one hand,
the removal of a disturbed surface layer and the
preferential etching attack on the grain boundary
network and, on the other hand, the demand on
insignificant surface topography.
Methods used in the present work for polishing
and etching of the carbide phases in the different
grades are given in Tables 3-6. The conditions
should be considered as guide values in further
work, especially when etching WC-7-Co grades,
where the chemical composition of the actual grade
determines the etching response.
The chemical etching (Murakami) of WC in the
WC-Co grades can be replaced by electrolytic
etching (Table 6). However, the Murakami reagent
cannot be used for WC-y-Co alloys due to rapid
attack on the y-phase. A constant current source
(galvanostat) and a Pt cathode were used in the
electrolytic etching. The current density should be
kept very low in order to reduce the oxidation of the
surface with accompanying loss in SEM resolution.
Etching of grade 7F was made as a two-step
electrolytic etching where the ),-phase was etched
before the WC (Table 6). If the WC is etched in step
1, before the 7-phase, the 7-phase will be passivated
and not affected during etching in step 2. When the
Abrasive a Time (approx.)
15/lm diamond 4 min
6/~m diamond 4 min
3/~m diamond 2 3 min
4 rain
3/zm diamond 2 min
1/zm diamond 2 min
 Microstructural characterization of cemented carbides 67

Table 4. Reagents for etching of carbide phases

Reagent Application

(1)" 20% Murakami Deep etching during surface

20 % NaOH in water fresh solutions mixed in equal preparation (all grades)
20 % K a [Fe(CN6)] in water proportions at time of etching
Chemical etching Etching of WC in the W C - C o grades
(2) ~' 10 % Na2CO.a in water Etching of WC in W C - 7 - C o grades
Electrolytic etching
(3) a 100 g Na2CO a
50 g NaOH mixed in water to 1000 ml solution Etching of 7-phase in grade ),F
50 g KNaCaHaO~. 4H~O
Electrolytic etching
(4) 50 Na2CO a Simultaneous etching of 7'- phase
25 NaOH mixed in water to 1000 ml solution and WC in grade yC
25 KNaC4H40,.4H20
Electrolytic etching

" Reagents according to Seco Tools AB and Sandvik Coromant AB, Sweden.

Table 5. Chemical etching of WC Co grades before grain size

measurements

Etching
Grades reagent Etching procedure

A I I W C Co no. l Immersion of specimen in room

grades temperature solution for 30 s

Table 6. Electrolytic etching of WC-?,-Co grades before grain

size measurement topography

Current
Etching density Time
Grade reagent (mA/cm 2) (s)

Step 1 ." Etching of ?,-phase

7C 4 15 30
?'F 3 15 5

Step 2. Etching o.f WC

?'C (Simultaneous etching of WC and 7-phase)
,,F 2 15 10
BSE-12kV

two-step procedure was applied to grade ?C, the

binder contrast at low accelerating voltage in SEM
was drastically decreased (Fig. 6). By etching grade
yC in a diluted y etch reagent (no. 4 in Table 4), both
carbide phases WC and y were etched simul-
taneously, without loss in binder contrast. However,
this last procedure could not be applied to yF due to
unfavourable etch attack on the y-phase. These
observations during the experimental work empha-
size the strong influence of carbide phase chemistry BSE-6kV
and surface conditions on the etching response. Fig. 6. Loss in Co contrast at low accelerating voltage due to
The y etch reagents (Table 4) are water solutions unfavourable carbide etching.
68 Anders Nordgren

Reference
-- fine

Microsh~c ture ]
! I of wc-~-c0 I
.;:. ; .. (, ?.. Iwc-

:'.~-"./..::')~ i .4~-.-.:.'..v..~!:i

Linear intercept chord lengths: IWC, t T, lCo

Equivalent circle diameters: dWC, d 7
4 ~/m
d ~ (--~--A)
A = apparent a r e a of an individual grain.
Carbide contiguity C
carbide/binder boundaries WC/Co, T/CO
c a r b l d e / c a r b l d e botundaries WC/WC, WC/T, T/T
Fig. 7. Etched surface of a WC-7-Co grade before grain size Area (volUme) fractions VWC, V 7, VCo
measurement.
Fig. 8. Structural parameters for cemented carbides.

of three components: Na2CO 3 (sodium carbonate),

NaOH (sodium hydroxide) and KNaC4H406 . 4H~O
(potassium sodium tartrate). Out of these three the
active component in the etch attack on the 7-phase
is NaOH. In general the etching effect of reagent no.
3 is relatively independent of variations in the
relative amounts of Na2CQ, N a O H and
KNaC4H4Q.4H20. Figure 7 shows the surface
topography, channelling contrast for WC and
etched ~,-phase grain boundaries on a specimen
surface of a WC-y-Co grade, prepared according to
the procedures in Tables 3 and 6.
5 STRUCTURAL PARAMETERS
Quantitative characterization of cemented carbide
microstructure usually involves the measurement of
(i) carbide grain size distributions and mean
carbide size,
(ii) carbide contiguity,
(iii) binder width distributions and binder mean
free path,
(iv) volume fractions.
5.1 Carbide grain size
microscopy and image analysis point of view,
especially for materials with both WC and ?-phase
and for fine grained materials.
The problems in revealing the complete grain
boundary network make it difficult to take full
advantage of advanced, automatic systems. Thus,
grain size in cemented carbide is usually determined
by semi-automatic analysis using intercept chord
length measurements (Fig. 8), i.e. the intersections
of a reference line grid by the grain boundaries are
manually marked by the operator. Intercept length
is not considered as an object specific parameter.
Manual marking of intercept length is not de-
pendent on the complete network being visible.
Small gaps in the network can be accepted.
5.2 Carbide contiguity
Carbide contiguity is defined a as the ratio of
carbide/carbide interface area to the total phase
boundary area carbide/carbide and carbide/binder
in the specimen volume, i.e.
C= Sc,~b/c~rb (1)
Scarb/car b -~ Searb/bin d

