JPH02294416A - Production of platinum powder - Google Patents

Production of platinum powder

Info

Publication number
JPH02294416A
JPH02294416A JP11408389A JP11408389A JPH02294416A JP H02294416 A JPH02294416 A JP H02294416A JP 11408389 A JP11408389 A JP 11408389A JP 11408389 A JP11408389 A JP 11408389A JP H02294416 A JPH02294416 A JP H02294416A
Authority
JP
Japan
Prior art keywords
ammonium
platinum
hydrazine
compd
particle size
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
Application number
JP11408389A
Other languages
Japanese (ja)
Inventor
Yuji Takeda
有司 武田
Masayuki Sakurai
桜井 正之
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ishifuku Metal Industry Co Ltd
Original Assignee
Ishifuku Metal Industry Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Ishifuku Metal Industry Co Ltd filed Critical Ishifuku Metal Industry Co Ltd
Priority to JP11408389A priority Critical patent/JPH02294416A/en
Publication of JPH02294416A publication Critical patent/JPH02294416A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To produce spherical platinum powder of uniform particle size by adding an ammonium compd. to an aq. soln. or suspension of a platinum compd. and using a hydrazine compd. as a reducing agent. CONSTITUTION:An ammonium compd. such as ammonium hydroxide, ammonium acetate, ammonium carbonate, ammonium borate, ammonium chloride or ammonium tartrate is added to an aq. soln. or suspension of a platinum compd. such as chloroplatinic acid, ammonium chloroplatinate or potassium chloroplatinate. A hydrazine compd. such as hydrazine hydrate, hydrazine hydrochloride or hydrazine sulfate as a reducing agent is then added to the soln. or suspension to deposit fine platinum particles whose particle size can be controlled to the range of 0.5-8.0mum.

Description

【発明の詳細な説明】 〈産業上の利用分野〉 開示技術は球形で粒度がコントロールできる電子工業等
で用いる白金粉末の製造の技術分野に属する。
DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The disclosed technology belongs to the technical field of manufacturing platinum powder used in the electronic industry etc., which is spherical and whose particle size can be controlled.

〈要旨の概要〉 而して、この出願の発明は電子工業や窯業において用い
られる白金粉末の製造において、塩化白金酸アンモニウ
ム、塩化白金酸カリウム等の溶液を塩酸ヒドラジン等の
還元剤により還元させて白金粉末を析出沈降させるよう
にした白金粉末製造方法に関する発明であり、特に、白
金化合物に対する還元剤に硫酸ヒドラジン等のビドラジ
ン化合物を用いるようにし、更に、添加剤としては水酸
化ア,ンモニウム等のアンモニア化合物を用い、析出す
る粉末の各々の形状が球形であり、0.5〜8.0μm
の範囲で粒度が均一にコントロールざれることが可能で
あるようにした白金粉末の製造方法に係る発明である。
<Summary of the gist> The invention of this application is to reduce a solution of ammonium chloroplatinate, potassium chloroplatinate, etc. with a reducing agent such as hydrazine hydrochloride in the production of platinum powder used in the electronics industry and the ceramic industry. This invention relates to a method for manufacturing platinum powder in which platinum powder is precipitated and precipitated. In particular, a hydrazine compound such as hydrazine sulfate is used as a reducing agent for the platinum compound, and further, as an additive, ammonium hydroxide or the like is used. Using an ammonia compound, the shape of each powder to be precipitated is spherical and 0.5 to 8.0 μm.
This invention relates to a method for producing platinum powder that allows the particle size to be uniformly controlled within the range of .

