CN101250061A - Zirconia toughened boride ultra-temperature ceramic-based composite material and preparation thereof - Google Patents
Zirconia toughened boride ultra-temperature ceramic-based composite material and preparation thereof Download PDFInfo
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- CN101250061A CN101250061A CNA2008100642046A CN200810064204A CN101250061A CN 101250061 A CN101250061 A CN 101250061A CN A2008100642046 A CNA2008100642046 A CN A2008100642046A CN 200810064204 A CN200810064204 A CN 200810064204A CN 101250061 A CN101250061 A CN 101250061A
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Abstract
The invention relates to a zirconia toughening boride superhight temperature ceramic base composite material and a relative preparation method, which resolves the low toughness problem of prior boride superhigh temperature ceramic composite material. The inventive zirconia toughening boride superhight temperature ceramic base composite material is prepared from boride powder, silicon carbide particles and yttria partially stabilized zirconia particles. The preparation method comprises 1, mixing boride powder, silicon carbide particles and yttria partially stabilized zirconia particles, 2, washing the mixture via ultrasonic wave, ball grinding, mixing and drying, 3, sintering the dried mixture at held temperature, cooling to room temperature and taking off to obtain the zirconia toughening boride superhight temperature ceramic base composite material. The invention has simple preparation and low cost, while the product toughness can reach 6.0-6.8MPam<1/2>.
Description
Technical field
The present invention relates to a kind of boride ultra-temperature ceramic-based composite material and preparation method thereof.
Background technology
Boride has high-melting-point, high heat conductance, high conductivity, good chemical stability and thermal shock resistance; At present with ZrB
2-SiC is the boride ultra-temperature stupalith system of representative, has been subjected to paying close attention to of international numerous scholars, but the problem of its poor toughness fails to be well solved always, and toughness value only is 4～5MPam
1/2, limited giving full play to of material property to a great extent.
Summary of the invention
The present invention seeks in order to solve the problem of existing boride ultra-temperature ceramic-based composite material poor toughness, and a kind of Zirconia toughened boride ultra-temperature ceramic-based composite material and preparation method thereof is provided.
Zirconia toughened boride ultra-temperature ceramic-based composite material of the present invention by volume per-cent is made by 70%～80% boride powder, 0～10% silicon-carbide particle and 10%～30% yttrium oxide PSZ particle; Wherein contain yttrium oxide 2mol%～3mol% in the yttrium oxide PSZ particle; Boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
The method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material realizes according to the following steps: one, by total composite volume than 70%～80% boride powder, 0～10% silicon-carbide particle and 10%～30% yttrium oxide PSZ particle are mixed; Two, mixture is put into dehydrated alcohol and carried out ultrasonic cleaning, carry out ball milling in the ball mill of packing into then and mix, mix back gained slurry and dry again; Three, the mixture after will drying places sintering oven, in sintering atmosphere is vacuum or inert atmosphere, is warmed up to 1750～1850 ℃ with the speed of 10～30 ℃/min, insulation 30～90min, be cooled to room temperature and take out, promptly get Zirconia toughened boride ultra-temperature ceramic-based composite material; Contain yttrium oxide 2mol%～3mol% in the used yttrium oxide PSZ of step 1; The used boride powder of step 1 is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
The present invention is incorporated into the yttrium oxide PSZ in the boride ultra-temperature ceramic-based material system, to improve its toughness, obtain Zirconia toughened boride ultra-temperature ceramic-based composite material, tetragonal phase zirconium oxide can take place in the time of 950 ℃ in the material application process to be changed to the monocline phase zircite, in addition, material is done the time spent being subjected to load because the effect of internal stress, can take place equally the four directions in opposite directions monocline change mutually; This phase transformation meeting produces 3%～5% volumetric expansion, in crack propagation process, makes that a part of strain energy is consumed, and delays crack propagation, thereby improves the fracture toughness property of material.Preparation technology of the present invention is simple, cost is low, the gained Zirconia toughened boride ultra-temperature ceramic-based composite material, and its toughness value is up to 6.0～6.8MPam
1/2, and bending strength all is higher than 770MPa, just says that also the intensity that does not have material in toughness reinforcing causes adverse influence, is more suitable for being used for the termination parts of superelevation velocity of sound aircraft.
