Effect of Rapid Thermal Cooling on Mechanical Rock Properties

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Rock Mech Rock Eng DOI 10.1007/s00603-013-0523-3 ORIGINAL PAPER Effect of Rapid Thermal Cooling on Mechanical Rock Properties Kwangmin Kim John Kemeny Mark Nickerson Received: 10 October 2012 / Accepted: 15 November 2013 Ó Springer-Verlag Wien 2013 Abstract Laboratory tests have been conducted to investigate the effects of rapid thermal cooling on various rock specimens including igneous, sedimentary, and metamorphic rocks. At first, various types of thermal loading were conducted: heating up to 100, 200, and 300 C, followed by rapid cooling with a fan. In addition, multiple cyclic thermal cooling (10, 15 and 20 cycles) with a maximum temperature of only 100 C was conducted. Experiments included edge notched disc (END) tests to determine the Mode I fracture toughness, Brazilian disc tests to determine tensile strength, seismic tests to determine P-wave velocity, and porosity tests leading to meaningful results. Even though only small changes of temperature (rapid cooling from 100 C to room temperature) were applied, the results showed that crack growth occurred in some rock types (granite, diabase with ore veins, and KVS) while crack healing occurred in other rock types (diabase without ore veins, quartzite, and skarn). To better understand the results, 3D transient thermomechanical analysis was conducted using the ANSYS program. The results indicated that there was a thin region near the outside of the specimen where large tensile stresses occur and microcracking would be expected, and that there was a large area in the middle of the specimen where lower magnitude compressive stresses occur and crack closure would be expected. It was found that the more heterogeneous and more coarse-grained rock types K. Kim (&) J. Kemeny Mining and Geological Engineering, The University of Arizona, Tucson, AZ, USA e-mail: kimkm@email.arizona.edu M. Nickerson Marco Industries, Tucson, AZ, USA are more likely to exhibit crack growth, while less heterogeneous and more fine-grained rocks are more likely to exhibit crack healing. Keywords Rapid thermal cooling Crack healing Cyclic thermal loading Mechanical rock properties 1 Introduction There are many important engineering applications in which rock is subjected to thermal loading. These include deep drilling and deep underground mining, underground storage of high-level nuclear waste, and geothermal energy extraction. It also includes the daily and seasonal temperature fluctuations of rock along highways, railways, and dam and bridge foundations. In some of these applications, the occurrence of high thermal stresses and associated rock fracturing is due to the large, slow changes in temperature. In this case thermal stresses are generated by geometric constraints (rock unable to expand freely) or the heterogeneous distribution of rock properties. In underground nuclear waste storage, for example, the heating of underground drifts to over 150 C can generate compressive tangential stresses as high as 60 MPa at the boundary of the excavations (Kemeny et al. 2006). Also, experiments have shown that when hard rocks such as granite and quartzite are slowly heated to temperatures over 250 C, tensile cracking occurs due to the mismatch in elastic and thermal properties between grains and phase transitions in the individual minerals (Zomeni 1997; Meredith and Atkinson 1985). In other applications, high thermal stresses and associated cracking are due to smaller but rapid changes in temperature. In this case, thermal stresses are generated by the transient distribution of temperatures in the rock. The

K. Kim et al. Fig. 1 Tensile stresses on the surface and compressive stress in the center on cooling (Timoshenko and Goodier 1970) historic method of rock excavation by heating up the rock with a fire and then dousing the rock with cold water is an example of this type of thermal loading. More modern examples include the sudden flow of cold air due to ventilation in a deep underground excavation, and the solar heating and cooling of rock slopes (Glamheden and Lindblom 2002; Bellopede et al. 2006; Yavuz et al. 2006; Kingery 1955). In general, the applications involving slow heating or cooling are analyzed using steady-state heat flow, while applications involving rapid heating or cooling must be analyzed with transient heat flow. Rapid heating or cooling of rock is generally accompanied by regions of both tension and compression. For example, if a cold temperature is suddenly applied to a warm or hot rock volume, a tensional tangential stress is generated at the surface of the rock where the cold temperature is applied, accompanied by compressive stresses behind the tension region. Figure 1 shows an example of this, for the simple case of an elastic plate with a temperature T o and a suddenly applied cooler temperature T a applied to the surface y =±c (Timoshenko and Goodier 1970). With time, as steady-state conditions prevail, the tensile and compressive stresses decrease to zero. In theory, a maximum thermal stress of EaDT/(1 - m) could be generated (where E is the Young s modulus, a is the coefficient of thermal expansion, DT (T o - T a ) is the change in temperature, and m is Poisson s ratio). For example, for a rock at a depth of 2,000 m at a temperature of 80 C, and the rapid application of a cooler temperature of 25 C, a maximum tensile stress at the boundary of the excavation of about 17 MPa could be generated (assuming E = 50 GPa, a = 5 9 10-6 / C and m = 0.2). This is sufficient to result in tensile cracking. The convective heat transfer coefficient (also referred to as the film coefficient) dictates the speed or efficiency of heat transfer (Welty et al. 2009). For