CN101417880A - Low temperature sintered boride base ceramic materials and preparation method thereof - Google Patents
Low temperature sintered boride base ceramic materials and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low temperature sintering boride-based ceramic material and a preparation method thereof. The invention solves the problem of over high sintering temperature and pressure and low sintered density of the boride-based ceramic material in the prior art. The boride-based ceramic material is prepared by boride powders, carborundum powders and additives which are the mixture powders of alumina and yttria. The method is as follows: first, the boride powders, the carborundum powders and additives are mixed; second, the mixture is put in absolute ethyl alcohol for ultrasonic cleaning and dispersion, ball mill mixing and drying; and third, the mixture is cooled after hot-press sintering. The prepared low-temperature boride-based ceramic material after sintering at the condition of 1800 DEG C to 1850 DEG C and 30 Mpa are uniform and compact in structure, small in grain size and strong in mechanical property simultaneously, the relative density is above 96 percent and the intensity and toughness are respectively reach 786MPa and 7.12 MPam<1/2>. The method is simple and practical in technology, low in cost and easy for popularization.
Description
Technical field
The present invention relates to a kind of boride base ceramic materials and preparation method thereof.
Background technology
Borides mainly comprises zirconium boride 99.5004323A8ure (ZrB
2) and hafnium boride (HfB
2).This class material not only has characteristics such as high-melting-point, high rigidity, have simultaneously good conduction, heat conduction, neutron controllability and with the characteristics such as unreactiveness of molten metal, not only obtained using widely, also be expected to become one of candidate material of various key positions such as course of new aircraft of future generation, numbers of hot-side engine or parts simultaneously in electrode materials, casting high temperature material, high-temperature structural material field.Borides and structure thereof performance characterization and the anti-oxidant ablation behavioral study under extreme environments such as high temperature, high overload is that this material is used impassable gordian technique.And design, the preparation of carrying out material are the starting point and the emphasis of work, only have under preparation technology's prerequisite of good organization, structure and performance in acquisition, could guarantee that boride material applies in the actual environment safely and efficiently, also provide possibility simultaneously for it is extensive use of.
As far back as the late 1960s and the beginning of the seventies, U.S. Air Force associating Manlabs company has just carried out the correlative study of diboride.They utilize zone refining technology (Floating zone refining) and high pressure hot pressing and sintering technique (High-pressure hot pressing) to prepare monocrystalline and polycrystalline material respectively.Subsequently, because the needs of aerospace applications, the scientific worker has also carried out sintering, preparation and the performance study of borides in succession both at home and abroad.At present, both at home and abroad the emphasis of research and focus are that tiny silicon-carbide particle, whisker or wafer is incorporated into mutually as second and emerges a kind of ceramic matric composite in the boride.
Boride is a hexagonal system C32 type metalloid structural compounds, and interatomic bond is stronger covalent bonds, and this strong bond has determined high-melting-point, high rigidity and the chemical stability of boride material, also makes simultaneously the extremely difficult sintering of this stupalith.A certain amount of oxide compound of collection is all covered (as boron oxide B in the boride powder surface of selling on the market at present in addition
2O
3, zirconium white ZrO
2, hafnia HfO
2Deng), the existence of these oxide compounds has reduced boride volume diffusion and crystal boundary rate of diffusion, thereby has further reduced the sinterability energy of material.
For overcoming above-mentioned defective, traditional way is to carry out sintering to prepare boride and matrix material thereof under high temperature, high pressure, and wherein more than 2000 ℃, sintering pressure is greater than 100MPa mostly for sintering temperature.High like this temperature and pressure has proposed higher requirement to agglomerating plant, and simultaneously long-time use also can reduce the work-ing life of equipment, improves the production cost of material, is unfavorable for industrialization promotion.Because the too high meeting of sintering temperature causes the inner crystal grain of stupalith to be grown up unusually, cause internal stress and tiny crack, thereby have a strong impact on the mechanical property of material in addition.Therefore, too high sintering temperature or pressure have limited the development and the utilization of borides to a certain extent, prepare dense structure under lower temperature conditions, well behaved boride base ceramic materials is the target that vast researcher is seek assiduously always.
