JPH03295871A - Method for joining alumina ceramic to metal - Google Patents
Method for joining alumina ceramic to metalInfo
- Publication number
- JPH03295871A JPH03295871A JP9704490A JP9704490A JPH03295871A JP H03295871 A JPH03295871 A JP H03295871A JP 9704490 A JP9704490 A JP 9704490A JP 9704490 A JP9704490 A JP 9704490A JP H03295871 A JPH03295871 A JP H03295871A
- Authority
- JP
- Japan
- Prior art keywords
- alumina ceramic
- metal
- thickness
- plating layer
- plating
- 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 18
- 239000002184 metal Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims description 6
- 238000007747 plating Methods 0.000 claims abstract description 35
- 238000005219 brazing Methods 0.000 abstract description 16
- 229910000833 kovar Inorganic materials 0.000 abstract description 3
- 230000008961 swelling Effects 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 24
- 239000000956 alloy Substances 0.000 description 24
- 238000007789 sealing Methods 0.000 description 19
- 229910000679 solder Inorganic materials 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910017309 Mo—Mn Inorganic materials 0.000 description 1
- PCEXQRKSUSSDFT-UHFFFAOYSA-N [Mn].[Mo] Chemical compound [Mn].[Mo] PCEXQRKSUSSDFT-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
この発明は、アルミナセラミックと金属とをろう付けに
より接合する方法に関する。The present invention relates to a method of joining alumina ceramic and metal by brazing.
アルミナセラミックと金属との接合は各種の分野で用い
られているが、特に電力用平形サイリスタのケースや真
空遮断器の真空パルプにおいては、単に接合強度だけで
はなく接合部の気密性も重要な特性となっている。この
ような接合は一般に銀ろう付けで行われているが、アル
ミナセラミックは金属に直接ろう付けをすることができ
ないので、アルミナセラミックの接合面にはMo(モリ
ブデン)、Mo−Mn(モリブデン−マンガン)、W(
タングステン)などの高融点金属粉の焼き付け、いわゆ
るメタライジングが行われ、更にその上に酸化防止を目
的としてNiにッケル)めっきが施されている。
一方、アルミナセラミックにろう付けされるコバール合
金やFe−42合金などの封着合金はろう材に対してあ
程度の濡れ性を有しているものの、真空雰囲気でろう付
けされる場合にも表面が酸化されて濡れ性が低下し、酸
化しないようにすると超高真空の雰囲気を用意しなけれ
ばならないので経済的に引き合わなくなる。また、ろう
付は工程で銀ろうが封着合金の粒界に侵入すると封着合
金が脆化し、アルミナセラミックと封着合金とでは封着
合金の方が熱膨張係数がやや大きいので、ろう材の凝固
により封着合金に引張応力が作用し、この応力によって
クラックが発生することがある。
これらのことから、封着合金の接合面にも事前にNiめ
っきが施されている。
に発明が解決しようとする課題】
ところが、Niめっきを施した従来のアルミナセラミッ
クにおいて、ろう付けの際に800〜900℃の高温に
さらされるとめっき層にふくれが生じ、そのために気密
性が損なわれるという問題があった。
また、封着合金においても、めっき層が薄過ぎるとろう
付は時に銀ろうによってめっき層が浸食され本来の目的
が達成されない一方、逆に厚過ぎるとめっき層と封着合
金との密着性が悪くなり、ろう付は時の加熱でふくれを
生じるという問題かった。
そこで、この発明は、アルミナセラミック及び封着合金
に最適なNiめっきを施し、上記現象が生じないように
したアルミナセラミックと金属との接合方法を提供する
ことを目的とするものである。
[l!!!を解決するための手段]
この発明は、メタライズ層を有するアルミナセラミック
と金属とを接合する場合において、アルミナセラミック
の接合面に2〜15μmの厚さのNiめっきを施し、金
属の接合面に2〜10μmの厚さのNiめっきを施すも
のとする。Bonding of alumina ceramics and metals is used in various fields, but in particular in the cases of power flat thyristors and vacuum pulp for vacuum circuit breakers, not only the bond strength but also the airtightness of the joint are important characteristics. It becomes. Such joining is generally done by silver brazing, but since alumina ceramic cannot be brazed directly to metal, Mo (molybdenum), Mo-Mn (molybdenum-manganese) is used on the joint surface of alumina ceramic. ), W(
Baking of high melting point metal powder such as tungsten), so-called metallization, is performed, and Ni plating is further applied to prevent oxidation. On the other hand, although sealing alloys such as Kovar alloy and Fe-42 alloy that are brazed to alumina ceramics have a certain degree of wettability to the brazing material, even when brazed in a vacuum atmosphere, the surface is oxidized, resulting in a decrease in wettability, and preventing oxidation requires an ultra-high vacuum atmosphere, which is not economically viable. In addition, during the brazing process, if silver solder enters the grain boundaries of the sealing alloy, the sealing alloy becomes brittle, and the coefficient of thermal expansion of the sealing alloy is slightly larger than that of the alumina ceramic and the sealing alloy. Solidification causes tensile stress to act on the sealing alloy, and this stress may cause cracks to occur. For these reasons, the joint surfaces of the sealing alloy are also plated with Ni in advance. [Problems to be Solved by the Invention] However, when conventional alumina ceramics plated with Ni are exposed to high temperatures of 800 to 900°C during brazing, the plating layer bulges, which impairs airtightness. There was a problem that Also, with regard to sealing alloys, if the plating layer is too thin, the plating layer will sometimes be eroded by the silver solder and the original purpose will not be achieved, while on the other hand, if the plating layer is too thick, the adhesion between the plating layer and the sealing alloy will deteriorate. The problem was that the brazing would cause blisters due to the heat generated over time. SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a method for joining alumina ceramic and metal in which the alumina ceramic and sealing alloy are coated with optimal Ni plating to prevent the above phenomenon from occurring. [l! ! ! [Means for Solving the Problems] In the case of joining an alumina ceramic having a metallized layer and a metal, the present invention applies Ni plating to a thickness of 2 to 15 μm on the joint surface of the alumina ceramic, and coats the joint surface of the metal with Ni plating with a thickness of 2 to 15 μm. Ni plating with a thickness of ~10 μm shall be applied.