very rapid cooling of a hot rock specimen dropped into cold water, for example, the heat transfer coefficient could be above 2,000 W/m 2 K. For moving air, the heat transfer coefficient ranges from 100 to 500 W/ m 2 K. This paper describes a series of experiments that were conducted on specimens of igneous, sedimentary, and metamorphic rocks. Specimens were slowly heated to temperatures of 100, 200 and 300 C, followed by rapid cooling with a fan blowing room temperature air (25 C). Based on the speed of the fan and the shape of the specimens, a heat transfer coefficient of 100 W/m 2 K was used in this study. Experiments conducted on specimens with and without the slow heating/rapid cooling cycle include the edged notched disc (END) test to determine the Mode I fracture toughness, Brazilian disc tests to determine tensile strength, seismic tests to determine P-wave velocity, and a comparison of oven-dried and immersed mass to determine the void volume and porosity (Bowles 1978; ASTM 2002). Rock types tested include Coconino sandstone from northern Arizona, Sierrita and South Mountain Granite from southern Arizona, and a number of rock types from the mining district near Superior, Arizona. These include diabase, quartzite, KVS (Cretaceous Volcanic Sediments) and Skarn. Some of the diabase specimens that were tested contained very prominent pyrite quartz veins (referred to as ore veins), and other specimens did not. In some of the tests, a single cycle of slow heating followed by rapid cooling was conducted at temperatures of 100, 200 and 300 C. In other tests, multiple thermal cycles (10, 15 and 20 cycles) with a maximum temperature of only 100 C were conducted. The low-temperature, multiple cycle tests are relevant to some important rock engineering applications where rapid small to moderate changes in temperature are repeatedly applied to a rock surface, such as in deep underground mining and deep drilling for petroleum or geothermal resources. The next section of the paper (Sect. 2) describes the rock specimen preparation and the various thermal loading cycles that were conducted on the different rock types. Section 3 describes fracture toughness and tensile strength results of Coconino sandstone slowly heated from room temperature (25 C) and rapidly cooled from 100, 200 and 300 C. Section 4 describes single and multiple thermal cycle results of testing of the remaining rock types with a maximum temperature of only 100 C. Section 5 describes the thermo-mechanical 3D ANSYS finite element modeling that was conducted. Finally, Sect. 6 presents conclusions on the study. 2 Heat Treatment and Specimen Preparation All testing utilized cylindrical discs that were cut from cylindrical core. In the case of specimens of Coconino sandstone, Sierrita granite and South Mountain granite,

Effect of Rapid Thermal Cooling on Rocks 50.8-mm diameter cylinders were first produced from rock blocks using a diamond core drill at the University of Arizona lab, followed by sawing of the specimens to the desired thickness (50.8 mm for porosity tests and 25.4 mm for Brazilian disc tests). In the case of specimens of diabase, quartzite, KVS and skarn, rock core was obtained from the mining client and cut to the desired thickness at the University of Arizona. The specific dimensions (diameter and thickness) for each test are given in Table 1. A small electric furnace was used for heating the specimens, which included a fully programmable digital electronic controller and display unit. The temperature inside the furnace was raised and maintained within ±0.1 C. To minimize cracking caused by a temperature gradient, a very low heating rate, less than 1 C/min, is recommended in the ASTM procedures. In this study, the heating rate inside the furnace was maintained at 1 2 C/ min for the slow heating portion of the thermal cycle, thus minimizing the effects of transient heat flow. Slow heating results in a uniform thermal expansion, which in some rocks can be accompanied by thermal cracking, particularly at temperatures above 350 C (Zomeni 1997). This is not expected to impact the results of the testing that was conducted at 100, 200 and 300 C in this study. Following the slow heating, specimens were quickly transferred to a metal table and a small portable fan was used to blow room temperature air at a velocity of approximately 10 m/s. In general, rock specimens were heated up to 100, 200 or 300 C for about 2 3 h and rapidly cooled with a fan. The fan was run for several hours even though the numerical analysis presented in Sect. 5 indicates that the effects of rapid cooling occur within the first 10 min or so. Thus, one cycle of thermal loading took about 4 6 h and the rock properties were investigated before and after thermal loading. Even though the goal of the study was to test rock samples from the Superior mining district, preliminary testing was conducted using Coconino sandstone for two reasons. First of all, Coconino sandstone was tested due to its relatively homogeneous rock properties. Secondly, due to the shortage of samples from the mine, the testing of Coconino sandstone allowed us to conduct a set of tests. 