At present, at ZrB
2-SiC and HfB
2In-SiC the material system, people select for use metal sintering auxiliary agent such as Fe, Ni, Cu etc. successfully to prepare the higher ceramic matric composite of relative density at a lower temperature by liquid-phase sintering process.But the adding of metal sintering auxiliary agent has been introduced the soft phase of low temperature to the crystal boundary of material place, thereby this soft phase at high temperature is easy to the softening high-temperature behavior that has sharply reduced material, and this to material in the use under the hot conditions is and disadvantageous.In addition, on this basis, Italy and American Studies person adopt AlN, Si
3N
4Reduce the sintering temperature of borides etc. the ceramic mould sintering aid, attempt under low temperature, to prepare composite ceramic material.Though the adding of these stupaliths has reduced the sintering temperature of boride base ceramic materials to a certain extent, because these sintering aid fusing points are higher, the sintering temperature of boride base ceramic materials still remains on more than 1870 ℃.
Summary of the invention
The objective of the invention is provides a kind of low temperature sintered boride base ceramic materials and preparation method thereof in order to solve boride base ceramic materials sintering temperature and hypertonia in the prior art, problem that sintered density is low.
Low temperature sintering boride base ceramic materials of the present invention by volume per-cent is made by 60%～94% boride powder, 5%～30% silicon carbide powder and 1%～10% additive, wherein additive is aluminum oxide and yttrium oxide mixed powder, and the mol ratio of alumina powder and yttrium oxide powder is 5:3.
Described boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder.Described silicon carbide powder is silicon carbide whisker, silicon-carbide particle or silicon carbide whisker plate.
The preparation method of low temperature sintering boride base ceramic materials of the present invention is realized by following step: one, by volume per-cent mixes 60%～94% boride powder, 5%～30% silicon carbide powder and 1%～10% additive, wherein additive is aluminum oxide and yttrium oxide mixed powder, and the mol ratio of alumina powder and yttrium oxide powder is 5:3; Two, the mixed powder of step 1 is put into dehydrated alcohol and carry out ultrasonic cleaning and dispersion, ball milling mixes 5～10h then, again oven dry; Three, will place sintering oven through the mixture that step 2 is handled, at 1800～1850 ℃, hot pressing pressure is under 30MPa, vacuum or the inert gas atmosphere, insulation 30～60min takes out after cooling to room temperature then with the furnace, promptly obtains the boride-based ceramics based composites.
Boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder in the step 1; Silicon carbide powder is silicon carbide whisker, silicon-carbide particle or silicon carbide whisker plate.Rare gas element is an argon gas in the step 3.
The present invention is the direct aluminum oxide (Al that particle is tiny
2O
3) and yttrium oxide (Y
2O
3) powder directly mixes with boride matrix powder and SiC powder with certain proportion, and with the once sintered moulding of hot pressed sintering mode.In the sintering process, Al
2O
3And Y
2O
3Well reaction and one-tenth are given birth to yttrium aluminum garnet (YAG).On the one hand, YAG provides liquid phase, has increased the sintering motivating force of boride base ceramic materials; The more important thing is the adding of YAG, can effectively consume the inertia oxide film on boride surface, eliminated the lattice oxygen defective, improved the intergranular transmission and diffusion of material, thereby better reduced the sintering temperature of boride base ceramic materials.Homogeneous microstructure, the densification of the present invention's low temperature sintered boride base ceramic materials that sintering obtains under 1800～1850 ℃, 30MPa, and grain fineness number is tiny, the while good mechanical performance, relative density is more than 96%, flexural strength and fracture toughness property are respectively up to 786MPa and 7.12MPam
1/2The features simple and practical process of the inventive method, with low cost, be easy to promote.
