CN101602597A - Zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material and preparation method thereof - Google Patents
Zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material and preparation method thereof Download PDFInfo
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Abstract
Zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material and preparation method thereof, it relates to ceramic matric composite and preparation method thereof.It has solved existing ZrB
2The problem that poor, the critical temperature difference of the thermal shock resistance of ultra-temperature ceramic-based composite material is low, intensity is high, fracture toughness property is low and critical crack size is low.Zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is made by zirconium boride 99.5004323A8ure powder, silicon carbide powder and carbon black powders.Method: one, take by weighing after the raw material wet mixing slurry; Two, grind after the slurry oven dry mixed powder; Three, mixed powder sintering postcooling takes out promptly.The thermal shock resistance of material is good among the present invention, and its critical temperature difference is 470～1000 ℃, and intensity is 132.03～695.54MPa, and fracture toughness property is 2.01～6.57MPam
1/2, critical crack size is 65.9～249.9 μ m.
Description
Technical field
The present invention relates to ceramic matric composite and preparation method thereof.
Background technology
Zirconium diboride (ZrB
2) pottery is because have good, good neutron controllability of high-melting-point, high rigidity, electrical and thermal conductivity and excellent chemical stability, become the high temperature resistant structure ceramics of tool advantage, reentered, stride at hypersonic flight, atmospheric layer and have a wide range of applications in the extreme environments such as aerial flight and rocket propulsion system; But ZrB
2The thermal shock resistance of ultra-temperature ceramic-based composite material is poor, shows that the critical temperature difference only is 350 ℃ (thermal shock resistance of the high more material of the critical temperature difference is good more), and 70% sample lost efficacy when the critical temperature difference is higher than 400 ℃, i.e. thermal shock cracking; Also show ZrB
2The intensity of ultra-temperature ceramic-based composite material is lower than 5.0MPam usually above 800MPa, fracture toughness property
1/2, cause the critical crack size of material to be lower than 39 μ m[critical crack sizes and can pass through Griffith fracture theory formula
Quantitative calculation is come out, and wherein σ is intensity and K
ICBe fracture toughness property], and ZrB
2Ultra-temperature ceramic-based composite material make and the course of processing in inevitably introduce impurity, can produce defectives such as tiny crack, when material being subjected to high temperature difference or high hot-fluid suddenly ballistic the time, catastrophic destruction can be taken place, cause ZrB
2The inefficacy of base ceramic base composite material member.
Summary of the invention
The present invention seeks in order to solve existing ZrB
2The problem that poor, the critical temperature difference of the thermal shock resistance of ultra-temperature ceramic-based composite material is low, intensity is high, fracture toughness property is low and critical crack size is low, and zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material and preparation method thereof is provided.
Zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is made by 50%～75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5%～30% carbon black powders by volume; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98%, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98%, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98%, and particle diameter is 40～100nm.
The preparation method of zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 50%～75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5%～30% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1850～1950 ℃, pressure are heat preservation sintering 45～75min under the argon gas atmosphere of 25～40MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
The micro-nano carbon black particle that adds among the present invention enters tiny crack and weak interface combination, makes the fracture toughness property of material raise and the intensity reduction, has improved the critical crack size of material, promptly helps improving the shock resistance of material; Comparing of zirconium boride-carborundum among the present invention-carbon black ternary high-toughness ultra-temperature ceramic-based composite material with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites, raw materials cost has reduced by 5%～30%, density has reduced by 4%～25%, the weight of material has reduced, and is more suitable for being applied to aerospace field; The thermal shock resistance of zirconium boride-carborundum among the present invention-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is good, and its critical temperature difference is 470～1000 ℃, and intensity is 132.03～695.54MPa, and fracture toughness property is 2.01～6.57MPam
1/2, critical crack size is 65.9～249.9 μ m.
Embodiment
Embodiment one: present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is made by 50%～75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5%～30% carbon black powders by volume; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98%, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98%, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98%, and particle diameter is 40～100nm.
Embodiment two: present embodiment and embodiment one are different is that zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is made by 58% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 22% carbon black powders by volume.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is that zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is made by 65% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 15% carbon black powders by volume.Other is identical with embodiment one.
