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Soils and Foundations 60 (2020) 1299–1311
www.elsevier.com/locate/sandf
Technical Paper
Received 28 March 2019; received in revised form 25 August 2020; accepted 26 August 2020
Available online 15 September 2020
Abstract
Extensive particle fracture has been noticed in projectile penetration tests. However current models for predicting projectile penetra-
tion depths do not consider particle fracture. Therefore, in order to understand the role of particle shape on single grain strength and the
subsequent comminution process, single grain crushing tests on sand grains of different shapes and sizes were performed. High-
resolution, three dimensional images of grain surface, were created using confocal microscope and fracture of the grains were captured
with high-speed imaging. Acoustic emissions during single grain crushing was used to estimate the energy released during grain fracture.
It was found that local stress fields influence particle strength and in natural granular material surface flaws maybe the critical flaw caus-
ing fracture. The estimated critical flaw size causing fracture were submicron in size. The mass specific fracture energy increased with
increasing failure stress and decreasing particle size and is significantly greater than that computed from pure diametrical breaking.
Except for large angular grains, mass specific energies for different shapes were similar. Angular sands required multiple events to break.
The outcome of this work can be utilized in geomechanics to understand the comminution process and in power industry to estimate the
energy required for comminution.
Ó 2020 Production and hosting by Elsevier B.V. on behalf of The Japanese Geotechnical Society. This is an open access article under the CC BY-
NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Keywords: Single grain crushing; Sand; Particle morphology; Acoustic emission; Fracture energy; High speed imaging
https://doi.org/10.1016/j.sandf.2020.08.004
0038-0806/Ó 2020 Production and hosting by Elsevier B.V. on behalf of The Japanese Geotechnical Society.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
A. Sharma, D. Penumadu Soils and Foundations 60 (2020) 1299–1311
different sizes. Fracture in brittle material is understood to momentum of the falling ball and deformation of the
occur when the stress intensity factor at one of the flaws, rod. The fracture energy was computed as the area under
either volume or surface, exceeds the critical value. The the force displacement curve. The authors state that the
crack then propagates instantly and uninhibited until it method is best suited for elastic spheres but could be
emerges at a boundary. This may lead to the formation applied to irregular particles if a large number of particles
of either two or many progenies of smaller sizes and differ- with similar shape were tested. Once again, the method
ent shapes. Energy is dissipated in the creation of new sur- may not be suitable for very angular particles as the initial
faces, sound, and motion of the progenies. The knowledge breaking and crushing of the asperities and surface features
of the ratio of energy dissipated in creating new surfaces to will be significantly different from grain to grain. In this
the overall energy required for comminution will help in work no assumption of particle shape is made for deter-
the design of efficient systems for creating fines. mining the fracture energy of natural sand grains. The
Fracture of single particles are governed by stress field at energy is directly measured using the non-destructive tech-
the contacts (Zhang et al., 1990). Stress field at the contacts nique of acoustic emission. The measured energy is then
are in turn influenced by the loading geometry and surface scaled by computing the elastic energy at fracture of a
features. These geometrical and loading features may man- smooth spherical manufactured fused silica grain.
ifest as decrease in strength with angularity (Nakata et al., In this work, single particle crushing data on rounded
2001b). The crushing strength then influences the stress and angular sands are presented. In order to better under-
strain behavior and the comminution process in high stress stand the cause of the variability of strength, in addition to
isotropic compression, one-dimensional (1D) compression angularity, thin sections were prepared to facilitate obser-
(McDowell, 2002; Nakata et al., 2001a), and triaxial load- vation of defects in the grains. Thin sections can also reveal
ing (Nakata et al., 1999). The effect of surface features on if a sand grain is single crystal or multi-crystalline. Further,
the strength of single grain is explained using high resolu- high-resolution three-dimensional (3D) images of grain
tion three-dimensional (3D) surface images captured with surfaces were created to gain further insights on the effect
confocal microscope. Also, the role of particle morphology of local stress field and grain-platen contact, on single par-
on fracture is shown with the help of high-speed images. ticle strength. High speed images of particle crushing were
It is generally agreed that the coordination number captured to observe fracture initiation and if possible,
influences particle fracture (Einav, 2007; McDowell et al., crack propagation during particle crushing. Energy
1996; Sammis et al., 1987; Tsoungui et al., 1999) and is released during crushing was measured using acoustic emis-
the dominant factor in the comminution process. Smaller sion (AE) for different particle shapes and sizes. These
particles with fewer neighbors are more likely to fracture observations have been synthesized to present a probable
before larger particles with higher coordination number. framework for comminution process and the observation
The dominance of the coordination number leads to a frac- of fractal nature of comminuted remains.