Basically a number of parameters are available as
measures of carbide grain size in planar sections
through the material, e.g. grain area or the
corresponding equivalent circle diameter (Fig. 8).
These parameters are object specific. In order to
evaluate them, every single grain has to be detected
and the complete grain boundary network has to be
outlined. This demand represents a considerable
challenge from a specimen preparation, electron
where S is the interface area per unit volume of the
different types.
The contiguity is thus a measure of the degree of
contact between the carbide grains. The contiguity
can be evaluated on planar, two-dimensional sec-
tions 1 using the following relationship
2Nca~b/°arb (2)
CN = Ncarb/bind Aft 2Nearb/car b
 Microstructural characterization o f cemented carbides 69

where Nearb/ear b and Ne,~b/b,n d are the number of Reference

ine
carbide/carbide and carbide/binder boundaries per
unit length of reference line, respectively.
In semi-automatic analysis the different types of
boundaries are marked during tracking of a
reference line grid projected on the structure image.
However, the procedure has to be modified in order
to evaluate the same quantity using an automatic
Step 1: Measuremen~ of Ncarb/blndon polished
system. cross sections by deEectlon of the
binder pools.
Alternatively, the contiguity can be evaluated
Measured qua/z~ity nbind=Ncarb/bind.
using mean values on carbide size and binder
width,' i.e. Reference
line

/ ~ Vb"~"e" (3) :;..'..:-: [ -..[.."

C a -- 1 /bin,ler V e a r b i d e
where

/carbide is the mean intercept carbide size,

/binder is the mean free path of binder,
V~.,rb~d~, V~,,~,~e,.are the volume fractions of the Step 2: Measurement of (Ncarb/bind* 2Ncarb/carh)
on etched sections by detection of the
different phases (V~,~b,,e = 1 - Vbi,de,.). carbide ~rains.
Measured qu~untity ncarb = Ncarb/bind ÷ 2Ncarb/car b
The relationship can be derived from basic
2 Ncarb/car b ncarb - nbind
stereological considerations) Equation (3) shows cN = Ncarb/bind ÷ 2Ncarb/car b ncarb
the interrelationship between the basic structural
Fig. 9. Two-step procedure for measurement of contiguity C~
parameters. Three parameter values are thus suf- using automatic image analysis.
ficient to fully characterize the microstructure.

