JP2955622B2 - Ceramic brazing method - Google Patents
Ceramic brazing methodInfo
- Publication number
- JP2955622B2 JP2955622B2 JP13364990A JP13364990A JP2955622B2 JP 2955622 B2 JP2955622 B2 JP 2955622B2 JP 13364990 A JP13364990 A JP 13364990A JP 13364990 A JP13364990 A JP 13364990A JP 2955622 B2 JP2955622 B2 JP 2955622B2
- Authority
- JP
- Japan
- Prior art keywords
- brazing
- furnace
- temperature
- torr
- active
- 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.)
- Expired - Lifetime
Links
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、セラミックスに対し、セラミックスもしく
は金属をろう付するセラミックスのろう付方法に関す
る。Description: FIELD OF THE INVENTION The present invention relates to a method for brazing ceramics or metal to ceramics.
（従来の技術） 従来、セラミックスに対するセラミックス又は金属と
のろう付は、チタン（Ti）、ジルコニウム（Zr）等の活
性金属を含むろう材（以下活性ろうという）を用いて１
×10-4torr以下の高真空中あるいはアルゴン（Ar）及び
／又はヘリウム（He）等不活性ガス雰囲気中（希ガス雰
囲気中）で加熱することにより行われていた。(Prior Art) Conventionally, brazing of ceramics or metal to ceramics is performed using a brazing material containing an active metal such as titanium (Ti) or zirconium (Zr) (hereinafter referred to as active brazing).
Heating is performed in a high vacuum of 10-4 torr or less or in an inert gas atmosphere (in a rare gas atmosphere) such as argon (Ar) and / or helium (He).
（発明が解決しようとする課題） 従来のろう付方法により接合した製品は、接合強度の
バラつきが大きく、信頼性に欠けるという問題点を有し
ていた。(Problems to be Solved by the Invention) A product joined by a conventional brazing method has a problem in that there is a large variation in joining strength and lacks reliability.
本発明はかかる問題点にかんがみ、接合強度のバラつ
きの少い、信頼性の高いセラミックスのろう付方法の提
供を目的とする。The present invention has been made in view of the above problems, and has as its object to provide a highly reliable brazing method for ceramics with less variation in bonding strength.
（問題点を解決するための手段） 発明者らは、接合強度のバラつく原因について調べた
結果、セラミックスと活性ろうとの間に未接合部分が点
在していることに起因しているとの推論を得た。(Means for Solving the Problems) As a result of investigating the cause of the variation in the bonding strength, the inventors have found that unbonded portions are scattered between the ceramic and the active solder. Got inference.
そこで、この点在する未接合部分（欠陥）をなくすこ
とのできるろう付方法について研究を重ね、本発明を完
成するに至った。Therefore, the inventors have repeatedly studied a brazing method that can eliminate the interspersed unjoined portions (defects), and have completed the present invention.
即ち、本発明の特徴は、セラミックスに対し、セラミ
ックスもしくは金属を、活性ろうを用い、炉中にてろう
付するセラミックスのろう付方法において、前記活性ろ
うの融点もしくは液相線温度以上まで１×10-4torr以下
の真空下で昇温し、該活性ろうの融点もしくは液相線温
度以上に達した後、アルゴン（Ar）及び／又はヘリウム
（He）等の不活性ガスを炉内に導入し、該炉内を500tor
r以上の圧力に上昇させてから降温することにある。That is, a feature of the present invention is that, in a method of brazing ceramics or metal to ceramics using an active braze and brazing in a furnace, the method comprises the steps of: The temperature is raised under a vacuum of 10 -4 torr or less, and after reaching the melting point or liquidus temperature of the active solder, the inert gas such as argon (Ar) and / or helium (He) is introduced into the furnace. And 500 torr
It is to lower the temperature after increasing the pressure to r or more.
