JPS6256371A - Manufacture of silicon carbide sintered body - Google Patents
Manufacture of silicon carbide sintered bodyInfo
- Publication number
- JPS6256371A JPS6256371A JP60195750A JP19575085A JPS6256371A JP S6256371 A JPS6256371 A JP S6256371A JP 60195750 A JP60195750 A JP 60195750A JP 19575085 A JP19575085 A JP 19575085A JP S6256371 A JPS6256371 A JP S6256371A
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- temperature
- sintering
- powder
- sintered body
- 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.)
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Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔発明の技術分野〕
本発明は高密度の炭化ケイ素焼結体の製造方法に関する
。DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to a method for manufacturing a high-density silicon carbide sintered body.
炭化ケイ素焼結体は、例えばガスタービン部品。 Silicon carbide sintered bodies are used, for example, in gas turbine parts.
高温用熱交換器のような高温構造材料として礪め率、優
れた耐酸化性と耐食性、高い熱衝撃性及び常温と高温度
特性を挙げることができる。As a high-temperature structural material such as a high-temperature heat exchanger, it can be cited for its shrinkage rate, excellent oxidation resistance and corrosion resistance, high thermal shock resistance, and room temperature and high temperature characteristics.
しかしながら炭化ケイ素焼結体の出発原材である８１Ｃ
粉末は焼結し難い材料であるため、これまで高密度の焼
結体を得よりとする際には、７７ｇ圧焼結法が採用され
ていた。しかしながら前記力ロ圧焼結法によれば複雑な
形状の焼結体を製造することが難かしぐ、また生産性も
挙がらないと云う欠点があった・
前記加圧焼結法の有する欠点を除去、改善するため、在
来種々の提案がなされており、なかでも特開昭５０−７
８６０９号「高密度炭化珪素セラミックの製造方法」１
次に特開昭５２−６７ｉ６号「炭化ケイ素焼結体」に炭
化ケイ素、ホウ素含有添加剤及び炭素質添加剤からなる
サブミクロン粒度の粉末を成形し、不活性雰囲気中の約
１９５０〜２３００℃で無加圧焼結する方法が開示され
ている。However, 81C, which is the starting material for silicon carbide sintered bodies,
Since powder is a material that is difficult to sinter, a 77g pressure sintering method has been used to obtain a high-density sintered body. However, according to the force-pressure sintering method, it is difficult to produce sintered bodies with complicated shapes, and the productivity is low. , various proposals have been made in order to improve the
No. 8609 “Method for manufacturing high-density silicon carbide ceramic” 1
Next, submicron particle size powder consisting of silicon carbide, a boron-containing additive, and a carbonaceous additive is molded into JP-A No. 52-67i6 "silicon carbide sintered body" and heated to about 1950 to 2300°C in an inert atmosphere. A method of pressureless sintering is disclosed.
ところで、炭化ケイ素粉粒子は一般に酸化膜で被覆され
ておシ、前記無加圧焼結方法によれば。By the way, silicon carbide powder particles are generally coated with an oxide film, according to the pressureless sintering method.
前記酸化膜を還元除去して炭化ケイ素粉末粒子間の焼結
性を高めるため炭素を添加する必要がちる。It is necessary to add carbon to reduce and remove the oxide film and improve the sinterability between silicon carbide powder particles.
