Diamond technology

Characterisation techniques
for the study of high-strength,
coarse diamond
P roduct characterisation is a subject of
increasing importance within the
superabrasives industries. In this context,
The capability of Element Six to produce diamond crystals of very high perfection
and coarse size has facilitated the creation of a range of products especially
suitable for use in demanding applications. The performance requirements of
characterisation may be considered the
laboratory measurement of certain properties
such products necessitate the highest level of consistency and tightly defined
of a superabrasive product believed to particle sizing. Accordingly, a comprehensive suite of laboratory techniques must
perform important roles in the product’s be employed to understand the product characteristics with sufficient rigour.
behaviour in application. Within the realm A range of techniques for measuring particle size, shape and strength are presented,
of particulate (‘grit’) superabrasives, the with specific reference to the study of high-strength, coarse diamond. The principles
primary properties would be particle size
of operation of these techniques are described, together with appropriate statistical
and strength. In application, these
properties variously influence (among methods for analysing their results. Many of the techniques presented are
others) workpiece material removal rate, complementary, and relationships between these are explored in this article by
workpiece surface finish, tool life and J. Gallagher, P. Scanlon and S.G. Nailer.
the power requirements of the tool.
Product characterisation has perhaps two
principal roles: it may be used to monitor These characterisation methods will be (HP/HT) conversion from graphite, using
the characteristics of products from batch discussed in more detail later, but it may nickel-iron solvent/catalyst alloys. The
to batch (that is, as a method of quality be said that in their most common forms presence of highly perfect particles, in
assessment) and, subject to a sound such techniques are not rigorous enough some instances over 1.1 mm in size,
understanding of the effect of product to enable sufficient characterisation of locate the products in a regime where the
characteristics on performance, it may be superabrasive products whose performance more commonly-used techniques are
used in the design of products for specific requirements necessitate the greatest limited in their ability to effectively
requirements whilst reducing the need understanding, ideally at the particle-to- measure key product characteristics,
for expensive and time-consuming particle level. certainly with the degree of resolution
testing in final application. now required.
For a number of decades since the early Coarse, high-strength For the purposes of brevity, the three
1960’s, superabrasive grit products have diamond products product grades studied here are labelled A,
been characterised mainly by bulk size B and C. Product strength increases from A
and strength measurements. The use of A suite of diamond products with crystals to C, and the special requirements of sizing
sieving as a bulk size measurement is well of very high perfection and coarse size result in specification in terms of stones-
established, and to this day the majority has been created for use in demanding per-carat rather than traditional sieve-based
of superabrasive grit products are defined applications. The products are synthesised definitions1. Optical micrographs of products
for size according to their sieving using high-pressure, high-temperature A, B and C are presented in Fig 1.
characteristics. Strength classification has
been mostly performed by friability
testing, in which a bulk sample of a
product is subjected to a controlled series
of impacts, the mass proportion of
particles that retain a specified size after
impact being interpreted as a measure of
the strength of the product. As the original
strength of superabrasive products may
be compromised by high-temperature
tool manufacture (due to either intrinsic
crystal impurities or tool manufacturing
conditions), strength may also be assessed
by heating the product to suitable Product A Product B Product C
1
elevated temperatures and examining Product grades A, B and C are available as NDG80, NDG100 and NDG120 respectively,
and are supplied in sizes 150 SPC, 210 SPC, 280 SPC, 320 SPC, 350 SPC and 420 SPC.
the consequent strength reduction by a
technique such as friability testing. Fig 1 Optical micrographs of the three coarse grit products.