tal particle size distribution of the crushed particles which
has been observed in high stress (Zhong et al., 2018) and 2. Materials
large strain tests (Coop et al., 2004). Zhang et al. (1990)
on the other hand observed grain crushing occurring ini- Three different sands, Ottawa sand, Q-Rok and Euro-
tially in the larger particles with smaller particles remaining quarz Siligran were used for single grain crushing tests.
intact. Also, Kanda et al. (1985), and Tavares and King These sands have very similar mineralogy, more than
(1998) have shown increasingly more energy is required 99.5% quartz, but very different particle morphology.
to fracture smaller particles. The fracture energy measured Ottawa sand is unground silica with sub-rounded grains,
for grains of different shapes in this work may help to shed Q-Rok is unground silica with angular grains, and Siligran
more light on the interplay of size dependence of strength grains are sub-angular in shape. The maximum grain size
and the coordination number at various stages of the high of Ottawa sand and Q-Rok was 850 lm, and 710 lm for
stress compression. Siligran. Particle shape and size play major roles in deter-
Particle fracture energy has generally been computed mining the fracture strength of single grains. The sands
with the assumption of elastic spherical grains. Kanda were first washed and then divided into three size fractions
et al. (1985) integrated the force displacement curve to using US standard sieves; retained on #30 sieve (R30),
compute elastic energy at fracture assuming Hertzian con- passing #30 sieve and retained on #35 sieve (P30R35),
tact between a sphere and a flat plate. Though this and passing #35 and retained on #40 sieve (P35R40).
approach may be useful for spherical grains, it is inade- Shape parameters for each fraction were computed from
quate to compute displacements in irregular particles. two dimensional (2D) images using computational geome-
Tavares and King (1998) placed single particles on the try (Zheng and Hryciw, 2016) and are presented in Table 1.
end of a long rod and applied impact load by dropping a The values obtained from the computational geometry
ball on the particles. The elastic waves produced in the algorithm are comparable to those presented in
rod from impact were recorded by strain gage. Forces Krumbein and Sloss (1963). Roundness indicates the
and displacements were computed assuming one- degree of angularity; roundness values close to unity indi-
dimensional wave propagation and conservation of cate smooth rounded grains. Sphericity indicates the close-
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A. Sharma, D. Penumadu Soils and Foundations 60 (2020) 1299–1311
Table 1 the load cell frame enabling very precise and zero compli-
Shape parameters for different size fractions for Ottawa sand, Q-Rok and ance displacement measurements. The base plate was
Siligran.
5 mm thick and made of Silicon Carbide (SiC). The bound-
Fraction Sand Median d [lm] Roundness Sphericity ary conditions in single grain crushing can have significant
R30 Ottawa 644 0.73 0.85 influence on the fracture force (Shipway and Hutchings,
Q-Rok 524 0.49 0.76 1993a) as it affects the contact area with the grain, and con-
Siligran 555 0.66 0.82
P30R35 Ottawa 486 0.73 0.82
sequently the stress distribution within the grain. Hard pla-
Q-Rok 461 0.45 0.74 tens were chosen to reduce the contact area between the
Siligran 479 0.55 0.77 grain and the platen and to determine the smallest critical
P35R40 Ottawa 404 0.68 0.85 fracture force. Single grains were placed on SiC base plate
Q-Rok 387 0.45 0.74 and compressed with the diamond surface of the flat punch
Siligran 411 0.59 0.78
indenter at 0.1 mm per minute. A seating load of 0.2 N was
used to ensure seating of the indenter on the sand grains.
ness of the shape of the 2D image of the grain to a circle The initial height of the specimen was measured as the dif-
and is computed as the ratio of the length and width of ference in the displacement values at the base and the top
the grain. Sphericities of all the sands are similar, and of the grain at seating load. Approximately 30 specimens
though the roundness values are different for different were tested for each size fraction.
