JPH01317134A - Glass composition for bonding silicon carbide sintered form - Google Patents
Glass composition for bonding silicon carbide sintered formInfo
- Publication number
- JPH01317134A JPH01317134A JP22980387A JP22980387A JPH01317134A JP H01317134 A JPH01317134 A JP H01317134A JP 22980387 A JP22980387 A JP 22980387A JP 22980387 A JP22980387 A JP 22980387A JP H01317134 A JPH01317134 A JP H01317134A
- Authority
- JP
- Japan
- Prior art keywords
- bonding
- silicon carbide
- weight
- glass
- glass composition
- 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
- 239000011521 glass Substances 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 title claims abstract description 17
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 21
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 3
- 229910011255 B2O3 Inorganic materials 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract description 3
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 238000005238 degreasing Methods 0.000 abstract 1
- 235000011837 pasties Nutrition 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 12
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は炭素珪素焼結体同志を接合させるガラス組成の
接合材に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a bonding material having a glass composition for bonding carbon-silicon sintered bodies together.
炭化珪素焼結体は高温構造材として期待されている。そ
れは熱伝導率か大きく、耐熱強度か高く、同時に耐摩耗
性、耐食性かあるからである。Silicon carbide sintered bodies are expected to be used as high-temperature structural materials. This is because it has high thermal conductivity, high heat resistance strength, and at the same time wear resistance and corrosion resistance.
しかし用途としてガスターヒンの内燃機関やロータ、高
精泥機械部品のように形状、寸法、精度なとの要求か高
い複雑形状な構造物の場合は予しめ一体形状て製作する
ことか難しい。このため単純形状の部品を作っておいて
、それらを接着して複雑な形状の構造体に仕上げること
か考えられる。However, in the case of complex-shaped structures that require high requirements for shape, size, and precision, such as internal combustion engines, rotors, and high-refined mud machine parts, it is difficult to manufacture them in one piece in advance. For this reason, one idea would be to make parts with simple shapes and then glue them together to create a structure with a complex shape.
この意味において接合技術か重要視されるようになって
きた。In this sense, bonding technology has come to be viewed as important.
この炭化珪素焼結体同志を接合する方法には珪酸アルカ
リ系、リン酸塩系、シリカツル系等の無機接着剤かある
か、この方法は接合温度か１００〜４００°Ｃと低く気
密性も悪く、強度、耐熱性も十分てない欠点かあった。Is there a method for joining these sintered silicon carbide bodies together using an inorganic adhesive such as an alkali silicate adhesive, a phosphate adhesive, or a silica vine adhesive? However, it also had the disadvantage of not having sufficient strength and heat resistance.
本発明の目的は炭化珪素焼結体同志を接合するために、
接合界面に気泡や熱膨張係数の差異などによる亀裂の生
しない接合強度か大である接合材を提供することにある
。The purpose of the present invention is to join silicon carbide sintered bodies together,
The object of the present invention is to provide a bonding material that has high bonding strength and does not cause cracks due to bubbles or differences in thermal expansion coefficients at the bonding interface.
（問題点を解決するための手段）
本件の発明者は、上記の問題点を解決するために比較的
低い共融点を持ち炭化珪素焼結体接合面に気泡、亀裂か
生しない酸化物ツルターガラスについて鋭意研究を行っ
た結果、上記の目的に適う接合用ガラス組成物を見出し
、本件発明を完成させるに至った。(Means for Solving the Problems) In order to solve the above problems, the inventor of the present invention has developed an oxide sulter glass that has a relatively low eutectic point and does not generate bubbles or cracks on the bonded surface of silicon carbide sintered bodies. As a result of extensive research, we have discovered a bonding glass composition that meets the above objectives, and have completed the present invention.
すなわち本件発明の要旨は、炭化珪素焼結体同志を接合
させるガラス組成てあって５ｉ０２４０〜６０重量％、
８０２０〜３０重量％、Ａｌ２０３９〜２０重量％、Ｃ
ａ０ ３〜１５重量％、Ｚｒ０２０〜３重量％よりなる
ことを特徴とする炭化珪素焼結体の接合ガラス組成物に
ある。That is, the gist of the present invention is that the glass composition for bonding the silicon carbide sintered bodies together contains 5i0240 to 60% by weight,
8020-30% by weight, Al2039-20% by weight, C
A bonded glass composition of a silicon carbide sintered body characterized by comprising 3 to 15% by weight of a0 and 20 to 3% by weight of Zr0.