58 INDUSTRIAL DIAMOND REVIEW 3/06

Diamond technology
In this article, a selection of products is
used to assess the suitability of, and
interpretation of results from, a suite of
characterisation techniques. Two types
of study are presented: the comparison
of different grades in a single size, and the
comparison of different sizes in similar
grades. The former comparison is performed
using products A, B and C in size 210
SPC. The latter comparison is performed
using product C in the two coarsest sizes
available, 150 SPC and 210 SPC.
Characterisation of particle size
Methods of measuring particle size in a
diamond product vary from basic bulk size
analysis through to the examination of its
size distribution on a level of individual
particles. The following subsections discuss
notable size measurement techniques.
Particle sieving
Sieving is a well-established method of
sorting diamond particles according to
size. The selection of appropriate sieves
determines the upper (coarsest) and lower
(finest) sizes of particles in a specific size
band, and diamond grit products are most
commonly available in sizes defined by
these upper and lower sieves (for example,
US Mesh Size [1], FEPA size [2], DIN size [3]).
As a size measurement technique, sieving
indicates the percentage mass of particles
within a specific size band. However, as
the sieves used in size measurement are
typically simply the upper and lower
defining sieves of a product’s ‘as-sold’
size, this technique tends not to detect
slight differences in sizing, such as the
proportion of coarse to fine particles, and
hence, the mean particle diameter.
‘Particles per carat’ measurement
A more precise indication of particle sizing
may be achieved by the measurement of
particles per carat (abbreviated to ‘PPC’). As
a measurement of the number of particles
per unit mass, the PPC number is valuable
for diamond tool manufacturers as it relates
the concentration of diamond grit in the tool
matrix to the number of particles operating
on the tool surface. For this measurement,
Element Six uses proprietary equipment.
Whilst PPC measurement is sensitive
to the average particle size (and hence,
the location of the size distribution), it is
unable to measure the form of the size
distribution (its spread and shape), which
limits its application in the most demanding
characterisation studies.
60
Particle size distribution
measurement by image analysis
An introduction to image analysis
measurement of size
Image analysis is an increasingly common
technique used to measure both size and
shape parameters of diamond particles.
Computerised optical image analysis
systems tend to operate on the same basic
principles: a particle is viewed by optical
image capture, the greyscale (or colour)
particle image is converted into a binary
image using a detection threshold, and
a range of measurements (specified by
size and shape parameters) are obtained
from the binary image. The process is then
repeated for many other particles until a
suitable sample size has been studied.
The measurements from individual
particles are then combined to form
distribution graphs of the various
parameters measured. These distributions
provide detailed information on the entire
sample measured and can identify subtle
differences in size and shape that may
exist between two samples.
The parameter chosen for size
measurement of the coarse grit products
was the diameter of the maximum
inscribed circle within a particle. In the
illustration shown in Fig 2, this particle
diameter is represented by the thick
arrowheaded line.
The output of an image analysis test is
a series of values (particle diameters in
this case) for each of the particles measured
(around 1500 here). These values are
commonly represented graphically by a
frequency distribution (showing the number
of particles with sizes within a particular
band) or a probability distribution (showing
the proportion of particles with sizes within
a particular band). A cumulative probability
distribution of the particle diameters of
product C in 210 SPC is shown in Fig 3.
In Fig 3, the horizontal axis corresponds
to the particle diameter (in µm), whilst the
vertical axis corresponds to the cumulative
probability of occurrence of a particular
diameter (that is, the probability of
occurrence of that diameter or less). The
measured data points (grouped together
for ease of viewing) are shown as blue
diamonds, whilst the orange line
represents a fitted Normal probability
distribution. The assumption that measured
data correspond to known probability
distributions is a critical issue in product
characterisation, and is examined further
in the following section.
Fig 2 Schematic illustration of the
image parameter particle diameter
1
Cumulative probability
Measured data
Fitted curve
0
500 600 700 800 900 1000 1100
Particle diameter (µm)
Fig 3 Cumulative distribution of particle
diameters of product C, 210 SPC
Statistical form of size distributions
It is frequently necessary to summarise the
location, spread and shape of a distribution
by a few selected statistics. Due to the
nature of their size processing, the products
studied here exhibit unimodal symmetrical
distributions of particle size. Consequently,
if the measured data of each sample can
be shown to fit a Normal (Gaussian)
distribution, then the distributions may be
used to display the size results graphically,
and the mean and standard deviation may
be used to described distribution location
and spread.
The Normal (Gaussian) distribution is
perhaps the most important and widely
applied distribution within statistics. The
probability of occurrence P(x) of a value
x is:
where µ, the mean (the location), and σ,
the standard deviation (the spread), are
the parametric statistics of the distribution
function. There is no descriptor for shape
in the Normal distribution due to it being
constrained to a symmetrical ‘bell’ shape.
In the example shown in Fig 3, the
measured data was fitted to a Normal
distribution of mean µ = 781.1 µm and
standard deviation σ = 55.5 µm. The
degree of fit between the measured data
and Normal distribution was expressed
INDUSTRIAL DIAMOND REVIEW 3/06

