JP3018655B2 - Manufacturing method of fine powder - Google Patents
Manufacturing method of fine powderInfo
- Publication number
- JP3018655B2 JP3018655B2 JP3270162A JP27016291A JP3018655B2 JP 3018655 B2 JP3018655 B2 JP 3018655B2 JP 3270162 A JP3270162 A JP 3270162A JP 27016291 A JP27016291 A JP 27016291A JP 3018655 B2 JP3018655 B2 JP 3018655B2
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- powder
- aqueous solution
- group
- mol
- fine powder
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は微粉末の製造方法に関
し、特にたとえばＳｎ粉，Ｐｂ粉，Ｚｎ粉，Ｎｉ粉，Ｉ
ｎ粉，Ｓｂ粉，Ｃｄ粉，Ａｓ粉，Ｐｂ−Ｓｂ−Ｓｎ粉，
Ｐｂ−Ｓｂ−Ａｓ粉，Ｒｅ粉，Ｍｏ粉，Ｓｅ粉，Ｔｅ
粉，Ｃｕ粉，ＣｄＳ粉などの微粉末の製造方法に関す
る。ここで、Ｓｎ粉は、はんだ材料やセンサ材料などと
して用いられる。Ｐｂ粉は、はんだ材料，塗料用顔料材
料，成型材料，焼結材料，電池材料などとして用いられ
る。Ｚｎ粉は、防錆材料や電池材料などとして用いられ
る。Ｎｉ粉は、電極ペースト材料，電池や燃料電池の電
極材料などとして用いられる。Ｉｎ粉は、はんだ材料，
焼結材料，歯科用材料などとして用いられる。Ｓｂ粉
は、抵抗材料やセンサ材料などとして用いられる。Ｃｄ
粉は、触媒，粉末冶金材料，各種セラミック材料，Ｎｉ
−Ｃｄ電池材料などとして用いられる。Ａｓ粉は、セン
サ材料などとして用いられる。Ｐｂ−Ｓｂ−Ｓｎ粉およ
びＰｂ−Ｓｂ−Ａｓ粉は、電池材料などとして用いられ
る。Ｒｅ粉は、フィラメント材料や触媒などとして用い
られる。Ｍｏ粉は、粉末冶金材料や電子管用材料などと
して用いられる。Ｓｅ粉は、光半導体や触媒などとして
用いられる。ＣｄＳ粉は、太陽電池材料などとして用い
られる。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a fine powder, particularly, for example, Sn powder, Pb powder, Zn powder, Ni powder, and I powder.
n powder, Sb powder, Cd powder, As powder, Pb-Sb-Sn powder,
Pb-Sb-As powder, Re powder, Mo powder, Se powder, Te
The present invention relates to a method for producing fine powder such as powder, Cu powder, and CdS powder. Here, the Sn powder is used as a solder material, a sensor material, or the like. Pb powder is used as a solder material, a pigment material for paint, a molding material, a sintered material, a battery material, and the like. Zn powder is used as a rust preventive material, a battery material, and the like. Ni powder is used as an electrode paste material, an electrode material for batteries and fuel cells, and the like. In powder is a solder material,
Used as a sintering material, dental material, etc. Sb powder is used as a resistance material or a sensor material. Cd
Powder is catalyst, powder metallurgy material, various ceramic materials, Ni
-Used as a Cd battery material and the like. As powder is used as a sensor material or the like. Pb-Sb-Sn powder and Pb-Sb-As powder are used as battery materials and the like. Re powder is used as a filament material, a catalyst, or the like. Mo powder is used as a powder metallurgy material, a material for an electron tube, or the like. Se powder is used as an optical semiconductor, a catalyst, or the like. CdS powder is used as a solar cell material or the like.