Embodiment
Embodiment one: present embodiment Zirconia toughened boride ultra-temperature ceramic-based composite material by volume per-cent is made by 70%～80% boride powder, 0～10% silicon-carbide particle and 10%～30% yttrium oxide PSZ particle; Wherein contain yttrium oxide 2mol%～3mol% in the yttrium oxide PSZ particle; Boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
Embodiment two: present embodiment and embodiment one be not both Zirconia toughened boride ultra-temperature ceramic-based composite material by volume per-cent make by 70% boride powder, 10% silicon-carbide particle and 20% yttrium oxide PSZ particle.Other is identical with embodiment one.
Embodiment three: not being both in the yttrium oxide PSZ particle of present embodiment and embodiment one contains yttrium oxide 3mol%.Other is identical with embodiment one.
Embodiment four: the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material realizes according to the following steps: one, by total composite volume than 70%～80% boride powder, 0～10% silicon-carbide particle and 10%～30% yttrium oxide PSZ particle are mixed; Two, mixture is put into dehydrated alcohol and carried out ultrasonic cleaning, carry out ball milling in the ball mill of packing into then and mix, mix back gained slurry and dry again; Three, the mixture after will drying places sintering oven, in sintering atmosphere is vacuum or inert atmosphere, is warmed up to 1750～1850 ℃ with the speed of 10～30 ℃/min, insulation 30～90min, be cooled to room temperature and take out, promptly get Zirconia toughened boride ultra-temperature ceramic-based composite material; Contain yttrium oxide 2mol%～3mol% in the used yttrium oxide PSZ of step 1; The used boride powder of step 1 is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
Embodiment five: present embodiment and embodiment four be not both that the particle diameter of boride powder is 0.5～10 μ m in the step 1, the particle diameter of silicon-carbide particle is 0.5～2.0 μ m, and yttrium oxide PSZ particle grain size is 0.5～2.0 μ m.Other step and parameter are identical with embodiment four.
Embodiment six: the quality purity that is not both boride powder and silicon-carbide particle in the step 1 of present embodiment and embodiment four is all greater than 98%.Other step and parameter are identical with embodiment four.
Embodiment seven: the step 2 that is not both of present embodiment and embodiment four packs that to carry out that ball milling mixes in the ball mill be that to adopt diameter be wolfram varbide or the zirconium oxide balls of 5～10mm into, carries out planetary type ball-milling with the speed of 150～250r/min and mixes.Other step and parameter are identical with embodiment four.
Embodiment eight: the step 2 that is not both of present embodiment and embodiment four packs that to carry out that ball milling mixes in the ball mill be that to adopt diameter be wolfram varbide or the zirconium oxide balls of 6～8mm into, carries out planetary type ball-milling with the speed of 200r/min and mixes.Other step and parameter are identical with embodiment four.
Embodiment nine: present embodiment and embodiment four not to be both in the step 2 oven dry be on rotatory evaporator, with 50～80 ℃ conditions evaporation oven dry.Other step and parameter are identical with embodiment four.
Embodiment ten: present embodiment and embodiment four not to be both in the step 2 oven dry be on rotatory evaporator, with 60 ℃ conditions evaporation oven dry.Other step and parameter are identical with embodiment four.
Embodiment 11: not being both in the step 3 when sintering atmosphere is inert atmosphere of present embodiment and embodiment four, pressure is 10～50MPa.Other step and parameter are identical with embodiment four.
Embodiment 12: present embodiment and embodiment four be not both that inert atmosphere is argon gas or nitrogen in the step 3.Other step and parameter are identical with embodiment four.
