CN104030688A - Preparation method of low-temperature reactive sintered silicon carbide - Google Patents
Preparation method of low-temperature reactive sintered silicon carbide Download PDFInfo
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- CN104030688A CN104030688A CN201410276905.1A CN201410276905A CN104030688A CN 104030688 A CN104030688 A CN 104030688A CN 201410276905 A CN201410276905 A CN 201410276905A CN 104030688 A CN104030688 A CN 104030688A
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Abstract
The invention discloses a preparation method of low-temperature reactive sintered silicon carbide. The method is characterized by sequentially comprising the following steps: evenly mixing carbon powder, silicon carbide powder and a proper amount of molding agent so as to form mixed powder; molding the mixed powder in a die pressing manner so as to obtain a ceramic biscuit; respectively molding metallic aluminum and silicon-aluminum alloy powder in a die in a pressing manner so as to obtain a metallic aluminum compaction and a silicon-aluminum alloy compaction; sequentially stacking the metallic aluminum compaction, the ceramic biscuit and the silicon-aluminum alloy compaction and sintering in a vacuum furnace in a heat preservation manner so as to obtain the reactive sintered silicon carbide. Based on the improvement of special raw materials, a formula and a machining process, compared with the reactive sintered silicon carbide product produced by utilizing other process routes, the reactive sintered silicon carbide product disclosed by the invention contains a small amount of free silicon, and is high in density and fracture toughness and good in bullet resistance. The content of free silicon in the prepared reactive sintered silicon carbide product is decreased by 8-12%; the density of the prepared reactive sintered silicon carbide product is between 3.07g/cm<3> and 3.12g/cm<3>.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, relate to the preparation technology of matrix material, especially a kind of preparation method of low temperature reaction sintering silicon carbide ceramics.
Background technology
Silicon carbide (SiC) is a kind of important engineering ceramic material, its hardness high (its hardness is only second to a few materials such as diamond, cubic boron nitride and norbide), and stable chemical nature, has good wear and corrosion behavior.In addition, it has the advantages such as intensity is high, high temperature resistant, thermal conductivity is good, density is low, good thermal shock, is the ideal material of the furnace lining etc. of oil, metallurgy, chemical industry, machinery, Aeronautics and Astronautics aircraft field mechanical sealing member, high-load long lifetime kiln furnitures, heat exchanger tube, pyroceramic radiant burner, airspace engine combustion chamber, nuclear fuel cools stacks coating material and the high temperature gas cooled reactor under the extreme environmental conditions such as high temperature, high pressure, burn into radiation, wearing and tearing.
Silicon carbide can be produced by various processes.The silicon carbide better performances that adopts hot-pressing sintering technique to manufacture, but production cost also significantly improves thereupon; The silicon carbide that adopts pressureless sintering to prepare, its ingredient requirement is higher, and sintering temperature is high, and product size changes greatly, and complex process and performance are not high; The silicon carbide products density that adopts reaction sintering technology to produce is high, and ballistic performance is better, and preparation cost is relatively low.
Traditional reaction sintering technology is at vacuum environment and the temperature higher than silicon fusing point (1410 ℃), the silicon liquid of melting is penetrated in the porous ceramics biscuit that contains carbon, after silicon reacts with carbon in biscuit internal in-situ Formed SiClx.Compare with hot pressed sintering or non-pressure sintering technology, reaction sintering can carry out at relatively low temperature, can effectively suppress many adverse effects and variation that material at high temperature occurs.
But traditional reaction sintering technology also has some limitation.First, the sintering temperature that traditional reaction sintering technology is generally selected is between 1480-1750 ℃, and sintering temperature is still higher, and carborundum grain is comparatively thick; In addition, due to the silicon carbide volume forming in reaction sintering process, to have increased twice many, complete in order to guarantee carbon and the pasc reaction of biscuit inside, carbon content in biscuit must be lower than Theoretical Calculation numerical value, otherwise the silicon carbide that causes reaction sintering to form is blocked to the through hole on biscuit top layer, make biscuit heart portion underburnt carbon residue, thereby product properties is significantly declined.Therefore, in silicon carbide reaction-sintered goods, exist a large amount of free silicas, correspondingly also in the performance that has to a certain degree reduced product.
Summary of the invention
In order to overcome the defect existing in prior art, the present invention uses novel reaction sintering infiltration agent, has reduced greatly reaction sintering temperature, has reduced the contents of free si in goods simultaneously, has prepared a kind of low temperature reaction sintering thyrite.
Technical scheme of the present invention is achieved in that a kind of preparation method of low temperature reaction sintering silicon carbide, it is characterized in that comprising the following steps successively:
Step 1, mixes rear formation mixed powder by carbon dust, carborundum powder and appropriate forming agent, after die forming, obtains biscuit of ceramics;
Step 2, by metallic aluminium and silumin powder respectively in mould press forming obtain aluminium pressed compact and silumin pressed compact;
Step 3, is stacked together metallic aluminium base, biscuit of ceramics and silumin pressed compact in turn, and heat preservation sintering in vacuum oven, obtains silicon carbide reaction-sintered.
Described forming agent is resol, polyoxyethylene glycol, Walocel MT 20.000PV or paraffin, and the mass percent of forming agent in mixed powder is 5 ~ 15%, and the mass percent of carbon dust in mixed powder is 3 ~ 15%, and all the other are carborundum powder; Described metallic aluminium base quality is 1 ~ 4 times of carbon dust quality in biscuit; Described silumin pressed compact quality is 2 ~ 5 times of carbon dust quality in biscuit, and the chemical composition of silumin is: the mass percent of silicon is 60 ~ 75%, and all the other are aluminium; Described high-temperature vacuum condition is respectively: sintering range is 1200 ~ 1350 ℃, and soaking time is 1 ~ 3h, and in sintering process, vacuum tightness is not less than 5 * 10
-1pa.
With respect to prior art, the present invention has the following advantages: the processing method that the present invention proposes, by the improvement of special raw material, formula, complete processing, make the silicon carbide reaction-sintered product that silicon carbide reaction-sintered product is produced than other operational path have contents of free si still less, higher density, higher fracture toughness property and better ballistic performance.The contents of free si of conventionally general silicon carbide reaction-sintered product is between 14 ~ 18%, and density is about 3.0 ~ 3.05g/cm
3, the contents of free si of the silicon carbide reaction-sintered product that the present invention is prepared is reduced to 8 ~ 12%, density 3.07 ~ 3.12 g/cm
3.
Accompanying drawing explanation
Fig. 1 is ceramics biscuits of carbonized bricks, metallic aluminium base and silumin pressed compact stacked configuration schematic diagram.
Embodiment
Embodiment 1
A preparation method for low temperature reaction sintering silicon carbide, preparation technology comprises the following steps:
Step 1, mixes 5 parts of 10 parts of carbon dusts, 85 parts of carborundum powders, phenol resin solution, and after ball milling, spray-drying process, in mould, press forming obtains ceramics biscuits of carbonized bricks;
Step 2, by metallic aluminium powder press molding in mould, obtains metallic aluminium base; The silumin powder press molding in mould that is Si75Al25 by chemical composition, obtains silumin pressed compact;
Step 3, is stacked together ceramics biscuits of carbonized bricks 2, metallic aluminium base 1 and silumin pressed compact 3, as shown in Figure 1.The quality of metallic aluminium base is 4 times of carbon dust quality in ceramics biscuits of carbonized bricks, and the quality of silumin pressed compact is 5 times of carbon dust quality in silicon carbide biscuit;
Step 4 is reacted above-mentioned pressed compact to melting infiltration sintering in vacuum oven, and the processing condition of melting infiltration sintering are: sintering range is 1350 ℃, and soaking time is 1h, and in sintering process, vacuum tightness 2 * 10
-1pa.
