JPH05809A - Method for producing silicon nitride-silicon carbide composite powder - Google Patents
Method for producing silicon nitride-silicon carbide composite powderInfo
- Publication number
- JPH05809A JPH05809A JP3175839A JP17583991A JPH05809A JP H05809 A JPH05809 A JP H05809A JP 3175839 A JP3175839 A JP 3175839A JP 17583991 A JP17583991 A JP 17583991A JP H05809 A JPH05809 A JP H05809A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- composite powder
- silicon nitride
- silicon carbide
- producing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 24
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 6
- 239000010703 silicon Substances 0.000 title claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005755 formation reaction Methods 0.000 description 3
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000003961 organosilicon compounds Chemical class 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- -1 aminosilicon compound Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
(57)【要約】
【構成】 シリカ粉末を少なくともアンモニアと炭化水
素を含む混合気流中１５００℃以上で加熱することを特
徴とする窒化けい素−炭化けい素複合粉末の製造方法。
また、雰囲気にさらにＮ2 を添加することもできる。
【効果】 シリカを原料とすることから原料単位重量当
たりの収量が多い。また、１回の加熱工程で、結晶性の
よい安定な粉末を得られる。しかもＮ2 を添加すること
により、その複合粉末中のＳｉ3 Ｎ4 とＳｉＣの生成割
合の制御を可能とした。
(57) [Summary] [Structure] A method for producing a silicon nitride-silicon carbide composite powder, which comprises heating silica powder at 1500 ° C or higher in a mixed gas stream containing at least ammonia and hydrocarbon.
Further, N 2 can be added to the atmosphere. [Effect] Since silica is used as the raw material, the yield per unit weight of the raw material is large. Further, a stable powder having good crystallinity can be obtained by one heating step. Moreover, the addition of N 2 made it possible to control the production ratio of Si 3 N 4 and SiC in the composite powder.
Description
【０００１】[0001]
【産業上の利用分野】本発明は構造用ファインセラミッ
クスの中で、特に高温高強度を必要とする構造材料用原
料となる窒化けい素−炭化けい素複合粉末の製造方法に
関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a silicon nitride-silicon carbide composite powder which is a raw material for a structural material which requires high temperature and high strength among structural fine ceramics.
【０００２】[0002]
【従来の技術】従来の技術として、特開昭６０−２００
８１２〜２００８１４号，及び特開昭６０−２３５７０
７号，並びに特開昭６１−６３５１０号等が挙げられ
る。2. Description of the Related Art As a conventional technique, Japanese Patent Laid-Open No. 60-200
812 to 200814, and JP-A-60-23570.
No. 7, JP-A-61-63510 and the like.
【０００３】上記特許公開公報はいずれも、シアノ基を
含む有機珪素化合物，アミノ珪素化合物あるいはシラザ
ン化合物をガス化した後、１２００〜１４００℃でＮＨ
3 ，Ｎ2 ，Ｈ2 等の非酸化性ガスと反応させることによ
り、窒化けい素−炭化けい素の複合粉末を得るものであ
る。In all of the above-mentioned patent publications, after gasifying an organosilicon compound, an aminosilicon compound or a silazane compound containing a cyano group, NH at 1200 to 1400 ° C.
By reacting with a non-oxidizing gas such as 3 , N 2 , H 2 or the like, a composite powder of silicon nitride-silicon carbide is obtained.
【０００４】[0004]
【発明が解決しようとする課題】従来技術においては、
原料となる有機珪素化合物は、生成する粉末の主要な構
成元素であるＳｉの含有割合が少なく、原料単位重量当
たりの生成粉の収量が小さい。DISCLOSURE OF THE INVENTION In the prior art,
The organosilicon compound as a raw material has a small content ratio of Si, which is a main constituent element of the produced powder, and has a small yield of the produced powder per unit weight of the raw material.
【０００５】また、得られた生成粉は結晶性が悪いこと
から、空気中等での取り扱いを可能とするため、非酸性
雰囲気下での加熱（１５００℃程度）による結晶化処理
を必要とする。Further, since the obtained powder has poor crystallinity, it can be handled in air or the like, and therefore needs to be crystallized by heating in a non-acidic atmosphere (about 1500 ° C.).
【０００６】本発明の目的は、原料単位当りの収量が多
く、結晶性の良い粉末が得やすい窒化けい素−炭化けい
素複合粉末の製造方法を提供することである。It is an object of the present invention to provide a method for producing a silicon nitride-silicon carbide composite powder, which has a large yield per raw material unit and is easy to obtain a powder having good crystallinity.
