JPH10102103A - Method for producing highly crystalline platinum powder - Google Patents
Method for producing highly crystalline platinum powderInfo
- Publication number
- JPH10102103A JPH10102103A JP28016096A JP28016096A JPH10102103A JP H10102103 A JPH10102103 A JP H10102103A JP 28016096 A JP28016096 A JP 28016096A JP 28016096 A JP28016096 A JP 28016096A JP H10102103 A JPH10102103 A JP H10102103A
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- platinum powder
- salt
- platinum
- powder
- highly crystalline
- Prior art date
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
(57)【要約】
【目的】 品質の安定した高結晶性白金粉末を得ること
ができ、安全に製造でき、自動化可能な白金粉末の製造
方法を提供しようとするものである。
【構成】 スペーサとして、アルカリ塩またはアルカリ
土類金属塩から選んだ少なくとも一種の塩を用い、これ
を白金ブラックと湿式混合してから乾燥して粉砕し、こ
れを焼成して希酸処理してガスと塩とを除去した後、水
洗、乾燥して高結晶性の白金粉末を得る。アリカリ塩ま
たはアルカリ土類金属塩から選んだ少なくとも一種の塩
としては、炭酸カルシウムを好適に用いることができ、
かかる塩の混合量によって完成白金粉末の平均粒径を調
整することが出来る。
(57) [Abstract] [Object] It is an object of the present invention to provide a method for producing platinum powder which can obtain highly crystalline platinum powder of stable quality, which can be safely produced, and which can be automated. [Constitution] At least one salt selected from an alkali salt or an alkaline earth metal salt is used as a spacer, which is wet-mixed with platinum black, dried, pulverized, fired, and treated with a dilute acid. After removing the gas and salt, it is washed with water and dried to obtain a highly crystalline platinum powder. As at least one salt selected from alkali salts or alkaline earth metal salts, calcium carbonate can be suitably used,
The average particle size of the finished platinum powder can be adjusted by the amount of the salt mixed.
Description
【０００１】[0001]
【発明の属する技術分野】この発明は、有毒ガスの発生
無しに低コストで製造することが出来、粒度分布範囲が
狭く、高純度な白金粉末を得ることが出来る高結晶性白
金粉末の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing highly crystalline platinum powder which can be produced at low cost without generating toxic gas, has a narrow particle size distribution range, and can produce high-purity platinum powder. About.
【０００２】[0002]
【従来の技術】一般に、白金粉末は、導体ペースト、抵
抗ペースト、誘電体ペースト、その他の主原料として用
いられ、集積回路等の各種の回路網、サーマルヘッド、
チップ抵抗器、積層コンデンサ、その他の用途に活用さ
れている。このため従来は、白金王水溶解液に還元剤と
しての塩化アンモニウム等を投入して、塩化白金酸アン
モニウム等を析出させ、この塩化白金酸アンモニウムを
焼成して塩化水素ガスやアンモニアガスを除去し、その
後熱濃硫酸処理により不純物を除去して水洗乾燥させる
ことにより、白金ブラックの２倍から３倍の結晶度であ
る、結晶度６５００ｃｐｓ程度の白金粉末を得ていた。2. Description of the Related Art Generally, platinum powder is used as a conductor paste, a resistance paste, a dielectric paste, and other main raw materials, and is used for various circuit networks such as integrated circuits, thermal heads, and the like.
It is used for chip resistors, multilayer capacitors, and other applications. For this reason, conventionally, ammonium chloride or the like as a reducing agent is added to a solution of platinum aqua regia to precipitate ammonium chloroplatinate and the like, and the ammonium chloroplatinate is calcined to remove hydrogen chloride gas and ammonia gas. Then, impurities were removed by hot concentrated sulfuric acid treatment, followed by washing and drying to obtain platinum powder having a crystallinity of about 6500 cps, which is twice to three times the crystallinity of platinum black.
【０００３】[0003]
【発明が解決しようとする課題】この様な従来の白金粉
末の製造方法によれば、強酸性液体の取り扱いを要し、
かつ塩化水素ガスやアンモニアガス等の有毒ガスの発生
が有った為、慎重な手作業を余儀なくされ多大な費用と
時間を必要とした。また、不純物の溶解除去のために熱
濃硫酸を用いなければならず、溶解工程の所用時間がロ
ットによりまちまちであるため、自動化もままならない
状態であり、溶解液や溶解ロスの回収も要求され、きわ
めて煩雑なものであり、かつ得られる白金粉末の純度や
粒度分布もあまり好ましいものではなかった。According to such a conventional method for producing platinum powder, handling of a strongly acidic liquid is required,
In addition, due to the generation of toxic gases such as hydrogen chloride gas and ammonia gas, careful manual work was required, which required a great deal of cost and time. In addition, hot concentrated sulfuric acid must be used for dissolving and removing impurities, and the time required for the dissolving process varies depending on the lot, so automation cannot be maintained, and recovery of the dissolving solution and dissolution loss is also required. It was extremely complicated, and the purity and particle size distribution of the obtained platinum powder were not very favorable.
