JPS5826077A - セラミツクス焼結体及びその製造方法 - Google Patents

セラミツクス焼結体及びその製造方法

Info

Publication number
JPS5826077A
JPS5826077A JP56124102A JP12410281A JPS5826077A JP S5826077 A JPS5826077 A JP S5826077A JP 56124102 A JP56124102 A JP 56124102A JP 12410281 A JP12410281 A JP 12410281A JP S5826077 A JPS5826077 A JP S5826077A
Authority
JP
Japan
Prior art keywords
oxide
sintered body
powder
weight
sintering
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
JP56124102A
Other languages
English (en)
Other versions
JPH0244785B2 (ja
Inventor
小松　通奏
博康 大田
柘植　章彦
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=JPS5826077(A) "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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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】 本発明は、窒化ケイ素を主成分とするセ２ミツクス焼結
体及びそのＩＩ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＠度で、長時間酸化雰囲気下にあっても機械的強度の
低下度合が小さいセラミックス焼結体及びその製造方法
に関する。
セラミックス焼結体は、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、ホッ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（８ｉ）　（Ｄ粉
末で予め必要とする形を成形し、これｔ窒素又はアン毫
ニアガス雰囲気中で徐々に加熱して窒化と同一に焼結す
るという方法である。
また、ホットプレス法は、窒化ケイ素（ＳｉｌＮ４）の
粉末に、焼結助剤（例えば、Ｙ＠　Ｏ＠　ｔ　ＭｇＯ２
Ｍｚ”ｓ　）を添加し、これを所定の製（例えば黒鉛の
Ｉｔ）＋２）ｓｏｏｋ４Ｆ／ａｉ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Ｏ
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ｍ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、８’ｌＮ４粉末と焼結助剤【／母
２フィンのような粘結剤で予め成形し、これを非酸化性
雰囲気下でホッ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次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、ホットプレス法に匹敵して、機械的
強度ｅ耐熱衝撃性にすぐれた高密度焼結体１製造できる
普通焼結法を提案した（特開昭５５−１１３６７４号、
Ｉ＃８＠６５−１１６６７０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った。
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った。
本発明の目的紘、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っても
機械的強度の低下が小さいセラミックス焼結体、とりわ
け窒化ケイ素を主成分とする＋１１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１本発明のセラミックス焼結体は、酸化イツトリウ
ム（Ｙ露０謬）０．１〜１０重量％；酸化アルミニウム
（Ａｚ、ｏ、　）　０．１〜１０重量％；窒化アル１ニ
ウム（Ａ４Ｎ）０．１〜１０重量％；酸化リチウム（Ｌ
ｉ、０）、酸化ベリリウム（ＢｅＯ）　、酸化カルシウ
ム（Ｃａｂ）、酸化パナゾウム（ＶｓＯｓ　）　ｓ酸化
マンガン（ＭｎＯｓ　）　、酸化モリブデン（Ｍｏ５＝
　）、及び酸化タングステン（ＷＯｓ）のそれぞれの酸
化物から成る評よシ選ばれる少なくとも１８Ｉ［の酸化
物、若しくはこれらと、酸化、ｙａン（ＢｍＯｓ）、酸
化マグネシウム（ＭｇＯ）、酸化チタン（Ｔｉｅ、）、
酸化り曹ム（Ｃｆｆ０ｓ）、酸化コ／＃ルト（Ｃｏｏ　
）、酸化ニッケル（ＮｉＯ）、酸化ジルコニウムＣＺ’
０＊）、酸化二オツ（Ｎｂ怠Ｏｓ）、酸化ハフニウム（
ＨｆＯ，）、及び酸化タンタル（Ｔａｍｅｓ）のそれぞ
れの酸化物から成る評よｐ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帆１〜５重量ｔｓ：及
び残部は窒化ケイ素（ＳｉｌＮ４）から成ることを特徴
とするものである。
本発明のセラミックス焼結体は、５ｉｓＮａＹｒ主成分
とするものであシｓ　５ｔｓＮ４は７０重量−以上Ｏ配
合比で用いられることが好ましい。使用されるＳ　ｉ、
Ｎ４は、α相型、β相型のいずれであってもよいが、α
相型が好んで用いられる。
Ｙ　ｍ　Ｏｓ及びＡ４０ｍ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−動超えると、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。