しかして、前記無加圧焼結法によれば、炭化ケイ素の重
量に対し０．１〜ｌ、Ｑ Ｗ ／ Ｏの炭素が使用され
面積を有する炭化ケイ累粉末粒子の全表面を完全に被覆
するには至らない。これを改善するために一般には有機
化合物溶液をもって炭化ケイ素粉末に均一に分散させた
後、不活性雰囲気中で加熱して有機化合物から析出する
炭素によって炭化ケイ累の表面を被覆している前記酸化
膜を還元して除去する方法が提案されているが、この方
法によってもなお析出した炭素粒子は炭化ケイ素粉末粒
子の表面で局部的に分散された状態となり、酸化膜は局
部的にしか還元除去されない。更に加熱処理後の成形体
（脱脂成形体）は一般に大気中で黒鉛製匣鉢に納められ
、焼成炉内に設置され真空又は不活性雰囲気中で焼結さ
れるが、大気にさらされ九時に下記の反応式により容易
ｌこ
ｓ ｉ Ｃ＋Ｏ，→ ＳｉＣ＋ ＣＯ↑再酸化されてし
ま５゜
そのため、焼結時には部分的Ｅこ炭化ケイ素が露出され
るにすぎず、残された酸化膜は炭化ケイ累粉末粒子間で
起きるネック生長を妨害し、かつ焼結体内で介在物と成
り、焼結の進行を場所的に不均一化して、異常粒成長を
助長するため、全体として焼結性を低下させる。According to the pressureless sintering method, carbon is used in an amount of 0.1 to 1, Q W / O based on the weight of silicon carbide, and the entire surface of the silicon carbide powder particles having an area is completely covered. It's not enough to do that. To improve this, generally an organic compound solution is uniformly dispersed in silicon carbide powder and then heated in an inert atmosphere to coat the surface of the silicon carbide with carbon precipitated from the organic compound. A method has been proposed to remove the film by reducing it, but even with this method, the precipitated carbon particles remain locally dispersed on the surface of the silicon carbide powder particles, and the oxide film can only be reduced and removed locally. Not done. Furthermore, the molded body after heat treatment (degreased molded body) is generally placed in a graphite sagger in the atmosphere, placed in a firing furnace, and sintered in a vacuum or inert atmosphere, but when exposed to the atmosphere, According to the reaction equation below, it is easily re-oxidized. Therefore, during sintering, only a portion of silicon carbide is exposed, and the remaining oxide film is silicon carbide. It obstructs neck growth that occurs between powder particles, and becomes inclusions within the sintered body, making the progress of sintering uneven locally and promoting abnormal grain growth, resulting in a decrease in sinterability as a whole. let
したがりて、従来ＳｉＣ粉末を無加圧ｖ８結するために
は、２１００″Ｃ前後の高温焼成が行なわれ、また、約
０．５μｍ以下の非常に入手し難く、かつ高価なＳｉＣ
超微粉末が必要とされている。Therefore, conventionally, in order to bond SiC powder without pressure, high-temperature firing of around 2100''C is performed, and SiC powder with a diameter of about 0.5 μm or less is very difficult to obtain and expensive.
Ultrafine powder is required.
本発明は前記欠点を除去・改善するち密なＳｉＣ焼結体
の製造方法を提供することを目的とする。An object of the present invention is to provide a method for manufacturing a dense SiC sintered body that eliminates and improves the above-mentioned drawbacks.
焼結時における焼結速度の局所的バラツキ、異常粒成長
及びスケルトン構造の発生原因が、微細なＳｉＣ粉末に
不可避な表面酸化膜を除去して清浄ｆｉｓｉｃ粉末表面
を実現した状態で焼結を進行させ得なかつ九ために生じ
たことを見出し、真空昇温過程で生ずる炭素による酸化
皮＠還元反応が終了するのを真空計等で確認した後、初
めて焼結が始まる高温域へ昇温させるよう制御したち密
ＳｉＣ焼結体を製造する方法である。The causes of local variations in sintering speed, abnormal grain growth, and skeleton structure during sintering are eliminated by removing the inevitable surface oxide film on fine SiC powder and proceeding with sintering to achieve a clean fisic powder surface. After confirming with a vacuum gauge, etc., that the oxidized skin @ reduction reaction due to carbon generated during the vacuum heating process has finished, we decided to raise the temperature to a high temperature range where sintering only begins. This is a method for manufacturing a controlled dense SiC sintered body.
次に本発明を以下詳細に説明する。The present invention will now be described in detail.
本発明によれば出発原料である８ｉＣ粉末は平均粒径が
１μｍ以下又は比表面積が５ ｍ” ７１１以上である
ことが望まれる。According to the present invention, it is desired that the starting material 8iC powder has an average particle size of 1 μm or less or a specific surface area of 5 m''711 or more.