as the square of the Pearson product
moment correlation, R2. The resultant R2
value of 0.994 indicated a very high positive
correlation between the two data sets.
This approach was repeated for all
products reported here, with similarly
high degrees of fit between the measured
data and Normal distributions. Hence, it
is concluded that in this instance it is
valid to consider the particle diameter
measurements as Normal distributions.
It must be stressed that the assumption
that particle size distribution measurements
generally adhere to Normal distributions
does not always hold. A prime example of
an exception to this assumption is the case
of ‘full-size’ diamond products blended
from ‘half sizes’. If 25/30 and 30/35 US
mesh products were blended to form a
size 25/35 product, the resultant size
distribution would (in all but the most
extreme blend ratios) exhibit two ‘peaks’
separated by a ‘valley’. This distribution
would likely fail a test for ‘Normality’,
and hence the parametric statistics of
mean and standard deviation would not
accurately describe the relationship
between a particle size value and its
probability of occurrence. In this case, non-
parametric statistics such as percentiles
are most appropriate for describing the
distribution. These are discussed later.
Size distribution results may be used to
give an indication of the particles per carat
of a sample. By assuming that a diamond
particle is the same size in each of its three
Cartesian dimensions, the mass of a particle
(i.e., the inverse of PPC) can be shown to
be proportional to the cube of its diameter.
Fig 4 is a graph of the mean particle
diameter of products in various sizes (as
measured by image analysis) compared
to the inverse cube roots of their PPC
values. The relationship between these
two measurements is appropriately linear,
and enables the generation of distributions
of particles per carat (also termed ‘stones
per carat’). Stones per carat distributions
(in probability density form), derived
from image analysis measurements, are
shown in Fig 5.
Characterisation of particle strength
Laboratory measurement of particle
strength is a very common characterisation
requirement, as the strength of a diamond
grit product determines its suitability
for use in the processing of particular
workpiece materials. The two main
methods of measuring grit strength are
INDUSTRIAL DIAMOND REVIEW 3/06
friability (impact) testing and single particle
(compressive) strength testing. Whilst their
principles of operation are quite different,
with careful experimental design and
sound interpretation of results, the two
methods can provide complementary
information on a product’s strength.
Friability measurement
An introduction to friability testing
Friability testing, also known as friatesting,
toughness testing and dynamic strength
testing, measures a diamond sample’s
resistance to impact. The development of
a technique for the measuring the impact
strength of diamond grits began in the
1950s at De Beers’ Diamond Research
Laboratory, the first ‘friatester’ being
announced in the following decade [4].
Since then there have been numerous
modifications and alternative versions,
culminating in Element Six’s proprietary
electronic friatester. Whilst many subtle
differences exist, all share the basic
principles of: the sizing of the initial sample,
controlled crushing of the sample by a
steel ball in an oscillating capsule, and
subsequent sizing of the crushed sample.
The test result may also be expressed in
a number of ways, including percentage
residue (the mass proportion of sample
retained on a specific sieve after a fixed
number of oscillations) and half-life index
(the number of oscillations required to
obtain 50 % residue).
In its most common form, the output
from a friability test is one number, which
offers a ‘figure of merit’ of sample strength.
However, in many instances a greater
understanding of the range of crystal
strengths present is required.
Mathematical form of
friability breakdown
Examining friability residue as a function
of time can provide this extra understanding.
This is performed by testing at a number
of different cycles (or times, as friatesters
operate with fixed oscillation frequencies).
The resultant residue-time graph is akin
to a ‘distribution’ of particle strengths. As
with the image analysis size distributions
discussed earlier, it may be desirable to
compare the results with an appropriate
theoretical model in order to better
understand product behaviour and simplify
graphical representation. Friability residue-
time behaviour of diamond grit was
examined by Belling and Dyer [5], and the
friability residue was found to be calculable
Diamond technology
from the following equation, adapted from
a function proposed by Rosin and Rammler
[6] to explain the comminution of coal:
where R is the mass residue (retained on
a specific sieve after testing), R0 is the
initial sample mass, t is the test time,
and k and n are constants related to
product strength and homogeneity. By
considering R/R0 to be the percentage
residue (%R), the Rosin-Rammler
equation reduces to:
The measurement accuracy of the test
generally becomes poorer at very coarse
mesh sizes due to the statistical errors
induced by the small numbers of particles
per carat (and hence, in the capsule).
Here, however, careful optimisation of
experimental conditions reduced such
errors to acceptable levels.
A friability residue-time graph of product
B in 210 SPC is shown below in Fig 6. The
measured data points are represented by
blue diamonds, whilst the fitted Rosin-
Rammler curve (with k and n found to be
0.013 and 0.878 respectively) is represented
by an orange curve. The square of the
Pearson product moment correlation,
R2, was found to be 0.998, indicating a
very high degree of fit.
With the friability residue-time results
of the other products exhibiting similarly
1000
Mean particle diameter (µm)
Coarse grit,
900 150 SPC
800 Coarse grit,
Standard grit, 210 SPC
700
25/30 US mesh
600
Standard grit,
500 30/35 US mesh
400
0.1 0.125 0.15 0.175 0.2
Particles per carat -(1/3)
Fig 4 Relationship between mean particle
diameter and particles per carat
Coarse grit, 150 SPC
Probability density
Coarse grit, 210 SPC
0 100 200 300 400 500
Particles per carat
Fig 5 Probability density distributions of stones per
carat of coarse grit products in 150SPC and 210SPC
61
Diamond technology

