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Abstract
Mechanical strength of polycrystalline ice I h was investigated by uniaxial compression tests at wide ranges of
temperature, y10 to y1738C, and of strain rate, 4 = 10y4 to 4 = 10y6 sy1. A systematic change of the deformation type
from brittle fracture to ductile deformation was observed to take place at a critical strain rate and temperature. A systematic
increase of the strength was also found with decreasing temperature and increasing strain rate. In both the ductile and brittle
regions, a similar relation was found to hold: ´˙ s A s nexpŽyErRT . where ´˙ is the strain rate, s is the peak stress for
ductile deformation and failure stress for brittle fracture, R is the gas constant and T is the absolute temperature. The
apparent activation energy E and exponent n are 48 kJrmol and 6.5 in the brittle region and 64 kJrmol and 3.4 in the
ductile region, respectively. The maximum stress Ž smax : peak and failure stress. has a good correlation with the strain Ž ´ max .
at that stress irrespective of the temperature and strain rate. An empirical equation, ´ max s 0.41 q 0.015smax , where the unit
of smax is MPa, can be applied to both the ductile and brittle regions. q 1997 Elsevier Science B.V.
estimate the time scale of the crater relaxation and Parameswaran and Jones Ž1975. obtained the brittle
physical conditions of the crust Že.g. temperature compressive strength of polycrystalline ice at
gradient in the crust. ŽThomas and Schubert, 1986.. y1968C under uniaxial compression and revealed
The measurements of mechanical properties of ice that ice at that temperature was brittle and several
I h at temperatures lower than y308C were carried times or by one order stronger than ice near the
out by Jones and Glen Ž1969., Parameswaran and melting point. Schulson Ž1990. also studied the brit-
Jones Ž1975.. Jones and Glen Ž1969. conducted creep tle compressive strength of ice at temperatures be-
measurements of single crystals of ice at tempera- tween y10 and y508C. He made uniaxial compres-
tures of y30 to y908C to derive a flow law show- sion tests using granular ice with different grain sizes
ing the mechanism of the plastic deformation. and found that the brittle strength was proportional
Fig. 1. Sketch of the experimental apparatus for the deformation experiment at low temperatures and unconfining conditions.
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 217
Fig. 2. Stress–strain and tangent modulus–strain curves of the ductile deformation at 2 = 10y4 sy1 and y428C. The correction method to
exclude the error of the strain caused by the icerplate interface is shown.
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 219
sample increased when decreasing this ratio from 2.5 the loading plates and the initial sample length, thus
to 1, and Paterson Ž1978. recommended a sample this calculated strain includes unexpected errors con-
ratio larger than 2.5 for the deformation test. Our tributed by the icerplate interface. Thus we must
sample ratio is about 2, which is slightly smaller than exclude these errors from the raw strain to derive the
the recommended value because the temperature dif- correct intrinsic strain. The effect of this interface on
ference in the sample becomes larger for the large the deformation and the correction method is noted
lengthrdiameter ratio to severely affect the sample in a later section. As it is unavoidable that the
strength. According to the result of Mogi Ž1966., the surfaces of a cylindrical sample can be slightly un-
strength at a ratio of 2 becomes 2–4% larger than the parallel, a pair of ball seats were set on the upper
strength at a ratio larger than 2.5. Thus, our obtained cooling plate for correction. These copper seats were
strength includes an artificial effect of the lengthrdi- bonded to the ice surfaces and slightly constrained
ameter ratio of several percents. the sample at both ends. The cryostat consists of a
Unconfined uniaxial compression tests under con- stainless-steel chamber and pistons with copper cool-
stant strain rates were conducted on a mechanical ing plates ŽFig. 1.. The ice sample was set in vacuum
testing machine ŽTENSILON UCT-10-UW. set in a ŽF 100 Pa. and its temperature was controlled by
cold room at y108C. The available maximum load regulating a flux of liquid nitrogen flowing into the
was 10 5 N. Stress and strain were measured by a copper cooling plates. The samples could be cooled
load cell and a displacement gage, respectively, at to a temperature from y10 to y1738C without
every 10 mm displacement or 2.5 = 10y5 strain by a forming cracks and were kept at this temperature
micro-computer with a 12 bit ArD converter. The during each deformation experiment. Temperatures
raw strain is calculated by the displacement between measured by using thermocouples located at the
Fig. 3. Stress–strain and tangent modulus–strain curves of the brittle failure at 2 = 10y4 sy1 and y728C. The correction method to exclude
the error of the strain caused by the icerplate interface is shown.