その理由は、それより大きい粒度のものを用いふＯ
ると、焼結体の密度が約’ｃｒｆ’ｔｔ ／ ｃ ｃ以
上で、かつ均一な焼結粒径とすることが困難であるから
である。前記ＳＩＣの結晶系はα型及びβ型の二種に分
別されるが、その何れか、及びそれらの混合物も使用で
きる。前記の如きＳｉＣ粉末は各種の方法で製造できる
が、得られたままのＳｉＣ粉末には焼と
結性を阻害し、かつ焼結体内の欠陥Ｙなる遊離炭素、遊
離シリカ及び遊離シリコン等々各種不純物されている。The reason for this is that if a larger particle size is used, the density of the sintered body will be approximately 'crf'tt/cc or more, and it will be difficult to obtain a uniform sintered particle size. be. The crystal system of SIC is classified into two types, α type and β type, and either type or a mixture thereof can be used. The SiC powder as described above can be produced by various methods, but the as-obtained SiC powder contains various impurities such as free carbon, free silica, and free silicon, which inhibit sintering and sinterability and form defects Y in the sintered body. has been done.
しかし、その後の大気中酸素によるＳｉＣ粉末表面の酸
化は通学道けられない。我々は比表面積の異なる各櫨Ｓ
ｉＣ粉末中の言有液素量を比較検討し、表の結果を得た
。８ｉＣ粉末表面に酸化皮膜を形成する酸素原子間距離
の平均値は１．６〜３．２ Ａ ＯＪ間にある。これは
酸化皮膜は２原子層未満であることを意味している。However, the subsequent oxidation of the SiC powder surface due to atmospheric oxygen makes it impossible to walk to school. We have each oak S with different specific surface area.
The stated amount of liquid element in the iC powder was compared and the results shown in the table were obtained. The average value of the distance between oxygen atoms that forms an oxide film on the surface of the 8iC powder is between 1.6 and 3.2 A OJ. This means that the oxide film is less than two atomic layers.
これ以上の＠厚及び酸素含有赦は、綿化不充分によるＳ
ｉＯ２相及びｓｉｏ、粉末の混在又は金ｐＡ酸化物の残
留によυ生じ得るもので、本発明における対象出発原料
には不適である。Thickness and oxygen content greater than this are due to insufficient cottonization.
This may occur due to the presence of the iO2 phase, sio, powder, or residual gold pA oxide, and is therefore unsuitable as the target starting material for the present invention.
本発明に係る脱脂成形体はＳｉＣ粉末と焼結助剤からな
るが、焼結助剤としてはＢ及びその化合物のように、高
温でＳＩＣ粒子内に拡散して空孔を増加させることによ
り、焼結性を向上させる元素を添加し得る０本発明ζこ
於いては、少なくとも焼結助剤としてＳＩＣ粉末表面の
酸化皮膜を除去するための炭素が脱脂成形体に含まれて
いなければならない、さらｊここの炭素はＳｉＣ表面に
均一に分散していることが好ましく、そのためには無定
形炭素でもよいが、更にはフェノール樹脂等非酸化性雰
凹気中で加熱処理により −６分解し炭素が残留す
るものが優も好ましい。この過剰ＣはＳｉＣ粉末粒子表
面の酸素を次式によりて還元除去するためであフ（Ｓ
ｉ Ｃ＋２０−４８ ｉ Ｃ＋Ｃｏ↑）その適正量はＳ
ｉＣ中の酸化皮膜珪に依存し、冥用土は。The degreased molded body according to the present invention is made of SiC powder and a sintering aid, and the sintering aid, like B and its compounds, diffuses into the SIC particles at high temperatures and increases the number of pores. In the present invention, an element that improves sinterability may be added. In this case, the degreased compact must contain at least carbon as a sintering aid for removing the oxide film on the surface of the SIC powder. Furthermore, it is preferable that the carbon here be uniformly dispersed on the SiC surface, and for that purpose, amorphous carbon may be used, but it is also possible to decompose the carbon by -6 decomposition by heat treatment in a non-oxidizing atmosphere such as phenol resin. It is also preferable to have a good residual amount. This excess C is because the oxygen on the surface of the SiC powder particles is reduced and removed by the following formula (S
i C+20-48 i C+Co↑) The appropriate amount is S
Depends on the silicon oxide film in iC, and the soil is.