【０００４】そこでこの発明は、自動化可能であり、品
質の安定した高結晶性白金粉末を提供出来る白金粉末の
製造方法を提供することを目的とする。Accordingly, an object of the present invention is to provide a method for producing platinum powder that can be automated and can provide highly crystalline platinum powder with stable quality.
【０００５】[0005]
【課題を解決するための手段】この発明の目的は、白金
ブラックと、アルカリ塩またはアルカリ土類金属塩から
選んだ少なくとも一種の塩とを湿式混合して乾燥後粉砕
し、その粉砕体を焼成してガスを除去後希酸によって塩
を溶解させて水洗除去し、これを乾燥して白金粉末を得
る高結晶性白金粉末の製造方法によって達成出来る。SUMMARY OF THE INVENTION An object of the present invention is to provide platinum black and at least one salt selected from alkali salts or alkaline earth metal salts by wet mixing, drying and pulverizing, and firing the pulverized body. After removing the gas, the salt is dissolved with a dilute acid, washed and removed with water, and dried to obtain a platinum powder.
【０００６】この発明の目的は、白金ブラックと炭酸カ
ルシウムとを湿式混合して乾燥後粉砕し、しかる後にこ
の粉砕体を焼成して炭酸ガスを除去してから残余の酸化
カルシウムを希酸にて溶解させて水洗除去し、これを乾
燥して白金粉末を得る高結晶性白金粉末の製造方法によ
って達成出来る。It is an object of the present invention to provide a method of mixing platinum black and calcium carbonate by wet mixing, drying and pulverizing the powder, and then calcining the pulverized product to remove carbon dioxide gas, and then removing the remaining calcium oxide with a dilute acid. It can be achieved by a method for producing a highly crystalline platinum powder which is dissolved, washed and removed, and dried to obtain a platinum powder.
【０００７】この発明の目的は、アルカリ塩またはアル
カリ土類金属塩から選んだ少なくとも一種の塩と白金ブ
ラックとの混合比率は２：１から１６：１の範囲である
「請求項１」または「請求項２」の高結晶性白金粉末の
製造方法によって達成出来る。[0007] An object of the present invention is that the mixing ratio of at least one salt selected from alkali salts or alkaline earth metal salts and platinum black is in the range of 2: 1 to 16: 1. This can be achieved by the method of claim 2 for producing a highly crystalline platinum powder.
【０００８】更に、この発明の目的は、アルカリ塩また
はアルカリ土類金属塩から選んだ少なくとも一種の塩の
白金ブラックへの混合量によって完成白金粉末の平均粒
径を制御する「請求項１」または「請求項２」の高結晶
性白金粉末の製造方法によって達成できる。Further, an object of the present invention is to control the average particle size of the finished platinum powder by controlling the amount of at least one salt selected from alkali salts or alkaline earth metal salts mixed with platinum black. This can be achieved by the method of claim 2 for producing a highly crystalline platinum powder.
【０００９】[0009]
【発明の実施の形態】この発明によれば、先ず、アルカ
リ塩またはアルカリ土類金属塩から選んだ少なくとも一
種の塩と白金ブラックとが水を加えられて湿式混合され
る。この湿式混合によって塩と白金ブラックとがほぼ均
等に混在する所となり、乾燥後の粉砕において１／１０
ミクロン程度に微細粉砕される。塩と白金ブラックとの
混合比は、２：１から１６：１の範囲で好適な品質の高
結晶性白金粉末が得られる。白金ブラックは、白金塩水
溶液を還元して得るか、電解によって得られる。DESCRIPTION OF THE PREFERRED EMBODIMENTS According to the present invention, at least one salt selected from an alkali salt or an alkaline earth metal salt and platinum black are wet mixed with water. Due to this wet mixing, the salt and the platinum black are mixed almost uniformly, and 1/10 in the pulverization after drying.
Finely pulverized to about a micron. When the mixing ratio of the salt to the platinum black is in the range of 2: 1 to 16: 1, a highly crystalline platinum powder of suitable quality can be obtained. Platinum black is obtained by reducing an aqueous solution of a platinum salt or obtained by electrolysis.