220 M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229
center, upper and lower ends of the sample and both the precise parallel compression was rather difficult
cooling plates showed that the temperature differ- to determine at strain rates faster than 10y3 sy1 . The
ence between the ends was within 18C. experimental conditions of temperature and strain
Transparent windows were used to observe the rate are y10 to y1738C and 4 = 10y3 to 4 = 10y6
deforming sample. This observation enabled us to sy1 , respectively, and the testing conditions are listed
exclude the unparallel compression data. However, in Table 1.
Fig. 4. Ža. Photograph of the deformed sample with many internal cracks sub-mm size in R910702-1. The deformation type is brittle failure.
Žb. Disrupted ice fragments made by brittle failure in R910702-1. The fragment size is in the order of mm to sub-mm. The unit of scale is 1
mm.
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 221
3. Results and discussion must be corrected. The curves are reconstructed with
the slope of the maximum tangent modulus ŽFigs. 2
3.1. Deformation types and 3. and we redefine the zero strain at the point
where the extrapolated line crosses the axis. The
An example of a stress–strain curve at 2 = 10y4 correct strain is measured from this redefined zero
y1
s and y428C is shown in Fig. 2 Žsolid line.. The point. After this strain correction, the intrinsic strain
dashed line is the tangent modulus, which is a local at the peak stress can be obtained. The same correc-
slope of the stress–strain curve and calculated by tion on the strain is applied in Fig. 3.
using the least-square method on five successive data The maximum stress occurs at 0.72% corrected
points. This modulus varies with the strain according strain where the tangent modulus becomes 0 GPa.
to the rheological response of the ice to stress, so it We define this as the peak stress. The corrected
is a useful indicator of the visco-elasticity. At the strain at the peak stress is shown in Table 1. After
initial stage of deformation, the stress gradually in- the peak, the stress rapidly falls and the tangent
creases until the ends of the sample are in good modulus reaches a minimum value at 0.9% corrected
contact with the piston and at 0.8% of raw strain it strain. Then the decreasing rate of the stress becomes
rapidly increases with a sharp increase of the tangent much smaller. This type of deformation with a drop
modulus from 0 to 3 GPa. The tangent modulus of stress is referred to as ductile deformation al-
becomes maximum at 1% raw strain, then it de- though it is not purely ductile because of the cracks
creases with increasing strain. A raw strain smaller that appear. According to the observation of the
than 1% is significantly affected by displacement at deformation process through the optical window,
the icerplate interface so that the stress–strain curve small cracks were generated homogeneously within
Fig. 5. Maximum tangent modulus versus reciprocal of temperature at various strain rates.
222 M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229
the samples. This result suggests that the mechanism ferred to as brittle failure and is often observed at
of this ductile deformation is a dislocation glide with lower temperatures and higher strain rates. By direct
cracks ŽDGC. as studied by Shoji and Higashi Ž1978.. observation of the deforming sample it can be seen
The generated cracks accelerate the formation of that the number of cracks increases gradually and
new dislocations from the crack surfaces and soften homogeneously at low stresses ŽFig. 4a., and then
the ice sample. Ductile deformation was frequently rapidly increases just before the failure. The ice
observed at relatively high temperatures and low sample broke into small pieces, with an average size
strain rates. of several mm ŽFig. 4b., although at high confining
A stress–strain curve at a lower temperature of pressures an ice sample usually breaks into two
y728C and 2 = 10y4 sy1 is shown in Fig. 3. At pieces by a shear fracture ŽDurham et al., 1983..