ＡｊＮは、主成分であるＳ　ｉ、Ｎ、　０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、得られ次焼結体の
機械的強度及び耐熱衝撃性を低下せしめる。
Ｉｔ、Ｌｉ１Ｏ、Ｂｅ０１Ｂ２０Ｂ、　ＭｇＯ１ＣａＯ
、’ｒｉｏ、。
ＶｍＯｓ＊　Ｃｒａｂｓ％ＭｎＯ麿、Ｃｏ０５ＮｉＯ１
ＺｒＯｓｓＮｂ＊ＯａｓＭｏｓｓ、ＨｆＯ，、”ＩＯＩ
％ｗｏｓなどの酸化物は、いずれも上記したＹ雪Ｏｓｓ
　ＡＴＯｓなどの焼結促進剤の機能を助長するものであ
るっ更に、Ｌｉ２Ｏ、Ｂｅ０１ＣａＯ１■、０６、Ｍｎ
ｏ＊　、ＭＯＯ３、ＷＯｌなどの酸化物ｔ１．９００℃
程度の亀度で、酸化雰囲気下において、焼結体＊面に１
化抵抗の大きい保護被膜を形成するために、得られ次焼
結体の機械的強度の低下を防止する機能を有する。特に
、　Ｌｉ！０．　Ｂｅｄ。
Ｖ、Ｏ，はそＯ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ｔｓｔ超えると、かえって焼
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。
本発明の七フィックス焼結体の製造方法は、酸化イツト
リウム（ＹｍＯｓ）粉末０．１〜１０重ｉｔｓ；酸化ア
ルｉ＝ウム（Ａ４０ｍ　）粉末０．１〜１０重量％；窒
化アル建ニウム（Ａ／＝Ｎ）粉末０．１−１０重量％：
酸化リチウム（Ｌ　’ｓｏ　）　、酸化ベリリウム（Ｂ
ｅｄ）、酸化カルシウム（Ｃａｂ）、酸化パナジク’　
（ＹｍＯｓ　）、Ｈ化マンガン（Ｍｎ０ｍ　）　、　Ｉ
Ｉ化モリブデン（Ｍｏ０１　）　、及び酸化タングステ
ン（ＷＯｍ）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
化がロン（ＢｍＯｓ　）、酸化マグネシウム（Ｍ’ｇＯ
）、酸化チタｙ　（Ｔ　ｆｏｇ　）　、酸化り”　ム（
Ｃｒａｂｓ　）、酸化コバルト（Ｃｏｄ）、酸化ニッケ
ル（ＮｉＯ）、酸化ジルコニクＡ　（Ｚｒ０ｍ　）、酸
化ニオブ（ＮｂｍＯｓ　）　。
酸化ハフニウム（ＨｆＯ，）、及び酸化タンタル（’ｌ
’ａ＊Ｑ５　）のそれぞれの酸化物から成る群よシ選ば
れる１１１ｆｒＬ（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−二及び残部が窒化ケイ：ｌ
Ａ　（Ｓ　１ｓＮａ　）粉末から成る混合粉末を成形し
、鉄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Ｏ
Ｓ−ルンル等の粉砕混合機によシ、ｎ−ブチルアルコー
ル勢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ィン勢の粘結剤
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
ルコ°ン等があげられる。
酸化性雰囲気ではｇ　ｉ、Ｎ４が酸化して８ｉ０１にな
るため不可である。なお、この焼結時に、５０〜５００
ｋｙ／−の圧力を印加したホットプレス状態、また社、
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った後に、更に加圧
雰囲気下で焼結を行なつ次ものであっても焼結体の特性
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 表に示し次ように、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【適量添加した後
、プムライニングが一ルミルで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ｔ−ｖ４Ｉｌ！シ
た。なお、８ｉ、Ｎ４の粉末は、α相型５ｉｓＮ４８５
　％　！−含む平均粒径１．２μの粉末である。ま九％
　ＹＩＯＩ粉末の平均粒径は１．０μ、ＡＪ４０．粉末
の平均粒径は０．５μ、ＡＡＮの平均粒径は１．５μ、
各種の酸化物の平均粒径は１．０μであった。
得られた混合粉末に、更にパラフィンを７重量％添加し
た後、室温下、７００ｋｔ／−の成形圧で長さ６０■、
幅４０簡、及び厚みｌＯ■の板状体を成形し次。得られ
た各成形体を、まず７００℃で加熱処理して７４２フイ
ンを熱分解除去し、ついてｉ！Ｉ票ガスを通流（３１７
ｍ　）　Ｌながら１７５０℃て焼結した。
得られた各焼結体につき、相対密度、室温下でＯ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危
機の室温下でＯ抗折強度、並びに耐熱衝撃性を一定した
。
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。それ七九の測定項目は以下の仕様に従
り次。
相対密度：組成比から算出した理論密度に対する相対比
（４）で示した。
抗折５ｊ１度：３点曲げ強記試験によるもので、試片の
サイ）ｅ３Ｘ３Ｘ３０■、りシス ヘッドスピード０．５■／−、スイン ２０閣、温度室温。測定は各試片４ 枚にり自行ないその平均値で示した。
耐熱衝撃性：抗折強ＩｊＩＬ測朝試験片と同一形状の試
験片′ｔあるｉｌ＆に加熱した抜水中に投入して急冷し
、試験片へのクツツ ク発生の有無を蛍光探傷法で観察し、 クランク発生時における加熱＠度と 水温との差ΔＴ’＆もって表示した。
表から明らかなように、本発明方法によって得られた焼
結体（実施例１〜１６）は、相対密度は理論密度の９５
−以上と高密度であシ、またその抗折強度も８５ｋｆ／
−以上と大きく、耐熱衝撃性ｔΔＴで表わしてには７０
０℃以上である。とルわけ、９００℃で５ｏｏｏ時間の
酸化処理後にあってもその抗折強度の低下の小さいこと
が判明しｆＩ−。
以上詳述したように、本発明方法はホットプレスするこ
とを必要としないので大量生産に適合し、しかも高ｌ！
Ｆ度で耐熱衝撃性に優れ、かつ９００℃程度の温度での
酸化雰囲気下にお妙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。

