JPS62278169A - Ceramic sintered body parts and manufacture - Google Patents
Ceramic sintered body parts and manufactureInfo
- Publication number
- JPS62278169A JPS62278169A JP61119287A JP11928786A JPS62278169A JP S62278169 A JPS62278169 A JP S62278169A JP 61119287 A JP61119287 A JP 61119287A JP 11928786 A JP11928786 A JP 11928786A JP S62278169 A JPS62278169 A JP S62278169A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- ceramic sintered
- silicon nitride
- silicon
- body part
- 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
- 239000000919 ceramic Substances 0.000 title claims description 45
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 24
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 9
- 239000006104 solid solution Substances 0.000 claims description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 7
- 230000003746 surface roughness Effects 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 150000004767 nitrides Chemical class 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- 230000000737 periodic effect Effects 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 150000001247 metal acetylides Chemical class 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 229910021332 silicide Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 150000003377 silicon compounds Chemical class 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910003178 Mo2C Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006378 damage Effects 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
- 238000001125 extrusion Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000003966 growth inhibitor Substances 0.000 description 1
- 239000008241 heterogeneous mixture Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- WHOPEPSOPUIRQQ-UHFFFAOYSA-N oxoaluminum Chemical compound O1[Al]O[Al]1 WHOPEPSOPUIRQQ-UHFFFAOYSA-N 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000004804 winding Methods 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】 ３、発明の詳細な説明 〔産業上の利用分野］ 本発明は、セラミックス焼結体部品に関し。[Detailed description of the invention] 3. Detailed description of the invention [Industrial application field] The present invention relates to ceramic sintered parts.
さらに詳しくは、セラミックス焼結体を塑性変形せしめ
ることによって得られた、例えば切削用エンドミル刃や
タービン用プロペラなどの複雑形状部品および皿バネや
コイルスプリングなどの弾性部品などとして有用なセラ
ミックス焼結体部品に関する。More specifically, ceramic sintered bodies are obtained by plastically deforming ceramic sintered bodies and are useful as complex-shaped parts such as cutting end mill blades and turbine propellers, as well as elastic parts such as disc springs and coil springs. Regarding parts.
［従来の技術１
セラミックス焼結体は、耐熱性、耐摩耗性ならびに耐食
性に優れた材料として各種工業分野で注目を集めている
。ところが、このセラミックス焼結体は極めて硬度が高
いため、その加工にあたっては、例えばダイヤモンド研
磨などにより目的の形状とすることが一般的であった。[Prior Art 1 Ceramic sintered bodies are attracting attention in various industrial fields as materials with excellent heat resistance, wear resistance, and corrosion resistance. However, since this ceramic sintered body has extremely high hardness, it is common to process it into a desired shape by, for example, diamond polishing.
したがって、大型のもの、あるいは複雑形状のものを製
造することは困難であり、また、製造コストの上昇を招
来するなどの加工上の問題がある。Therefore, it is difficult to manufacture large-sized ones or those with complicated shapes, and there are processing problems such as increased manufacturing costs.
さらに、また、セラミックス焼結体よりなる弾性部材の
製造もその加工上、強度上の問題が存在する故に困難で
あるとされている。Furthermore, it is said that manufacturing an elastic member made of a ceramic sintered body is difficult due to problems in processing and strength.
セラミックス焼結体のなかでも、とくに、窒化ケイ素（
Ｓｉ３Ｎａ）、炭化ケイ素（ＳｉＣ）などのケイ素化合
物系の焼結体は耐熱性、耐腐食性および高温強度に優れ
ていると同時に、他のセラミックス焼結体、例えばジル
コニア（Ｚ ｒｏ２）、アルミナ（Ａｌ２Ｏ２）などに
比べてはるかに高い耐熱衝撃性を備えているため、上記
したような部材への要請が高まっているだけに、かかる
加工上の問題は深刻なものとなっている。Among ceramic sintered bodies, silicon nitride (
Sintered bodies based on silicon compounds such as Si3Na) and silicon carbide (SiC) have excellent heat resistance, corrosion resistance, and high-temperature strength. Since it has much higher thermal shock resistance than materials such as Al2O2), the demand for the above-mentioned members is increasing, and such processing problems have become serious.
［発明が解決しようとする問題点〕
本発明は、従来のかかる問題を解消し、セラミックス焼
結体を塑性加工することによって得られた複雑形状もし
くは大型部品または弾性部品などのセラミックス焼結体
部品およびその製造方法の提供を目的とする。[Problems to be Solved by the Invention] The present invention solves the conventional problems and provides ceramic sintered body parts such as complex-shaped or large-sized parts or elastic parts obtained by plastic working of ceramic sintered bodies. and its manufacturing method.