前記の組成の限定理由を説明するとＳｉＯ□の含有量は
ガラスの熱膨張係数を炭化珪素の熱膨張係数に近い値と
するためには４０重量％以上とすることか必要てあり、
又ガラス溶解温度を１４５０°Ｃ以下とするためには６
０重量％以下とすることか必要である。ＣａＯはガラス
溶解時の融液の粘度を低下させ均質なガラスを製造する
ために不可欠てあり ３重量％未満ては粘度の低下か不
十分てあり、１５重量％を越える場合には熱膨張係数か
炭化珪素焼結体のそれより大きくなる。Ａｌ２Ｏ３の量
は９重量％未満ては耐湿性か劣り、２０重量％を越える
場合は溶融温度か高くなる。Ｂ２Ｏ３の含有量は２０重
量％未満ては溶融温度か高くなり、３０重量％を越える
場合はガラスの化学的安定性か低下し好ましくない。To explain the reason for the above composition limitation, the content of SiO□ needs to be 40% by weight or more in order to make the thermal expansion coefficient of glass close to that of silicon carbide.
Also, in order to keep the glass melting temperature below 1450°C, 6
It is necessary that the content be 0% by weight or less. CaO is essential for reducing the viscosity of the melt during glass melting and producing homogeneous glass.If it is less than 3% by weight, the viscosity will be insufficiently reduced, and if it exceeds 15% by weight, the coefficient of thermal expansion will decrease. or larger than that of silicon carbide sintered body. If the amount of Al2O3 is less than 9% by weight, the moisture resistance will be poor, and if it exceeds 20% by weight, the melting temperature will be high. If the content of B2O3 is less than 20% by weight, the melting temperature will increase, and if it exceeds 30% by weight, the chemical stability of the glass will decrease, which is not preferable.
Ｚ ｒ ０２は必須成分てはないか３重量％以下を含有
させることにより化学的耐久性を白玉させる効果かある
。Although Zr 02 is not an essential component, it is effective to improve chemical durability by containing it in an amount of 3% by weight or less.
炭化珪素と酸化物ツルターガラスとは通常１０００°Ｃ
以上て反応して発泡し、接合面に気泡か存在する。従っ
て接合時には減圧下て昇降温速度も５°Ｃ／ｍｉｎ以上
て行うことか望ましく、このことにより接合部の気泡の
残留を防ぐことかできる。Silicon carbide and oxide sulter glass are usually heated at 1000°C.
The above reaction causes foaming, and bubbles are present at the joint surface. Therefore, during bonding, it is desirable to perform the bonding under reduced pressure and at a rate of temperature rise and fall of 5° C./min or more, thereby preventing air bubbles from remaining in the bonded portion.
ガラス粉末の製造は、前記ガラス組成の原料粉末を秤量
しライカイ機なとて混合後、該混合粉末を白金ルツボに
入れ、電気炉中て１４００〜１５００°Ｃて溶融し、溶
融物を水中に投入しガラス化する。更に該ガラスをアル
ミナボールミル等て粉砕し微粉末とする。接合に用いる
ガラス粉末の粒度は微粉末であることが望ましく例えば
０．５〜１ ｇ’ｍ程度のものか良好である。To manufacture glass powder, the raw material powders having the above glass composition are weighed and mixed using a Raikai machine, then the mixed powder is placed in a platinum crucible, melted at 1400 to 1500°C in an electric furnace, and the melt is immersed in water. and vitrify it. Further, the glass is ground into fine powder using an alumina ball mill or the like. The particle size of the glass powder used for bonding is preferably fine, for example, about 0.5 to 1 g'm.
又、該ガラス粉末の塗布は通常行なわれているガラス粉
末に有機ビヒクルを混合しペースト状にして、スクリー
ン印刷、ドクターブレード法、若しくは、へヶ塗り等て
行うことか可能であるが塗布面を均一に又平滑に塗布す
ることは接合面の精度及び所定の強度を維持することに
必要である。The glass powder can be applied by mixing the glass powder with an organic vehicle and making it into a paste, which is usually done by screen printing, doctor blading, or by applying it on the surface. Uniform and smooth application is necessary to maintain the precision and desired strength of the joint surfaces.