【０００２】[0002]
【従来の技術】従来の微粉末の製造方法としては、たと
えば機械的粉砕法，電解法、噴霧法，揮発凝集法，還元
法などがある。ここで、機械的粉砕法としては、スタン
プミル法，ボールミル法，渦流ミル法などがある。ま
た、電解法としては、湿式電解法，乾式電解法などがあ
る。さらに、噴霧法としては、ガス噴霧法，水噴霧法な
どがある。揮発凝集法は、たとえばＺｎ粉末の製造など
に用いられる。また、還元法としては、高温還元法，塩
類溶液還元法などがある。高温還元法は、金属化合物を
高温下で還元性ガスで還元する方法である。また、塩類
還元法としては、金属塩溶液に金属粉を入れて微粉末を
置換析出させる方法，ヒドラジンなどによる還元法，次
亜リン酸ナトリウムやＤＭＡＢなどによる還元法などが
ある。2. Description of the Related Art Conventional fine powder production methods include, for example, a mechanical pulverization method, an electrolytic method, a spray method, a volatile coagulation method, and a reduction method. Here, the mechanical pulverization method includes a stamp mill method, a ball mill method, a vortex mill method and the like. Examples of the electrolytic method include a wet electrolytic method and a dry electrolytic method. Further, examples of the spraying method include a gas spraying method and a water spraying method. The volatile aggregation method is used, for example, for producing Zn powder. Examples of the reduction method include a high-temperature reduction method and a salt solution reduction method. The high-temperature reduction method is a method of reducing a metal compound with a reducing gas at a high temperature. Examples of the salt reduction method include a method in which a metal powder is put into a metal salt solution to displace and precipitate fine powder, a reduction method using hydrazine or the like, a reduction method using sodium hypophosphite, DMAB, or the like.
【０００３】[0003]
【発明が解決しようとする課題】機械的粉砕法では、得
られる粉末が片状であり、かさ密度が小さい。また、粉
砕機の磨耗その他の原因による不純物の混入がある。さ
らに、金属や合金の粉砕中に粉末が酸化されやすい。ま
た、この方法は、粉塵公害の原因となりやすい。電解法
では、設備コストが大きくなり、また粉末が酸化しやす
い。噴霧法では、粉末の粒径が数１０μｍと大きく、ま
た設備コストが大きくなる。揮発凝集法は、Ｚｎなどの
蒸気圧の高い金属の粉末の製造に限定される。高温還元
法では、得られた粉末の粒径が大きく、また不純物が混
入しやすい。塩類溶液還元法のうち置換析出法では、置
換析出するために添加する金属粉が高価であり、また不
純物が混入する場合がある。さらに、粉末を析出させる
ための取扱が不便である。塩類溶液還元法のうちヒドラ
ジン，次亜リン酸ナトリウム，ＤＭＡＢなどの還元剤を
用いて粉末を沈澱させる方法では、還元できる金属が限
定され、また生成粉末中にリンやホウ素などが不純物と
して混入する場合がある。In the mechanical pulverization method, the powder obtained is flaky and has a low bulk density. Further, impurities are mixed in due to wear of the pulverizer and other causes. Further, the powder is easily oxidized during grinding of the metal or alloy. In addition, this method is likely to cause dust pollution. In the electrolytic method, the equipment cost is increased and the powder is easily oxidized. In the spraying method, the particle size of the powder is as large as several tens of μm, and the equipment cost is increased. Volatile agglomeration is limited to the production of powders of metals with high vapor pressure, such as Zn. In the high-temperature reduction method, the particle size of the obtained powder is large and impurities are easily mixed. In the displacement precipitation method among the salt solution reduction methods, the metal powder added for the displacement precipitation is expensive, and impurities may be mixed. Furthermore, handling for precipitating the powder is inconvenient. In the salt solution reduction method in which the powder is precipitated using a reducing agent such as hydrazine, sodium hypophosphite, DMAB, etc., the metals that can be reduced are limited, and phosphorus and boron are mixed as impurities in the resulting powder. There are cases.
【０００４】それゆえに、この発明の主たる目的は、安
全かつ簡単に粒径の小さい高純度微粉末を製造すること
ができ、公害が少なく、低コストの微粉末の製造方法を
提供することである。[0004] Therefore, a main object of the present invention is to provide a low-cost, low-cost method for producing fine powder which can safely and easily produce high-purity fine powder having a small particle size. .
