JPH01119568A - 加圧自己燃焼焼結法 - Google Patents

加圧自己燃焼焼結法

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Publication number
JPH01119568A
JPH01119568A JP62277150A JP27715087A JPH01119568A JP H01119568 A JPH01119568 A JP H01119568A JP 62277150 A JP62277150 A JP 62277150A JP 27715087 A JP27715087 A JP 27715087A JP H01119568 A JPH01119568 A JP H01119568A
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JP
Japan
Prior art keywords
mixture
self
sintering method
vessel
hip
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.)
Granted
Application number
JP62277150A
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English (en)
Other versions
JPH0515669B2 (ja
Inventor
Yoshio Miyamoto
欽生 宮本
Hirohiko Nakada
博彦 仲田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Osaka University NUC
Sumitomo Electric Industries Ltd
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Osaka University NUC
Sumitomo Electric Industries Ltd
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Application filed by Osaka University NUC, Sumitomo Electric Industries Ltd filed Critical Osaka University NUC
Priority to JP62277150A priority Critical patent/JPH01119568A/ja
Priority to US07/263,245 priority patent/US4999144A/en
Priority to DE8888310147T priority patent/DE3879619T2/de
Priority to EP88310147A priority patent/EP0314492B1/en
Publication of JPH01119568A publication Critical patent/JPH01119568A/ja
Publication of JPH0515669B2 publication Critical patent/JPH0515669B2/ja
Granted legal-status Critical Current

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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。

