JPS6241777A - Method of joining silicon carbide sintered body - Google Patents
Method of joining silicon carbide sintered bodyInfo
- Publication number
- JPS6241777A JPS6241777A JP60180697A JP18069785A JPS6241777A JP S6241777 A JPS6241777 A JP S6241777A JP 60180697 A JP60180697 A JP 60180697A JP 18069785 A JP18069785 A JP 18069785A JP S6241777 A JPS6241777 A JP S6241777A
- Authority
- JP
- Japan
- Prior art keywords
- bonding
- silicon carbide
- sintered body
- organosilicon polymer
- carbide sintered
- 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
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】
〔産業上の利用分野］
本発明は、セラミック部材特に炭化珪素焼結体の接合方
法に関する３
〔従来の技術〕
従来、炭化珪素焼結体を含む各種セラミックスの接合に
は、例えば特開昭５９−１８２２８１号公報に記載され
ているように、セラミックス自体より低融点の金属、酸
化物からなる接合材を接合部に介在させ、接合部に圧力
を加えながら加熱し接合材を溶融せしめて接合させ、さ
らに後処理として接合部分を加熱して接合材を基材に浸
透させて基材と接合部との異質性を軽減させて接合部と
基材との一体化を図る手段が採られていた。[Detailed Description of the Invention] [Industrial Field of Application] The present invention relates to a method for joining ceramic members, particularly sintered silicon carbide bodies. For example, as described in Japanese Unexamined Patent Publication No. 59-182281, a bonding material made of a metal or oxide with a lower melting point than the ceramic itself is interposed in the bonded part, and the bonded part is heated while applying pressure. The materials are melted and bonded, and as a post-treatment, the bonded area is heated to infiltrate the bonding material into the base material, reducing the heterogeneity between the base material and the bonded area, and integrating the bonded area and base material. Measures were taken to achieve this.
しかしながら、この接合材を用いる方法においては、い
かなる接合材の選択と浸透処理を施しても、接合基材と
接合部との完全な均質化は期待することはできず、接合
部分における基体との組織の相違に基づく機械的性質の
変動は避けることができない。However, in the method using this bonding material, no matter what kind of bonding material is selected and the penetration treatment is performed, complete homogenization of the bonding base material and the bonded area cannot be expected, and the Variations in mechanical properties due to differences in structure cannot be avoided.
本発明は、かかるセラミックス特に炭化珪素焼結体の接
合における均質化を達成することができる接合法を従供
することを目的とする。An object of the present invention is to provide a joining method that can achieve homogeneity in joining such ceramics, particularly sintered silicon carbide bodies.
本願出願人は、先に特開昭６０−１６８６９号公叩にお
いて、ＳｉとＣとから主骨格を構成する有機珪素ポリマ
ーを出発原料としてのＳｉＣ粒子に混合し、更にこれに
Ａｌ化合物を添加したとき高温度での高強ｌｔを示す微
細構造を有する焼結体が得られることを開示した。The applicant of the present application previously disclosed in Japanese Patent Application Laid-Open No. 60-16869 that an organic silicon polymer whose main skeleton is composed of Si and C was mixed with SiC particles as a starting material, and further an Al compound was added thereto. It was disclosed that a sintered body having a microstructure exhibiting high strength lt at high temperatures can be obtained.
本発明は１、かかる有機珪素ポリマーを出発原料とＬ７
て用いた炭化珪素焼結体はそれ自体優れた接合性を有し
、また有機珪素ポリマーの特性と焼結助剤の種類とを組
み合わせることによって、接合剤を用いなくとも高温で
も劣化しない優れた接合を比較的容易に得ることができ
るという新規な知見に基づいて完成したものである。The present invention provides 1, such an organosilicon polymer as a starting material and L7.
The silicon carbide sintered body used in this process has excellent bonding properties in itself, and by combining the characteristics of the organosilicon polymer and the type of sintering aid, it has an excellent bonding property that does not deteriorate even at high temperatures without using a bonding agent. This was completed based on the new finding that bonding can be achieved relatively easily.
これによって、複雑な形状を持った部材、製品であって
も、どの部分も均質であって、しかも優れた高温特性を
有する炭化珪素からなるものを得ることができる。As a result, even if the member or product has a complicated shape, it is possible to obtain a product made of silicon carbide that is homogeneous in every part and has excellent high-temperature properties.