【００１０】湿式混合後、約１２０゜Cの温度で乾燥して
から遊星ミル等を用いて粉砕してから約９００゜C前後の
温度で焼成する。この焼成工程によって、ガスが除去さ
れると共に、白金粉末の結晶度が調整される。焼成工程
終了後、例えば３倍希釈の硝酸水溶液等の希酸を用いて
酸処理を行い、塩を溶解し、これを水洗して塩を流出さ
せてから乾燥し、メッシュパスさせて白金粉末を得る。
この酸処理によって、スペーサとして介在する塩は完全
に溶出して水洗によって除去されるため乾燥によって９
９．９％以上の純度の白金粉末が得られる。このためロ
ス回収は不用となる。かくして得られる白金粉末の平均
粒径は、白金ブラックに混合するアルカリ塩またはアル
カリ土類金属塩から選んだ少なくとも一種の塩の混合量
等によって制御出来る。After wet mixing, the mixture is dried at a temperature of about 120 ° C., pulverized using a planetary mill or the like, and then fired at a temperature of about 900 ° C. This firing step removes gas and adjusts the crystallinity of the platinum powder. After the calcination step is completed, an acid treatment is performed using a dilute acid such as a three-fold diluted nitric acid aqueous solution to dissolve the salt, wash it with water, drain the salt, dry, and pass through a mesh to remove the platinum powder. obtain.
By this acid treatment, the salt interposed as a spacer is completely eluted and removed by washing with water, so that the salt is removed by drying.
A platinum powder having a purity of 9.9% or more is obtained. For this reason, loss recovery becomes unnecessary. The average particle size of the platinum powder thus obtained can be controlled by the amount of at least one kind of salt selected from alkali salts or alkaline earth metal salts mixed with platinum black.
【００１１】[0011]
【実施例１】白金ブラック２０ｇと炭酸カルシウム４０
ｇとに水を加えて湿式混合してから乾燥機に入れて１２
０゜Cで乾燥した後、遊星ミル内に投入して粉砕した。こ
の粉砕粉を横型管状炉に入れて４時間かけて１０００゜C
に上昇させてから２時間の間１０００゜Cに維持し、その
後４時間かけて常温まで冷却させて、炭酸ガスを除去す
ると共に白金粉末の結晶度を促進させた。Example 1 20 g of platinum black and 40 of calcium carbonate
g and water and wet-mixed, then put in a dryer for 12
After drying at 0 ° C., it was charged into a planetary mill and pulverized. This pulverized powder is put in a horizontal tubular furnace, and is heated at 1000 ° C for 4 hours.
Then, the temperature was maintained at 1000 ° C. for 2 hours, and then cooled to room temperature over 4 hours to remove carbon dioxide gas and promote the crystallinity of the platinum powder.
【００１２】冷却後の粉砕粉に、３倍希釈硝酸水溶液を
間隔をおいて３回注入して酸化カルシウムを溶解させて
から、これを５回水洗して、完全に酸化カルシウムを除
去した。その後、残留分を乾燥機にいれて１２０゜Cで乾
燥させ、ナイロンメッシュを用いてメッシュパスさせ、
高結晶性の白金粉末を得た。After cooling, the calcium oxide was dissolved by injecting a three-fold diluted nitric acid aqueous solution into the pulverized powder three times at intervals, and then washed five times with water to completely remove the calcium oxide. Thereafter, the residue was put in a dryer and dried at 120 ° C., and passed through a mesh using a nylon mesh.
A highly crystalline platinum powder was obtained.
【００１３】得られた白金粉末の結晶度は１２１００ｃ
ｐｓ、比表面積は１．１ｍ2／ｇ、純度９９．９％、１
０％平均粒径０．３５μｍ、５０％平均粒径０．６２μ
ｍ、９０％平均粒径１．１３μｍであった。特に、従来
の白金粉末の１０％平均粒径と９０％平均粒径との差が
約１７μｍ前後であった点と比較すると、この発明によ
る白金粉末はその差が１μｍ未満であり、極めて安定し
たシャープな粒度分布となる。また、白金粉末の外観
は、図１に示す写真（１００００倍）の通りである。The crystallinity of the obtained platinum powder is 12100 c
ps, specific surface area 1.1 m 2 / g, purity 99.9%, 1
0% average particle size 0.35μm, 50% average particle size 0.62μ
m, 90% average particle size 1.13 μm. In particular, when compared with the point where the difference between the 10% average particle size and the 90% average particle size of the conventional platinum powder was about 17 μm, the difference of the platinum powder according to the present invention was less than 1 μm and was extremely stable. It has a sharp particle size distribution. The external appearance of the platinum powder is as shown in the photograph (10000 times) shown in FIG.