Description

【発明の詳細な説明】 イ、産業上の利用分野 本発明はセラミックス焼結体を容易に得る方法に関する
。
口、従来の技術 セラミックス焼結体を容易に得る方法として特開昭６０
−２４６２７０号公報に開示されているように、金属元
素と非金属元素との混合物からセラミックスを合成する
際、発生する反応熱を利用しセラミックスを合成すると
同時に焼結する自己燃焼焼結法がある。特に特開昭６０
−２４６２７０号では、熱間静水圧プレス（以下ＨＩＰ
と称する）を用いて加圧下にて行なういわゆる加圧自己
燃焼焼結法が好ましいとされている。
ハ９発明が解決しようとする問題点 加圧自己燃焼焼結法によってセラミックスを焼結するに
は、金属元素と非金属元素の混合物を気密容器内に挿入
した後、該気密容器内に設置した反応開始用の熱源に気
密容器外部からエネルギーを与えることによって熱源を
加熱し金属元素と非金属元素の混合物の一端からセラミ
ックスの合成反応を開始させその反応熱によって連鎖的
にセラミックスの合成焼結を行なう。
熱源として一般にはＷ、Ｍｏなどのフィラメントを用い
る。しかし加圧自己燃焼焼結法における加圧手段として
も最も一般的なＨＩＰを用いるために、金属元素と非金
属元素の混合物に静水圧をかけるため、気密容器内に該
金属元素と非金属元素の混合物を挿入することが不可欠
である。従ってこの気密容器内にＷ、Ｍｏなどのフィラ
メントを設置しかつ気密容器の外部にＷ、Ｍｏなどのフ
ィラメントの給電用のリード線を気密を保ったまま引き
出す必要がある。気密容器に用いる材料としては、ガラ
ス・石英・白金管などが一般に推奨されている。
これらの気密容器Ｗ、Ｍｏなどのフィラメントを気密を
保ったまま外部にリード線を引き出しながら設置するの
は工業的にはきわめて困難なことであり、加圧自己燃焼
焼結法が工業的に未だ実用化していない大きな原因の一
つといわれている。
二１発明の構成 （ａ）問題点を解決するための手段 本説明は、加圧自己燃焼焼結法によって、金属元素と非
金属元素の混合物からセラミックスを合成する際に発生
する反応熱を利用してセラミックスを合成焼結を行なう
にあたり、その合成反応の開始用の熱源として、金属元
素と非金属元素の混合物を挿入した気、密容器の外部に
配置した、金属元素と非金属元素の混合物の一端を加熱
し、連鎖的に反応を進行させるいわゆる自己燃焼反応を
おこさせ、その際に発生する反応熱によって気密容器内
部の金属元素と非金属元素の混合物を瞬間的に加熱し、
該金属元素と非金属元素の混合物からセラミックスを合
成する反応を開始させ、その反応熱によって、連鎖的に
セラミックスの合成と焼結を行なうものである。
（ｂ）作用 上記のように本発明では、加圧自己燃焼焼結法の反応開
始に用いる熱源として、金属元素と非金属元素の混合物
を挿入した気密容器の外部に配置した、金属元素と非金
属元素の混合物の、自己燃焼反応を用いるものである。
従って、従来技術のように、ガラスや石英製の気密容器
の内部に、気密を保ったままで、外部にリード線を出し
ながら、ＷやＭｏのフィラメントを設置する必要がない
ことはいうまでもない。また気密容器の外部に配置した
金属元素と非金属元素の混合物の自己燃焼反応を開始さ
せるための、加熱方法は、この外部配置金属元素と非金
属元素の混合物は、焼結する必要がない、即ち加圧する
必要がないため、気密容器内に、気密をたもったままで
フィラメントを設置　。
するような工業的にきわめて困難な加熱源を必要とせず
、簡単なフィラメント等で、直接加熱するだけでよい。
なお本発明は、目的とする化合物の生成反応熱を利用し
て、該化合物を合成焼結する方法であるため、出発原料
としては、十分な反応熱が生じるものであればよいこと
はいうまでもない。特に好ましいのは金属元素と非金属
元素の混合物から、セラミックスを合成焼結することで
あり、その中でも金属元素として周期律表ｍａ、　ＩＶ
ａ　、　Ｖａ　、　ＶＩａ族金属の１種以上、非金属元
素としてＢＳＣ，Ｎ。
Ｓｉの１種以上であると十分な生成反応熱かえられるた
め好ましい。また加圧方法としては、ホットプレスのよ
うな一軸加圧でもよいが、工業的には、熱間静水圧プレ
ス（ＨＩＰ）が好ましい。
実施例１ 市販の、Ｔｉ粉末を！ｉ５．６２ｇ、　Ｂ粉末を１０．
８１ｇをボールミルにて十分に混合した後、プレスにて
加圧成型したのち、パイレックスガラス製の容器に真空
封入した。この試料をＣ製の容器内に設置し該パイレッ
クスガラス製の容器の周囲にＴｉとＣの粉末を等モル混
ぜた混合粉末でおおった。このＣ製の容器をＨＩＰ内に
設置したのち、まずＨＩＰ内を真空に排気した後、ＨＩ
Ｐ内を８５０℃まで加熱した後、ＨＩＰ内にＡｒガスを
３００気圧まで導入した。ここでＣ製の容器内のＴｉと
Ｃの粉末内にあらかじめ用意してあったＷフィラメント
にＨ１Ｐ外部から通電加熱することによって、ＴｉとＢ
との加圧自己燃焼焼結をおこなった。
得られた焼結体はＴｉＢ　２−１０ｗｔ％Ｔｉの組成を
有する理論密度の約９９．８％の焼結体であった。従来
の技術にしたがうと、ＴｉとＢとの混合粉末の圧粉体を
パイレクスガラス製の容器に真空封入する際にＷフィラ
メントを該真空容器にいわゆるハーメチックシール（ガ
ラスと金属とを真空を保ったまま接合することをいう）
によって装着する必要があり、工業的にはきわめて歩留
まりが悪く、例えば１００回テストを行なったところ、
９２回しか成功しなっかった。−力木発明によれば、ハ
ーメチックシールのような工業的に歩留まりの悪い工程
をまったく必要としないため１００回テストを行なった
ところ１００回とも成功した。
実施例２ 市販のＳｉ粉末２８ｇとＣ粉末１２ｇとを十分に混合し
た後加圧成型を行ない圧粉体を作成した。この圧粉体を
白金部の真空容器に真空封入したのち、周囲をＴ１とＣ
の粉末を等モル混ぜた混合粉末にてかこったのちＣ製の
容器内に設置した。このＣ製容器をＨＩＰにいれ、ＨＩ
Ｐ内を１０００℃に加熱した後Ａｒガスを導入しＨＩＰ
内を４５０気圧まで加圧した。
しかるのちＣ製の容器内のＴｉとＣの粉末内にあらかじ
め用意してあったＷフィラメントにＨＩＰ外部から通電
加熱することによって、加圧自己燃焼焼結を行なった。
その結果理論密度９９，９％のＳｉＣの焼結体かえられ
た。
実施例３ 市販のアナターゼ型結晶構造を有するＴ１０２２４０ｇ
、Ａ１粉末１０８ｇ、　Ｃ粉末３６ｇとを十分に混合し
たのち加圧成型を行なった。
この圧粉体を、パイレックスガラス製の容器に真空封入
したのち、Ｃ製の反応容器内に設置し、該パイレックス
ガラス容器の周囲にＴｉとＢの粉末を１：２モルの比率
で混ぜた混合粉末でおおった。
このＣ製容器をＨＩＰ内に設置したのち、８８０℃まで
加熱し、后ガスを４５０気圧まで導入した。
ここでＣ製容器内のＴｉとＢの混合粉末内にあらかじめ
用意してあったＷフィラメントにＨＩＰ外部より通電加
熱することによって、加圧自己燃焼焼結を行なった。
その結果理論密度の９７．２％のＡｌ１−０．−ＴｉＣ
複合セラミックスを得た。
効　　果 以上説明してきたように、本発明を用いることによって
、加圧自己燃焼焼結法を工業的に利用することが可能と
なった。

