JPS63319263A - Silicon nitride-based ceramic - Google Patents
Silicon nitride-based ceramicInfo
- Publication number
- JPS63319263A JPS63319263A JP62154362A JP15436287A JPS63319263A JP S63319263 A JPS63319263 A JP S63319263A JP 62154362 A JP62154362 A JP 62154362A JP 15436287 A JP15436287 A JP 15436287A JP S63319263 A JPS63319263 A JP S63319263A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- sintering
- metallic
- tin
- si3n4
- 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
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 23
- 239000000919 ceramic Substances 0.000 title claims abstract description 15
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 20
- 239000000654 additive Substances 0.000 claims abstract description 10
- 239000010419 fine particle Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract 3
- 239000002245 particle Substances 0.000 claims description 11
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 4
- 239000000203 mixture Substances 0.000 abstract 3
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- 238000005452 bending Methods 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔発明の目的〕
（産業上の利用分野）
本発明は常温においても、また高温においても機械的性
質の優れた窒化ケイ素を主成分とするセラミックス焼結
体に関する。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Industrial Field of Application) The present invention relates to a ceramic sintered body mainly composed of silicon nitride, which has excellent mechanical properties both at room temperature and at high temperature.
（従来の技術） 窒化ケイ素系セラミックスは高強度で耐熱性。(Conventional technology) Silicon nitride ceramics have high strength and heat resistance.
耐食性が高いなどの優れた特徴をもつセラミックスとし
て知られている。しかしながら、構造材料として実用化
するには破壊靭性値が低く、また特に高温において強度
が低下するという問題がある。It is known as a ceramic with excellent characteristics such as high corrosion resistance. However, for practical use as a structural material, there are problems in that the fracture toughness value is low and the strength particularly decreases at high temperatures.
（発明が解決しようとする問題点）
窒化ケイ素系セラミックスにおいては、高温における強
度低下と低い破壊靭性値が問題として残っている。(Problems to be Solved by the Invention) In silicon nitride ceramics, problems remain such as a decrease in strength at high temperatures and a low fracture toughness value.
本発明の目的は上記した問題点を解決し、機械的特性の
優れた窒化ケイ素系セラミックスを提供しようとするも
のである。An object of the present invention is to solve the above problems and provide silicon nitride ceramics with excellent mechanical properties.
本発明の窒化ケイ素−添加物系の焼結体からなる窒化ケ
イ素系セラミックスは、添加物の反応により形成される
焼結体中の粒界第２相中および、窒化ケイ素粒子内部に
窒化チタンあるいはチタン金属を含むことを特徴とする
。The silicon nitride ceramics made of the silicon nitride-additive-based sintered body of the present invention has titanium nitride or It is characterized by containing titanium metal.
窒化ケイ素粉末に焼結添加物として、酸化イツトリウム
、酸化アルミニウムなどを混合する際に、窒化チタン、
金属チタンあるいは、焼結のための加熱時に窒化チタン
もしくは、還元されて金属チタンに変る酸化チタン等の
微粒子を同時に加えた粉末をつくり、焼結することによ
って、添加物の反応により形成される焼結体中の粒界第
２相中および、窒化ケイ素粒子内部に窒化チタンあるい
はチタン金属を含む窒化ケイ素系セラミックスをつくる
ことができる。窒化チタンあるいはチタン金属は窒化ケ
イ素および、焼結添加物と反応せず、微粒子として存在
し、また窒化ケイ素とのなじみがいいため窒化ケイ素粒
子内部にも微粒子として存在することができるのである
。When mixing yttrium oxide, aluminum oxide, etc. as sintering additives to silicon nitride powder, titanium nitride,
By creating a powder to which fine particles of titanium metal or titanium nitride or titanium oxide, which is reduced and converted to titanium metal, are simultaneously added during heating for sintering, and sintering it, the sintered material is formed by the reaction of additives. Silicon nitride ceramics containing titanium nitride or titanium metal in the grain boundary second phase in the compact and inside the silicon nitride particles can be produced. Titanium nitride or titanium metal does not react with silicon nitride or sintering additives and exists as fine particles, and since it is compatible with silicon nitride, it can also exist as fine particles inside silicon nitride particles.
