JPH02141508A - Manufacture of silver-platinum complex fine powder - Google Patents
Manufacture of silver-platinum complex fine powderInfo
- Publication number
- JPH02141508A JPH02141508A JP29436288A JP29436288A JPH02141508A JP H02141508 A JPH02141508 A JP H02141508A JP 29436288 A JP29436288 A JP 29436288A JP 29436288 A JP29436288 A JP 29436288A JP H02141508 A JPH02141508 A JP H02141508A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- platinum
- fine powder
- water solution
- solution
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 24
- IHWJXGQYRBHUIF-UHFFFAOYSA-N [Ag].[Pt] Chemical compound [Ag].[Pt] IHWJXGQYRBHUIF-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 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 49
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 20
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 20
- 239000004332 silver Substances 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 6
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 6
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 6
- 150000003058 platinum compounds Chemical class 0.000 claims abstract description 4
- 229940100890 silver compound Drugs 0.000 claims abstract description 4
- 150000003379 silver compounds Chemical class 0.000 claims abstract description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract 3
- 239000012279 sodium borohydride Substances 0.000 claims abstract 3
- 239000002131 composite material Substances 0.000 claims description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 3
- HAAYBYDROVFKPU-UHFFFAOYSA-N silver;azane;nitrate Chemical compound N.N.[Ag+].[O-][N+]([O-])=O HAAYBYDROVFKPU-UHFFFAOYSA-N 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 3
- 239000000084 colloidal system Substances 0.000 abstract 3
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 7
- 229910000679 solder Inorganic materials 0.000 description 7
- 238000013508 migration Methods 0.000 description 6
- 230000005012 migration Effects 0.000 description 6
- 239000010946 fine silver Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000010944 silver (metal) Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 229910010277 boron hydride Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は微細な銀−白金複合微粉末の製造方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing fine silver-platinum composite fine powder.
（従来の技術とその問題点）
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使われているのは銀と白金
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
ンとハンダクヮレを防止するためであり、このためには
数％〜１０％の白金を加える必要がある。(Conventional technology and its problems) In the field of electronics industry, conductive paste is used to create thick film circuits, and the paste currently in use is a mixture of fine powders of 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 platinum in an amount of several to 10%.
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。Although the addition of platinum has excellent effects in the above two points, the method of mixing fine powders of silver and platinum has the disadvantage that it is difficult to disperse platinum evenly, so the effects cannot be fully utilized. was.
（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 provided. The present invention aims to provide a method for producing fine powder.
（問題点を解決するための手段）
本発明の銀−白金複合微粉末の製造方法は、白金化合物
水溶液に水素化ホウ素す） ＩＪウムを加えて白金コロ
イド液とし、このコロイド液にＬ−アスコルビン酸又は
Ｌ−アスコルビン酸塩を加え、更に銀化合物水溶液を加
えて銀を還元することを特徴とするものである。(Means for Solving the Problems) The method for producing the silver-platinum composite fine powder of the present invention involves adding boron hydride to an aqueous solution of a platinum compound to obtain a platinum colloidal solution, and adding L-ascorbin to this colloidal solution. This method is characterized by adding an acid or L-ascorbate and further adding an aqueous silver compound solution to reduce silver.
（作用）
銀微粉末中に白金を均一に分散させるのにＬアスコルビ
ン酸又はＬ−アスコルビン酸塩による還元を利用する理
由は、銀微粉末中に白金を均一に分散させるのにＬ−ア
スコルビン酸又はＬ−アスコルビン酸塩の還元力が最適
であるためである。(Function) The reason why reduction with L-ascorbic acid or L-ascorbate is used to uniformly disperse platinum in fine silver powder is that L-ascorbic acid is used to uniformly disperse platinum in fine silver powder. Or, this is because the reducing power of L-ascorbate is optimal.
ここで本発明の実施例について説明する。Examples of the present invention will now be described.
（実施例）
塩化白金酸水溶液（５０ｇ／β’） ４０ｄ、を撹拌し
ながら水素化ホウ素ナトリウムを加えて白金（粒径１０
０〜５００人）が均一に分散したコロイド液を作った。(Example) Platinum (particle size 10
(0 to 500 people) made a uniformly dispersed colloidal solution.
このコロイド液にＬ−アスコルビン酸水溶液（１００ｇ
／ Ａ ）１５０−を加え、撹拌しながらアンモニア
性硝酸銀錯体水溶液（５０ｇ ／ Ｒ） ７００ｍｆ
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。Add L-ascorbic acid aqueous solution (100 g
/A) Add 150- and while stirring, ammoniacal silver nitrate complex aqueous solution (50g/R) 700mf
was added and reduced. After filtration and water washing, the obtained powder had platinum uniformly and finely dispersed in fine silver powder.