［問題点を解決するための手段および作用］本発明者ら
は、上記目的を達成すべく、ケイ素化合物よりなる焼結
体に焦点を絞って鋭意研究を重ねる中で、窒化ケイ素を
含む２種以上のケイ素化合物が混合されてなる粒状晶の
異種混合物の焼結体、すなわち窒化ケイ素系セラミック
スに、特定の条件下で応力を加えると、異種化合物間の
、いわば「異相界面すべり現象」により焼結体が塑性変
形することを見出して本発明を完成するに到った。[Means and effects for solving the problem] In order to achieve the above object, the present inventors conducted extensive research focusing on sintered bodies made of silicon compounds, and found two types containing silicon nitride. When stress is applied under specific conditions to a sintered body of a heterogeneous mixture of granular crystals made by mixing the above-mentioned silicon compounds, that is, silicon nitride ceramics, sintering occurs due to the so-called "heterogeneous interface sliding phenomenon" between the different types of compounds. The present invention was completed by discovering that the aggregate undergoes plastic deformation.
すなわち、本発明のセラミックス焼結体部品は、窒化ケ
イ素を少なくとも５０体端％含有してなる窒化ケイ素系
セラミックス焼結体の塑性変形物よりなることを特徴と
し、その製造方法は、窒化ケイ素を少なくとも５０体端
％含有する窒化ケイ素系セラミックス焼結体を、非酸化
性雰囲気中、温度１４００℃以上、応力３０ ｋｇ／
ａｍ２以下、および歪速度１０−”／秒以下の条件で塑
性変形せしめることを特徴とする。That is, the ceramic sintered body part of the present invention is characterized by being made of a plastically deformed silicon nitride-based ceramic sintered body containing at least 50% silicon nitride, and the method for manufacturing the same includes silicon nitride. A silicon nitride-based ceramic sintered body containing at least 50% of the body mass was heated in a non-oxidizing atmosphere at a temperature of 1400°C or higher and under a stress of 30 kg/
It is characterized in that it is plastically deformed under conditions of am2 or less and a strain rate of 10-''/sec or less.
本発明のセラミックス焼結体部品は窒化ケイ素（Ｓ４３
Ｎａ）を少なくとも５０体端％含有する窒化ケイ素系セ
ラミックス焼結体を塑性変形せしめて得られるものであ
り、その種類、形状などはとくに限定されるものではな
い、すなわち、このような部品の具体例としては、切削
用エンドミル刃、タービン用プロペラ、食品用押出フィ
ーダー、油圧ポンプ用スクリュー、穀物搬送用ポンプス
クリュー、紡績用糸道、自動車ロータ、カッター、はさ
み、磁気テープ切断用スリッター、ヒーターなどの複雑
形状部品、および、板バネ、皿バネ、スプリングワッシ
ャーなどの弾性部品などをあげることができる。The ceramic sintered body part of the present invention is made of silicon nitride (S43
It is obtained by plastically deforming a silicon nitride ceramic sintered body containing at least 50% Na), and its type and shape are not particularly limited. Examples include end mill blades for cutting, propellers for turbines, extrusion feeders for food, hydraulic pump screws, grain conveying pump screws, yarn paths for spinning, automobile rotors, cutters, scissors, magnetic tape cutting slitters, heaters, etc. Examples include complex-shaped parts and elastic parts such as leaf springs, disc springs, and spring washers.
この窒化ケイ素系セラミックス焼結体は、少なくとも５
０体端％のＳｉ３Ｎ４とこれとは異種の粒状晶よりなる
化合物から構成されている。異種の化合物としてはとく
に限定されるものではないが、好適なものとして炭化ケ
イ素（ＳｉＣ）および炭窒化ケイ素（Ｓｔ（Ｃ，Ｎ））
のうち少なくとも１種をあげることができ、この場合、
ＳｆＣおよび／または５ｉ（Ｃ，Ｎ）の含有量が全体の
５０体積％未満であることが好ましい。This silicon nitride ceramic sintered body has at least 5
It is composed of a compound consisting of 0% Si3N4 and granular crystals different from this. Although the different types of compounds are not particularly limited, silicon carbide (SiC) and silicon carbonitride (St(C,N)) are preferred.
At least one of these can be mentioned; in this case,
It is preferable that the content of SfC and/or 5i(C,N) is less than 50% by volume of the total.