50.8 9 25.4 mm (diameter 9 thickness) specimens of Coconino sandstone were prepared, and two types of tests were conducted on the specimens before and after thermal loading. END tests were conducted on some specimens to determine the Mode I fracture toughness K IC (Donovan 2006), and Brazilian disc tests were conducted on other specimens to determine the tensile strength. Details on the number and type of tests conducted on Coconino sandstone are provided in Sect. 3. Figure 3 shows a picture of an END test being conducted on Coconino sandstone. The results of the testing of the Coconino sandstone are described in Sect. 3. Testing of specimens from the Superior mine district were conducted with diabase, quartzite, KVS and skarn cores taken from depths of 1,000 2,000 m. These specimens were tested to investigate the possible effects of rapid cooling due to mining ventilation on the stability of underground drifts. Based on a mining depth of up to 2,500 m and a thermal gradient of 30 C/km, specimens were slowly heated to 100 C and rapidly cooled with a fan. Due to a shortage of specimens available for testing from the mining client, additional thermal testing with specimens of Sierrita Granite and South Mountain Granite from Arizona were used. Three types of tests were conducted before and after the 100 C thermal loading cycles: Brazilian disc tests to determine the tensile strength, seismic velocity tests to determine the P-wave velocity, and porosity tests. A summary of tests conducted for each rock type is shown in Table 1. Table 1 Tests at each rock type and specific dimensions (diameter 9 thickness) at each test Rock types Tests END tests (Mode I fracture toughness) Brazilian disc tests (tensile strength) Porosity tests (void volume change) Seismic velocity tests (seismic velocity) Initial study: various thermal loadings (100, 200, 300 C) Coconino sandstone 50.8 9 25.4 mm 50.8 9 25.4 mm Tests were out of the scope in the initial study Actual testing of mining samples: cyclic thermal loading (25 100 C) Skarn Due to complication of having 50.8 9 25.4 mm 63.5 9 50.8 mm Due to a shortage of specimens Quartzite notch in the study 50.8 9 25.4 mm 63.5 9 50.8 mm available for testing Diabase 50.8 9 25.4 mm 63.5 9 50.8 mm 63.5 9 38.1 mm Granite Due to a shortage of specimens 50.8 9 50.8 mm 50.8 9 25.4 mm KVS available for testing 50.8 9 50.8 mm Due to a shortage of specimens Diabase (with ore vein) 50.8 9 50.8 mm available for testing

K. Kim et al. Fig. 2 The tested samples (left to right) skarn, quartzite, diabase (upper) and diabase (with ore veins), KVS, Sierrita granite (lower) As shown in Table 1, different tests were conducted in the preliminary phase and in the second phase. In the preliminary phase using Coconino sandstone, END tests containing a notch were conducted to determine the fracture toughness. Even though the fracture toughness is an important rock property, the thermal stresses in the notch area due to rapid thermal cooling with a fan are very complex, and the results can be difficult to interpret. Therefore, these tests were not conducted in the second phase where samples from the mine were tested and there were a limited number of specimens available. In addition, not all tests were conducted on all rock types in the second phase due to a shortage of specimens available for testing from the mining client (cores were taken from depths of 1,000 2,000 m and most of the core was used for assay and not available for geotechnical testing). Details on the number and type of tests conducted on diabase, quartzite, KVS, skarn, and Sierrita and South Mountain granite are provided in the various tables in Sect. 4. Pictures of these different rock types are shown in Fig. 2. The results of the testing of these rock types are described in Sect. 4. 3 Effect of Rapid Thermal Cooling on Mode I Fracture Toughness (K IC ) and Tensile Strength of Coconino Sandstone This section describes the results of specimens of Coconino sandstone subjected to rapid thermal cooling. Specimens are heated to 100, 200, and 300 C at a slow heating rate of 1 2 C/min, followed by rapid cooling to room temperature using a fan. There are many methods for determining the Mode I fracture toughness, K IC, and there is not a single Fig. 3 The END (edge notched disc) test for Mode I fracture toughness with sandstone (Donovan 2006) standardized test method for Mode I fracture toughness. In this study, the END test was used to investigate K IC as a function of thermal loading (Donovan 2006). The advantage of this test is that it is a fast and easy method using core-based specimens. Since the primary focus of this study is to look at changes in rock properties due to thermal loading, the END test is appropriate. Figure 3 shows an END test being conducted on a specimen of Coconino sandstone. Brazilian disc testing was also conducted on some specimens to determine the tensile strength. Details on the number of specimens tested at each temperature are given in Table 7. Figure 4 shows the results of tests where each specimen was subjected to one cycle of slow heating and rapid cooling prior to either fracture toughness or tensile strength testing. Specimens were heated to either 100, 200 or 300 C. 10 13 END tests were conducted at each

Effect of Rapid Thermal Cooling on Rocks Fig. 4 The effect of temperature on Mode I fracture toughness and tensile strength Fracture toughness (MPam^0.5) 1.000 0.900 0.800 0.700 0.600 0.500 0.400 0.300 0.200 0.100 0.000 25 C 25-100 C 25-200 C 25-300 C No thermal loading 100 deg. 200 deg. 300 deg. Average Tensile Strength (MPa) 8.00 7.00 6.00 5.00 4.00 3.00 2.00 No thermal loading 100 deg. 200 deg. 300 deg. Average 1.00 0.00 25 C 25-100 C 25-200 C 25-300 C temperature to determine K IC, and five Brazilian specimens were tested at each temperature to determine the tensile strength. Error bars (average ± standard deviation) and the average trend line are shown in Fig. 4. The K IC and tensile strength results are consistent in showing a significant drop at 300 C. The fracture toughness decreases from an unheated value of about 0.7 to about 0.6 MPaHm when heated to 300 C. The tensile strength decreases from an unheated value of about 6 MPa to a little less than 5 MPa when heated to 300 C. The K IC results indicate a slight increase in toughness at 100 and 200 C, while the tensile strength results indicate a drop at 100 and 200 