accurate fits to the Rosin-Rammler equation,
it is possible to compare the strength
characteristics of the three products by
means of elegantly simple negative
exponential curves, as shown in Fig 7.
It is hoped that this section has
demonstrated that an appreciation of the
mathematical basis of friability behaviour,
together with an appropriately designed
test methodology, may facilitate a greater
understanding of the strength profile of
a diamond product. Regrettably this
experimental approach is prohibitively
time-consuming, and so a more efficient
method of extracting a similar degree of
strength information is highly desirable.
Single particle compressive
strength measurement
An introduction to single particle
strength testing
Single particle (compressive) strength
(SPS) testing, also known as compressive
failure force (CFF) testing and static
100
90
Friability residue (%)
strength testing, measures the force
required to crush a particle, expressed
in the unit Newtons (N). This technique
became prominent in the 1990s, with both
commercially available test equipment [7]
and proprietary equipment by diamond
manufacturers.
In most test methodologies, particles are
transported individually between a piston
and a load cell, each terminated by a
polycrystalline diamond (PCD) ‘anvil’. As
the piston compresses a particle over time,
the load cell registers the applied force.
At some stage of the compression process,
the diamond will fracture (either partially
or catastrophically), and there will be an
instantaneous reduction in the applied
force. Examination of the force-time curve
allows a failure force to be assigned for
each particle. The failure forces of the many
particles studied are compiled into a
distribution which gives detailed information
on the spread of particle strengths within
a sample. An alternative test methodology
replaces the piston/anvil arrangement with
a pair of rolling cylinders [8].
Whilst such strength testing systems are
Measured data practicable and informative, the validity of
of single particle strength testing
equipment. For this study, a proprietary
Element Six machine was used. The unit
incorporates a crushing system with
force measurement capability greater
than other widely-available systems,
whilst retaining compatibility with more
established systems. Analysis of the entire
force-time trace allows interpretation of
the progression of particle failure as well
as its assigned failure force. The unit also
possesses sophisticated image analysis
capability, enabling measurement of
normalised failure strength and particle
size, crystallinity and morphology.
Statistical form of strength distributions
As stated earlier in this article, it is
frequently necessary to summarise the
location, spread and shape of a distribution
by a few selected statistics. Investigations
into single particle strength distributions
of diamond grit products have shown that
a relatively homogenous, simply-sized (that
is, unblended) product exhibits a strength
profile of the form of a Weibull distribution.
As a ‘time-to-failure’ distribution, the Weibull
is one of the most widely used lifetime

80
70
Fitted curve the results will be significantly compromised distributions in reliability engineering [9].
60 unless certain issues are considered: In the two-parameter Weibull distribution,
50
40 the probability of occurrence P(x) of a
30 ◆ A sufficient number of particles
20 value x is:
10
must be measured to reduce
0 sampling (and hence, experimental)
0 100 200 300 400 500
Time (s) error. Single particle strength
distributions may be very broad
Fig 6 Friability residue-time curve where β, the shape, and η, the scale
of product B, 210 SPC (particularly in the case of coarser
(spread), are the parametric statistics of
products), and so increased sample
the distribution function. For modelling
sizes must be used to counteract
single particle strength distributions, a
100 this. The study of 400-500 particles
90 Product A, 210 SPC third parameter (γ, the location) tends
Friability residue (%)