Embodiment
Embodiment one: present embodiment low temperature sintering boride base ceramic materials by volume per-cent is made by 60%～94% boride powder, 5%～30% silicon carbide powder and 1%～10% additive, wherein additive is aluminum oxide and yttrium oxide mixed powder, and the mol ratio of alumina powder and yttrium oxide powder is 5:3.
The boride base ceramic materials density of present embodiment is good, and relative density is more than 96%, and flexural strength is up to 786MPa, and fracture toughness property is up to 7.12MPam
1/2
Embodiment two: what present embodiment and embodiment one were different is: low temperature sintered boride base ceramic materials by volume per-cent is made by 68%～87% boride powder, 10%～25% silicon carbide powder and 3%～7% additive.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: low temperature sintered boride base ceramic materials by volume per-cent is made by 75% boride powder, 20% silicon carbide powder and 5% additive.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is: the particle diameter of boride powder is 2～10 μ m.Other is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is: the particle diameter of boride powder is 4～8 μ m.Other is identical with embodiment one.
Embodiment seven: what present embodiment and embodiment one were different is: the particle diameter of boride powder is 6 μ m.Other is identical with embodiment one.
Embodiment nine: what present embodiment and embodiment one were different is: silicon carbide powder is silicon carbide whisker, silicon-carbide particle or silicon carbide whisker plate.Other is identical with embodiment one.
Embodiment ten: what present embodiment and embodiment nine were different is: other is identical with embodiment nine for particle diameter 0.5～5 μ m of silicon-carbide particle.
Embodiment 11: what present embodiment and embodiment nine were different is: other is identical with embodiment nine for particle diameter 1～4 μ m of silicon-carbide particle.
Embodiment 12: what present embodiment and embodiment nine were different is: other is identical with embodiment nine for the particle diameter 2 μ m of silicon-carbide particle.
Embodiment 13: what present embodiment and embodiment nine were different is: the diameter of silicon carbide whisker is that 0.8～1.5 μ m, length are 5～100 μ m.Other is identical with embodiment nine.
Embodiment 14: what present embodiment and embodiment nine were different is: the diameter of silicon carbide whisker is that 1 μ m, length are 50 μ m.Other is identical with embodiment nine.
Embodiment 15: what present embodiment and embodiment nine were different is: the length of silicon carbide whisker plate is that 1～10 μ m, width are that 0.5～2 μ m, thickness are 0.1～1 μ m.Other is identical with embodiment nine.
Embodiment 16: what present embodiment and embodiment nine were different is: the length of silicon carbide whisker plate is that 2～8 μ m, width are that 1～1.5 μ m, thickness are 0.2～0.8 μ m.Other is identical with embodiment nine.
Embodiment 17: what present embodiment and embodiment nine were different is: the length of silicon carbide whisker plate is that 5 μ m, width are that 1.2 μ m, thickness are 0.5 μ m.Other is identical with embodiment nine.
Embodiment 18: what present embodiment and embodiment one were different is: the particle diameter of alumina powder is 0.5～2 μ m.Other is identical with embodiment one.
Embodiment 19: what present embodiment and embodiment one were different is: the particle diameter of alumina powder is 0.8～1.5 μ m.Other is identical with embodiment one.
Embodiment 20: what present embodiment and embodiment one were different is: the particle diameter of alumina powder is 1.0 μ m.Other is identical with embodiment one.
Embodiment 21: what present embodiment and embodiment one were different is: the particle diameter of yttrium oxide powder is 0.5～2 μ m.Other is identical with embodiment one.
Embodiment 22: what present embodiment and embodiment one were different is: the particle diameter of yttrium oxide powder is 0.8～1.5 μ m.Other is identical with embodiment one.
Embodiment 23: what present embodiment and embodiment one were different is: the particle diameter of yttrium oxide powder is 1.0 μ m.Other is identical with embodiment one.