sands, it does not vary significantly for the different size
fractions. Thin section images of sands observed under 3.2. Single particle crushing with acoustic emission (AE)
cross polarized light indicated that Ottawa sand grains measurement
were single crystal. Q-Rok grains may contain polycrys-
talline grains, and Siligran grains may contain other min- A separate testing system, Psylotech l-TS was used for
eral inclusions or bulging recrystallization regions as single grain crushing test with AE measurement. The sys-
shown in Fig. 1. In addition to the sand grains, four tem was equipped with 1.6 kN load cell and 9 mm linear
350 lm diameter and three 800 lm diameter fused silica variable displacement transformer (LVDT). A proprietary
spheres were also tested. technology incorporated in the system enabled a floating
window scale which could resolve displacements to sub-
micron resolution and force to sub newton resolution. This
3. Experimental methods floating window keeps moving as the limits of the window
is reached enabling the record of both full-scale measure-
3.1. Single particle crushing ments and high-resolution windowed measurements
throughout the duration of the test. This presents a unique
Most of the single grain diametrical compression tests opportunity to measure small variations in force due to
were performed with Zwick Z2.5 hardness testing machine. surface features and at the same time the capability to frac-
The hardness measuring head was equipped with a 200 N ture particles of reasonable size. The base plate and flat
loadcell, a 0.02 lm resolution depth measuring device, punch diamond indenter used in the Psylotech system were
and a 3 mm diameter flat punch diamond indenter. The the same as those used with Zwick system. Mistras Group
transducer that measured displacements was separate from AEWIN was used to record and analyze AE signals. A
general-purpose AE sensor, R15a, was attached to the
loading head as shown in Fig. 2. The sampling rate was
1 MHz, and the threshold amplitude was set at 40 dB to
cancel testing system vibrations. A 120 kHz high pass filter
was applied to cancel audible noise. Approximately 25
specimens were tested from the R30 size fraction and 15
specimens from P35R40 size fraction.
AE measures transient elastic waves that is generated in
a medium when energy is suddenly released. In engineering
material, generation of elastic waves generally coincides
with the formation and propagation of cracks. AE can cap-
ture this dynamic phenomenon. The five parameters that
are generally used to characterize AE signals are amplitude
(A), counts (C), duration (D), rise time (RT) and the mea-
sured area under rectified signal envelope (MARSE), which
is also known as energy (E), with arbitrary units. These
parameters are shown in Fig. 3. An event is triggered when
Fig. 1. Thin section images of multigrain Q-Rok (a) - (b), mineral the rising signal crosses the threshold and lasts until the sig-
inclusion in Siligran (c), and bulging recrystallization in Siligran (d). nal is smaller than the threshold. Though the sensor was
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A. Sharma, D. Penumadu Soils and Foundations 60 (2020) 1299–1311
placed on a dark surface and the start and end focus eleva-
tions were set below the base surface and above the top of
the grain respectively. Three dimensional images for the
three different sands displaying typical surface features of
the sands are shown in Fig. 4. In addition, six grains were
imaged at higher resolution of 150X to determine the sur-
face roughness of the grains. For each grain the roughness
was determined from approximately 50 lm square area as
the average sum of the differences of the surface points
from the mean surface height. The roughness values of
the sands were similar; 0.35, 0.52 and 0.20 lm for Ottawa
sand, Q-Rok and Siligran respectively. These values are
higher than those reported by (Altuhafi et al., 2016).
force as observed in the curves for Q-Rok (Q). The break- High speed images captured during these tests further
ing of the small asperities in Q2 (Fig. 4(c)) and the ultimate illustrate the role of particle shape and surface features
failure is seen in the response of Q2 in Fig. 5. Furthermore, on particle strength. Ottawa sand and Siligran generally
if the grains are polycrystalline, the bond between the exhibited diametrical fracture as seen in Fig. 6. Surface fea-
grains which are weaker, will determine the strength of tures, however, may profoundly influence the type of fail-
the grain. The polycrystalline nature of Q4 can be seen in ure; the large surface depression (Fig. 4(e)) is responsible
Fig. 4(d), which fractured at a very low stress with three for failure in S2, as the particle fails by chipping at the flaw
large progenies. (Fig. 6(m)- (o)). The asperities breaking in Q2, flattens the
Fig. 6. Highspeed images of particle fracture, showing the effect of particle shape and surfaces features on the type of fracture.