C. However, because these trends do not exceed the bounds set by the error bars in Fig. 4, these small trends may not be statistically significant. Additional work was carried out looking at the effects of multiple cycles of slow heating/rapid cooling of Coconino specimens to just 100 C. These results are of interest in several rock engineering applications, including the effect of mining ventilation in deep mines, and the effect of daily and seasonal temperature variations in surface rock slopes and foundations. Cyclic thermal loading was repeated 10, 15 and 20 times, and the results of K IC and Brazilian testing are shown in Fig. 5. Error bars (average ± standard deviation) and the average trend line are shown in Fig. 5. At each step of cyclic thermal loading, 12 and 5 specimens were tested to investigate the fracture toughness and the tensile strength, respectively. Figure 5 shows that after 20 cycles, there is a clear trend of the fracture toughness increasing from 1 to 1.18 MPaHm and a possible trend of the tensile strength decreasing from 6.3 to 6 MPa. The decrease in tensile strength in Fig. 5 is consistent with an increase in crack density due to the rapid cooling (Ferrero and Marini 2001). One possible explanation for the increase in the fracture toughness in Fig. 4 is blunting. Other investigators have shown that microcracks can blunt a macrocrack tip and increase the fracture toughness (Meredith and Atkinson 1985; Balme et al. 2004; Nasseri et al. 2007; Darot et al. 1985; Gordon 1976). 4 Rapid Cooling Effect on Porosity, Seismic Velocity and Tensile Strength in Igneous and Metamorphic Rocks This section describes the results of thermal tests conducted with diabase, quartzite, KVS and skarn cores taken from depths of 1,000 2,000 m. These specimens were

K. Kim et al. Fig. 5 The effect of cyclic thermal loading (100 C) on Mode I fracture toughness and tensile strength Fracture toughness (MPam^0.5) 1.400 1.200 1.000 0.800 0.600 0.400 0.200 No thermal loading 10 cycles 15 cycles 20 cycles Average 0.000 0 10 15 20 Cycles Tensile Strength (MPa) 8.00 7.00 6.00 5.00 4.00 3.00 2.00 No thermal loading 10 cycles 15 cycles 20 cycles Average 1.00 0.00 0 10 15 20 Cycles tested to investigate the possible effects of rapid cooling due to mining ventilation on the stability of underground drifts. Based on a mining depth of 2,000 2,500 m with an expected rock temperature between 80 and 90 C, five thermal loading cycles were applied to the specimens to simulate ventilation stoppages; specimens were slowly heated to 100 C and rapidly cooled to room temperature (about 22 25 C) with a fan. Due to a shortage of specimens available for testing, additional thermal testing with specimens of Sierrita Granite and South Mountain Granite from Arizona were used. Pictures of these different rock types are shown in Fig. 2. Three types of tests were conducted, Brazilian disc tests to determine the tensile strength, seismic velocity tests to determine the P-wave velocity, and porosity tests to determine the void volume change. These tests were conducted after the samples were subjected to five heating/ rapid cooling cycles. END tests for fracture toughness were not conducted on these specimens due to the added complexity of the notch on the thermal stresses, as discussed in the previous section. Details on the number and dimensions of specimens tested are given in Tables 1, 2, 3, 4, 5, and Table 7 compares the testing described in this section (igneous and metamorphic rocks) with the testing described in Sect. 3 (sandstone). Porosity (n) was simply measured by (Bowles 1978; ASTM 2002): n ¼ V V 100 ð%þ; ð1þ V T where V T is the total volume of a specimen and V V is the void volume. Void volume is given by: V V ¼ M sat M dry ðcm 3 Þ ð2þ c w where, c w is the unit weight of water, 0.997 g/cm 3 (in 25 C water temperature). M sat is the saturated surface-dry mass measured by immersing in cold water for more than 48 h and removing the surface moisture with a wet towel.

Effect of Rapid Thermal Cooling on Rocks M dry is the oven-dry mass measured after drying in the oven for more than 48 h. The results are very interesting and revealed two distinct types of behavior. In some of the rock types that were tested, the results after slow heating/rapid cooling cycles are consistent with microcrack initiation and propagation. This includes a decrease in the P-wave velocity, a decrease in the tensile strength, and an increase in the porosity. The rock types that exhibited this behavior included granite, KVS, and the subset of the diabase specimens that contained ore veins. In other rock types that were tested, the results after thermal loading are consistent with crack closing or healing. This included an increase in the P-wave velocity, an increase in the tensile strength, and a decrease in porosity. The rock types that exhibited this behavior included quartzite, skarn and the subset of the diabase specimens that did not include ore veins. Detailed results on the rock types that exhibited crack growth are given in Sect. 4.1, and the results on the rock types that exhibited crack closure are given in Sect. 4.2 Table 2 Average porosity change before and after 5-cyclic thermal loading Rock type Sierrita granite/5 samples (50.8 9 50.8) Diabase (ore vein)/5 samples (50.8 9 50.8) KVS/3 samples (50.8 9 50.8) Before thermal loading (%) After 5-cyclic thermal loading (%) 0.19 0.32 68 0.97 1.56 61 2.64 3.68 39 Increase percentage (%) 4.1 Rock Types that Exhibited Crack Growth After Cyclic Thermal Loading Porosity and seismic testing results using granite, diabase (with ore veins), and KVS specimens showed an increase in crack density after 5 cycles of slow heating/rapid cooling from 100 C. Sierrita granite specimens (14 specimens/50.8 9 38.1 mm) were used for the seismic tests to investigate P-wave velocity change. Due to the shortage of specimens, the seismic tests were not conducted with KVS and diabase. The seismic test results are shown in Fig. 6. The average P-wave velocity decreased from 5.61 to 5.31 km/s, a 5.3 % decrease of P-wave velocity and an indication that the crack density has increased. This increase of crack density was also observed in the porosity (voids volume divided by total volume) tests shown in Table 2. Porosity results for Sierrita granite, diabase (with ore vein) and KVS are shown in Table 2. Porosity results show increases of 68, 61 and 39 % for the granite, diabase and KVS, respectively. The porosity results in Table 2 agree with the seismic results in Fig. 6 indicating an increase in crack density due to rapid thermal cooling for Sierrita Granite. 