JPS6169904A - Production of pulverous tungsten oxide powder - Google Patents
Production of pulverous tungsten oxide powderInfo
- Publication number
- JPS6169904A JPS6169904A JP19326984A JP19326984A JPS6169904A JP S6169904 A JPS6169904 A JP S6169904A JP 19326984 A JP19326984 A JP 19326984A JP 19326984 A JP19326984 A JP 19326984A JP S6169904 A JPS6169904 A JP S6169904A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- tungsten
- tungsten oxide
- oxide powder
- powder
- 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
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は０．２μｍ以下の酸化タングステン微粉末の製
造法に関する。これら微粉末は、例えば酸化タングステ
ン焼結体製造用の原料とじて用いられ、焼結密度の向上
に効果がある。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing fine tungsten oxide powder of 0.2 μm or less. These fine powders are used, for example, as raw materials for producing tungsten oxide sintered bodies, and are effective in improving sintered density.
通常酸化タングステンはパラタングステン酸アンモニウ
ムあるいはタングステン酸を空気中で加熱分ｍすること
により得られる。タングステン酸を加熱分解する場合に
は比較的微細な酸化タングステンが得られ易い。しかし
これら方法においても０．２μｍ程度が限度で、それ以
下の微粉末の製造は困難であった。（以下、粒度は電子
顕微Ｊ［察による粒度を指す。）〔発明が解決しようと
する問題点〕
本発明は、これら従来製造困難であった０゜２μｍ以下
の酸化タングステン微粉末の製造方法を提供しようとす
るものである。Tungsten oxide is usually obtained by heating ammonium paratungstate or tungstic acid in air. When tungstic acid is thermally decomposed, relatively fine tungsten oxide is easily obtained. However, even in these methods, the particle size is limited to about 0.2 μm, and it is difficult to produce fine powder smaller than that. (Hereinafter, the particle size refers to the particle size observed by electron microscopy.) [Problems to be solved by the invention] The present invention solves a method for producing fine tungsten oxide powder of 0.2 μm or less, which has been difficult to produce in the past. This is what we are trying to provide.
本発明は各種タングステン複合酸化物の分解過程を種々
検討の結果完成されたもので、本発明の特徴とするとこ
ろは、タングステンと銅の複合酸化物粉末を水素雰囲気
中で加熱分解して銅を全屈まで還元し、次いで酸処理を
して銅を溶解除去することにあり、さらには、銅を溶解
除去して得られるタングステン低級酸化物を空気中で焙
焼することにある。The present invention was completed as a result of various studies on the decomposition process of various tungsten composite oxides.The feature of the present invention is that copper is produced by thermally decomposing tungsten and copper composite oxide powder in a hydrogen atmosphere. The purpose is to reduce the tungsten to full strength, and then perform acid treatment to dissolve and remove the copper.Furthermore, the tungsten lower oxide obtained by dissolving and removing the copper is roasted in air.
従来酸化タングステン微粉末の製造が困難であった原因
の１つは、パラタングステン酸アンモニウム或いはタン
グステン酸の加熱分薄に際し、分解により世塵内に発生
した酸化タングステンの微粒子が、分解の進行に伴ない
世塵内の隣接する粒子同士が互いにくいあって成長して
いくためと考えられる。One of the reasons why it has been difficult to produce fine tungsten oxide powder in the past is that when ammonium paratungstate or tungstic acid is heated and thinned, the fine particles of tungsten oxide that are generated in the dust due to decomposition are released as the decomposition progresses. This is thought to be due to the fact that adjacent particles in the free world grow by clinging to each other.
本発明はタングステン化合物の分解に際し。The present invention is applicable to the decomposition of tungsten compounds.
世塵内部で酸化タングステン粒子同士が隣接するのをで
きるだけ防ぎ、粒子の成長を押えようという主旨のもと
に成されたものである。本発明者等はタングステン複合
酸化物の分解時の挙動を種々検討した結果、銅−タング
ステン複合酸化物を水素中で分解する場合には銅が優先
的に還元され、タングステンの低級酸化物が金属鋼中に
分散すること、又分解後の複合粉末を酸で処理する場合
には飛が７８解除去され酸化タングステン微粉末が遊歴
することを見出し本発明を完成するに到った。This was done with the aim of preventing tungsten oxide particles from adjoining each other inside the dust as much as possible and suppressing the growth of the particles. As a result of various studies on the behavior of tungsten composite oxides during decomposition, the present inventors found that when copper-tungsten composite oxides are decomposed in hydrogen, copper is preferentially reduced, and lower tungsten oxides are reduced to metals. We have completed the present invention by discovering that tungsten oxide is dispersed in steel, and that when the composite powder after decomposition is treated with acid, 78 particles are removed and fine tungsten oxide powder floats around.