そして、このＳｉＣおよび／または５ｔ（Ｃ，Ｎ）の５
０体積％以下が、周期律表の■ａ、ＶａおよびＶＩａ族
元素の炭化物、窒化物、炭酸化物、酸窒化物、ケイ化物
もしくはこれらの相互固溶体により置換されていること
が焼結体の強度の向上並びに熱及び電気伝導性の向上と
いう点において好ましい、このような化合物もしくは相
互固溶体の具体例としては、Ｔｉｃ、ＺｒＣ，ＨｆＣ１
ＶＣ１ＮｂＣ，ＴａＣ，Ｃｒ３ ｃ２．Ｍｏ２Ｃ，ＷＣ
ｌ５ ｉＣ； ＴｉＮ、ＺｒＮ、ＨｆＮ、ＶＮ、ＮｂＮ
、ＴａＮ、ＣｒＮ、Ｓｉ３ Ｎａ ；ＴｆＯ１Ｔｉ０２
゜Ｚ ｒｏ２．ＨｆＯ□、Ｃ’ｒ２０３ 、Ｔａ２ｏｓ
、５ｉ０２ ；Ｔｉ （Ｃ，Ｎ）、Ｔｉ （Ｃ，
Ｏ）、Ｔｉ （Ｎ、Ｏ）、Ｔｉ （Ｃ，Ｎ、Ｏ）、
（Ｔｉ。Then, 5 of this SiC and/or 5t(C,N)
The strength of the sintered body is that 0% by volume or less is replaced by carbides, nitrides, carbonates, oxynitrides, silicides, or mutual solid solutions of elements of group ■a, Va, and VIa of the periodic table. Specific examples of such compounds or mutual solid solutions that are preferable from the viewpoint of improving thermal conductivity and improving thermal and electrical conductivity include Tic, ZrC, HfC1
VC1NbC, TaC, Cr3 c2. Mo2C, W.C.
l5 iC; TiN, ZrN, HfN, VN, NbN
, TaN, CrN, Si3Na; TfO1Ti02
゜Z ro2. HfO□, C'r203, Ta2os
, 5i02 ; Ti (C, N), Ti (C,
O), Ti (N, O), Ti (C, N, O),
(Ti.
Ｚ ｒ） （Ｃ、Ｎ）、（Ｔｉ 、Ｔａ）Ｃ１（Ｔｉ
。Z r) (C, N), (Ti, Ta) C1 (Ti
.
Ｎｂ）Ｃ１（Ｔｉ、Ｔａ、Ｗ）Ｃなどをあげることがで
きる。Nb)C1(Ti, Ta, W)C, etc. can be mentioned.
また、これらの化合物もしくは相互固溶体は単独で添加
しても２種以上を添加してもよいが、とくに、２種以上
の金属化合物が互いに固溶してなる固溶体の形で添加す
ると、焼結時に発生する気孔が減少するため焼結体の強
度の向上という点でさらに効果的である。In addition, these compounds or mutual solid solutions may be added alone or in combination of two or more types, but in particular, when two or more metal compounds are added in the form of a solid solution formed as a solid solution with each other, sintering This is more effective in terms of improving the strength of the sintered body because the pores that sometimes occur are reduced.
上記に加えて、本発明の窒化ケイ素系セラミックス焼結
体中には、さらに、酸化ケイ素、ならびに、周期律表の
Ｈａ、ｍａ、■族元素および希土類元素の酸化物、窒化
物およびこれらの相互固溶体から選ばれる少なくとも１
種を粒界相として含有せしめられていると、焼結体の強
度を高める上で効果的である。このような粒界相を構成
する化合物もしくは固溶体の具体例としては、例えば、
５ｉ０２．ＭｇＯ１Ｃａｂ、Ｓｃ２０３、Ｙ２０３ 、
Ｎｉｐ、Ｃｏｏ、Ｆｅｄ、Ｆｅ２ ｏ３、Ｆｅ３０４
、Ｌａ２０３ 、Ｃｅ２０３ 、Ｐｒ２ ｏ、、Ｎｄ２
０３．Ｓｍ２０３．Ｅｕ２０３．Ｄｙ２０３ 、。In addition to the above, the silicon nitride-based ceramic sintered body of the present invention further contains silicon oxide, oxides and nitrides of Ha, ma, Group II elements of the periodic table, and rare earth elements, and their interactions. At least one selected from solid solutions
Inclusion of seeds as a grain boundary phase is effective in increasing the strength of the sintered body. Specific examples of compounds or solid solutions constituting such a grain boundary phase include, for example,
5i02. MgO1Cab, Sc203, Y203,
Nip, Coo, Fed, Fe2 o3, Fe304
, La203 , Ce203 , Pr2 o, , Nd2
03. Sm203. Eu203. Dy203,.
Ｅｒ２ ｏ３ 、Ｔｂ２０３ 、Ｍｇ３ Ｎ２ 、Ｃａ
３ Ｎ２、ＳｃＮ、ＹＮ、ＣｅＮ、ＤｙＮ、Ｙｓ Ｆｅ
５ ｏＬ２、Ｎ ｉ Ｆｅ２０４ 、ＭｇＦ６２Ｑ４、
Ｉ、ａＦｅ０３などをあげることができる。この粒成長
抑制剤の含有量は、例えば焼結体全体の０．１〜７体積
％に設定することが好ましい。Er2 o3 , Tb203 , Mg3 N2 , Ca
3 N2, ScN, YN, CeN, DyN, Ys Fe
5 oL2, N i Fe204 , MgF62Q4,
I, aFe03, etc. can be mentioned. The content of this grain growth inhibitor is preferably set to, for example, 0.1 to 7% by volume of the entire sintered body.
