JP2969728B2 - Powder alloying method - Google Patents
Powder alloying methodInfo
- Publication number
- JP2969728B2 JP2969728B2 JP2031858A JP3185890A JP2969728B2 JP 2969728 B2 JP2969728 B2 JP 2969728B2 JP 2031858 A JP2031858 A JP 2031858A JP 3185890 A JP3185890 A JP 3185890A JP 2969728 B2 JP2969728 B2 JP 2969728B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- particle size
- alloy
- alloying method
- 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.)
- Expired - Fee Related
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） この発明は、粉末合金化方法に関するものである。さ
らに詳しくは、この発明は、合金化時の見掛け粒径の増
大がなく、均一微細粒径での合金製造が可能な、電極、
リード線、接点、発熱体等の形成に、あるいはろう材料
として有用な粉末合金の製造法に関するものである。Description: TECHNICAL FIELD The present invention relates to a powder alloying method. More specifically, the present invention provides an electrode, which does not increase the apparent particle size at the time of alloying and can produce an alloy with a uniform fine particle size.
The present invention relates to a method for producing a powder alloy useful for forming a lead wire, a contact, a heating element, and the like, or as a brazing material.
（従来の技術とその課題） 従来より、導電ペースト用材料、ろう材料等として金
属、あるいは合金の粉末が利用されてきている。たとえ
ば、各種電子部品のプリント回路の形成に使用される導
電ペーストとしては、導電性物質としてAg粉末が多用さ
れてきている。通常、このAg粉末に適量なバインダーを
加えたものが使用されている。(Prior art and its problems) Conventionally, metal or alloy powders have been used as conductive paste materials, brazing materials, and the like. For example, as a conductive paste used for forming a printed circuit of various electronic components, Ag powder has been frequently used as a conductive substance. Usually, a material obtained by adding an appropriate amount of a binder to this Ag powder is used.
しかしながら、この導電ペーストについては、回路パ
ターンのファイン化にともなって、これまでのものでは
導電性物質のマイグレーションによる回路の危険が生じ
ることが懸念されている。このマイグレーションは、Ag
単独で使用すると生じやすいと考えられることから、こ
れを防止するためにAgに30％程度のPdまたは数％のPtを
添加した混合粉末を用いて導電ペーストを調整すること
が行われてもいる。However, with respect to this conductive paste, there is a concern that with the refinement of the circuit pattern, there is a danger of a circuit due to migration of a conductive substance in the past. This migration uses Ag
Since it is thought that it is likely to occur when used alone, in order to prevent this, a conductive powder is adjusted using a mixed powder obtained by adding about 30% of Pd or several% of Pt to Ag. .
しかしながら、単にこのような混合物の使用によって
はマイグレーション防止の効果が充分とはいえないた
め、最近では、Agを主体とする合金の粉末化が検討され
ている。However, since the effect of preventing migration cannot be said to be sufficient simply by using such a mixture, powdering of an alloy mainly composed of Ag has recently been studied.
たとえば、このような例に見られるように合金の粉末
化についての関心が高まってきており、Ag合金に限られ
ることなく、均一で、かつ微細な粒径の合金粉末を生産
性よく製造するための方法が精力的に検討されてきてい
る。しかしながら、現状においては、実用に供すること
のできる粉末合金化の方法はいまだ確立されておらず、
これまでに提案されている方法にもいくつかの問題があ
る。For example, as shown in such an example, interest in powdering alloys has been increasing, and is not limited to Ag alloys, but in order to produce uniform and fine-grained alloy powders with good productivity. These methods have been energetically studied. However, at present, a powder alloying method that can be put to practical use has not yet been established,
The methods proposed so far also have some problems.
たとえば、特開昭58−11701号には、Ag塩とPd塩との
水溶液から共沈殿を生じさせ、共沈物を水素ガスによっ
て還元してAg−Pd合金粉末を製造する方法が開示されて
いる。しかしながらこの方法の場合には、沈殿物の水素
ガス還元の際に、隣接する粒子が溶着して見掛上の粒径
が大きくなることが避けられないという欠点がある。For example, JP-A-58-11701 discloses a method for producing an Ag-Pd alloy powder by causing coprecipitation from an aqueous solution of an Ag salt and a Pd salt and reducing the coprecipitate with hydrogen gas. I have. However, in the case of this method, there is a disadvantage that it is inevitable that adjacent particles are welded to increase the apparent particle size when the precipitate is reduced with hydrogen gas.
また、この欠点は、他種金属の組合せからなる合金粉
末の製造においても認められるものであった。This disadvantage has also been observed in the production of alloy powders composed of a combination of other metals.