銅−タングステン粉末は、タングステン酸塩の水溶液に
銅塩の水溶液を添加することにより容易に得られる。こ
れら湿式法により得られた粉末は一般に微細で無定形で
あることが多い。Copper-tungsten powder is easily obtained by adding an aqueous solution of a copper salt to an aqueous solution of a tungstate. Powders obtained by these wet methods are generally fine and often amorphous.
銅−タングステン複合酸化物粉末を空気中で加熱する時
は複合酸化物は分解せずＣｕＷＯ４なる構造を保持する
が、銅−タングステン複合酸化物粉末を水素雰囲気中で
加熱する時は分解して銅は金属鋼まで還元される。還元
温度は一般の銅酸化物の還元温度２５０℃〜３００℃以
上であれば良い。本発明の方法においては特に還元条件
を規定するものではないが、少なくとも銅が金属まで還
元されることが必要である。When copper-tungsten composite oxide powder is heated in air, the composite oxide does not decompose and maintains the structure of CuWO4, but when copper-tungsten composite oxide powder is heated in a hydrogen atmosphere, it decomposes and becomes copper. is reduced to metallic steel. The reduction temperature may be at least 250°C to 300°C, which is the reduction temperature of common copper oxides. Although the method of the present invention does not particularly specify reduction conditions, it is necessary that at least copper be reduced to metal.
タングステンは低級酸化物となり鋼中に微細に分散する
。Tungsten becomes a lower oxide and is finely dispersed in steel.
得られた複合粉末を酸で処理すると銅は容易
）に溶解して酸化タングステン微粉末が残留する。When the obtained composite powder is treated with acid, copper is easily removed.
), leaving fine tungsten oxide powder.
一般にタングステンは低級酸化物となっているため、必
要に応じ空気中で焙焼してＷＯｌとする。Since tungsten is generally a lower oxide, it is roasted in air to form WOl if necessary.
得られた粉末は微細で粒径０．１μｍ以下の微粒子より
成る。これは分解に際し鋼が酸化タングステン粒子同士
の接触を防げ、粒子の成長を押えるためと考えられる。The obtained powder consists of fine particles with a particle size of 0.1 μm or less. This is thought to be because the steel prevents tungsten oxide particles from coming into contact with each other during decomposition, suppressing particle growth.
以下実施例に従い本発明の方法を詳細に説明する。The method of the present invention will be described in detail below with reference to Examples.
実施例Ｉ
Ｗ ０３ａ度約１５Ｗ／Ｖ％のタングステン酸アンモニ
ウム水溶液に硝酸調水溶液を重量比でＷＯ３：Ｃｕが１
０ ： ２．７になるよう添加した。Example I W 03a A nitric acid aqueous solution was added to an ammonium tungstate aqueous solution of about 15 W/V% at a weight ratio of WO3:Cu of 1.
It was added so that the ratio was 0:2.7.
生成物を水洗・乾燥して銅−タングステン複合酸化物粉
末を得た。Ｘ線回折の結果生成物は無定形であったが、
粉末を空気巾約６００℃で焙焼したものはＣｕ Ｗ Ｏ
４のピークが観察された。The product was washed with water and dried to obtain a copper-tungsten composite oxide powder. As a result of X-ray diffraction, the product was amorphous, but
The powder roasted at an air width of about 600℃ is CuWO.
4 peaks were observed.
乾燥後の複合酸化物粉末を水素雰囲気中３゜Ｏ℃〜４０
０’Ｃで１．５時間加熱して分解した。After drying, the composite oxide powder was heated in a hydrogen atmosphere at 3°O°C to 40°C.
Decomposition was achieved by heating at 0'C for 1.5 hours.
生成物は金Ｒ銅の色を持った微粉末である。The product is a fine powder with a gold/copper color.
次に生成物を希硝酸中で約１時間煮沸して銅を溶解し、
さらに水洗ならびにアルコールで洗い、最後に空気中で
乾燥して酸化タングステン微粉末を得た。粉末は青白色
で第３図はそのＸ線回折図形を示したものである。第１
図は得られた粉末の電子顕微鏡写真を示したものである
が、粉末は０．１μｍ以下の微粒子から成るのが解る。The product is then boiled in dilute nitric acid for about an hour to dissolve the copper,
Further, it was washed with water and alcohol, and finally dried in air to obtain a fine tungsten oxide powder. The powder was blue-white in color, and Figure 3 shows its X-ray diffraction pattern. 1st
The figure shows an electron micrograph of the obtained powder, and it can be seen that the powder consists of fine particles of 0.1 μm or less.