Embodiment 13: present embodiment and embodiment four be not both that the speed with 15 ℃/min is warmed up to 1750 ℃ in the step 3, insulation 60min.Other step and parameter are identical with embodiment four.
Embodiment 14: the method that present embodiment prepares Zirconia toughened boride ultra-temperature ceramic-based composite material realizes according to the following steps: one, by total composite volume than 70% zirconium boride 99.5004323A8ure powder, 10% silicon-carbide particle and 20% yttrium oxide PSZ particle are mixed; Two, mixture is put into dehydrated alcohol and carried out ultrasonic cleaning, carry out ball milling in the ball mill of packing into then and mix, mix back gained slurry and dry again; Three, the mixture after will drying places sintering oven, in sintering atmosphere is that nitrogen, pressure are under the condition of 30MPa, is warmed up to 1850 ℃ with the speed of 15 ℃/min, insulation 60min, be cooled to room temperature and take out, promptly get Zirconia toughened boride ultra-temperature ceramic-based composite material; Contain yttrium oxide 2mol% in the used yttrium oxide PSZ of step 1.
In the present embodiment gained Zirconia toughened boride ultra-temperature ceramic-based composite material after tested, toughness value is 6.5MPam
1/2, bending strength is 998.3MPa.
Embodiment 15: the method that present embodiment prepares Zirconia toughened boride ultra-temperature ceramic-based composite material realizes according to the following steps: one, by total composite volume than 70% zirconium boride 99.5004323A8ure powder, 10% silicon-carbide particle and 20% yttrium oxide PSZ particle are mixed; Two, mixture is put into dehydrated alcohol and carried out ultrasonic cleaning, carry out ball milling in the ball mill of packing into then and mix, mix back gained slurry and dry again; Three, the mixture after will drying places sintering oven, in sintering atmosphere is that argon gas, pressure are under the condition of 30MPa, is warmed up to 1850 ℃ with the speed of 15 ℃/min, insulation 60min, be cooled to room temperature and take out, promptly get Zirconia toughened boride ultra-temperature ceramic-based composite material; Contain yttrium oxide 3mol% in the used yttrium oxide PSZ of step 1.
In the present embodiment gained Zirconia toughened boride ultra-temperature ceramic-based composite material after tested, toughness value is 6.8MPam
1/2, bending strength is 856.7MPa.
Claims (10)
1. Zirconia toughened boride ultra-temperature ceramic-based composite material, it is characterized in that Zirconia toughened boride ultra-temperature ceramic-based composite material by volume per-cent make by 70%～80% boride powder, 0～10% silicon-carbide particle and 10%～30% yttrium oxide PSZ particle; Wherein contain yttrium oxide 2mol%～3mol% in the yttrium oxide PSZ particle; Boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
2. Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 1, it is characterized in that Zirconia toughened boride ultra-temperature ceramic-based composite material by volume per-cent make by 70% boride powder, 10% silicon-carbide particle and 20% yttrium oxide PSZ particle.
3. the method for preparing the described Zirconia toughened boride ultra-temperature ceramic-based composite material of claim 1 is characterized in that this method realizes according to the following steps: one, by total composite volume than 70%～80% boride powder, 0～10% silicon-carbide particle and 10%～30% yttrium oxide PSZ particle are mixed; Two, mixture is put into dehydrated alcohol and carried out ultrasonic cleaning, carry out ball milling in the ball mill of packing into then and mix, mix back gained slurry and dry again; Three, the mixture after will drying places sintering oven, in sintering atmosphere is vacuum or inert atmosphere, is warmed up to 1750～1850 ℃ with the speed of 10～30 ℃/min, insulation 30～90min, be cooled to room temperature and take out, promptly get Zirconia toughened boride ultra-temperature ceramic-based composite material; Contain yttrium oxide 2mol%～3mol% in the used yttrium oxide PSZ of step 1; The used boride powder of step 1 is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
4. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3, the particle diameter that it is characterized in that boride powder in the step 1 is 0.5～10 μ m, the particle diameter of silicon-carbide particle is 0.5～2.0 μ m, and yttrium oxide PSZ particle grain size is 0.5～2.0 μ m.
5. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3, the quality purity that it is characterized in that boride powder and silicon-carbide particle in the step 1 is all greater than 98%.
6. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3, it is characterized in that step 2 packing into, to carry out that ball milling mixes in the ball mill be that to adopt diameter be wolfram varbide or the zirconium oxide balls of 5～10mm, carries out planetary type ball-milling with the speed of 150～250r/min and mix.
7. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3 is characterized in that oven dry is on rotatory evaporator in the step 2, with 50～80 ℃ condition evaporation oven dry.
8. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3 is characterized in that in the step 3 that when sintering atmosphere was inert atmosphere, pressure was 10～50MPa.
9. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3 is characterized in that inert atmosphere is argon gas or nitrogen in the step 3.
10. the method for preparing Zirconia toughened boride ultra-temperature ceramic-based composite material according to claim 3 is characterized in that the speed with 15 ℃/min is warmed up to 1750 ℃ in the step 3, insulation 60min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060554A (en) * | 2010-11-30 | 2011-05-18 | 哈尔滨工业大学 | High-strength high-toughness zirconium diboride-silicon carbide-zirconia ceramic-based composite material and preparation method thereof |
| CN102161588A (en) * | 2011-01-04 | 2011-08-24 | 武汉理工大学 | Preparation method of ZrB2/SiC/Zr-Al-C ceramic |
| CN102173813A (en) * | 2011-02-23 | 2011-09-07 | 哈尔滨工业大学 | Preparation method of complex phase ceramic material containing zirconium boride |
| CN103922398A (en) * | 2014-03-17 | 2014-07-16 | 山东理工大学 | Water quenching method for preparing flaky nanometer zirconia |
| CN108358646A (en) * | 2018-05-23 | 2018-08-03 | 广东工业大学 | A kind of boronation zirconia-based ceramic and preparation method thereof |
| CN117209287A (en) * | 2023-09-15 | 2023-12-12 | 佛山市陶莹新型材料有限公司 | High-toughness ceramic material and preparation method thereof |
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2008
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060554A (en) * | 2010-11-30 | 2011-05-18 | 哈尔滨工业大学 | High-strength high-toughness zirconium diboride-silicon carbide-zirconia ceramic-based composite material and preparation method thereof |
| CN102161588A (en) * | 2011-01-04 | 2011-08-24 | 武汉理工大学 | Preparation method of ZrB2/SiC/Zr-Al-C ceramic |
| CN102173813A (en) * | 2011-02-23 | 2011-09-07 | 哈尔滨工业大学 | Preparation method of complex phase ceramic material containing zirconium boride |
| CN103922398A (en) * | 2014-03-17 | 2014-07-16 | 山东理工大学 | Water quenching method for preparing flaky nanometer zirconia |
| CN103922398B (en) * | 2014-03-17 | 2017-06-30 | 山东理工大学 | The preparation method of water quenching synthesizing flaky nano zirconia |
| CN108358646A (en) * | 2018-05-23 | 2018-08-03 | 广东工业大学 | A kind of boronation zirconia-based ceramic and preparation method thereof |
| CN108358646B (en) * | 2018-05-23 | 2021-09-03 | 广东工业大学 | Zirconium boride-based ceramic and preparation method thereof |
| CN117209287A (en) * | 2023-09-15 | 2023-12-12 | 佛山市陶莹新型材料有限公司 | High-toughness ceramic material and preparation method thereof |
| CN117209287B (en) * | 2023-09-15 | 2024-04-09 | 佛山市陶莹新型材料有限公司 | High-toughness ceramic material and preparation method thereof |
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