このような欠点を克服するものとして、金属粉末をグ
リセリン等の有機化合物中で加熱する方法も提案されて
いるが、この方法の場合には、高純度な合金粉末を得る
ことが難しく、有機化合物の洗浄・除去処理のための時
間とコストの増加が避けられず、スケールアップ上から
も制約が大きいという欠点がある。As a method for overcoming such disadvantages, a method of heating a metal powder in an organic compound such as glycerin has been proposed. However, in this method, it is difficult to obtain a high-purity alloy powder, and the organic compound is difficult to obtain. However, there is a disadvantage that the time and cost for the cleaning / removal process are unavoidably increased, and that there is a large restriction in terms of scale-up.
このため、これまでに知られている方法では、合金化
時の見掛け粒径の増大を抑え、しかも高純度で生産性よ
く合金粉末を製造することはできなかった。この見掛け
粒径の増大は、導電ペーストとしてのスクリーン印刷等
の目づまり、焼成後の体積減少、ペーストへのフィラー
量配合の制限、ペースト混練時間の増大等の原因となる
ことから、生産性の向上とともに是非とも解決しなけれ
ばならない問題であった。For this reason, according to the methods known so far, it has not been possible to suppress the increase in apparent particle size during alloying and to produce alloy powder with high purity and high productivity. This increase in apparent particle size causes clogging such as screen printing as a conductive paste, reduces the volume after firing, restricts the amount of filler in the paste, and increases the kneading time of the paste. It was a problem that had to be solved along with the improvement.
この発明は、以上の通りの事情に鑑みてなされたもの
であり、従来方法の欠点を解消し、合金化時の隣接粉末
界面での溶着による見掛上の粒径増大を抑え、高生産性
で微細均一粒径の粉末合金を製造することのできる新し
い方法を提供することを目的としている。The present invention has been made in view of the above circumstances, has solved the drawbacks of the conventional method, suppressed the apparent increase in particle size due to welding at the interface between adjacent powders during alloying, and has achieved high productivity. It is an object of the present invention to provide a new method capable of producing a powder alloy having a fine and uniform particle size.
（課題を解決するための手段） この発明は、上記の課題を解決するものとして、２種
以上の金属の微細粉末を水素ガスを含む希ガス雰囲気下
に熱処理することを特徴とする粉末合金化方法を提供す
る。(Means for Solving the Problems) According to the present invention, there is provided a powder alloying method comprising heat treating fine powders of two or more metals in a rare gas atmosphere containing hydrogen gas. Provide a way.
この発明が対象とする金属としては、Ag、Au、Pd、P
t、Rh、Ru、Ir、Os、Ni、Ｗ、Cd、Cu、Hg、Zn、Sn、M
o、Cr、Zr、Ｃ、Ti等々の任意のものが含まれ、これら
金属の２種以上の組合せから所要の粉末合金を製造す
る。この組合せとしては、たとえば、Ag−Pt、Ag−Pd、
Pd−Pt、Ag−Cd、Hg−Pt、Hg−Mo、Pt−Ir、Pd−Ag−Ni
−Ｗ、Pt−Ru−Ｗ、Ag−Mo、Au−Pt−Ir、Au−Ag−Pt等
が例示される。The metals targeted by the present invention include Ag, Au, Pd, P
t, Rh, Ru, Ir, Os, Ni, W, Cd, Cu, Hg, Zn, Sn, M
O, Cr, Zr, C, Ti, etc. are included, and a required powder alloy is produced from a combination of two or more of these metals. As this combination, for example, Ag-Pt, Ag-Pd,
Pd-Pt, Ag-Cd, Hg-Pt, Hg-Mo, Pt-Ir, Pd-Ag-Ni
-W, Pt-Ru-W, Ag-Mo, Au-Pt-Ir, Au-Ag-Pt and the like are exemplified.
２種以上の金属の粉末は、各々単独の粉末を混合使用
してもよいし、あるいは共沈法によって溶液から生成さ
せた複合粉末等を使用してもよい。この際の金属の粉末
は、粒径が10μｍ以下の微細なものを用いるのが好まし
い。このような粉末の使用によって10μｍ以下の微細均
一な粒径の合金粉末が製造されることになる。As the powders of two or more metals, a single powder may be mixed and used, or a composite powder or the like generated from a solution by a coprecipitation method may be used. In this case, it is preferable to use a fine metal powder having a particle size of 10 μm or less. By using such a powder, an alloy powder having a fine and uniform particle size of 10 μm or less is produced.
加熱処理は、水素ガスを含む希ガス、つまりAr、Ne、
He、Xe等のガスの雰囲気下において、特にその気流中に
おいて、600℃以下の温度において行うのが好ましい。
処理時間は１〜３時間程度とすることができる。製造さ
れる合金粉末の粒径は、原料とする金属粉の大きさ、加
熱温度とその処理時間等の調整によって容易に制御する
ことができる。The heat treatment is performed using a rare gas containing hydrogen gas, that is, Ar, Ne,
It is preferable to carry out the reaction at a temperature of 600 ° C. or lower in an atmosphere of a gas such as He or Xe, particularly in the gas stream.
