JPS59199578A - Silicon nitride sintered body - Google Patents
Silicon nitride sintered bodyInfo
- Publication number
- JPS59199578A JPS59199578A JP58071776A JP7177683A JPS59199578A JP S59199578 A JPS59199578 A JP S59199578A JP 58071776 A JP58071776 A JP 58071776A JP 7177683 A JP7177683 A JP 7177683A JP S59199578 A JPS59199578 A JP S59199578A
- Authority
- JP
- Japan
- Prior art keywords
- silicon nitride
- sintered body
- nitride sintered
- sintering
- density
- 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.)
- Pending
Links
- 229910052581 Si3N4 Inorganic materials 0.000 title claims description 13
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims description 13
- 230000000737 periodic effect Effects 0.000 claims description 3
- 150000001247 metal acetylides Chemical class 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims 1
- 238000005245 sintering Methods 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- Ceramic Products (AREA)
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】
（イ）技術分野
本発明は高温強度を向上させた窒化ケイ素セラミック焼
結体に関するものである。DETAILED DESCRIPTION OF THE INVENTION (a) Technical Field The present invention relates to a silicon nitride ceramic sintered body with improved high-temperature strength.
（ロ）技術の背景
窒化ケイ素の焼結体の高温特性を向上させるため、各種
焼結助剤の検荊がなされている。なかでもＹ２Ｃ１＋
−／ｕ２０３系添加物よりなる 窒化ケイ素焼結体は高
温強度の高いものが得られることでよく知られている。(b) Background of the technology In order to improve the high-temperature properties of silicon nitride sintered bodies, various sintering aids have been tested. Especially Y2C1+
It is well known that silicon nitride sintered bodies made of -/u203-based additives have high high-temperature strength.
しかしながら破壊靭性値が低いことや８［］ ０ ＝Ｃ
−１０００′ｃの温度において強度低下が起る等の問題
がある。そこで現在Ｍ２Ｏ３を添加していない焼結体の
開発が世界各国で進められている。なかでもＹ２Ｏ３お
よびＬａ系の酸化物系の添加は有効であるが、焼結性が
良くないＱ−ｆおよび８００°Ｃ〜１０００°Ｃの耐酸
化性が悪いＩＪＦ等の欠点がありいまだＹ２Ｏ３やＬａ
系の酸化物添加ではホットプレス法、雰囲気加圧焼結、
熱間静水圧加圧（ＨＩＰ）による微密化焼結の検剃がさ
れている。おそらくは１．Ω２０３− Ｙ２Ｏ３系焼結
助剤を用いた場合には、その粒界層の性質により８００
°Ｃ〜１００口°Ｃにおける耐酸化性が劣ること、また
Ｙ２Ｏ３またはＬａ系酸化物を添加した場合には高密度
なものは高温強度は高いものの通常の焼結方法では窒化
ケイ素焼結体の密度が充分に」二らないため様々な手法
を用いて密度向」二の努力がなされている。充分に密度
が高くなって、いない場合には、窒化ケイ素β］ε結体
中の空孔部より酸化が起り耐久・ビ１には劣る。密度向
」二のためのいずれの方法においても、製ノ告経費か高
くなり安（市に製造する方法が待ち望まれていた。However, the fracture toughness value is low and 8 [ ] 0 = C
There are problems such as a decrease in strength at a temperature of -1000'c. Therefore, the development of sintered bodies to which M2O3 is not added is currently underway in various countries around the world. Among them, the addition of Y2O3 and La-based oxides is effective, but there are still drawbacks such as Q-f, which has poor sinterability, and IJF, which has poor oxidation resistance at 800°C to 1000°C. La
Hot press method, atmosphere pressure sintering,
Microdensity sintering by hot isostatic pressing (HIP) has been inspected. Probably 1. Ω203- When Y2O3-based sintering aid is used, the resistance is 800 due to the properties of the grain boundary layer.
The oxidation resistance between °C and 100°C is poor, and when Y2O3 or La-based oxides are added, high-density products have high high-temperature strength, but silicon nitride sintered bodies cannot be produced using normal sintering methods. Since the density is not sufficiently reduced, efforts are being made to increase the density using various methods. If the density is sufficiently high, oxidation occurs from the pores in the silicon nitride β]ε structure, resulting in poor durability. In either method, the production cost would be high, and a method for producing the product in the city would be eagerly awaited.