ここに活性金属とは、チタン（Ti）、ジルコニウム
（Zr）、ハフニウム（Hf）、ニオブ（Nb）、タンタル
（Ta）等従来公知のものであり、通常のろう材のみでは
濡らすことのできないセラミックス表面の濡れ性を改善
するため、ろう材に加えられるものである。Here, the active metal is a conventionally known material such as titanium (Ti), zirconium (Zr), hafnium (Hf), niobium (Nb), and tantalum (Ta), and is a ceramic which cannot be wet with ordinary brazing material alone. It is added to the brazing filler metal to improve the surface wettability.
このような活性ろうは、例えば通常のろう材組成物に
活性金属を加えて溶融・固化させたものや、活性金属箔
とろう材箔とをはり合わせたもの、圧延したものの他、
活性金属粉末とろう材粉末との混合物なども用いること
ができる。Such an active brazing material is, for example, a material obtained by adding an active metal to a normal brazing material composition and melting and solidifying, a material obtained by bonding an active metal foil and a brazing material foil, a rolled material,
A mixture of active metal powder and brazing filler metal powder can also be used.
活性金属以外のろう材成分は、従来公知の全てのもの
が使用可能である。例えば、Ag−Cu系、Ag−Cu−In系、
Au−Cu系、Ni−Ｐ系、Au−Ni系等がる。As the brazing filler metal components other than the active metal, all conventionally known brazing filler metals can be used. For example, Ag-Cu-based, Ag-Cu-In-based,
Au-Cu system, Ni-P system, Au-Ni system and the like.
セラミックスも、酸化物系、非酸化物系全てに適用で
きる。Ceramics can also be applied to all oxides and non-oxides.
本発明に用いる炉は、真空引きができ、更にAr及び／
またはHe等の不活性ガスを導入できる構造のものであれ
ば良い。The furnace used in the present invention can be evacuated, and further contains Ar and / or
Alternatively, any structure that can introduce an inert gas such as He may be used.
昇温時に炉内を真空雰囲気にすることは、活性ろうの
酸化等による変質を避けるために従来から行われている
方法であり、その真空度は通常１×10-4torr以下とさ
れ、本発明においても同様である。The use of a vacuum atmosphere in the furnace at the time of raising the temperature is a method conventionally used in order to avoid deterioration of the active brazing due to oxidation or the like, and the degree of vacuum is usually set to 1 × 10 -4 torr or less. The same applies to the invention.
本発明では、炉内温度が用いている活性ろうの融点又
は液相線温度より高い温度、即ち、該活性ろうが完全に
溶融した後、炉内にAr及び／又はHe等を導入し、導入前
より500torr以上高い圧力とすることが肝要である。こ
こで用いるAr、Heガスは露点が−90℃以下の、いわゆる
高純度ガスが望ましいが、昇温時ほどの影響はないため
普通純度のものでも良い。500torr未満の圧力差では効
果は少い。In the present invention, the furnace temperature is higher than the melting point or liquidus temperature of the active brazing used, that is, after the active brazing is completely melted, Ar and / or He are introduced into the furnace and introduced. It is important that the pressure be at least 500 torr higher than before. The Ar and He gases used here are desirably so-called high-purity gases having a dew point of -90 ° C. or less, but may be ordinary-purity gases because they are not so affected as when the temperature is raised. The effect is small when the pressure difference is less than 500 torr.
また、不活性ガスは希ガスであれば効果に違いはな
い。In addition, there is no difference in the effect as long as the inert gas is a rare gas.
（作用） 詳細には不明であるが、本発明により接合強度のバラ
つきが減少する理由として以下のように考えられる。(Operation) Although it is unknown in detail, the reason why the present invention reduces the variation in bonding strength is considered as follows.
昇温時において、炉内は真空雰囲気となっているた
め、活性ろうが融けた際生じる接合部の未接触部分（気
泡と考えることができる）もまた真空である。At the time of temperature increase, the inside of the furnace is in a vacuum atmosphere, so that the non-contact portion (which can be considered as a bubble) of the joint generated when the active solder melts is also in a vacuum.