4.2 Rock Types That Exhibited Crack Healing After Cyclic Thermal Loading Crack healing, or a decrease in crack density, was observed in some of the test results due to cyclic thermal loading. A decrease in crack density could occur due to a residual closing of cracks when subjected to compressive stresses, or a residual thermal strain that can occupy the crack space and thereby reduce the overall crack porosity (Zomeni 1997; Kim and Kemeny 2008). The area of the test specimens that is expected to undergo compression due to rapid Fig. 6 P-wave velocity change before and after 5-cyclic thermal loading 6.50 Sierrita Granite before and after 5 cyclic thermal shock 6.00 Vp (Km/sec) 5.50 5.00 4.50 Before thermal loading After 5 cyclic thermal loading

K. Kim et al. Fig. 7 P-wave velocity change before and after 5-cyclic thermal loading in diabase (no ore veins) 7.00 6.00 Diabase (no ore vein) before and after 5 cyclic thermal loading 5.00 Vp (Km/sec) 4.00 3.00 2.00 1.00 0.00 Before thermal loading After 5 cyclic thermal loading Table 3 Average porosity change before and after 5-cyclic thermal loading Rock type Diabase/3 samples (63.5 9 50.8) Skarn (ore vein)/3 samples (63.5 9 50.8) Quartzite/3 samples (63.5 9 50.8) Before thermal loading (%) After 5-cyclic thermal loading (%) 0.29 0.25 14 5.82 4.10 26 1.58 1.57 1 Decrease percentage (%) cooling is discussed in Sect. 5 on numerical modeling (see Fig. 13). Diabase (without ore veins), quartzite and skarn showed a decrease of crack density after the thermal loading in the seismic, porosity and tensile strength tests. Seismic tests were conducted with only diabase due to the shortage of the specimens, and it shows the increase of average P-wave velocity in all but one specimen (very top points in Fig. 7). The overall results in Fig. 7 show an average increase in P-wave velocity of about 6 %, from 4.36 to 4.61 km/s. It is noted that diabase specimens containing prominent ore veins have shown crack growth after rapid cooling (possibly due to a significant different coefficient of thermal expansion between the host rock and the ore vein) as discussed in Sect. 4.1, but the diabase specimens used in the results shown in Fig. 7 do not contain ore veins. Thus, we see a characteristic difference depending on whether or not the diabase specimens contain ore veins. Crack healing was observed in the porosity tests of diabase as well as skarn and quartzite. Table 3 shows the test results. It is noted that diabase specimens in the porosity test are from the same cores which were used in the above seismic tests. All specimens showed a consistent decrease of porosity and Table 3 shows average porosity decreases of 13.8, 25.7 and 0.6 % for diabase, skarn and quartzite, respectively. An interesting result in the table is that skarn containing ore veins shows the biggest decrease in porosity (possibly due to the large initial porosity counteracting the effect of mismatch in coefficient of thermal expansion). Standard Brazilian disc tests were also conducted to determine the tensile strength with the same specimens used for the porosity tests. The average tensile strength change of each rock type is shown in Fig. 8. Figure 8 shows that the tensile strength increases by 8 28 % in the tests with diabase, quartzite and skarn after five-cyclic thermal loading, and the degree of increase is proportional to the rock strength. The summarized tensile strength test results are shown in Table 4. From the results shown in this section, we see that three kinds of tests (seismic, porosity, and tensile tests) consistently show crack closing or healing in the three rock types. Crack growth during thermal loading is the usual mechanism that has been reported by many investigators (Zomeni 1997; Glamheden and Lindblom 2002; Bellopede et al. 2006; Yavuz et al. 2006; Schön 1996). Crack healing due to transient thermal loading is not commonly observed. Crack healing is most likely due to the areas of compression that occur during rapid cooling, as discussed in Sect. 5. Another possibility is that changes in water saturation due to the thermal loading may be causing changes in the mechanical properties. In other words, the water content could have decreased due to the thermal loading, and this could result in the changes in P-wave velocity, tensile strength and porosity. To investigate this possibility, additional testing was conducted where specimens of diabase, skarn, quartzite, Coconino sandstone and Sierrita granite were fully saturated and the P-wave velocity was measured before and after saturation. The average P-wave