first, stress increases slowly with strain, and beyond The elastic modulus can be obtained from a slope
about 0.5% of raw strain increases rapidly. The of the stress–strain curve of a deformation test at a
tangent modulus also increases and then becomes constant strain rate. This method was applied to a
almost constant, about 4.2 GPa between 0.4 and single ice crystal by Higashi et al. Ž1964., who found
1.1% of corrected strain. The failure occurred at 52.4 that the modulus was dependent on temperature and
MPa and 1.16% corrected strain Žfailure stress and strain rate. Gold Ž1977. reviewed the strain-rate-de-
strain for other experiments are shown in Table 1.. pendence of the modulus for values between 10y3
The tangent modulus just before the failure de- and 10y6 sy1 at y108C. We here give relations
creased because the stress was relaxed by the rapid between maximum tangent modulus and temperature
generation of cracks. This deformation type is re- for each strain rate. Fig. 5 shows the temperature-de-
Fig. 6. Maximum stress versus reciprocal of temperature at 4 = 10y5 sy1 and y10 ; y1738C. The data in each region are fitted by Eqs.
Ž2. and Ž3..
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 223
pendence of a maximum tangent modulus at three sy1 and y10 to y1738C. The circles and dots refer
different strain rates. Though the strain-rate-depen- to ductile deformation and brittle failure, respec-
dence is not apparent, there is a large temperature- tively. The slope of the lines discontinuously changes
dependence: the maximum tangent modulus in- at two temperatures, y638C and y1038C; the for-
creases linearly from 1 to 5 GPa with the increasing mer almost corresponds to the boundary between
reciprocal of temperature. This result implies that the ductile deformation and brittle failure. The data of
viscous property of ice is contributing to the modu- brittle failure give two straight lines with different
lus above y738C. The elastic modulus of ice derived slopes. We distinguish three regions at these two
from ultrasonic experiments is about 10 GPa at a temperatures: a ductile region, brittle region I and
strain rate larger than 10 2 sy1 ŽYamaji and Kuroiwa, brittle region II. The slope is steepest in the ductile
1956., but smaller than 5 GPa at y108C and a strain region and almost independent of temperature in
rate lower than 1 sy1 ŽGold, 1977.. In our tempera- brittle region II where the stress is constant about 70
ture conditions Žy10 to y1738C., the maximum MPa. Kirby et al. Ž1985. divided the ductile region
modulus is 5 GPa and does not seem to change much into three sub-regions Žductile regimes A, B, and C.
at temperatures below y738C. in their high confining pressure tests. The ductile
region in Fig. 6 seems to correspond to the ductile
3.2. Brittle–ductile boundary regime B. In a strain rate and temperature condition
where Kirby et al. Ž1985. observed their ductile
Fig. 6 shows the temperature-dependence of peak regime C, our brittle region I appeared and brittle
and failure stresses Žmaximum stress. at 4 = 10y5 failure occurred instead of ductile deformation. This
Fig. 7. Comparison of our results with previous results lower than y738C for the unconfined experiments. The lines of our data at
3.5 = 10y4 and 3.5 = 10y6 sy1 are calculated by using Eq. Ž3..
224 M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229
apparent difference in deformation type is caused by ary. This boundary is expressed by the following
the difference of confining pressures. equation:
The failure stress of unconfined low temperature E bd
ice obtained by other studies is compared with our
results in Fig. 7. The earlier data are so scattered
´˙ bd s A bd exp ž /
RT
Ž 1.