【０００５】[0005]
【課題を解決するための手段】この発明は、元素周期率
表の６Ａ族，７Ａ族，１Ｂ族，２Ｂ族，３Ｂ族，４Ｂ
族，５Ｂ族，６Ｂ族および８族の金属または非金属の塩
である水溶性の化合物または水溶性錯体の水溶液を準備
するステップと、水溶液に三塩化チタンを添加し、三塩
化チタンの還元作用を用いて、金属粉末，金属および非
金属の２種類以上を含有する合金粉末または化合物粉末
のいずれかの微粉末を製造するステップを含む、微粉末
の製造方法である。この発明において、６Ａ族の元素と
してＭｏ、７Ａ族の元素としてＲｅ、１Ｂ族の元素とし
てＣｕ，Ａｇ，Ａｕ、２Ｂ族の元素としてＺｎ，Ｃｄ、
３Ｂ族の元素としてＩｎ、４Ｂ族の元素としてＳｎ，Ｐ
ｂ、５Ｂ族の元素としてＳｂ，Ａｓ，Ｂｉ、６Ｂ族の元
素としてＴｅ，Ｓｅ，Ｓ、８族の元素としてＮｉ，Ｒ
ｕ，Ｒｈ，Ｐｄ，Ｐｔ，Ｏｓ，Ｉｒなどが含まれる。こ
の発明の微粉末の製造方法においては、水溶液の温度が
その溶液の沸点以下に設定される。 また、水溶液と三塩
化チタンとの反応が大気中または加圧中で行われる。 こ
の発明の微粉末の製造方法で製造したＳｎ粉，Ｐｂ粉ま
たはＩｎ粉は、たとえば、はんだ材料として用いられ
る。 さらに、この発明の微粉末の製造方法で製造したＰ
ｂ粉またはＩｎ粉は、たとえば、焼結材料として用いら
れる。 また、この発明の微粉末の製造方法で製造したＮ
ｉ粉は、たとえば、電極材料として用いられる。 さら
に、この発明の微粉末の製造方法で製造したＣｄＳ粉
は、たとえば、太陽電池材料として用いられる。 According to the present invention, there is provided a periodic table of the elements of groups 6A, 7A, 1B, 2B, 3B, 4B.
Preparing an aqueous solution of a water-soluble compound or complex that is a metal or non-metal salt of Group 5, 5B, 6B, and 8; and adding titanium trichloride to the aqueous solution to reduce titanium trichloride. A method for producing a fine powder of any one of an alloy powder or a compound powder containing two or more kinds of metal powder, metal and nonmetal by using the method. In the present invention, Mo as a Group 6A element, Re as a Group 7A element, Cu, Ag, Au as a Group 1B element, Zn, Cd as a Group 2B element,
In as a 3B group element, Sn and P as a 4B group element
b, Sb, As, Bi as group 5B elements, Te, Se, S as group 6B elements, Ni, R as group 8 elements
u, Rh, Pd, Pt, Os, Ir and the like. This
In the method for producing fine powder according to the invention of
It is set below the boiling point of the solution. Also, aqueous solution and trisalt
The reaction with titanium oxide is performed in the air or under pressure. This
Powder, Sn powder and Pb powder produced by the method for producing fine powder of the present invention.
Or In powder is used as a solder material, for example.
You. Further, the P powder produced by the method for producing fine powder of the present invention
b powder or In powder is used, for example, as a sintered material.
It is. Further, the N powder produced by the method for producing fine powder of the present invention is
The i powder is used, for example, as an electrode material. Further
CdS powder produced by the method for producing fine powder of the present invention
Is used, for example, as a solar cell material.
【０００６】[0006]
【作用】金属や非金属の化合物または錯体が、三塩化チ
タンによって還元される。The metal or nonmetal compound or complex is reduced by titanium trichloride.
【０００７】[0007]
【発明の効果】この発明によれば、安全かつ簡単に粒径
の小さい高純度微粉末を製造することができる。しか
も、微粉末を製造する際に、粉塵公害などが発生せず、
低コストで微粉末を製造することができる。According to the present invention, a high-purity fine powder having a small particle size can be produced safely and easily. Moreover, when producing fine powder, dust pollution does not occur,
Fine powder can be produced at low cost.
【０００８】この発明の上述の目的，その他の目的，特
徴および利点は、以下の実施例の詳細な説明から一層明
らかとなろう。The above and other objects, features and advantages of the present invention will become more apparent from the following detailed description of the embodiments.