さらに、本発明のセラミックス焼結体部品は、平均粒径
２−以下の粒状晶組織を有するものであることが好まし
く、また、この焼結体部品の表面の少なくとも一部は表
面粗さが６戸以下であることが好ましい。Furthermore, the ceramic sintered body part of the present invention preferably has a granular crystal structure with an average grain size of 2 or less, and at least a part of the surface of this sintered body part has a surface roughness of 6. It is preferable that the temperature is less than
つぎに、本発明のセラミックス焼結体部品の製造方法に
ついて説明する。Next, a method for manufacturing a ceramic sintered body component according to the present invention will be explained.
本発明の製造方法においては、まず、通常の焼結法を適
用して窒化ケイ素を少なくとも５０体積％含有する窒化
ケイ素系セラミックス焼結体を製造し、この窒化ケイ素
系セラミックス焼結体を所定条件下で塑性変形せしめる
。このとき、Ｓｉ３Ｎ４焼結体表面の少なくとも一部、
例えば、後述する塑性変形工程を経て製品化したときに
とくに平滑さが要求される面を研削または研磨して、前
述したようにその表面粗さを６μ以下としておくと、塑
性変形後にも、この平滑面がそのまま保持されるため、
とくに複雑形状の部品を製造する際に有利である。さら
に、この焼結体は平均粒径が２−以下の粒状結晶を有し
、また、その機械的強度、例えば曲げ強度が６０ ｋｇ
／ ｔａｒｓ２以上であることが好ましい。In the manufacturing method of the present invention, first, a silicon nitride ceramic sintered body containing at least 50% by volume of silicon nitride is manufactured by applying a normal sintering method, and the silicon nitride ceramic sintered body is sintered under predetermined conditions. It is plastically deformed at the bottom. At this time, at least a part of the surface of the Si3N4 sintered body,
For example, if a surface that requires particularly smoothness is ground or polished to a surface roughness of 6μ or less when the product is manufactured through the plastic deformation process described below, this surface roughness can be maintained even after plastic deformation. Because the smooth surface remains intact,
This is particularly advantageous when manufacturing parts with complex shapes. Furthermore, this sintered body has granular crystals with an average grain size of 2 or less, and its mechanical strength, for example, bending strength, is 60 kg.
/tars2 or more is preferable.
そして、続く塑性変形工程においては、まず。In the following plastic deformation process, first.
焼結体及び使用するモールドの酸化を防止するために、
Ａｒ、Ｎ２などの還元性雰囲気もしくは真空中で行なう
ことが必要である。また、変形温度は１４００℃以上で
あることが必要であり、この温度が１４００℃未満であ
る場合には応力印加状態でクラックが生じたり、破壊が
起こるため好ましくない、とくに、焼結体およびモール
ドの酸化防止と後述するモールドの強度の限界との２点
から、１４００〜１６５０℃の範囲に設定することが好
ましい、つぎに、変形応力は３０ｋｇ／ｌｌｌ１１２以
下に設定する。この応力が３０ ｋｇ／ ｍｍ２を超え
ると高価なモールドが破壊したり、焼結体にクラックが
生じるという不都合が生ずる。好ましくは１０ ｋｇ／
ｗｍ２以下である。さらに、歪速度は１０−３７秒以
下に設定する。１０−３／秒を超えると、焼結体は変形
せずに破壊してしまう、好ましくは１０゛Ｓ〜１０’／
秒である。これらの諸条件はそれぞれ独立した条件では
なく、互いに関連し合うものであるため、総括的な最適
値にそれぞれ設定することが好ましい。To prevent oxidation of the sintered body and the mold used,
It is necessary to carry out the process in a reducing atmosphere such as Ar or N2 or in vacuum. In addition, the deformation temperature must be 1400°C or higher; if this temperature is lower than 1400°C, cracks may occur or breakage may occur under stress, which is undesirable, especially for sintered bodies and molds. It is preferable to set the temperature in the range of 1400 to 1650° C. from the viewpoint of preventing oxidation and limiting the strength of the mold described later. Next, the deformation stress is set to 30 kg/ll112 or less. If this stress exceeds 30 kg/mm2, there will be problems such as destruction of the expensive mold or cracks in the sintered body. Preferably 10 kg/
wm2 or less. Further, the strain rate is set to 10-37 seconds or less. If the speed exceeds 10-3/sec, the sintered body will be destroyed without being deformed, preferably 10゛S~10'/sec.
