JPH04246106A - Silver-palladium-platinum composite pulverized powder and its production - Google Patents
Silver-palladium-platinum composite pulverized powder and its productionInfo
- Publication number
- JPH04246106A JPH04246106A JP9125691A JP2569191A JPH04246106A JP H04246106 A JPH04246106 A JP H04246106A JP 9125691 A JP9125691 A JP 9125691A JP 2569191 A JP2569191 A JP 2569191A JP H04246106 A JPH04246106 A JP H04246106A
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- platinum
- silver
- 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 40
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 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 73
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 35
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 28
- 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
- 239000001257 hydrogen Substances 0.000 claims abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000010946 fine silver Substances 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 description 10
- 239000006072 paste Substances 0.000 description 10
- 229910000679 solder Inorganic materials 0.000 description 8
- 238000013508 migration Methods 0.000 description 6
- 230000005012 migration Effects 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002156 mixing Methods 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
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 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
- 238000000034 method Methods 0.000 description 2
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 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
- 238000005275 alloying Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 238000001816 cooling Methods 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
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000002265 prevention Effects 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
- 238000005245 sintering Methods 0.000 description 1
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は微細な銀−パラジウム−
白金複合微粉末とその製造方法に関するものである。[Industrial Application Field] The present invention is based on fine silver-palladium
This invention relates to a platinum composite fine powder and its manufacturing method.
【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
とパラジウムの微粉末を混合したペーストであるが、銀
とパラジウムと白金の微粉末を混合したペーストもある
。このＡｇ−Ｐｄ−Ｐｔペーストにおいてパラジウムを
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１０〜３０％のパラジ
ウムを加える必要がある。また、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防止をさらに促進す
るためであり、このためには ０．１〜５％の白金を加
える必要がある。[Prior Art] In the field of electronics industry, conductive paste is used to fabricate thick film circuits, and the current mainstream is a paste containing a mixture of fine powders of silver and palladium. There is also a paste made by mixing fine powder. The reason why palladium is mixed in this Ag-Pd-Pt paste is to prevent migration and solder cracking, and for this purpose it is necessary to add 10 to 30% palladium. Further, the reason for mixing platinum is to further promote migration and prevention of solder cracking, and for this purpose it is necessary to add 0.1 to 5% platinum.
【０００３】パラジウムと白金の添加は上記２点で優れ
た効果があるが、銀とパラジウムと白金の微粉末を混合
する方法では、パラジウムと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 palladium and platinum has excellent effects in the above two points, but the method of mixing fine powders of silver, palladium, and platinum has difficulty dispersing palladium and platinum uniformly, so the effect is not achieved. It had the disadvantage of not being able to make full use of it.
【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−Ｐｄ−Ｐｔペーストの特性
を改善するために銀微粉末中にパラジウムと白金を均一
に分散させた銀−パラジウム−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 was made to solve the above-mentioned drawbacks, and in order to improve the properties of Ag-Pd-Pt paste, palladium and platinum were uniformly dispersed in fine silver powder. The present invention aims to provide a fine silver-palladium-platinum composite 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
パラジウムと白金を均一に分散させた銀−パラジウム−
白金複合微粉末及び銀微粉末中にパラジウムと白金を均
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 ２００〜 ６００
℃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-palladium-based silver powder in which palladium and platinum are uniformly dispersed in fine silver powder.
Preferably, chemical reduction or hydrogen reduction is used to uniformly disperse palladium and platinum in the platinum composite fine powder and silver fine powder, and further alloying is performed at 200 to 600.
It is characterized by heat treatment in the range of °C.
【０００６】[0006]
【作用】而して銀微粉末中にパラジウムと白金を均一に
分散させる理由は、ペーストとして用いたときパラジウ
ムと白金が均一に分散した銀−パラジウム−白金膜を形
成するためである。[Operation] The reason why palladium and platinum are uniformly dispersed in fine silver powder is that when used as a paste, a silver-palladium-platinum film is formed in which palladium and platinum are uniformly dispersed.
【０００７】また銀微粉末中にパラジウムと白金を均一
に分散させるのに水素還元を利用する理由は、銀微粉末
中にパラジウムと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、銀微粉末中にパラジウムと白金を均一に分
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−パラジウム−白金複合微
粉末を ２００〜 ６００℃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、 ６００℃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 palladium and platinum in fine silver powder is that this method is suitable for selecting conditions for uniformly dispersing palladium and 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 palladium and platinum in fine silver powder. Furthermore, the reason why silver-palladium-platinum composite fine powder is heat-treated in the range of 200 to 600°C is that temperatures below 200°C are too low to cause sufficient diffusion, while temperatures above 600°C cause sintering of the fine powders. This is because the knot begins. Examples of the present invention will now be described.
