CN1238304C - Method for preparing Al4SiC4 ceramics - Google Patents
Method for preparing Al4SiC4 ceramics Download PDFInfo
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- CN1238304C CN1238304C CN 200410013683 CN200410013683A CN1238304C CN 1238304 C CN1238304 C CN 1238304C CN 200410013683 CN200410013683 CN 200410013683 CN 200410013683 A CN200410013683 A CN 200410013683A CN 1238304 C CN1238304 C CN 1238304C
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Abstract
The present invention discloses a method for preparing Al4SiC4 ceramics. The proportion by weight of the components of aluminium powder to graphite powder to polycarbonsilane is (2 to 4): (0.2 to 3.8): (1 to 5). The present invention comprises the steps: (a) the aluminium powder and the graphite powder are thoroughly mixed first, and meanwhile, the polycarbonsilane is dissolved in an organic solvent, then the mixed powder of the aluminium powder and the graphite powder is put into the organic solution of the polycarbonsilane, and the organic solvent is heated up until the complete volatilization of the organic solvent; (b) the dried powder is taken out for cracking under the shield of argon at the temperature of 800 DEG C to 1400 DEG C; (c) the cracked materials are thoroughly pulverized and mixed; (d) the mixed material is put an in graphite mould, the graphite mould is sintered in a hot-pressing sintering furnace at the temperature of 1600 DEG C to 2200 DEG C under the pressure of 10 to 40MPa and under the shield of argon, and then, thermal insulation is carried out for 1 to 5 hours. The present invention uses the organic matter pre-cracking synthesizing method; therefore, the sintering activity among sintered bodies is enhanced, the high-temperature sintering time is shortened, and the density of a sintered sample is from 88% to 99%.
Description
Technical field:
The present invention relates to a kind of Al
4SiC
4The preparation method of pottery.
Background technology:
Al
4SiC
4The ternary block pottery has high-melting-point, low density, good normal temperature and mechanical behavior under high temperature, excellent oxidation-resistance and erosion resistance, and has the favorable conductive thermal conductivity, and therefore lower thermal expansivity etc. have very application prospects.The Japanese is with Al
4SiC
4Powder joins and strengthens its antioxidant property in the fire-resistant carbon brick of oxide compound.When its weight percent only is 5%, and do not add Al
4SiC
4The fire-resistant carbon brick of the oxide compound of powder is compared its antioxidant property and is obviously improved.The people is also arranged at present to Al
4SiC
4Ternary block pottery synthetic carried out some researchs.People such as Koji Inoue adopt two kinds of approach to prepare Al
4SiC
4Pottery.A kind of is the Al that obtains pure phase by aluminium, powdered carbon and silica flour in insulation under 1700 ℃ of argon shield atmosphere after 4 hours
4SiC
4Powder; Second kind of approach is to cold pressing under 80MPa earlier by aluminium, powdered carbon and kaolin, uses the pressure cold isostatic compaction of 100MPa again, insulation pre-treatment in 1 hour under 700 ℃ of argon shield atmosphere then, and grind into powder was 1700 ℃ of vacuum-treat 4 hours then.Above-mentioned two kinds of Al that method makes
4SiC
4Powder is used pulse electrifying sintering process (Pulse ElectronicCurrent Sintering again after pulverizing; PECS) under vacuum condition, 1700 or 1800 ℃ of sintering 30 minutes, pressure is 20～80MPa.The sintered compact density increases with pressure, and its value is 80～97%.These two kinds of methods all must earlier synthetic Al
4SiC
4Powder carries out sintering again, and it is loaded down with trivial details to exist preparation technology, the shortcoming that production cost is higher.In addition if seek out the preparation technology that the sintered compact of high-compactness must adopt High Temperature High Pressure.
Summary of the invention:
Purpose of the present invention just provides that a kind of technology is simple, cost is lower and Al
4SiC
4The ceramic dense degree can reach 88～99% Al
4SiC
4The preparation method of pottery.Realize that technical scheme of the present invention is as follows: a kind of Al
4SiC
4The preparation method of pottery, its each components by weight is an aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 1～5, preparation process is: (one) is at first with aluminium powder and Graphite Powder 99 thorough mixing; Simultaneously Polycarbosilane is dissolved in and forms clear solution in the organic solvent, then mixed aluminium and graphite powder mix are placed the organic solution of Polycarbosilane, stir after at least 10 minutes, with solution heating and continue to stir and organic solvent is evaporated into stop when solution becomes the thickness thickener stirring, organic solvent is volatilized fully but still continue heating.(2) in 800～1400 ℃ of cracking, the cracked purpose is to make inorganicization of organism Polycarbosilane to the powder of taking-up oven dry, is transformed into the SiC particle of amorphous or crystallite under argon shield.(3) fully to pulverize and be mixed to granularity be 2～50 μ m to the powder after the cracking.(4) material that mixes is placed the mould of graphite material, in hot-pressed sintering furnace in 1～5 hour sintering of 1600～2200 ℃ of constant temperature.Sintering process is vacuum or argon shield, and sintering pressure is 10～40MPa.To the Al that makes according to aforesaid method
4SiC
4Carry out sample detection, its performance is as follows: the density of a, sintered sample is 88～99%; The normal temperature and the mechanical behavior under high temperature of b, sintered sample see Table 1; C, reach 10～50 hours, oxidizing temperature in the anti-oxidant test of 1700 ℃ constant temperature, sintered sample shows excellent high-temperature oxidation resistance.The rate of body weight gain of sample unit surface square is 0.01～10%, and sample size does not have considerable change, and oxide skin does not have obscission.