（ハ）発明の開示
本発明は以上述べた問題点を解決した焼結体を提供する
ものである。その特徴は添加物として耐酸化性、焼結性
をともに向」ニさせる事ができる事を特徴としたもので
ある。本発明者は、Ｙ２Ｏ５系やＬａ系の酸化物の欠点
を解消するため、各種炭化物、窒化物、酸化物を添加し
た系を鋭意検討した結果本発明が得られた。即ち、Ｙ２
Ｏ６およびＬａ系元素の酸化物の１種以」二〇、 １〜
２０重量％およびＴｉ 、 Ｔａ 、 Ｗ等の周期律表
ＩＶａ、Ｖａ、ＶＩａ族元素の炭化物の１種以１［］、
０１〜３０重量％残部窒化ケイ素の組成にする事により
、焼結性が向上すると共（０耐酸化性も向上する焼結体
が得られたのである。(C) Disclosure of the Invention The present invention provides a sintered body that solves the above-mentioned problems. Its characteristic feature is that it can improve both oxidation resistance and sinterability as an additive. In order to eliminate the drawbacks of Y2O5-based and La-based oxides, the present inventors have intensively studied systems to which various carbides, nitrides, and oxides are added, and as a result, the present invention was obtained. That is, Y2
One or more oxides of O6 and La-based elements"20, 1-
20% by weight and at least one carbide of group IVa, Va, VIa elements of the periodic table such as Ti, Ta, W, etc.
By adjusting the composition to 0.01 to 30% by weight with the remainder being silicon nitride, a sintered body with improved sinterability (0) and improved oxidation resistance was obtained.
Ｙ２Ｏ３およびＬａ系の酸化物は０１重量％米満では、
炭化物の添加によっても焼結が進みにくく、２０重１１
（％をこえると、かえって炭化物の添加効果が少なくな
る。炭化物の添加は０．０１％米満では効果が少なく、
６０重量％をこえると今度は焼結体特性を下げる。この
ため」二記の範囲のものが有効である。本願発明の第１
の特徴は、Ｔｉ、Ｔａ、Ｗ等の周期律表の第１Ｖａ、Ｖ
ａ、Ｖｉａ族元素の炭化物を添加することにより容易に
高密度な窒化ケイ素焼結体を得ることができる点にある
。ここでいう容易にとは公知の焼結方法において従来の
Ｙ２Ｏ３およびＬａ系酸化物単独に比較して、高密度に
なることを意味し、例えばＨＩＰホットプレス等の加圧
焼結を組合わせても本発明の効果を得ることができる。Y2O3 and La-based oxides are 01% by weight in US meter,
Even with the addition of carbide, sintering does not progress easily, and the 20 weight 11
(If it exceeds 0.01%, the effect of adding carbide will actually decrease. Addition of carbide has little effect at 0.01% USM,
If it exceeds 60% by weight, the properties of the sintered body will deteriorate. For this reason, the scope specified in item 2 is valid. First of the claimed invention
The characteristics of Ti, Ta, W, etc. are the first Va and V of the periodic table.
A. By adding a carbide of a Via group element, a high-density silicon nitride sintered body can be easily obtained. Here, "easily" means that a known sintering method can achieve higher density than conventional Y2O3 and La-based oxides alone, for example, by combining pressure sintering such as HIP hot press. Also, the effects of the present invention can be obtained.
本願発明の第２の特徴は、公知の焼結助剤系以上の高温
強度を得ることができる点にある。通常の概念では、易
焼結性の焼結体はｌｉ’Ｑ温強度は劣ると考えられてい
たにもがかわらず、本発明では、比較的容易に密度向上
かでき、しかも高温強度は公知のもの以上の特性を示す
という驚くべき事実を発見したものである。特に構造材
料として注１・１されている窒化ケイ素焼結体における
高温特性の耐久性の向上は不可欠の検Ｓ」項１−１であ
った。本発明により高密度な焼結体を得ることができ、
内部からの酸化劣化等が起りにくく耐久性に富む材料を
開発することができた効果は極めて大きい。本発明の組
み合わせにより焼結ｉｊｌ：、耐酸化性が向」二する原
因については、明らかではないが、添加系の粒界層が焼
結進行と共に変化し、焼結時には焼結しやすく焼結体に
なると高温特性の良好な粒界層に変質していく事による
ものと考えられる。窒化ケイ素の結晶（１１１￥造はα
、Ｂいずれでも効果ある。次に実施例によって説明する
。The second feature of the present invention is that it is possible to obtain high-temperature strength higher than that of known sintering aid systems. Despite the conventional concept that easily sinterable sintered bodies are thought to have inferior li'Q temperature strength, in the present invention, the density can be increased relatively easily, and the high temperature strength is known. They discovered the surprising fact that they exhibit properties superior to those of . In particular, improvement of the durability of high-temperature properties of silicon nitride sintered bodies, which are mentioned in Note 1.1 as a structural material, is essential for the inspection S section 1-1. According to the present invention, a high-density sintered body can be obtained,
The effect of being able to develop a material that is highly durable and resistant to internal oxidative deterioration is extremely significant. The reason why the combination of the present invention improves sintering resistance and oxidation resistance is not clear, but the grain boundary layer of the additive system changes as sintering progresses, making it easier to sinter during sintering. This is thought to be due to the fact that when it becomes a solid grain, it transforms into a grain boundary layer with good high-temperature properties. Silicon nitride crystal (111 yen is α
, B are both effective. Next, an example will be explained.