本発明におけるＳｉとＣとから主骨格を構成する有機珪
素ポリマーとは、８００℃程度の温度で側鎖が殆ど分解
する５ｉ−Ｃ結合からなる非晶質に近い連続体を形成し
、さらに１０００℃以上では１０００オームストロング
以下の微細ＳｉＣを析出する化合物を意味する。In the present invention, the organosilicon polymer whose main skeleton is composed of Si and C forms a nearly amorphous continuum consisting of 5i-C bonds whose side chains almost decompose at a temperature of about 800°C. ℃ or higher means a compound that precipitates fine SiC of 1000 ohmstrong or less.
同有機珪素ポリマーの添加量は接合性の面からのみ言え
ば出発原料に対し３〜２０重量％である必要がある。３
重量％よりも少ないと添加剤の種類にもよるが、接合時
の加圧力を大きくしなければ十分な接合強度が得られず
、また２０重量％よりも多いと価格的に不利になるのみ
ならず、均一な組織を得るのが困難となり、接合体の強
度が劣化する。これらの点と焼結体自体の特性とのバラ
ンスの点からいって６〜１０重量％の範囲にあることが
望ましい。The amount of the organosilicon polymer added needs to be 3 to 20% by weight based on the starting material only from the viewpoint of bondability. 3
If it is less than 20% by weight, it will depend on the type of additive, but sufficient bonding strength will not be obtained unless the pressure during bonding is increased, and if it is more than 20% by weight, it will only be disadvantageous in terms of price. First, it becomes difficult to obtain a uniform structure, and the strength of the bonded body deteriorates. In view of the balance between these points and the properties of the sintered body itself, the content is preferably in the range of 6 to 10% by weight.
本発明においては、ＳｉＣ焼結体の焼結性と接合性を向
上させるために金属ＡβまたはＡｌ化合物を添加する。In the present invention, a metal Aβ or an Al compound is added to improve the sinterability and bondability of the SiC sintered body.
Ａ１化合物としては高温で比較的安定な非酸化物であれ
ば何でも良いが、取扱い上、金属Ａｌ１或いは窒化Ａｌ
、硼化１が望ましい。Any non-oxide compound that is relatively stable at high temperatures may be used as the A1 compound, but due to handling considerations, metal Al1 or nitride Al
, boric acid 1 are preferable.
特に金属Ａｆは価格的に有利で、窒化Ａ１は焼結体の特
性が最も良い。In particular, metal Af is advantageous in terms of cost, and nitride A1 has the best properties as a sintered body.
さらに、有機珪素ポリマーの種類と金属Ａ１またはＡ１
化合物との組合せを適宜選択することによって、接合の
ための有機珪素ポリマーとＡ１との挙動を調整できて接
合部の特性を向上することができる。即ち、有機珪素ポ
リマーとして、主骨格あるいは側鎖にＡｆを含んだ有機
珪素ポリマーを用い、Ａｅとして金属Ａｌを用いること
によって接合部の応力を最も低下させることができる。Furthermore, the type of organosilicon polymer and metal A1 or A1
By appropriately selecting the combination with the compound, the behavior of the organosilicon polymer for bonding and A1 can be adjusted, and the characteristics of the bonded portion can be improved. That is, by using an organosilicon polymer containing Af in its main skeleton or side chain as the organosilicon polymer and using metal Al as Ae, the stress at the joint can be reduced most.
また、有機珪素ポリマーとして、主骨格あるいは側鎖に
Ｂを含んだ有機珪素ポリマーを用い、Ａ１化合物として
窒化Ａ６を用いると接合部の高温強度が最も高い接合体
を得ることができる。Furthermore, if an organosilicon polymer containing B in its main skeleton or side chain is used as the organosilicon polymer, and A6 nitride is used as the A1 compound, a bonded body with the highest high temperature strength at the bonded portion can be obtained.
