CN1112466C - Preparation method of nanometer silicon carbide whiskers - Google Patents
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 238000000352 supercritical drying Methods 0.000 claims abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 239000005543 nano-size silicon particle Substances 0.000 claims description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 229960004756 ethanol Drugs 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 239000012300 argon atmosphere Substances 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000004964 aerogel Substances 0.000 claims description 5
- 150000003857 carboxamides Chemical group 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract 1
- 238000005299 abrasion Methods 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000005262 decarbonization Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 5
- 239000002010 green coke Substances 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本发明属于一种碳化硅晶须的制备方法，具体地说涉及一种制备直径为纳米级的碳化硅晶须的方法。The invention belongs to a method for preparing silicon carbide whiskers, in particular to a method for preparing silicon carbide whiskers with a diameter of nanoscale.
碳化硅晶须具有低密度、高熔点、高强度、高模量、热膨胀率低及耐腐蚀、耐磨等优良特性，作为金属基、陶瓷基等复合材料的补强增韧剂，被广泛应用于机械、电子、航空航天及能源等领域。Silicon carbide whiskers have excellent properties such as low density, high melting point, high strength, high modulus, low thermal expansion, corrosion resistance, and wear resistance. They are widely used as reinforcing and toughening agents for metal-based, ceramic-based and other composite materials. In the fields of machinery, electronics, aerospace and energy.
碳化硅晶须的制备方法主要是使用不同硅源、炭源的碳热还原法。美国的Cutel[AM.Ceram.SOc.Bull.，1975，54(2)：195]利用酸处理碳化稻壳为原料，外加SiO2调整原料的SiO2与C的比例，均匀加入复合催化剂碳化钨，装入石墨坩埚中，通入Ar气作保护性体，于高温下进行碳热还原反应制备出亚微米级的碳化硅晶须。此外还有利用超细炭粉与高岭土为原料，过碳热还原制备碳化硅晶须[纤维复合材料，1992，(1)：20-22]。由于炭源反应活性低，且Si源与炭源难以达到均匀混合，上述方法制得的碳化硅晶须主要为亚微米级。The preparation method of silicon carbide whiskers is mainly the carbothermal reduction method using different silicon sources and carbon sources. U.S. Cutel[AM.Ceram.SOc.Bull., 1975,54(2):195] uses acid treatment carbonized rice husk as raw material, adds SiO 2 to adjust the ratio of SiO 2 and C of the raw material, and evenly adds composite catalyst tungsten carbide , put it into a graphite crucible, pass through Ar gas as a protective body, and carry out carbothermal reduction reaction at high temperature to prepare submicron silicon carbide whiskers. In addition, silicon carbide whiskers are prepared by using ultra-fine carbon powder and kaolin as raw materials through carbothermal reduction [Fiber Composite Materials, 1992, (1): 20-22]. Due to the low reactivity of the carbon source and the difficulty in uniform mixing of the Si source and the carbon source, the silicon carbide whiskers prepared by the above method are mainly submicron.
本发明的发明目的是提供一种直径分布均匀的直径为纳米级的碳化硅晶须的制备方法。The object of the present invention is to provide a method for preparing nano-scale silicon carbide whiskers with uniform diameter distribution.
本发明的制备方法具体步骤如下：The specific steps of the preparation method of the present invention are as follows:
(1)将炭质水性中间相溶解于有机溶剂或氨水，得到炭质溶胶-凝胶，然后加入无水乙醇或丙酮脱除其中的有机溶剂或氨水，制得净炭质溶胶；(1) dissolving the carbonaceous water-based mesophase in an organic solvent or ammonia water to obtain a carbonaceous sol-gel, and then adding absolute ethanol or acetone to remove the organic solvent or ammonia water therein to obtain a clean carbonaceous sol;
(2)加入无水乙醇或丙酮脱除硅溶胶中的溶液，制得净硅溶胶；(2) add dehydrated alcohol or acetone to remove the solution in the silica sol, make net silica sol;
(3)将净炭质溶胶和净硅溶胶按炭和硅摩尔比(3-8)∶1于室温下搅拌混和24小时，制得二元净炭质-硅溶胶；(3) Stir and mix the net carbonaceous sol and the net silica sol at room temperature for 24 hours according to the molar ratio of carbon to silicon (3-8): 1, to obtain a binary net carbonaceous-silica sol;
(4)将二元净炭质—硅溶胶于100-150℃干燥4-6小时，得到二元干凝胶；或将二元净炭质-硅溶胶放入高压釜中，在240-280℃，6.0-8.5MPa下进行超临界干燥，时间为20-180分钟，放出超临界介质之后，以惰性气体吹扫至室温，制得二元气凝胶；(4) Dry the binary net carbonaceous-silica sol at 100-150°C for 4-6 hours to obtain a binary xerogel; or put the binary net carbonaceous-silica sol in an autoclave, ℃, 6.0-8.5MPa for supercritical drying, the time is 20-180 minutes, after the supercritical medium is released, it is purged to room temperature with an inert gas to obtain a binary airgel;
(5)将所制得的二元干凝胶或二元气凝胶置于石墨坩锅中，在氩气气氛下以(1-20)℃/min的升温速率升到1300-1600℃，进行碳热还原反应，维持温度0.5-4小时，制得未提纯直径为纳米级的碳化硅晶须；(5) Place the prepared binary xerogel or binary aerogel in a graphite crucible, raise the temperature to 1300-1600°C at a rate of (1-20)°C/min under an argon atmosphere, and carry out Carbothermal reduction reaction, maintain the temperature for 0.5-4 hours, and prepare unpurified silicon carbide whiskers with a nanometer diameter;
(6)将未提纯的直径为纳米级的碳化硅晶须在450-480℃下灼烧16-24小时脱碳，然后在HF溶液中脱去SiO2，制得纯直径为纳米级的碳化硅晶须。(6) Decarburize unpurified silicon carbide whiskers with a diameter of nanometer at 450-480°C for 16-24 hours, and then remove SiO 2 in HF solution to obtain pure silicon carbide whiskers with a diameter of nanometer Silicon whiskers.
所述的有机溶剂是有机酰胺、乙二醇、丙酮。Described organic solvent is organic amide, ethylene glycol, acetone.
所述的超临界介质是乙醇、二氧化碳。The supercritical medium is ethanol and carbon dioxide.
本发明与现有技术相比具有如下优点：Compared with the prior art, the present invention has the following advantages:
所得的纳米碳化硅晶须直径分布均匀，长径比大，晶须转化率高，原料易得且反应活性高。The obtained nano-silicon carbide whiskers have uniform diameter distribution, large length-to-diameter ratio, high whisker conversion rate, easy-to-obtain raw materials and high reactivity.
本发明的实施例如下：Embodiments of the present invention are as follows:
实施例1Example 1
(1)将含炭1.5mol的由石油生焦制得的炭质水性中间相，溶解于120ml丙酮中，制成炭质溶胶，分四次加入总量500ml乙醇，脱除其中的丙酮溶液，制得净炭质溶胶。将含硅0.5mol的硅溶胶，用同样的方法脱除硅溶胶中的溶剂制得净硅溶胶；(1) Dissolve the carbonaceous aqueous mesophase produced by petroleum green coke containing 1.5mol of carbon in 120ml of acetone to make a carbonaceous sol, add a total of 500ml of ethanol in four times, remove the acetone solution therein, A net carbonaceous sol is obtained. With the silica sol containing 0.5mol of silicon, the solvent in the silica sol is removed by the same method to obtain a net silica sol;
(2)将净炭质溶胶和净硅溶胶于室温下搅拌混和24小时，制得净二元溶胶；(2) Stir and mix the net carbonaceous sol and the net silica sol at room temperature for 24 hours to obtain the net binary sol;
(3)将净二元溶胶于100℃下干燥6小时，得到二元干凝胶；(3) drying the net binary sol at 100° C. for 6 hours to obtain a binary xerogel;
(4)将所制得的二元干凝胶置于石墨坩埚中，在氩气气氛下以1℃/min的速率升温到1300℃进行碳热还原反应，维持温度4小时，制得未提纯纳米碳化硅晶须；(4) Place the prepared binary xerogel in a graphite crucible, heat up to 1300°C at a rate of 1°C/min under an argon atmosphere for carbothermal reduction reaction, and maintain the temperature for 4 hours to obtain unpurified Nano silicon carbide whiskers;
(5)将未提纯纳米碳化硅晶须于480℃下灼烧16小时脱碳，然后在HF溶液中脱去SiO2，水洗至中性，于120℃干燥制得纯纳米碳化硅晶须，晶须直径为50-90nm，长度为1-5μm。碳化硅晶须的转化率为60％。(5) Decarburize the unpurified nano silicon carbide whiskers by burning at 480°C for 16 hours, then remove SiO 2 in HF solution, wash with water until neutral, and dry at 120°C to obtain pure nano silicon carbide whiskers, The whiskers have a diameter of 50-90 nm and a length of 1-5 μm. The conversion of silicon carbide whiskers was 60%.