80 is a reasonable compromise
70
Product B, 210 SPC not to be required.
Product C, 210 SPC between experimental accuracy
60 A cumulative probability distribution
50 and test time.
40 of the single particle strength of product
30
20 ◆ Anvil wear must be monitored C in 210 SPC is shown in Fig 8. The
10 carefully, as successive crushing of measured data are represented by blue
0
0 100 200 300 400 500 diamond particles causes significant diamonds, and the fitted Weibull
Time (s)
damage to the PCD anvils, resulting distribution with shape β = 2.42 and
Fig 7 Friability residue-time curves in a gradual reduction in recorded scale η = 907.2 is represented by an
of the three products in size 210 SPC particle strength. Beyond cumulative orange curve. An R 2 value of 0.995
loads of around 200,000 N, strength suggests a high degree of fit.
results are affected on a statistically Whilst the Weibull distribution fit is
1
0.9 significant level. informative and allows simplified graphical
Cumulative probability

Measured data
0.8 Fitted curve representation of the measured data, its
0.7 ◆ The use of inappropriate
0.6 parameters β and η are not especially
0.5 statistics to describe the measured
0.4 intuitive, and their calculation is not as
0.3 strength distribution will lead to
0.2 straightforward as that of the parametric
misinterpretation of the results. This
0.1 statistics of the Normal distribution,
0 topic is discussed further shortly.
0 500 1000 1500 2000 µ and σ. Consequently the Weibull
Single particle compressive strength (N)
The study of the products featured parameters have perhaps little value for
Fig 8 Cumulative probability distribution here placed significant demands on the handling distributions on a day-to-day
of strength of product C, 210 SPC robustness and measurement capabilities laboratory basis.

62 INDUSTRIAL DIAMOND REVIEW 3/06

 Diamond technology

Percentiles of single particle strength (N)

Product A, 210 SPC
Product 10th 25th 50th 75th 90th

Probability density
Product B, 210 SPC
Product C, 210 SPC 353.6 535.8 771.4 1047.5 1291.8 Product C, 210 SPC

Fig 9 Single particle strength distribution statistics of product C in size 210 SPC

A highly appropriate solution to this The main contributors to the higher

problem is the use of percentiles. These
are non-parametric statistics that form no
part of a probability distribution function.
Quite simply, the nth percentile is the
value below which n% of the data lie. The
50th percentile (the value below which
half of the data points lie) is also known
strength of product C compared to products 0 500 1000 1500 2000
Single particle compressive strength (N)
B and A are an increased proportion of
well-shaped crystals and a decreasing Fig 10 Particle strength probability density
population of crystals with inclusions. In distributions of three coarse products
addition to shape and inclusion content,
particle size influences failure strength (as
Fig 11 demonstrates) – the coarser size Product C, 150 SPC

as the median. Typically, the 10th, 25th,
50th, 75th and 90th percentiles might be
quoted, representing five points along the
cumulative probability distribution curve.
The ‘major’ percentiles of single particle
strength for product C in 210 SPC are
listed in the table in Fig 9. Stated another
way, these percentiles are the strength
values corresponding to the cumulative
probability values 0.1, 0.25, 0.5, 0.75 and
0.9 in the graph in Fig 8.
Because no assumptions are made as
Probability density
Product C, 210 SPC
of product C yields higher single particle
strength results simply by virtue of
requiring a greater volume of diamond
to be crushed by the test apparatus.
This significant influence of product
size may be counteracted by measuring 0 500 1000 1500 2000 2500
Single particle compressive strength (N)
normalised failure force. By dividing the
failure force of a particle by its projected Fig 11 Particle strength probability density
area, a measure of the pressure applied distributions of product C in two sizes
to induce particle failure (in such units as
N/mm2 or MPa) is obtained. This facility
is dependent on the strength testing unit Product C, 150 SPC

to the form of the distribution, percentiles
can be used to describe distributions of
any shape or number of peaks, including
size distributions of blended ‘full-size’
products previously described.
Single particle strength of
high-strength, coarse diamond
The suite of high-strength, coarse products
introduced earlier were studied using
the Element Six single particle strength
machine described above. The previous
Probability density
Product C, 210 SPC
having accurate image analysis capability.
Single particle normalised failure force
distributions of the products in the two
sizes are shown in Fig 12. The distributions
again fit the Weibull form.
At first glance the forms of the curves 0 1000 2000 3000 4000
Single particle normalised compressive strength (N/mm2)
in Fig 12 appear similar to those in Fig 11.
However, closer inspection shows that the Fig 12 Normalised strength distributions
order of the curves has become reversed. of product C in two sizes
It is a fundamental characteristic of brittle
materials that the larger an object
100 Product A, 210 SPC
becomes, the greater the probability of Product B, 210 SPC
Particle survival (%)