between y73 and y1968C that a distinctive rela- where ´˙ bd is the strain rate, A bd is a constant
tionship between stress and temperature at the same Ž1.59 = 10 6 sy1 ., E bd is a constant Ž42.6 kJrmol.,
strain rate can not be recognized. The previous re- R is the gas constant and T is temperature. Accord-
sults show that the upper limit of the failure stress is ing to the data compiled by Gold Ž1977. the brittle–
about 50 MPa. This stress is about 70% of our ductile boundary at y108C appears at 10y3 sy1 ;
obtained stress at temperatures lower than y1008C. however, our results show that the transition can be
The difference between their upper limit and our inferred to be at 10y2 sy1 from an extrapolation of
results may be caused by the crystal size of the the data over an order of magnitude. Schulson and
sample. In our experiments, the grain size of the Buck Ž1995. recently showed that a small amount of
sample is almost the same in each experiment, thus confinement increases the transition rate quite signif-
errors on the strength caused by grain size differ- icantly. As our sample is slightly confined at both
ences are ruled out. This may contribute to the ends, the difference of the strain rate on the transi-
systematic variation of failure strength in the low tion may be explained by this effect. Another impor-
temperature region. tant effect on the transition is the grain size. Batto
Fig. 8 shows deformation types for each strain and Schulson Ž1993. studied the systematic change
rate and temperature. The two deformation types are of the brittle–ductile boundary with the change of
clearly separated by a linear brittle–ductile bound- ice grain size and they showed that the transition
Fig. 8. Deformation types of the ice sample at each experimental condition. The brittle–ductile boundary is also shown and given by Eq. Ž1..
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 225
strain rate varied from 10y3 to 10y5 sy1 when the Table 2
grain size increased from 1 to 10 mm at y108C. Power index n d and n b in Eqs. Ž2. and Ž3. for the ductile region
and brittle region I
Thus, the strain rate found by Gold seems to be the
result of a grain size of about 1 mm. The grain size Ductile region Brittle region I
in our experiments is 0.9 " 0.4 mm, thus the extrap- T Ž8C. nd T Ž8C. nb
olated strain rate when using their results for our y32 3.3"0.3 y74 7.1"1.1
grain size is nearly 10y2 sy1 and may be consistent y42 3.6"0.3 y84 5.8"0.8
with our results.
While the ductile deformation found by Jones and
and n is the power law exponent. The power index n
Glen Ž1969. at 2 = 10y7 sy1 is consistent with our
is calculated by fitting the data sets at each tempera-
result, Durham et al. Ž1983. showed in their experi-
ture ŽTable 2. and the results show that n is quite
ments at confining pressures larger than 100 MPa
different for the two regions: it is about 3.4 for the
that the boundary at 3.5 = 10y6 sy1 was y1338C,
ductile region and 6.5 for the brittle region; this may
which is lower than our y838C. The ductile region
indicate different deformation mechanisms for the
is extended to lower temperatures by the increased
two regions. Fig. 10 shows the relations between the
confining pressure.
peak stress and temperature at different strain rates
together with least-square method lines. The peak
3.3. Deformation and failure mechanisms
stress data can be expressed by the following equa-
tion ŽHigashi et al., 1964.:
The maximum stress in both regions depends on
Ed
the strain rate as shown in Fig. 9. The relations can ´˙d s A d sdn d exp y
be described by a power law equation, ´˙ A s n, ž
RT / Ž 2.
where s is the maximum stress, ´˙ is the strain rate where sd is the peak stress, A d is a constant, Ed is
Fig. 9. Maximum stress versus strain rate at various temperatures. The lines are fitted by Eqs. Ž2. and Ž3..
226 M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229
Fig. 10. Peak stress versus reciprocal of temperature at various strain rates. The lines are fitted by using Eq. Ž2..
an apparent activation energy related to the yield where s b is the failure stress, n b and A b are
mechanism. The value of Edrn d is directly derived constants, E b is an apparent activation energy related
from the fitted lines shown in Fig. 9 and the results to the crack formation and growth. The least-square
range from 17.7 to 21.9 kJrmol ŽTable 3.. The method lines for the data in each strain rate show
averages of n d and Ed in the ductile region were that the value of E brn b ranges from 5.7 to 9.6
estimated as 3.4 and 64 kJrmol. According to kJrmol ŽTable 3.. The average numerical values in
Durham et al. Ž1983., Ed is 61 kJrmol and n d s 4.0
and Barnes et al. Ž1971. reports an Ed-value Žy34 ;
y458C. of 67.3 kJrmol and an n d of 3.18. Our Table 3
activation energy nearly equals their values. Activation energy Ed and E b in Eqs. Ž2. and Ž3. for the ductile
region and brittle region I
The temperature-dependence of the failure stress
in brittle region I is shown in Fig. 11 for each strain Strain rate Ductile region Brittle region I
Žsy1 . Ed r n d Eb r n b
rate. The data are scattered at strain rates higher than ŽkJrmol. ŽkJrmol.