Embodiment four: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 50%～75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5%～30% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1850～1950 ℃, pressure are heat preservation sintering 45～75min under the argon gas atmosphere of 25～40MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Embodiment five: present embodiment and embodiment four are different is to take by weighing 55% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 25% carbon black powders in the step 1 by volume.Other step and parameter are identical with embodiment four.
Embodiment six: present embodiment and embodiment four are different is to take by weighing 60% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 20% carbon black powders in the step 1 by volume.Other step and parameter are identical with embodiment four.
Embodiment seven: present embodiment and embodiment four are different is to take by weighing 70% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 10% carbon black powders in the step 1 by volume.Other step and parameter are identical with embodiment four.
Embodiment eight: what present embodiment and embodiment four, five, six or seven were different is that planetary ball mill is adopted in the ball milling wet mixing in the step 1, dispersion agent is a dehydrated alcohol, drum's speed of rotation is 200～400r/min, and abrading-ball zirconium oxide balls, ratio of grinding media to material are 4: 1.Other step and parameter are identical with embodiment four, five, six or seven.
Embodiment nine: present embodiment and embodiment eight are different is that the temperature of evaporation oven dry in the step 2 is 65 ℃.Other step and parameter are identical with embodiment eight.
Embodiment ten: what present embodiment and embodiment nine were different is to grind in the step 2 to adopt agate mortar to grind repeatedly.Other step and parameter are identical with embodiment nine.
Embodiment 11: present embodiment and embodiment ten are different is that in the step 3 mixed powder to be placed temperature be that 1850 ℃, sintering pressure are heat preservation sintering 75min under the argon gas atmosphere of 40MPa.Other step and parameter are identical with embodiment ten.
Embodiment 12: present embodiment and embodiment ten are different is that in the step 3 mixed powder to be placed temperature be that 1950 ℃, sintering pressure are heat preservation sintering 45min under the argon gas atmosphere of 25MPa.Other step and parameter are identical with embodiment ten.
Embodiment 13: present embodiment and embodiment ten are different is that in the step 3 mixed powder to be placed temperature be that 1900 ℃, sintering pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa.Other step and parameter are identical with embodiment ten.
Embodiment 14: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1900 ℃, pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material cuts into the sample (three-point bending method) of 36mm * 4mm * 3mm or the sample of 22mm * 4mm * 2mm (single notched beam method) in the present embodiment, and after specimen surface carried out polished finish, carry out Micro-Structure Analysis and Mechanics Performance Testing; Micro-Structure Analysis: from the microstructure observation of sample, carbon black granules is evenly distributed in the matrix as can be seen; Mechanics Performance Testing: the result is as shown in table 1, and the critical temperature difference height of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, intensity is low, fracture toughness property is high and critical crack size is high, and material property is good.
Table 1
| Intensity/MPa | Fracture toughness property/MPam 1/2 | Critical crack size/μ m | The critical temperature difference/℃ |
| 415.55 | 6.57 | 249.9 | 485 |
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, test through the shrend thermal shock test, the result as shown in fig. 1, material is keeping the high remaining rate of the complete sum flexural strength of structure under the thermal shocking temperature difference, the thermal shock resistance of material has improved significantly.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is compared with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites in the present embodiment, raw materials cost approximately reduced by 5% and density approximately reduced by 4%.
Embodiment 15: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 70% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 10% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1900 ℃, pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material cuts into the sample (three-point bending method) of 36mm * 4mm * 3mm or the sample of 22mm * 4mm * 2mm (single notched beam method) in the present embodiment, and after specimen surface carried out polished finish, carry out Micro-Structure Analysis and Mechanics Performance Testing; Micro-Structure Analysis: from the microstructure observation of sample, carbon black granules is evenly distributed in the matrix as can be seen; Mechanics Performance Testing: the result is as shown in table 2, and the critical temperature difference height of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, intensity is low, fracture toughness property is high and critical crack size is high, and material property is good.
Table 2
| Intensity/MPa | Fracture toughness property/MPam 1/2 | Critical crack size/μ m | The critical temperature difference/℃ |
| 695.54 | 5.65 | 65.9 | 470 |
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, test through the shrend thermal shock test, the result as shown in Figure 2, material is keeping the high remaining rate of the complete sum flexural strength of structure under the thermal shocking temperature difference, the thermal shock resistance of material has improved significantly.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is compared with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites in the present embodiment, raw materials cost approximately reduced by 10% and density approximately reduced by 8%.