section demonstrated the fitting of a Weibull
distribution to a measured strength data
set, and by extending this principle to other
results, the strength distributions of all of
the products were also found to conform
incorporation of critical flaws. In crystals Product C, 210 SPC
such as diamond, such flaws may take
the form of included foreign elements, or
line or planar defects. Hence, in terms of 100
intrinsic crystal strength (per unit volume),
Friability residue (%)

0
to Weibull distributions. The single particle more finely-sized products tend to be 0 200 400 600 800 1000120014001600
strength distributions of products A, B stronger than their coarser counterparts, Compressive strength (N)

and C in size 210 SPC (in their Weibull
forms) are presented in Fig 10.
In Fig 10 there is a clear progression
from the lower strength product A to the
higher strength product C: a decreasing
proportion of weak crystals, and (hence)
an increasing proportion of strong crystals.
Note also the shape of the curves: the
strength distribution of product C is
reasonably symmetrical, but product
A’s distribution is highly skewed. This
significant departure from Normality is
the principal reason why the Normal
parameters of mean and standard deviation
are inappropriate for describing single
particle strength distributions.
and this is observed in most standard saw
grit product ranges.
Relationship between friability
strength and compressive strength
As previously discussed, friability testing
and single particle strength testing use very
different mechanisms and methodologies
for assessing diamond grit strength, and
yet in the studies performed here, both
techniques have provided information
on the range of particle strengths present
in a product.
The graphs presented in Fig 13 allow
comparison of the results from these two
techniques. The lower left graph contains
0
0 100 200 300 400 500 600 700 800
Time (s)
Fig 13 Comparison of friability
and compressive strength curves
the friability residue-time curves of products
A, B and C in size 210 SPC (also shown
in Fig 7). The upper right graph contains
the single particle strength distributions
of the same products, but arranged to
show the probability of particle survival
rather than particle failure (that is, the
same form as the friability curves).