含有酸累貫貨の１．０〜３． Ｑ、 ＠が適正値である
。Contains acid cumulative amount of 1.0 to 3. Q and @ are appropriate values.
１．０倍未満では全ｔＲ素の還元ができない。また。If it is less than 1.0 times, all tR elements cannot be reduced. Also.
３、０倍以上では全酸素の還元が終了した後にも過剰Ｃ
が残留し焼結の障害となる。3. At 0 times or more, excess C remains even after all oxygen has been reduced.
remains and becomes an obstacle to sintering.
成形体の脱脂は不活性雰囲気中でゆるやかに昇温するこ
とによフ、約１０００℃以下でのガス放出が無くなるま
で充分になされることが望ましい。It is desirable that the molded body be degreased sufficiently by slowly raising the temperature in an inert atmosphere until no gas is released at temperatures below about 1000°C.
ＣｂＡＴ−糸切
以上の様にして製作した脱脂済成形体の主要成分は８４
Ｃ＠末粒子、その表面を覆う酸化皮膜及び焼結助剤とし
ての非晶質炭素及びホウ素等々となる。従って焼結は余
計な不純物等の蒸発連敗を図るため真空で昇温させるの
が好ましい。この昇温時に我々は、１３５０℃〜１５５
０℃の範囲で真空度が急激に低下する現象を発見した。CbAT - The main components of the degreased molded body produced by thread cutting and above are 84
C@ powder particles, an oxide film covering the surface thereof, and amorphous carbon and boron as sintering aids. Therefore, during sintering, it is preferable to raise the temperature in a vacuum to prevent unnecessary evaporation of impurities. At this temperature increase, we
We discovered a phenomenon in which the degree of vacuum decreases rapidly in the 0°C range.
その様子は図に示す様に昇温速度及び脱脂成形体の厚さ
に依存することも判明した。これは成形体よりのガス放
出によるものであり、その詳細を明らかにするため、我
々は各種８ｉＣ粉末について実験を行い表の如き結果を
得た。As shown in the figure, it was also found that the behavior depended on the temperature increase rate and the thickness of the degreased molded body. This is due to gas release from the compact, and in order to clarify the details, we conducted experiments on various 8iC powders and obtained the results shown in the table.
重量減少二ガス放出量
ガス放出量はＳｉＣ原料粉末に２ける含有酸素量の１．
６〜２．５倍の重量に相当している。Weight reduction 2 Gas release amount The gas release amount is 1.2% of the amount of oxygen contained in the SiC raw powder.
This corresponds to 6 to 2.5 times the weight.
我々は８ｉＣ粉末表面に於て次式の様な還元反応が進行
していると推定した。We inferred that a reduction reaction as shown in the following equation is proceeding on the surface of the 8iC powder.
■ ｓｉｏ＋ｚｃ→、 Ｓ ｉｃ＋ｃｏ↑■ ＳｉＯ
−＋ ＳｉＯ↑
ＳｉＣ粉末表面に物理的又は化学的に吸着された酸素は
皮膜を形成し、ｓｉｃ粒子間の直接接触を妨げ、粒界拡
散を抑制するので完全に除去することが望ましい、しか
るに昇温速度が速いと酸化皮膜が部分的に除去され未だ
還元反応が進行中で、ガス放出中の状態で高温に達して
、焼結が始まりてしまり、するとＳｉＣ粉末表面でも清
浄な部分では焼結反応が速く進むが、酸化皮膜が残留し
ている部分では焼結反応速度が抑制される。このため焼
結反応の進行が場所的に不均一となシ異常粒成長及び柱
状−板状粒成長を誘起し、スケルトン構造が形成されち
密化が進まなくなることを確認した。■ sio+zc→, S ic+co↑■ SiO
-+ SiO↑ Oxygen physically or chemically adsorbed on the SiC powder surface forms a film that prevents direct contact between SIC particles and suppresses grain boundary diffusion, so it is desirable to completely remove it. If the heating rate is high, the oxide film is partially removed and the reduction reaction is still in progress, and the high temperature is reached while gas is being released and sintering begins. Although the reaction proceeds quickly, the sintering reaction rate is suppressed in areas where the oxide film remains. For this reason, it was confirmed that the progress of the sintering reaction was locally non-uniform, inducing abnormal grain growth and columnar-plate grain growth, forming a skeleton structure and preventing densification from proceeding.