【０００８】[0008]
【実施例１】硝酸パラジウム水溶液（５０ｇ／ｌ） １
８０ｍｌとジニトロジアミン白金水溶液（５０ｇ／ｌ）
４２ｍｌとゼラチン １．７ｇ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パラジウムと白金が
（粒径 １００〜 ５００Å） 均一に分散したコロイ
ド液を作った。[Example 1] Palladium nitrate aqueous solution (50g/l) 1
80ml and dinitrodiamine platinum aqueous solution (50g/l)
42 ml and 1.7 g of gelatin were added, and while stirring, sodium borohydride was added to prepare a colloidal solution in which palladium and platinum (particle size: 100 to 500 Å) were uniformly dispersed.
【０００９】このコロイド液に硝酸銀水溶液（５０ｇ／
ｌ） ９７８ｍｌ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 １７０℃に加熱した
後、Ｈ２ を１７ｋｇ／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パラジ
ウムと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 ０．５ミクロンのほぼ
球状のＡｇ−Ｐｄ１５％−Ｐｔ ３．５％複合微粉末と
なっていた。[0009] Silver nitrate aqueous solution (50g/
1) 978 ml was added, and this mixed solution was placed in an autoclave and heated to 170° C. in a N2 atmosphere, and then H2 was pressurized at 17 kg/cm2 to reduce it. After cooling, filtration and washing with water resulted in a powder in which palladium and platinum were uniformly and finely dispersed in fine silver powder. Furthermore, the obtained fine powder was subjected to scanning electron microscopy, X-ray diffraction, and chemical analysis, and it was found that it was a nearly spherical Ag-Pd 15%-Pt 3.5% composite fine powder with an average particle size of 0.5 microns. was.
【００１０】0010
【実施例２】硝酸パラジウム水溶液（５０ｇ／ｌ） ２
４０ｍｌとジニトリジアミン白金水溶液（５０ｇ／ｌ）
１２ｍｌとゼラチン ２．５ｇ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パラジウムと白金（
粒径 １００〜 ５００Å） が均一に分散したコロイ
ド液を作った。[Example 2] Palladium nitrate aqueous solution (50 g/l) 2
40ml and dinitridiamine platinum aqueous solution (50g/l)
Add 12 ml and 2.5 g of gelatin, add sodium borohydride while stirring, and add palladium and platinum (
A colloidal liquid in which particles (with a particle size of 100 to 500 Å) were 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） ９４
８ｍｌを加え還元した。濾過、水洗後、得られた粉末は
銀微粉末中にパラジウムと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
．７ミクロンのほぼ球状のＡｇ−Ｐｄ２０％−Ｐｔ１％
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.
8 ml was added and reduced. After filtration and washing with water, the obtained powder was a finely dispersed palladium and platinum in fine silver powder. Furthermore, as a result of scanning electron microscopy, X-ray diffraction, and chemical analysis of the obtained fine powder, the average particle size was 0.
．． 7 micron almost spherical Ag-Pd20%-Pt1%
It was a composite fine powder.
【００１２】0012
【実施例３】実施例１で作ったＡｇ−Ｐｄ１５％−Ｐｔ
３．５％複合微粉末を ３５０℃で１時間熱処理を行
った。[Example 3] Ag-Pd15%-Pt made in Example 1
The 3.5% composite fine powder 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 １．１ミクロンのほぼ球状のＡｇ−
Ｐｄ１５％−Ｐｔ ３．５％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 1.1 microns.
It was a 15% Pd-3.5% Pt alloy fine powder.
【００１４】実施例１及び３で作ったＡｇ−Ｐｄ１５％
−Ｐｔ ３．５％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−Ｐｄ−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−Ｐｄ１５％、Ｐｔ ３．５％複合微粉末
で１０分３０秒、Ａｇ−Ｐｄ−Ｐｔ ３．５％合金微粉
末で９分４０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-Pd 15% made in Examples 1 and 3
-Pt 3.5% composite and alloy powder were made into a paste, screen printed on an alumina substrate, and then baked at 900°C for 30 minutes to form an Ag-Pd-Pt thick film circuit. As a result of conducting migration and solder crack tests using this circuit, the average time until migration occurred was 10 minutes and 30 seconds for Ag-Pd 15%, Pt 3.5% composite fine powder, Ag-Pd-Pt Almost no solder cracks were observed after conducting the solder immersion test 10 times for 9 minutes and 40 seconds using 3.5% alloy fine powder.
