JPH0244785B2 - - Google Patents

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Publication number
JPH0244785B2
JPH0244785B2 JP56124102A JP12410281A JPH0244785B2 JP H0244785 B2 JPH0244785 B2 JP H0244785B2 JP 56124102 A JP56124102 A JP 56124102A JP 12410281 A JP12410281 A JP 12410281A JP H0244785 B2 JPH0244785 B2 JP H0244785B2
Authority
JP
Japan
Prior art keywords
oxide
weight
powder
sintered body
silicon nitride
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.)
Expired - Lifetime
Application number
JP56124102A
Other languages
English (en)
Other versions
JPS5826077A (ja
Inventor
Michikana Komatsu
Hiroyasu Oota
Akihiko Tsuge
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.)
Toshiba Corp
Original Assignee
Tokyo Shibaura Electric Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=14876969&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=JPH0244785(B2) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Tokyo Shibaura Electric Co Ltd filed Critical Tokyo Shibaura Electric Co Ltd
Priority to JP56124102A priority Critical patent/JPS5826077A/ja
Priority to EP82107134A priority patent/EP0071997B1/en
Priority to DE8282107134T priority patent/DE3262429D1/de
Priority to US06/406,440 priority patent/US4407970A/en
Publication of JPS5826077A publication Critical patent/JPS5826077A/ja
Publication of JPH0244785B2 publication Critical patent/JPH0244785B2/ja
Granted legal-status Critical Current