く従来技術〉 当業者に周知の如く、例えば、電子工槃や窯業において
、白金粉末を不活性液体のビヒクル中に分散させて白金
ペーストと成し、該ペーストをセラミック材等に塗布し
たり印刷したりしてコーティングした後に、焼成して白
金膜を得て種々の電気的な特性や装飾的特性を具備させ
るようにした技術が開発され、実用化されており、当然
のことながらかかるセラミック材等にコーティングする
白金粉末の粒度が均一であり、粒子の粒径が整ってその
分布幅が狭いことが最終製品の精度向上にプラスするた
めに得られる白金粉末についての粒度や粒径均一につい
て高精度のものが得られる技術が研究されている。
As is well known to those skilled in the art, for example, in the electronics and ceramic industries, platinum powder is dispersed in an inert liquid vehicle to form a platinum paste, and the paste is coated or printed on ceramic materials, etc. A technique has been developed and put into practical use in which a platinum film is obtained by coating the ceramic material with various electrical properties and decorative properties. The particle size and particle size uniformity of the platinum powder obtained as a coating is uniform, and the uniform particle size and narrow distribution width of the platinum powder improves the precision of the final product. Research is being carried out on techniques that can provide high precision.

く発明が解決しようとする課題〉 しかしながら、従来の白金粉末の製造方法は、白金化合
物の水溶液中に水酸化ナトリウムを加え、ヒドラジン、
ギ酸、水素化ほう素ナトリウム等の還元剤により白金粉
末を得る方法が用いられていた。
Problems to be Solved by the Invention However, in the conventional method for producing platinum powder, sodium hydroxide is added to an aqueous solution of a platinum compound, hydrazine,
A method of obtaining platinum powder using a reducing agent such as formic acid or sodium borohydride has been used.

ざりながら、このような方法によって得られる白金粉末
は、粒子形状が不規則で、しかも、粒子同士が凝集し、
粒度が不均一のものしか得られない欠点があった。
However, the platinum powder obtained by this method has an irregular particle shape, and the particles tend to aggregate with each other.
There was a drawback that only particles with non-uniform particle size could be obtained.

〈発明の目的〉 この出願の発明の目的は上述従来技術に基づく電子工業
や窯業に用いられる白金粉末の製造の問題点を解決すべ
き技術的課題とし、粒子の形状が規則的で、しかも、粒
子同士が凝集せず、粒度が均一でその分布幅が狭く、最
終製品に対するコーティング精度等が著しく向上するこ
とが出来るようにして窯業や電子工業における成形技術
利用分野に益する優れた白金粉末の製造方法を提供Vん
とするものである。
<Object of the Invention> The object of the invention of this application is to solve the technical problem of manufacturing platinum powder used in the electronic industry and ceramic industry based on the above-mentioned prior art, and to solve the problem of producing platinum powder that has a regular particle shape, and This is an excellent platinum powder that does not agglomerate with each other, has a uniform particle size, has a narrow distribution width, and can significantly improve the coating precision of the final product, which is beneficial to the field of molding technology in the ceramics and electronics industries. The manufacturing method is provided by V.

〈課題を解決するための手段・作用〉 上述目的に沿い先述特許請求の範囲を要旨とするこの発
明の構成は前述課題を解決するために、白金化合物の水
溶液にヒドラジン等で還元する際に、アンモニア化合物
を添加することによって粒子形状が球形で、しかも、粒
度が均一な白金粉末が得られるようにし、この運元プロ
セスにおいて、アンモニア化合物の添加量を制御するこ
とによって、得られる白金粉末の粒径を0.5〜8.0
μmの範囲にコントロール出来るようにした技術的手段
を講じたものでおる。
<Means/effects for solving the problem> In order to solve the above-mentioned problem, the structure of the present invention, which is summarized in the above-mentioned claims, is to solve the above-mentioned problem by reducing the aqueous solution of a platinum compound with hydrazine or the like. Platinum powder with a spherical particle shape and uniform particle size can be obtained by adding an ammonia compound, and by controlling the amount of the ammonia compound added in this source process, the resulting platinum powder particles are Diameter 0.5-8.0
Technical measures have been taken to enable control within the μm range.

又、この出願の発明の製造方法において使用可能な白金
化合物は、塩化白金酸Hz (PtCjs )5H 2
0 ,塩化白金酸アンモニウム(NH.s)z(PjC
Js)、塩化白金駁カリウムK2 (PtC1’s )
等で、水溶液の状態でも、水に懸濁した状態でも良い。
Further, the platinum compound that can be used in the production method of the invention of this application is chloroplatinic acid Hz (PtCjs)5H 2
0, ammonium chloroplatinate (NH.s)z (PjC
Js), platinum potassium chloride K2 (PtC1's)
etc., and may be in the form of an aqueous solution or suspended in water.