このような粒界第２相中および、窒化ケイ素粒子内部に
窒化チタンあるいはチタン金属を含む窒化ケイ素系セラ
ミックスは、焼結体に応力がかかって、破壊するときに
、亀裂が窒化チタンあるいはチタン金属粒子によって曲
げられ、あるいは分岐するため、破壊エネルギーの増大
をもたらし、破壊靭性値の向上および、高温における強
度の劣化を防止する作用をする。特に、この窒化チタン
あるいは金属チタンは窒化ケイ素粒子内部にも存在する
ため、この作用が強くはたらく。よって、破壊靭性の向
上と同時に高温強度も優れた焼結体が得られる。In silicon nitride-based ceramics containing titanium nitride or titanium metal in the second phase of grain boundaries and inside silicon nitride particles, when stress is applied to the sintered body and the sintered body breaks, cracks form in the titanium nitride or titanium metal. Since the particles are bent or branched, it increases fracture energy, improves fracture toughness, and prevents deterioration of strength at high temperatures. In particular, since this titanium nitride or metallic titanium also exists inside the silicon nitride particles, this effect is strong. Therefore, a sintered body with improved fracture toughness and excellent high-temperature strength can be obtained.
（実施例）
平均粒径１．０μ酸化イツトリウム（Ｙ２０ａ）、平均
粒径０．５μアルミナＵｎａｏａ）、平均粒径１．０μ
窒化アルミニウム（ＡｆｉＮ）、平均粒径０．５μ酸化
チタンおよび平均粒径０．６μ窒化チタンをそれぞれ表
に示す組成に選び、溶媒としてｎ−ブタノールを用いて
ゴムライニングボールミルにて約２４時間混合を行い、
参考例を含めて、１０種の原料粉末を調整した。(Example) Yttrium oxide (Y20a) with an average particle size of 1.0μ, average particle size of 0.5μ alumina (Unaoa), average particle size of 1.0μ
Aluminum nitride (AfiN), titanium oxide with an average particle size of 0.5μ, and titanium nitride with an average particle size of 0.6μ were selected as shown in the table, and mixed for about 24 hours in a rubber-lined ball mill using n-butanol as a solvent. conduct,
Ten types of raw material powders were prepared including reference examples.
原料粉末を１７８０℃、３００ｋｇ／ｄの条件で９０分
間ホットプレスした。また、原料粉末にステアリン酸（
粘結剤）を重量比で７％それぞれ添加配合し７００ｋｇ
／ｃｄの成形圧で長さ６０ｍｍ幅４０ｍ＋厚さ１０閣の
棒状成形体を得た。この成形体につき、まず７００℃で
加熱処理を施し、粘結剤を揮発除去後、窒素ガス雰囲気
下でそれぞれ表に示す温度で１２０分間常圧焼結を行い
、窒化ケイ素系セラミックス焼結体を得た。The raw material powder was hot pressed at 1780° C. and 300 kg/d for 90 minutes. In addition, stearic acid (
700 kg of 700 kg of 700 kg of 700 kg of each (binder) added by weight
A rod-shaped molded body having a length of 60 mm, a width of 40 m, and a thickness of 10 mm was obtained at a molding pressure of /cd. This molded body was first heat-treated at 700°C to remove the binder by volatilization, and then sintered under atmospheric pressure for 120 minutes at the temperatures shown in the table in a nitrogen gas atmosphere to form a silicon nitride ceramic sintered body. Obtained.
上記によって得た焼結体につき、抗折強度及び破壊靭性
値をそれぞれ測定した結果を併せて表に示した。The results of measuring the bending strength and fracture toughness of the sintered bodies obtained above are also shown in the table.