Seconds. These conditions are not independent conditions, but are related to each other, so it is preferable to set each to an overall optimal value.
なお、かかる塑性変形工程に使用するモールドの材料と
しては、＃酸化性、耐摩耗性、耐圧強度に優れているも
のが好ましく、具体的には、黒鉛、Ｓｉ３Ｎ４．ＳｉＣ
などがあげられ、なかでもＳｉＣは好適である。The material for the mold used in this plastic deformation process is preferably one that has excellent oxidation resistance, wear resistance, and pressure resistance, and specifically, graphite, Si3N4. SiC
Among them, SiC is preferable.
［実施例］
実施例１
５６．５ｖｏ１％Ｓ ｉ３ Ｎ４−４０ｖａ１％５ｉＣ
−３ｖｏ１％Ｄｙ２０３−０ 、５ｖｏ１％ＭｇＯなる
組成を有するセラミックス焼結体を塑性加工することに
より第１図（Ｌ）および（ｂ）に示したようなスズリン
グワッシャー１を製造した。このスプリングワッシャー
１はねじれを伴った略Ｃ字状の形状であり、ねじれおよ
びスリット１ａによってスプリング特性が付与される。[Example] Example 1 56.5vo1%S i3 N4-40va1%5iC
A tin ring washer 1 as shown in FIGS. 1(L) and (b) was manufactured by plastically working a ceramic sintered body having a composition of -3vol%Dy203-0 and 5vol%MgO. This spring washer 1 has a substantially C-shaped shape with twist, and the twist and slit 1a provide spring characteristics.
すなわち、まず、略Ｃ字状のリング状セラミックス焼結
体を製造し１表面を研磨してその表面粗さを約５−とじ
、しかるのち、このセラミックス焼結体の上下方向から
応力を印加することによりねじれを付与した。このとき
の条件は、Ａｒ雰囲気中、温度１６００℃、応力５ ｋ
ｇ／ ｍｍ２．歪速度４×１０４／秒および変形時間３
時間にそれぞれ設定した。That is, first, a substantially C-shaped ring-shaped ceramic sintered body is manufactured, one surface is polished to a surface roughness of about 5-5, and then stress is applied from above and below to this ceramic sintered body. This gives it a twist. The conditions at this time were an Ar atmosphere, a temperature of 1600°C, and a stress of 5k.
g/mm2. Strain rate 4×104/sec and deformation time 3
Each time was set.
このようにして得られたスプリングワッシャー１は優れ
たバネ弾性を有し、１０００℃までは、抗折力値で最低
８０ ｋｇ／ ｍｍ２の強度を有し、耐熱性、耐酸化性
、耐薬品性に優れているとともに、耐熱衝撃性も極めて
良好であるため、特殊環境下、例えばヒートサイクル環
境下、高温腐食性環境下および放射線照射環境下などで
効果を発揮することが確認された。したがって、このス
プリングワッシャーは、とくに、耐海水性が要求される
船舶用の締結用部品として極めて有用である。The spring washer 1 thus obtained has excellent spring elasticity, has a transverse rupture strength of at least 80 kg/mm2 up to 1000°C, and has good heat resistance, oxidation resistance, and chemical resistance. In addition to being excellent in thermal shock resistance, it has been confirmed that it is effective under special environments, such as heat cycle environments, high-temperature corrosive environments, and radiation irradiation environments. Therefore, this spring washer is particularly useful as a fastening component for ships that requires seawater resistance.
実施例２
５７ｖｏ１％ Ｓ ｉ３ Ｎａ −２８ｖｏ１％
５ｉＣ−２ｖｏ１％ ５ｉ０２ −２ｖａ１％ ＣｅＯ
２−１ｖｏ１％ＭｇＯ−１０ｖｏ１％ＴｉＮなる組成の
セラミックス焼結体を塑性加工することにより第２図に
示したような皿バネ２を製造した。この皿バネ２は傾斜
面２ａおよび２ｂによってスプリング特性が付与される
。この皿バネ２を製造する際には、例えばこのバネの最
終形状に近い形状を有する治具、すなわちプレス型など
を用いて芒性変形せしめた。このときの条件は、Ｎ２雰
囲気中、温度１６５０℃、応力２０ ｋｇ／ ■２．歪
速度５×１０４／秒および変形吟間４時間にそれぞれ設
定した。Example 2 57vo1% Si3Na -28vo1%
5iC-2vo1% 5i02-2va1% CeO
A disc spring 2 as shown in FIG. 2 was manufactured by plastically working a ceramic sintered body having a composition of 2-1vol%MgO-10vol%TiN. This disc spring 2 is given spring characteristics by the inclined surfaces 2a and 2b. When manufacturing this disc spring 2, for example, a jig having a shape close to the final shape of this spring, ie, a press mold, etc., was used to cause the spring to undergo annular deformation. The conditions at this time were N2 atmosphere, temperature 1650°C, stress 20 kg/2. The strain rate was set at 5 x 104/sec and the deformation time was set at 4 hours.