種々のめっき厚さについて実験し、メタライズ層を有す
るアルミナセラミックに対しては、2〜15μmのNi
めっきを施すことでふくれを防止できることが確認でき
た。
同様に、封着合金に対しては、2〜10μmのNiめっ
きを施すことでろう材との濡れ性を改善し、しかもろう
材の侵入を有効に防止しながらふくれ防止もできること
が確認できた。We experimented with various plating thicknesses and found that for alumina ceramics with metallized layers, 2-15 μm of Ni
It was confirmed that blistering can be prevented by plating. Similarly, it was confirmed that applying Ni plating of 2 to 10 μm to the sealing alloy improves its wettability with the brazing metal, effectively preventing the intrusion of the brazing metal, and preventing blistering. .
まず、第1表はアルミナセラミックのNiめっき層の厚
さと加熱後のめっき層のふくれとの関係を調べたもので
ある。これによれば、厚さが2〜15μmにおいてはふ
くれは発生せず、15μmを超えるとふくれは大きく、
数も多くなり、更に25μm以上になるとやや減少する
傾向にあることが分かる。
第1表
に至らない。したがって、めっき層がこの中間的な厚さ
の場合に最もふくれが発生し昌いことになると考えられ
る。
次に、第2表は封着合金(コバール合金)に各種の厚さ
のNiめっきを施した後、封着合金とめっき層の密着性
、及びろう付は後のめっき層の状態を調べたものである
。
第2表
これは以下の如く説明できる。めっき層やメタライズ層
の内部に吸蔵されているガスは、ろう付は時の加熱で放
出されるが、このガスはめっき層が比較的薄い場合には
めっき層を透過してしまうため、ふくれを起こさせるよ
うな応力は働かない。
逆に、めっき層が相当厚くなると、めっき層は放出ガス
の応力以上の強度を持つためふくれの発生封着合金とめ
っき層との密着性は、めっきを施した封着合金を850
°Cの真空中で30分加熱した後に取り出し、めっき層
のふくれの有無により判定したものである。また、めっ
き層の状態は、めっきを施した封着合金とメタライジン
グしたアルミナセラミックとを850℃の真空中で30
分加熱、ろう付けした後、その断面を光学顕微鏡及び電
子顕微鏡で観察したものである。
封着合金とNiめっき層との密着性は、めっき層の厚さ
が10μm以下では異常は認められず良好な密着性を呈
していた。しかし、10μmを超えると、ふくれが発生
しているものが認められた。
特に、15μm程度で顕著であり、更に厚くなると減少
する傾向となっていた。
一方、ろう付は後の断面観察においては、めっき層の厚
さが2μm以下ではめっき層として存在せずにろう層に
拡散しており、銀ろうに含まれるCu(銅)と合金化し
ていた。更に電子顕微鏡により詳細に観察したところ、
封着合金の粒界からAg(銀)が検出された。このAg
は銀ろうの成分であり、封着合金には含まれていない成
分であるので、ろう付けによって封着合金の粒界に銀ろ
うが侵入したものであるといえる。First, Table 1 shows the relationship between the thickness of the Ni plating layer of alumina ceramic and the swelling of the plating layer after heating. According to this, no blistering occurs when the thickness is between 2 and 15 μm, and when the thickness exceeds 15 μm, the blisters become large.
It can be seen that the number also increases and tends to decrease slightly when the thickness becomes 25 μm or more. It does not reach Table 1. Therefore, it is thought that blistering occurs most when the plating layer has an intermediate thickness. Next, Table 2 shows the adhesion between the sealing alloy and the plating layer after Ni plating of various thicknesses was applied to the sealing alloy (Kovar alloy), and the condition of the plating layer after brazing. It is something. Table 2 This can be explained as follows. Gases stored inside the plating layer or metallized layer are released by heating during brazing, but if the plating layer is relatively thin, this gas will permeate through the plating layer, causing blistering. There is no stress that would cause it to occur. On the other hand, if the plating layer becomes considerably thick, the plating layer will have a strength greater than the stress of the emitted gas, so blistering will occur.
After heating in a vacuum at °C for 30 minutes, the samples were taken out and judged based on the presence or absence of blistering of the plating layer. In addition, the state of the plating layer was determined by combining the plated sealing alloy and the metallized alumina ceramic in a vacuum at 850°C.
After heating and brazing for several minutes, the cross section was observed using an optical microscope and an electron microscope. Regarding the adhesion between the sealing alloy and the Ni plating layer, no abnormality was observed when the thickness of the plating layer was 10 μm or less, and good adhesion was exhibited. However, when the thickness exceeded 10 μm, blistering was observed in some cases. It was particularly noticeable at around 15 μm, and tended to decrease as the thickness increased further. On the other hand, later cross-sectional observations of brazing showed that when the thickness of the plating layer was less than 2 μm, it did not exist as a plating layer but was diffused into the solder layer, and was alloyed with Cu (copper) contained in the silver solder. . Further detailed observation using an electron microscope revealed that
Ag (silver) was detected from the grain boundaries of the sealing alloy. This Ag
Since this is a component of silver solder and is not included in the sealing alloy, it can be said that the silver solder has entered the grain boundaries of the sealing alloy during brazing.
この発明によれば、アルミナセラミック及び封着合金の
接合面に施したNiめっき層のろう付けによるふくれの
発生を有効に防止し、気密性を有する用途におけるアル
ミナセラミックと金属との接合の信転性を向上させるこ
とができる。
手続補正書(自発)
発明の名称 アルミナセラミックと金属との接合方法補
正をする者
補正の内容
1、明細書第2頁、第10行のrFe−42合金」を「
Fe 42Ni合金 」と補正する。
2、明細書第2頁、第11行の「あ程度」を「ある程度
」と補正する。
事件との関係 特許出願人According to the present invention, it is possible to effectively prevent the occurrence of blistering caused by brazing the Ni plating layer applied to the joint surface of the alumina ceramic and the sealing alloy, and to improve the reliability of the joint between the alumina ceramic and the metal in airtight applications. can improve sex. Procedural amendment (voluntary) Name of the invention Person amending the joining method of alumina ceramic and metal Contents of amendment 1, “rFe-42 alloy” on page 2, line 10 of the specification”
Corrected as "Fe42Ni alloy". 2. On page 2 of the specification, line 11, "to some extent" is amended to "to some extent." Relationship to the case Patent applicant
Claims (1)
を接合する場合において、アルミナセラミックの接合面
に2〜15μmの厚さのNiめっきを施し、金属の接合
面に2〜10μmの厚さのNiめっきを施すことを特徴
とするアルミナセラミックと金属との接合方法。1) When joining an alumina ceramic having a metallized layer and a metal, apply Ni plating with a thickness of 2 to 15 μm on the joint surface of the alumina ceramic, and apply Ni plating with a thickness of 2 to 10 μm on the joint surface of the metal. A method for joining alumina ceramic and metal, characterized by applying
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9704490A JP2650460B2 (en) | 1990-04-12 | 1990-04-12 | Joining method of alumina ceramic and metal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9704490A JP2650460B2 (en) | 1990-04-12 | 1990-04-12 | Joining method of alumina ceramic and metal |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH03295871A true JPH03295871A (en) | 1991-12-26 |
JP2650460B2 JP2650460B2 (en) | 1997-09-03 |
Family
ID=14181611
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9704490A Expired - Lifetime JP2650460B2 (en) | 1990-04-12 | 1990-04-12 | Joining method of alumina ceramic and metal |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2650460B2 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9806380B2 (en) | 2013-05-31 | 2017-10-31 | General Electric Company | High temperature electrochemical cell structures, and methods for making |
US10103410B2 (en) | 2014-05-23 | 2018-10-16 | General Electric Company | Method for joining ceramic to metal, and sealing structure thereof |
-
1990
- 1990-04-12 JP JP9704490A patent/JP2650460B2/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9806380B2 (en) | 2013-05-31 | 2017-10-31 | General Electric Company | High temperature electrochemical cell structures, and methods for making |
US10103410B2 (en) | 2014-05-23 | 2018-10-16 | General Electric Company | Method for joining ceramic to metal, and sealing structure thereof |
Also Published As
Publication number | Publication date |
---|---|
JP2650460B2 (en) | 1997-09-03 |
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