5.3 Contiguity by automatic methods
A two-step procedure was developed for evaluation
of the contiguity C x using automatic systems where
the different types of phase boundaries are not
directly marked by an operator. The procedure is
based on intercept length measurements of the
binder and the carbide phases. A similar procedure
was used by Werlefors and Eskilsson?
S t e p 1: Measurement of Ncarbide/bin(le r o n
polished, planar sections by detection of the
binder pools.
//bind = Nearb/bin d
- - S t e p 2 . Measurement of (N,..~,.~,/~,,nd+ 2No=rb/e.,~b )
on etched sections by detection of the carbide
grains
n,.~,.,, = N~,.~,.b/i,md+ 2N~,v/,.a,, h
where n(,a,.~,and n~,,,,d are the measured numbers of
boundary intersections per unit length of ref-
erence line. The number of intersections is equal
to twice the number of intercept chords.
The two steps are schematically shown in Fig. 9.
The value of 2N,,.~,.b/c~,.b can be calculated from the
two measured quantities.
2N(~,b/c~, , = n , ~ , , - - n,,i,,~, (6)
Hence, the contiguity Cx can be determined by
insertion into eqn (2)
Cx- = 2N"a"b/"a"" -- nea"b- - rtmnd (7)
" N,,.~,.~,/~,,,d+ 2N,,,,.~,/,.a,.b n,,..m,
n,,~rb and n,,i,,, ~ are evaluated as field specific mean
values of several fields of view. The two-step
measurement does not have to be made on the same
specimen area because n,:a,,b and n~>~nd are not related
(4) to specific carbide grains.
5.4 Binder width
For low binder fractions it is possible to detect
(5) binder pools as individual objects on polished cross
sections and thus to evaluate object specific para-
meters, e.g. binder pool areas. However, at high
binder fractions the binder appears as a more or less
continuous phase with few individual binder pools.
This was the case for grades 31C, 18C and 18F.
Hence, intercept chord lengths were determined for
70 Anders Nordgren
Table 7. Evaluated parameters
Parameters Symbols
Carbide grain size
Frequency size distributions and mean
values for the
----equivalent carbide diameter dwc, dy
d = (4/n. A)'~
where A is the apparent grain area
----carbide intercept chord lengths lwc, ly
Contiguity
--according to Section 5.3 C~
--according to eqn (3) Cj
Binder width
Frequency size distributions and mean /co
values (mean free path) for binder
intercept chord length
Volume fractions Vwc, V~, Vco
the binder throughout the measurements, for all
grades. The parameters evaluated in this work are
given in Table 7.
6 AUTOMATIC IMAGE ANALYSIS
An automatic image analysis system (IBAS 2,
Kontron GmbH) was utilized in the measurements.
The system is software oriented with extensive
possibilities for different types of image processing
on digital image information and offers a large set
of different parameters. SEM micrographs were fed
into the image analyzer via a TV scanner. In such a
set-up, contrast is reduced and the noise level of the
image increases during image transfer, from the
scanned surface in SEM via photographic material
and TV scanner, to the digital storage in image
memory. The ideal link is an SEM directly interfaced
to the image analyzer so that the detector signal can
be directly stored in digital image memories, or by
a equivalent set up where digital image data are
transferred without conversions to analog signals.
Hence, possibilities exist for further improvements
of image quality and results of measurements as
compared to the results in the present work.
The major steps in the image analysis sequence
for carbide grain size measurement of a WC-7-Co
alloy are shown in Fig. 10a.
--Image input. In the first step both images are
stored in the digital image memory; the 6 kV
image with a significant contribution of chan-
nelling contrast in the WC phase, and the
12 kV image mainly carrying Z-contrast.
--Phase images. Gray level discrimination in the
12 kV image is used to separate the WC, 7 and
Co areas in the field of view. The phase images
are stored in separate memories. Discrimi-
nation errors due to the finite resolution of the
SEM and the TV scanner (halo effect) are
eliminated by image processing.
--Grain boundary detection. The grain boundary
network is detected using a high pass gradient
filter, i.e. an enhancement routine sensitive to
changes in gray level. Such an operation is
performed on both images and the result is
combined by image addition. The gradient
filter registers differences in gray level between
different grains (WC-WC in 6 kV image and
WC-7 in 12 kV image) and between the dark,
etched grain boundary network and the back-
ground. Hence, in the combined image the
major part of the network will appear with
only small segments missing.
--Automatic linking. An automatic routine for
reconstruction of the network, based on the
dilation of free unconnected ends, operates on
the combined image, linking free ends together.
--Manual editing. Defects in the network re-
maining after the automatic linking are manu-
ally corrected for. A cursor and a digitizer
tablet are used for the tracking of grain
boundaries.
--Grain type separation. The gradient filter does
not distinguish between different types of phase
boundaries or grains. Therefore, WC and y
grains are separated from the total grain
population using image subtraction where the
phase images are used as masks.
--Parameter evaluation. Object specific data for
the individual grain surfaces and intercept
distributions are evaluated for all carbides
(WC+7) as well as for the separate carbide
types.
7 WC-Co GRADES
7.1 Carbide grain size distributions
Measured frequency size distributions for WC in
the investigated WC-Co alloys are shown in Fig.
11. Equivalent circle diameter (dwc) and intercept
chord length (/we) are used as a measure of carbide
grain size. Carbide frequencies are normalized with
respect to the total number of detected carbide
grains or chords. Mean values dwc and lwc are given
in Table 8.
The mean carbide size is largest for grade 18C
where dwc = 1-90 Ftm compared to 1.34/tm for the
 Microstructural characterization of cemented carbides 71

(a) (b) A. Grey level images (image input)

A. Imag___~e
inp___~ut T

Im~age i Image 2 ]
]12 kV BSE 6 kV BSE |
~Zcontrast Channelling+|
Z contrast |

IB. Grey level discrimination I

Phas----~imag------Ts-o~
WC--~~ an--~Co 12 kV 6 kV
from Image 1
B. B ~ phase images after grey level discriminationof the 12 kV Linage
C. Grain boundary detection[[

ofGradlentimage[iltering [Gradient 2filtering

of image

1 Image I WC T phase
-~I addition I ' boundaries

C. Detectedgrainboundaries D. All grains after aurmmatic E. All grainsaftermanual

after gradient filtering grain boundary reconstruction editing of boundary network
D. Automatic grain boundary
reconstruction

E. Manual editing of network

F. Grain type separation ~f ~

[G. Parameterevaluation ]
F. Graintype separation

WC c~ralns T phasegrains

Fig. 10. (a) Flow diagram of grain size measurement in WC-?-Co grades using automatic image analysis; (b) Binary images during
image analysis of a WC 7-Co grade.

second coarse grained material 31C. The size
distribution for these two grades are relatively
broad, especially for 18C. Distributions and dwc
values for the three fine grained alloys are rather
similar, grade 18F (1.09~m) and 10F1 (1"13/lm)
being somewhat coarser than grade 10F2 (0.95 ~m).
The results of the measurements correspond fully
to the visual impression of the microstructures
in Figs 1 and 11. When comparing the mean
values of carbide chord length lwc, the different
grades are not as well separated from each other as
for dwc. Hence, if small differences in size dis-
tributions are investigated, the equivalent diameter
is probably a more sensitive measure of carbide
grain size.
The high fraction of short chords < 0.5/~m is due
to the random sectioning of the detected carbide
surfaces by the reference line grid. The carbide
grains are only occasionally intersected by the
reference lines at positions corresponding to maxi-
mum possible chord length. Instead a large number
of shorter chords are generated and the mean chord
length lwc therefore becomes lower than the mean
equivalent diameter (Table 8). Chord length data
72 Anders Nordgren

~b $ I 217groinsI t~ t" I. Ell chords

'~ ~ot r.c I td-,-'.~ PmI 30 t~,..I,i' Ilwc=1.~ pm

10

EQUIVALENTOlAM.d~c(pm) INTERCEPTLF-Nb"IHIv,,clpm)