【００１４】[0014]
【図１】FIG.
【００１５】[0015]
【実施例２】白金ブラック２０ｇと炭酸カルシウム８０
ｇとに水を加えて湿式混合した後、乾燥機に入れて１２
０゜Cで乾燥してから遊星ミル内に投入して充分微細にな
るように粉砕した。その後、この粉砕粉を横型管状炉に
入れて、４時間かけて１０００゜Cまで上昇させ、２時間
の間１０００゜Cに維持し、その後４時間かけて冷却し
た。この焼成工程により炭酸ガスが除去され、残りは白
金と酸化カルシウムのみとなる。そこで、焼結粉に３倍
希釈硝酸水溶液を注ぎ炭酸カルシウムを溶解させ、これ
を３回繰り返した後、５回水洗して、酸化カルシウムを
完全に除去した。その後、残留分を乾燥機に入れて１２
０゜Cで乾燥してからメッシュパスして高結晶性白金粉末
を得た。Example 2 20 g of platinum black and 80 of calcium carbonate
g and water, and wet-mixed.
After drying at 0 ° C., it was charged into a planetary mill and pulverized to a sufficiently fine size. Thereafter, the pulverized powder was placed in a horizontal tubular furnace, raised to 1000 ° C over 4 hours, maintained at 1000 ° C for 2 hours, and then cooled over 4 hours. This firing step removes carbon dioxide, leaving only platinum and calcium oxide. Therefore, a three-fold diluted nitric acid aqueous solution was poured into the sintered powder to dissolve calcium carbonate, and this was repeated three times, followed by washing five times with water to completely remove calcium oxide. Thereafter, the residue is put into a dryer and
After drying at 0 ° C., the mixture was passed through a mesh to obtain highly crystalline platinum powder.
【００１６】この実施例によって得られた白金粉末の結
晶度は１１９２３ｃｐｓ、比表面積１．７ｍ2／ｇ、純
度９９．９％、１０％平均粒径０．３４μｍ、５０％平
均粒径０．６０μｍ、９０％平均粒径１．０２μｍ、で
あった。また、得られた高結晶性白金粉末の外観は、図
２に示す写真（１００００倍）の通りである。The platinum powder obtained in this example has a crystallinity of 11,923 cps, a specific surface area of 1.7 m 2 / g, a purity of 99.9%, a 10% average particle size of 0.34 μm, and a 50% average particle size of 0.60 μm. , 90% average particle size 1.02 μm. The appearance of the obtained highly crystalline platinum powder is as shown in the photograph (10000 times) shown in FIG.
【００１７】[0017]
【図２】FIG. 2
【００１１】[0011]
【発明の効果】以上の通りこの発明によれば、アルカリ
塩またはアルカリ土類金属塩から選んだ少なくとも一種
の塩をスペーサとして白金ブラックと湿式混合してから
粉砕し、その後焼結してガスを除去し、塩を溶解除去す
るものであるので、次の様な効果が得られる。 （１）不安定な濃酸溶解処理工程が不要であるので、製
造工程が短縮され、自動化も可能となる。ちなみに、製
造時間は従来の２／３に短縮され、自動化した場合には
従来の約１／３の時間で製造可能となる。 （２）結晶度が高まり、従来の約２倍の結晶度が得られ
る。 （３）粒度分布幅が狭く、安定した粒度の微細白金粉末
を提供できる。 （４）有毒ガスの発生が無く、その対策装置を設ける必
要が無い為、安全且つ経済的に製造出来る。 （５）９９．９％以上の高純度白金粉末を得ることが出
来る。またそれによって、ロス回収作業が不用となる。 （６）アルカリ塩またはアルカリ土類金属塩の混合量の
調節等によって簡単にPt粒子径を調整することが出来
る。As described above, according to the present invention, at least one kind of salt selected from alkali salts or alkaline earth metal salts is wet-mixed with platinum black as a spacer, crushed, and then sintered to form a gas. Since it removes and dissolves and removes salts, the following effects can be obtained. (1) Since an unstable concentrated acid dissolving process is unnecessary, the manufacturing process is shortened and automation becomes possible. By the way, the manufacturing time is reduced to 2/3 of the conventional time, and when it is automated, it can be manufactured in about 1/3 of the conventional time. (2) The degree of crystallinity is increased, and a degree of crystallinity approximately twice as high as that of the related art is obtained. (3) A fine platinum powder having a narrow particle size distribution width and a stable particle size can be provided. (4) Since there is no generation of toxic gas and there is no need to provide a countermeasure device, it can be manufactured safely and economically. (5) High purity platinum powder of 99.9% or more can be obtained. This also makes loss recovery work unnecessary. (6) The Pt particle diameter can be easily adjusted by adjusting the mixing amount of the alkali salt or alkaline earth metal salt.
