CN1134404A - Preparation method of alpha-Si3N4 whisker - Google Patents
Preparation method of alpha-Si3N4 whisker Download PDFInfo
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- CN1134404A CN1134404A CN 95111332 CN95111332A CN1134404A CN 1134404 A CN1134404 A CN 1134404A CN 95111332 CN95111332 CN 95111332 CN 95111332 A CN95111332 A CN 95111332A CN 1134404 A CN1134404 A CN 1134404A
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- silicon nitride
- nitride crystal
- crystal whisker
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- whisker
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Abstract
By using silicon oxide powder of proper size as material and at the nitrogen atmosphere of certain pressure, monocrystalline Alpha-Si3N4 whisker with integral crystalline structure and excellent surface quality is produced through direct reaction at 1200-1600 deg.C in graphite container. The product may be used for reinforcing and flexibilizing composite material and as special functional material.
Description
The invention belongs to the material engineering field, particularly a kind of method for preparing ceramic whisker.
The single-crystal ceramic whisker is because mechanical property and unique physicalies such as its good intensity, Young's modulus, and is used widely in various types of matrix materials (metal matrix, ceramic base, resin base etc.).Range of application and prospect with silicon carbide and silicon nitride is the most wide again in various whiskers.Though not as silicon carbide, it has lower hot exapnsion coefficient and thermal conductivity and advantages such as higher dielectric constant and resistivity to silicon nitride crystal whisker aspect intensity and modulus.Thereby be better than silicon carbide whisker in the application of many occasions, so be subjected to extensive attention in recent years.
Document (1-12) has been reported several methods that prepare silicon nitride crystal whisker.Document 1 (Japanese Patent: JP0427600[9227600]) is a raw material with the silicon oxide-carbon mixture that makes by water glass and hydrocarbon polymer, and needs a kind of Special Metal catalyzer; Document 2 (WANG, Ming Jong and WADA, Harue: " Synthesis andcharaterization of silicon nitride whiskers ", J.Mater.Sci., 25 (1990), 1690-1698) method of mentioning need keep the oxygen of certain dividing potential drop, and products therefrom is Pei Ta-silicon nitride crystal whisker; Document 3 (Canadian Patent: be raw material CA2000457) with silicon oxide and silicon nitride crystal whisker mixture, and the mixed gas and the magnesium-yttrium-transition metal catalyzer that need ammonia and carbon-hydrogen compound to form; Document 4 (Japanese Patent: JP0251499[9051499]) need elder generation with silicon or SiO 2 powder and metal-powder mixed sintering, and then count under the atmosphere of hydrogen at nitrogen-percent five body constituents integration, and add the further thermal degradation of iron powder; Document 5 (Japanese Patent: JP0274598[9074598]) then with silicon-dioxide and iron, nickel, chromium, the mixture of cobalt etc. are raw material, still need to react under the mixed atmosphere of carbon-hydrogen compound and ammonia; It is raw material that document 6 (Japanese Patent: JP0234598[9034598]) has been introduced a kind of halogenide and ammonia with silicon, prepares the method for silicon nitride crystal whisker with CVD (Chemical Vapor Deposition) method; It is the method for feedstock production silicon nitride crystal whisker with silicon-dioxide, carbon and fluorochemical that document 7 (Japanese Patent: JP01301594[89301594]) has been introduced a kind of; Document 8 (Japanese Patent: JP01301595[89301595] all to need with the metal be catalyzer for the method introduced with document 9 (Japanese Patent: JP013001596[89301596]); It is the method for raw material with the rice husk that document 10 (Japanese Patent: JP01179800[89179800]) has been introduced a kind of, but the technology more complicated; Document 11 (Japanese Patent: JP01278500[89278500]) and document 12 (Chinese patent: CN1056908A) then introduced the method for preparing Pei Ta-silicon nitride crystal whisker; The method of document 11 needs silicon dioxide powder is burnt till amorphous silicon nitride in advance in ammonia and hydrocarbon atmosphere, and reacting by heating forms under the metal halide substance environment then; 12 need of document are the amorphous oxides of silicon and carbon dust mixed sintering by a certain percentage in advance, and need to feed an amount of argon gas controls reaction speed.
The purpose of this invention is to provide a kind of method for preparing alpha-silicon nitride crystal whisker.Prepare alpha-silicon nitride crystal whisker by this method and do not need Special Metal catalyzer, production process is simple, is suitable for producing in batches.