【０００９】[0009]
【実施例】実施例１ まず、ＰｂＣｌ2 を準備した。このＰｂＣｌ2 ０．０３
ｍｏｌ／Ｌに有機錯化剤としてのエチレンジアミン四酢
酸（ＥＤＴＡ）０．０４ｍｏｌ／Ｌ、クエン酸０．１０
ｍｏｌ／Ｌを加えてｐＨ１０に調整し、混合水溶液を得
た。この混合水溶液に還元剤としてＴｉＣｌ3 ０．０３
ｍｏｌ／Ｌを添加し、混合水溶液の温度６０℃で約１０
分間攪拌した。このようにして、黒色の還元Ｐｂ粉末の
沈澱を得た。沈澱したＰｂ粉末は、アルコールで脱水，
乾燥し、取り出した。得られたＰｂ粉末の粒径は０．４
〜０．５μｍであり、一般的にＰｂ粉の製造に用いられ
ている機械的粉砕法や噴霧法で得られる粉粒に比べて、
均一で微細な粉粒を得ることができた。 Example 1 First, PbCl 2 was prepared. This PbCl 2 0.03
mol / L: 0.04 mol / L of ethylenediaminetetraacetic acid (EDTA) as an organic complexing agent, and 0.10 of citric acid
The pH was adjusted to 10 by adding mol / L to obtain a mixed aqueous solution. TiCl 3 0.03 as a reducing agent was added to this mixed aqueous solution.
mol / L, and about 10
Stirred for minutes. Thus, a precipitate of black reduced Pb powder was obtained. The precipitated Pb powder is dehydrated with alcohol,
Dried and removed. The particle size of the obtained Pb powder is 0.4
０．５0.5 μm, compared to powder obtained by a mechanical pulverization method or a spray method generally used for the production of Pb powder,
Uniform and fine powder particles could be obtained.
【００１０】実施例２ まず、ＳｂＣｌ3 を準備した。このＳｂＣｌ3 ０．０４
ｍｏｌ／ＬにＥＤＴＡ０．０４ｍｏｌ／Ｌ、クエン酸
０．２０ｍｏｌ／Ｌを加えて水溶液とした。この水溶液
に２８％アンモニア水を加えてｐＨ１０に調整し、混合
水溶液を得た。この混合水溶液に還元剤としてＴｉＣｌ
3 ０．０３ｍｏｌ／Ｌを添加し、混合水溶液の温度６０
℃で約１０分間攪拌した。このようにして、粒径０．５
μｍの銀白色のＳｂの樹枝状粉末を得た。 Example 2 First, SbCl 3 was prepared. This SbCl 3 0.04
EDTA 0.04 mol / L and citric acid 0.20 mol / L were added to the mol / L to prepare an aqueous solution. The aqueous solution was adjusted to pH 10 by adding 28% aqueous ammonia to obtain a mixed aqueous solution. TiCl as a reducing agent is added to this mixed aqueous solution.
3 0.03 mol / L was added, and the temperature of the mixed aqueous solution was 60
The mixture was stirred at about 10 minutes. Thus, a particle size of 0.5
A silvery white Sb dendritic powder of μm was obtained.
【００１１】実施例３ まず、ＩｎＣｌ3 を準備した。このＩｎＣｌ3 ０．０４
ｍｏｌ／Ｌに有機錯化剤としてのニトリロ三酢酸（ＮＴ
Ａ）０．１０ｍｏｌ／Ｌ、クエン酸０．３０ｍｏｌ／Ｌ
を加えて水溶液とした。この水溶液に２８％アンモニア
水を加えてｐＨ１０に調整し、混合水溶液を得た。この
混合水溶液に還元剤としてＴｉＣｌ3 ０．０４ｍｏｌ／
Ｌを添加し、混合水溶液の温度６０℃で約１０分間攪拌
した。このようにして、粒径０．８μｍの銀白色のＩｎ
粉末を得た。 Example 3 First, InCl 3 was prepared. This InCl 3 0.04
mol / L of nitrilotriacetic acid (NT) as an organic complexing agent
A) 0.10 mol / L, citric acid 0.30 mol / L
Was added to obtain an aqueous solution. The aqueous solution was adjusted to pH 10 by adding 28% aqueous ammonia to obtain a mixed aqueous solution. To this mixed aqueous solution, as a reducing agent, TiCl 3 0.04 mol /
L was added and the mixture was stirred at a temperature of 60 ° C. for about 10 minutes. Thus, silver-white In with a particle size of 0.8 μm
A powder was obtained.