我々は昇温中に真空度を監視し、 １３５０℃〜１５
５０℃周辺のガス放出によシ真空度が低下する領域を緩
やかに昇温させ、大麗部材であるため中心部からのガス
放出に時間を要する成形体では更に約１５５０℃付近で
温度を保持させることにより、ガス放出による真空度の
低下が完全に回復する迄待りた・
この様にしてＳｉＣ粉末粒子表面の酸化皮襖を完全に除
去し、清浄面にし念状態で、 １８００℃〜２２００揮
散が発生するので、真空よりもＡｒ等の不活性雰囲気を
導入する方がより好ましい。We monitor the degree of vacuum during temperature rise, from 1350℃ to 15
The temperature is gradually increased in the area where the degree of vacuum decreases due to gas release around 50°C, and the temperature is further maintained at around 1550°C in the molded product, which takes time to release gas from the center because it is a Dairei member. The oxidized skin on the surface of the SiC powder particles was completely removed in this way, and the vacuum was heated to 1800°C to 2200°C while keeping the surface clean. Since volatilization occurs, it is more preferable to introduce an inert atmosphere such as Ar than a vacuum.
本発明の好ましい態様をまとめれば以下の如くになる。Preferred embodiments of the present invention can be summarized as follows.
■ＳＩＣ原料粉として平均粒径１μｍ以下、比表面積５
ｍχ／Ｉ以上のものを用いる。■As SIC raw material powder, average particle size is 1μm or less, specific surface area is 5
Use one having mχ/I or more.
■脱脂を非酸化性雰囲気中で１０００℃以下の温度で行
なう、（ガス放出がなくなるまでン■１３５０〜１５５
０℃の温度で脱脂済のＳｔＣ成形体を保持する。この時
、 酸化皮部の除去の判定をｃｏ、ｃ
ｏ、等の放出による真空度■焼結（１８００〜２２００
℃２ 時にＡｒ、Ｈｅ、Ｎｅ。■ Degreasing is carried out in a non-oxidizing atmosphere at a temperature below 1000℃ (keep until no gas is released ■1350~155℃)
The degreased StC molded body is held at a temperature of 0°C. At this time, the removal of the oxidized skin part is judged as co, c.
Vacuum degree due to release of o, etc.■ Sintering (1800-2200
Ar, He, Ne at 2°C.
ＣＯ等の非酸化性ガス、不活性ガスを導入する。Introduce a non-oxidizing gas such as CO or an inert gas.
出発原料として比表面′！ｊＩ１５ｍ”／ｊｌ、全酸素
含有量１．Ｑｗｌｏ 、その他不純物は全てＱ、 ｌ
ｗ ／ ｏ未満であるα型８ｉＣ粉末を選び、非晶質Ｂ
（０，３Ｗ１０ ）とＣ源となるノボラック樹脂（３
，５ｗ１０）を加え。Specific surface as a starting material! jI15m"/jl, total oxygen content 1.Qwlo, all other impurities are Q, l
Select α-type 8iC powder that is less than w/o, amorphous B
(0,3W10) and novolac resin (3
, 5w10) was added.