The present invention is raw material with granularity less than 0.5 millimeter single silicon oxide powder, or directly evenly be layed in the crystal vessel (the alleged container of the present invention includes the object that can place and preserve solid matter of Any shape) with powdery, or after being cold-pressed into idiosome, put into crystal vessel, or be mixed into to be coated with behind the slurry to invest on 1600 ℃ of liner plates that decomposition do not take place with water and put into crystal vessel again, need not any additives, also need not any other gas except that nitrogen, only need in crystal vessel, to pass to the nitrogen of 0.1MPa～200MPa pressure, can to obtain crystalline structure in 0.5 hour～5.0 hours complete in insulation between 1200 ℃～1600 ℃, surface quality is good, length is 10 μ m～1000 μ m, and diameter is monocrystalline alpha-silicon nitride crystal whisker of 0.5 μ m～5.0 μ m.Typical pattern under transmission electron microscope as shown in Figure 1.
Description of drawings of the present invention:
Fig. 1 is the transmission electron microscope photo of alpha-silicon nitride crystal whisker of being obtained by the embodiment of the invention one.
With aforementioned the whole bag of tricks relatively, although existing preparation silicon nitride crystal whisker method all take silicon-containing compound as raw material, But need to mix with the certain proportion carbon dust, or need add certain catalyst, other gas that maybe need be except nitrogen Body is controlled reaction speed. We's rule need be except silica other raw material, and primary first-order equation finishes, Have the advantages such as obvious raw material are single, process is simple, without any need for the gas that might pollute, Be suitable for batch production.
Below provide two embodiment of the present invention:
Embodiment one: be applied on the liner plate that does not decompose below 1600 ℃ (as aluminum oxide etc.) after-100 purpose silica powders and water are mixed into slurry, oven dry or seasoning are placed in the crystal vessel, pass to 0.7MPa pressure nitrogen gas (99.90%) 1500 ℃ of reactions two hours.The whisker that makes with above-mentioned technology is defined as monocrystalline alpha-silicon nitride crystal whisker through X-ray and transmissioning electric mirror test, mean length 90 μ m, and mean diameter 1.5 μ m, its transmission electron microscope pattern is as shown in Figure 1.Obvious oxidation does not take place during at 1250 ℃ through differential thermal analysis.Though (present embodiment mentions that nitrogen gas purity is 99.90%, and this purity requirement is not to be essential condition for enforcement of the present invention.)
Embodiment two: with the starting material identical, is placed in the crystal vessel identical with embodiment one through being cold-pressed into idiosome with embodiment one, and at the 150MPa pressure nitrogen gas, 1450 ℃ of reactions 1.5 hours down.Resulting product is monocrystalline alpha-silicon nitride crystal whisker on the idiosome surface, mean length 80 μ m, mean diameter 1.7 μ m.
Claims (6)
1. a method for preparing alpha-silicon nitride crystal whisker is characterized in that with single silicon oxide powder be raw material, passes to the nitrogen of certain pressure in crystal vessel, reacts certain hour at a certain temperature.
2. according to the described method for preparing alpha-silicon nitride crystal whisker of claim 1, the granularity of silicon oxide powder is less than 0.5mm.
3. according to the described method for preparing alpha-silicon nitride crystal whisker of claim 1, the nitrogen gas pressure scope is 0.1MPa～200MPa.
4. according to the described method for preparing alpha-silicon nitride crystal whisker of claim 1, temperature of reaction is 1200 ℃～1600 ℃.
5. according to the described method for preparing alpha-silicon nitride crystal whisker of claim 1, the reaction times is 0.5 hour～5.0 hours.
6. according to the described method for preparing alpha-silicon nitride crystal whisker of claim 1～5, resulting product is length 10 μ m～1000 μ m, the alpha crystal formation monocrystalline silicon nitride crystal whisker of diameter 0.5 μ m～5.0 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95111332 CN1134404A (en) | 1995-04-25 | 1995-04-25 | Preparation method of alpha-Si3N4 whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95111332 CN1134404A (en) | 1995-04-25 | 1995-04-25 | Preparation method of alpha-Si3N4 whisker |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1134404A true CN1134404A (en) | 1996-10-30 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95111332 Pending CN1134404A (en) | 1995-04-25 | 1995-04-25 | Preparation method of alpha-Si3N4 whisker |
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| CN (1) | CN1134404A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327046C (en) * | 2005-07-15 | 2007-07-18 | 清华大学 | Monocrystalline Si3N4 nanometer belt and micro belt preparation method |
| CN101864620A (en) * | 2010-07-30 | 2010-10-20 | 哈尔滨工业大学 | Preparation method of silicon nitride whisker |
-
1995
- 1995-04-25 CN CN 95111332 patent/CN1134404A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327046C (en) * | 2005-07-15 | 2007-07-18 | 清华大学 | Monocrystalline Si3N4 nanometer belt and micro belt preparation method |
| CN101864620A (en) * | 2010-07-30 | 2010-10-20 | 哈尔滨工业大学 | Preparation method of silicon nitride whisker |
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