【００１２】実施例４ まず、ＣｄＣｌ2 を準備した。このＣｄＣｌ2 ０．０４
ｍｏｌ／ＬにＥＤＴＡ・２Ｎａ０．０４ｍｏｌ／Ｌ、ク
エン酸０．１０ｍｏｌ／Ｌを加えて水溶液とした。この
水溶液に２８％アンモニア水を加えてｐＨ１０に調整し
た。ｐＨを調整した水溶液に還元剤としてＴｉＣｌ
3 ０．０４ｍｏｌ／Ｌを添加し、水溶液の温度８０℃で
約１０分間攪拌した。このようにして、粒径０．５μｍ
の銀白色のＣｄ粉末を得た。 Example 4 First, CdCl 2 was prepared. This CdCl 2 0.04
EDTA · 2Na (0.04 mol / L) and citric acid (0.10 mol / L) were added to the mol / L to form an aqueous solution. The pH of the aqueous solution was adjusted to 10 by adding 28% aqueous ammonia. TiCl as a reducing agent in the pH adjusted aqueous solution
3 0.04 mol / L was added, and the mixture was stirred at a temperature of 80 ° C. for about 10 minutes. Thus, the particle size is 0.5 μm
A silver-white Cd powder was obtained.
【００１３】実施例５ まず、ＮｉＣｌ2 を準備した。このＮｉＣｌ2 ０．０４
ｍｏｌ／ＬにＮＴＡ０．１０ｍｏｌ／Ｌ、酒石酸ナトリ
ウム０．１０ｍｏｌ／Ｌを加えて水溶液とした。この水
溶液に２８％アンモニア水を加えてｐＨ１０に調整し、
混合水溶液を得た。この混合水溶液に還元剤としてＴｉ
Ｃｌ3 ０．０４ｍｏｌ／Ｌを添加し、混合水溶液の温度
８０℃で約１０分間攪拌した。このようにして、粒径
０．８μｍの黒色のＮｉ粉末を得た。 Example 5 First, NiCl 2 was prepared. This NiCl 2 0.04
An aqueous solution was prepared by adding 0.10 mol / L of NTA and 0.10 mol / L of sodium tartrate to the mol / L. This aqueous solution was adjusted to pH 10 by adding 28% aqueous ammonia,
A mixed aqueous solution was obtained. This mixed aqueous solution contains Ti as a reducing agent.
0.03 mol / L of Cl 3 was added, and the mixture was stirred at a temperature of 80 ° C. for about 10 minutes. Thus, black Ni powder having a particle size of 0.8 μm was obtained.
【００１４】実施例６ まず、ＳｎＣｌ2 とＰｂＣｌ2 とを準備した。これらの
ＳｎＣｌ2 ０．０４ｍｏｌ／ＬとＰｂＣｌ2 ０．０２ｍ
ｏｌ／ＬとにＥＤＴＡ０．０８ｍｏｌ／ＬとＮＴＡ０．
１０ｍｏｌ／Ｌ、酒石酸０．３０ｍｏｌ／Ｌを加えて水
溶液とした。この水溶液に２８％アンモニア水を加えて
ｐＨ１０に調整した。ｐＨを調整した水溶液に還元剤と
してＴｉＣｌ3 ０．０４ｍｏｌ／Ｌを添加し、混合水溶
液の温度８０℃で約１５分間攪拌した。このようにし
て、粒径１．０μｍの黒色のＳｎ−Ｐｂ粉末を得た。 Example 6 First, SnCl 2 and PbCl 2 were prepared. These SnCl 2 0.04 mol / L and PbCl 2 0.02 m
ol / L, EDTA 0.08 mol / L and NTA0.
10 mol / L and tartaric acid 0.30 mol / L were added to obtain an aqueous solution. The pH of the aqueous solution was adjusted to 10 by adding 28% aqueous ammonia. 0.04 mol / L of TiCl 3 was added as a reducing agent to the pH-adjusted aqueous solution, and the mixture was stirred at a temperature of 80 ° C. for about 15 minutes. Thus, a black Sn-Pb powder having a particle size of 1.0 μm was obtained.