Embodiment 2
A preparation method for low temperature reaction sintering silicon carbide, preparation technology comprises the following steps:
Step 1, mixes 8 parts of 8 parts of carbon dusts, 84 parts of carborundum powders, phenol resin solution, and after ball milling, spray-drying process, in mould, press forming obtains ceramics biscuits of carbonized bricks;
Step 2, by metallic aluminium powder press molding in mould, obtains metallic aluminium base; The silumin powder press molding in mould that is Si60Al40 by chemical composition, obtains silumin pressed compact;
Step 3, is stacked together ceramics biscuits of carbonized bricks, metallic aluminium base and silumin pressed compact, as shown in Figure 1.The quality of metallic aluminium base is 5 times of carbon dust quality in ceramics biscuits of carbonized bricks, and the quality of silumin pressed compact is 2 times of carbon dust quality in silicon carbide biscuit;
Step 4 is reacted above-mentioned pressed compact to melting infiltration sintering in vacuum oven, and the processing condition of melting infiltration sintering are: sintering range is 1200 ℃, and soaking time is 3h, and in sintering process, vacuum tightness 1 * 10
-1pa.
Embodiment 3
A preparation method for low temperature reaction sintering silicon carbide, comprises the following steps successively:
Step 1, mixes rear formation mixed powder by 5 parts of 3 parts of carbon dusts, 92 parts of carborundum powders and polyoxyethylene glycol, after die forming, obtains biscuit of ceramics;
Step 2, obtains aluminium pressed compact by metallic aluminium press forming in mould, and the silumin powder press forming in mould that is Si75Al25 by chemical composition obtains silumin pressed compact;
Step 3, is stacked together metallic aluminium base, biscuit of ceramics and silumin pressed compact in turn, and heat preservation sintering in vacuum oven, obtains silicon carbide reaction-sintered.Described metallic aluminium base quality is 1 times of carbon dust quality in biscuit; Described silumin pressed compact quality is 2 times of carbon dust quality in biscuit.
Step 4 is reacted above-mentioned pressed compact to melting infiltration sintering in vacuum oven, and the processing condition of melting infiltration sintering are: sintering range is 1200 ℃, and soaking time is 1h, and in sintering process, vacuum tightness 5 * 10
-1pa.
Embodiment 4
A preparation method for low temperature reaction sintering silicon carbide, comprises the following steps successively:
Step 1, mixes rear formation mixed powder by 15 parts of 15 parts of carbon dusts, 70 parts of carborundum powders and Walocel MT 20.000PVs, after die forming, obtains biscuit of ceramics;
Step 2, obtains aluminium pressed compact by metallic aluminium press forming in mould, and the silumin powder press forming in mould that is Si60Al40 by chemical composition obtains silumin pressed compact;
Step 3, is stacked together metallic aluminium base, biscuit of ceramics and silumin pressed compact in turn, and heat preservation sintering in vacuum oven, obtains silicon carbide reaction-sintered.Described metallic aluminium base quality is 4 times of carbon dust quality in biscuit; Described silumin pressed compact quality is 5 times of carbon dust quality in biscuit.
Step 4 is reacted above-mentioned pressed compact to melting infiltration sintering in vacuum oven, and the processing condition of melting infiltration sintering are: sintering range is 1350 ℃, and soaking time is 3h, and in sintering process, vacuum tightness 1 * 10
-1pa.
Above specific embodiment, the present invention is further understood in exemplary illustration and help.But embodiment detail is only for the present invention is described, do not represent the whole technical schemes of the present invention under conceiving, therefore should not be construed as the restriction to technical scheme of the present invention.Some do not depart from the unsubstantiality of the present invention's design changes, for example, to have simple the change or replacement of technical characterictic of same or similar technique effect, all belong to rights protection scope of the present invention.
Claims (2)
1. a preparation method for low temperature reaction sintering silicon carbide, is characterized in that comprising the following steps successively:
Step 1, mixes rear formation mixed powder by carbon dust, carborundum powder and appropriate forming agent, after die forming, obtains biscuit of ceramics;
Step 2, by metallic aluminium and silumin powder respectively in mould press forming obtain aluminium pressed compact and silumin pressed compact;
Step 3, is stacked together metallic aluminium base, biscuit of ceramics and silumin pressed compact in turn, and heat preservation sintering in vacuum oven, obtains silicon carbide reaction-sintered.