アセトンを分散媒にして湿式混合後、乾燥造粒し九＊
４３．５Ｘ３３．５ｍｍ” の金型を使い、造粒粉よ
り２０ｊｌ／Ｐ及び６０ｇ／Ｐの試料を多数、加圧成形
（１ｔｏｎ ／ｃ♂）した、これら試料を窒素雰囲気中
で７００℃まで８時間をかけて加熱することにより、脱
脂済成形体を得た。この成形体を黒鉛匣鉢に入れて焼成
炉に納めた。ＲＴ（室温ンよシ約１３５０℃までは手動
で通電加熱した。１３５０℃〜１５５０″Ｃ同辺では顕
著なガス放出が認められた。この付近における昇温速度
（ｄＴ／ｄｔ）と真空度の変化は図の如くであり、昇温
速度が遅いと１４００℃の近傍に鋭いガス放出ピークが
現れるが昇温速度が速くなるとガス放出ピークは高温＊
＃ｃ遷移し、低く幅広くなりた。また６０Ｊｌ／Ｐよシ
も２ＯＮ／Ｐの試料の方がガス放出ピークは鋭い形状と
なった。尚１通常のＤＴＡ 、ＴＧＡでの解析を試みた
が、検出感圧が不足して評価できなかった。After wet mixing using acetone as a dispersion medium, dry granulation is performed.
Using a mold of 43.5 x 33.5 mm, many samples of 20 jl/P and 60 g/P were pressure-molded (1 ton/c♂) from granulated powder. These samples were heated to 700°C in a nitrogen atmosphere for 8 hours. By heating over a period of time, a degreased molded body was obtained. This molded body was placed in a graphite sagger and placed in a firing furnace. It was manually heated with electricity from room temperature to about 1350°C. Significant gas release was observed in the vicinity of 1350°C to 1550"C. The temperature increase rate (dT/dt) and degree of vacuum change in this area are as shown in the figure. A sharp gas release peak appears in the vicinity, but as the heating rate increases, the gas release peak becomes higher temperature *
It transitioned to #c and became low and wide. In addition, the gas release peak of the 2ON/P sample had a sharper shape than the 60Jl/P sample. Note: 1. Analysis using conventional DTA and TGA was attempted, but the detection pressure sensitivity was insufficient and evaluation could not be performed.
室温から焼結温度（２１００″Ｃ）までの昇温過程を攬
々変化させて実験した結果を表に示す。The table shows the results of experiments in which the heating process from room temperature to the sintering temperature (2100''C) was varied frequently.
（ｐ人ト乍白）
参考例 １ ７ｍｍ（２（Ｗ／ｐ）２０分Ａｒ ２０
００”Ｃ／ＨＡｒ ０ｆ−Ｔ Ａｒ実施例
１ 、ｖ ｖ
、 ｖ＃２０．５’Ｉ（）ｔ
ｌ ３ 〃 、 〃 −１０伝良
７Ｈ〃ｏｌ−１〃〃４
０．５Ｈ−−５〃〃
’５００℃、４（〃 ｏＨ＃−６０，５Ｈ〃
＃ ７ 〃 〃 ２５σ嘔
〃 ＯＨ＃、 ８
０．５Ｈ＃
〃 ９
〃１０
参考例°２ ２１ｍｒ＋（６０Ｉ！／ｐ） ３０分Ａｒ
２０００’（ン＋Ｉ Ａｒ ＯＨＡｒ
＃ ３ 〃 ｖ
ｖ ＃ ■、 ４
０．５Ｈ＃〃５ 〃−１００
０’Ｃ／ｉ（＃ＯＨ。(p person to white) Reference example 1 7mm (2 (W/p) 20 minutes Ar 20
00”C/HAr 0f-T Ar example
1, v v
, v#20.5'I()t l 3 〃 , 〃 -10Denryo7H〃ol-1〃〃4
0.5H--5〃
'500℃, 4 (〃 oH#-60,5H〃 #7 〃 〃 25σ 〃 OH#, 8
0.5H#
〃 9 〃10 Reference example °2 21mr+(60I!/p) 30 minutes Ar
2000'(n+I Ar OHAr
#3〃v
v # ■, 4
0.5H#〃5〃-100
0'C/i (#OH.