Embodiment 24: the preparation method of present embodiment low temperature sintered boride base ceramic materials is realized by following step: one, by volume per-cent mixes 60%～94% boride powder, 5%～30% silicon carbide powder and 1%～10% additive, wherein additive is aluminum oxide and yttrium oxide mixed powder, and the mol ratio of alumina powder and yttrium oxide powder is 5:3; Two, the mixed powder of step 1 is put into dehydrated alcohol and carry out ultrasonic cleaning and dispersion, ball milling mixes 5～10h then, again oven dry; Three, will place sintering oven through the mixture that step 2 is handled, at 1800～1850 ℃, hot pressing pressure is under 30MPa, vacuum or the inert gas atmosphere, hot pressed sintering 30～60min takes out after cooling to room temperature then with the furnace, promptly obtains the low temperature sintered boride base ceramic matric composite.
The low temperature sintered boride base ceramic materials density of present embodiment is good, and relative density is more than 96%, and the flexural strength of material is up to 786MPa, and fracture toughness property is up to 7.12MPam
1/2
Embodiment 25: what present embodiment and embodiment 24 were different is: in the step 1 by volume per-cent 68%～87% boride powder, 10%～25% silicon carbide powder and 3%～7% additive are mixed.Other is identical with embodiment 24.
Embodiment 26: what present embodiment and embodiment 24 were different is: in the step 1 by volume per-cent 75% boride powder, 20% silicon carbide powder and 5% additive are mixed.Other is identical with embodiment 24.
Embodiment 27: what present embodiment and embodiment 24 were different is: boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder in the step 1.Other is identical with embodiment 24.
Embodiment 28: what present embodiment and embodiment 24 were different is: the particle diameter of boride powder is 2～10 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 29: what present embodiment and embodiment 24 were different is: the particle diameter of boride powder is 4～8 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 30: what present embodiment and embodiment 24 were different is: the particle diameter of boride powder is 6 μ m in the step 1.Other is identical with embodiment 24.
The embodiment hentriaconta-: what present embodiment and embodiment 24 were different is: silicon carbide powder is silicon carbide whisker, silicon-carbide particle or silicon carbide whisker plate in the step 1.Other is identical with embodiment 24.
Embodiment 32: what present embodiment was different with the embodiment hentriaconta-is: particle diameter 0.5～5 μ m of silicon-carbide particle.Other is identical with the embodiment hentriaconta-.
Embodiment 33: what present embodiment was different with the embodiment hentriaconta-is: other is identical with the embodiment hentriaconta-for particle diameter 1～4 μ m of silicon-carbide particle.
Embodiment 34: what present embodiment was different with the embodiment hentriaconta-is: other is identical with the embodiment hentriaconta-for the particle diameter 2 μ m of silicon-carbide particle.
Embodiment 35: what present embodiment was different with the embodiment hentriaconta-is: the diameter of silicon carbide whisker is that 0.8～1.5 μ m, length are 5～100 μ m.Other is identical with embodiment nine.
Embodiment 36: what present embodiment was different with the embodiment hentriaconta-is: the diameter of silicon carbide whisker is that 1 μ m, length are 50 μ m.Other is identical with the embodiment hentriaconta-.
Embodiment 37: what present embodiment was different with the embodiment hentriaconta-is: the length of silicon carbide whisker plate is that 1～10 μ m, width are that 0.5～2 μ m, thickness are 0.1～1 μ m.Other is identical with the embodiment hentriaconta-.
Embodiment 38: what present embodiment was different with the embodiment hentriaconta-is: the length of silicon carbide whisker plate is that 2～8 μ m, width are that 1～1.5 μ m, thickness are 0.2～0.8 μ m.Other is identical with the embodiment hentriaconta-.
Embodiment 39: what present embodiment was different with the embodiment hentriaconta-is: the length of silicon carbide whisker plate is that 5 μ m, width are that 1.2 μ m, thickness are 0.5 μ m.Other is identical with the embodiment hentriaconta-.