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Description

【発明の詳細な説明】
本発明は、窒化ケイ素を主成分とするセラミツ
クス焼結体及びその製造方法に関し、更に詳しく
は、高密度で、機械的強度及び耐熱衝撃性が優
れ、且つ900℃程度の温度で、長時間酸化雰囲気
下にあつても機械的強度の低下度合が小さいセラ
ミツクス焼結体及びその製造方法に関する。 セラミツクス焼結体は、熱的性質が優れ、且つ
高密度を有しているために、各種構造材料の先端
にあるものとして各産業分野で広く注目を集めて
いるが、その代表的なものとして窒化ケイ素の焼
結体がある。 従来から、窒化ケイ素焼結体の製造において
は、反応焼結法、ホツトプレス法及び普通焼結法
が一般に採用されている。 このうち、反応焼結法は、金属ケイ素（Si）の
粉末で予め必要とする形を成形し、これを窒素又
はアンモニアガス雰囲気中で徐々に加熱して窒化
と同時に焼結するという方法である。 また、ホツトプレス法は、窒化ケイ素
（Si3N4）の粉末に、焼結助剤（例えば、Y2O3、
MgO、Al2O3）を添加し、これを所定の型（例え
ば黒鉛の型）の中で1700〜1800℃の高温下、150
〜500Kg／cm2の圧力を印加して焼結する方法であ
る。この方法によれば、高密度で機械的強度も大
きく、かつ耐熱衝撃性又は高温酸化雰囲気下での
機械的強度の低下が小さい等の優れた熱的性質を
有する焼結体を得ることができる。しかし、一方
で、この方法は複雑で大型形状の焼結体を得るこ
とが困難で、しかも量産性に劣るという欠点を有
する。 他方、普通焼結法は、Si3N4粉末と焼結助剤を
パラフインのような粘結剤で予め成形し、これを
非酸化性雰囲気下でホツトプレスすることなくそ
のまま加熱して焼結する方法である。しかし、こ
の方法では、高密度で機械的強度及び耐熱衝撃性
に優れた焼結体を得ることは困難である。 そのため、本発明者らは、上記普通焼結法に関
し種々の検討を加えた結果、ホツトプレス法に匹
敵して、機械的強度・耐熱衝撃性にすぐれた高密
度焼結体を製造できる普通焼結法を提案した（特
開昭55−113674号、特開昭55−116670号）。 しかしながら、これらの方法で得られた窒化ケ
イ素焼結体の高温酸化雰囲気下における機械的強
度の低下に対する抵抗性は必ずしも満足のいくも
のではなかつた。 本発明者らは、更に上記の点に関し、鋭意研究
を重ねた結果、本発明を完成するに到つた。 本発明の目的は、高密度で耐熱衝撃性に優れ、
しかも、900℃程度の温度で、長時間酸化雰囲気
下にあつても機械的強度の低下が小さいセラミツ
クス焼結体、とりわけ窒化ケイ素を主成分とする
セラミツクス焼結体及びその製造方法を提供する
ことである。 即ち、本発明のセラミツクス焼結体は、酸化イ
ツトリウム（Y2O3）0.1〜10重量％；酸化アルミ
ニウム（Al2O3）0.1〜10重量％；窒化アルミニウ
ム（AlN）0.1〜10重量％；酸化リチウム
（Li2O）、酸化ベリリウム（BeO）、酸化カルシウ
ム（CaO）、酸化バナジウム（V2O5）、酸化マン
ガン（MnO2）、酸化モリブデン（MoO3）、及び
酸化タングステン（WO3）のそれぞれの酸化物
から成る群より選ばれる少なくとも１種の酸化
物、若しくはこれらと、酸化ボロン（B2O3）、酸
化マグネシウム（MgO）、酸化チタン（TiO2）、
酸化クロム（Cr2O3）、酸化コバルト（CoO）、酸
化ニツケル（NiO）、酸化ジルコニウム（ZrO2）、
酸化ニオブ（Nb2O5）、酸化ハフニウム（HfO2）、
及び酸化タンタル（Ta2O5）のそれぞれの酸化物
から成る群より選ばれる１種若しくはそれ以上の
ものとを組合せて成る酸化物0.1〜５重量％；及
び残部は窒化ケイ素（Si3N4）から成ることを特
徴とするものである。 本発明のセラミツクス焼結体は、Si3N4を主成
分とするものであり、Si3N4は70重量％以上の配
合比で用いられることが好ましい。使用される
Si3N4は、α相型、β相型のいずれであつてもよ
いが、α相型が好んで用いられる。 Y2O3及びAl2O3はいずれも焼結促進剤として機
能する。これら成分は、その配合比がそれぞれ10
重量％を超えると、得られた焼結体の機械的強度
及び耐熱衝撃性が低下して好ましくない。これら
の成分は、通常、両者を合わせて３〜15重量％の
配合比にあることが好ましい。 AlNは、主成分であるSi3N4の焼結過程におけ
る蒸発を抑制する機能のほか、他の成分と反応し
て焼結に資する液相を生成して全体の焼結促進に
寄与する。その配合比が10重量％を超えると、得
られた焼結体の機械的強度及び耐熱衝撃性を低下
せしめる。 また、Li2O、BeO、B2O3、MgO、CaO、
TiO2、V2O5、Cr2O3、MnO2、CoO、NiO、
ZrO2、Nb2O5、MoO3、HfO2、Ta2O5、WO3な
どの酸化物は、いずれも上記したY2O3、Al2O3な
どの焼結促進剤の機能を助長するものである。更
に、Li2O、BeO、CaO、V2O5、MnO2、MoO3、