Claims (1)

  1. 【特許請求の範囲】 （１１酸化イツトリウム０．１−１０重量優；酸化アル
    建ニウム０．１〜ｌＯ重ＵＳ：窒化アルミニ９４０．１
    〜１Ｏ重量Ｉｓ：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
    ら成る評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ｌロン、酸化マグネシクム、酸化チタ
    ン、酸化クロム、酸化コ／４ルト、酸化ニッケル、酸化
    ジルコニウム、酸化ニオブ、酸化へ７ニクム、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ｔ組合せて成る酸化物０．
    １〜５重ｉｔｓ：及び残部性窒化ケイ素から成ることｔ
    特徴とするセラミックス焼結体。 （２）酸化イツトリウム粉末０．１〜ｌＯ重量％；酸化
    アルミニウム粉末０．１〜１０１１１ｔ％　：窒化アル
    ンニウム粉末０．１〜ｌＯ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−四ン、酸化
    マグネシウム、酸化チタン、酸化クロ・ム、酸化コバル
    ト、酸化ニッケル、酸化ジルコニウム、酸化ニオブ、酸
    化ハフニウム、及び酸化メンタルのそれぞれの酸化物粉
    末から成る群よシ選ばれる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０１〜５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七りイ
    ッ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)

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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

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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)

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

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JP56124102A Granted 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

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US (1) US4407970A (ja)
EP (1) EP0071997B1 (ja)
JP (1) JPS5826077A (ja)
DE (1) DE3262429D1 (ja)

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CN116715521A (zh) * 2023-06-07 2023-09-08 中国科学院新疆理化技术研究所 一种接触式温控器中CaYNbMnO7热敏电阻的冷辅助制备方法

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JPS60191063A (ja) * 1984-03-06 1985-09-28 京セラ株式会社 窒化珪素質焼結体
KR20230053774A (ko) * 2021-10-14 2023-04-24 엘티메탈 주식회사 몰리브덴 산화물계 소결체, 이를 포함하는 스퍼터링 타겟 및 산화물 박막
CN116715521A (zh) * 2023-06-07 2023-09-08 中国科学院新疆理化技术研究所 一种接触式温控器中CaYNbMnO7热敏电阻的冷辅助制备方法

Also Published As

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JPH0244785B2 (ja) 1990-10-05
EP0071997A1 (en) 1983-02-16
DE3262429D1 (en) 1985-03-28
EP0071997B1 (en) 1985-02-20
US4407970A (en) 1983-10-04

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