【０００７】[0007]
【課題を解決するための手段】本発明は、シリカ（Ｓｉ
Ｏ2 ）粉末を少なくともアンモニア（ＮＨ3 ）と炭化水
素を含む混合気流中１５００℃以上で加熱することを特
徴とする窒化けい素（Ｓｉ3 Ｎ4 ）−炭化けい素（Ｓｉ
Ｃ）複合粉末の製造方法である。The present invention relates to silica (Si
O 2 ) powder is heated at 1500 ° C. or higher in a mixed gas stream containing at least ammonia (NH 3 ) and hydrocarbon, silicon nitride (Si 3 N 4 ) -silicon carbide (Si)
C) A method for producing a composite powder.
【０００８】[0008]
【作用】熱力学的に見て、ＳｉＯ2 −ＮＨ3 −Ｃ3 Ｈ8
系においては１５００℃（１７２３Ｋ）以下でＳｉＣを
生成させにくい。これは図２に示すように、ＮＨ3 の熱
分解によるＮ2 分圧との関係において、１５００℃以下
ではＳｉＣが安定に存在しにくいためであると考えてい
る。１５００℃以上においては、Ｓｉ3 Ｎ4 の生成と同
時にＳｉＣを生成させることができる。また、ＳｉＯ2
−ＮＨ3 −Ｃ3 Ｈ8 系にＮ2 ガスを導入し、ＮＨ3 の分
圧を下げることにより、Ｓｉ3 Ｎ4 の生成を抑制し、Ｓ
ｉＣ生成割合を増加できることを見出した。すなわち、
ＳｉＯ2 −ＮＨ3 −Ｃ3 Ｈ8 系において１５００℃以上
とすることで、Ｓｉ3 Ｎ4 とＳｉＣの複合粉末を得るこ
とができる。しかもＮ2 を添加することにより、その複
合粉末中のＳｉ3 Ｎ4 とＳｉＣの生成割合の制御を可能
とした。[Function] Thermodynamically, SiO 2 —NH 3 —C 3 H 8
In the system, it is difficult to generate SiC at 1500 ° C. (1723 K) or lower. This is because, as shown in FIG. 2, SiC is unlikely to exist stably at 1500 ° C. or lower in relation to the N 2 partial pressure due to the thermal decomposition of NH 3 . At 1500 ° C. or higher, SiC can be generated simultaneously with the generation of Si 3 N 4 . In addition, SiO 2
By introducing N 2 gas into the —NH 3 —C 3 H 8 system and reducing the partial pressure of NH 3 , the production of Si 3 N 4 is suppressed, and S
It was found that the iC generation rate can be increased. That is,
By setting the temperature in the SiO 2 —NH 3 —C 3 H 8 system to 1500 ° C. or higher, a composite powder of Si 3 N 4 and SiC can be obtained. Moreover, the addition of N 2 made it possible to control the production ratio of Si 3 N 4 and SiC in the composite powder.
【０００９】図１に符号１で示されているように、Ｓｉ
Ｏ2 −ＮＨ3 −Ｃ3 Ｈ8 系によるＳｉ3 Ｎ4の生成反応
は比較的低温から標準生成自由エネルギーΔＧ°が負で
あることから、反応が極めて進行しやすく、容易にＳｉ
3 Ｎ4 粉末を得ることができる。また、符号２で示され
る反応も比較的低温からΔＧ°が負であり、Ｓｉ3 Ｎ4
と同時にＳｉＣも生成する。As indicated by reference numeral 1 in FIG.
Since the standard free energy of formation ΔG ° is negative at a relatively low temperature, the reaction for producing Si 3 N 4 by the O 2 —NH 3 —C 3 H 8 system is extremely easy to proceed, and Si is easily formed.
3 N 4 powder can be obtained. Also, in the reaction indicated by reference numeral 2, ΔG ° is negative from a relatively low temperature, and Si 3 N 4
At the same time, SiC is also generated.
【００１０】[0010]
【実施例】ＳｉＯ2 粉末３ｇを窒化けい素製ボートに充
填した。このボートを内径５０ｍｍのアルミナ製炉芯管
を有する管状炉内へ入れ、アンモニアガス２ｌ／ｍｉ
ｎ、Ｃ3 Ｈ8 ガス０．２ｌ／ｍｉｎの混合ガスを流しな
がら１６００℃で２時間加熱した。EXAMPLE 3 g of SiO 2 powder was filled in a silicon nitride boat. This boat was put into a tubular furnace having an alumina furnace core tube with an inner diameter of 50 mm, and ammonia gas 2 l / mi
The mixture was heated at 1600 ° C for 2 hours while flowing a mixed gas of n and C 3 H 8 gas at 0.2 l / min.