また、より均一で高強度の接合を行なうための焼結体を
製造するためには、通常の焼結温度より５０〜１００℃
低い温度で焼結するのが望ましい。これは、焼結体の接
合部分の界面焼結の駆動力を多く残存させ、また界面焼
結を促進するＡ１のような接合に有効な成分の揮散が抑
制されるためと考えられる。但し、焼結体自体の密度が
若干低下し、マトリックスの強度も低下するので、気密
性を要求される部材の製造には通常の焼結体を使用する
こともできる。In addition, in order to produce a sintered body for more uniform and high-strength bonding, it is necessary to increase the temperature by 50 to 100 degrees
It is desirable to sinter at low temperatures. This is thought to be because a large amount of the driving force for interfacial sintering remains in the bonded portion of the sintered body, and the volatilization of components effective for bonding, such as A1, which promotes interfacial sintering, is suppressed. However, since the density of the sintered body itself is slightly lowered and the strength of the matrix is also lowered, a normal sintered body can also be used for producing members that require airtightness.
高温での強力な接合状態を実現するためには、接合処理
のための雰囲気としては非酸化性あるいは還元性雰囲気
が適しており、特に１トール以下の真空雰囲気が最も適
している。空気中の処理によって得た接合部は、常温で
の強度は良好であるが、高温での接合強度は劣化する。In order to realize a strong bonding state at high temperatures, a non-oxidizing or reducing atmosphere is suitable as the atmosphere for the bonding process, and in particular, a vacuum atmosphere of 1 Torr or less is most suitable. The joint obtained by the treatment in air has good strength at room temperature, but the joint strength at high temperature deteriorates.
接合温度としては、１０００〜２４００℃の範囲が適し
ており、１０００℃よりも低いと拡散過程を励起できな
いので接合状態を得ることができず、２４００℃を超え
ると接合母体の特性が劣化する。A suitable bonding temperature is in the range of 1000 to 2400°C; if it is lower than 1000°C, the diffusion process cannot be excited and a bonded state cannot be obtained, and if it exceeds 2400°C, the properties of the bonded matrix will deteriorate.
接合のための加圧力は１００ｋｇ／ｃｊ以上が必要でこ
れより低いと接合しない。最適な接合は加圧力が１５０
０ｋｇ／ｃ＋ｄ以上の圧力で得られるが、加圧力が５０
００ｋｇ／ｃａｌを超えると接合部にチッピング等の欠
陥が生し易く、設備費も増大する。The pressure for bonding must be 100 kg/cj or more; if it is lower than this, bonding will not occur. The optimal bonding force is 150
It can be obtained at a pressure of 0 kg/c+d or more, but if the applied pressure is 50
If it exceeds 0.00 kg/cal, defects such as chipping are likely to occur in the joint, and equipment costs will increase.
平均粒径０．４μｍのα−５ｉＣ粉末１００重量部に対
して、有機珪素ポリマー７重量部を加え、溶媒としてヘ
キサンを７００重量部加えて、ボールミルで１４時間混
合したのち、ヘキサンを除去乾燥し、更に粉砕篩い分け
し、有機珪素ポリマーで表面被覆されたＳｉＣ粉末を得
た。To 100 parts by weight of α-5iC powder with an average particle size of 0.4 μm, 7 parts by weight of an organosilicon polymer was added, and 700 parts by weight of hexane was added as a solvent. After mixing in a ball mill for 14 hours, the hexane was removed and dried. The powder was further crushed and sieved to obtain SiC powder whose surface was coated with an organic silicon polymer.
この有機珪素ポリマーを被覆したＳｉＣ粉末１００重量
部に対してノボラック型フェノール樹脂５．７重量部、
平均粒径５ Ｉ７ ｍのＡＮ粉末０．７重量部、ヘキサ
メチレンテトラミン０．６重量部、平均粒径２μｍのＡ
ＩＮ粉末１．５重量部からなる配合物をエタノールを分
散剤として混合し、乾燥、粉砕、篩い分けして３７μｍ
以丁の成形用粉末を得た。5.7 parts by weight of novolac type phenolic resin for 100 parts by weight of SiC powder coated with this organosilicon polymer;
0.7 parts by weight of AN powder with an average particle size of 5 I7 m, 0.6 parts by weight of hexamethylenetetramine, A with an average particle size of 2 μm
A formulation consisting of 1.5 parts by weight of IN powder was mixed with ethanol as a dispersant, dried, crushed, and sieved to 37 μm.
A powder for molding was obtained.