Claims (3)

    【特許請求の範囲】
  1. （１）加圧下金属元素と非金属元素の混合物からセラミ
    ックスを合成する際に発生する反応熱を利用してセラミ
    ックスを合成焼結する加圧自己燃焼焼結法において、該
    金属元素と非金属元素の混合物を気密容器内に挿入した
    後、反応開始用の熱源として金属元素と非金属元素との
    混合物にて気密容器をおおったのち該外部金属元素と非
    金属元素の混合物の一端を加熱することによって、連鎖
    的に反応が進行することによって発生する反応熱を用い
    ることを特徴とする加圧自己燃焼焼結法。
  2. （２）特許請求の範囲第１項記載の加圧自己燃焼焼結法
    において、金属元素として周期律表IIIａ，IVａ，Ｖａ
    ，VIａ族金属の１種以上、非金属元素としてＢ，Ｃ，Ｎ
    ，Ｓｉの１種以上であることを特徴とする加圧自己燃焼
    焼結法。
  3. （３）特許請求の範囲第１、２項記載の加圧自己燃焼焼
    結法において、加圧法として熱間静水圧プレス（ＨＩＰ
    ）を用いることを特徴とする加圧自己燃焼焼結法。
JP62277150A 1987-10-30 1987-10-30 加圧自己燃焼焼結法 Granted JPH01119568A (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP62277150A JPH01119568A (ja) 1987-10-30 1987-10-30 加圧自己燃焼焼結法
US07/263,245 US4999144A (en) 1987-10-30 1988-10-27 Pressure self-combustion sintering method
DE8888310147T DE3879619T2 (de) 1987-10-30 1988-10-28 Autothermisches drucksinterverfahren.
EP88310147A EP0314492B1 (en) 1987-10-30 1988-10-28 Pressure self-combustion sintering method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62277150A JPH01119568A (ja) 1987-10-30 1987-10-30 加圧自己燃焼焼結法

Publications (2)

Publication Number Publication Date
JPH01119568A true JPH01119568A (ja) 1989-05-11
JPH0515669B2 JPH0515669B2 (ja) 1993-03-02

Family

ID=17579497

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62277150A Granted JPH01119568A (ja) 1987-10-30 1987-10-30 加圧自己燃焼焼結法