~ F 22~ chords
Ir~ =1.~~ I
+t , +<'==[ 3° I ,I. I

I 2 3 ~, 5
t~ll.,m)

i
+ FI '°++°'
,,0,..1[

1 2 3 ~. 5
d,,t::(Nm) lwclPm)
';4) I
~ot- J-] 3~ gm,ns ~].~ I]we =O~pm

2o i
EQUIVALENT DIAM c~Im.~) INTERCEPT LENGTH L,~llJml

~oL ~' t.57 chon:Is

D-I I'f~ =O.~,r.
2O
10 10
~ g
dwclpm). I<,~:(pm)

Fig. 11. Frequency grain size distributions for WC in the WC~::o grades.

have to be evaluated when calculating the contiguity

of the carbide phase. Grade dQfa
".".:.,...
" dwclrneasurecl)
The nominal grain size values are based on lw~imeosurecl)
planimetric measurements using LOM. The large 3
/
difference between nominal and measured values /
/
(Fig. 12) mainly reflects a difference in resolution I
between different methods of measurement. The t 7
I I
i I
_z 2
i
Table 8. Measured mean carbide size (dwc, /wc) and nominal / 7 /
/ / /
values according to manufacturers grade data for the WC-Co / / /
/ N f /
grades / /
/ / /
/
dw(~ /we Nominal(pm) / '4 / /
/ \
Grade (ktm) (Itm) / \ / /
/ \
/ \
31C 1"34 1"16 3 1 \ i// /
/
18C 1'90 1'71 3"5 / / /
/ i/ /
18F 1"09 0"96 1"9 31..~c 18c 18~ IOF~ 10F~2
10FI 1.13 0-97 2-4
10F2 0"95 0"87 2 Fig. 12. Comparison of different measures of mean WC grain
size.
 Microstructural characterization of cemented carbides 73

nominal values are based on detection of relatively Table 9. Mean free path leo of the Co binder in the WC Co
coarse carbides, while the values from the SEM alloys
based analysis in the present work also includes
1('o
very small carbides. However, although the differ- Grade (/am)
ence in mean carbide size is considerable between
nominal and measured values, the ranking of the 31C 0-99
materials is the same, the only divergence being that 18C 0"68
18F 0"43
grade 10F2 is even more fine grained than expected 10FI 0"27
from the nominal values. 10F2 0"27

7.2 Binder width distribution

The dimensions of the binder pools were measured A 1.0 Coarse /= 31C
5 g i.,d we-co / --
using linear intercept chord lengths. Distributions
and mean chord length data for the W C - C o alloys ,2 /
are shown in Fig. 13 and Table 9. As can be =. /
/ Fine grolnecl
~0b 13zocho~l z 05 / / WC-Co
d~- 30~ ' tc==0'99proI ~SF

z //.., 10F_2,I0F.__!
= I
1
,
z
INTERCEPTLEN611t[eolp~)
i •i8 • /I"
/
I I I
10 20 30
BINDER VOLUME FRACTION Vco(%)
Fig. 14. Binder mean free path as a function of binder fraction
lO and W C grain size.

tco(Pml expected the mean free path lwc through the binder
II.~,~ chon:ls decreases with decreasing binder fraction. The
~F *
influence of WC grain size on lco is shown by
oF'LI comparing the coarse grained 18C with the fine
grained 18F. The /co value for 18F is only
lO
approximately 60 % of the value for 18C (Fig. 14).
tcolpm)
The fine carbide population in 18F can be imagined
{%) 10F1 as occupying the large binder pools between coarse
.,- 50J-I 1.204.chords WC grains and thus decreasing the free path
through the binder. The values in Fig. 14 show

~2ol-
,oil
I
good agreement with data of Roebuck and Bennet 5
and of Sigl and Fischmeister. 6
L
7.3 Volume fractions
INTERCEPT LENGTH [co(pro)
(%
The volume fraction of Co was measured on
50 1~ chords
Ico:O.27pm polished sections imaged in SEM at a low acceler-
t,.O
ating voltage (6 kV). The result is shown in Table 10
where the measured values are compared with the
1o
nominal binder content. The agreement is fully
1 /- acceptable over the whole range of Co contents.
tCo(Pm) Due to the high contrast between WC and Co in
Fig. 13. Binder intercept chord length distributions for the SEM, the detection of the phase boundaries can be
W C - C o grades. made with high accuracy. The introduction of an
74 Anders Nordgren

Table 10. Volume fractions of binder phase in the W C - C o Table 12. Contiguity C~ for the WC-Co alloys based on
alloys (measured values according to image analysis compared measured values of mean carbide size, binder mean free path
with nominal values) and volume fraction

Nominal V Image analysis /we /Co

Grade (%) (%) Grade (,urn) (llm) Go Vwc C,

31C 31 30.0+2.3 31C 1-157 0"986 0'300 0"700 0'50

18C 18 16.7+ 1.0 18C 1'708 0"676 0'167 0-833 0'49
18F 18 17.2_+ 1.5 18F 0"963 0-434 0"172 0"828 0"54
10F1 10 10.2+0.5 10F1 0'968 0"266 0"102 0'898 0"58
10F2 10 9.3_+0.5 10F2 0"871 0"270 0"093 0"907 0'67