The processing time can be about 1 to 3 hours. The particle size of the alloy powder to be produced can be easily controlled by adjusting the size of the metal powder as a raw material, the heating temperature, the treatment time, and the like.
特にこの発明の方法においては、共沈粉末を原料とす
ることが有効でもある。この共沈粉末の使用によって粉
末の凝集を抑えつつ、均一微細粉末の製造が容易に実現
される。たとえば、この共沈による複合粉末は、金属イ
オンの２種以上のものを含んだ水溶液、アルコール溶
液、あるいはその混合物に還元剤を添加すること等によ
り製造される。また、その他様々な手段が採用される。In particular, in the method of the present invention, it is also effective to use a coprecipitated powder as a raw material. The use of this coprecipitated powder facilitates the production of a uniform fine powder while suppressing the aggregation of the powder. For example, the composite powder by this coprecipitation is produced by adding a reducing agent to an aqueous solution or an alcohol solution containing two or more kinds of metal ions, or a mixture thereof. In addition, various other means are employed.
（作 用） この発明の方法においては、水素ガスを含む希ガス雰
囲気下での加熱によって合金化時の粉末の溶着による見
掛上の粒径増大を抑えることができ、均一微細な粉末合
金を生成させることができる。さらに、水素ガスを含む
雰囲気で熱処理するので粉末合金は脱酸され酸素量も低
下する。(Operation) In the method of the present invention, by heating in a rare gas atmosphere containing hydrogen gas, it is possible to suppress an apparent increase in particle diameter due to welding of powder during alloying, and to obtain a uniform fine powder alloy. Can be generated. Further, since the heat treatment is performed in an atmosphere containing hydrogen gas, the powder alloy is deoxidized and the amount of oxygen decreases.
（実施例） 次に実施例を示し、さらに詳しくこの発明の粉末合金
化方法について説明する。(Example) Next, an example is shown and the powder alloying method of the present invention will be described in more detail.
実施例１〜３ Agイオン、Pdイオンを含有する水溶液より、粒径が５
μｍのAg70重量％、Pd30重量％の共沈粉を得た。この粉
末を200〜250℃の温度においてH210vol％を含むAr気流
中で２時間熱処理を行った。Examples 1 to 3 From the aqueous solution containing Ag ions and Pd ions, the particle size was 5
A co-precipitated powder of 70% by weight of Ag and 30% by weight of Pd was obtained. This powder was heat-treated at a temperature of 200 to 250 ° C. in an Ar gas stream containing 10 vol% of H 2 for 2 hours.
表１に示したように、いずれの場合にも平均粒径５μ
ｍのAg−Pd合金粉末を得た。その純度は99.9％以上であ
った。As shown in Table 1, the average particle size was 5 μm in each case.
m-Ag-Pd alloy powder was obtained. Its purity was more than 99.9%.
粉末相互の溶着・凝集による粒径の見掛上の増大は抑
止され、均一微細な、かつ高純度のAg−Pd合金粉を得
た。The apparent increase in particle size due to welding and agglomeration of the powders was suppressed, and a uniform, fine and high-purity Ag-Pd alloy powder was obtained.
実施例４〜６ 平均５μｍのAgとPdの混合粉を実施例１と同様にして
H25〜20vol％を含むArおよびHe気流中において220〜230
℃の温度において２時間加熱した。得られた合金粉末の
粒径は５μｍであった。Examples 4 to 6 A mixed powder of Ag and Pd having an average of 5 μm was prepared in the same manner as in Example 1.
220 to 230 in an Ar and He gas flow containing 5 to 20 vol% H2
Heated at a temperature of ° C. for 2 hours. The particle size of the obtained alloy powder was 5 μm.
比較例１〜３ 実施例１の共沈粉を、H2およびN2気流中において230
〜280℃の温度において２時間加熱した。処理後の粒径
は見掛上11〜12μｍと増大していた。The coprecipitated powder of Comparative Examples 1 to 3 Example 1, the H 2 and N 2 gas stream 230
Heated at a temperature of 280280 ° C. for 2 hours. The particle size after the treatment was apparently increased to 11 to 12 μm.