そこで、炉内にAr及び／又はHe等を導入して導入前よ
り500torr以上高い圧力にすると、活性ろうは溶融（液
体）状態にあるため、その圧力をパスカルの原理によっ
て伝達し、接合部の「気泡」を消滅させるものと考えら
れる。Therefore, if Ar and / or He is introduced into the furnace and the pressure is set to 500 torr or more higher than before the introduction, the active solder is in a molten (liquid) state. It is thought that the "bubbles" disappear.
但し、溶融した活性ろうの粘度はかなり高いため、50
0torr以上の圧力差がない場合には圧力の伝達が不十分
となり効果が少いものと考えられる。However, since the viscosity of molten active wax is quite high, 50
When there is no pressure difference of 0 torr or more, it is considered that the pressure transmission is insufficient and the effect is small.
（実施例） セラミックスとして３×４×20mmのサイアロンを用
い、金属として３×４×20mmのタングステンを用いて、
接合部に２重量％のTi含有Ag−Cuろう箔（田中貴金属社
製、TKC−710、厚み75μｍ）をはさみ、３×４×40mmの
接合体となるようカーボンジグで押さえ、真空炉にセッ
トした。ロータリーポンプで荒引き後、ターボポンプに
て減圧し、炉内が１×10-4torrになった時点で炉の昇温
を開始し、真空引きしたまま該活性ろうの融点である約
785℃より30℃高い815℃まで昇温した。このとき、炉内
真空度は５×10-5torrであった。(Example) Using sialon of 3 × 4 × 20 mm as ceramics and tungsten of 3 × 4 × 20 mm as metal,
A 2% by weight Ti-containing Ag-Cu brazing foil (Tanaka Kikinzoku Co., Ltd., TKC-710, thickness 75 μm) is sandwiched between the joints, pressed with a carbon jig to form a 3 × 4 × 40 mm joined body, and set in a vacuum furnace. did. After roughing with a rotary pump, the pressure was reduced with a turbo pump, and when the inside of the furnace became 1 × 10 -4 torr, the temperature of the furnace was started.
The temperature was raised to 815 ° C, which is 30 ° C higher than 785 ° C. At this time, the degree of vacuum in the furnace was 5 × 10 −5 torr.
然る後、ターボポンプを停止し、Arボンベより炉内に
Arガスを導入し、第１表に示すように実施例１では500t
orr、実施例２では760torr、比較例１では450torrの圧
力が維持されるように、ロータリーポンプ側の弁とArガ
ス導入側の弁の流量を調節しながら、室温まで降温し
た。After that, stop the turbo pump and put it into the furnace from the Ar cylinder.
Ar gas was introduced, and as shown in Table 1, in Example 1, 500 t
The temperature was lowered to room temperature while adjusting the flow rates of the valve on the rotary pump side and the valve on the Ar gas introduction side so that the pressure of orr, the pressure of 760 torr in Example 2 and the pressure of 450 torr in Comparative Example 1 were maintained.
なお、比較例２ではArガス導入せずに室温まで降温し
た。In Comparative Example 2, the temperature was lowered to room temperature without introducing Ar gas.
このようにして各実施例1,2及び比較例1,2毎に20本ず
つの接合体をつくり、JISR1601にしたがって抵抗試験を
行い、平均強度及び標準偏差を求めた。結果は第１表に
示す如くであった。In this way, 20 joints were prepared for each of Examples 1 and 2 and Comparative Examples 1 and 2, and a resistance test was performed in accordance with JISR1601, and average strength and standard deviation were determined. The results were as shown in Table 1.