【図１】この発明による実施例１によって得られた高結
晶性白金粉末の外観写真である。FIG. 1 is an appearance photograph of a highly crystalline platinum powder obtained in Example 1 according to the present invention.
【図２】この発明による実施例２によって得られた高結
晶性白金粉末の外観写真である。FIG. 2 is a photograph showing the appearance of a highly crystalline platinum powder obtained in Example 2 according to the present invention.
Claims (4)
カリ土類金属塩から選んだ少なくとも一種の塩とを湿式
混合して乾燥後粉砕し、その粉砕体を焼成してガスを除
去後希酸によって塩を溶解させて水洗除去し、これを乾
燥してＰｔ粉末を得る高結晶性白金粉末の製造方法。1. Platinum black and at least one salt selected from the group consisting of an alkali salt and an alkaline earth metal salt are wet-mixed, dried and pulverized, and the pulverized product is calcined to remove a gas. Is dissolved in water, washed and removed, and dried to obtain a Pt powder.
混合して乾燥後粉砕し、しかる後にこの粉砕体を焼成し
て炭酸ガスを除去してから残余の酸化カルシウムを希酸
にて溶解させて水洗除去し、これを乾燥して白金粉末を
得る高結晶性白金粉末の製造方法。2. Platinum black and calcium carbonate are wet-mixed, dried and pulverized. Thereafter, the pulverized product is calcined to remove carbon dioxide gas, and the remaining calcium oxide is dissolved in dilute acid and washed with water. A method for producing a highly crystalline platinum powder which is removed and dried to obtain a platinum powder.
ら選んだ少なくとも一種の塩と白金ブラックとの混合比
率は２：１から１６：１の範囲である「請求項１」また
は「請求項２」の高結晶性白金粉末の製造方法。3. The method according to claim 1, wherein the mixing ratio of at least one salt selected from alkali salts or alkaline earth metal salts to platinum black is in the range of 2: 1 to 16: 1. Method for producing highly crystalline platinum powder.
ら選んだ少なくとも一種の塩の白金ブラックへの混合量
によって完成白金粉末の平均粒径を制御する「請求項
１」または「請求項２」の高結晶性白金粉末の製造方
法。4. The average particle size of the finished platinum powder is controlled by the amount of at least one salt selected from alkali salts or alkaline earth metal salts mixed with platinum black. A method for producing highly crystalline platinum powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28016096A JP3946798B2 (en) | 1996-09-30 | 1996-09-30 | Method for producing highly crystalline platinum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28016096A JP3946798B2 (en) | 1996-09-30 | 1996-09-30 | Method for producing highly crystalline platinum powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10102103A true JPH10102103A (en) | 1998-04-21 |
| JP3946798B2 JP3946798B2 (en) | 2007-07-18 |
Family
ID=17621154
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28016096A Expired - Lifetime JP3946798B2 (en) | 1996-09-30 | 1996-09-30 | Method for producing highly crystalline platinum powder |
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| Country | Link |
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| JP (1) | JP3946798B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011038165A (en) * | 2009-08-13 | 2011-02-24 | Sumitomo Metal Mining Co Ltd | Method for recovering high quality rhodium powder |
| EP3351324A4 (en) * | 2015-09-18 | 2018-10-24 | Tanaka Kikinzoku Kogyo K.K. | Precious metal powder production method |
| CN117483777A (en) * | 2023-11-02 | 2024-02-02 | 重庆材料研究院有限公司 | Preparation method of micron-sized spherical platinum powder with high tap density |
-
1996
- 1996-09-30 JP JP28016096A patent/JP3946798B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011038165A (en) * | 2009-08-13 | 2011-02-24 | Sumitomo Metal Mining Co Ltd | Method for recovering high quality rhodium powder |
| EP3351324A4 (en) * | 2015-09-18 | 2018-10-24 | Tanaka Kikinzoku Kogyo K.K. | Precious metal powder production method |
| US10569334B2 (en) | 2015-09-18 | 2020-02-25 | Tanaka Kikinzoku Kogyo K.K. | Process for producing noble-metal powder |
| CN117483777A (en) * | 2023-11-02 | 2024-02-02 | 重庆材料研究院有限公司 | Preparation method of micron-sized spherical platinum powder with high tap density |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3946798B2 (en) | 2007-07-18 |
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