JPH04246105A - Silver-platinum composite pulverized powder and its production - Google Patents
Silver-platinum composite pulverized powder and its productionInfo
- Publication number
- JPH04246105A JPH04246105A JP3025690A JP2569091A JPH04246105A JP H04246105 A JPH04246105 A JP H04246105A JP 3025690 A JP3025690 A JP 3025690A JP 2569091 A JP2569091 A JP 2569091A JP H04246105 A JPH04246105 A JP H04246105A
- Authority
- JP
- Japan
- Prior art keywords
- platinum
- silver
- powder
- fine powder
- fine
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- IHWJXGQYRBHUIF-UHFFFAOYSA-N [Ag].[Pt] Chemical compound [Ag].[Pt] IHWJXGQYRBHUIF-UHFFFAOYSA-N 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 30
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006722 reduction reaction Methods 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052709 silver Inorganic materials 0.000 claims description 9
- 239000004332 silver Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 5
- 239000010946 fine silver Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 229910000679 solder Inorganic materials 0.000 description 7
- 238000013508 migration Methods 0.000 description 5
- 230000005012 migration Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000010944 silver (metal) Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 229960005070 ascorbic acid Drugs 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
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- HAAYBYDROVFKPU-UHFFFAOYSA-N silver;azane;nitrate Chemical compound N.N.[Ag+].[O-][N+]([O-])=O HAAYBYDROVFKPU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は微細な銀−白金複合微粉
末とその製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fine silver-platinum composite powder and a method for producing the same.
【０００２】0002
【従来の技術】電子工業の分野では、厚膜回路を作製す
るのに導電性ペーストが利用されていて現在の主流は銀
とパラジウム又は銀と白金の微粉末を混合したペースト
である。このＡｇ−Ｐｔペーストにおいて白金を混合す
る理由は、マイグレーションとハンダクワレを防止する
ためであり、このためには ０．５〜２０％の白金を加
える必要がある。BACKGROUND OF THE INVENTION In the field of electronics industry, conductive pastes are used to fabricate thick film circuits, and the current mainstream paste is a mixture of fine powders of silver and palladium or silver and platinum. The reason why platinum is mixed in this Ag-Pt paste is to prevent migration and solder cracking, and for this purpose it is necessary to add 0.5 to 20% platinum.
【０００３】白金の添加は上記２点で優れた効果がある
が、銀と白金の微粉末を混合する方法では、白金を均一
に分散することが困難なためその効果を十分に生かせな
いという欠点を有していた。Addition of platinum has excellent effects on the above two points, but the method of mixing fine powders of silver and platinum has the disadvantage that it is difficult to uniformly disperse platinum, so the effects cannot be fully utilized. It had
【０００４】0004
【発明の目的】本発明は上記の欠点を解消せんがために
なされたものであり、Ａｇ−Ｐｔペーストの特性を改善
するために銀微粉末中に白金を均一に分散させた銀−白
金複合微粉末及びその製造方法を提供せんとするもので
ある。OBJECT OF THE INVENTION The present invention has been made to solve the above-mentioned drawbacks, and in order to improve the properties of Ag-Pt paste, a silver-platinum composite in which platinum is uniformly dispersed in fine silver powder is developed. The present invention aims to provide a fine powder and a method for producing the same.
【０００５】[0005]
【問題点を解決するための手段】本発明は銀微粉末中に
白金を均一に分散させた銀−白金複合微粉末及び銀微粉
末中に白金を均一に分散させるのに好ましくは化学還元
または水素還元を利用し、さらに合金化させるのに ２
００〜 ５００℃の範囲で熱処理することを特徴とする
ものである。[Means for Solving the Problems] The present invention provides a silver-platinum composite fine powder in which platinum is uniformly dispersed in a silver fine powder, and a chemical reduction method or a method for uniformly dispersing platinum in a silver fine powder. To further alloy by using hydrogen reduction 2
It is characterized by heat treatment in the range of 00 to 500°C.