この成形用粉末を１４００ ｋｇ／ｃｕｔの圧力でラバ
ープレスして２０ Ｘ １０ Ｘ ５０１１＋１１の圧
粉体を得、これをＡｒ雰囲気丁で、２２００℃で６０分
間保持した。This molding powder was rubber pressed at a pressure of 1400 kg/cut to obtain a green compact of 20×10×5011+11, which was held at 2200° C. for 60 minutes in an Ar atmosphere.
この焼結体の２個の試料の平滑な面を密着させ、２００
０１ｔｇ／ｃＩＩｌの圧力で加圧しつつ真空中で１７０
０℃まで加熱し、６０分保持した。炉冷後、試料を取出
し接合強度を測定したところ、４０００Ｊ ／ｅ−の強
度を示し、１５００℃まで強度劣化をおこさなかった。The smooth surfaces of the two samples of this sintered body were brought into close contact, and
170 in vacuum while pressurizing at a pressure of 0.1 tg/cIIl.
It was heated to 0°C and held for 60 minutes. After cooling in the furnace, the sample was taken out and the bonding strength was measured, and it showed a strength of 4000 J/e-, with no strength deterioration up to 1500°C.
〔発明の効果］
本発明によって、基体の炭化珪素焼結体と全く同質の接
合部を有する部材を製造できるので、高温ガス・タービ
ン・ロータのような大型部材を一体の焼結体として製造
する必要がなく、しかも接合で得た任意の形状の構造体
も、構造体全体を単−Ｍｉｍ体とすることが可能である
。[Effects of the Invention] According to the present invention, it is possible to manufacture a member having a joint portion that is completely the same as that of the silicon carbide sintered body of the base body, so that a large member such as a high-temperature gas turbine rotor can be manufactured as an integrated sintered body. Even if the structure is not necessary and has an arbitrary shape obtained by bonding, the entire structure can be made into a single Mim body.
しかも、接合に際しては、従来の接合とは異なり接合面
は必ずしも平坦である必要はなく、接合時の加圧力を増
大すれば、接合面の多少の凹凸は接合後の特性に影響を
与えることはない。Moreover, unlike conventional bonding, the bonding surfaces do not necessarily have to be flat, and if the pressure applied during bonding is increased, slight irregularities on the bonding surfaces will not affect the properties after bonding. do not have.
Claims (1)
珪素ポリマーとを含有してなる出発原料に、焼結助剤と
してＡｌ化合物と必要に応じて有機質結合剤とを添加し
た混合物の成形体を、不活性雰囲気中で２０５０〜２３
５０℃の温度で焼結して得た焼結体同士を、１００〜５
０００ｋｇ／ｃｍ＾２の圧力で密着させつつ真空中で１
０００〜２４００℃に加熱することを特徴とする炭化珪
素焼結体の接合方法。1. A mixture obtained by adding an Al compound as a sintering aid and an organic binder as necessary to a starting material containing silicon carbide powder and an organosilicon polymer whose main skeleton is mainly composed of Si and C. The molded body is heated to 2050-23 in an inert atmosphere.
The sintered bodies obtained by sintering at a temperature of 50°C are
1 in vacuum while adhering under a pressure of 000 kg/cm^2
A method for joining silicon carbide sintered bodies, the method comprising heating to 000 to 2400°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60180697A JPS6241777A (en) | 1985-08-16 | 1985-08-16 | Method of joining silicon carbide sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60180697A JPS6241777A (en) | 1985-08-16 | 1985-08-16 | Method of joining silicon carbide sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6241777A true JPS6241777A (en) | 1987-02-23 |
Family
ID=16087725
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60180697A Pending JPS6241777A (en) | 1985-08-16 | 1985-08-16 | Method of joining silicon carbide sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6241777A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010155241A (en) * | 1997-07-25 | 2010-07-15 | Centre National De La Recherche Scientifique (Cnrs) | Silicon carbide foam with high specific surface area and improved mechanical properties |
-
1985
- 1985-08-16 JP JP60180697A patent/JPS6241777A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010155241A (en) * | 1997-07-25 | 2010-07-15 | Centre National De La Recherche Scientifique (Cnrs) | Silicon carbide foam with high specific surface area and improved mechanical properties |
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