このようにして得られた皿バネ２は、優れた弾性を有し
、１０００℃までは、抗折力値で最低８０ ｋｇ／ ａ
ｒ１１２の強度を有し、上記実施例１と同様に、耐熱性
、耐酸化性、＃薬品性に優れているとともに、耐熱衝撃
性も極めて高いものであった。The disc spring 2 thus obtained has excellent elasticity and has a transverse rupture strength of at least 80 kg/a up to 1000°C.
It had a strength of r112, and similarly to Example 1, it was excellent in heat resistance, oxidation resistance, and chemical resistance, and also had extremely high thermal shock resistance.
実施例３
７０ｖａ１％ Ｓ ｉ３ Ｎ４−２５ｖｏ１％ ＺｒＯ
２； ・２ ｖｏ１％Ｙ２０３−３ ｖｏ１％ Ｓ ｉ
０２ す６組成ヲ有し、直径３＋ｅｍφの棒状セラミ
ックス焼結体を作製し、その表面粗さが４−以下となる
ように研磨した。ついでこの棒状焼結体を溝付治具に、
Ａｒ雰囲気中、１６５０″Ｃ１応力１０ ｋｇ／ ｍｍ
２、歪速度５Ｘ１０４／秒および変形時間１０時間で巻
きつけてコイルスプリングを得た。このコイルスプリン
グは優れたバネ特性を示し、１０００℃まで抗折力値は
８０ ｋｇ／ ｍｔａ”を保持し、しかも、温度上昇に
伴う横弾性係数の劣化はみられなかった。Example 3 70va1% Si3 N4-25vo1% ZrO
2; ・2 vo1%Y203-3 vo1% Si
02 A rod-shaped ceramic sintered body having a composition of 6 and a diameter of 3+emφ was prepared and polished so that its surface roughness was 4- or less. Next, use this rod-shaped sintered body as a grooved jig.
In Ar atmosphere, 1650″C1 stress 10 kg/mm
2. A coil spring was obtained by winding at a strain rate of 5×10 4 /sec and a deformation time of 10 hours. This coil spring exhibited excellent spring characteristics, maintaining a transverse rupture force value of 80 kg/mta'' up to 1000°C, and no deterioration of the transverse elastic modulus accompanying temperature rise was observed.
さらに耐酸化性、＃腐食性、耐ヒートサイクル特性も良
好であるため、ヒートサイクル環境下、腐食あるいは放
射線環境下など、金属製バネの使用が不可能な環境下へ
の応用が可能である。Furthermore, since it has good oxidation resistance, #corrosion resistance, and heat cycle resistance properties, it can be applied to environments where metal springs cannot be used, such as heat cycle environments, corrosive or radiation environments.
［発明の効果］
以上の説明から明らかなように、本発明のセラミックス
焼結体部品は、２種以上のケイ素化合物を含む焼結体を
、その異種化合物間の異相界面すべり現象を利用して塑
性変形せしめることにより製造されたものであり、セラ
ミックスとしての優れた特性、すなわち、耐熱性、耐酸
化性、耐薬品性、さらには耐熱衝撃性を備えていると同
時に、機械的強度も充分高いため、高温雰囲気中、酸性
またはアルカリ性水溶液中、溶融塩浴中、あるいは放射
線環境下などの特殊環境下で使用することが可能である
。また、その製造方法もプレス加工や鍛造などによる圧
縮、引張り、曲げ、ねじり加工などを適用することがで
きるため簡便である。したがって、その工業的価値は極
めて大である。[Effects of the Invention] As is clear from the above description, the ceramic sintered body part of the present invention is produced by manufacturing a sintered body containing two or more types of silicon compounds by utilizing the sliding phenomenon between the different phase interfaces between the different types of compounds. It is manufactured by plastic deformation, and has excellent properties as a ceramic, such as heat resistance, oxidation resistance, chemical resistance, and thermal shock resistance, as well as sufficiently high mechanical strength. Therefore, it can be used in special environments such as high-temperature atmospheres, acidic or alkaline aqueous solutions, molten salt baths, and radiation environments. Further, the manufacturing method thereof is simple because compression, tension, bending, twisting, etc. by press working, forging, etc. can be applied. Therefore, its industrial value is extremely large.