WO3などの酸化物は、900℃程度の温度で、酸化
雰囲気下において、焼結体表面に酸化抵抗の大き
い保護被膜を形成するために、得られた焼結体の
機械的強度の低下を防止する機能を有する。特
に、Li2O、BeO、V2O5はその効果に資すること
大である。しかしながら、それらの配合比が５重
量％を超えると、かえつて焼結体の機械的強度及
び耐熱衝撃性を低下せしめて好ましくない。 本発明のセラミツクス焼結体の製造方法は、酸
化イツトリウム（Y2O3）粉末0.1〜10重量％；酸
化アルミニウム（Al2O3）粉末0.1〜10重量％；窒
化アルミニウム（AlN）粉末0.1〜10重量％；酸
化リチウム（Li2O）、酸化ベリリウム（BeO）、
酸化カルシウム（CaO）、酸化バナジウム
（V2O5）、酸化マンガン（MnO2）、酸化モリブデ
ン（MoO3）、及び酸化タングステン（WO3）の
それぞれの酸化物から成る群より選ばれる少なく
とも１種の酸化物粉末、若しくはこれらと、酸化
ボロン（B2O3）、酸化マグネシウム（MgO）、酸
化チタン（TiO2）、酸化クロム（Cr2O3）、酸化コ
バルト（CoO）、酸化ニツケル（NiO）、酸化ジル
コニウム（ZrO2）、酸化ニオブ（Nb2O5）、酸化
ハフニウム（HfO2）、及び酸化タンタル
（Ta2O5）のそれぞれの酸化物から成る群より選
ばれる１種若しくはそれ以上のものとを組合せて
成る酸化物粉末0.1〜５重量％；及び残部が窒化
ケイ素（Si3N4）粉末から成る混合粉末を成形
し、該成形体を非酸化性雰囲気中で焼結すること
を特徴とするものである。 本発明方法において、これらの各成分の混合
は、通常のボールミル等の粉砕混合機により、ｎ
−ブチルアルコール等の溶媒を用いて行なうこと
ができる。 このように調製された混合粉末にパラフイン等
の粘結剤を添加して適宜な圧力を印加し、所定形
状の成形体とする。 この成形体を非酸化性雰囲気中、1500〜1900
℃、好ましくは1600〜1800℃で加熱して焼結せし
め、焼結体とする。非酸化性雰囲気としては、窒
素、アルゴン等があげられる。酸化性雰囲気では
Si3N4が酸化してSiO2になるため不可である。な
お、この焼結時に、50〜500Kg／cm2の圧力を印加
したホツトプレス状態、または、非酸化性ガス雰
囲気中、加圧状態で焼結してもよい。或いは、普
通焼結法による焼結を行なつた後に、更に加圧雰
囲気下で焼結を行なつたものであつても焼結体の
特性は何ら損われるものではない。 以下において、本発明を、実施例及び参考例を
掲げて更に詳細に説明する。 実施例及び参考例 表に示したように、各成分を所定の配合比（重
量％）で配合し、ここにｎ−ブチルアルコールを
適量添加した後、ゴムライニングボールミルで24
時間それぞれ混合して本発明に係る実施例として
16種類、並びに参考例として11種類、計27種類の
混合粉末を調製した。なお、Si2N4の粉末は、α
相型Si3N485％を含む平均粒径1.2μの粉末である。
また、Y2O3粉末の平均粒径は1.0μ、Al2O3粉末の
平均粒径は0.5μ、AlNの平均粒径は1.5μ、各種の
酸化物の平均粒径は1.0μであつた。 得られた混合粉末に、更にパラフインを７重量
％添加した後、室温下、700Kg／cm2の成形圧で長
さ60mm、幅40mm、及び厚み10mmの板状体を成形し
た。得られた各成形体を、まず700℃で加熱処理
してパラフインを熱分解除去し、ついで窒素ガス
を通流（３／min）しながら1750℃で焼結し
た。 得られた各焼結体につき、相対密度、室温下で
の抗折強度、空気中900℃で、100時間、1000時
間、及び5000時間それぞれ酸化処理した後の室温
下での抗折強度、並びに耐熱衝撃性を測定した。 それらの結果を、実施例１〜16及び参考例１〜
11として表に示した。それぞれの測定項目は以下
の仕様に従つた。 相対密度：組成比から算出した理論密度に対する
相対比（％）で示した。 抗折強度：３点曲げ強度試験によるもので、試片
のサイズ３×３×30mm、クロスヘツドスピード
0.5mm／min、スパン20mm、温度室温。測定は
各試片４枚につき行ないその平均値で示した。 耐熱衝撃性：抗折強度測定用試験片と同一形状の
試験片をある温度に加熱した後水中に投入して
急冷し、試験片へのクラツク発生の有無を蛍光
探傷法で観察し、クラツク発生時における加熱
温度と水温との差ΔTをもつて表示した。 表から明らかなように、本発明方法によつて得
られた焼結体（実施例１〜16）は、相対密度は理
論密度の95％以上と高密度であり、またその抗折
強度も85Kg／mm2以上と大きく、耐熱衝撃性もΔT
で表わしてほぼ700℃以上である。とりわけ、900
℃で5000時間の酸化処理後にあつてもその抗折強
度の低下の小さいことが判明した。 以上詳述したように、本発明方法はホツトプレ
スすることを必要としないので大量生産に適合
し、しかも高密度で耐熱衝撃性に優れ、かつ900
℃程度の温度での酸化雰囲気下における機械的強
度の低下の小さい焼結体を製造できるので、その
工業的有用性は大である。
【表】
【表】