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０．４μｍのほぼ
球状のＡｇ−Ｐｔ５％複合微粉末となっていた。In addition, the obtained fine powder was observed using a scanning electron microscope, X-ray diffraction,
As a result of chemical analysis, it was found to be a substantially spherical Ag-Pt 5% composite fine powder with an average particle size of 0.4 μm.
実施例で作ったＡｇ−Ｐｔ５％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Ａｇ−Ｐｔ厚膜回路を形成した。The Ag-Pt 5% composite and alloy powder made in the example were made into a paste, and after screen printing on an alumina substrate,
An Ag--Pt thick film circuit was formed by firing at .degree. C. for 30 minutes.
この回路を使ってＡｇの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ずる
までの平均時間は、Ａｇ−Ｐｔ５％複合微粉末で１０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。As a result of conducting Ag migration and solder corrosion tests using this circuit, the average time until migration occurred was 10 minutes and 30 seconds with Ag-Pt 5% composite fine powder after 10 solder immersion tests. Hardly any solder cracks were observed.
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 the platinum dispersed in the silver fine powder in the present invention is not limited, a particle size of 1000 Å or less is more preferable in view of the characteristics when used as a paste.
（従来例）
平均粒径１．０μｍのＡｇ微粉末と平均粒径１．２μｍ
のＰｔ微粉末をＡｇ−Ｐｔ５％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３分１０秒でハ
ンダ浸漬テストを５回行った後、かなりのハンダクヮレ
が見られた。(Conventional example) Ag fine powder with an average particle size of 1.0 μm and an average particle size of 1.2 μm
Pt fine powder was mixed at a ratio of 5% Ag-Pt, made into a paste, screen printed on an alumina substrate, baked at 900℃ for 30 minutes, and tested for migration and solder cracking using an Ag-Pt thick film circuit. As a result, the average time until migration occurred was 3 minutes and 10 seconds, and considerable solder cracking was observed after conducting the solder immersion test five times.
尚、本発明で得られた銀−白金複合微粉末を２００〜５
００℃で熱処理した後、ペースト化すれば、Ａｇのマイ
グレーションが発生するまでの時間を一層長くすること
ができるものである。Incidentally, the silver-platinum composite fine powder obtained in the present invention was
If it is made into a paste after being heat-treated at 00° C., it is possible to further lengthen the time until Ag migration occurs.
また上記実施例では白金化合物水溶液として塩化白金酸
水溶液、銀化合物水溶液としてアンモニア性硝酸銀錯体
水溶液を用いたが、本発明はこれに限るものではない。Further, in the above embodiments, a chloroplatinic acid aqueous solution was used as the platinum compound aqueous solution, and an ammoniacal silver nitrate complex aqueous solution was used as the silver compound aqueous solution, but the present invention is not limited to this.
（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。(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.
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。Moreover, the manufacturing method of the present invention allows silver-platinum composite powder to be easily manufactured.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
て白金コロイド液とし、このコロイド液にＬ−アスコル
ビン酸又はＬ−アスコルビン酸塩を加え、更に銀化合物
水溶液を加えて銀を還元することを特徴とする銀−白金
複合微粉末の製造方法。1. Adding sodium borohydride to an aqueous platinum compound solution to obtain a platinum colloidal solution, adding L-ascorbic acid or L-ascorbate to this colloidal solution, and further adding an aqueous silver compound solution to reduce silver. A method for producing a silver-platinum composite fine powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29436288A JP2613282B2 (en) | 1988-11-21 | 1988-11-21 | Method for producing silver-platinum composite fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29436288A JP2613282B2 (en) | 1988-11-21 | 1988-11-21 | Method for producing silver-platinum composite fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02141508A true JPH02141508A (en) | 1990-05-30 |
| JP2613282B2 JP2613282B2 (en) | 1997-05-21 |
Family
ID=17806730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29436288A Expired - Lifetime JP2613282B2 (en) | 1988-11-21 | 1988-11-21 | Method for producing silver-platinum composite fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2613282B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013500862A (en) * | 2009-08-05 | 2013-01-10 | ビー・エイ・エス・エフ、コーポレーション | Production of diesel oxidation catalyst by precipitation of colloidal nanoparticles |
| CN104416164A (en) * | 2013-09-04 | 2015-03-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Platinum black and method for preparing same |
-
1988
- 1988-11-21 JP JP29436288A patent/JP2613282B2/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013500862A (en) * | 2009-08-05 | 2013-01-10 | ビー・エイ・エス・エフ、コーポレーション | Production of diesel oxidation catalyst by precipitation of colloidal nanoparticles |
| US9687818B2 (en) | 2009-08-05 | 2017-06-27 | Basf Corporation | Preparation of diesel oxidation catalyst via deposition of colloidal nanoparticles |
| CN104416164A (en) * | 2013-09-04 | 2015-03-18 | 中国科学院苏州纳米技术与纳米仿生研究所 | Platinum black and method for preparing same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2613282B2 (en) | 1997-05-21 |
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