次に、還元剤については、ヒドラジン水和物、塩酸ヒド
ラジン、硫酸ヒドラジン等のヒドラジン化合物に限定し
、ギ酸、水素化ほう素ナトリウム等の他の還元剤では、
不規則形状に凝集した粉末しか得られない。
Next, the reducing agent is limited to hydrazine compounds such as hydrazine hydrate, hydrazine hydrochloride, and hydrazine sulfate; other reducing agents such as formic acid and sodium borohydride are
Only irregularly shaped agglomerated powders are obtained.

又、還元剤の使用量は、反応における理論母より過剰で
あれば良い。
Further, the amount of the reducing agent used may be in excess of the theoretical value in the reaction.

次に、添加剤として用いるアンモニア化合物については
、水酸化アンモニウム、酢酸アンモニウム、炭酸アンモ
ニウム、ほう酸アンモニウム、塩化アンモニウム、酒石
酸アンモニウム等で特に限定はしない。
Next, the ammonia compound used as an additive is not particularly limited, and may include ammonium hydroxide, ammonium acetate, ammonium carbonate, ammonium borate, ammonium chloride, ammonium tartrate, and the like.

而して、アンモニア化合物の添加量は、Pt’lmoJ
に対しNH3として4〜1 3moノとし、この範囲で
制御することによって、白金粉末の粒径を0.5〜8.
0μmの範囲でコントロールすることが出来る。
Therefore, the amount of ammonia compound added is Pt'lmoJ
In contrast, the particle size of the platinum powder is set to 4 to 13 mo, and the particle size of the platinum powder is controlled within this range.
It can be controlled within a range of 0 μm.

第1図にPt11110Jに対するNtl3の添加量と
白金粉末の粒径との関係を示す。
FIG. 1 shows the relationship between the amount of Ntl3 added to Pt11110J and the particle size of platinum powder.

アンモニアの添加量が1moJlに対して4!IIOJ
未満では、球形が失われて、粒度が不均一になり、13
mofを越えると粒径が細かくなりすぎて、粒子同士が
凝集してくる。
The amount of ammonia added is 4 per moJl! IIOJ
If it is less than 13, the spherical shape is lost and the particle size becomes non-uniform.
If mof is exceeded, the particle size becomes too fine and the particles tend to aggregate with each other.

次に反応温度は特に限定しないが、50℃以上の高温で
反応することが望ましい。
Next, the reaction temperature is not particularly limited, but it is desirable to carry out the reaction at a high temperature of 50° C. or higher.

50℃未満の低温で反応すると反応が速度が遅く、作業
性が悪いうえ、生成される粉末も粒度が不均一になる1
頃向にある。
If the reaction is carried out at a low temperature below 50°C, the reaction rate will be slow, workability will be poor, and the resulting powder will have non-uniform particle size1.
It's in the corner.

〈実施例〉 《実施例1》 Pt509を含む塩化白金酸水溶液250mを80℃に
加熱して、これをaとする。
<Example><<Example1>> 250 m of a chloroplatinic acid aqueous solution containing Pt509 is heated to 80°C, and this is designated as a.

80%ヒドラジン水和物25d1及び、883として3
53を含む酢酸アンモニウムに純水を800d加え80
℃に加熱し、これをbとする。
80% hydrazine hydrate 25d1 and 3 as 883
Add 800d of pure water to ammonium acetate containing 53
Heat to ℃ and call this b.

そして、反応方法は、aを80’Cに保持したまま攪拌
し、これにbを徐々に滴下した。
The reaction method was as follows: a was stirred while being maintained at 80'C, and b was gradually added dropwise thereto.

滴下終了後は、1時間攪拌し、反応を終了させた。After the dropwise addition was completed, the mixture was stirred for 1 hour to complete the reaction.

1qられた沈澱は、周知の工程で、洗浄、ろ過、乾燥を
行った。
1 q of precipitate was washed, filtered, and dried using well-known steps.