【０００６】[0006]
【作用】而して銀微粉末中に白金を均一に分散させる理
由は、ペーストとして用いたとき白金が均一に分散した
銀−白金膜を形成するためである。[Operation] The reason why platinum is uniformly dispersed in the fine silver powder is that when used as a paste, a silver-platinum film in which platinum is uniformly dispersed is formed.
【０００７】また銀微粉末中に白金を均一に分散させる
のに水素還元を利用する理由は、銀微粉末中に白金を均
一に分散させる条件を選ぶのに、この方法が適している
からであり、化学還元を利用する理由は、銀微粉末中に
白金を均一に分散させるのに還元剤の種類により種々の
条件を選ぶことができるためである。また銀−白金複合
微粉末を ２００〜 ５００℃の範囲で熱処理する理由
は、合金化させるのに ２００℃以下では低すぎて拡散
が十分に起こらず、５００℃以上では微粉末同士の焼結
が始まるためである。ここで本発明の実施例について説
明する。[0007] Furthermore, the reason why hydrogen reduction is used to uniformly disperse platinum in fine silver powder is that this method is suitable for selecting conditions for uniformly dispersing platinum in fine silver powder. The reason why chemical reduction is used is that various conditions can be selected depending on the type of reducing agent to uniformly disperse platinum in fine silver powder. Furthermore, the reason why silver-platinum composite fine powder is heat-treated at a temperature in the range of 200 to 500°C is that below 200°C is too low to cause sufficient diffusion, and above 500°C the fine powders will not sinter. This is to begin. Examples of the present invention will now be described.
【０００８】[0008]
【実施例１】ジニトロジアミン白金水溶液（５０ｇ／ｌ
）３０ｍｌにゼラチン ０．５ｇを加えこれを撹拌しな
がら水素化ホウ素ナトリウムを加えて白金が（粒径 １
００〜 ５００Å）均一に分散したコロイド液を作った
。[Example 1] Dinitrodiamine platinum aqueous solution (50 g/l
) Add 0.5 g of gelatin to 30 ml, add sodium borohydride while stirring, and add platinum (particle size 1
00-500 Å) A uniformly dispersed colloidal liquid was prepared.
【０００９】このコロイド液に硝酸銀水溶液（５０ｇ／
ｌ） １，１７０ｍｌ を加え、この混合液をオート
クレーブ中に装入し、Ｎ２雰囲気中で １５０℃に加熱
した後、Ｈ２ を２０ｋｇ／ｃｍ２ 加圧し、還元した
。冷却後、濾過、水洗して得られた粉末は銀微粉末中に
白金が均一微細に分散したものであった。また得られた
微粉末を走査電子顕微鏡観察、Ｘ線回折、及び化学分析
を行った結果、平均粒径 ０．６ミクロンのほぼ球状の
Ａｇ−Ｐｔ ２．０％複合微粉末となっていた。[0009] Silver nitrate aqueous solution (50g/
After adding 1,170 ml of 1,170 ml of this mixed solution into an autoclave and heating it to 150° C. in a N2 atmosphere, 20 kg/cm2 of H2 was applied to reduce the mixture. After cooling, filtration and washing with water resulted in a powder in which platinum was uniformly and finely dispersed in fine silver powder. Further, the obtained fine powder was subjected to scanning electron microscopy, X-ray diffraction, and chemical analysis, and as a result, it was found to be a substantially spherical Ag-Pt 2.0% composite fine powder with an average particle size of 0.6 microns.
【００１０】0010
【実施例２】ジニトロジアミン白金水溶液（５０ｇ／ｌ
） ２５２ｍｌこれにゼラチン ３．０ｇを加え撹拌し
ながら水素化ホウ素ナトリウムを加えて白金（粒径 １
００〜 ５００Å） が均一に分散したコロイド液を作
った。[Example 2] Dinitrodiamine platinum aqueous solution (50 g/l
) To 252 ml of this, add 3.0 g of gelatin, add sodium borohydride while stirring, and add platinum (particle size 1
A colloidal solution in which 00 to 500 Å) was uniformly dispersed was prepared.