2 = 10y5 sy1 ; however, a general trend of increasing
4=10y4 18.1"0.7 –
stress with decreasing temperature is clear and can 2=10y4 17.7"0.4 8.9"1.6
be written as: 8=10y5 18.7"0.7 –
4=10y5 21.9"1.2 6.6"0.9
2=10y5 19.6"0.7 9.6"1.0
Eb 8=10y6 18.0"1.2 6.0"0.2
´˙ b s A b s bn b exp y
ž / Ž 3. 4=10y6 18.5 5.7
RT
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 227
Fig. 11. Failure stress versus reciprocal of temperature at various strain rates. The lines are fitted by using Eq. Ž3..
the brittle region are E b s 48 kJrmol and n b s 6.5 same equation. This relationship is expected to pro-
ŽTables 2 and 3. although the E brn b values are vide very useful insight in the criteria of ice strength
somewhat fluctuating. The failure stress is known to in the deformation process with crack formation.
become several times larger at low temperatures
ŽParameswaran and Jones, 1975; Durham et al.,
1983.. Our results showed clear systematic changes 4. Conclusion
of stress with both strain rate and temperature. We studied the mechanical strength of polycrys-
Fig. 12 shows the relationship between the maxi- talline ice I h by uniaxial compression tests at temper-
mum stress and the corrected strain at that stress for atures from y10 to y1738C and strain rates of
both the ductile and brittle regions. Except for three 4 = 10y4 to 4 = 10y6 sy1 .
data points around the lowest stress level, the strain As a result, a systematic change from brittle
linearly increases with the stress according to the fracture to ductile deformation was observed to take
empirical equation: place at a critical strain rate and temperature. The
boundary bwteen ductile and brittle is expressed by
´max s 0.41 q 0.015smax Ž 4. the equation:
´˙ bd s A bd exp Ž yE bdrRT .
irrespective of the temperature and strain rate, where where ´˙ bd is a strain rate, A bd is a constant Ž1.59 =
the unit of smax is MPa. Thus, it is surprising that 10 6 sy1 ., E bd is a constant Ž42.6 kJrmol., R is the
both failure and peak stress can be described by the gas constant and T is temperature.
228 M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229
Fig. 12. Corrected strain at maximum stress versus maximum stress for both ductile deformation and brittle failure. The line is fitted by Eq.
Ž4..
We also found a systematic increase in strength and strain rate and can be applied to both the ductile
with decreasing temperature and increasing strain and brittle regions.
rate. In both the ductile and brittle regions, a similar
relation was found to hold:
Acknowledgements
´˙ s A s n exp Ž yErRT .
The authors gratefully acknowledge S. Nakatubo
where ´˙ is the strain rate, s is the peak stress for of the Institute of Low Temperature Science,
ductile deformation and failure stress for brittle frac- Hokkaido University for making the experimental
ture. The apparent activation energy E and exponent apparatus and for his technical support. Dr. H. Narita
n are 48 kJrmol and 6.5 in the brittle region and 64 of the Institute of Low Temperature Science,
kJrmol and 3.4 in the ductile region, respectively. Hokkaido University and Prof. T. Yamamoto of the
Finally, a correlation between the maximum stress Department of Earth and Planetary Science,
Ž smax : peak and failure stress. and the strain at the Hokkaido University gave useful comments and ad-
maximum stress Ž ´ max . was revealed. The derived vice for the experiments. This work was supported
empirical equation is ´ max s 0.41 q 0.015smax , by grants-in-aid for Encouragement of Scientist
where the unit of smax is MPa. This relationship is Ž03740207. from the Ministry of Education, Science,
suitable for all the data irrespective of temperature Sports and Culture, Japan.
M. Arakawa, N. Maenor Cold Regions Science and Technology 26 (1997) 215–229 229