【００１５】実施例７ まず、ＲｅＣｌ2 を準備した。このＲｅＣｌ2 ０．０４
ｍｏｌ／ＬにＥＤＴＡ・２Ｎａ０．０４ｍｏｌ／Ｌ、酒
石酸ナトリウム０．３０ｍｏｌ／Ｌを加えて水溶液とし
た。この水溶液に２８％アンモニア水を加えてｐＨ１０
に調整した。ｐＨを調整した水溶液に還元剤としてＴｉ
Ｃｌ3 ０．０４ｍｏｌ／Ｌを添加し、水溶液の温度６０
℃で約１０分間攪拌した。このようにして、粒径１．０
μｍの暗灰色のＲｅ粉末を得た。 Example 7 First, ReCl 2 was prepared. This ReCl 2 0.04
EDTA · 2Na (0.04 mol / L) and sodium tartrate (0.30 mol / L) were added to the mol / L to form an aqueous solution. 28% ammonia water was added to this aqueous solution to adjust the pH to 10
Was adjusted. Ti as a reducing agent in the pH adjusted aqueous solution
0.03 mol / L of Cl 3 was added, and the temperature of the aqueous solution was adjusted to 60.
The mixture was stirred at about 10 minutes. Thus, a particle size of 1.0
A μm dark gray Re powder was obtained.
【００１６】実施例８ まず、ＮａＭｏＯ4 を準備した。このＮａＭｏＯ4 ０．
０４ｍｏｌ／Ｌに尿素０．０８ｍｏｌ／Ｌ、クエン酸ナ
トリウム０．２０ｍｏｌ／Ｌを加えて水溶液とした。こ
の水溶液に２８％アンモニア水を加えてｐＨ１０に調整
した。ｐＨを調整した水溶液に還元剤としてＴｉＣｌ3
０．０４ｍｏｌ／Ｌを添加し、水溶液の温度８０℃で約
１０分間攪拌した。このようにして、粒径０．８μｍの
灰黒色のＭｏ粉末を得た。 Example 8 First, NaMoO 4 was prepared. This NaMoO 40 .
An aqueous solution was prepared by adding 0.08 mol / L of urea and 0.20 mol / L of sodium citrate to 04 mol / L. The pH of the aqueous solution was adjusted to 10 by adding 28% aqueous ammonia. TiCl 3 as a reducing agent is added to the pH adjusted aqueous solution.
0.04 mol / L was added, and the mixture was stirred at a temperature of 80 ° C. for about 10 minutes. Thus, a gray-black Mo powder having a particle size of 0.8 μm was obtained.
【００１７】実施例９ まず、ＳｅＣｌ4 を準備した。このＳｅＣｌ4 ０．０４
ｍｏｌ／ＬにＥＤＴＡ・２Ｎａ０．０４ｍｏｌ／Ｌ、ク
エン酸ナトリウム０．２０ｍｏｌ／Ｌを加えて水溶液と
した。この水溶液に２８％アンモニア水を加えてｐＨ１
０に調整し、混合水溶液を得た。この混合水溶液に還元
剤としてＴｉＣｌ3 ０．０４ｍｏｌ／Ｌを添加し、混合
水溶液の温度８０℃で約１０分間攪拌した。このように
して、粒径０．８μｍの暗赤色のＳｅ粉末を得た。 Example 9 First, SeCl 4 was prepared. This SeCl 4 0.04
EDTA · 2Na (0.04 mol / L) and sodium citrate (0.20 mol / L) were added to the mol / L to form an aqueous solution. 28% aqueous ammonia was added to this aqueous solution to adjust the pH to 1
It was adjusted to 0 to obtain a mixed aqueous solution. 0.04 mol / L of TiCl 3 was added as a reducing agent to the mixed aqueous solution, and the mixture was stirred at a temperature of 80 ° C. for about 10 minutes. Thus, a dark red Se powder having a particle size of 0.8 μm was obtained.
【００１８】実施例１０ まず、ＴｅＣｌ2 を準備した。このＴｅＣｌ2 ０．０４
ｍｏｌ／ＬにＥＤＴＡ０．０４ｍｏｌ／Ｌ、クエン酸
０．２０ｍｏｌ／Ｌを加えて水溶液とした。この水溶液
に２８％アンモニア水を加えてｐＨ１０に調整し、混合
水溶液を得た。この混合水溶液に還元剤としてＴｉＣｌ
3 ０．０４ｍｏｌ／Ｌを添加し、混合水溶液の温度８０
℃で約１０分間攪拌した。このようにして、粒径０．８
μｍの黒色のＴｅ粉末を得た。 Example 10 First, TeCl 2 was prepared. This TeCl 2 0.04
EDTA 0.04 mol / L and citric acid 0.20 mol / L were added to the mol / L to prepare an aqueous solution. The aqueous solution was adjusted to pH 10 by adding 28% aqueous ammonia to obtain a mixed aqueous solution. TiCl as a reducing agent is added to this mixed aqueous solution.