（発明の効果） 上述したように本発明では、炉内を真空下で昇温さ
せ、活性ろうの融点もしくは液相線温度以上に達した
後、不活性ガスを導入して、500torr以上高い圧力まで
上昇させてから降温させるようにしたことにより、接合
部分の強度のバラつきが減少し、全体として高強度の接
合が得られ、セラミックス接合体の用途が拡大されるこ
ととなったものである。 (Effects of the Invention) As described above, in the present invention, the temperature inside the furnace is raised under vacuum, and after reaching the melting point or liquidus temperature of the active brazing or more, an inert gas is introduced and the pressure is increased by 500 torr or more. By lowering the temperature after raising the temperature, the variation in the strength of the bonding portion is reduced, and a high-strength bonding is obtained as a whole, and the application of the ceramic bonded body is expanded.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) C04B 37/00 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int. Cl. 6 , DB name) C04B 37/00
Claims (1)
は金属を、活性金属を含むろう材を用い、炉中にてろう
付するセラミックスのろう付方法において、前記ろう材
の融点もしくは液相線温度以上まで１×10-4torr以下の
真空下で昇温し、該ろう材の融点もしくは液相線温度以
上に達した後、アルゴン（Ar）及び／又はヘリウム（H
e）等の不活性ガスを炉内に導入し、該炉内を500torr以
上の圧力に上昇させてから降温することを特徴とするセ
ラミックスのろう付方法。1. A method for brazing ceramics in which a ceramic or a metal is brazed in a furnace by using a brazing material containing an active metal. The temperature was raised under a vacuum of × 10 −4 torr or less, and after reaching the melting point or liquidus temperature of the brazing material, argon (Ar) and / or helium (H
e) A method for brazing ceramics, which comprises introducing an inert gas such as that described above into a furnace, raising the pressure in the furnace to a pressure of 500 torr or more, and then lowering the temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13364990A JP2955622B2 (en) | 1990-05-23 | 1990-05-23 | Ceramic brazing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13364990A JP2955622B2 (en) | 1990-05-23 | 1990-05-23 | Ceramic brazing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0431373A JPH0431373A (en) | 1992-02-03 |
| JP2955622B2 true JP2955622B2 (en) | 1999-10-04 |
Family
ID=15109733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13364990A Expired - Lifetime JP2955622B2 (en) | 1990-05-23 | 1990-05-23 | Ceramic brazing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2955622B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105728981B (en) * | 2016-05-05 | 2018-08-14 | 哈尔滨工业大学（威海） | Weld Si3N4The solder and its method for welding of ceramics-stainless steel |
| CN107363359A (en) * | 2017-08-09 | 2017-11-21 | 北京工业大学 | A kind of method of compound high-entropy alloy solder ceramic soldering and metal |
-
1990
- 1990-05-23 JP JP13364990A patent/JP2955622B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0431373A (en) | 1992-02-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4797328A (en) | Soft-solder alloy for bonding ceramic articles | |
| JPH0367985B2 (en) | ||
| JP3040203B2 (en) | High temperature stable composite and method for producing the same | |
| JPH03174370A (en) | Method for joining ceramics and metal | |
| JP2783366B2 (en) | Silver alloy brazing for bonding ceramic members to each other or directly to metal members | |
| US4859531A (en) | Method for bonding a cubic boron nitride sintered compact | |
| JP2955622B2 (en) | Ceramic brazing method | |
| JP3095490B2 (en) | Ceramic-metal joint | |
| JPS59232692A (en) | Brazing filler metal for joining ceramics and metal or the like and composite body composed of ceramics and metal or the like using said brazing filler metal | |
| JP2892172B2 (en) | Metal foil clad ceramic product and method of manufacturing the same | |
| JP3095187B2 (en) | Brazing filler metal for metal / ceramics | |
| JPH0632869B2 (en) | Brazing method for ceramics and metal | |
| JPH06126472A (en) | Pressure joining method | |
| JP2816042B2 (en) | Joining method of copper plate and alumina or AlN substrate | |
| JPH0526599B2 (en) | ||
| JP2986624B2 (en) | Active metal brazing | |
| JPS63169348A (en) | Amorphous alloy foil for jointing ceramics | |
| JP2003335585A (en) | Process for joining ceramics through active metal soldering | |
| JP3335701B2 (en) | Joining method of ceramics and metal | |
| JPH0680481A (en) | Production of bonded material of oxide ceramics and metal | |
| JPH01224279A (en) | Bonding of ceramic to metal | |
| JPH06128049A (en) | Production of joined material of oxide ceramics and metal | |
| JPH0547513B2 (en) | ||
| JP3292767B2 (en) | Joining method of silicon carbide ceramics and silicon | |
| JPH07133167A (en) | Method for joining oxide ceramics to fe-ni system metal |