接合は、ガラス粉末を塗布した炭化珪素焼結体の接合面
を昇温速度か例えば約１．５°Ｃ／ａ＋ｉｎて５００〜
７００°Ｃに加熱し、バインターを空気中で除去し、得
られた脱脂後の炭化珪素焼結体接合面を重ね合せ、窒素
ガス１００〜５００ Ｔｏｒｒの雰囲気下て昇降温速度
２０〜５０６Ｃ／ｍｉｎ、接合温度１１００〜１５００
℃、 ５〜２０分間保持して接合を行う。The bonding is performed by heating the bonding surfaces of the silicon carbide sintered bodies coated with glass powder at a heating rate of approximately 1.5°C/a+in, for example, to 500°C or more.
Heating to 700°C, removing the binder in the air, stacking the bonded surfaces of the resulting degreased silicon carbide sintered bodies, and heating and cooling in a nitrogen gas atmosphere of 100 to 500 Torr at a temperature increase/decrease rate of 20 to 506 C/min. , bonding temperature 1100-1500
℃ and held for 5 to 20 minutes to perform bonding.
第１表に示すガラス組成の原料粉末を白金ルツボに入れ
電気炉中て１４５０°Ｃに加熱し、生成した融液を水中
に投入し固化させガラスを調製した。次にこのガラスを
アルミナボールミルを用い粉砕した。このガラス粉末を
エチルアルコールに懸濁させ、沈降速度の差によって分
級し、粒径１ｇｍ以下のガラス粉末を調製した。このガ
ラス粉末を有機ビヒクルと混練してペースト化し接合に
用いた。Raw material powder having the glass composition shown in Table 1 was placed in a platinum crucible and heated to 1450°C in an electric furnace, and the resulting melt was poured into water and solidified to prepare glass. Next, this glass was crushed using an alumina ball mill. This glass powder was suspended in ethyl alcohol and classified based on the difference in sedimentation rate to prepare glass powder with a particle size of 1 gm or less. This glass powder was kneaded with an organic vehicle to form a paste and used for bonding.
炭化珪素焼結体は寸法２０ｍｍＸ ２０ｍｍＸ ２２ｍ
ｍの常圧焼結晶を用い、接合面２０ｍｍＸ ２０ｍｍを
３ｇｍのダイヤモンドペーストてミラー研摩したものを
使用した。The dimensions of the silicon carbide sintered body are 20 mm x 20 mm x 22 m.
A 20 mm x 20 mm joint surface was mirror-polished with 3 gm of diamond paste using a pressureless sintered crystal of 20 mm.
接合は上記ガラス粉末ペーストをスクリーン印刷て炭化
珪素焼結体の接合面に１５０ ｐ、 ｍの厚みに印刷し
、昇温速度１．５°Ｃ／ｍｉｎて７００°Ｃに加熱し、
３０分間保持しバインダーを空気中で除去し、得られた
炭化珪素焼結体を脱脂後接台面を重ね合せ、次いで３０
０Ｔｏｒｒの窒素ガス雰囲気中て昇降温速度３０℃／
ｍｉｎ 、接合温度１４００°Ｃで５分間保持して接合
を完了させた。For bonding, the above glass powder paste was screen printed on the bonding surface of the silicon carbide sintered body to a thickness of 150 μm, and heated to 700°C at a heating rate of 1.5°C/min.
After holding for 30 minutes, the binder was removed in the air, and the resulting silicon carbide sintered body was degreased, and the surfaces to be attached were placed on top of each other, and then heated for 30 minutes.
Temperature increase/decrease rate of 30℃/in a nitrogen gas atmosphere of 0 Torr
The bonding temperature was maintained at 1400°C for 5 minutes to complete the bonding.
得られた炭化珪素焼結体の接合強度を同しく第１表に示
す。この表より従来の無機接着剤の接合強度４ｋｇ／
ｍ ｒｒｆ （工業材料（１９８３） ３１巻９号９３
〜９４頁にＳｉＣ同志の接合強度３８ＭＰａ ）に比へ
接合強度は上昇した。又、実施例によるものは接合界面
に気泡や亀裂の発生は認められなかった。The bonding strength of the obtained silicon carbide sintered body is also shown in Table 1. From this table, the bonding strength of conventional inorganic adhesives is 4 kg/
m rrf (Industrial Materials (1983) Vol. 31 No. 9 93
The bond strength increased to 38 MPa (see page 94). In addition, no bubbles or cracks were observed at the bonding interface in the examples.