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A. Sharma, D. Penumadu Soils and Foundations 60 (2020) 1299–1311
Table 2
Weibull analysis for fracture stress and flaw size for different size clusters of Ottawa sand, Q-Rok and Siligran.
Stress Flaw size,cf
Centroid[lm] Sand Number of grains ro [MPa] m cfo [lm] m
663 Ottawa 36 144 2.89 0.05 4.10
699 Q-Rok 22 49 1.12 0.14 1.63
737 Siligran 59 93 1.84 0.07 2.66
532 Ottawa 42 157 2.87 0.04 4.36
513 Q-Rok 64 87 1.31 0.09 1.80
526 Siligran 50 96 2.49 0.06 3.71
395 Ottawa 49 210 2.61 0.04 4.02
372 Q-Rok 38 130 1.27 0.07 1.64
389 Siligran 19 138 1.93 0.05 2.81
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A. Sharma, D. Penumadu Soils and Foundations 60 (2020) 1299–1311
Table 3
Median values of characteristic AE parameters at maximum force.
Sand Amplitude, A[dB] Rise time, RT[ls] Duration, D[ls] Counts, C MARSE, E
Ottawa sand 99 41 2080 225 1625
Q-Rok 91.5 43.5 1699 178 606
Siligran 95 41 1926 204 913
Fig. 11. Maximum force required to fail particles of different sizes and
Fig. 12. Energy released at grain fracture expressed as mass specific
energy released in fracture. The color bar scale has been limited to the
energy for sand grains and spheres as a function of strength.
median energy released in Ottawa sand.
5=3 mass specific energies for the grains are lower than the
1 F
ESE=M ¼ 2:4961 ð4Þ upper bound line. The mass specific energy decreases at a
pqE2=3 d 2 faster rate with decreasing failure stress for sand particles
where q is the density of the grain (2.65 and 2.22 g/cm3 for than for the spheres. The mass specific energies computed
sand and fused silica respectively) and other terms have by Kanda et al. (1985) were similar to those computed
been previously defined for Eq. (3). The values for m and from Eq. (4).
E for fused silica sphere were 72 GPa and 0.17 and those The mass specific energy required to crush particles
used for silicon carbide base were 410 GPa and 0.16 respec- increases with decreasing particle size as shown in
tively. The values for sand grains and diamond platen were Fig. 13. The values computed by Kanda et al. (1985) and
the same as used in Eq. (2). The above equation was Yashima et al. (1987) are similar for larger particle sizes
applied separately to each contact of the sphere with the but significantly underestimate energies released by smaller
top diamond plate and the bottom silicon carbide plate, particles. They computed elastic energy assuming Hertzian
and the total specific energy was computed as the sum of contact and employed Weibull relationship for size depen-
the two. Similar approach was followed by Kanda et al. dence of strength. King and Bourgeois (1993) have
(1985) and Yashima et al. (1987), they computed compres- reported similar values for 0.5–0.7 mm quartz and the val-
sive strength of spheres using r ¼ 0:9F =d 2 as proposed by
Hiramatsu and Oka (1966). Here Eq. (2), which is generally
used in geomechanics is consistently used for both sand
grains and silica spheres. The average mass specific elastic
energy for two 350l m spheres from AE measurement
was 0.0022 J/kg and that obtained from Eq. (4) was
20.278 kJ/kg, a scaling factor of 9.221 106. All specific
energy values were scaled using this scaling factor and
are shown in Fig. 12. Also shown in Fig. 12 are mass speci-
fic energies for spherical fused silica and quartz at different
failure stresses computed using Eq. (4). The mass specific
energies for the spheres appear as the upper bound limit.
At higher failure stresses which generally correspond to
smaller particle sizes the energies released at fracture are
close to this upper bound. The Q-Rok grains which are
close to the upper bound are associated with multiple Fig. 13. Energy released at fracture for different grain sizes expressed as
events leading up to fracture. At lower failure stress the mass specific energy.