Effect of Rapid Thermal Cooling on Rocks Fig. 8 Average tensile strength change before and after 5-cyclic thermal loading 12.00 11.00 Diabase Quartzite Tensile Strength (MPa) 10.00 9.00 8.00 7.00 6.00 5.00 Skarn 4.00 Before thermal loading After 5 cyclic thermal loading Table 4 Average tensile strength before and after 5-cyclic thermal loading Rock type Diabase/10 samples (50.8 9 25.4) Quartzite/11 samples (50.8 9 25.4) Skarn/9 samples (50.8 9 25.4) Table 5 Average P-wave velocity before and after saturation Rock type Diabase/3 samples (63.5 9 38.1) Skarn/3 samples (63.5 9 38.1) Quartzite/2 samples (63.5 9 38.1) Sandstone/10 samples (50.8 9 50.8) Sierrita granite/14 samples (50.8 9 25.4) Before thermal loading (MPa) After 5-cyclic thermal loading (MPa) 8.02 9.30 16 8.70 11.12 28 6.04 6.51 8 Before saturation (km/s) 3.81 4.52 4.26 4.32 4.10 4.60 3.10 3.64 5.60 5.89 Increase percentage (%) After saturation (km/s) velocities before and after full saturation of the specimens are shown in Table 5. Due to the shortage of specimens from some rock types, only 2 3 specimens are used for diabase, skarn and quartzite, whereas 10 14 specimens are used for Coconino sandstone and Sierrita granite. The results in Table 5 are very consistent in showing increases in P-wave velocity for all rock types due to saturation. This is also in agreement with other researchers (Schön 1996). Thus, based on the results shown in Table 5, the possible loss of saturation during the thermal tests cannot explain the apparent crack healing (velocity increase) that is observed, since loss of saturation after heat treatment would cause P-wave velocities to decrease, not increase. 5 Three-Dimensional Transient Thermo-Mechanical Modeling This section describes the simulation of the rapid cooling experiments using the ANSYS 3D finite element program (Srinivas et al. 2010). A three-dimensional finite element mesh of a 2-in. diameter by 2-in. thick specimen has been created and subjected to the boundary conditions shown in Fig. 9a. At time t = 0 the specimen is assumed to be at a uniform temperature of 100 C. It is noted that the ANSYS model used in this analysis does not include cracks. To determine whether a crack of a given size will grow, the stresses from the model at different locations are input into a simple fracture mechanics model, as described later in this section. To simulate rapid cooling after the specimen is removed from the oven and placed on the steel table, airflow convection boundary conditions are applied to the sides and top of the specimen and conduction is applied to the bottom of the specimen, as shown in Fig. 9a. Air flow traveling from the left to the right of the specimen with a velocity of 10 m/s is assumed, resulting in a convective film coefficient that varies with position around the sides and top of the specimen, as shown in Fig. 10. The thermal and mechanical properties for a hard rock such as granite have been assumed, as given in Table 6. It is noted that the air velocity in Table 6 was used to estimate the Reynolds number and the Nusselt number. Based on the properties of air (kinematic viscosity, Prandtl s number) and an air

K. Kim et al. Fig. 9 a Boundary conditions for the ANSYS simulations, b locations referred to in Figs. 11 and 13 Fig. 10 Assumed film coefficient for various places around the specimen velocity of 10 m/s across a 50-mm cylinder, a Reynolds number of 33,000 and an average Nusselt s number of 107 were calculated. Also, the variable film coefficient shown in Fig. 10 uses a basis value of 100 W/m 2 K (multiplier = 1). The results for temperature versus time are shown in Figs. 11 and 12. Figure 11 shows plots of temperature versus time at a number of different locations around and inside the three-dimensional specimen (refer to Fig. 9b for the location of the different lines on the graphs).

Effect of Rapid Thermal Cooling on Rocks Table 6 The thermal and mechanical properties used in the ANSYS simulations Properties Values Air velocity (m/s) 10 Diameter (m) 0.0508 Height (m) 0.058 Elastic modulus (Mpa) 55 Poisson s ratio 0.25 CTE (coefficient of thermal expansion) 3.57E-06 Conductivity (W/m K) 0.972 Specific heat (J/kg K) 1,058 Density (kg/m 3 ) 2,700 Ambient temp. ( C) 25 Initial rock temp. ( C) 100 Fig. 12 Distribution of temperature ( C) at 105 s Fig. 11 Temperature ( C) versus time for various places in the specimen (refer to Fig. 9b) Figure 11 shows that the most rapid cooling occurs at the front-bottom and front-top locations, and the least rapid cooling occurs at the center-middle location, as expected. The generation of thermal stresses is driven by Fig. 13 Maximum principal stress (MPa) versus time for various places in the specimen (refer to Fig. 9b) the transient distribution of temperatures within the specimen, and Fig. 11a shows that the largest temperature change, and thus the largest thermal stresses, occurs at around 100 s. At 100 s the temperature at the center of the specimen is still above 98 C while the temperature at the

K. Kim et al. Fig. 14 Distribution of maximum principal stress (MPa) at 105 s front-bottom has cooled to about 42 C. Figure 12 shows the three-dimensional temperature distribution at 105 s. It shows rapid cooling at the side and top boundaries, particularly the top and bottom corners of the specimen. The results for maximum principal stress versus time are shown in Figs. 13 and 14. Figure 13 shows plots of maximum principal stress versus time at a number of different locations around and inside the three-dimensional specimen (refer to Fig. 9b for the location of the different lines on the graphs). Figure 13 shows that tensile stresses are occurring on the outside of the specimen and compressive stresses are occurring in the center of the specimen. The maximum tensile stresses are occurring at around 100 s, and Fig. 13 shows that at two locations, the front-middle and back-middle locations, the tension at 100 s exceeds 7 MPa. Figure 14 shows the three-dimensional distribution of maximum principal stresses at 105 s. It shows that at 105 s, the zone of tension is a thin skin with a thickness of 0.2 0.3 in. (5.1 