このようにして得られた白金粉末は1μmで粒度が均一
な球形粉末であった。
The platinum powder thus obtained was a spherical powder with a uniform particle size of 1 μm.

(実施例2) Pt509を含む塩化白金酸アンモンに、NH3として
21tjを含むNt14 0N水溶液250dを加え、
80℃に加熱し攪拌する。
(Example 2) 250 d of Nt14 0N aqueous solution containing 21tj as NH3 was added to ammonium chloroplatinate containing Pt509,
Heat to 80°C and stir.

これに80℃に加熱した塩酸ヒドラジン409を含む水
溶液800mIlを徐々に滴下した。
To this, 800 ml of an aqueous solution containing hydrazine hydrochloride 409 heated to 80° C. was gradually added dropwise.

滴下終了後は、1時間攪拌し、反応を終了させた。After the dropwise addition was completed, the mixture was stirred for 1 hour to complete the reaction.

得られた沈澱は、周知の工程で、洗浄、ろ過、乾燥を行
った。
The obtained precipitate was washed, filtered, and dried using well-known steps.

このようにして得られた白金粉末は5μmで粒度が均一
な球形粉末であった。
The platinum powder thus obtained was a spherical powder with a uniform particle size of 5 μm.

〈発明の効果〉 以上、この出願の発明によれば、粒子形状が規則的に球
形で、しかも、粒度が均一な白金粉末が容易に製造出来
、従来の方法では得られない画期的な白金粉末製造方法
とする優れた効果が秦ざれる。
<Effects of the Invention> As described above, according to the invention of this application, platinum powder with a regularly spherical particle shape and uniform particle size can be easily produced, and a groundbreaking platinum powder that cannot be obtained by conventional methods can be produced. The powder manufacturing method has excellent effects.

而して、塩化白金酸の白金化合物に対する還元剤に@酸
ヒドラジン等のヒドラジン化合物を用いたことにより、
析出する白金粉末に形状を規則的に均一にする優れた効
果が奏される。
By using a hydrazine compound such as @acid hydrazine as a reducing agent for the platinum compound of chloroplatinic acid,
This provides an excellent effect of making the precipitated platinum powder regular and uniform in shape.

又、添加剤として塩化アンモニウム等のアンモニア化合
物を適宜に制御することにより、白金粉末の粒径を0.
5〜8.0μmの範囲にコントロールすることが出来、
セラミック材等への塗布や印刷等のコーティング等に際
しての白金薄膜の精度を高めることが出来るという優れ
た効果が奏される。
In addition, by appropriately controlling an ammonia compound such as ammonium chloride as an additive, the particle size of platinum powder can be reduced to 0.
It can be controlled within the range of 5 to 8.0 μm,
An excellent effect is achieved in that the precision of the platinum thin film can be improved when coating ceramic materials or the like, printing or the like.

又、各粒子の形状を確実に球形にすることが出来、粒度
を均一にする効果もある。
Moreover, the shape of each particle can be reliably made into a spherical shape, and there is also an effect of making the particle size uniform.

【図面の簡単な説明】[Brief explanation of drawings]

図面の第1図はこの出願の発明の実施例における白金1
モルに対するアンモニアの添加量(モル)と平均粒径と
の関係を示す特性曲線グラフ図である。 第1図
Figure 1 of the drawings shows platinum 1 in an embodiment of the invention of this application.
FIG. 2 is a characteristic curve graph showing the relationship between the amount of ammonia added (mol) and the average particle size. Figure 1

Claims (2)

