JPS59162206A - Manufacture of fine nickel and cobalt powder - Google Patents
Manufacture of fine nickel and cobalt powderInfo
- Publication number
- JPS59162206A JPS59162206A JP3655883A JP3655883A JPS59162206A JP S59162206 A JPS59162206 A JP S59162206A JP 3655883 A JP3655883 A JP 3655883A JP 3655883 A JP3655883 A JP 3655883A JP S59162206 A JPS59162206 A JP S59162206A
- Authority
- JP
- Japan
- Prior art keywords
- nickel
- cobalt
- powder
- fine
- hydrazine
- 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.)
- Granted
Links
Abstract
Description
【発明の詳細な説明】
本発明は湿式法によるニッケル及びコバルト微粉末の製
造方法に係り、詳しくは粒度分布幅が小さく均一で、非
凝集性のニッケル及びコバルトの金属微粉末の製造方法
に関する
近時ニッケル及びコバルトの金属微粉末は粉末冶金分野
だけでな（、電子工業分野において、へ銀、パラジウム
等の貴金属に替って、例えば電子部品用ペースト材料等
として実用化されつつある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fine nickel and cobalt powder by a wet process, and more specifically, a method for producing fine nickel and cobalt metal powder that has a small and uniform particle size distribution and is non-agglomerative. Fine metal powders of nickel and cobalt are being put into practical use not only in the field of powder metallurgy (but also in the electronics industry), for example, as paste materials for electronic parts, instead of precious metals such as silver and palladium.
ニッケル及びコバル（）微粉を得る従来の製造方法とし
ては、
（１） ニッケル又はコバルトのカーボニル塩を熱分
解する方法
（２）ニッケル又はコバルトの酸化物あるいは塩を融点
以下の温度で水素または炭素で還元する方法
（３）真空あるいは不活性ガス中でニッケルメタルを蒸
発凝縮せしめるガス中蒸発法
等が広く知られている。Conventional manufacturing methods for obtaining fine powder of nickel and cobalt include (1) thermal decomposition of carbonyl salts of nickel or cobalt; (2) oxidation of nickel or cobalt oxides or salts with hydrogen or carbon at a temperature below the melting point; Method of Reduction (3) The evaporation method in gas, in which nickel metal is evaporated and condensed in vacuum or inert gas, is widely known.
（１）の方法は広く工業的に実施されている方法である
が、得られるニッケル粉末は粒径０．５〜１０μｍと粒
度分布幅が広く粒子形状も一定しないものであり、さら
に電子工業分野で必要とする粒径の小さい粒度分布幅の
小さいものとするには、粉砕、篩分けを必要とし、製品
の収率も悪い。Method (1) is a method that is widely practiced industrially, but the resulting nickel powder has a wide particle size distribution of 0.5 to 10 μm, and the particle shape is not uniform. In order to obtain the required small particle size and narrow particle size distribution width, crushing and sieving are required, and the yield of the product is also poor.
また（２）の方法は酸化物あるいは塩等の化合物の粒度
、粒子形態の影響が顕著であること及び高温で反応させ
るため粒子の焼結が生じ易い等の欠点がある。更に（３
）の方法は温度、雰囲気の圧力などにより蒸発速度が支
配され、金属微粉末の製造能力は極めて低く、大量の金
属微粉末を連続して製造しにくい欠点を有する。In addition, method (2) has drawbacks such as the significant influence of the particle size and particle morphology of compounds such as oxides or salts, and the fact that the reaction is carried out at high temperatures, which tends to cause sintering of the particles. Furthermore (3
The method (2) has the drawback that the evaporation rate is controlled by temperature, atmospheric pressure, etc., and the production capacity of fine metal powder is extremely low, making it difficult to continuously produce a large amount of fine metal powder.
また、従来実施されていた電気化学的還元法及び化学的
還元法等の湿式法で得られる粉末番１、その粒度分布が
０．５〜２００μｍのどとく粒径が広い範囲に分布する
と同時に粒子形状も一定しな℃・ものであり、さらに粉
砕、篩分けを必要とする。In addition, powder No. 1 obtained by conventional wet methods such as electrochemical reduction method and chemical reduction method has a particle size distribution of 0.5 to 200 μm, a wide range of particle size, and a particle shape. Also, the temperature is not constant and requires further crushing and sieving.
また、化学的還元法では、燐（Ｐ）、ホウ素（Ｂ）等の
不純物を数％〜１０数％含有し、その製品収率も低かっ
た。Further, in the chemical reduction method, impurities such as phosphorus (P) and boron (B) were contained in a range of several percent to ten-odd percent, and the product yield was low.
これら湿式法で得られる微粉末は一般に粒径力；小さく
なるほど通常の沖過法では回収が困難であると言った処
理上多くの問題点を有して℃・た。The fine powders obtained by these wet methods generally have many problems in processing, such as the smaller the particle size, the more difficult it is to recover by the normal filtration method.
本発明は、これら従来法の欠点を解消すべくなされたも
ので、その目的は湿式法によりかつ簡便な設備で容易に
直径２μｍ以下に自由に粒度をコントロールし、粒度分
布幅が小さく、均一で、非凝集性の高純度のニッケル及
びコ／くルト金属微粉末を大量に高収率で製造する方法
を提供することにある。The present invention was made to eliminate these drawbacks of conventional methods, and its purpose is to easily and freely control the particle size to a diameter of 2 μm or less using a wet method and with simple equipment, and to achieve a uniform particle size distribution with a small width. The object of the present invention is to provide a method for producing non-agglomerated, high-purity nickel and co/metal metal fine powders in large quantities and at a high yield.
本発明者らは、前記目的を達成すべく種々研究を重ねた
結果、ニッケルまたはコノくルトをイオンとして含有す
る硫酸ニッケル、硫酸コバルト、塩化ニッケル、塩化コ
バルト、硝酸ニッケル、硝酸コバルト等々の水溶液（以
下ニッケルイオン水溶液、コバルトイオン水溶液という
）に水素化ホウ素ナトリウＡ （ＮａＢＨ４の他Ｎａ、
Ｂ２Ｈ６、Ｎａ２Ｂ ａＨｓｏ及びＮａ２Ｂ６Ｈｇ等の
ホウ化水素とＮａの付加化合物に当る組成の化合物の総
称をいう。以下ＳＢＨと称す。）及びヒドラジン（ＮＨ
２ＮＨ，） を同時に混合添加し、溶液中のニッケル
またはコバルトを金属微粉凝集体に還元した後、詐金輝
微粉凝集体を膠及び／またはアルコールで処理すること
により直径２μｍ以下の粒度分布幅が小さく、均一な非
凝集性の高純度のニッケル及びコバルト金属微粉末が得
られることを見出し本発明を完成したものである。As a result of various studies to achieve the above object, the present inventors have discovered that aqueous solutions of nickel sulfate, cobalt sulfate, nickel chloride, cobalt chloride, nickel nitrate, cobalt nitrate, etc. containing nickel or conolite as ions ( (hereinafter referred to as nickel ion aqueous solution, cobalt ion aqueous solution), sodium borohydride A
A general term for compounds with compositions corresponding to addition compounds of borohydride and Na, such as B2H6, Na2B aHso, and Na2B6Hg. Hereinafter referred to as SBH. ) and hydrazine (NH
2NH,) is mixed and added at the same time to reduce the nickel or cobalt in the solution to metal fine powder aggregates, and then the false gold powder aggregates are treated with glue and/or alcohol to reduce the particle size distribution width with a diameter of 2 μm or less. The present invention was completed by discovering that uniform, non-agglomerated, highly pure nickel and cobalt metal fine powders can be obtained.
すなわち本発明は、ニッケルイオン溶液またはコバルト
イオン溶液にＳＢＨ及びヒドラジンを同時に混合添加し
、前記溶液中めニッケルまたはコバルトイオンを金属微
粉凝集体に還元した後、該金属微粉凝集体を膠及び／ま
たはアルコールで処理することにより金属微粉分散体を
鞠るととを特徴とするニッケル及びコバルト微粉末の製
造法にある。That is, in the present invention, SBH and hydrazine are simultaneously mixed and added to a nickel ion solution or a cobalt ion solution, the nickel or cobalt ions in the solution are reduced to metal fine powder aggregates, and then the metal fine powder aggregates are treated with glue and/or A method for producing fine nickel and cobalt powder, characterized by dispersing a fine metal powder dispersion by treating it with alcohol.
本発明によるニッケル及びコバルト微粉末の製造法にお
いては、ニッケルイオン溶液またはコバルトイオン溶液
の声を苛性ソーダ、苛性カリ、アンモニア等、好ましく
はアンモニア及び硫酸塩酸等の鉱酸好ましくは硫酸によ
り６．０〜１０、好ましくは８．０〜９．５に保ち、ま
た、水溶液の温度を３０〜９０°Ｃ１好ましくは４０〜
８０°Ｃに保ち、前記水溶液中のニッケルまたはコバル
ト含有量に対しモル比（ＳＢＨ／Ｎ１ｏｒＣｏ、
／Ｎ１ｏｒＣｏ ）において、１．２５ｘ１０ 〜０
．１２５好ましくは２．５ＸｌＯ〜０，０５量のＳＢＨ
及び０５〜２．５好ましくは１．０〜２．０量のヒドラ
ジンを混合し水溶液としたものを添加する。この操作に
より水溶液中のニッケルまたはコバルトは金属微粉凝集
体に還元され、沢過助剤または凝集剤を使用することな
く、自然重力ｐ過、減圧Ｐｂにより簡単に短時間で固液
分離できる。固液分離され、治過器に保持された上記ニ
ッケルまたはコバルトの金属微粉凝集体に膠及び／また
はアルコール、好ましくは膠及びアルコールを添加洗滌
し、ニッケルまたはコバルトの金属微粉分散体とする。In the method for producing fine nickel and cobalt powder according to the present invention, a nickel ion solution or a cobalt ion solution is mixed with a mineral acid such as caustic soda, caustic potash, ammonia, etc., preferably ammonia and a mineral acid such as sulfuric acid, preferably sulfuric acid, to give a concentration of 6.0 to 10 , preferably 8.0 to 9.5, and the temperature of the aqueous solution to 30 to 90°C, preferably 40 to
The molar ratio (SBH/N1orCo,
/N1orCo), 1.25x10~0
．． 125 preferably 2.5XlO to 0.05 amount of SBH
and 05 to 2.5, preferably 1.0 to 2.0, of hydrazine are mixed and an aqueous solution is added. By this operation, nickel or cobalt in the aqueous solution is reduced to fine metal powder aggregates, and solid-liquid separation can be easily performed in a short time by natural gravity p-filtration and reduced pressure Pb without using a filtering aid or flocculant. Glue and/or alcohol, preferably glue and alcohol, are added to the nickel or cobalt metal fine powder aggregate, which is separated into solid and liquid and held in a filtration device, and washed to obtain a nickel or cobalt metal fine powder dispersion.
この操作において使用する膠は濃度０．５〜５ｇ／ｌの
水溶液として、ニッケルまたはコバルトの金属微粉量に
対して０．１〜５重量パーセントを添加し処理する。The glue used in this operation is treated as an aqueous solution with a concentration of 0.5 to 5 g/l, and 0.1 to 5 percent by weight is added to the amount of nickel or cobalt metal fine powder.
続いて水により過剰の膠を洗浄後、アルコールを添加す
ることにより水を置換除去する。尚アルコールは水を置
換するアルコールであればどんなものでもよいが、メタ
ノール、エタノールが好ましい。この様にして得られた
金属微粉分散体は、真空乾燥、凍結乾燥等特殊な乾燥法
を使用することなく、通常の乾燥法、雰囲気にて温度６
０〜９０９０６０〜６０分乾燥することにより直径２μ
ｍ以下の粒度分布幅の小さい、均一な微粉末とすること
ができる。Subsequently, after washing excess glue with water, alcohol is added to remove the water by displacement. The alcohol may be any alcohol as long as it displaces water, but methanol and ethanol are preferred. The metal fine powder dispersion obtained in this way can be dried at a temperature of 6.5 cm using a normal drying method in an atmosphere without using special drying methods such as vacuum drying or freeze drying.
0~909060~2μ in diameter by drying for 60 minutes
A uniform fine powder with a narrow particle size distribution width of m or less can be obtained.
前記還元反応において、ニッケルまたはコバルトイオン
溶液の濃度は特に限定されないが、取扱い液量及び反応
フントロールの点よす０．５〜４，０ｍ５！−に′が好
ましい。In the reduction reaction, the concentration of the nickel or cobalt ion solution is not particularly limited, but it is 0.5 to 4.0 m5 depending on the amount of liquid handled and reaction load! − and ′ are preferred.
以上のごとき本発明方法によると、従来内蓋とされてい
た直径２μｍ以下のニッケル及びコバルトの金属微粉末
を湿式法により、乾式法に比較して、簡便な設備で容易
に大量に高収率で製造できるという優れた効果を有し、
さらに得られた金属微粉末は粒度分布幅か小さく均一な
非凝集性の粉末であり、比表面積は１〜１０ ｍ ／
９ ｓ純度９９．５％以上の優れた特性をも有し電子工
業分野において使用可能なものである。According to the method of the present invention as described above, nickel and cobalt fine metal powders with a diameter of 2 μm or less, which were conventionally used as inner lids, can be easily produced in large quantities using a wet method with simple equipment and in high yield compared to the dry method. It has the excellent effect of being able to be manufactured with
Furthermore, the obtained metal fine powder is a uniform non-agglomerated powder with a small particle size distribution width, and a specific surface area of 1 to 10 m /
It also has excellent properties with a purity of 99.5% or higher and can be used in the electronic industry.
以下、本発明を実施例および比較例に基づいてさらに具
体的に説明するが、本発明はこれら実施例に限定される
ものではない。Hereinafter, the present invention will be explained in more detail based on Examples and Comparative Examples, but the present invention is not limited to these Examples.
実施例１
硫ｍニッケル（ＮｉＳ０４・６Ｈ２０）を水に溶解し、
アンモニア（ＮＨ，ＯＨ）及び硫酸（Ｈ２８０４）によ
り溶液中の声を調整した。一方８ＢＨ及びヒドラジンを
混合し水に溶解したヒドラジン水溶液を第１表に示す如
き、−及び反応温度を保持しながら添加し、水溶液中の
ニッケルを金属微粉凝集体に還元した。Example 1 Nickel sulfate (NiS04.6H20) was dissolved in water,
The voice in solution was adjusted by ammonia (NH,OH) and sulfuric acid (H2804). On the other hand, an aqueous hydrazine solution in which 8BH and hydrazine were mixed and dissolved in water was added while maintaining the - and reaction temperature as shown in Table 1, and the nickel in the aqueous solution was reduced to metal fine powder aggregates.
この場合、硫酸ニッケル水溶液々量及び濃度、混合添加
した８ＢＨ及びヒドラジンの量（ｍｏｌ）及びＳＢＨ／
Ｎｉモル比、ヒドラジン／Ｎｉモル比、ヒドラジン水溶
液中のヒドラジン濃度、−及び反応温度条件を第１表に
示す如く変更し試験篇１〜５を行なった。In this case, the amount and concentration of the nickel sulfate aqueous solution, the amount (mol) of 8BH and hydrazine mixed and added, and the SBH/
Tests 1 to 5 were conducted by changing the Ni molar ratio, hydrazine/Ni molar ratio, hydrazine concentration in the hydrazine aqueous solution, and reaction temperature conditions as shown in Table 1.
次で生成した金属微粉凝集体含有スラリーを自然重力濾
過器により治過し、濾過器中に保持されたニッケル微粉
凝集体を水にて通液洗滌涙過→渉度２ｇ／ｌの膠溶液１
１を通液濾過→水にて通液洗滌流過→メタノール（ＣＨ
３０Ｈ） １ ｌを通液濾過、の各処理をしだ後８０℃
、６０分の乾燥条件にて乾燥しニッケル微粉末を得た。The slurry containing fine metal powder aggregates generated in the next step was filtered using a natural gravity filter, and the nickel fine powder aggregates retained in the filter were washed with water.
1. Liquid filtration → Washing and filtration with water → Methanol (CH
30H) After each process of liquid filtration and filtration of 1 liter, heat at 80°C.
The powder was dried under drying conditions for 60 minutes to obtain fine nickel powder.
各試験例において得られた微粉末景及びその特性値を第
２表に示す。Table 2 shows the fine powder appearance and its characteristic values obtained in each test example.
第２表並びに添付の試験扁１より得られたＮｉ微粉末の
２０．０００倍の走査電子顕微鏡参考写真屋１に明らか
な如く比表面積が大で平均粒径は何れも２μ以下で走査
電子顕微鏡による観察によるとその粒度分布幅が非常に
小さく均一な非凝集性のニッケル微粉末であることがわ
かった。As is clear from Table 2 and the attached test plate 1, the Ni powder obtained from the scanning electron microscope 20.000 times larger has a large specific surface area, and the average particle size is less than 2 μm. According to the observation by , it was found to be a non-agglomerated fine nickel powder with a very small and uniform particle size distribution.
実施例２
硫酸コバル） （ＣｏＳ０４・７Ｈ２０）を水に溶解し
、アンモニア水（ＮＨ４０Ｈ）及び硫酸（Ｈ２ＳＯ４）
により溶液中の〆］を９０に調整したコバルト濃度＝２
０、５ ｍｏｌ ／ ｌの水溶液５１ＫＳＢＨ６，２５
Ｘ１０モル（ＳＢＨ／ＣＯモル比２．５Ｘ１Ｄ−２）及
びヒドラジン５モル（ヒドラジン７００モル比２．０）
を混合し、水に溶解したヒドラジン濃度２０重量％の水
溶液を反応ｐ）（９，０、反応温度７０°Ｃに保持しな
がら添加し、コバルトを金属微粉凝集体に還元した後、
実施例１と同様な処理を行なった後コバルト微粉末１４
５Ｉを得た。そのＣ（ｌ純度は９９．５％比表面積２．
２７７Ｌ″／ｙ、平均粒径０．５μｍであり、走査電子
顕微鏡による観察にて、その粒径範囲は０、４〜０．６
μｍと粒度分布幅が小さく均一な粉末であることがわか
った。Example 2 Cobal sulfate) (CoS04.7H20) was dissolved in water, aqueous ammonia (NH40H) and sulfuric acid (H2SO4)
Cobalt concentration = 20.5 mol/l aqueous solution 51 KSBH6.25 with the cobalt concentration adjusted to 90 by
X10 moles (SBH/CO molar ratio 2.5X1D-2) and 5 moles of hydrazine (hydrazine 700 molar ratio 2.0)
An aqueous solution of hydrazine dissolved in water with a concentration of 20% by weight was added to reaction p) (9,0, while maintaining the reaction temperature at 70 ° C., and after reducing cobalt to metal fine powder aggregates,
After performing the same treatment as in Example 1, fine cobalt powder 14
I got 5I. Its C (l purity is 99.5% specific surface area 2.
277L''/y, average particle size 0.5 μm, and the particle size range was 0.4 to 0.6 when observed with a scanning electron microscope.
It was found that the powder was uniform with a small particle size distribution width of μm.
尚得られたＣＯ微粉末の２０．０００倍の走査電子顕微
鏡写真を参考写真、亮２として添付した。A scanning electron micrograph of the obtained CO fine powder at a magnification of 20,000 times is attached as a reference photograph, Ryo 2.
比較側１
実施例１及び２と同様な方法で調整した濃度０．５ｍ０
１／ｌ、ｐｌ′Ｉ９０のニッケルイオン水溶液またはコ
バルトイオン水溶液５１ＶＣ８ＢＨ，１，８７５モル（
ＳＢＨ／Ｎｉ又はＣＯのモル比０．７５ ）また目ヒド
ラジン５モル（ヒドラジン／ Ｎｉ又はＣｏのモル比２
．０）を反応温度６０℃に保持しながら、ＳＢＨ及びヒ
ドラジンを夫々単独で添加し、生成した粉末スラリーを
実施例１と同様な方法で処理し粉末を得た。Comparison side 1 Concentration 0.5m0 adjusted in the same manner as Examples 1 and 2
1/l, pl'I90 nickel ion aqueous solution or cobalt ion aqueous solution 51VC8BH, 1,875 mol (
SBH/Ni or CO molar ratio 0.75) or hydrazine 5 mol (hydrazine/Ni or Co molar ratio 2
．． While maintaining the reaction temperature of 0) at 60° C., SBH and hydrazine were added individually, and the resulting powder slurry was treated in the same manner as in Example 1 to obtain powder.
各々の粉末をＸ線回折及び化学分析した結果、ニッケル
イオン水溶液にＳＢＨを単独添加した場合、生成Ｎｉ粉
末はＮｉＯとＮｉ２Ｂの混合ピークを示し、Ｎｉ品位９
０％、Ｂ品位５％であった。同様にＳＢＨをコバルトイ
オン水溶液に単独添加した場合も生成ＣＯ粗粉末メタル
コバルトとコバルトホライドの混合物でありＣＯ品位８
６％ Ｂ品位４％であった。ヒドラジンをニッケル水溶
液又はコバルトイオン水溶液に単独添加した場合夫々生
成した粉末は硫酸ニッケルヒドラジン及び硫酸コバルト
ヒドラジンであった。すなわち、本発明の目的を達成す
るためＮｉイオン又はＣＯイオンを含有する溶液にＳＢ
Ｈ及びヒドラジンの同時添加が必須であることを示して
いる。As a result of X-ray diffraction and chemical analysis of each powder, when SBH was added alone to a nickel ion aqueous solution, the produced Ni powder showed a mixed peak of NiO and Ni2B, and the Ni grade was 9.
0%, B grade 5%. Similarly, when SBH is added alone to a cobalt ion aqueous solution, the CO produced is a mixture of coarse powder metal cobalt and cobalt holide, and the CO grade is 8.
6% B grade 4%. When hydrazine was added alone to an aqueous nickel solution or an aqueous cobalt ion solution, the powders produced were nickel hydrazine sulfate and cobalt hydrazine sulfate, respectively. That is, in order to achieve the purpose of the present invention, SB is added to a solution containing Ni ions or CO ions.
This shows that simultaneous addition of H and hydrazine is essential.
比較例２
実施例１の試験慕１及び実施例２と同様な方法で生成し
たニッケルまたはコバルト微粉凝集体を膠及び／または
アルコール処理することなく単に水にて洗浄し、濾過後
、８０℃、２４０分乾燥し、ニッケルまたはコバルト微
粉各々１４．．５ ｇ、 １４６Ｆを得た。生成した微
粉末のＸ線回折及び走査電子顕微鏡観察の結果、酸化物
のピークが認められると同時に、凝集、固結が著しく、
超音波分散によっても容易に分散しなかった。Comparative Example 2 A nickel or cobalt fine powder aggregate produced in the same manner as Test 1 of Example 1 and Example 2 was simply washed with water without being treated with glue and/or alcohol, and after filtration, it was heated at 80°C. Dry for 240 minutes and add nickel or cobalt fine powder for 14 minutes each. ．． 5 g of 146F was obtained. As a result of X-ray diffraction and scanning electron microscopy observation of the produced fine powder, oxide peaks were observed, and at the same time, significant agglomeration and caking occurred.
It was not easily dispersed even by ultrasonic dispersion.
即ちこの結果より膠及び／またはアルコール処理が本発
明目的達成のために必要であることが判る。That is, from this result, it can be seen that glue and/or alcohol treatment is necessary to achieve the object of the present invention.
叙上の実施例及び比較例に明らかな如く本発明によるニ
ッケル及びコバルト微粉末の製造法は従来の湿式法によ
り得られる微粉末よりその特性において優れかつ簡便な
設備を用いて大量に高収率で製造しうるもので甚だ有用
な発明である。As is clear from the above examples and comparative examples, the method for producing fine nickel and cobalt powder according to the present invention has superior properties to fine powders obtained by conventional wet methods, and can be produced in large quantities at high yields using simple equipment. It is an extremely useful invention as it can be manufactured using
代理人 弁理士 木 村 三 朗Agent: Patent Attorney Sanro Kimura
Claims (4)
ルトイオンを含有する水溶液に水素化ホウ素ナトリウム
及びヒドラジンを同時に混合添加し、前記水溶液中のニ
ッケルまたはコバルトを金属微粉凝集体に還元し、該金
属微粉凝集体を膠及び／またはアルコールで処理するこ
とにより金属微粉分散体を得ることを特徴とするニッケ
ル及びコバルト微粉末の製造法。(1) Mixing and adding sodium borohydride and hydrazine simultaneously to an aqueous solution containing nickel ions or an aqueous solution containing cobalt ions, reducing nickel or cobalt in the aqueous solution to metal fine powder aggregates, and reducing the metal fine powder aggregates. A method for producing nickel and cobalt fine powder, which comprises obtaining a metal fine powder dispersion by treating nickel and cobalt fine powder with glue and/or alcohol.
度を６０〜９０℃に保持することを特徴とする特許請求
の範囲第１項記載のニッケル及びコバルト微粉末の製造
法。(2) The method for producing fine nickel and cobalt powder according to claim 1, characterized in that during the reduction, the pH of the aqueous solution is maintained at 6.0 to 10 and the temperature is maintained at 60 to 90°C.
合添加するに当り、水溶液中のニッケルまたはコバルト
含有量に対し、水素化ホウ素ナトリウムのモル比が１．
２５ Ｘ １０−’−０，１２５、ヒドラジンのモル比
が０．５〜２．５であることを特徴とする特許請求の範
囲第１項記載のニッケル及びコバルト微粉末の製造法。(3) When adding the sodium borohydride and hydrazine together, the molar ratio of sodium borohydride to the nickel or cobalt content in the aqueous solution is 1.
25 X 10-'-0,125, and the molar ratio of hydrazine is 0.5 to 2.5. The method for producing fine nickel and cobalt powder according to claim 1.
。 の水溶液をニッケルまたはコバルト微粉末量に対し０．
１〜５重量％添伽処理することを特徴とする特許請求の
範囲第１項記載のニッケル及びコバルト微粉末の製造法
。(4) A glue concentration of 0.5 to 5 g/l in the metal fine powder aggregate
. of an aqueous solution of 0.0% for the amount of nickel or cobalt fine powder.
2. The method for producing fine nickel and cobalt powder according to claim 1, wherein the nickel and cobalt fine powders are added in an amount of 1 to 5% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3655883A JPS59162206A (en) | 1983-03-08 | 1983-03-08 | Manufacture of fine nickel and cobalt powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3655883A JPS59162206A (en) | 1983-03-08 | 1983-03-08 | Manufacture of fine nickel and cobalt powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59162206A true JPS59162206A (en) | 1984-09-13 |
| JPH0249364B2 JPH0249364B2 (en) | 1990-10-30 |
Family
ID=12473080
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3655883A Granted JPS59162206A (en) | 1983-03-08 | 1983-03-08 | Manufacture of fine nickel and cobalt powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59162206A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100415491B1 (en) * | 1997-12-12 | 2004-01-31 | 미츠이 긴조쿠 고교 가부시키가이샤 | Nickel fine powder and process for producing the same |
| CN1319685C (en) * | 2005-01-13 | 2007-06-06 | 南京大学 | Production for nanometer nickel powder |
| JP2010202943A (en) * | 2009-03-04 | 2010-09-16 | Mitsuboshi Belting Ltd | Metal colloid particle aggregate and method for producing the same |
| CN103706804A (en) * | 2013-12-25 | 2014-04-09 | 南昌航空大学 | Environment-friendly preparing method of nickel nanocrystalline |
| CN104001551A (en) * | 2014-05-30 | 2014-08-27 | 绍兴文理学院 | Poly(tert-butyl acrylamide) nanosphere loaded Ni-B catalyst as well as preparation method and application of poly(tert-butyl acrylamide) nanosphere loaded Ni-B catalyst |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5395165A (en) * | 1977-01-31 | 1978-08-19 | Murata Manufacturing Co | Minute particle metal nickel powder manufacturing process |
-
1983
- 1983-03-08 JP JP3655883A patent/JPS59162206A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5395165A (en) * | 1977-01-31 | 1978-08-19 | Murata Manufacturing Co | Minute particle metal nickel powder manufacturing process |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100415491B1 (en) * | 1997-12-12 | 2004-01-31 | 미츠이 긴조쿠 고교 가부시키가이샤 | Nickel fine powder and process for producing the same |
| CN1319685C (en) * | 2005-01-13 | 2007-06-06 | 南京大学 | Production for nanometer nickel powder |
| JP2010202943A (en) * | 2009-03-04 | 2010-09-16 | Mitsuboshi Belting Ltd | Metal colloid particle aggregate and method for producing the same |
| CN103706804A (en) * | 2013-12-25 | 2014-04-09 | 南昌航空大学 | Environment-friendly preparing method of nickel nanocrystalline |
| CN104001551A (en) * | 2014-05-30 | 2014-08-27 | 绍兴文理学院 | Poly(tert-butyl acrylamide) nanosphere loaded Ni-B catalyst as well as preparation method and application of poly(tert-butyl acrylamide) nanosphere loaded Ni-B catalyst |
| CN104001551B (en) * | 2014-05-30 | 2016-02-17 | 绍兴文理学院 | The Ni-B Catalysts and its preparation method of poly-N-tert-butyl acrylamide nanosphere load and application |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0249364B2 (en) | 1990-10-30 |
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