7.6 mm). The zone of tension that exceeds 5 MPa is very thin, with a thickness of 5 mm or less. The thermal stress results presented in Figs. 13, 14 support the experimental results. In general, the ANSYS results show that in the first 5 min or so of rapid cooling, a thin zone of high tensile stresses (above 6 MPa) are occurring on the outside of the specimen, and a core of compression is occurring near in the center portion of the specimen. Figure 13 shows that tensile stresses above 6 MPa are occurring in some locations for 5 min. Based on fracture mechanics, for a crack of length 2a subjected to a tensile stress r, the Mode I stress intensity factor is given by (Kundu 2008): p K I ¼ r ffiffiffiffiffi pa : ð3þ and the crack velocity due to subcritical crack growth is given by: Crack velocity ¼ A K n I : ð4þ K IC where K IC is the fracture toughness and A and n are subcritical crack growth properties. For Coconino sandstone, using the K IC value of 0.7 MPaHm from Fig. 4 and A and n values of 0.018 m/s and 36 from Ko and Kemeny (2011), and assuming a tensile stress of 6.5 MPa is applied to a 4-mm-long crack for 5 min, the equation above predicts an increase in crack length of about 2.1 %. Even though this is small, the results indicate that some tensile cracking at the outside of the specimen could occur in rocks that contain microcracks with lengths on the order of millimeters, as would be expected in granite, sandstone and other similar rocks. For fine-grained volcanic or igneous rocks with microcracks on the order of 0.1 mm, crack growth would not be expected. For example, using the same properties but considering a 0.4 mm rather than a 4 mm crack length, the increase in crack length predicted from subcritical crack growth is only 2 9 10-18 %. This demonstrates that the smaller cracks in fine-grained rocks are not expected to grow, but this result is only approximate since the actual K IC, A and n values for the fine-grained rocks are not being used. Also, this assumes that the K IC for the 4 and 0.4 mm cracks are the same, which may not be the case. The compressive stresses in the center of the specimen are expected to result in crack closure. From fracture mechanics, the closure at the center of a crack of length 2a under a compressive stress r is given by Kundu (2008): Crack closure ¼ 4ra E : ð5þ Figure 14 shows that compressive stresses on the order of 2.5 MPa are occurring in the center of the specimen. Assuming a 4-mm crack under a stress of 2.5 MPa and using the E for Coconino sandstone from Ko and Kemeny (2011) of 24 GPa, the equation above predicts a crack closure of about 8 9 10-7 m. Again, even though this is a very small displacement, it would be occurring in many cracks in the region subjected to compression and is expected to result in some crack healing based on Meglis et al. (1996) and others. The general interpretation is that in the case of sedimentary and coarser grained igneous rocks, there is a thin zone of microcracking on the outside of the specimen and a thick zone of crack closure at the center of the specimen. In the case of fine-grained rocks, the zone of microcracking would not exist. The P-wave velocity tests measure wave propagation from the top to the bottom of the specimen, and thus the wave speed is a measure of the average effective elastic properties through both the regions subjected to tension and compression. Similarly, the porosity tests measure the average porosity through the specimen, including the sections subjected to tensile and compressive stresses.

Effect of Rapid Thermal Cooling on Rocks Table 7 Average property changes before and after various thermal loadings (summary of test results) Sandstone/various thermal loadings Various temperatures (100, 200, 300 C) Heat treatment Mode 1 fracture toughness (MpaHm) Tensile strength (Mpa) No thermal loading 0.714 (13 samples) 5.87 (5 samples) Crack growth (blunting) 25 100 C 0.777 (12 samples) 5.16 (5 samples) Crack growth (blunting) 25 200 C 0.751 (12 samples) 5.18 (5 samples) Crack growth 25 300 C 0.623 (10 samples) 4.84 (5 samples) Sandstone/various thermal loadings Various cyclic thermal loading (25 100 C) Heat treatment Mode 1 fracture toughness (MpaHm) Tensile strength (Mpa) No thermal loading 0.996 (12 samples) 6.36 (5 samples) Crack healing (compaction) 10 cycles (25 100 C) 1.029 (12 samples) 6.77 (5 samples) Crack growth 15 cycles (25 100 C) 0.978 (12 samples) 5.97 (5 samples) Crack growth (blunting) 20 cycles (25 100 C) 1.168 (12 samples) 5.89 (5 samples) Various rock types/5-cyclic thermal loading (25 100 C) Rock type Rock property Porosity (ave. change %) crack healing ;/crack growth ; Tensile strength (ave. change %) crack healing ;/crack growth; Seismic velocity (ave. change %) crack healing ;/crack growth ; Crack healing Skarn Quartzite Diabase Crack growth Granite KVS Diabase (with ore vein) 26 % decrease (3 samples) (5.82 4.10 %) 1 % decrease (3 samples) (1.58 1.57 %) 14 % decrease (3 samples) (0.29 0.25 %) 68 % increase (5 samples) (0.19 0.32 %) 39 % increase (3 samples) (2.64 3.68 %) 61 % increase (5 samples) (0.97 1.56 %) 8 % increase (9 samples) (6.04 6.51 Mpa) 28 % increase (11 samples) (8.70 11.12 Mpa) 16 % increase (10 samples) (8.02 9.30 Mpa 6 % increase (6 samples) (4.36 4.61 km/s) 5 % decrease (14 samples) (5.61 5.31 km/s) 6 Summary and Conclusions A set of laboratory experiments and 3D numerical modeling was conducted, looking at the effects of rapid thermal cooling on mechanical properties. Rapid thermal cooling occurs in several important mining and geotechnical engineering applications, including the ventilation of mines at deep depth and deep drilling. Tests were conducted by slowly heating specimens of granite, sandstone and other rocks in an oven, followed by rapid cooling