The normal temperature of table 1 sintered sample and mechanical behavior under high temperature
| Performance | Detected value | |
| Flexural strength (MPa) | Room temperature | 200～350 |
| High temperature (1000～1300) | 200～500 | |
| Fracture toughness property (MPa.m 1/2) | 2～6 | |
| Vickers' hardness (Gpa) | 3～25 | |
Technique effect of the present invention is: 1, Polycarbosilane is dissolved in the organic solution, and dissolving is fast, and the organic solvent boiling point is low, just can full scale clearance go out before pre-cracking, avoids bringing impurity into by organic solvent; 2, solvent can be realized original powder full and uniform dispersion with mixing of powder, 3, saved Al
4SiC
4The high temperature building-up process of powder is with Al
4SiC
4Synthetic unite two into one with sintering, at Al
4SiC
4Building-up process in finish the sintering of ceramic of compact simultaneously; 4, use the pre-cracked synthesis mode of organism, strengthened the sintering activity between the powder, help ceramic post sintering; 4, can be in short sintering time, lower sintering pressure obtains the sintered compact of higher densification down; 5, the sample that goes out of sintering has 88～99% density, normal temperature and mechanical behavior under high temperature preferably, excellent antioxidant property, excellent high-temperature stability etc.
Embodiment:
Embodiment one: a kind of Al
4SiC
4The preparation method of pottery, its each components by weight is an aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 1～5, preparation process is: (one) is at first with aluminium powder and Graphite Powder 99 thorough mixing; Simultaneously Polycarbosilane is dissolved in and forms clear solution in the organic solvent, then mixed aluminium and graphite powder mix are placed the organic solution of Polycarbosilane, stir after at least 10 minutes, with solution heating and continue to stir and organic solvent is evaporated into stop when solution becomes the thickness thickener stirring, but still continue heating, oven dry is volatilized organic solvent fully.(2) in 800～1400 ℃ of cracking, the cracked purpose is to make complete inorganicization of organism Polycarbosilane to the powder of taking-up oven dry, is transformed into the SiC particle of amorphous or crystallite under argon shield.(3) fully to pulverize and be mixed to granularity be 2～50 μ m to the powder after the cracking.(4) material that mixes is placed the mould of graphite material, in hot-pressed sintering furnace in 1～5 hour sintering of 1600～2200 ℃ of constant temperature.Sintering process is vacuum or argon shield, and sintering pressure is 10～40MPa.
Embodiment two: the difference of present embodiment and embodiment one is that its each components by weight is: aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 1～2.Preparation process is identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is that its each components by weight is: aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 2.1～5.Preparation process is identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is, in (two) step of preparation process: the cracked temperature is 800 ℃～1150 ℃.All the other each components are identical with embodiment one with preparation process.
Embodiment five: the difference of present embodiment and embodiment four is, in (two) step of preparation process: the cracked temperature is 1155 ℃～1400 ℃.All the other each components are identical with embodiment four with preparation process.
Embodiment six: the difference of present embodiment and embodiment one is that sintering temperature is 1600 ℃～1850 ℃ in (four) step of preparation process.Sintering time 2～5 hours.All the other each components are identical with embodiment one with preparation process.In this embodiment, sintering temperature is selected low, and sintering time is longer.
Embodiment seven: the difference of present embodiment and embodiment six is that sintering temperature is 1855 ℃～2200 ℃ in (four) step of preparation process.Sintering time 1 hour～2 hours 55 minutes.All the other each components are identical with embodiment six with preparation process.In this embodiment, sintering temperature is selected higher, and sintering time is shorter.
Embodiment eight: the difference of present embodiment and embodiment one is, in the step (four) of preparation process, sintering be divided into two the step carry out: at first sintering temperature is 1600 ℃～2100 ℃, sintering time 1 hour～2 hours 55 minutes, sintering pressure 10～25Mpa, furnace temperature is raise 50-100 ℃ then, be forced into 10～40MPa, be incubated 0.5～2 hour.