尚酸処理後の粉末中の残留銅はＣｕとして０．１３％で
あった。The residual copper in the powder after the acid treatment was 0.13% as Cu.
〔実施例２〕
実施例１で得た酸化タングステン微粉末を空気中５００
℃で約１時間焙焼して黄白色の酸化タングステン微粉末
を得た。第４図は生成物のＸ線回折図形を示したもので
ＷＯ３のピークが１ｖ５される。第２図は得られた粉末
の電子顕微鏡写真であるが、粉末は０．１μｍ以下の微
粒子から成っているのが解る。[Example 2] The fine tungsten oxide powder obtained in Example 1 was exposed to
The mixture was roasted at ℃ for about 1 hour to obtain yellowish white fine tungsten oxide powder. FIG. 4 shows the X-ray diffraction pattern of the product, in which the peak of WO3 is 1v5. FIG. 2 is an electron micrograph of the obtained powder, and it can be seen that the powder consists of fine particles of 0.1 μm or less.
以上述べてきたように１本発明の方法によれば、従来製
造困難であった０、２μｍ以下の酸化タングステン微粉
末を容易に製造できる。本発明の方法によれば工業的規
模での酸化タングステン微粉末の製造が可能でその利用
価値は大きい。As described above, according to the method of the present invention, it is possible to easily produce fine tungsten oxide powder of 0.2 μm or less, which has been difficult to produce in the past. According to the method of the present invention, fine tungsten oxide powder can be produced on an industrial scale, and its utility value is great.
第１図ならびに第２図は本発明の方法で作られた酸化タ
ングステン微粉末の電子顕微鏡写真を示したもので、又
第３図ならびに第４図は本発明の方法で作られた酸化タ
ングステン微粉末のＸ線回折図形を示したものである。Figures 1 and 2 show electron micrographs of fine tungsten oxide powder produced by the method of the present invention, and Figures 3 and 4 show fine tungsten oxide powder produced by the method of the present invention. This shows the X-ray diffraction pattern of the powder.
Claims (1)
で加熱して銅を金属まで還元し、次いで酸処理をして銅
を溶解除去することを特徴とする酸化タングステン微粉
末の製造法。 ２、タングステンと銅の複合酸化物粉末を水素雰囲気中
で加熱して銅を金属まで還元し、次いで酸処理をして銅
を溶解除去し、得られたタングステン低級酸化物を空気
中で焙焼することを特徴とする酸化タングス微粉末の製
造法。[Claims] 1. A tungsten oxide microorganism characterized in that a composite oxide powder of tungsten and copper is heated in a hydrogen atmosphere to reduce the copper to metal, and then treated with an acid to dissolve and remove the copper. Powder manufacturing method. 2. Heat the tungsten and copper composite oxide powder in a hydrogen atmosphere to reduce the copper to metal, then perform acid treatment to dissolve and remove the copper, and roast the resulting tungsten lower oxide in air. A method for producing fine tung oxide powder, characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19326984A JPS6169904A (en) | 1984-09-14 | 1984-09-14 | Production of pulverous tungsten oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19326984A JPS6169904A (en) | 1984-09-14 | 1984-09-14 | Production of pulverous tungsten oxide powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6169904A true JPS6169904A (en) | 1986-04-10 |
Family
ID=16305126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19326984A Pending JPS6169904A (en) | 1984-09-14 | 1984-09-14 | Production of pulverous tungsten oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6169904A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6914032B2 (en) * | 2001-12-27 | 2005-07-05 | Korea Institute Of Machinery And Materials | Method of producing tungsten-copper based composite powder and sintered alloys for heat-sink using said composite powder |
| CN103945964A (en) * | 2011-11-15 | 2014-07-23 | 昭和电工株式会社 | Method for producing fine tungsten powder |
-
1984
- 1984-09-14 JP JP19326984A patent/JPS6169904A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6914032B2 (en) * | 2001-12-27 | 2005-07-05 | Korea Institute Of Machinery And Materials | Method of producing tungsten-copper based composite powder and sintered alloys for heat-sink using said composite powder |
| CN103945964A (en) * | 2011-11-15 | 2014-07-23 | 昭和电工株式会社 | Method for producing fine tungsten powder |
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