【００１１】このコロイド液にＬ−アスコルビン酸溶液
（ １００ｇ／ｌ） ５００ｍｌを加え、撹拌しな
がらアンモニア性硝酸銀錯体溶液（５０ｇ／ｌ） １，
４９３ｍｌを加え還元した。濾過、水洗後、得られた粉
末は銀微粉末中に白金が均一微細に分散したものであっ
た。また得られた微粉末を走査電子顕微鏡観察、Ｘ線回
折、及び化学分析を行った結果、平均粒径 ０．４ミク
ロンのほぼ球状のＡｇ−Ｐｔ２０％複合微粉末となって
いた。[0011] 500 ml of L-ascorbic acid solution (100 g/l) was added to this colloidal solution, and while stirring, an ammoniacal silver nitrate complex solution (50 g/l) was added.
493 ml was added and reduced. After filtration and water washing, the obtained powder had platinum uniformly and finely dispersed in fine silver powder. Further, the obtained fine powder was subjected to scanning electron microscopy, X-ray diffraction, and chemical analysis, and as a result, it was found to be a substantially spherical Ag-Pt 20% composite fine powder with an average particle size of 0.4 microns.
【００１２】0012
【実施例３】実施例１で作ったＡｇ−Ｐｔ ２．０％複
合微粉末を ３５０℃で１時間熱処理を行った。[Example 3] The Ag-Pt 2.0% composite fine powder prepared in Example 1 was heat treated at 350°C for 1 hour.
【００１３】得られた粉末は焼結されておらず微細なも
のであって、これを走査顕微鏡観察及びＸ線回折を行っ
た結果、平均粒径 １．０ミクロンのほぼ球状のＡｇ−
Ｐｔ２．０％合金微粉末となっていた。The obtained powder was not sintered and was fine, and as a result of scanning microscope observation and X-ray diffraction, it was found that the powder was approximately spherical with an average particle size of 1.0 microns.
It was a 2.0% Pt alloy fine powder.
【００１４】実施例１及び３で作ったＡｇ−Ｐｔ ２．
０％複合及び合金粉末をペースト化し、アルミナ基板上
にスクリーン印刷後、 ９００℃で３０分間焼成してＡ
ｇ−Ｐｔ厚膜回路を形成した。この回路を使ってマイグ
レーション及びハンダクワレテストを行った結果、マイ
グレーションが発生するまでの平均時間は、Ａｇ−Ｐｔ
２．０％複合微粉末で８分２０秒、Ａｇ−Ｐｔ ２．０
％合金微粉末で７分３０秒でハンダ浸漬テストを１０回
行った後のハンダクワレはほとんど見られなかった。Ag-Pt prepared in Examples 1 and 3 2.
0% composite and alloy powder were made into a paste, screen printed on an alumina substrate, and then baked at 900℃ for 30 minutes to obtain A.
A g-Pt thick film circuit was formed. As a result of performing migration and solder corrosion tests using this circuit, the average time until migration occurs is as follows: Ag-Pt
8 minutes 20 seconds with 2.0% composite fine powder, Ag-Pt 2.0
After conducting the solder immersion test 10 times for 7 minutes and 30 seconds using % alloy fine powder, hardly any solder cracks were observed.
【００１５】尚、本発明における銀微粉末中に分散され
た白金の大きさは限定するものではないが、ペーストと
して使用したときの特性上、粒径１０００Å以下がより
好ましい。Although the size of platinum dispersed in the silver fine powder in the present invention is not limited, it is more preferable to have a particle size of 1000 Å or less in view of the properties when used as a paste.