第１図（ａ）、（ｂ）および第２図は本発明のセラミッ
クス焼結体部品の実施例を示し、第１図（ａ）はスプリ
ングワッシャーの正面図、第１図（ｂ）はその側面図、
第２図は皿バネの断面図である。
１・・・スプリングワッシャー、 ２・・・皿バネ（
ａ）（ｂ）
第２図1(a), 2(b) and 2 show examples of the ceramic sintered body parts of the present invention, FIG. 1(a) is a front view of a spring washer, and FIG. 1(b) is a front view of the spring washer. Side view,
FIG. 2 is a sectional view of the disc spring. 1...Spring washer, 2...Disc spring (
a) (b) Figure 2
Claims (8)
窒化ケイ素系セラミックス焼結体の塑性変形物よりなる
ことを特徴とするセラミックス焼結体部品。(1) A ceramic sintered body part comprising a plastically deformed silicon nitride ceramic sintered body containing at least 50% by volume of silicon nitride.
素および／または炭窒化ケイ素を５０体積％未満含有す
る特許請求の範囲第１項記載のセラミックス焼結体部品
。(2) The ceramic sintered body component according to claim 1, wherein the silicon nitride ceramic sintered body contains less than 50% by volume of silicon carbide and/or silicon carbonitride.
体積％以下が、周期律表のIVａ、ＶａおよびVIａ族元素
の炭化物、窒化物、炭酸化物、窒酸化物、ケイ化物もし
くはこれらの相互固溶体により置換されている特許請求
の範囲第２項記載のセラミックス焼結体部品。(3) 50% of the silicon carbide and/or silicon carbonitride
Claim 2, wherein not more than % by volume is replaced by carbides, nitrides, carbonates, nitrides, silicides, or mutual solid solutions of elements of groups IVa, Va, and VIa of the periodic table. Ceramic sintered parts.
化ケイ素ならびに周期律表のIIａ、IIIａ、VIII族元素
および希土類元素の酸化物、窒化物およびこれらの相互
固溶体から選ばれる少なくとも１種を粒界相として含有
する特許請求の範囲第１項または第２項に記載のセラミ
ックス焼結体部品。(4) The silicon nitride-based ceramic sintered body further contains at least one selected from silicon oxide, oxides, nitrides, and mutual solid solutions of elements of groups IIa, IIIa, and VIII of the periodic table, and rare earth elements. A ceramic sintered body component according to claim 1 or 2, which contains the interfacial phase.
の粒状晶組織を有する特許請求の範囲第１項、第２項ま
たは第４項記載のセラミックス焼結体部品。(5) The ceramic sintered body part according to claim 1, 2 or 4, wherein the ceramic sintered body part has a granular crystal structure with an average grain size of 2 μm or less.
面粗さが６μｍ以下である特許請求の範囲第１項、第２
項、第４項または第５項記載のセラミックス焼結体部品
。(6) Claims 1 and 2, wherein the surface roughness of at least a portion of the ceramic sintered body component is 6 μm or less.
5. Ceramic sintered body part according to item 4 or 5.
ケイ素系セラミックス焼結体を、非酸化性雰囲気中、温
度１４００℃以上、応力３０ｋｇ／ｍｍ＾２以下、およ
び歪速度１０＾−＾３／秒以下の条件で塑性変形せしめ
ることを特徴とするセラミックス焼結体部品の製造方法
。(7) A silicon nitride-based ceramic sintered body containing at least 50% by volume of silicon nitride is heated in a non-oxidizing atmosphere at a temperature of 1400°C or higher, a stress of 30 kg/mm^2 or lower, and a strain rate of 10^-^3/sec. A method for producing a ceramic sintered body part characterized by plastically deforming it under the following conditions.