Embodiment 40: what present embodiment and embodiment 24 were different is: the particle diameter of alumina powder is 0.5～2 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 41: what present embodiment and embodiment 24 were different is: the particle diameter of alumina powder is 0.8～1.5 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 42: what present embodiment and embodiment 24 were different is: the particle diameter of alumina powder is 1.0 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 43: what present embodiment and embodiment 24 were different is: the particle diameter of yttrium oxide powder is 0.5～2 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 44: what present embodiment and embodiment 24 were different is: the particle diameter of yttrium oxide powder is 0.8～1.5 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 45: what present embodiment and embodiment 24 were different is: the particle diameter of yttrium oxide powder is 1.0 μ m in the step 1.Other is identical with embodiment 24.
Embodiment 46: present embodiment and embodiment 24 are different: to mix be to carry out in planetary ball mill to ball milling in the step 2, and wherein ball-milling medium is that diameter is 2～10mm zirconium white or tungsten-carbide ball.Other is identical with embodiment 24.
When silicon carbide was silicon-carbide particle or silicon carbide whisker plate in the present embodiment, ball milling speed was 160～250r/min; When silicon carbide was silicon carbide whisker, ball milling speed was 160～200r/min.
Embodiment 47: present embodiment and embodiment 24 are different: oven dry is to carry out at rotatory evaporator in the step 2, and wherein the rotary evaporation actuator temperature is controlled at 50～70 ℃, rotating speed at 40～100r/min.Other is identical with embodiment 24.
Embodiment 48: what present embodiment and embodiment 24 were different is: rare gas element is an argon gas in the step 3.Other is identical with embodiment 24.
Embodiment 49: what present embodiment and embodiment 24 were different is: the speed with 10～30 ℃/min in the step 3 is warmed up to 1800～1850 ℃.
Embodiment 50: what present embodiment and embodiment 24 were different is: hot pressing temperature is 1810～1840 ℃ in the step 3.
Embodiment 51: what present embodiment and embodiment 24 were different is: hot pressing temperature is 1820 ℃ in the step 3.
Embodiment 52: what present embodiment and embodiment 24 were different is: hot pressing temperature is 1840 ℃ in the step 3.
Embodiment 53: the preparation method of present embodiment low temperature sintered boride base ceramic materials is realized by following step: one, by volume per-cent is that 2 μ m zirconium boride 99.5004323A8ure powder, 10% diameter are that 0.5～2 μ m, length are that the additive of 5～100 μ m silicon carbide whiskers and 3% mixes with 87% particle diameter, wherein additive is aluminum oxide and the yttrium oxide mixed powder that particle diameter is 1 μ m, and the mol ratio of alumina powder and yttrium oxide powder is 5:3; Two, the mixed powder of step 1 is put into dehydrated alcohol and carry out ultrasonic cleaning and dispersion, mix 5～10h with 180r/min rotating speed ball milling then, again oven dry; Three, will place sintering oven through the mixture that step 2 is handled, be under 30MPa, vacuum or the inert gas atmosphere at 1800 ℃, hot pressing pressure, and hot pressed sintering 60min takes out after cooling to room temperature then with the furnace, promptly obtains the boride-based ceramics based composites.
The boride-based ceramics based composites density of present embodiment preparation is good, and relative density is 98.8%, and bending strength is 786MPa, fracture toughness property 6.48MPam
1/2
Embodiment 54: what present embodiment and embodiment 53 were different is: in the step 1 by volume per-cent be that 2 μ m zirconium boride 99.5004323A8ure powder, 20% diameter are that 0.5～2 μ m, length are that the additive of 5～100 μ m silicon carbide whiskers and 3% mixes with 77% particle diameter.Other is identical with embodiment 53.
The boride-based ceramics based composites density of present embodiment preparation is good, and relative density is 98.7%, and three-point bending strength is 783MPa, and fracture toughness property is 6.65MPam
1/2
Embodiment 55: what present embodiment and embodiment 54 were different is: in the step 1 by volume per-cent be that 2 μ m zirconium boride 99.5004323A8ure powder, 20% diameter are that 0.5～2 μ m, length are that the additive of 5～100 μ m silicon carbide whiskers and 6% mixes with 74% particle diameter.