〃６
ｏ、５１（＃実施例 １１
〃＃５００”Ｃ／Ｈ〃ＯＨ＃〜 １２
ｏ、ｓ）（＃″ １３
〃 〃 ２５ｏ″ｃ／Ｈ＃ ＯＨ＃”
１４
０．５Ｈ’２０００℃／ＨＡｒ
０．５ＨＡｒ ２．８９Ｖ
＃ Ｖ ３．０２３．
０７
３．０８
３．１１
３．１６
３．１７
３．１７
３．１８
＃Ａｒ ３．１８
Ａｒ ３
．１８２００ｆｆＣ／ＨＡｒ Ｏ，５ＨＡｒ
２．８１Ｖ
Ｖ ２．８８２．９３
２．９５
２．９６
３．００
３．０４
３．１５
３．１８
＃Ａｒ ３．１７
Ａｒ
３．１７〔発明の効果〕
以上説明したように本発明によれば、ち密で良好なＳｉ
Ｃ焼結体８得ることができる。〃6
o, 51 (#Example 11
〃#500”C/H〃OH#~12
o, s) (#″ 13
〃 〃 25o″c/H# OH#”
14
0.5H'2000℃/HAr
0.5HAr 2.89V
#V 3.023.
07 3.08 3.11 3.16 3.17 3.17 3.18 #Ar 3.18 Ar 3
．． 18200ffC/HAr O,5HAr
2.81V
V 2.882.93 2.95 2.96 3.00 3.04 3.15 3.18 #Ar 3.17 Ar
3.17 [Effects of the Invention] As explained above, according to the present invention, dense and good Si
A C sintered body 8 can be obtained.
第１図は温度−真空度特性図。
代理人 弁理士 則 近 ｗｌ 佑同 竹
花 喜久男
真
空
曳
一嫉じＣ）
第１図Figure 1 is a temperature-vacuum characteristic diagram. Agent Patent Attorney Nori Chika wl Yudo Take Hana Kikuo Shinku Hikiichi Jealousy C) Figure 1
Claims (2)
粉末表面を覆う酸化皮膜の全てが還元除去されるまで焼
結開始温度未満の温度にＳｉＣ粉末成形体を保持し、そ
の後焼結開始温度以上に昇温することを特徴とする炭化
ケイ素焼結体の製造方法。(1) In the temperature raising process of sintering the SiC powder compact, the SiC
A silicon carbide sintered body, characterized in that the SiC powder compact is maintained at a temperature below the sintering start temperature until all of the oxide film covering the powder surface is reduced and removed, and then the temperature is raised above the sintering start temperature. manufacturing method.
あることを特徴とした特許請求の範囲第１項記載の炭化
ケイ素焼結体の製造方法。(2) The method for manufacturing a silicon carbide sintered body according to claim 1, wherein the holding temperature is in a range of 1350°C to 1550°C.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60195750A JPS6256371A (en) | 1985-09-06 | 1985-09-06 | Manufacture of silicon carbide sintered body |
| US06/903,141 US4853299A (en) | 1985-09-06 | 1986-09-03 | Silicon carbide sintered body and method of manufacturing the same |
| DE19863630369 DE3630369A1 (en) | 1985-09-06 | 1986-09-05 | SILICON CARBIDE SINTER BODY AND METHOD FOR THE PRODUCTION THEREOF |
| DE3645097A DE3645097C2 (en) | 1985-09-06 | 1986-09-05 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60195750A JPS6256371A (en) | 1985-09-06 | 1985-09-06 | Manufacture of silicon carbide sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6256371A true JPS6256371A (en) | 1987-03-12 |
Family
ID=16346342
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60195750A Pending JPS6256371A (en) | 1985-09-06 | 1985-09-06 | Manufacture of silicon carbide sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6256371A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63236764A (en) * | 1987-03-24 | 1988-10-03 | 三菱マテリアル株式会社 | Manufacture of silicon carbide sintered body |
| JPH02199065A (en) * | 1989-01-30 | 1990-08-07 | Kazumichi Kijima | Sintered silicon carbide having high thermal conductivity and production thereof |
| JPH02199066A (en) * | 1989-01-30 | 1990-08-07 | Kazumichi Kijima | Sintered silicon carbide having electrical conductivity and production thereof |
| JP2016540717A (en) * | 2013-10-30 | 2016-12-28 | ゼネラル・エレクトリック・カンパニイ | Method for repairing matrix cracks in infiltrated ceramic matrix composites. |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56169181A (en) * | 1980-05-30 | 1981-12-25 | Ibigawa Electric Ind Co Ltd | Manufacture of high strength silicon carbide sintered body |