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A. Sharma, D. Penumadu Soils and Foundations 60 (2020) 1299–1311
ues reported by Tavares and King (1998) for quartz for size specific energy with increasing grain size. Also, the com-
range tested in this study are also similar to those com- pressive strength decreases with increasing size and the par-
puted in this study. As particle size decreases greater energy ticles with higher specific energies are associated with high
is required for fracture. Also shown in Fig. 13 is the mass fracture stress. Hence both strength and specific energy
specific energy computed assuming a single diametrical show similar trend with particle size, and King and
break and surface energy. The average value of surface Bourgeois (1993) have noted that the distribution of mass
energy can range from 0.675 J/m2 (Brace and Walsh, specific fracture energy is identical to the probability of
1962) to 2.678 J/m2 (Tromans and Meech, 2004), the line fracture.
shown in the figure was drawn using 2.678 J/m2. The mass
specific energies of smaller particles are significantly larger 5. Conclusions
than that computed assuming diametrical breaking. With
the high stresses required to fracture smaller particles there In this research work, results of single grain crushing
is a greater possibility of larger number of progenies than tests have been presented along with some detailed imaging
that from a diametrical break. With increasing particle size of grain surfaces, high speed imaging of fracture and mea-
and angularity, the mass specific energy based on surface surement of acoustic emissions of grain fracture. Local
energy provides a lower limit estimation. Luo et al. stress fields at contacts play a major role in fracture
(2011) estimated the mass specific energy of Eglin (quartz) strength of single grains. Some differences in fracture
sand to be in the range of 5–25 kJ/kg based on one- strength may be attributed to grain shape and features at
dimensional dynamic compression tests in Split Hopkins contacts. For the size group presented, Weibull distribution
Pressure Bar (SHPB). Based on median particle size in their is found to be acceptable for modeling size dependent
tests (d50 = 350 lm), the average mass specific energy from strength of the grains. Weibull modulus is affected by par-
Fig. 13 is 3 kJ/kg. The mass specific energy from grain ticle shape and decreases with increasing angularity. The
crushing alone will not account for the momentum of the computed Weibull moduli are consistent with the assump-
particles and the energy lost in friction between particles tion of critical surface flaws for all sands. With decreasing
and along the sides of the container in SHPB tests. Thus, grain size, the flaw size is a greater proportion of the grain
energy estimates from such tests may always provide a size in rounded and high Weibull modulus grains, the flaw
higher value than that from single grain crushing. size increases at a faster rate for angular sands with smaller
If coordination number is the dominant phenomenon Weibull modulus. Acoustic emissions reveal that angular
that controls comminution process, then the effect of smal- sands release lower energy at break and may require
ler grains surrounding a larger grain is such that it offsets, greater number of events leading up to the failure. The
in some cases, orders of magnitude of higher energy energy released at fracture increases with fracture stress.
required to crush smaller particles than larger particles. Low strength angular particles may at times release larger
This may not be possible until enough fines have been cre- energy due to multiple small asperities breaking leading
ated. For example, if an 800 lm grain is surrounded by up to the main fracture. The mass specific energy required
300 lm grains, the energy required to crush the smaller to cause fracture increases with decreasing particle size.
grains is almost two orders of magnitude greater than that This coupled with stress reduction in grains with coordina-
required to crush the larger grain. Therefore, initially the tion number may explain the fractal distribution of com-
size dependence of strength maybe the dominant process minuted remains.
with a shift to coordination number dominating the com-
minution as more fines are produced. A stage may then Acknowledgements
be reached at which for a given input energy no more
crushing is possible. Therefore, for a starting particle size This research was funded in its entirety through Defense
distribution and relative density it is possible to arrive at Threat Reduction Agency (DTRA) Grant # HDTRA1-12-
a unique particle size distribution (McDowell and Bolton, 1-0045. We would like to acknowledge the support of our
1998; Sammis et al., 1987). Program Managers Dr. Suhithi Peiris, Dr. Douglas A. Dal-
The power law relationship between mass specific energy ton (Allen), and Dr. Fidel Ruz-Nuglo. Also acknowledged
and particle size (MSE=M / d a ) is characterized by 4.2, are support of Dr. Andrew A. Wereszczak and Dr. Ben-
6.9, 4.2 and 2.4 for the exponent a for Ottawa sand, jamin L. Hackett for the use of Zwick hardness testing sys-
Q-Rok, Siligran and fused silica respectively. Though, tem, Dr, Colin D. Sumrall and Dr. Cameron Hughes for
there were significant differences in the strengths of Ottawa help with sand thin sections, and Dr. J. Michael Starbuck
sand and Siligran, the similar value for a could be a conse- and Dr. Srdjan Simunovic for the high-speed camera.
quence of similar flaw size and flaw size scaling with parti-
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