【００１１】このようにして得た粉末をＳＥＭ観察した
結果、等軸状の均一な微粒子であった。またＸ線的には
α−Ｓｉ3 Ｎ4 とβ−ＳｉＣだけが同定された。さらに
炭素含有量を測定しβ−ＳｉＣの含有率を求めた結果、
１６．５ｗｔ％であった。As a result of SEM observation of the powder thus obtained, it was found to be equiaxed and uniform fine particles. Also, from the X-ray perspective, only α-Si 3 N 4 and β-SiC were identified. Furthermore, as a result of measuring the carbon content and determining the content rate of β-SiC,
It was 16.5 wt%.
【００１２】この他に、アンモニアとＣ3 Ｈ8 にＮ2を
表１に示すように変化させて実験を行った。これらの結
果を表１に示す。In addition to the above, experiments were conducted by changing N 2 to ammonia and C 3 H 8 as shown in Table 1. The results are shown in Table 1.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[0014]
【比較例】加熱温度を１４５０℃とし、ガスを表１に示
すように変化させた他は前記実施例と同様にして生成粉
を得た。その結果も表１に示す。Comparative Example A produced powder was obtained in the same manner as in the above example except that the heating temperature was 1450 ° C. and the gas was changed as shown in Table 1. The results are also shown in Table 1.
【００１５】[0015]
【発明の効果】シリカを原料とすることから原料単位重
量当たりの収量が多い。Since silica is used as the raw material, the yield per unit weight of the raw material is high.
【００１６】また、１回の加熱工程で、結晶性のよい安
定な粉末を得られる。Also, a stable powder having good crystallinity can be obtained by one heating step.
【００１７】しかもＮ2 を添加することにより、その複
合粉末中のＳｉ3 Ｎ4 とＳｉＣの生成割合の制御を可能
とした。Moreover, the addition of N 2 makes it possible to control the production ratio of Si 3 N 4 and SiC in the composite powder.
【図１】Ｓｉ3 Ｎ4 およびＳｉＣの生成反応における自
由エネルギーと温度との関係を表わす図である。FIG. 1 is a diagram showing a relationship between free energy and temperature in a production reaction of Si 3 N 4 and SiC.
【図２】Ｓｉ3 Ｎ4 およびＳｉＣの生成反応とＮ2 分圧
との関係を表わす図である。FIG. 2 is a diagram showing a relationship between a production reaction of Si 3 N 4 and SiC and an N 2 partial pressure.
１ Ｓｉ3 Ｎ4 の生成反応 ２ ＳｉＣの生成反応 ◆1 Si 3 N 4 formation reaction 2 SiC formation reaction ◆
Claims (1)
化水素を含む混合気流中１５００℃以上で加熱すること
を特徴とする窒化けい素−炭化けい素複合粉末の製造方
法。1. A method for producing a silicon nitride-silicon carbide composite powder, which comprises heating the silica powder at 1500 ° C. or higher in a mixed gas stream containing at least ammonia and hydrocarbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3175839A JPH05809A (en) | 1991-06-21 | 1991-06-21 | Method for producing silicon nitride-silicon carbide composite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3175839A JPH05809A (en) | 1991-06-21 | 1991-06-21 | Method for producing silicon nitride-silicon carbide composite powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05809A true JPH05809A (en) | 1993-01-08 |
Family
ID=16003118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3175839A Pending JPH05809A (en) | 1991-06-21 | 1991-06-21 | Method for producing silicon nitride-silicon carbide composite powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05809A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5525556A (en) * | 1994-04-14 | 1996-06-11 | The Dow Chemical Company | Silicon nitride/silicon carbide composite powders |
-
1991
- 1991-06-21 JP JP3175839A patent/JPH05809A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5525556A (en) * | 1994-04-14 | 1996-06-11 | The Dow Chemical Company | Silicon nitride/silicon carbide composite powders |
| US5538675A (en) * | 1994-04-14 | 1996-07-23 | The Dow Chemical Company | Method for producing silicon nitride/silicon carbide composite |
| US5643843A (en) * | 1994-04-14 | 1997-07-01 | The Dow Chemical Company | Silicon nitride/silicon carbide composite densified materials prepared using composite powders |
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