实施例2Example 2
(1)将含炭1.6mol的由石油生焦制得的炭质水性中间相，溶解于120ml乙二醇中，制成炭质凝胶，分四次加入总量1000ml乙醇，脱除其中的乙二醇溶液，制得净炭质溶胶。将含硅0.2mol的硅溶胶，用同样的方法脱除硅溶胶中得溶剂制得净硅溶胶；(1) Dissolve the carbonaceous aqueous mesophase obtained from petroleum green coke containing 1.6mol of carbon in 120ml of ethylene glycol to make a carbonaceous gel, add a total of 1000ml of ethanol in four times, and remove the Ethylene glycol solution to obtain a clean carbonaceous sol. With the silica sol containing 0.2mol of silicon, the solvent obtained in the silica sol is removed by the same method to obtain the net silica sol;
(2)将净炭质溶胶和净硅溶胶于室温下搅拌混和24小时，制得净二元溶胶；(2) Stir and mix the net carbonaceous sol and the net silica sol at room temperature for 24 hours to obtain the net binary sol;
(3)将净二元溶胶于150℃下干燥4小时，得到二元干凝胶；(3) drying the net binary sol at 150° C. for 4 hours to obtain a binary xerogel;
(4)将所制得的二元干凝胶置于石墨坩埚中，在氩气气氛下以20℃/min的速率升温到1600℃进行碳热还原反应，维持温度0.5小时，制得未提纯纳米碳化硅晶须；(4) Place the prepared binary xerogel in a graphite crucible, heat up to 1600°C at a rate of 20°C/min under an argon atmosphere for carbothermal reduction reaction, and maintain the temperature for 0.5 hours to obtain unpurified Nano silicon carbide whiskers;
(5)将未提纯纳米碳化硅晶须于450℃下灼烧24小时脱碳，然后在HF溶液中脱去SiO2，水洗至中性，于120℃干燥制得纯纳米碳化硅晶须，晶须直径为80-90nm，长度为1-4μm。碳化硅晶须的转化率为90％。(5) Decarburize the unpurified nano silicon carbide whiskers by burning at 450°C for 24 hours, then remove SiO 2 in HF solution, wash with water until neutral, and dry at 120°C to obtain pure nano silicon carbide whiskers, The whiskers have a diameter of 80-90 nm and a length of 1-4 μm. The conversion rate of silicon carbide whiskers was 90%.
实施例3Example 3
(1)将含炭0.4mol的由石油生焦制得的炭质水性中间相，溶解于30ml氨水溶液中，制成炭质凝胶，分三次加入总量600ml乙醇，脱除其中的氨水溶液，制得净炭质溶胶。将含硅0.1mol的硅溶胶，用同样的方法脱除硅溶胶中得溶剂制得净硅溶胶；(1) Dissolve the carbonaceous aqueous mesophase prepared from petroleum green coke containing 0.4mol of carbon in 30ml of ammonia solution to make a carbonaceous gel, add a total of 600ml of ethanol in three times, and remove the ammonia solution , to obtain a net carbonaceous sol. With the silica sol containing 0.1mol of silicon, the solvent obtained in the silica sol is removed by the same method to obtain the net silica sol;
(2)将净炭质溶胶和净硅溶胶于室温下搅拌混和24小时，制得净二元溶胶；(2) Stir and mix the net carbonaceous sol and the net silica sol at room temperature for 24 hours to obtain the net binary sol;
(3)将净二元溶胶，放入0.5升高压釜中的50ml不锈钢筒中，再在釜中加入420ml乙醇，升温至280℃，85MPa，维持温度、压力20分钟。放出乙醇，用氮气吹扫冷却至室温，制得二元炭质-硅气凝胶；(3) Put the net binary sol into a 50ml stainless steel cylinder in a 0.5-liter autoclave, then add 420ml of ethanol to the kettle, raise the temperature to 280°C, 85MPa, and maintain the temperature and pressure for 20 minutes. Emit ethanol, cool to room temperature with nitrogen purging, and make binary carbonaceous-silicon aerogel;
(4)将所制得的二元碳质-硅气凝胶置于石墨坩埚中，在氩气气氛下以3℃/min的速率升温到1400℃进行碳热还原反应，维持温度1小时，制得未提纯纳米碳化硅晶须；(4) Place the prepared binary carbonaceous-silicon aerogel in a graphite crucible, heat up to 1400°C at a rate of 3°C/min under an argon atmosphere for carbothermal reduction reaction, and maintain the temperature for 1 hour, Prepare unpurified nano silicon carbide whiskers;
(5)将未提纯纳米碳化硅晶须于460℃下灼烧20小时脱碳，然后在HF溶液中脱去SiO2，水洗至中性，于120℃干燥制得纯纳米碳化硅晶须，晶须直径为20-80nm，长度为3-10μm。碳化硅晶须的转化率为95％。(5) Decarburize the unpurified nano silicon carbide whiskers by burning at 460°C for 20 hours, then remove SiO 2 in HF solution, wash with water until neutral, and dry at 120°C to obtain pure nano silicon carbide whiskers, The whiskers have a diameter of 20-80 nm and a length of 3-10 μm. The conversion of silicon carbide whiskers was 95%.