| JPS5732035A (en) * | 1980-08-05 | 1982-02-20 | Toyota Motor Corp | Intake air quantity control method for internal combustion engine |
| JPS57166372A (en) * | 1981-04-02 | 1982-10-13 | Sumitomo Electric Industries | Manufacture of non-oxide ceramics |
| JPS59184769A (en) * | 1983-04-04 | 1984-10-20 | 日立化成工業株式会社 | Manufacture of high density silicon carbide sintered body |
| JPS605071A (en) * | 1983-06-21 | 1985-01-11 | イビデン株式会社 | Manufacture of silicon carbide sintered body |
| JPS6065765A (en) * | 1983-09-21 | 1985-04-15 | 科学技術庁無機材質研究所長 | Process for sintering cubic silicon carbide powder |
| JPS60186467A (en) * | 1984-03-01 | 1985-09-21 | イビデン株式会社 | Silicon carbide sintered body and manufacture |
| JPS6131356A (en) * | 1984-07-20 | 1986-02-13 | 松下電器産業株式会社 | Manufacture of sic sintered body |
| JPS61168567A (en) * | 1985-01-19 | 1986-07-30 | イビデン株式会社 | Manufacture of silicon carbide sintered body |
| JPS6153166B2 (en) * | 1982-03-16 | 1986-11-17 | Ishikawajimaharima Jukogyo Kk |
-
1985
- 1985-09-06 JP JP60195750A patent/JPS6256371A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56169181A (en) * | 1980-05-30 | 1981-12-25 | Ibigawa Electric Ind Co Ltd | Manufacture of high strength silicon carbide sintered body |
| JPS5732035A (en) * | 1980-08-05 | 1982-02-20 | Toyota Motor Corp | Intake air quantity control method for internal combustion engine |
| JPS57166372A (en) * | 1981-04-02 | 1982-10-13 | Sumitomo Electric Industries | Manufacture of non-oxide ceramics |
| JPS6153166B2 (en) * | 1982-03-16 | 1986-11-17 | Ishikawajimaharima Jukogyo Kk | |
| JPS59184769A (en) * | 1983-04-04 | 1984-10-20 | 日立化成工業株式会社 | Manufacture of high density silicon carbide sintered body |
| JPS605071A (en) * | 1983-06-21 | 1985-01-11 | イビデン株式会社 | Manufacture of silicon carbide sintered body |
| JPS6065765A (en) * | 1983-09-21 | 1985-04-15 | 科学技術庁無機材質研究所長 | Process for sintering cubic silicon carbide powder |
| JPS60186467A (en) * | 1984-03-01 | 1985-09-21 | イビデン株式会社 | Silicon carbide sintered body and manufacture |
| JPS6131356A (en) * | 1984-07-20 | 1986-02-13 | 松下電器産業株式会社 | Manufacture of sic sintered body |
| JPS61168567A (en) * | 1985-01-19 | 1986-07-30 | イビデン株式会社 | Manufacture of silicon carbide sintered body |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63236764A (en) * | 1987-03-24 | 1988-10-03 | 三菱マテリアル株式会社 | Manufacture of silicon carbide sintered body |
| JPH0451511B2 (en) * | 1987-03-24 | 1992-08-19 | Mitsubishi Materials Corp | |
| JPH02199065A (en) * | 1989-01-30 | 1990-08-07 | Kazumichi Kijima | Sintered silicon carbide having high thermal conductivity and production thereof |
| JPH02199066A (en) * | 1989-01-30 | 1990-08-07 | Kazumichi Kijima | Sintered silicon carbide having electrical conductivity and production thereof |
| JP2016540717A (en) * | 2013-10-30 | 2016-12-28 | ゼネラル・エレクトリック・カンパニイ | Method for repairing matrix cracks in infiltrated ceramic matrix composites. |
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