The boride-based ceramics matrix material density of present embodiment preparation is good, and relative density is 97.8%, and three-point bending strength is 730MPa, and fracture toughness property is 6.14MPam
1/2
Embodiment 56: what present embodiment and embodiment 54 were different is: in the step 1 by volume per-cent be that 2 μ m zirconium boride 99.5004323A8ure powder, 20% diameter are that 0.5～2 μ m, length are that the additive of 5～100 μ m silicon carbide whiskers and 10% mixes with 70% particle diameter.
The boride-based ceramics matrix material density of present embodiment preparation is good, and relative density is 97.5%, and three-point bending strength is 727MPa, and fracture toughness property is 6.23MPam
1/2
Embodiment 56: what present embodiment and embodiment 54 were different is: in the step 1 by volume per-cent be that 2 μ m zirconium boride 99.5004323A8ure powder, 30% diameter are that 0.5～2 μ m, length are that the additive of 5～100 μ m silicon carbide whiskers and 3% mixes with 67% particle diameter.
The matrix material relative density of present embodiment preparation is 96%, and bending strength is 767MPa, and fracture toughness property is 7.12MPam
1/2
Claims (10)
1, low temperature sintered boride base ceramic materials, it is characterized in that boride base ceramic materials by volume per-cent make by 60%～94% boride powder, 5%～30% silicon carbide powder and 1%～10% additive, wherein additive is aluminum oxide and yttrium oxide mixed powder, and the mol ratio of alumina powder and yttrium oxide powder is 5:3.
2, low temperature sintered boride base ceramic materials according to claim 1 is characterized in that boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder.
3, low temperature sintered boride base ceramic materials according to claim 1, the particle diameter that it is characterized in that boride powder are 2～10 μ m.
4, low temperature sintered boride base ceramic materials according to claim 1 is characterized in that silicon carbide powder is silicon carbide whisker, silicon-carbide particle or silicon carbide whisker plate.
5, low temperature sintered boride base ceramic materials according to claim 1 is characterized in that the alumina powder particle diameter is 0.5～2 μ m, and the yttrium oxide powder particle diameter is 0.5～2 μ m.
6, the preparation method of low temperature sintered boride base ceramic materials, the preparation method who it is characterized in that low temperature sintered boride base ceramic materials is realized by following step: one, by volume per-cent mixes 60%～94% boride powder, 5%～30% silicon carbide powder and 1%～10% additive, wherein additive is aluminum oxide and yttrium oxide mixed powder, and the mol ratio of alumina powder and yttrium oxide powder is 5:3; Two, the mixed powder of step 1 is put into dehydrated alcohol and carry out ultrasonic cleaning and dispersion, ball milling mixes 5～10h then, again oven dry; Three, will place sintering oven through the mixture that step 2 is handled, at 1800～1850 ℃, hot pressing pressure is under 30MPa, vacuum or the inert gas atmosphere, insulation 30～60min takes out after cooling to room temperature then with the furnace, promptly obtains the boride-based ceramics based composites.
7, the preparation method of low temperature sintered boride base ceramic materials according to claim 6 is characterized in that boride powder is zirconium boride 99.5004323A8ure powder or hafnium boride powder in the step 1.
8, the preparation method of low temperature sintered boride base ceramic materials according to claim 6, the particle diameter that it is characterized in that boride powder in the step 1 is 2～10 μ m.
9, the preparation method of low temperature sintered boride base ceramic materials according to claim 6 is characterized in that silicon carbide powder is silicon carbide whisker, silicon-carbide particle or silicon carbide whisker plate in the step 1.
10, the preparation method of low temperature sintered boride base ceramic materials according to claim 6 is characterized in that rare gas element is an argon gas in the step 3.
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