Claims (1)

  1. 【特許請求の範囲】 １ 酸化イツトリウム0.1〜10重量％；酸化アル
    ミニウム0.1〜10重量％；窒化アルミニウム0.1〜
    10重量％；酸化リチウム、酸化ベリリウム、酸化
    カルシウム、酸化バナジウム、酸化マンガン、酸
    化モリブデン、及び酸化タングステンのそれぞれ
    の酸化物から成る群より選ばれる少なくとも１種
    の酸化物、若しくはこれらと、酸化ボロン、酸化
    マグネシウム、酸化チタン、酸化クロム、酸化コ
    バルト、酸化ニツケル、酸化ジルコニウム、酸化
    ニオブ、酸化ハフニウム、及び酸化タンタルのそ
    れぞれの酸化物から成る群より選ばれる１種若し
    くはそれ以上のものとを組合せて成る酸化物0.1
    〜５重量％；及び残部は窒化ケイ素から成ること
    を特徴とするセラミツクス焼結体。 ２ 酸化イツトリウム粉末0.1〜10重量％；酸化
    アルミニウム粉末0.1〜10重量％；窒化アルミニ
    ウム粉末0.1〜10重量％；酸化リチウム、酸化ベ
    リリウム、酸化カルシウム、酸化バナジウム、酸
    化マンガン、酸化モリブデン、及び酸化タングス
    テンのそれぞれの酸化物粉末から成る群より選ば
    れる少なくとも１種の酸化物粉末、若しくはこれ
    らと、酸化ボロン、酸化マグネシウム、酸化チタ
    ン、酸化クロム、酸化コバルト、酸化ニツケル、
    酸化ジルコニウム、酸化ニオブ、酸化ハフニウ
    ム、及び酸化タンタルのそれぞれの酸化物粉末か
    ら成る群より選ばれる１種若しくはそれ以上のも
    のとを組合せて成る酸化物粉末0.1〜５重量％；
    及び残部が窒化ケイ素粉末から成る混合粉末を成
    形し、該成形体を非酸化性雰囲気中で焼結するこ
    とを特徴とするセラミツクス焼結体の製造方法。
JP56124102A 1981-08-10 1981-08-10 セラミツクス焼結体及びその製造方法 Granted JPS5826077A (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP56124102A JPS5826077A (ja) 1981-08-10 1981-08-10 セラミツクス焼結体及びその製造方法
EP82107134A EP0071997B1 (en) 1981-08-10 1982-08-06 Sintered body of ceramics and preparation thereof
DE8282107134T DE3262429D1 (en) 1981-08-10 1982-08-06 Sintered body of ceramics and preparation thereof
US06/406,440 US4407970A (en) 1981-08-10 1982-08-09 Sintered body of ceramics and preparation thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP56124102A JPS5826077A (ja) 1981-08-10 1981-08-10 セラミツクス焼結体及びその製造方法

Publications (2)

Publication Number Publication Date
JPS5826077A JPS5826077A (ja) 1983-02-16
JPH0244785B2 true JPH0244785B2 (ja) 1990-10-05

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US (1) US4407970A (ja)
EP (1) EP0071997B1 (ja)
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DE (1) DE3262429D1 (ja)

Families Citing this family (55)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4511525A (en) * 1981-11-26 1985-04-16 Tokyo Shibaura Denki Kabushiki Kaisha Process for producing sintered silicon nitride-base body
EP0107919A1 (en) * 1982-10-01 1984-05-09 The British Ceramic Research Association Limited Silicon nitride ceramic bodies
JPS59116175A (ja) * 1982-12-22 1984-07-04 株式会社東芝 セラミツクス焼結部材
US5178647A (en) * 1983-07-29 1993-01-12 Kabushiki Kaisha Toshiba Wear-resistant member
JPS6054976A (ja) * 1983-09-02 1985-03-29 日本碍子株式会社 窒化珪素焼結体
SE451195B (sv) * 1984-02-29 1987-09-14 Sandvik Ab Keramiskt material baserat pa kiselnitrid
JPS60191063A (ja) * 1984-03-06 1985-09-28 京セラ株式会社 窒化珪素質焼結体
DE3471647D1 (en) * 1984-08-11 1988-07-07 Hutschenreuther Process for making a fully-crystalline silicon nitride sintered body
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US4407970A (en) 1983-10-04

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