Embodiment 16: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 65% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 15% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1900 ℃, pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material cuts into the sample (three-point bending method) of 36mm * 4mm * 3mm or the sample of 22mm * 4mm * 2mm (single notched beam method) in the present embodiment, and after specimen surface carried out polished finish, carry out Micro-Structure Analysis and Mechanics Performance Testing; Micro-Structure Analysis: from the microstructure observation of sample, carbon black granules is evenly distributed in the matrix as can be seen; Mechanics Performance Testing: the result is as shown in table 3, and the critical temperature difference height of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, intensity is low, fracture toughness property is high and critical crack size is high, and material property is good.
Table 3
| Intensity/MPa | Fracture toughness property/MPam 1/2 | Critical crack size/μ m | The critical temperature difference/℃ |
| 499.93 | 4.78 | 91.4 | 490 |
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, test through the shrend thermal shock test, the result as shown in Figure 3, material is keeping the high remaining rate of the complete sum flexural strength of structure under the thermal shocking temperature difference, the thermal shock resistance of material has improved significantly.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is compared with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites in the present embodiment, raw materials cost approximately reduced by 15% and density approximately reduced by 12%.
Embodiment 17: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 60% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 20% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1900 ℃, pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material cuts into the sample (three-point bending method) of 36mm * 4mm * 3mm or the sample of 22mm * 4mm * 2mm (single notched beam method) in the present embodiment, and after specimen surface carried out polished finish, carry out Micro-Structure Analysis and Mechanics Performance Testing; Micro-Structure Analysis: from the microstructure observation of sample, carbon black granules is evenly distributed in the matrix as can be seen; Mechanics Performance Testing: the result is as shown in table 4, and the critical temperature difference height of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, intensity is low, fracture toughness property is high and critical crack size is high, and material property is good.
Table 4
| Intensity/MPa | Fracture toughness property/MPam 1/2 | Critical crack size/μ m | The critical temperature difference/℃ |
| 265.95 | 3.25 | 149.3 | 825 |
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, test through the shrend thermal shock test, the result as shown in Figure 4, material is keeping the high remaining rate of the complete sum flexural strength of structure under the thermal shocking temperature difference, the thermal shock resistance of material has improved significantly.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is compared with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites in the present embodiment, raw materials cost approximately reduced by 20% and density approximately reduced by 16%.
Embodiment 18: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 55% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 25% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1900 ℃, pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material cuts into the sample (three-point bending method) of 36mm * 4mm * 3mm or the sample of 22mm * 4mm * 2mm (single notched beam method) in the present embodiment, and after specimen surface carried out polished finish, carry out Micro-Structure Analysis and Mechanics Performance Testing; Micro-Structure Analysis: from the microstructure observation of sample, carbon black granules is evenly distributed in the matrix as can be seen; Mechanics Performance Testing: the result is as shown in table 5, and the critical temperature difference height of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, intensity is low, fracture toughness property is high and critical crack size is high, and material property is good.
Table 5
| Intensity/MPa | Fracture toughness property/MPam 1/2 | Critical crack size/μ m | The critical temperature difference/℃ |
| 232.13 | 2.81 | 146.5 | 910 |
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, test through the shrend thermal shock test, the result as shown in Figure 5, material is keeping the high remaining rate of the complete sum flexural strength of structure under the thermal shocking temperature difference, the thermal shock resistance of material has improved significantly.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is compared with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites in the present embodiment, raw materials cost approximately reduced by 25% and density approximately reduced by 21%.
Embodiment 19: the preparation method of present embodiment zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 50% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 30% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1900 ℃, pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material cuts into the sample (three-point bending method) of 36mm * 4mm * 3mm or the sample of 22mm * 4mm * 2mm (single notched beam method) in the present embodiment, and after specimen surface carried out polished finish, carry out Micro-Structure Analysis and Mechanics Performance Testing; Micro-Structure Analysis: from the microstructure observation of sample, carbon black granules is evenly distributed in the matrix as can be seen; Mechanics Performance Testing: the result is as shown in table 6, and the critical temperature difference height of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, intensity is low, fracture toughness property is high and critical crack size is high, and material property is good.