INDUSTRIAL DIAMOND REVIEW 3/06 63

Diamond technology
Fig 14 Schematic illustration of
the image parameter elongation
Fig 13 shows that, whilst the two types
of curves are somewhat different in
shape, there are similarities in the manner
in which they rank the three products.
Ultimately, the shorter measurement time
and the additional image-based information
offered by the Element Six single particle
strength tester make it especially valuable
as a method of characterising high-strength,
coarse diamond.
Measurement of elevated-temperature
product strength
Many diamond tool manufacturing
techniques involve sintering or infiltration
processes at temperatures in excess of
800 °C. Consequently it is necessary to
understand any strength reduction of the
diamond that may be induced by such
processes. Strength degradation of
diamond can occur at high temperature by
three mechanisms: internal graphitisation,
surface oxidation and surface graphitisation.
The latter two mechanisms occur due to
the presence of certain metals (those that
may act as solvent/catalysts in diamond
synthesis) in the matrix material, or as a
result of poor toolmaking practices.
Internal graphitisation of diamond is the
mechanism of main concern to diamond
producers, as it derives from the inclusion
of solvent/catalyst metals from synthesis.
At the temperatures and pressures
associated with toolmaking processes
graphite is the thermodynamically stable
form of carbon, and at sufficiently high
temperatures metal inclusions will
recatalyse the conversion of the
surrounding diamond to graphite. The
consequent volume increase creates
stress points in the crystal that may
induce premature fracture.
The high-temperature strength reduction
caused by such intrinsic impurities may
be measured by strength testing following
heat treatment of the diamond. A
64
temperature of 1100 °C is most commonly
used by Element Six as it is more likely
to induce a detectable strength drop than
lower temperatures. Additionally, by heating
in an inert atmosphere (such as argon)
reactions at the diamond surface are
prevented, thus isolating the effect of internal
graphitisation. For subsequent strength
measurement, either friability testing or
single particle compressive strength testing
may be used, though as long as friability
testing offers lower experimental error it
will be the more appropriate technique
for measuring small strength reductions.
Characterisation of particle shape
The above sections have addressed the
characterisation of the principal properties
that are believed to affect the behaviour
of a high-strength, coarse diamond product
in abrasive application: size (and size
distribution) and strength (before and after
exposure to high temperatures).
As image analysis becomes more widely
used as a characterisation tool in the
diamond industry, there is increased interest
in the ability to quantifiably measure particle
shape. It is evident (even from the briefest
study of saw grit product advertising
literature) that high strength products
consist mainly of symmetrical, cubo-
octahedral particles whilst low strength
products consist mainly of particles that
are elongated and irregularly-shaped.
Hence, particle shape is a significant
contributor to particle strength, even though
its measurement many not be able to give
accurate strength prediction.
The three products A, B and C in size
210 SPC were studied for particle shape
using the parameter elongation, which has
perhaps the clearest relationship with
product strength. For this measurement, an
ellipse with the same geometrical moment
of inertia as the particle is considered. The
more elongated the particle is, the more
elongated the ellipse is. The elongation
value is derived from the ratios of the minor
and major axes of this ellipse, with higher
elongation values corresponding to more
elongated particles. A schematic illustration
of the elongation parameter is shown in
Fig 14, with the major and minor axes
signified by thick arrowheaded lines.
Most image analysis systems offer
parameters relating to particle elongation,
some systems simply comparing the
longest and shortest dimensions of a
particle (whatever their orientation). The
definition based on an ellipse is preferable
1
Cumulative probability
Measured data
Fitted curve
0
0 0.1 0.2 0.3 0.4
Elongation
Fig 15 Cumulative probability distribution
of shape of product C, 210 SPC
as it is independent of particle orientation
and returns an elongation value of 0 for
squares, hexagons and octagons (the
typical two-dimensional projections of
ideal diamond morphologies).
Statistical form of shape distributions
Previous sections discussed the
mathematical foundations for fitting
probability distributions to measured data
of size (the Normal distribution) and strength
(the Weibull distribution). Particle strength
distributions were frequently found to
be highly skewed, and to compensate for
the inadequacy of describing them in
terms of means and standard deviations,
the concept of non-parametric statistics
(percentiles) was introduced.
Distributions of particle shape are also
typically skewed, but they may take a
number of different forms. The Gamma
probability distribution, whilst it may not
have the same logical physical significance
to diamond characterisation as the
Weibull distribution (whose time-to-failure
prediction is most suitable for describing
single particle strength), is a versatile
function for modelling a range of skewed
distribution forms [10].
In the Gamma distribution, the probability
of occurrence P(x) of a value x is:
where k, the shape, and θ, the scale
(spread) are the parametric statistics of
the distribution function, and Γ(k) is a
Gamma function. As in the case of the
Weibull distribution, these parametric
statistics are perhaps less intuitive than
the percentiles for describing particle
shape distributions on a practical basis.
The distribution of particle elongation
of product C in size 210 SPC is shown in
Fig 15. The measured data points are
represented by blue diamonds, and a
fitted Gamma distribution, with k and θ
values of 2.502 and 0.030 respectively, is
shown as an orange curve. An R2 value
INDUSTRIAL DIAMOND REVIEW 3/06