なお、抵折強度は３点曲げ強度試験によるもので試料サ
イズ３Ｘ４Ｘ４０ｎｍ、試験条件はクロスヘッドスピー
ド０ 、５ ｍｍ ／分、スパン３０閣、温度は常温及
び１２００℃とし各温度での測定は８回行いその平均値
で示した。また破壊靭性値（Ｋｚｃ）はＪＩＳＲ１６０
１に基ずきダイヤモンドカッターにて試料面中央部に幅
０．３ｍｍ深さ０．７５ｍｎのＵ溝をっけスパン３０ｍ
、 クロスヘッドスピード０．５ｍ／ｗｉｎの条件によ
り常温で実験し、次式に従って求めた。The bending strength was determined by a 3-point bending strength test. The sample size was 3 x 4 x 40 nm, the test conditions were a crosshead speed of 0, 5 mm/min, a span of 30 degrees, and the temperature was room temperature and 1200°C, and each temperature was measured 8 times. The results are shown as the average value. In addition, the fracture toughness value (Kzc) is JISR160
Based on 1, a U-groove with a width of 0.3 mm and a depth of 0.75 mm is cut in the center of the sample surface using a diamond cutter, and the span is 30 m.
, An experiment was conducted at room temperature under the conditions of a crosshead speed of 0.5 m/win, and was determined according to the following formula.
Ｋｘｃ＝ Ｙｃｒａ””
Ｙ：形状因子
０２曲げ強度
ａ：亀裂長さ
表より炭化ケイ素ウィスカーと添加物の重量割合が３０
％以内であれば常温、高温ともに強度が高く、破壊靭性
値も優れていることがわかる。Kxc= Ycra"" Y: Shape factor 02 Bending strength a: Crack length From the table, the weight ratio of silicon carbide whiskers and additives is 30
% or less, it can be seen that the strength is high both at room temperature and high temperature, and the fracture toughness value is also excellent.
［発明の効果〕
以上説明したように本発明の窒化ケイ素系セラミックス
は破壊靭性値、並びに高温強度がともにゝ優れたもので
ある。[Effects of the Invention] As explained above, the silicon nitride ceramic of the present invention has excellent fracture toughness and high-temperature strength.
以下余白Margin below
Claims (1)
ラミックスにおいて、添加物の反応により形成される焼
結体中の粒界第２相中および窒化ケイ素粒子の内部に２
〜３０重量％の窒化チタンあるいはチタン金属微粒子が
分散していることを特徴とする窒化ケイ素系セラミック
ス。In silicon nitride ceramics consisting of a silicon nitride-additive-based sintered body, 2 is present in the grain boundary second phase in the sintered body formed by the reaction of the additive and inside the silicon nitride particles.
A silicon nitride ceramic characterized by dispersing ~30% by weight of titanium nitride or titanium metal fine particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62154362A JP2573230B2 (en) | 1987-06-23 | 1987-06-23 | Silicon nitride ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62154362A JP2573230B2 (en) | 1987-06-23 | 1987-06-23 | Silicon nitride ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63319263A true JPS63319263A (en) | 1988-12-27 |
| JP2573230B2 JP2573230B2 (en) | 1997-01-22 |
Family
ID=15582498
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62154362A Expired - Lifetime JP2573230B2 (en) | 1987-06-23 | 1987-06-23 | Silicon nitride ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2573230B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0327894A (en) * | 1989-06-21 | 1991-02-06 | Denki Kagaku Kogyo Kk | Ceramics for constituting member of positioning pin |
| GB2249546A (en) * | 1990-10-08 | 1992-05-13 | Matsushita Electric Works Ltd | Ceramic - metal composites |
| JPH04202059A (en) * | 1990-11-30 | 1992-07-22 | Sumitomo Electric Ind Ltd | Silicon nitride-based composite sintered body |
| JPH04202058A (en) * | 1990-11-30 | 1992-07-22 | Sumitomo Electric Ind Ltd | Silicon nitride-based composite sintered body |
| EP1134204A1 (en) * | 2000-03-16 | 2001-09-19 | Kabushiki Kaisha Toshiba | Silicon nitride wear resistant member and manufacturing method thereof |