第 １ 表
〔発明の効果〕
本発明により炭化珪素焼結体同志の接合に適したガラス
組成か得られ、複雑形状の成形品の組合せか可能となる
。Table 1 [Effects of the Invention] According to the present invention, a glass composition suitable for bonding sintered silicon carbide bodies can be obtained, and it is possible to combine molded products with complex shapes.
Claims (1)
てＳｉＯ＿２ ４０〜６０重量％、Ｂ＿２Ｏ＿３ ２０
〜３０重量％、Ａｌ＿２Ｏ＿３ ９〜２０重量％、Ｃａ
Ｏ ３〜１５重量％よりなることを特徴とする炭化珪素
焼結体の接合ガラス組成物。 ２、炭化珪素焼結体同志を接合させるガラス組成であっ
てＳｉＯ＿２ ４０〜６０重量％、Ｂ＿２Ｏ＿３ ２０
〜３０重量％、Ａｌ＿２Ｏ＿３ ９〜２０重量％、Ｃａ
Ｏ ３〜１５重量％、さらにＺｒＯ＿２を３重量％以下
よりなることを特徴とする炭化珪素焼結体の接合ガラス
組成物。[Claims] 1. Glass composition for bonding silicon carbide sintered bodies together, including SiO_2 40 to 60% by weight, B_2O_3 20
~30% by weight, Al_2O_3 9-20% by weight, Ca
A bonded glass composition of silicon carbide sintered body, characterized by comprising 3 to 15% by weight of O. 2. Glass composition for bonding silicon carbide sintered bodies together, with SiO_2 40 to 60% by weight, B_2O_3 20
~30% by weight, Al_2O_3 9-20% by weight, Ca
A bonded glass composition of silicon carbide sintered body characterized by comprising 3 to 15% by weight of O and further 3% by weight or less of ZrO_2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22980387A JPH01317134A (en) | 1987-09-16 | 1987-09-16 | Glass composition for bonding silicon carbide sintered form |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22980387A JPH01317134A (en) | 1987-09-16 | 1987-09-16 | Glass composition for bonding silicon carbide sintered form |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01317134A true JPH01317134A (en) | 1989-12-21 |
Family
ID=16897911
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22980387A Pending JPH01317134A (en) | 1987-09-16 | 1987-09-16 | Glass composition for bonding silicon carbide sintered form |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01317134A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012072700A2 (en) | 2010-12-02 | 2012-06-07 | Commissariat à l'énergie atomique et aux énergies alternatives | Method for preparing a glass/silicon-carbide composite material |
| JP2014094855A (en) * | 2012-11-08 | 2014-05-22 | Toshiba Corp | Silicon carbide ceramic joined body, and manufacturing method for the same |
| CN110903102A (en) * | 2019-11-25 | 2020-03-24 | 西北工业大学 | SiCfCaO-Y at port of/SiC nuclear cladding tube2O3-Al2O3-SiO2Glass packaging method |
| CN114478043A (en) * | 2022-01-12 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | Connection method of silicon carbide ceramic based on liquid phase sintering |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6374934A (en) * | 1986-09-18 | 1988-04-05 | Nobuo Takusagawa | Glass coated sintered silicon carbide and production thereof |
-
1987
- 1987-09-16 JP JP22980387A patent/JPH01317134A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6374934A (en) * | 1986-09-18 | 1988-04-05 | Nobuo Takusagawa | Glass coated sintered silicon carbide and production thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012072700A2 (en) | 2010-12-02 | 2012-06-07 | Commissariat à l'énergie atomique et aux énergies alternatives | Method for preparing a glass/silicon-carbide composite material |
| JP2014094855A (en) * | 2012-11-08 | 2014-05-22 | Toshiba Corp | Silicon carbide ceramic joined body, and manufacturing method for the same |
| CN110903102A (en) * | 2019-11-25 | 2020-03-24 | 西北工业大学 | SiCfCaO-Y at port of/SiC nuclear cladding tube2O3-Al2O3-SiO2Glass packaging method |
| CN110903102B (en) * | 2019-11-25 | 2022-03-15 | 西北工业大学 | SiCfCaO-Y at port of/SiC nuclear cladding tube2O3-Al2O3-SiO2Glass packaging method |
| CN114478043A (en) * | 2022-01-12 | 2022-05-13 | 中国科学院上海硅酸盐研究所 | Connection method of silicon carbide ceramic based on liquid phase sintering |
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