Probability density
0 0.1
Elongation
Fig 16 Particle elongation probability density
distributions of three coarse products
Single particle strength statistic (N)
1500
1250
1000
750
500
250
0
0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 1.35 1.40
Grouped aspect ratio
Fig 17 Relationship between particle shape
and strength within the three products
of 0.999 suggests a very high degree of
fit between the measured data and the
selected Gamma distribution. With the
other two product grade exhibiting similarly
good fits, particle elongation distributions
of the three are shown in Fig 16.
Fig 16 shows that the highest grade
product, C, consists of a comparatively
narrow range of highly uniform crystals,
whereas the lowest grade product, A,
contains a significantly higher proportion
of more elongated crystals. This correlation
between low shape values (that is, ‘good’
particle shapes) and high particle strength
values is generally seen for standard saw
grit diamond products.
The proprietary Element Six single
particle strength testing unit is able to
obtain measurements of shape (using
its image analysis capability) and strength
on individual particles, which facilitates
an extra level of understanding. The
measurement of particle elongation in
this system is called aspect ratio, and is
simply the ratio of the longest and shortest
dimensions of the particle (irrespective
of their mutual orientation). Hence, the
least elongated shape (a circle) has an
aspect ratio of 1, with more elongated
shapes returning higher aspect ratio values.
Fig 17 shows a graph relating particle
aspect ratio to strength, as measured by
the Element Six strength testing unit.
For above graph, the results for the three
product grades were combined in order
to maximise the data set. The aspect
ratio values were rounded to the nearest
INDUSTRIAL DIAMOND REVIEW
multiple of 0.05 and grouped accordingly.
Product A, 210 SPC Each aspect ratio grouping possessed its
Product B, 210 SPC
Product C, 210 SPC
own strength distribution, the 25th, 50th
and 75th percentiles of which were
calculated and plotted on the graph. This
graph demonstrates that within a product
the less elongated particles are likely to
0.2 0.3 0.4 be stronger. However the 25th and 75th
percentiles indicate that there is some
scatter of the strength results within each
aspect ratio grouping, so consequently
it is not possible to infer the strength of
a particle from its shape alone.
75th percentile of strength
50th percentile of strength
25th percentile of strength Conclusions
As opportunities for ever coarser and
stronger synthetic diamond grit products
emerge, established laboratory techniques
such as sieving and friability testing are
becoming increasingly limited in their
ability to effectively describe key product
characteristics.
It has been shown that a knowledge
of grit friability as a function of time can
lead to a test methodology that examines
the different populations of crystals
within a product. Nevertheless, the
technique is limited in its application by
its time-consuming nature and its reduced
measurement repeatability for coarser
grit particles.
The ability of techniques such as single
particle compressive strength testing
and image analysis to measure particles
individually will give them ever greater
importance in the realm of product
characterisation, whilst their complexity
places especial importance on robust
testing procedures and appropriate
statistical analysis of results.
In its most sophisticated form, single
particle strength testing is a highly
informative method of assessing product
strength, and results presented here
demonstrate the capability of Element
Six to measure very high-strength, coarse
diamonds. Image analysis may be used
to measure particle size and shape
distributions. A correlation between
mean particle size and the number of
particles per carat has been shown, and
relationships between particle shape and
strength have been explored.
A thorough understanding of the effects
of particle size, shape and impurities on
strength will be increasingly valuable as
further developments of coarser and
stronger diamond types continue to push
the boundaries of destructive testing in
the laboratory. ◆
3/06
Diamond technology
References
[1] ‘Standard specification for wire cloth
and sieves for testing purposes’,
ASTM E11-04.
[2] ‘Superabrasives grit sizes’,
http://www.fepa-abrasives.org.
[3] ‘Grain sizes of diamond or cubic
boron nitride’, DIN 848-1988.
[4] Belling N.G. and Dyer H.B. (1964)
‘Impact strength determination of
diamond abrasive grit’, Industrial
Diamond Information Bureau booklet,
London.
[5] Belling N.G. (1972) ‘Determination of
the strength of diamond abrasive grit
using the Friatester’, De Beers Industrial
Diamond Division internal report.
[6] Rosin P. and Rammler E. (1933)
‘The laws governing the fineness of
powdered coal’, J. Inst. Fuel, pp 29-36.
[7] Vollstädt H. and List E. (2003) ‘Controlling
the stability of the properties of
superabrasive powders’, 4th Zhengzhou
International Superhard Materials and
Related Products Conference.
[8] ‘Diamond Characterization’, Diamond
Innovations information brochure,
http://www.abrasivesnet.com/en/product
/mbs/diamond/down/DI%20MBS%20
DiamondChar.pdf.
[9] Montgomery D. C. (1997) Introduction to
Statistical Quality Control, John Wiley,
New York.
[10] Hogg R.V. and Craig A.T. (1978)
Introduction to Mathematical Statistics,
4th edition, Macmillan, New York.
Authors
J. Gallagher and S.G. Nailer work for the
Market Support Centre, Element Six Ltd.,
Shannon Airport, Shannon, Co.Clare, Ireland.
www.e6.com
P. Scanlon works for the Department of Physics,
University of Limerick, Limerick, Ireland.
Acknowledgements
The authors wish to express their gratitude
to the following Element Six personnel: Mr
Jarlath Walsh, Dr Ger Dolan and Mr Kieran
O’Loughlin, for experimental measurements;
Mr Mike Fish, Dr Derek Wright, Mr Brendan
Kirwan, Mr Gerry Flynn and Dr Clinton
Dickerson for their advice and contribution
of knowledge.
This article is based on a paper presented
at the 1st International Industrial Diamond
Conference held in Barcelona, Spain in
October 2005 and is printed with kind
permission of Diamond At Work Ltd.
65