に）実施例
α型を９０％以上含有する窒化ケイ素に次表（第１表）
に示すように各種添加物組成を混合させ、成形し１９６
０°ｃ ４ Ｑａｔｒｎ Ｎ２１時間焼結させた。2) Examples of silicon nitride containing 90% or more of α type
Mix various additive compositions and mold as shown in 196
Sintered at 0°C 4 Qatrn N for 21 hours.
そして焼結体の特性を評価した。評価項目は、密度、常
温強度、高温強度である。Then, the properties of the sintered body were evaluated. The evaluation items are density, room temperature strength, and high temperature strength.
第 １ 表
第１表が示すように本発明の組成の焼結体は、密度耐熱
強度の向上したものである事がわかる。Table 1 As shown in Table 1, it can be seen that the sintered body having the composition of the present invention has improved density heat resistance strength.
代理人 弁理士 」二 代 哲 司Agent Patent Attorney 2nd generation Tetsuji
Claims (1)
種以、Ｊ二０．１〜２０重量％および周期律表の第■ａ
、Ｖａ、■ａ族元索の炭化物の１種以上０．０１〜６０
重量％残部窒化ケイ素からなることを特徴とする窒化ケ
イ素焼結体(2) Yttrium oxide and oxides of La-based elements 1
Species, J2 0.1 to 20% by weight and Periodic Table ■a
, Va, ■ One or more types of carbides of Group A 0.01 to 60
A silicon nitride sintered body characterized in that the balance by weight is silicon nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58071776A JPS59199578A (en) | 1983-04-22 | 1983-04-22 | Silicon nitride sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58071776A JPS59199578A (en) | 1983-04-22 | 1983-04-22 | Silicon nitride sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS59199578A true JPS59199578A (en) | 1984-11-12 |
Family
ID=13470299
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58071776A Pending JPS59199578A (en) | 1983-04-22 | 1983-04-22 | Silicon nitride sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59199578A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62278169A (en) * | 1986-05-26 | 1987-12-03 | 東芝タンガロイ株式会社 | Ceramic sintered body parts and manufacture |
| US4810678A (en) * | 1986-11-10 | 1989-03-07 | Nissan Motor Co., Ltd. | Gas pressure sintering of silicon nitride with addition of rare earth oxides |
| JPH03218972A (en) * | 1988-12-16 | 1991-09-26 | Ngk Spark Plug Co Ltd | Silicon nitride-based sintered body |
| JPH0426553A (en) * | 1990-05-17 | 1992-01-29 | Ngk Insulators Ltd | Silicon nitride sintered compact having thermal shock resistance and its production |
-
1983
- 1983-04-22 JP JP58071776A patent/JPS59199578A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62278169A (en) * | 1986-05-26 | 1987-12-03 | 東芝タンガロイ株式会社 | Ceramic sintered body parts and manufacture |
| JPH0568427B2 (en) * | 1986-05-26 | 1993-09-28 | Toshiba Tungaloy Co Ltd | |
| US4810678A (en) * | 1986-11-10 | 1989-03-07 | Nissan Motor Co., Ltd. | Gas pressure sintering of silicon nitride with addition of rare earth oxides |
| JPH03218972A (en) * | 1988-12-16 | 1991-09-26 | Ngk Spark Plug Co Ltd | Silicon nitride-based sintered body |
| JPH0426553A (en) * | 1990-05-17 | 1992-01-29 | Ngk Insulators Ltd | Silicon nitride sintered compact having thermal shock resistance and its production |
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