3 0.04 mol / L was added, and the temperature of the mixed aqueous solution was 80
The mixture was stirred at about 10 minutes. Thus, a particle size of 0.8
A black Te powder of μm was obtained.
【００１９】実施例１１ まず、ＣｕＣｌ2 を準備した。このＣｕＣｌ2 ０．０４
ｍｏｌ／ＬにＥＤＴＡ０．０６ｍｏｌ／Ｌ、クエン酸
０．２０ｍｏｌ／Ｌを加えて水溶液とした。この水溶液
に２８％アンモニア水を加えてｐＨ１０に調整し、混合
水溶液を得た。この混合水溶液に還元剤としてＴｉＣｌ
3 ０．０４ｍｏｌ／Ｌを添加し、混合水溶液の温度８０
℃で約１０分間攪拌した。このようにして、粒径０．６
５μｍの赤色のＣｕ粉末を得た。 Example 11 First, CuCl 2 was prepared. This CuCl 2 0.04
EDTA 0.06 mol / L and citric acid 0.20 mol / L were added to the mol / L to prepare an aqueous solution. The aqueous solution was adjusted to pH 10 by adding 28% aqueous ammonia to obtain a mixed aqueous solution. TiCl as a reducing agent is added to this mixed aqueous solution.
3 0.04 mol / L was added, and the temperature of the mixed aqueous solution was 80
The mixture was stirred at about 10 minutes. Thus, a particle size of 0.6
A 5 μm red Cu powder was obtained.
【００２０】実施例１２ まず、ＣｄＣｌ2 とＮａ2 Ｓ2 Ｏ3 を準備した。これら
のＣｄＣｌ2 ０．０８ｍｏｌ／ＬとＮａ2 Ｓ2 Ｏ3 ０．
０４ｍｏｌ／Ｌとにクエン酸０．３４ｍｏｌ／Ｌ、ＥＤ
ＴＡ０．０８ｍｏｌ／Ｌ、ＮＴＡ０．２０ｍｏｌ／Ｌを
加えて混合水溶液とした。この混合水溶液に還元剤とし
てＴｉＣｌ3 ０．０４ｍｏｌ／Ｌを添加し、２８％アン
モニア水を加えてｐＨ１０に調整した。そして、混合水
溶液の温度８０℃で約３０分間攪拌した。このようにし
て、粒径０．８μｍの黄色のＣｄＳ粉末を得た。また、
同様な方法により、化合物半導体であるＩｎＳｂ合金粉
末なども作製することができる。 Example 12 First, CdCl 2 and Na 2 S 2 O 3 were prepared. These CdCl 2 0.08 mol / L and Na 2 S 2 O 3 0.
0.44 mol / L citric acid 0.34 mol / L, ED
A mixed aqueous solution was prepared by adding 0.08 mol / L of TA and 0.20 mol / L of NTA. 0.04 mol / L of TiCl 3 was added as a reducing agent to the mixed aqueous solution, and the pH was adjusted to 10 by adding 28% aqueous ammonia. Then, the mixture was stirred at a temperature of 80 ° C. for about 30 minutes. Thus, a yellow CdS powder having a particle size of 0.8 μm was obtained. Also,
In a similar manner, an InSb alloy powder or the like as a compound semiconductor can be manufactured.