additional carbide phase, as in the WC-7-Co
grades, increases the demands on noise free, high
quality imaging of the specimen surface.
7.4 Carbide contiguity
The contiguity of the carbide skeleton was de-
termined according to the procedures discussed in
Section 5, i.e. in the first case based on the
measurement of the frequency of different types of
phase boundaries (Nwc/co, Nwc/we) and in the
second case utilizing the measured mean chord
lengths/co and/we and the volume fractions Vco and
Vwc
2Nwc/wc
C~ = Nwc/co + 2Nwc/w c
c, iwc l/co
= ]
The results of the calculations are given in Tables
11 and 12. The contiguity C N varies from approxi-
mately 0.45 in coarse grained, high Co alloys to 0.59
in grade 10F2. Comparison of C s for grade 18C
and 18F indicates that the contiguity increases with
decreasing carbide grain size. Furthermore, the
coarse grained alloy 18C has approximately the
same contiguity as for grade 30C, even though the
binder fraction in the latter case is considerably
Table 11. Contiguity C N for the W C - C o alloys based on the
higher. The fine WC grain populations can be
imagined as acting as a filler in the binder and thus
connecting larger WC grains and increasing the
contiguity. The results indicate that the fine WC
carbide populations are of importance in obtaining
a high contiguity.
In the correlation diagram in Fig. 15, it is shown
that the C~ values are 5-10% higher than the C N
values. However, the ranking of the WC-Co grades
is the same and both procedures can be considered
as giving an equivalent result.
In Fig. 16 measured C~ values for the WC-Co
grades are compared with data of Roebuck and
Bennet 5 and of Exner. 1~ Roebuck and Bennet
studied a range of WC-Co alloys using SEM,
(2) Murakami etched specimens and semi-automatic
image analysis. Their materials, B, D and Q, are
compared with 10F1, 18F and 31C in Table 13. The
(3) measured contiguity shows good agreement for
comparable binder widths and carbide grain sizes.
The expected higher contiguity in Q compared to
31C due to the lower binder content is counteracted
by the coarser carbides in Q.
lOFle/
,dl, os 31C 9 , ~

- /
I

detection of different types of phase boundaries

Nwc/co +
2Nwc/wc Nwc/co 2Nwc/wc
Grade (urn-l) (ltm-1) (,am -1) CN
I I
31C 1"113 0'613 0-500 0'45 0.5 1.0
18C 0'910 0-514 0"396 0.44 C = 2 Nwctwc
18F 1-576 0"767 0"809 0"51 N 2 Nwetwc + Nwc/co
10F1 1-698 0'782 0"916 0-54
10F2 1"856 0'759 1"097 0-59 Fig. 15. Comparison of carbide contiguity C N and C~ accord-
ing to eqns (2) and (3), respectively.
 Microstructural characterization o f c e m e n t e d carbides 75

(a)
1.0 V/C-Co: Exner ref (12)
' B, O,g :Roebuck and Benneff ref ( 5 )
• Aufomatic
O Limif~l ~ifing
x Full corl~ction
0.8 1o0
~ 20
>..-

0.6 10F.~.22~
EQUIVALENTDIAH.d~c(pm)
Z
10F1 (%1
E 50
,31C Limited 126 ~r~ins ~6 30
y dLf!n3.
I- m \ o(2
,¢ z
~.d

lO
0.2 WC- Co
IO
c~(~m)
(%
I I I I
0 10 20 30 .----~'---]12~, grains
BINDER VOLUME FRACTION Vco (%) 30

Fig. 16. C a r b i d e c o n t i g u i t y C~ for the W C - C o grades.

10

Table 13. Comparison with data of Roebuck and Benner ~ 2 3 ~* 5 2 3 L, 5

dwe(Pm) dv~z(IJm)

Mean Binder mean Binder

carbide size ./~ee path Jbaction Contiguity (b)
Grade /~,, (~am) l~. (/am) V~,o Cx !O/o~_...

10F2 0"87 0"27 0"102 0"59 ~oF

B" 0"88 0"22 0"099 0"66
18F 0"96 0'43 0" 172 0'51
D" 1"00 0"42 0-165 0"53 ~_ 2oFI
31C 1"16 0"99 0"300 0"45
Qo 1"25 0"71 0'255 0"41
2 3 ~, 5
EQUIVALENT OlAM dwe(iJm)
" F r o m Ref. 5. (%), =o
501- Limif~l l
I e_~_~_n~ I WC
~0F ~ . 1_3t.2grains

The contiguity for the three fine grained alloys

ollt: z

c~

18F, 10F1 and 10F2 shows good agreement with lO

the data of Exner. lz For binder fractions > 20% I I
1 2 3 ~, 5
the values according to Exner are lower than the dwclMm) ~a

values in the present work and in the work by

Roebuck and Bennet) According to Exner and ~01- ¢-I* 1371 grains
Fischmeister a the contiguity is independent of
carbide grain size; a result which is not supported
by the present work. Furthermore, the contiguity lo
decreases with increasing sintering temperature and
I 2 3 ~, 5 1 2 3 ~ 5
increasing sintering time, a important variables dwc(IJm) d~ q~n)
which should be known in an extended comparison F i g . 17. Influence of manual editing of the grain boundary
of results from different works. network on the measured WC grain size distribution in (a) a
coarse grained alloy, and (b) a fine grained alloy.
7.5 Influence of manual editing
manual editing where missing parts of the network
The automatic reconstruction of the grain boundary are added and mistakes in the automatic linking of
network is normally succeeded by a sequence of the grain boundaries are corrected for. The influence
76 Anders Nordgren

of the manual editing on carbide size distribution

was investigated for grades 18C and 10F1. Size
distributions evaluated from the uncorrected image,
without any manual editing, were compared with
0,8
two levels of manual editing.
In the first case a short time ( ~ 1 min) was spent J
>_-
on each image in adding missing parts of the grain
boundary network. The efforts were concentrated t.O
B 0.6
on eliminating very large, artificial grains generated o
Z
IOF2 Full correction
due to small gaps in the network connecting several
10F1 31C
small grain areas into one large grain. The expected 0.6
18C ~ \ Automatic
effect of the editing is thus a decrease in the
frequency of large grains and an increase in the
number of small grains. 0.2 WC-Co (12)
In the second case the limited, manual editing
was extended into a complete correction of the
network. Not only were large, artificial grains
divided into their correct subareas, but, in addition, 0 I0 20 30
grain boundaries that were not properly positioned BINDER VOWME FRACTION Vco (%)
by the automatic linking were moved and redrawn Fig. 18. Carbide contiguity C s evaluated from uncorrected
at their correct position. Furthermore, by com- networks (automatic reconstruction) and fully corrected grain
paring with the original gray level image, correction boundary networks (manual editing succeeding automatic
linking).
of the network was made where the grain bound-
aries were so weak that they had not been detected The largest difference between the uncorrected
by the image analyzer. and the fully corrected distribution is obtained for
For this extended manual editing considerable the fine grained material 10F1. The difference in
time (-~ 5 min) was necessary, however, without mean carbide diameter dwc is 20 %. For the coarse
dramatic visual changes in the network (Fig. 10b), grained grade 18C the difference in dwc is only 3 %.
In Fig. 17 WC size distributions for grade 18C and The uncorrected result of the automatic analysis is
10F1 are shown for the three cases: thus fully sufficient for coarse grained alloys in most
--uncorrected (automatic reconstruction without applications.
manual editing) In Fig. 18 contiguity values based on uncorrected
--limited editing networks are compared with values for fully
--full correction. corrected networks. The Cz~ values for the corrected
networks are higher due to the increased number of
It is apparent for both grades that the limited carbide/carbide interfaces (2Nwc/wc) and the lower
editing results in a decrease in the number of large mean carbide size (/we)-
grains and a decrease in the mean carbide size As can be expected due to the incomplete
(Table 14) compared to the uncorrected network. detection of the finest carbide grains in grade 18F,
However, further changes due to extended editing 1OF 1 and 10F2 the difference in contiguity is largest
are marginal for both materials. The dwc and/we for these alloys (7-15 %) (Table 15). The difference
values change insignificantly. for the coarse grained alloys 30C and 18C is less
Table 14. Mean values dwc and/we for uncorrected, limited than 5 %.
editing and fully corrected grain boundary networks (grades
18C and 10F1) Table 15. Contiguity C., based on uncorrected and fully
corrected grain boundary networks
Grade 18C Grade IOF1
Grade Cy (uncorrected) C r (fully corrected)
Grain boundary network dwc lwc dwc /wc
31C 0.44 0'45
Uncorrected 1.83 1.82 1"33 1.19 18C 0"42 0"44
(automatic analysis) 18F 0"48 0"51
Limited editing 1.76 1.71 1.18 1.01 10F1 0'47 0"54
Fully corrected 1.78 1"71 1"12 0"97 10F2 0"54 0-59
 Microstructural characterization of cemented carbides
Table 16. Principal differences between two different methods of WC-Co cemented carbide structure characterization
SEM
Microscopy Back scattered electrons
• atomic number contrast
• channelling contrast at low accelerating voltage
Magnification x500(~ x 10000
Specimen sur/ace • Polished (for Co measurement)
• Etched (for WC measurement)
hnage analysis Automatic detection of grain boundary network
It can be concluded that the limited manual
editing, which concentrates on eliminating large,
artificial grain areas, results in size distributions and
contiguity data very close to correct values for all
W C - C o grades. For coarse grained alloys, the
results of the automatic analysis, without any
manual interaction, are fully sufficient. Based on
these results the W C - 7 - C o alloys were analysed
using limited editing of the grain boundary net-
works.
7.6 Comparison with conventional methods
The results from the automatic analysis of W C - C o
grades 31C, 18C and 10F2 were compared with
conventional LOM based semi-automatic structure
analysis. Table 16 shows the principal differences
between the methods. The most important factor is
the difference in contrast and resolution of the
image forming system. The semi-automatic analysis
was based on magnified light optical micrographs
(LOMs) of etched specimens. Apart from lower
lateral resolution of LOM compared to SEM the
mechanisms of contrast are completely different.
The high atomic number contrast between binder
and carbide phase and the channelling contrast
between carbide grains with different crystal orien-
tation have no correspondence in LOM. Thus, the
ability to detect very thin binder ligaments and
small carbide grains can be expected to be con-
siderably lower in LOM as compared to SEM.
However, the high magnification used in SEM in
order to image the grain boundary network and the
fine carbide grains makes it difficult to obtain a
statistically sound result for very coarse, low
frequent, carbide grains.
The LOM micrographs were evaluated using the
intercept method where the chords through binder
pools and carbide grains were manually marked.
The contiguity was calculated based on the manual
detection of different types of phase boundaries.
77
LOM
Reflection mode
x 1000, micrographs magnified to x 2500
Etched
Manual marking of intercept chords and phase
boundaries
Mean values for carbide size (/we), binder mean free
path (/co), volume fractions (V~o, Vwc) and con-
tiguity (C~.) were determined for grades 31C, 18C
and 10F2, representing a wide range of Co contents
and carbide grain sizes.
The results of the method comparison are shown
in Figs 19-22. Very good agreement was obtained
for the binder volume fraction Vco (Fig. 19). The
deviations from the nominal values are well within
standards for both methods. However, when data
for ]co and ]we are compared (Figs 20 and 21) it is
apparent that the difference in resolution and
available contrast lead to different results.
The mean values leo and lwc according to the
LOM based analysis are generally higher than for
the SEM based analysis. This is due to the higher
resolution and the lower detection limit in SEM,
and thus the possibility to include smaller objects in
the analysis. As a consequence the differences
increase when the carbide grain size and the binder
3O
-
20
I /
U
18_c
~ 101 ~"TI7 I I
10 20 30
BINDERVOLUMEFRACTIONVco(%}
(SEM based automatic image analysis)
Fig. 19. Volume fraction of binder Vco according to the con-
ventional method (LOM) and SEM based automatic measure-
ment.
78 Anders Nordgren

1.5
1.0

o=

0.8

S
LOM bosed
ua. N 0.6 10F2 Qnolvsls

z
=R
~ OS 8 •- I 4 31C
zo 06
SEMbosed
r~

0.2
WC-Co (12)
I I I
05 1.0 1.S
BINDER MEAN FREE PATH Tco (pm)
(SEM bosed automotic imoge on(~[ysis)
1 I I
Fig. 20. Binder mean free path/co according to conventional lO zo 30
method (LOM) and SEM based automatic measurement. BINDER VOLUME FRACTION Vco ( % )
Fig. 22. Carbide contiguity CN according to the conventional
method (LOM) and SEM based automatic measurement.
2.0

ranking of the materials are equal to the SEM-

based analysis.
Thus, the high lateral resolution and the favor-
15 able contrast in SEM enables the detection of
E-= thinner binder ligaments and finer carbide grains
~i than when using LOM. The importance of these
principal differences becomes most apparent when
analysing fine grained material and when deter-
1.0 mining the contiguity of the carbide network.

8 W C - 7 - C o GRADES
,
1.0 15 2.0
MEAN CARBfDE LNTERCEPT LENGTH ~wc 8.1 Carbide grain size distributions
(SEM bosed outomotic im~je anatysis)

Fig. 21. Mean carbide grain size/we according to the conven-
tional method (LOM) and SEM based automatic measure-
ment.
volume decrease (grade 10F2). Due to the poor
resolution the LOM based analysis is not able to
correctly represent the differences in structural
parameters between grades 31C, 18C and 10F2.
The measured contiguity depends on both the
ability to detect thin binder areas and to observe
small carbide grains. The C N values according to
the LOM based analysis are higher than the values
evaluated from the SEM micrographs (Fig. 22)
probably due to an underestimation of the number
of W C / C o interfaces, i.e. the thin binder ligaments
between the carbide grains were not properly
detected. However, the overall relationship and the
Carbide grain size distributions for WC, 7-phase
and WC + 7 (all grains) are shown in Figs 23 and 24
for the coarse grained ?C and the fine grained 7F,
respectively. The difference in carbide coarseness of
the two grades is reflected in both carbide types.
The 7-phase is coarser than WC for both grades.
When all grains are considered, the mean carbide
size (dAis) for 7C is approximately twice the value for
7F (Table 17).
8.2 Volume fractions
Due to the high solubility of WC into the 7-phase,
the nominal values cannot be directly compared
with values for sintered material. However, Chat-
field 13 calculated the volume fractions of WC, 7 and
Co in cemented carbide with the same nominal
 Microstructural characterization of cemented carbides 79

I% Table 18. Nominal, calculated ~a and measured volume fraction

5O
I ~ I '~ phose of WC, ),-phase and Co in grades yC and yF
211 groins z,Ob + J _90 groins
awc= 1.11pm

20
3c
'°t Grade Phase
Nominal
(v/o)
Calculated
(v/o)
Measured
(v/o)
lO
yC WC 49"5 32 36"4 4- 3
2 3 4 5 TiC
EO,UIVALENTDIAM.dwc(Pm) d~(IJm) 27'5~
5j 38"5 56 51"64-3
(%),
50' (YaNb)C 11 J
WC~-~+~ Co 12 12 11.64- 1
z,0 ,~ 301 grains
dAIL= .371urn 7F WC 57 52 49.3 4- 3
30 TiC 11 ]
k
20 28.5 34 37 4- 3
(TaNb)C 17"5 J
I0
Co 14'5 15 12"94- 1

dA, (pro)
Fig. 23. Frequency grain size distributions for WC, y-phase
and WC + y in grade yC.
8.3 Carbide contiguity

(%) The contiguity C N and C 1were determined for grade

50 (~'~ ~ phase~F: 7C and 7F according to the same procedures as for
z ~'g]oi ns
131~'~ _62 groins
c~ dwc=O60pm ~0 d~ =0.83pm the WC-Co alloys. Data for the whole carbide
~.
u._ 30
30 volume WC + 7 (all grains) were used. According to
20 20 Tables 19 and 20 the contiguity in the coarse
-~ lO 10 grained alloy yC is somewhat lower (CN = 0"61)
2 ~ L ~ 1 2 ~ L ~ than in grade 7F(C N = 0.70); a result consistent
E[IUIVALENT DIAM.dwc(Pm) d ~" (pm) with the values for the WC-Co alloys where the
(%:
50 ~ WC'~* contiguity increased with decreasing grain size. The
40 ] . 193 groins value for 7C is approximately equal to the value for
dAu:O.69pm
3O the fine grained WC-Co grade 10F2.
20
10 8.4 Influence of manual editing
1 2 ½ L 5
dAu (pm) The carbide grain size distributions for grade 7C
Fig. 24. Frequency grain size distributions for WC, y-phase and 7F in Figs 23 and 24 were evaluated for a grain
and WC + y in grade yF.
Table 19. Contiguity C N for grade 7C and yF based on the
detection of different types of phase boundaries
Table 17. Measured mean carbide size for grade yC and 7F
NvariJl(, o q.-
dwc d; da. 2N,.,.~,,~,.,.. Nt,.,,b,(o 2N,.,.h/,~.,.h
Grade (pm) (#m) (pm) Grade (#m 1) (#m 1) (Izm 1) Cx

yC 1-11 1'96 1'37 yC 1"416 0"546 0"870 0"61

?,F 0"60 0"83 0"69 7F 2'819 0"846 1'973 0"70

compositions as 7C and 7F based on experimentally Table 20. Contiguity C t for grade 7C and yF based on measured
determined phase diagram data. These values are mean values of carbide size, binder free path and volume
fraction
used in Table 18 as an estimate of the volume
fractions that can be expected in the present /earh /¢:o
materials. The agreement between calculated and Grade (j~m) (/2m) V..... ~/i'o CI
measured volume fractions in this work is fully
7C 1.147 0.456 0-884 0.116 0.67
acceptable. A substantial part of the WC in grade yF 0-548 0-278 0-871 0'129 0'71
7C is thus dissolved in the cubic 7-phase.

ERM 10
80 Anders Nordgren

(%: (%
5O
and detection of back scattered electrons;
Automotic WC~ 50 ~m_a_tic WC*~-$ - - a combination of atomic number and
z ~o . . . . . . 252 groins 1'32 Qroins
¢3 aA.=t~3 um ~,0 dAu=6.70 pm channelling contrast modes in image analy-
30 30
sis and automatic image processing in-
2O
cluding gradient filtering and grain bound-
g m 10
. ary reconstruction.
EQUIVALENT DIAM. dAu(IJm)
(%), . ( O / o ~
dau(pm) (3) The preparation of the specimen surface is of
vital importance in order to automatically
:t +5
I 301 groins t.0}- , I 193 groins detect the grain boundary network. Imper-
fections in specimen preparation can rarely
2O be compensated for in SEM or by image

'°f
10

2 3 ~
10
dAu[pm)
Fig. 25. Influence of manual editing of the grain boundary
network on the measured grain size distributions (WC + 7) in
grades 7C and 7F.
Table21. Contiguity CNbased on uncorrected grain boundary
network and network after limited manual editing
Grade C~ (uncorrected)
7C 0'60
7F 0"66
boundary network subjected to a limited manual
editing (see Section 7.5). The influence of the
manual editing on the whole carbide population is
shown in Fig. 25. Data for the uncorrected network,
after automatic reconstruction, are compared with
data for the corrected network. The difference
between distributions and mean values are neg-
ligible for both grades. F r o m this follows that the
calculated contiguity based on the two networks
becomes practically equal (Table 21).
9 CONCLUSIONS
enhancement during image analysis. The
etching procedures for W C - 7 - C o grades have
to be adapted to the individual grade due to
dA.(Om)
the strong influence of carbide chemistry and
surface condition on the etching response.
(4) The automatic measurements of carbide grain
size and contiguity are of fully sufficient
accuracy for a wide range of hard metals. In
cases where the contrast of the grain bound-
aries is very weak, a limited manual editing
C N (corrected)
is sufficient to obtain results close to actual
0"61 values. Automatic detection is easiest for
0'70 carbide phases with a constant gray level in
SEM. If the carbide phase has a pronounced
multi-phase structure, artefacts inside the
grains are detected and linked into the grain
boundary network thus creating artificial
grains.
(5) An accurate microstructural characterization
is the basis for the understanding of the
relationships between mechanical properties
and cemented carbide microstructure. The
methods developed provide a necessary met-
allographic tool. Basic principles of specimen
preparation, microscopy and image analysis
are of general validity and should be ap-
plicable to other types of materials.

(1) It has been possible to successfully apply ACKNOWLEDGEMENTS

modern automatic image analysis to the
microstructural characterization of a wide
range of cemented carbides.
(2) Automatic detection and parameter evalu-
ation were possible through the combination
of
--optimized specimen preparation with re-
spect to distortion free carbide grain sur-
faces, etched carbide grain boundary net-
work and minimum in surface topography;
- - h i g h resolution scanning electron micro-
scopy utilizing a low accelerating voltage
The present research was carried out within the
general research programme of the Swedish In-
stitute for Metals Research with financial support
from the Swedish Board for Technical Development
(STU) which is gratefully acknowledged. The
author would like to thank the members of the
research committee for their keen interest and
valuable comments :
Anders Olsson Uniroc AB, Fagersta
Jan Qvick Seco Tools AB,
Fagersta
 Microstructural characterization of cemented carbides
Leif ,~kesson Sandvik Coromant,
Stockholm
Arne Melander SIMR
H. Chandrasekaran SIMR
Special t h a n k s are d u e to C h r i s Chatfield, S a n d v i k
C o r o m a n t AB, S t o c k h o l m for s e m i - a u t o m a t i c
analysis o f W C - C o grades, to M i c a e l a H u m p h r e y s ,
S I M R for m e t a l l o g r a p h i c a s s i s t a n c e a n d i m a g e
analysis w o r k a n d to S a n d v i k C o r o m a n t A B a n d
Seco T o o l s A B for s u p p l y i n g c e m e n t e d c a r b i d e s
and grade data.
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9-2