实施例4Example 4
(1)如实施例3中步骤(1)、(2)，制得净二元溶胶；(1) As in steps (1) and (2) in Example 3, a net binary sol is obtained;
(2)将所制得的净二元溶胶，放入0.5升高压釜中的50ml不锈钢筒中，再在釜中通入二氧化碳气体，升温至200℃，70MPa，维持温度，压力50分钟；放出乙醇和二氧化碳，用氮气吹扫冷却至室温，制得二元碳质-硅气凝胶；(2) Put the prepared net binary sol into a 50ml stainless steel cylinder in a 0.5-liter autoclave, then feed carbon dioxide gas into the kettle, raise the temperature to 200°C, 70MPa, maintain the temperature, and pressure for 50 minutes; release ethanol and carbon dioxide, purged with nitrogen and cooled to room temperature to prepare binary carbonaceous-silicon airgel;
(3)将所制得的二元干凝胶置于石墨坩埚中，在氩气气氛下以5℃/min的速率升温到1350℃进行碳热还原反应，维持温度2小时，制得未提纯纳米碳化硅晶须；(3) Place the prepared binary xerogel in a graphite crucible, heat up to 1350°C at a rate of 5°C/min under an argon atmosphere for carbothermal reduction reaction, and maintain the temperature for 2 hours to obtain unpurified Nano silicon carbide whiskers;
(4)将未提纯纳米碳化硅晶须于460℃下灼烧20小时脱碳，然后在HF溶液中脱去SiO2，水洗至中性，于120℃干燥制得纯纳米碳化硅晶须，晶须直径为80-90nm，长度为10-50μm。碳化硅晶须的转化率为95％。(4) Decarburize the unpurified nano silicon carbide whiskers by burning at 460°C for 20 hours, then remove SiO 2 in HF solution, wash with water until neutral, and dry at 120°C to obtain pure nano silicon carbide whiskers, The whiskers have a diameter of 80-90 nm and a length of 10-50 μm. The conversion of silicon carbide whiskers was 95%.
实施例5Example 5
(1)将含碳0.6mol的由石油生焦制得的炭质水性中间相，溶解于20ml乙二醇中，制成炭质溶胶，分四次加入总量500ml丙酮，脱除其中的乙二醇溶液，制得净炭质溶胶。将含硅0.1mol的硅溶胶，用同样的方法脱除硅溶胶中得溶剂制得净硅溶胶；(1) Dissolve the carbonaceous aqueous mesophase obtained from petroleum green coke containing 0.6mol of carbon in 20ml of ethylene glycol to make a carbonaceous sol, add a total of 500ml of acetone in four times, and remove the ethylene glycol in it. diol solution to obtain a clean carbonaceous sol. With the silica sol containing 0.1mol of silicon, the solvent obtained in the silica sol is removed by the same method to obtain the net silica sol;
(2)将净炭质溶胶和净硅溶胶于室温下搅拌混和24小时，制得净二元溶胶；(2) Stir and mix the net carbonaceous sol and the net silica sol at room temperature for 24 hours to obtain the net binary sol;
(3)将所制得的净二元溶胶，放入0.5升高压釜中的50ml不锈钢筒中，再在釜中通入二氧化碳气体，升温至250℃，75MPa，维持温度，压力40分钟。放出二氧化碳，用氮气吹扫冷却至室温，制得二元碳质-硅气凝胶。(3) Put the obtained net binary sol into a 50ml stainless steel cylinder in a 0.5-liter autoclave, then pass carbon dioxide gas into the kettle, raise the temperature to 250°C, 75MPa, maintain the temperature and pressure for 40 minutes. Release carbon dioxide, blow with nitrogen and cool to room temperature to prepare binary carbonaceous-silicon aerogel.
(4)将所制得的二元干凝胶置于石墨坩埚中，在氩气气氛下以10℃/min的速率升温到1350℃进行碳热还原反应，维持温度3小时，制得未提纯纳米碳化硅晶须；(4) Place the prepared binary xerogel in a graphite crucible, heat up to 1350°C at a rate of 10°C/min under an argon atmosphere for carbothermal reduction reaction, and maintain the temperature for 3 hours to obtain unpurified Nano silicon carbide whiskers;
(5)将未提纯纳米碳化硅晶须于460℃下灼烧20小时脱碳，然后在HF溶液中脱去SiO2，水洗至中性，于120℃干燥制得纯纳米碳化硅晶须，晶须直径为50-90nm，长度为0.5-4μm。碳化硅晶须的转化率为98％。(5) Decarburize the unpurified nano silicon carbide whiskers by burning at 460°C for 20 hours, then remove SiO 2 in HF solution, wash with water until neutral, and dry at 120°C to obtain pure nano silicon carbide whiskers, The whiskers have a diameter of 50-90 nm and a length of 0.5-4 μm. The conversion of silicon carbide whiskers was 98%.
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