with a fan. Specimens were cooled from oven temperatures of 100, 200 and 300 C, and tested to evaluate the changes in mechanical properties that included END tests to determine the fracture toughness, Brazilian disc tests to determine the tensile strength, and P-wave velocity and porosity tests. The experimental results showed that rapid cooling can result in significant changes in rock properties. Not surprisingly, rapid cooling from 300 C to room temperature resulted in significant reductions in both the fracture toughness and the tensile strength. More importantly and more surprisingly, the results demonstrated that rapid cooling with low to moderate temperature changes can result in measurable changes in mechanical properties with two very different types of behavior depending on the rock type. In some of the rock types that were tested, the 100 C rapid cooling results were consistent with microcrack initiation and propagation. This includes a decrease in P-wave velocity, a decrease in tensile strength, and an increase in porosity. In other rock types that were tested, the 100 C rapid cooling results were consistent with microcrack

K. Kim et al. closing and crack healing. This includes an increase in P-wave velocity, increase in tensile strength, and decrease in porosity. The complete set of laboratory test results from this study is shown in Table 7. The results were explained by a 3D thermo-mechanical modeling using the ANSYS finite element program. The rapid cooling of a 2-in. (50.8 mm) diameter disc due to blowing air was simulated, and the results indicated that within the first 5 min of rapid cooling, there is a thin (less than 5 mm) region near the outside of the specimen where large tensile stresses (above 6 MPa) occur and microcracking might be expected. During the same short time period, there is a large area in the middle of the specimen where lower magnitude compressive stresses occur and crack closure would be expected. In the more heterogeneous and coarse-grained rocks that were tested, it was shown that time-dependent crack growth could occur on the outside of the specimen and dominate any closure occurring on the inside of the specimen, resulting in an overall increase in porosity, decrease in P-wave velocity, etc. In the less heterogeneous and finegrained rocks tested, it was shown that tension cracking on the outside could not occur, while crack closure on the inside could still occur, resulting in an overall decrease in porosity, increase in P-wave velocity, etc. Many of the tests conducted in this study involved up to 20 cycles of slow heating and rapid cooling. Since material fatigue is concerned with the behavior of materials under cyclic loading, it is likely that analyzing the results in terms of fatigue theory would be useful. Also it is noted that thermal fatigue in rocks has been investigated by Spagnoli et al. (2011), Li et al. (1992), Migliazza et al. (2011) and Ferrero et al. (2009). In this study, we chose to utilize subcritical crack growth theory to analyze and interpret the test results. The authors have experience with subcritical crack growth, and the subcritical crack growth properties for one of the tested rock types (Coconino sandstone) have been determined by one of the authors. We also note that microscopy could have been very helpful in interpreting the results from this study, particularly the rocks that showed crack healing after thermal loading. Microscopy such as in the studies by Leiss and Weiss (2000) and Royer-Carfagni (1999) would be utilized in future studies on the effects of rapid thermal cooling on rock fracturing. Acknowledgments This work is supported by Rio Tinto s Resolution Copper Company. References ASTM C 642 (2002) Standard test method for density, absorption, and voids in hardened concrete. Annual book of ASTM standards, American Society for Testing and Materials, Philadelphia, vol 04.02 Balme MR, Rocchi V, Jones C, Sammonds PR, Meredith PG, Boon S (2004) Fracture toughness measurements on igneous rocks using a high-pressure, high-temperature rock fracture mechanics cell. J Volcanol Geotherm Res 132:159 172 Bellopede R, Ferrero AM, Manfredotti L, Marini P, Migliazza M (2006) The effect of thermal stresses on the mechanical behavior of natural building stones. Fracture and failure of natural building stones, Part II. pp 397 425 Bowles JE (1978) Engineering properties of soils and their measurement, 2nd edn. McGraw-Hill, New York, pp 1 60 Darot M, Gueguen Y, Benchemam Z, Gaboriaud R (1985) Ductilebrittle transition investigated by micro-indentation: results for quartz and olivine. Phys Earth Planet Inter 40:180 186 Donovan JG (2006) Fracture toughness based models for the prediction of power consumption, product size, and capacity of jaw crushers. Doctor of philosophy dissertation, Mining and Mineral Engineering, Virginia Tech, Blacksburg Ferrero AM, Marini P (2001) Experimental studies on mechanical behavior of two thermal cracked marbles. Rock Mech Rock Eng 34(1):57 66 Ferrero AM, Migliazza M, Spagnoli A (2009) Theoretical modeling of bowing in cracked marble slabs under cyclic thermal loading. Constr Build Mater 23:2151 2159 Glamheden R, Lindblom U (2002) Thermal and mechanical behavior of refrigerated caverns in hard rock. Tunn Undergr Space Technol 17(4):341 353 Gordon JE (1976) The new science of strong materials, 2nd edn. Penguin, Harmondsworth, p 287 Kemeny J, Apted M, Martin D (2006) Rockfall at Yucca Mountain due to thermal, seismic, and time-dependence. In: Proceedings of international high level radioactive waste management conference, Las Vegas, NV Kim KM, Kemeny J (2008) Effect of thermal loading on compressional wave velocity, Mode I fracture toughness and tensile strength. 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