Embodiment nine: the difference of present embodiment and embodiment one is, in the step () of preparation process, aluminium powder and Graphite Powder 99 were mixed on planetary ball mill 5-24 hour, organic solvent is selected tetrahydrofuran (THF) for use, aluminium and graphite powder mix add in the tetrahydrofuran solution of Polycarbosilane, on magnetic stirring apparatus or mechanical stirrer, mix and stir, stir after 10-50 minute, mixing solutions is warming up to 80 ℃, continue to stir until the tetrahydrofuran solvent volatilization to the greatest extent, solution stops when becoming the thickness thickener stirring.
Claims (9)
1, a kind of Al
4SiC
4The preparation method of pottery is characterized in that its each components by weight is an aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 1～5, and preparation process is: (one) at first mixes aluminium powder with Graphite Powder 99; Simultaneously Polycarbosilane is dissolved in and forms clear solution in the organic solvent, then mixed aluminium and graphite powder mix are placed the organic solution of Polycarbosilane, stir after at least 10 minutes, with solution heating and continue to stir and organic solvent is evaporated into stop when solution becomes the thickness thickener stirring, but still continue heating, oven dry is volatilized organic solvent fully; (2) powder that takes out oven dry under argon shield in 800～1400 ℃ of cracking; (3) to pulverize and to be mixed to granularity be 2～50 μ m to the powder after the cracking; (4) material that mixes is placed the mould of graphite material, in 1600～2200 ℃ of constant temperature sintering 1～5 hour, sintering process was vacuum or argon shield in hot-pressed sintering furnace, and sintering pressure is 10～40MPa.
2, a kind of Al according to claim 1
4SiC
4The preparation method of pottery is characterized in that its each components by weight is: aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 1～2.
3, a kind of Al according to claim 1
4SiC
4The preparation method of pottery is characterized in that its each components by weight is: aluminium powder: Graphite Powder 99: Polycarbosilane=2～4: 0.2～3.8: 2.1～5.
4, a kind of Al according to claim 1
4SiC
4The preparation method of pottery, it is characterized in that in (two) step of preparation process: the cracked temperature is 800 ℃～1150 ℃.
5, a kind of Al according to claim 1
4SiC
4The preparation method of pottery, it is characterized in that in (two) step of preparation process: the cracked temperature is 1155 ℃～1400 ℃.
6, a kind of Al according to claim 1
4SiC
4The preparation method of pottery is characterized in that sintering temperature is 1600 ℃～1850 ℃ in (four) step of preparation process, sintering time 2～5 hours.
7, a kind of Al according to claim 1
4SiC
4The preparation method of pottery is characterized in that sintering temperature is 1855 ℃～2200 ℃ in (four) step of preparation process, sintering time 1 hour～2 hours 55 minutes.
8, a kind of Al according to claim 1
4SiC
4The preparation method of pottery, it is characterized in that in the step (four) in preparation process, sintering be divided into two the step carry out: at first sintering temperature is 1600 ℃～2100 ℃, sintering time 1 hour～2 hours 55 minutes, sintering pressure 10～25Mpa, furnace temperature is raise 50-100 ℃ then, be forced into 10～40MPa, be incubated 0.5～2 hour.
9, a kind of Al according to claim 1
4SiC
4The preparation method of pottery, it is characterized in that in the step () in preparation process, aluminium powder and Graphite Powder 99 were mixed on planetary ball mill 5-24 hour, organic solvent is selected tetrahydrofuran (THF) for use, and aluminium and graphite powder mix add in the tetrahydrofuran solution of Polycarbosilane, mixes on magnetic stirring apparatus or mechanical stirrer and stirs, stir after 10-50 minute, mixing solutions is warming up to 80 ℃, continues to stir until the tetrahydrofuran solvent volatilization to the greatest extent, solution stops when becoming the thickness thickener stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410013683 CN1238304C (en) | 2004-04-14 | 2004-04-14 | Method for preparing Al4SiC4 ceramics |
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|---|---|---|---|
| CN 200410013683 CN1238304C (en) | 2004-04-14 | 2004-04-14 | Method for preparing Al4SiC4 ceramics |
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| CN1562881A CN1562881A (en) | 2005-01-12 |
| CN1238304C true CN1238304C (en) | 2006-01-25 |
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|---|---|---|---|
| CN 200410013683 Expired - Fee Related CN1238304C (en) | 2004-04-14 | 2004-04-14 | Method for preparing Al4SiC4 ceramics |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423215B (en) * | 2008-11-27 | 2010-12-01 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing Al4SiC4 powder |
| CN102320848B (en) * | 2011-08-17 | 2013-04-24 | 武汉科技大学 | Al4SiC4-Al8SiC7 refractory material and preparation method thereof |
| CN109825903B (en) * | 2019-03-04 | 2021-08-06 | 中国科学院宁波材料技术与工程研究所 | Aluminum-containing silicon carbide fiber and preparation method thereof |
| CN114824990A (en) * | 2022-04-26 | 2022-07-29 | 安徽衡盛五金机电制品有限公司 | Rapid forming process method of wear-resistant carbon brush |
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