（発明の効果） この発明により、以上詳しく説明した通り、合金化時
の見掛上の粒径の増大を抑え、たとえば粒度が10μｍ以
下の微細粒径の均一粉末を高生産性で製造することがで
きる。しかも有機化合物を使用しないため、高純度品と
しての合金粉末の取得が可能となる。さらに、合金粉末
の酸素量も低くすることが可能となる。 (Effect of the Invention) According to the present invention, as described in detail above, it is possible to suppress an increase in apparent particle size at the time of alloying and to produce a uniform powder having a fine particle size of, for example, 10 µm or less with high productivity. Can be. Moreover, since no organic compound is used, it is possible to obtain an alloy powder as a high-purity product. Further, the amount of oxygen in the alloy powder can be reduced.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭62−210041（ＪＰ，Ａ) 特開 昭56−116801（ＪＰ，Ａ) 特開 昭60−106930（ＪＰ，Ａ) 特開 平２−217406（ＪＰ，Ａ) 特開 昭63−297502（ＪＰ，Ａ) 特公 昭44−28993（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.6，ＤＢ名) B22F 1/00 B22F 9/22 B22F 9/24 B22F 9/02 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-62-210041 (JP, A) JP-A-56-116801 (JP, A) JP-A-60-106930 (JP, A) JP-A-2- 217406 (JP, A) JP-A-63-297502 (JP, A) JP-B-44-28993 (JP, B1) (58) Fields investigated (Int. Cl. 6 , DB name) B22F 1/00 B22F 9 / 22 B22F 9/24 B22F 9/02
Claims (4)
む希ガス雰囲気下に熱処理することを特徴とする粉末合
金化方法。1. A powder alloying method comprising subjecting a fine powder of two or more metals to a heat treatment in a rare gas atmosphere containing hydrogen gas.
項（１）記載の粉末合金化方法。2. The powder alloying method according to claim 1, wherein the metal powder having a particle size of 10 μm or less is heat-treated.
記載の粉末合金化方法。3. The method according to claim 1, wherein the heating temperature is 600 ° C. or less.
The powder alloying method as described.
理する請求項（１）記載の粉末合金化方法。4. The powder alloying method according to claim 1, wherein the coprecipitated powder from the metal ion-containing solution is heat-treated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2031858A JP2969728B2 (en) | 1990-02-13 | 1990-02-13 | Powder alloying method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2031858A JP2969728B2 (en) | 1990-02-13 | 1990-02-13 | Powder alloying method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0428801A JPH0428801A (en) | 1992-01-31 |
| JP2969728B2 true JP2969728B2 (en) | 1999-11-02 |
Family
ID=12342748
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2031858A Expired - Fee Related JP2969728B2 (en) | 1990-02-13 | 1990-02-13 | Powder alloying method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2969728B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102458727B (en) * | 2009-04-24 | 2015-05-06 | 独立行政法人科学技术振兴机构 | Fine solid solution alloy particles and method for producing same |
-
1990
- 1990-02-13 JP JP2031858A patent/JP2969728B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0428801A (en) | 1992-01-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tan et al. | Preparation of gold, platinum, palladium and silver nanoparticles by the reduction of their salts with a weak reductant–potassium bitartrate | |
| Ayyappan et al. | Nanoparticles of Ag, Au, Pd, and Cu produced by alcohol reduction of the salts | |
| JP3277823B2 (en) | Production method of metal powder | |
| US4745094A (en) | Mono- or multi-metal microaggregates, a method for their preparation and their application in the catalysis of the photoreduction of water | |
| JP2013072091A (en) | Metal microparticle and method for producing the same, metal paste containing the metal microparticle, and metal coat made of the metal paste | |
| JP2012184451A (en) | Method for manufacturing metal fine powder and metal paste and metal film obtained by the same | |
| TWI432588B (en) | Copper powder for conductive paste, and conductive paste | |
| JP2005298921A (en) | Composite metal ultrafine particles and method for producing the same | |
| JP6453735B2 (en) | Method for producing noble metal powder | |
| EP0537502B1 (en) | Metal- and metal alloy powder comprising microcrystalline, spherical and dense particles and process and installation for preparing same | |
| JP2969728B2 (en) | Powder alloying method | |
| JPH0557324B2 (en) | ||
| EP0834369B1 (en) | Process for preparing metal powder | |
| JPH0428805A (en) | Method for alloying powder | |
| JP4061462B2 (en) | Composite fine particles, conductive paste and conductive film | |
| US3241949A (en) | Method of producing molybdenum alloy compositions from ammoniacal solutions | |
| JPH05311212A (en) | Production of fine powder of ag-pd alloy powder | |
| JP2550586B2 (en) | Method for producing fine silver alloy powder | |
| JP3300460B2 (en) | Method for producing ultrafine monodispersed gold particles | |
| JP2003034801A (en) | Metal powder and manufacturing method therefor | |
| JPH0699143B2 (en) | Nickel powder manufacturing method | |
| JP2003321701A (en) | Cu · In-based metal powder and method for producing the same | |
| JPS60141802A (en) | Alloy powder for forming dispersion-strengthening alloy | |
| JPS6357703A (en) | Production of fine metallic powder | |
| JPH07109505A (en) | Production of silver-palladium composite powder and silver-palladium composite powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |