JPH08311510A - Production of copper-tungsten mixed powder - Google Patents
Production of copper-tungsten mixed powderInfo
- Publication number
- JPH08311510A JPH08311510A JP7141308A JP14130895A JPH08311510A JP H08311510 A JPH08311510 A JP H08311510A JP 7141308 A JP7141308 A JP 7141308A JP 14130895 A JP14130895 A JP 14130895A JP H08311510 A JPH08311510 A JP H08311510A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- soln
- mixed powder
- mixed
- cobalt
- 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
【０００１】[0001]
【産業上の利用分野】本発明は、新規なＣｕ−Ｗ（銅−
タングステン）混合粉末の製造法に関するものである。The present invention relates to a novel Cu-W (copper-
(Tungsten) mixed powder manufacturing method.
【０００２】[0002]
【従来の技術】電気接点や、半導体のヒートシンク部材
として、従来からＣｕ−Ｗ（銅−タングステン）複合材
が使用されている。Ｃｕ−Ｗ複合材は、多孔質のタング
ステン焼結体に溶融した銅を含浸させて製造する溶浸法
や、Ｃｕ粉末とＷ粉末との混合物を加圧成型して焼結す
る混合焼結法によって製造されている。2. Description of the Related Art Conventionally, Cu-W (copper-tungsten) composite materials have been used as electrical contacts and semiconductor heat sink members. The Cu-W composite material is an infiltration method produced by impregnating molten tungsten into a porous tungsten sintered body, or a mixed sintering method in which a mixture of Cu powder and W powder is pressure-molded and sintered. Is manufactured by.
【０００３】しかしながら、上記溶浸法による製造方法
は、銅を含浸したブロックにおいて部分的な銅の含有率
のばらつきが多く、銅含浸ブロックはさらに研磨成形す
る工程が必要であり、工程数が多い上に材料の無駄が多
く歩留まりが悪いなどの課題を抱えている。一方、Ｃｕ
粉末とＷ粉末との混合物を加圧・焼結して製造する混合
焼結法は、Ｃｕ粉末とＷ粉末の比重の差が大きいため、
両者を均一に混合するのが難しく、偏析等が生じ易いと
いう問題点があった。また、機械的に混合するため、混
合時に銅粉末が押し潰されて扁平化し、燒結体中に銅の
プ−ルができる原因となっていた。さらに、上記混合中
に不純物が混入し易いという問題点もあった。However, in the manufacturing method by the above-mentioned infiltration method, there are many variations in the copper content rate in the block impregnated with copper, and the copper-impregnated block requires a step of further polishing and shaping, and the number of steps is large. In addition, there are many problems such as waste of material and poor yield. On the other hand, Cu
In the mixed sintering method in which a mixture of powder and W powder is pressed and sintered, the difference in specific gravity between Cu powder and W powder is large.
There is a problem that it is difficult to mix both uniformly and segregation easily occurs. In addition, since they are mechanically mixed, the copper powder is crushed and flattened during the mixing, which causes a pool of copper in the sintered body. Further, there is a problem that impurities are easily mixed during the above mixing.
【０００４】[0004]
【発明が解決しようとする課題】本発明の目的は、上記
の焼結法によってＣｕ−Ｗ複合材を製造する場合に、原
料として使用できる好ましいＣｕ−Ｗ混合粉末、すなわ
ちＣｕの割合が１０〜３０重量％程度で、均質かつ純度
の高いＣｕ−Ｗ混合粉末の製造法を提供することにあ
る。The object of the present invention is to provide a preferable Cu-W mixed powder which can be used as a raw material when the Cu-W composite material is produced by the above-mentioned sintering method, that is, the ratio of Cu is 10 to 10. An object of the present invention is to provide a method for producing a Cu—W mixed powder having a uniform and high purity of about 30% by weight.
【０００５】[0005]
【課題を解決するための手段】上記目的を達成するた
め、本発明は以下のような構成とした。すなわち、本発
明の銅−タングステン混合粉末の製造法は、銅もしくは
銅化合物と、タングステン酸ソ−ダと、コバルトもしく
はコバルト化合物および／またはニッケルもしくはニッ
ケル化合物とを含む溶液にアンモニア水を加え、ｐＨ４
〜７に調整して沈殿物を得たのち、得られた沈殿物を大
気中で焙焼し、さらに水素還元して、少量のコバルトも
しくはニッケルを含有する銅−タングステン混合粉末を
得ることを特徴としている。In order to achieve the above object, the present invention has the following constitution. That is, the method for producing a copper-tungsten mixed powder according to the present invention comprises adding ammonia water to a solution containing copper or a copper compound, soda tungstate, cobalt or a cobalt compound and / or nickel or a nickel compound, and adjusting the pH to 4
After adjusting to ~ 7 to obtain a precipitate, the obtained precipitate is roasted in the air and further hydrogen reduced to obtain a copper-tungsten mixed powder containing a small amount of cobalt or nickel. I am trying.
【０００６】以下、具体例を示す図１の工程図に基づい
て、詳細に説明する。本発明で使用される原料のうちタ
ングステン源として好適に使用されるものは、酸化タン
グステン、パラタングステン酸アンモニウム、タングス
テン酸ソ−ダ等であり、また、銅源として好適に使用さ
れるものは、酸化銅、硝酸銅、塩化銅、硫酸銅等の含銅
化合物である。なお、場合によっては金属銅を使用する
こともできる。Detailed description will be given below with reference to the process chart of FIG. 1 showing a specific example. Of the raw materials used in the present invention, those preferably used as a tungsten source are tungsten oxide, ammonium paratungstate, soda tungstate, etc., and those preferably used as a copper source are Copper-containing compounds such as copper oxide, copper nitrate, copper chloride, and copper sulfate. In addition, metallic copper can also be used depending on the case.
【０００７】さらに、ニッケル源として好ましいもの
は、酸化ニッケル、硝酸ニッケル、塩化ニッケル、硫酸
ニッケル等の含ニッケル化合物であり、コバルト源とし
て好ましいものは、酸化コバルト、硝酸コバルト、塩化
コバルト、硫酸コバルト等の含コバルト化合物である。
なお、上記化合物の代わりに、金属ニッケル、金属コバ
ルト等を使用することもできる。Further, preferable nickel sources are nickel-containing compounds such as nickel oxide, nickel nitrate, nickel chloride and nickel sulfate, and preferable cobalt sources are cobalt oxide, cobalt nitrate, cobalt chloride, cobalt sulfate and the like. Is a cobalt-containing compound.
Note that metal nickel, metal cobalt, or the like can be used instead of the above compound.
【０００８】これらの原料を、目的とする製品の組成が
得られる配合比で混合する。製品中に含まれる各金属の
量は、重量比で銅（Ｃｕ）が８〜１３％、コバルト（Ｃ
ｏ）が０〜３％、ニッケル（Ｎｉ）が０〜３％、タング
ステン（Ｗ）が８０〜９２％とするのが好ましい。上記
原料の混合方法としては、例えば、原料が硫酸銅、硫酸
コバルト、硫酸ニッケル等の水溶性化合物の場合は、水
を加えて順に溶解すればよい。この水溶液にタングステ
ン源であるパラタングステン酸アンモニウムを加えて、
スラリ−状で混合する。[0008] These raw materials are mixed in a compounding ratio so as to obtain a desired product composition. The amount of each metal contained in the product is 8 to 13% by weight of copper (Cu) and cobalt (C).
It is preferable that 0) is 0 to 3%, nickel (Ni) is 0 to 3%, and tungsten (W) is 80 to 92%. As a method for mixing the above-mentioned raw materials, for example, when the raw material is a water-soluble compound such as copper sulfate, cobalt sulfate, and nickel sulfate, water may be added and dissolved in order. Ammonium paratungstate, which is a tungsten source, is added to this aqueous solution,
Mix in slurry form.
【０００９】十分に混合したら、これに例えばアンモニ
ア水（ＮＨ4 ＯＨ）を加えてｐＨ調整を行う。好ましい
ｐＨ値は４〜７であり、５．５前後とするのが最も好ま
しい。これにより、タングステン、銅、コバルト（ニッ
ケル）等が水酸化物として沈殿する。After being sufficiently mixed, for example, aqueous ammonia (NH 4 OH) is added to adjust the pH. The preferable pH value is 4 to 7, and the most preferable pH value is around 5.5. As a result, tungsten, copper, cobalt (nickel), etc. are precipitated as hydroxides.
【００１０】ｐＨ調整を終えた混合スラリ−は、６０〜
９０℃程度（８０℃前後が最も好ましい）に加温し、攪
拌する。撹拌時間は１時間程度とするのが好ましい。こ
れらの条件は、他の条件に応じて適宜選択すればよい。The mixed slurry after the pH adjustment is 60-
Warm to about 90 ° C (most preferably around 80 ° C) and stir. The stirring time is preferably about 1 hour. These conditions may be appropriately selected according to other conditions.
【００１１】上記加温攪拌が終わったら、攪拌を停止し
て放置し、熟成させる。しかるのち、上澄み液を捨てて
洗浄を行う。この洗浄は、例えば硝酸アンモニウム（Ｎ
Ｈ4ＮＯ3 ）溶液を用いて行ない、洗浄後は廃液する。
この洗浄を適当回数（通常は２回でよい）繰り返し、得
られたスラリ−を遠心分離機、フィルタ−プレス等を用
いてろ過する。この場合のろ液は捨て、残りの混合水酸
化物を取り出して乾燥する。After completion of the heating and stirring, the stirring is stopped and the mixture is allowed to stand for aging. Then, discard the supernatant and wash. This cleaning is performed, for example, with ammonium nitrate (N
H 4 NO 3 ) solution and drain after washing.
This washing is repeated an appropriate number of times (usually twice), and the obtained slurry is filtered using a centrifuge, a filter press or the like. The filtrate in this case is discarded, and the remaining mixed hydroxide is taken out and dried.
【００１２】乾燥後の混合水酸化物は、ロータリキルン
等を用いて焙焼し、混合酸化物粉末とする。この場合の
焙焼温度は５００〜６００℃程度、時間は４〜６時間程
度が好ましい。The dried mixed hydroxide is roasted using a rotary kiln or the like to obtain mixed oxide powder. In this case, the roasting temperature is preferably about 500 to 600 ° C., and the time is preferably about 4 to 6 hours.
【００１３】上記焙焼によって得られた酸化物混合粉末
は、最後に水素ガス雰囲気下の電気炉内にて加熱還元す
る。これにより、少量のコバルトおよび／またはニッケ
ルを含むＣｕ−Ｗ混合粉末が得られる。この場合の加熱
還元条件は８５０〜１０００℃、１．５〜３時間程度で
ある。以下、本発明の実施例について、より具体的に説
明する。The oxide mixed powder obtained by the above roasting is finally reduced by heating in an electric furnace under a hydrogen gas atmosphere. Thereby, a Cu-W mixed powder containing a small amount of cobalt and / or nickel is obtained. The heat reduction conditions in this case are 850 to 1000 ° C. and about 1.5 to 3 hours. Hereinafter, examples of the present invention will be described more specifically.
【００１４】[0014]
【実施例】表１に示した原料を用いて、図１に示す工程
で混合粉末を製造した。使用した原料は、硫酸銅１６８
ｇ、硫酸コバルト（または硫酸ニッケル）３．９ｇ、タ
ングステン酸アンモニウム４９３ｇであり、最初に硫酸
銅と硫酸コバルトを水に溶解した。この溶液にパラタン
グステン酸アンモニウムを加え、混合したのち、アンモ
ニア水を加えてｐＨ値を５．５に調整した。[Examples] Using the raw materials shown in Table 1, mixed powders were produced in the steps shown in FIG. The raw material used is copper sulfate 168.
g, cobalt sulfate (or nickel sulfate) 3.9 g, and ammonium tungstate 493 g. First, copper sulfate and cobalt sulfate were dissolved in water. Ammonium paratungstate was added to this solution and mixed, and then aqueous ammonia was added to adjust the pH value to 5.5.
【００１５】[0015]
【表１】 [Table 1]
【００１６】次に、このスラリ−を８０℃に加温し、１
時間攪拌したのち、攪拌を止めて放置熟成した。これに
より、沈殿物と液が分離したので、その液を捨て、硝酸
アンモニウム溶液を加えて第１回の洗浄を行った。洗浄
後は廃液したのち、スラリ−に再度硝酸アンモニウム溶
液を加えて第２回目の洗浄を行ない、上記と同様に廃液
した。Next, this slurry was heated to 80 ° C.,
After stirring for an hour, the stirring was stopped and the mixture was left to mature. As a result, the precipitate and the liquid were separated, and the liquid was discarded, an ammonium nitrate solution was added, and the first washing was performed. After the washing, the liquid was drained, the ammonium nitrate solution was added to the slurry again to carry out the second washing, and the liquid was drained in the same manner as above.
【００１７】第２回目の洗浄を終えたスラリ−は、フィ
ルタ−プレスを用いてろ過し、ろ液は捨て、残りの混合
水酸化物を取り出した。この混合水酸化物は、乾燥した
のち、大気中で５５０℃で５時間焙焼した。これにより
均一な混合酸化物粉末が得られた。The slurry that had been washed for the second time was filtered using a filter press, the filtrate was discarded, and the remaining mixed hydroxide was taken out. This mixed hydroxide was dried and then roasted in the air at 550 ° C. for 5 hours. As a result, a uniform mixed oxide powder was obtained.
【００１８】この混合酸化物粉末は、電気炉を用いて、
水素気流中で還元した。還元温度は９５０℃、還元時間
は２時間であった。この還元により、銅とコバルト（ま
たはニッケル）とタングステンとが均一に混ざった金属
混合粉末が得られた。得られたＣｕ−Ｃｏ−Ｗ混合粉末
の組成は表２に示す通りであり、これらの金属粉末がき
わめて均一に分散していることが確認された。This mixed oxide powder was prepared using an electric furnace.
It was reduced in a stream of hydrogen. The reduction temperature was 950 ° C. and the reduction time was 2 hours. By this reduction, a metal mixed powder in which copper, cobalt (or nickel), and tungsten were uniformly mixed was obtained. The composition of the obtained Cu-Co-W mixed powder is as shown in Table 2, and it was confirmed that these metal powders were extremely uniformly dispersed.
【００１９】[0019]
【表２】 [Table 2]
【００２０】[0020]
【発明の効果】以上の説明の如く、本発明に係るＣｕ−
Ｗ混合粉末の製造法によれば、焼結法によってＣｕ−Ｗ
複合材を製造する場合に原料として使用できる、Ｃｕの
割合が１０〜３０重量％の純度の高い均一なＣｕ−Ｗ混
合粉末を、能率よく製造することができる。As described above, the Cu-
According to the method for producing the W mixed powder, Cu-W is produced by the sintering method.
A highly pure and uniform Cu—W mixed powder having a Cu content of 10 to 30% by weight, which can be used as a raw material when manufacturing a composite material, can be efficiently manufactured.
【図１】本発明の具体例を示す工程図である。FIG. 1 is a process drawing showing a specific example of the present invention.
Claims (1)
ソ−ダと、コバルトもしくはコバルト化合物および／ま
たはニッケルもしくはニッケル化合物とを含む溶液にア
ンモニア水を加え、ｐＨ４〜７に調整して沈殿物を得た
のち、得られた沈殿物を大気中で焙焼し、さらに水素還
元して、少量のコバルトもしくはニッケルを含有する銅
−タングステン混合粉末を得ることを特徴とする銅−タ
ングステン混合粉末の製造法。1. Ammonia water is added to a solution containing copper or a copper compound, soda tungstate, cobalt or a cobalt compound and / or nickel or a nickel compound, and the pH is adjusted to 4 to 7 to obtain a precipitate. After that, the obtained precipitate is roasted in the air and further hydrogen-reduced to obtain a copper-tungsten mixed powder containing a small amount of cobalt or nickel, and a method for producing a copper-tungsten mixed powder. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7141308A JPH08311510A (en) | 1995-05-15 | 1995-05-15 | Production of copper-tungsten mixed powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7141308A JPH08311510A (en) | 1995-05-15 | 1995-05-15 | Production of copper-tungsten mixed powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08311510A true JPH08311510A (en) | 1996-11-26 |
Family
ID=15288878
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7141308A Pending JPH08311510A (en) | 1995-05-15 | 1995-05-15 | Production of copper-tungsten mixed powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08311510A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402204C (en) * | 2003-01-21 | 2008-07-16 | 奥斯兰姆施尔凡尼亚公司 | Electrochemical displacement-deposition method for making composite metal powders |
| CN100446899C (en) * | 2005-04-14 | 2008-12-31 | 中南大学 | Prepn process of superfine W-Cu composite powder |
| CN102350508A (en) * | 2011-10-13 | 2012-02-15 | 北京科技大学 | Method for preparing doped-tungsten-based composite powder |
| CN102485380A (en) * | 2010-12-06 | 2012-06-06 | 北京有色金属研究总院 | Preparation method of submicron nearly spherical tungsten powder |
| CN103128310A (en) * | 2011-11-29 | 2013-06-05 | 中国科学院合肥物质科学研究院 | Wolfram-copper composite powder preparation method |
| CN103862058A (en) * | 2012-12-14 | 2014-06-18 | 重庆华浩冶炼有限公司 | Method for producing copper lead powder |
| CN112708794A (en) * | 2021-03-29 | 2021-04-27 | 陕西斯瑞新材料股份有限公司 | Method for preparing copper-tungsten alloy by adopting superfine tungsten powder |
| CN114833348A (en) * | 2022-05-07 | 2022-08-02 | 合肥工业大学 | Large-scale preparation method of controllable high-quality W-Cu composite powder |
-
1995
- 1995-05-15 JP JP7141308A patent/JPH08311510A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402204C (en) * | 2003-01-21 | 2008-07-16 | 奥斯兰姆施尔凡尼亚公司 | Electrochemical displacement-deposition method for making composite metal powders |
| CN100446899C (en) * | 2005-04-14 | 2008-12-31 | 中南大学 | Prepn process of superfine W-Cu composite powder |
| CN102485380A (en) * | 2010-12-06 | 2012-06-06 | 北京有色金属研究总院 | Preparation method of submicron nearly spherical tungsten powder |
| CN102350508A (en) * | 2011-10-13 | 2012-02-15 | 北京科技大学 | Method for preparing doped-tungsten-based composite powder |
| CN103128310A (en) * | 2011-11-29 | 2013-06-05 | 中国科学院合肥物质科学研究院 | Wolfram-copper composite powder preparation method |
| CN103862058A (en) * | 2012-12-14 | 2014-06-18 | 重庆华浩冶炼有限公司 | Method for producing copper lead powder |
| CN112708794A (en) * | 2021-03-29 | 2021-04-27 | 陕西斯瑞新材料股份有限公司 | Method for preparing copper-tungsten alloy by adopting superfine tungsten powder |
| CN114833348A (en) * | 2022-05-07 | 2022-08-02 | 合肥工业大学 | Large-scale preparation method of controllable high-quality W-Cu composite powder |
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