クス焼結体を研削もしくは研磨する工程を含む特許請求
の範囲第７項記載のセラミックス焼結体部品の製造方法
。(8) The method for manufacturing a ceramic sintered body component according to claim 7, which includes a step of grinding or polishing the silicon nitride ceramic sintered body prior to the plastic deformation step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61119287A JPS62278169A (en) | 1986-05-26 | 1986-05-26 | Ceramic sintered body parts and manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61119287A JPS62278169A (en) | 1986-05-26 | 1986-05-26 | Ceramic sintered body parts and manufacture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62278169A true JPS62278169A (en) | 1987-12-03 |
| JPH0568427B2 JPH0568427B2 (en) | 1993-09-28 |
Family
ID=14757663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61119287A Granted JPS62278169A (en) | 1986-05-26 | 1986-05-26 | Ceramic sintered body parts and manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62278169A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252582A (en) * | 1987-12-24 | 1989-10-09 | Hitachi Metals Ltd | Electrically conductive ceramic sintered compact |
| JPH03197003A (en) * | 1989-12-26 | 1991-08-28 | Agency Of Ind Science & Technol | Formation of composite ceramic |
| US5244621A (en) * | 1989-12-26 | 1993-09-14 | Mitsubishi Gas Chemical Company, Inc. | Process for shaping ceramic composites |
| WO1996010546A1 (en) * | 1994-10-04 | 1996-04-11 | Japan Represented By Director General Of Agency Of Industrial Science And Technology | Silicon nitride ceramic and method of shaping the same |
| JP2012101981A (en) * | 2010-11-11 | 2012-05-31 | National Institute For Materials Science | Lithium silicon nitride and method of producing the same |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5433511A (en) * | 1977-08-19 | 1979-03-12 | Denki Kagaku Kogyo Kk | Method of making sintered body |
| US4184882A (en) * | 1976-03-25 | 1980-01-22 | Westinghouse Electric Corp. | Silicon nitride-silicon carbide composite material |
| JPS5864269A (en) * | 1981-10-12 | 1983-04-16 | 住友電気工業株式会社 | Silicon nitride sintered body and manufacture |
| JPS5864271A (en) * | 1981-10-12 | 1983-04-16 | 住友電気工業株式会社 | Silicon nitride sintered body |
| JPS5888187A (en) * | 1981-11-17 | 1983-05-26 | 科学技術庁無機材質研究所長 | Manufacture of minute silicon nitride sintered body |
| JPS5895655A (en) * | 1981-11-30 | 1983-06-07 | 株式会社東芝 | Manufacture of ceramic sintered body |
| JPS59199578A (en) * | 1983-04-22 | 1984-11-12 | 住友電気工業株式会社 | Silicon nitride sintered body |
| JPS6252191A (en) * | 1985-08-29 | 1987-03-06 | 東芝タンガロイ株式会社 | Plasticity process of ceramic sintered body |
-
1986
- 1986-05-26 JP JP61119287A patent/JPS62278169A/en active Granted
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4184882A (en) * | 1976-03-25 | 1980-01-22 | Westinghouse Electric Corp. | Silicon nitride-silicon carbide composite material |
| JPS5433511A (en) * | 1977-08-19 | 1979-03-12 | Denki Kagaku Kogyo Kk | Method of making sintered body |
| JPS5864269A (en) * | 1981-10-12 | 1983-04-16 | 住友電気工業株式会社 | Silicon nitride sintered body and manufacture |
| JPS5864271A (en) * | 1981-10-12 | 1983-04-16 | 住友電気工業株式会社 | Silicon nitride sintered body |
| JPS5888187A (en) * | 1981-11-17 | 1983-05-26 | 科学技術庁無機材質研究所長 | Manufacture of minute silicon nitride sintered body |
| JPS5895655A (en) * | 1981-11-30 | 1983-06-07 | 株式会社東芝 | Manufacture of ceramic sintered body |
| JPS59199578A (en) * | 1983-04-22 | 1984-11-12 | 住友電気工業株式会社 | Silicon nitride sintered body |
| JPS6252191A (en) * | 1985-08-29 | 1987-03-06 | 東芝タンガロイ株式会社 | Plasticity process of ceramic sintered body |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01252582A (en) * | 1987-12-24 | 1989-10-09 | Hitachi Metals Ltd | Electrically conductive ceramic sintered compact |
| JPH03197003A (en) * | 1989-12-26 | 1991-08-28 | Agency Of Ind Science & Technol | Formation of composite ceramic |
| US5244621A (en) * | 1989-12-26 | 1993-09-14 | Mitsubishi Gas Chemical Company, Inc. | Process for shaping ceramic composites |
| WO1996010546A1 (en) * | 1994-10-04 | 1996-04-11 | Japan Represented By Director General Of Agency Of Industrial Science And Technology | Silicon nitride ceramic and method of shaping the same |
| US5767026A (en) * | 1994-10-04 | 1998-06-16 | Agency Of Industrial Science And Technology | Silicon nitride ceramic and process for forming the same |
| CN1079385C (en) * | 1994-10-04 | 2002-02-20 | 工业技术院长代表的日本国 | Silicon nitride ceramic and method of shaping the same |
| JP2012101981A (en) * | 2010-11-11 | 2012-05-31 | National Institute For Materials Science | Lithium silicon nitride and method of producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0568427B2 (en) | 1993-09-28 |
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