Table 6
| Intensity/MPa | Fracture toughness property/MPam 1/2 | Critical crack size/μ m | The critical temperature difference/℃ |
| 132.03 | 2.01 | 231.7. | ＞1000 |
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the present embodiment, test through the shrend thermal shock test, the result as shown in Figure 6, material is keeping the high remaining rate of the complete sum flexural strength of structure under the thermal shocking temperature difference, the thermal shock resistance of material has improved significantly.
Gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is compared with zirconium boride 99.5004323A8ure/20vol% silicon carbide ceramic of compact based composites in the present embodiment, raw materials cost approximately reduced by 30% and density approximately reduced by 25%.
Description of drawings
Fig. 1 is the thermal shock resistance properties spectrogram of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the embodiment 14; Fig. 2 is the thermal shock resistance properties spectrogram of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the embodiment 15; Fig. 3 is the thermal shock resistance properties spectrogram of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the embodiment 16; Fig. 4 is the thermal shock resistance properties spectrogram of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the embodiment 17; Fig. 5 is the thermal shock resistance properties spectrogram of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the embodiment 18; Fig. 6 is the thermal shock resistance properties spectrogram of gained zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material in the embodiment 19.
Claims (10)
1, zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is characterized in that zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material made by 50%～75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5%～30% carbon black powders by volume; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98%, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98%, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98%, and particle diameter is 40～100nm.
2, zirconium boride-carborundum according to claim 1-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is characterized in that zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material made by 58% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 22% carbon black powders by volume.
3, zirconium boride-carborundum according to claim 1-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is characterized in that zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material made by 65% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 15% carbon black powders by volume.
4, prepare the method for zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material according to claim 1, the preparation method who it is characterized in that zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material carries out according to the following steps: one, take by weighing 50%～75% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 5%～30% carbon black powders by volume, after the ball milling wet mixing slurry; Two, slurry evaporates oven dry on rotatory evaporator, grinds then, gets mixed powder; Three, mixed powder being placed temperature is that 1850～1950 ℃, pressure are heat preservation sintering 45～75min under the argon gas atmosphere of 25～40MPa, takes out behind the furnace cooling, promptly gets zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite material; Wherein the bulk purity of zirconium boride 99.5004323A8ure powder is greater than 98% in the step 1, and particle diameter is 2 μ m; The bulk purity of silicon carbide powder is greater than 98% in the step 1, and particle diameter is 1 μ m; The bulk purity of carbon black powders is greater than 98% in the step 1, and particle diameter is 40～100nm.
5, the preparation method of zirconium boride-carborundum according to claim 4-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is characterized in that taking by weighing by volume in the step 1 55% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 25% carbon black powders.
6, the preparation method of zirconium boride-carborundum according to claim 4-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is characterized in that taking by weighing by volume in the step 1 60% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 20% carbon black powders.
7, the preparation method of zirconium boride-carborundum according to claim 4-carbon black ternary high-toughness ultra-temperature ceramic-based composite material is characterized in that taking by weighing by volume in the step 1 70% zirconium boride 99.5004323A8ure powder, 20% silicon carbide powder and 10% carbon black powders.
8, according to the preparation method of claim 4,5,6 or 7 described zirconium boride-carborundum-carbon black ternary high-toughness ultra-temperature ceramic-based composite materials, it is characterized in that planetary ball mill is adopted in the ball milling wet mixing in the step 1, dispersion agent is a dehydrated alcohol, drum's speed of rotation is 200～400r/min, abrading-ball zirconium oxide balls, ratio of grinding media to material are 4: 1.
9, the preparation method of zirconium boride-carborundum according to claim 8-carbon black ternary high-toughness ultra-temperature ceramic-based composite material, it is characterized in that in the step 3 mixed powder placed temperature is that 1850 ℃, sintering pressure are heat preservation sintering 75min under the argon gas atmosphere of 40MPa.
10, the preparation method of zirconium boride-carborundum according to claim 8-carbon black ternary high-toughness ultra-temperature ceramic-based composite material, it is characterized in that in the step 3 mixed powder placed temperature is that 1900 ℃, sintering pressure are heat preservation sintering 60min under the argon gas atmosphere of 30MPa.
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