【００２１】このように、この発明の製造方法を用いれ
ば、安全かつ簡単に粒径の小さい高純度微粉末を得るこ
とができる。しかも、機械的粉砕法のように粉塵公害な
どが発生せず、しかも低コストで微粉末を製造すること
ができる。As described above, by using the production method of the present invention, a high-purity fine powder having a small particle size can be obtained safely and easily. Further, unlike the mechanical pulverization method, dust pollution and the like do not occur, and fine powder can be produced at low cost.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) B22F 9/24 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 7 , DB name) B22F 9/24
Claims (8)
族，２Ｂ族，３Ｂ族，４Ｂ族，５Ｂ族，６Ｂ族および８
族の金属または非金属の塩である水溶性の化合物または
水溶性錯体の水溶液を準備するステップ、および前記水
溶液に三塩化チタンを添加し、前記三塩化チタンの還元
作用を用いて、前記金属粉末，前記金属および前記非金
属の２種類以上を含有する合金粉末または化合物粉末の
いずれかの微粉末を製造するステップを含む、微粉末の
製造方法。1. Group 6A, 7A, 1B of the periodic table of elements
Groups 2B, 3B, 4B, 5B, 6B and 8
Preparing an aqueous solution of a water-soluble compound or a water-soluble complex that is a metal or nonmetal salt of group III, and adding titanium trichloride to the aqueous solution, and using the reducing action of the titanium trichloride to form the metal powder. , A method for producing a fine powder, comprising the step of producing a fine powder of either an alloy powder or a compound powder containing two or more of the metal and the non-metal.
族の元素としてＲｅ、前記１Ｂ族の元素としてＣｕ，Ａ
ｇ，Ａｕ、前記２Ｂ族の元素としてＺｎ，Ｃｄ、前記３
Ｂ族の元素としてＩｎ、前記４Ｂ族の元素としてＳｎ，
Ｐｂ、前記５Ｂ族の元素としてＳｂ，Ａｓ，Ｂｉ、前記
６Ｂ族の元素としてＴｅ，Ｓｅ，Ｓ、前記８族の元素と
してＮｉ，Ｒｕ，Ｒｈ，Ｐｄ，Ｐｔ，Ｏｓ，Ｉｒを含
む、請求項１に記載の微粉末の製造方法。2. The element of Group 6A is Mo, and the element of Group 7A is Mo.
Re as a group III element and Cu, A as a group 1B group element
g, Au, Zn, Cd, and 3
In as a group B element, Sn as a 4B element.
Pb, Sb, As, Bi as the group 5B element, Te, Se, S as the group 6B element, and Ni, Ru, Rh, Pd, Pt, Os, Ir as the group 8 element. 2. The method for producing a fine powder according to 1.
である、請求項１または請求項２に記載の微粉末の製造
方法。3. The method according to claim 1, wherein the temperature of the aqueous solution is equal to or lower than the boiling point of the solution.
が大気中または加圧中で行われる、請求項１ないし請求
項３のいずれかに記載の微粉末の製造方法。4. The method for producing a fine powder according to claim 1, wherein the reaction between the aqueous solution and the titanium trichloride is performed in the air or under pressure.
載の微粉末の製造方法で製造したＳｎ粉，Ｐｂ粉またはPowder, Sn powder or Pb powder produced by the method for producing fine powder described above.
Ｉｎ粉を含む、はんだ材料。Solder material containing In powder.
載の微粉末の製造方法で製造したＰｂ粉またはＩｎ粉をPb powder or In powder produced by the method for producing fine powder described above
含む、焼結材料。Including, sintered materials.
載の微粉末の製造方法で製造したＮｉ粉を含む、電極材Material containing Ni powder produced by the method for producing fine powder described above
料。Fees.
載の微粉末の製造方法で製造したＣｄＳ粉を含む、太陽Including CdS powder produced by the method for producing fine powder described above,
電池材料。Battery material.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3270162A JP3018655B2 (en) | 1991-09-20 | 1991-09-20 | Manufacturing method of fine powder |
| US08/257,268 US5435830A (en) | 1991-09-20 | 1994-06-09 | Method of producing fine powders |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3270162A JP3018655B2 (en) | 1991-09-20 | 1991-09-20 | Manufacturing method of fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0578716A JPH0578716A (en) | 1993-03-30 |
| JP3018655B2 true JP3018655B2 (en) | 2000-03-13 |
Family
ID=17482402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3270162A Expired - Lifetime JP3018655B2 (en) | 1991-09-20 | 1991-09-20 | Manufacturing method of fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3018655B2 (en) |
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|---|---|---|---|---|
| US7470306B2 (en) | 2002-06-14 | 2008-12-30 | Sumitomo Electric Industries, Ltd. | Method for producing fine metal powder |
| US7850760B2 (en) | 2004-04-30 | 2010-12-14 | Sumitomo Electric Industries, Ltd. | Process for production of chain metal powders, chain metal powders produced thereby, and anisotropic conductive film formed using the powders |
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Also Published As
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|---|---|
| JPH0578716A (en) | 1993-03-30 |
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