JP3402482B2 - Base paste for forming Pt film and method for forming Pt film - Google Patents
Base paste for forming Pt film and method for forming Pt filmInfo
- Publication number
- JP3402482B2 JP3402482B2 JP03393693A JP3393693A JP3402482B2 JP 3402482 B2 JP3402482 B2 JP 3402482B2 JP 03393693 A JP03393693 A JP 03393693A JP 3393693 A JP3393693 A JP 3393693A JP 3402482 B2 JP3402482 B2 JP 3402482B2
- Authority
- JP
- Japan
- Prior art keywords
- paste
- film
- weight
- parts
- alumina
- 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 - Fee Related
Links
Landscapes
- Vessels And Coating Films For Discharge Lamps (AREA)
- Manufacture Of Electron Tubes, Discharge Lamp Vessels, Lead-In Wires, And The Like (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は高純度のアルミナ母材上
に形成するＰt膜の接合強度を高めるための下地層の組
成及びＰt膜の形成方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a composition of an underlayer and a method of forming a Pt film for increasing the bonding strength of a Pt film formed on a high-purity alumina base material.
【０００２】[0002]
【従来の技術】高純度アルミナ母材上にＰt膜を導電性
膜や回路として形成することが、ハイブリッドＩＣ、セ
ンサー等において従来から行なわれている。斯かるＰt
膜の形成方法として従来からケミカルボンド法とアンカ
ーボンド法がある。ケミカルボンド法は粒径１〜２μｍ
のＰt微粉末にＣu、Ｃr、Ｎi等を微量添加し、これをビ
ヒクル、有機溶剤等ともに混練してペースト状にし、ア
ルミナ母材表面にスクリーン印刷した後、９００〜１２
００℃で焼成する方法であり、この方法では添加したＣ
u、Ｃr、ＮiがＰt微粒子とアルミナとを結合する。アン
カーボンド法はＣu、Ｃr、Ｎi等を添加せずにペースト
状にし、アルミナ母材表面に印刷した後に焼成する方法
であり、この方法ではアルミナ母材表面の微細な凹凸に
ペーストが入り込んで結合が行なわれる。2. Description of the Related Art The formation of a Pt film as a conductive film or a circuit on a high-purity alumina base material has been conventionally performed in hybrid ICs, sensors and the like. Such Pt
Conventionally, there are a chemical bond method and an anchor bond method as a film forming method. The chemical bond method has a particle size of 1-2 μm.
After adding a minute amount of Cu, Cr, Ni, etc. to the Pt fine powder of No. 1, kneading this with a vehicle, an organic solvent, etc. to form a paste, and screen-printing on the surface of the alumina base material, 900-12
This is a method of firing at 00 ° C.
u, Cr, and Ni bond the Pt fine particles and alumina. The anchor bond method is a method of forming a paste without adding Cu, Cr, Ni, etc., printing it on the surface of the alumina base material, and then firing it. In this method, the paste enters the fine irregularities on the surface of the alumina base material and bonds it. Is performed.
【０００３】[0003]
【発明が解決しようとする課題】上述した従来のＰt膜
形成方法にあっては、アルミナ母材との結合力が弱く、
剥離を生じやすい。特に高純度アルミナ母材表面は極め
て平滑で凹凸がないため、アンカーボンド法で形成した
Ｐt膜は簡単に剥がれてしまう。In the above-mentioned conventional Pt film forming method, the bonding force with the alumina base material is weak,
Easy to peel off. In particular, since the surface of the high-purity alumina base material is extremely smooth and has no irregularities, the Pt film formed by the anchor bond method is easily peeled off.
【０００４】[0004]
【課題を解決するための手段】上記課題を解決すべく本
発明は、高純度アルミナ母材とＰt膜との間にこれらを
結合するための下地層を設け、この下地層をＰt微粉末
が１００重量部、高純度アルミナ微粉末が５〜１５重量
部からなるものとし、更に高純度アルミナ母材が既焼成
の場合には中間層として上記の組成にＳiＯ2微粉末を
２．５〜１０重量部添加したものとした。In order to solve the above-mentioned problems, the present invention provides an underlayer between the high-purity alumina base material and the Pt film for bonding them, and this underlayer is made of Pt fine powder. 100 parts by weight, 5 to 15 parts by weight of high-purity alumina fine powder, and when the high-purity alumina base material is already fired, 2.5 to 10 parts by weight of SiO 2 fine powder is added to the above composition as an intermediate layer. It is assumed that the weight part is added.
【０００５】[0005]
【作用】高純度アルミナ母材の表面に高純度アルミナ微
粉末を含む下地ペーストを塗布し、この下地ペースト上
にＰtペーストを重ねて塗布し、これら下地ペーストと
Ｐtペーストを同時に焼成する。Function: A base paste containing high-purity alumina fine powder is applied to the surface of a high-purity alumina base material, a Pt paste is overlaid on the base paste, and these base paste and Pt paste are simultaneously fired.
【０００６】[0006]
【実施例】以下に本発明の実施例を添付図面に基づいて
説明する。ここで、図１は本発明を適用したメタルハラ
イドランプの封止部の断面図、図２は図１の要部拡大図
であり、メタルハライドランプは透光性の発光管１の開
口２を絶縁キャップ３で閉塞し、この絶縁キャップ３の
内側面にタングステン製の内側電極４を、外側面に外側
電極（リード）５をそれぞれ圧入し、これら内側電極４
と外側電極５とを本発明に係る方法で形成したＰt膜６
にて導通している。Embodiments of the present invention will be described below with reference to the accompanying drawings. Here, FIG. 1 is a cross-sectional view of a sealing portion of a metal halide lamp to which the present invention is applied, and FIG. 2 is an enlarged view of an essential part of FIG. 1, in which the metal halide lamp has an insulating cap for an opening 2 of a translucent arc tube 1. 3, the inner electrode 4 made of tungsten is press-fitted into the inner side surface of the insulating cap 3, and the outer electrode (lead) 5 is press-fitted into the outer side surface thereof.
And the outer electrode 5 formed by the method according to the present invention 6
Is conducting.
【０００７】また、絶縁キャップ３の表面と対向する開
口２の表面にも本発明に係る方法によってＰt膜７を形
成し、これらＰt膜６，７間にＡu系、Ｐd系或いはＰt系
等の低融点貴金属ろう材８が封止材として介在し、更に
絶縁キャップ３の内端面にはバックアークを防止するた
めの絶縁プレート９を設けている。Also, a Pt film 7 is formed on the surface of the opening 2 facing the surface of the insulating cap 3 by the method according to the present invention, and an Au-based, Pd-based or Pt-based film is formed between these Pt films 6 and 7. A low melting point noble metal brazing material 8 is interposed as a sealing material, and an insulating plate 9 for preventing back arc is provided on the inner end surface of the insulating cap 3.
【０００８】ところで、前記発光管１及び絶縁キャップ
３はいずれも純度９６％以上のアルミナ微粉末を原料と
した高純度アルミナ母材であり、発光管１については封
止前から焼成されており、絶縁キャップ３についてはＰ
t膜６の焼成と同時に焼成される。By the way, the arc tube 1 and the insulating cap 3 are both high-purity alumina base materials made of alumina fine powder having a purity of 96% or more, and the arc tube 1 is fired before sealing. P for insulation cap 3
The t film 6 is baked at the same time.
【０００９】また、Ｐt膜６は図２に示すように絶縁キ
ャップ３表面に下地層１０を介して形成されている。こ
の下地層１０はＰt粒子１１間にＡl2Ｏ3粒子１２が混在
し、Ａl2Ｏ3粒子１２が絶縁キャップ３を構成するアル
ミナ母材と結合し、Ｐt粒子１１がＰt膜６と溶融結合し
ている。尚、発光管１とＰt膜７との間にも同様の下地
層が介在しているが、この下地層にはＰt粒子間にＡl2
Ｏ3粒子の他にＳiＯ2粒子も混在している。Further, as shown in FIG. 2, the Pt film 6 is formed on the surface of the insulating cap 3 with the underlying layer 10 interposed therebetween. The undercoat layer 10 is Al 2 O 3 particles 12 are mixed between Pt particles 11, Al 2 O 3 particles 12 are bonded with the alumina base material constituting the insulating cap 3, melt bonding Pt particles 11 and the Pt film 6 is doing. Although a similar underlayer is also interposed between the arc tube 1 and the Pt film 7, Al 2 is present between Pt particles in this underlayer.
In addition to O 3 particles, SiO 2 particles are also mixed.
【００１０】以下に上記の下地層及びＰt膜を形成する
方法の一例を述べる。先ず、下地層を形成するための下
地ペーストを調製する。下地ペーストとしては未焼成の
アルミナからなる絶縁キャップ３用と既焼成のアルミナ
からなる発光管１用との２種類を調製する。An example of a method of forming the above-mentioned underlayer and Pt film will be described below. First, a base paste for forming a base layer is prepared. Two types of base pastes are prepared, one for the insulating cap 3 made of unbaked alumina and one for the arc tube 1 made of baked alumina.
【００１１】未焼成のアルミナ母材用の下地ペースト
は、粒径１〜２μｍ程度のＰt微粉末を１００重量部、
粒径０．１μｍ以下で純度９６％以上（好ましくは９
９．９９％）のＡl2Ｏ3微粉末を５〜１５重量部用意
し、これらをビヒクル及び有機溶剤とともに混練してペ
ースト状にする。The base paste for the unbaked alumina base material is 100 parts by weight of Pt fine powder having a particle size of about 1 to 2 μm,
A particle size of 0.1 μm or less and a purity of 96% or more (preferably 9% or more)
5 to 15 parts by weight of Al 2 O 3 fine powder (9.99%) is prepared and kneaded with a vehicle and an organic solvent to form a paste.
【００１２】また、既焼成のアルミナ母材用の下地ペー
ストは、上記のＰt微粉末及びＡl2Ｏ3粒子の他にＳiＯ2
粒子を２．５〜２０重量部添加し、これらをビヒクル及
び有機溶剤とともに混練してペースト状にする。The ground paste for the pre-fired alumina matrix is SiO 2 in addition to the Pt fine powder and Al 2 O 3 particles.
2.5 to 20 parts by weight of particles are added, and these are kneaded together with a vehicle and an organic solvent to form a paste.
【００１３】そして、未焼成のアルミナ母材上に下地層
及びＰt膜を形成するには、先ず下地ペーストをスクリ
ーン印刷或いは筆塗り等によって所定厚さ塗布し、次い
で、この下地ペーストを１５０℃で１０分間乾燥させ、
この後下地ペーストの上に純度１００％のＰtペースト
を塗布して乾燥させ、而る後、未焼成のアルミナ母材と
ともに１５００〜１６５０℃で２時間程度同時に焼成す
る。Then, in order to form a base layer and a Pt film on an unbaked alumina base material, first, a base paste is applied to a predetermined thickness by screen printing or brush coating, and then this base paste is heated at 150 ° C. Let it dry for 10 minutes,
After this, a Pt paste having a purity of 100% is applied onto the base paste and dried, and thereafter, it is simultaneously fired at 1500 to 1650 ° C. for about 2 hours together with an unfired alumina base material.
【００１４】また、既焼成のアルミナ母材上に下地層及
びＰt膜を形成するには、Ｐtペーストを塗布して乾燥さ
せるまでの工程は前記と同様であるが、アルミナ母材は
既に焼成されているので、下地ペーストとＰtペースト
を１２００〜１５００℃で２時間程度同時に焼成する。Further, in order to form the underlayer and the Pt film on the already fired alumina base material, the steps until the Pt paste is applied and dried are the same as the above, but the alumina base material has already been fired. Therefore, the base paste and the Pt paste are simultaneously fired at 1200 to 1500 ° C. for about 2 hours.
【００１５】ここで、既焼成の高純度アルミナ母材に対
してはＳｉＯ2粒子を含んだ下地ペーストを用いるの
は、Ａｌ 2 Ｏ 3 の母材への拡散により、下地層中のアルミ
ナとより強固な結合を促すからであり、Ａｌ2Ｏ3微粉末
を５〜１５重量部としたのは、Ａｌ2Ｏ3微粉末が１５重
量部より多いと、下地層と上部Ｐｔ膜とのＰｔの溶融結
合が弱く、５重量部より少ないと逆に母材と下地層との
結合が低下するからであり、またＳｉＯ2粒子を２．５
〜２０重量部としたのは、２０重量部より多いと、溶融
ガラスが上部Ｐt膜上に析出し、貴金属ろうとの濡れ性
を著しく低下させ、２．５重量部より少ないと、十分な
母材との強度が得られないからである。Here, the base paste containing SiO 2 particles is used for the pre-fired high-purity alumina base material because Al 2 O 3 is diffused into the base material and the alumina paste in the base layer is This is because it promotes a strong bond, and the reason why the Al 2 O 3 fine powder is 5 to 15 parts by weight is that if the Al 2 O 3 fine powder is more than 15 parts by weight, the Pt of the underlayer and the upper Pt film is This is because the fusion bond is weak, and when it is less than 5 parts by weight, the bond between the base material and the underlayer is decreased, and the SiO 2 particles are added to 2.5
The amount of ˜20 parts by weight is that when it is more than 20 parts by weight, the molten glass is deposited on the upper Pt film and remarkably deteriorates the wettability with the noble metal braze, and when it is less than 2.5 parts by weight, a sufficient base material is obtained. This is because the strength with
【００１６】[0016]
【発明の効果】以下の（表１）は下地ペーストとしてＰ
t微粉末と高純度アルミナ微粉末を含むものを用いた場
合の接合強度を下地ペーストを用いない従来例と比較し
たものであり、（表２）は下地ペーストとしてＰt微粉
末と高純度アルミナ微粉末とＳiＯ2を含むものを用いた
場合の接合強度を下地ペーストを用いない従来例と比較
したものである。The following (Table 1) shows P as the base paste.
The bonding strength when using the one containing t fine powder and the high-purity alumina fine powder is compared with that of the conventional example in which the base paste is not used. Table 2 shows the Pt fine powder and the high-purity alumina fine powder as the base paste. The bonding strength in the case of using the one containing the powder and SiO 2 is compared with the conventional example in which the base paste is not used.
【００１７】[0017]
【表１】 [Table 1]
【表２】 [Table 2]
【００１８】上記の表からも明らかなように本発明によ
れば、高純度アルミナ母材上にＰt膜を形成するにあた
り、高純度アルミナ母材とＰt膜との間にＰtとアルミナ
を含むペーストを焼成してなる層を介在せしめるように
したので、下地層のアルミナ粉末が高純度アルミナ母材
と結合し、一方下地層のＰt粒子が上層のＰtと溶融結合
し、全体として高純度アルミナ母材とＰt膜との接合強
度が大幅に向上する。As is clear from the above table, according to the present invention, in forming a Pt film on a high-purity alumina base material, a paste containing Pt and alumina between the high-purity alumina base material and the Pt film. Since the layer formed by firing is intercalated, the alumina powder of the underlayer is combined with the high-purity alumina base material, while the Pt particles of the underlayer are melt-bonded with Pt of the upper layer, so that the high-purity alumina matrix as a whole is formed. The bonding strength between the material and the Pt film is significantly improved.
【図１】本発明を適用したメタルハライドランプの封止
部の断面図FIG. 1 is a sectional view of a sealing portion of a metal halide lamp to which the present invention is applied.
【図２】図１の要部拡大図FIG. 2 is an enlarged view of a main part of FIG.
１…発光管、２…開口、３…絶縁キャップ、６，７…Ｐ
t膜、１０…下地層、１１…Ｐt粒子、１２…Ａl2Ｏ3粒
子。1 ... Arc tube, 2 ... Opening, 3 ... Insulation cap, 6, 7 ... P
t film, 10 ... Underlayer, 11 ... Pt particles, 12 ... Al 2 O 3 particles.
Claims (4)
６％以上の未焼成のアルミナ母材とＰｔ膜との間に設け
られる下地層を形成するためのペーストであって、この
ペーストはＰｔ微粉末１００重量部に対して高純度アル
ミナ微粉末を５〜１５重量部添加し、更にこれにビヒク
ル及び有機溶剤を加えて混練してなることを特徴とする
Ｐt膜形成用下地ペースト。1. A purity 9 constituting an insulating cap of a discharge lamp.
A paste for forming an undercoat layer provided between the 6% or more unfired the alumina base material and the Pt film, a high-purity alumina powder with respect to the paste Pt powder 100 parts by weight A base paste for forming a Pt film, which is obtained by adding 5 to 15 parts by weight, and further adding a vehicle and an organic solvent to the mixture and kneading.