【００１６】[0016]
【従来例】平均粒径 １．０ミクロンのＡｇ微粉末と平
均粒径 １．２ミクロンのＰｔ微粉末をＡｇ−Ｐｔ ２
．０％の割合に混合、ペースト化し、アルミナ基板上に
スクリーン印刷後、 ９００℃で３０分間焼成してＡｇ
−Ｐｔ厚膜回路を使ってマイグレーション及びハンダク
ワレテストを行った結果、マイグレーションが発生する
までの平均時間が２分４５秒でハンダ浸漬テストを５回
行った後、かなりのハンダクワレが見られた。[Conventional example] Ag fine powder with an average particle size of 1.0 microns and fine Pt powder with an average particle size of 1.2 microns are mixed into Ag-Pt 2
．． After mixing to a ratio of 0% and making it into a paste, screen printing it on an alumina substrate and baking it at 900℃ for 30 minutes to make Ag.
- As a result of conducting migration and solder cracking tests using Pt thick film circuits, the average time until migration occurred was 2 minutes and 45 seconds, and considerable solder cracking was observed after 5 solder immersion tests. .
【００１７】[0017]
【発明の効果】上記の説明で明らかなように本発明の銀
−白金複合粉末は銀微粉末中に白金を均一に分散させた
銀−白金複合微粉末であるので、ペーストに利用すると
、従来得られなかった白金が均一に分散した銀−白金膜
を形成できるので、従来の粉末にとって代わることので
きる画期的なものと言える。また本発明の製造方法は、
銀−白金複合粉末を容易に製造できるものである。Effects of the Invention As is clear from the above explanation, the silver-platinum composite powder of the present invention is a silver-platinum composite fine powder in which platinum is uniformly dispersed in fine silver powder. Since it is possible to form a silver-platinum film in which platinum that could not be obtained is uniformly dispersed, it can be said to be an epoch-making product that can replace conventional powders. Furthermore, the manufacturing method of the present invention includes:
Silver-platinum composite powder can be easily produced.
Claims (5)
銀−白金複合微粉末。1. Silver-platinum composite fine powder in which platinum is uniformly dispersed in silver fine powder.
を特徴とする特許請求の範囲第１項記載の銀−白金複合
微粉末。2. The silver-platinum composite fine powder according to claim 1, wherein the silver-platinum composite powder is heat-treated.
範囲であることを特徴とする特許請求の範囲第２項記載
の銀−白金複合微粉末。3. The silver-platinum composite fine powder according to claim 2, wherein the heat treatment temperature is in the range of 200 to 500°C.
際に還元反応を利用することを特徴とする銀−白金複合
微粉末の製造方法。4. A method for producing a silver-platinum composite fine powder, which comprises utilizing a reduction reaction when uniformly dispersing platinum in the silver fine powder.
際の還元反応が化学還元又は水素還元であることを特徴
とする特許請求の範囲第４項記載の銀−白金複合微粉末
の製造方法。5. Production of the silver-platinum composite fine powder according to claim 4, wherein the reduction reaction when platinum is uniformly dispersed in the silver fine powder is chemical reduction or hydrogen reduction. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3025690A JPH04246105A (en) | 1991-01-26 | 1991-01-26 | Silver-platinum composite pulverized powder and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3025690A JPH04246105A (en) | 1991-01-26 | 1991-01-26 | Silver-platinum composite pulverized powder and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04246105A true JPH04246105A (en) | 1992-09-02 |
Family
ID=12172788
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3025690A Pending JPH04246105A (en) | 1991-01-26 | 1991-01-26 | Silver-platinum composite pulverized powder and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04246105A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2015174462A1 (en) * | 2014-05-16 | 2017-05-25 | 国立研究開発法人産業技術総合研究所 | Thermoelectric conversion element and thermoelectric conversion module |
-
1991
- 1991-01-26 JP JP3025690A patent/JPH04246105A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPWO2015174462A1 (en) * | 2014-05-16 | 2017-05-25 | 国立研究開発法人産業技術総合研究所 | Thermoelectric conversion element and thermoelectric conversion module |
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