Country Status (4)

Country Link
US (1) US4999144A (ja)
EP (1) EP0314492B1 (ja)
JP (1) JPH01119568A (ja)
DE (1) DE3879619T2 (ja)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06247775A (ja) * 1993-02-19 1994-09-06 Yoshio Miyamoto ガス圧燃焼焼結法
WO2023162721A1 (ja) * 2022-02-24 2023-08-31 株式会社トクヤマ 炭化ケイ素粉末及びその製造方法

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* Cited by examiner, † Cited by third party
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EP0429665B1 (en) * 1989-06-12 1998-03-11 Kabushiki Kaisha Komatsu Seisakusho Method of producing sintered ceramic materials
EP0621859A1 (en) * 1992-01-16 1994-11-02 University Of Cincinnati Electrical heating element, related composites, and composition and method for producing such products using dieless micropyretic synthesis
US5310476A (en) 1992-04-01 1994-05-10 Moltech Invent S.A. Application of refractory protective coatings, particularly on the surface of electrolytic cell components
US6001236A (en) 1992-04-01 1999-12-14 Moltech Invent S.A. Application of refractory borides to protect carbon-containing components of aluminium production cells
US5651874A (en) 1993-05-28 1997-07-29 Moltech Invent S.A. Method for production of aluminum utilizing protected carbon-containing components
US5837632A (en) * 1993-03-08 1998-11-17 Micropyretics Heaters International, Inc. Method for eliminating porosity in micropyretically synthesized products and densified
US5449886A (en) * 1993-03-09 1995-09-12 University Of Cincinnati Electric heating element assembly
WO1995031416A1 (en) * 1994-05-13 1995-11-23 Micropyretics Heaters International Sinter-homogenized heating products
DE69526264T2 (de) 1994-09-08 2002-10-24 Moltech Invent Sa Aluminium Elektrolysezelle mit drainierfähige Kathode
US5794113A (en) * 1995-05-01 1998-08-11 The Regents Of The University Of California Simultaneous synthesis and densification by field-activated combustion
US5753163A (en) 1995-08-28 1998-05-19 Moltech. Invent S.A. Production of bodies of refractory borides
US6099978A (en) * 1996-02-28 2000-08-08 Micropyrctics Heaters International, Inc. Molybdenum silicide-containing products with high emissivity

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JPS5627441A (en) * 1979-08-14 1981-03-17 Matsushita Electric Ind Co Ltd Printer unit
JPS62256767A (ja) * 1986-04-30 1987-11-09 松下電器産業株式会社 炭窒化物と酸化物からなる複合焼結体の製造方法
JPS63239160A (ja) * 1986-11-28 1988-10-05 工業技術院長 無機化合物成形体の製造方法

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DE3588005T2 (de) * 1984-05-18 1995-08-24 Sumitomo Electric Industries Verfahren zum Sintern von keramischen Körpern mit einer verteilten Metallverstärkung.
JPH0791567B2 (ja) * 1985-02-15 1995-10-04 株式会社小松製作所 焼結方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5627441A (en) * 1979-08-14 1981-03-17 Matsushita Electric Ind Co Ltd Printer unit
JPS62256767A (ja) * 1986-04-30 1987-11-09 松下電器産業株式会社 炭窒化物と酸化物からなる複合焼結体の製造方法
JPS63239160A (ja) * 1986-11-28 1988-10-05 工業技術院長 無機化合物成形体の製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06247775A (ja) * 1993-02-19 1994-09-06 Yoshio Miyamoto ガス圧燃焼焼結法
WO2023162721A1 (ja) * 2022-02-24 2023-08-31 株式会社トクヤマ 炭化ケイ素粉末及びその製造方法

Also Published As

Publication number Publication date
US4999144A (en) 1991-03-12
EP0314492A1 (en) 1989-05-03
EP0314492B1 (en) 1993-03-24
DE3879619T2 (de) 1993-09-23
DE3879619D1 (de) 1993-04-29
JPH0515669B2 (ja) 1993-03-02

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