| US6784131B2 (en) | 2001-01-12 | 2004-08-31 | Kabushiki Kaisha Toshiba | Silicon nitride wear resistant member and method of manufacturing the member |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5874572A (en) * | 1982-07-30 | 1983-05-06 | 住友電気工業株式会社 | Plasticity working tool for copper and copper alloy |
| JPS58161975A (en) * | 1982-03-16 | 1983-09-26 | 日本特殊陶業株式会社 | Manufacture of silicon nitride sintered body |
| JPS5957963A (en) * | 1982-09-27 | 1984-04-03 | 日本特殊陶業株式会社 | Manufacture of nitride ceramic tool |
| JPS6117473A (en) * | 1985-05-17 | 1986-01-25 | 三菱マテリアル株式会社 | Silicon nitride base sintering material for cutting tool |
| JPS6172684A (en) * | 1984-09-18 | 1986-04-14 | 株式会社東芝 | High strength high abrasion resistance sliding member and manufacture |
| JPS63201063A (en) * | 1987-02-12 | 1988-08-19 | 日立金属株式会社 | Ceramic heater and manufacture |
-
1987
- 1987-06-23 JP JP62154362A patent/JP2573230B2/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58161975A (en) * | 1982-03-16 | 1983-09-26 | 日本特殊陶業株式会社 | Manufacture of silicon nitride sintered body |
| JPS5874572A (en) * | 1982-07-30 | 1983-05-06 | 住友電気工業株式会社 | Plasticity working tool for copper and copper alloy |
| JPS5957963A (en) * | 1982-09-27 | 1984-04-03 | 日本特殊陶業株式会社 | Manufacture of nitride ceramic tool |
| JPS6172684A (en) * | 1984-09-18 | 1986-04-14 | 株式会社東芝 | High strength high abrasion resistance sliding member and manufacture |
| JPS6117473A (en) * | 1985-05-17 | 1986-01-25 | 三菱マテリアル株式会社 | Silicon nitride base sintering material for cutting tool |
| JPS63201063A (en) * | 1987-02-12 | 1988-08-19 | 日立金属株式会社 | Ceramic heater and manufacture |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0327894A (en) * | 1989-06-21 | 1991-02-06 | Denki Kagaku Kogyo Kk | Ceramics for constituting member of positioning pin |
| GB2249546A (en) * | 1990-10-08 | 1992-05-13 | Matsushita Electric Works Ltd | Ceramic - metal composites |
| US5296301A (en) * | 1990-10-08 | 1994-03-22 | Matsushita Electric Works, Ltd. | Sintered ceramic-metal composite product and method of fabricating the same |
| US5389590A (en) * | 1990-10-08 | 1995-02-14 | Matsushita Electric Works, Ltd. | Method of fabricating a sintered ceramic composite |
| GB2249546B (en) * | 1990-10-08 | 1995-07-05 | Matsushita Electric Works Ltd | Sintered ceramic-metal composite product and method of fabricating the same |
| JPH04202059A (en) * | 1990-11-30 | 1992-07-22 | Sumitomo Electric Ind Ltd | Silicon nitride-based composite sintered body |
| JPH04202058A (en) * | 1990-11-30 | 1992-07-22 | Sumitomo Electric Ind Ltd | Silicon nitride-based composite sintered body |
| EP1134204A1 (en) * | 2000-03-16 | 2001-09-19 | Kabushiki Kaisha Toshiba | Silicon nitride wear resistant member and manufacturing method thereof |
| US6797660B2 (en) | 2000-03-16 | 2004-09-28 | Kabushiki Kaisha Toshiba | Silicon nitride wear resistant member and manufacturing method thereof |
| US6784131B2 (en) | 2001-01-12 | 2004-08-31 | Kabushiki Kaisha Toshiba | Silicon nitride wear resistant member and method of manufacturing the member |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2573230B2 (en) | 1997-01-22 |
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