上の既焼成のアルミナ母材とＰｔ膜との間に設けられる
下地層を形成するためのペーストであって、このペース
トはＰｔ微粉末１００重量部に対して高純度アルミナ微
粉末を５〜１５重量部、ＳｉＯ2微粉末を２．５〜２０
重量部添加し、更にこれにビヒクル及び有機溶剤を加え
て混練してなることを特徴とするＰt膜形成用下地ペー
スト。2. A purity of 96% or more constituting an arc tube of a discharge lamp.
A paste for forming an undercoat layer provided between the pre-baking of the alumina base material and the Pt film above, the paste 5 a high-purity alumina powder with respect to Pt fine powder 100 parts by weight 15 parts by weight of SiO 2 fine powder 2.5 to 20
A base paste for forming a Pt film, characterized by comprising adding parts by weight, and further kneading with a vehicle and an organic solvent.
６％以上の未焼成のアルミナ母材の表面に、Ｐｔ微粉末
１００重量部に対して高純度アルミナ微粉末を５〜１５
重量部添加し、更にこれにビヒクル及び有機溶剤を加え
て混練してなる下地ペーストを塗布し、次いで、この下
地ペーストの上にＰｔペーストを重ねて塗布し、この
後、前記未焼成の高純度アルミナ母材、下地ペースト及
びＰｔペーストを同時に焼成するようにしたことを特徴
とするＰｔ膜形成方法。3. A purity 9 constituting an insulating cap of a discharge lamp.
The surface of 6% or more unfired Alumina base material, a high-purity alumina powder with respect to Pt fine powder 100 parts by weight of 5 to 15
Parts by weight, and further, a vehicle and an organic solvent are added and kneaded to apply a base paste, and then a Pt paste is applied over the base paste, and then the unfired high-purity A method for forming a Pt film, which comprises simultaneously firing an alumina base material, a base paste and a Pt paste.
上の既焼成のアルミナ母材の表面に、Ｐｔ微粉末１００
重量部に対して高純度アルミナ微粉末を５〜１５重量
部、ＳｉＯ2微粉末を２．５〜２０重量部添加し、更に
これにビヒクル及び有機溶剤を加えて混練してなる下地
ペーストを塗布し、次いで、この下地ペーストの上にＰ
ｔペーストを重ねて塗布し、この後、前記下地ペースト
及びＰｔペーストを同時に焼成するようにしたことを特
徴とするＰｔ膜形成方法。4. A purity of 96% or more constituting an arc tube of a discharge lamp.
On the surface of the already fired the alumina base material of the upper, Pt powder 100
5 to 15 parts by weight of high-purity alumina fine powder and 2.5 to 20 parts by weight of SiO 2 fine powder are added to parts by weight, and a vehicle and an organic solvent are further added to the mixture to apply a base paste. And then P on the base paste
A method for forming a Pt film, characterized in that t paste is applied in an overlapping manner, and thereafter, the base paste and the Pt paste are simultaneously fired.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03393693A JP3402482B2 (en) | 1993-02-01 | 1993-02-01 | Base paste for forming Pt film and method for forming Pt film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03393693A JP3402482B2 (en) | 1993-02-01 | 1993-02-01 | Base paste for forming Pt film and method for forming Pt film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06231730A JPH06231730A (en) | 1994-08-19 |
| JP3402482B2 true JP3402482B2 (en) | 2003-05-06 |
Family
ID=12400401
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03393693A Expired - Fee Related JP3402482B2 (en) | 1993-02-01 | 1993-02-01 | Base paste for forming Pt film and method for forming Pt film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3402482B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69822058D1 (en) * | 1997-09-19 | 2004-04-08 | Matsushita Electric Industrial Co Ltd | High-pressure discharge lamp and method for producing the same |
| EP3030061B1 (en) * | 2013-07-29 | 2021-01-06 | Kyocera Corporation | Wiring substrate, wiring substrate with lead, and electronic device |
| JP2023005498A (en) * | 2021-06-29 | 2023-01-18 | ニッコー株式会社 | Wiring board and manufacturing method thereof |
-
1993
- 1993-02-01 JP JP03393693A patent/JP3402482B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06231730A (en) | 1994-08-19 |
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