【特許請求の範囲】[Claims] (1)白金化合物を湿式で還元させて粉末化する白金粉
末製造方法において、白金化合物に対する還元剤にヒド
ラジン化合物を用い、添加剤としてアンモニア化合物を
用いて析出する各粉末が球形で粒度が均一にされるよう
にすることを特徴とする白金粉末の製造方法。
(1) In a platinum powder production method in which a platinum compound is wet-reduced and powdered, a hydrazine compound is used as a reducing agent for the platinum compound, and an ammonia compound is used as an additive, so that each powder that is precipitated is spherical and has a uniform particle size. A method for producing platinum powder, characterized in that:
(2)上記添加剤として使用するアンモニア化合物を制
御することにより、上記粉末の粒径を0.5〜8.0μ
mの範囲にコントロールすることが出来るようにするこ
とを特徴とする特許請求の範囲第1項記載の白金粉末の
製造方法。
(2) By controlling the ammonia compound used as the additive, the particle size of the powder can be adjusted to 0.5 to 8.0μ.
2. The method for producing platinum powder according to claim 1, wherein the platinum powder can be controlled within a range of m.
JP11408389A 1989-05-09 1989-05-09 Production of platinum powder Pending JPH02294416A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11408389A JPH02294416A (en) 1989-05-09 1989-05-09 Production of platinum powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11408389A JPH02294416A (en) 1989-05-09 1989-05-09 Production of platinum powder

Publications (1)

Publication Number Publication Date
JPH02294416A true JPH02294416A (en) 1990-12-05

Family

ID=14628648

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11408389A Pending JPH02294416A (en) 1989-05-09 1989-05-09 Production of platinum powder

Country Status (1)

Country Link
JP (1) JPH02294416A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011162868A (en) * 2010-02-15 2011-08-25 Yamamoto Precious Metal Co Ltd Method for manufacturing noble metal fine particle
US8758476B2 (en) 2008-08-28 2014-06-24 Jx Nippon Mining & Metals Corporation Method of producing mixed powder comprising noble metal powder and oxide powder, and mixed powder comprising noble metal powder and oxide powder
JP2014169484A (en) * 2013-03-04 2014-09-18 Sumitomo Metal Mining Co Ltd Method for producing platinum powder
JP2015117387A (en) * 2013-12-16 2015-06-25 住友金属鉱山株式会社 Method for producing high-purity platinum powder
JP2015209569A (en) * 2014-04-25 2015-11-24 アサヒプリテック株式会社 Production method of platinum powder
CN108907217A (en) * 2018-07-27 2018-11-30 江苏北矿金属循环利用科技有限公司 A kind of method that short route prepares Ultrafine Platinum Powder
CN108941597A (en) * 2018-07-27 2018-12-07 江苏北矿金属循环利用科技有限公司 A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt
CN114604911A (en) * 2022-03-08 2022-06-10 金川集团股份有限公司 Method for removing potassium and sodium from ammonium chloroplatinate product

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5855204A (en) * 1981-09-28 1983-04-01 永大産業株式会社 Manufacture of member for building or furniture
JPS63312906A (en) * 1987-06-16 1988-12-21 Daido Steel Co Ltd Production of fine silver alloy powder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5855204A (en) * 1981-09-28 1983-04-01 永大産業株式会社 Manufacture of member for building or furniture
JPS63312906A (en) * 1987-06-16 1988-12-21 Daido Steel Co Ltd Production of fine silver alloy powder

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8758476B2 (en) 2008-08-28 2014-06-24 Jx Nippon Mining & Metals Corporation Method of producing mixed powder comprising noble metal powder and oxide powder, and mixed powder comprising noble metal powder and oxide powder
JP2011162868A (en) * 2010-02-15 2011-08-25 Yamamoto Precious Metal Co Ltd Method for manufacturing noble metal fine particle
JP2014169484A (en) * 2013-03-04 2014-09-18 Sumitomo Metal Mining Co Ltd Method for producing platinum powder
JP2015117387A (en) * 2013-12-16 2015-06-25 住友金属鉱山株式会社 Method for producing high-purity platinum powder
JP2015209569A (en) * 2014-04-25 2015-11-24 アサヒプリテック株式会社 Production method of platinum powder
CN108907217A (en) * 2018-07-27 2018-11-30 江苏北矿金属循环利用科技有限公司 A kind of method that short route prepares Ultrafine Platinum Powder
CN108941597A (en) * 2018-07-27 2018-12-07 江苏北矿金属循环利用科技有限公司 A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt
CN114604911A (en) * 2022-03-08 2022-06-10 金川集团股份有限公司 Method for removing potassium and sodium from ammonium chloroplatinate product
CN114604911B (en) * 2022-03-08 2023-09-22 金川集团股份有限公司 Method for removing potassium and sodium from ammonium chloroplatinate product

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