2. according to the preparation method of a kind of low temperature reaction sintering silicon carbide described in right 1, it is characterized in that: described forming agent is resol, polyoxyethylene glycol, Walocel MT 20.000PV or paraffin, the mass percent of forming agent in mixed powder is 5 ~ 15%, the mass percent of carbon dust in mixed powder is 3 ~ 15%, and all the other are carborundum powder; Described metallic aluminium base quality is 1 ~ 4 times of carbon dust quality in biscuit; Described silumin pressed compact quality is 2 ~ 5 times of carbon dust quality in biscuit, and the chemical composition of silumin is: the mass percent of silicon is 60 ~ 75%, and all the other are aluminium; Described high-temperature vacuum condition is respectively: sintering range is 1200 ~ 1350 ℃, and soaking time is 1 ~ 3h, and in sintering process, vacuum tightness is not less than 5 * 10
-1pa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106482563A (en) * | 2016-10-20 | 2017-03-08 | 合肥海宝节能科技有限公司 | The processing method of heat exchanger tube |
| CN107721430A (en) * | 2017-09-30 | 2018-02-23 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of the Boral alloy composite plate with crack arrest through hole |
| CN111811322A (en) * | 2020-07-22 | 2020-10-23 | 赛福纳米科技(徐州)有限公司 | Ceramic-titanium alloy-PE composite bulletproof deck and preparation method thereof |
| CN112390653A (en) * | 2020-11-16 | 2021-02-23 | 中国工程物理研究院材料研究所 | Method for preparing ceramic powder based on freezing casting molding |
| CN114180967A (en) * | 2021-12-30 | 2022-03-15 | 浙江立泰复合材料股份有限公司 | Hollow ceramic material and preparation method thereof |
| CN114702317A (en) * | 2022-03-24 | 2022-07-05 | 湖南太子新材料科技有限公司 | Low-temperature sintering method of high-performance silicon carbide ceramic material |
| EP4230336A4 (en) * | 2020-11-12 | 2024-03-20 | Ling Dong Nuclear Power Co Ltd | Silicon carbide cladding and brazing connection method therefor, and fuel rod and fuel assembly |
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| CN101289319A (en) * | 2008-06-03 | 2008-10-22 | 浙江东新密封有限公司 | Reaction sintering silicon carbide ceramic and production method thereof |
| CN102161594A (en) * | 2011-05-12 | 2011-08-24 | 浙江大学 | SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof |
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2014
- 2014-06-19 CN CN201410276905.1A patent/CN104030688A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289319A (en) * | 2008-06-03 | 2008-10-22 | 浙江东新密封有限公司 | Reaction sintering silicon carbide ceramic and production method thereof |
| CN102161594A (en) * | 2011-05-12 | 2011-08-24 | 浙江大学 | SiC whisker reinforced SiC ceramic matrix composite and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106482563A (en) * | 2016-10-20 | 2017-03-08 | 合肥海宝节能科技有限公司 | The processing method of heat exchanger tube |
| CN107721430A (en) * | 2017-09-30 | 2018-02-23 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of the Boral alloy composite plate with crack arrest through hole |
| CN111811322A (en) * | 2020-07-22 | 2020-10-23 | 赛福纳米科技(徐州)有限公司 | Ceramic-titanium alloy-PE composite bulletproof deck and preparation method thereof |
| EP4230336A4 (en) * | 2020-11-12 | 2024-03-20 | Ling Dong Nuclear Power Co Ltd | Silicon carbide cladding and brazing connection method therefor, and fuel rod and fuel assembly |
| CN112390653A (en) * | 2020-11-16 | 2021-02-23 | 中国工程物理研究院材料研究所 | Method for preparing ceramic powder based on freezing casting molding |
| CN114180967A (en) * | 2021-12-30 | 2022-03-15 | 浙江立泰复合材料股份有限公司 | Hollow ceramic material and preparation method thereof |
| CN114180967B (en) * | 2021-12-30 | 2023-01-31 | 浙江立泰复合材料股份有限公司 | Hollow ceramic material and preparation method thereof |
| CN114702317A (en) * | 2022-03-24 | 2022-07-05 | 湖南太子新材料科技有限公司 | Low-temperature sintering method of high-performance silicon carbide ceramic material |
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Application publication date: 20140910 |