【００１５】尚、本発明における銀微粉末中に分散され
たパラジウムと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１０００
Å以下がより好ましい。[0015] Although the sizes of palladium and platinum dispersed in the silver fine powder in the present invention are not limited, due to the characteristics when used as a paste, the particle size is 1000.
Å or less is more preferable.
【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Ｐｄ微粉末と平均粒径 ０．
５ミクロンのＰｔ微粉末をＡｇ−Ｐｄ１５％−Ｐｔ ３
．５％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
−Ｐｄ−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５分３０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, Pd fine powder with an average particle size of 1.2 microns, and an average particle size of 0.
5 micron Pt fine powder is Ag-Pd15%-Pt 3
．． It was mixed at a ratio of 5%, made into a paste, screen printed on an alumina substrate, and baked at 900°C for 30 minutes to form an Ag
- As a result of conducting migration and solder cracking tests using Pd-Pt thick film circuits, the average time until migration occurred was 5 minutes and 30 seconds, and after 5 solder immersion tests, considerable solder cracking was observed. It was done.
【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
−パラジウム−白金複合粉末は銀微粉末中にパラジウム
と白金を均一に分散させた銀−パラジウム−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
かったパラジウムと白金が均一に分散した銀−パラジウ
ム−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−パラジウム−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-palladium-platinum composite powder of the present invention is a silver-palladium-platinum composite fine powder in which palladium and platinum are uniformly dispersed in fine silver powder. When used in a paste, it is possible to form a silver-palladium-platinum film in which palladium and platinum are uniformly dispersed, which has not been possible in the past, so it can be said to be an epoch-making product that can replace conventional powders. Moreover, the manufacturing method of the present invention allows silver-palladium-platinum composite powder to be easily manufactured.
Claims (5)
に分散させた銀−パラジウム−白金複合微粉末。1. A silver-palladium-platinum composite fine powder in which palladium and platinum are uniformly dispersed in a fine silver powder.
理されたことを特徴とする特許請求の範囲第１項記載の
銀−パラジウム−白金複合微粉末。2. The silver-palladium-platinum composite fine powder according to claim 1, wherein the silver-palladium-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−パラジウム−白金複合微粉末。3. The silver-palladium-platinum composite fine powder according to claim 2, wherein the heat treatment temperature is in the range of 200 to 600°C.
に分散させる際に還元反応を利用することを特徴とする
銀−パラジウム−白金複合微粉末の製造方法。4. A method for producing a silver-palladium-platinum composite fine powder, which comprises utilizing a reduction reaction when uniformly dispersing palladium and platinum in the silver fine powder.
に分散させる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−パ
ラジウム−白金複合微粉末の製造方法。5. The silver-palladium-platinum composite according to claim 4, wherein the reduction reaction when palladium and platinum are uniformly dispersed in fine silver powder is chemical reduction or hydrogen reduction. Method for producing fine powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9125691A JPH04246106A (en) | 1991-01-26 | 1991-01-26 | Silver-palladium-platinum composite pulverized powder and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9125691A JPH04246106A (en) | 1991-01-26 | 1991-01-26 | Silver-palladium-platinum composite pulverized powder and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04246106A true JPH04246106A (en) | 1992-09-02 |
Family
ID=12172816
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9125691A Pending JPH04246106A (en) | 1991-01-26 | 1991-01-26 | Silver-palladium-platinum composite pulverized powder and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04246106A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015174462A1 (en) * | 2014-05-16 | 2015-11-19 | 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 JP9125691A patent/JPH04246106A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015174462A1 (en) * | 2014-05-16 | 2015-11-19 | 国立研究開発法人産業技術総合研究所 | Thermoelectric conversion element and thermoelectric conversion module |
| CN106463600A (en) * | 2014-05-16 | 2017-02-22 | 国立研究开发法人产业技术综合研究所 | Thermoelectric conversion element and thermoelectric conversion module |
| 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 |
| EP3144986A4 (en) * | 2014-05-16 | 2017-11-22 | National Institute of Advanced Industrial Science and Technology | Thermoelectric conversion element and thermoelectric conversion module |
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