JPH0551610A - Production of fine nickel powder - Google Patents

Production of fine nickel powder

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Publication number
JPH0551610A
JPH0551610A JP3207872A JP20787291A JPH0551610A JP H0551610 A JPH0551610 A JP H0551610A JP 3207872 A JP3207872 A JP 3207872A JP 20787291 A JP20787291 A JP 20787291A JP H0551610 A JPH0551610 A JP H0551610A
Authority
JP
Japan
Prior art keywords
nickel
hydroxide
particle size
strong alkali
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
Application number
JP3207872A
Other languages
Japanese (ja)
Other versions
JP2900650B2 (en
Inventor
Hisashi Miki
寿 三木
Kiyoshi Sato
喜代志 佐藤
Minoru Yonezawa
実 米沢
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.)
Murata Manufacturing Co Ltd
Original Assignee
Murata Manufacturing 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 Murata Manufacturing Co Ltd filed Critical Murata Manufacturing Co Ltd
Priority to JP3207872A priority Critical patent/JP2900650B2/en
Publication of JPH0551610A publication Critical patent/JPH0551610A/en
Application granted granted Critical
Publication of JP2900650B2 publication Critical patent/JP2900650B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions

Abstract

PURPOSE:To obtain a fine metallic Ni powder having a small grain diameter and a narrow grain size distribution and capable of being excellently dispersed by adding a strong alkali to the aq. soln. of a water-soluble Ni(II) salt to form Ni hydroxide and reducing the hydroxide under specified conditions. CONSTITUTION:A strong alkali is added to the aq. soln. of a water-soluble Ni(II) salt (e.g. NiCl2 and NiSO4) to form Ni(II) hydroxide. The hydroxide is reduced with a reducing agent (hydrazine or hydrazine hydrate) in a strong alkaline medium at pH10-14. At this time, the temp. is controlled to 55-70 deg.C, the Ni ion concn. to <=2mol/l and the reducing time to <=40min.

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【産業上の利用分野】本発明はニッケル微粉末の製造方
法、特に、積層コンデンサの内部電極材料として有用な
ニッケルの微粉末の製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing fine nickel powder, and more particularly to a method for producing fine nickel powder which is useful as an internal electrode material of a multilayer capacitor.

【０００２】[0002]

【従来の技術】近年、セラミック積層コンデンサの小型
化且つ大容量化が急激に進み、その生産コストの低減化
を図るべく、内部電極材料として白金、パラジウム等の
貴金属に代わりニッケルなどの卑金属を用い、かつ、誘
電体材料として非還元性誘電体磁器を用いることが、例
えば、特公昭５６−４６６４１号公報にて提案されてい
る。他方、この種の内部電極材料として用いる金属ニッ
ケル粉末の製造方法としては、例えば、特開昭５３−９
５１６５号公報にて塩化ニッケル、炭酸ニッケル及び酢
酸ニッケルのうちいずれか一種を含むニッケル含有溶液
にヒドラジン若しくはヒドラジン化合物を添加、混合し
て１００℃以下の温度で加熱する方法が提案されてい
る。2. Description of the Related Art In recent years, ceramic monolithic capacitors have been rapidly reduced in size and increased in capacity, and in order to reduce the production cost thereof, a base metal such as nickel is used as an internal electrode material instead of a noble metal such as platinum or palladium. Moreover, the use of a non-reducing dielectric ceramic as the dielectric material has been proposed in, for example, Japanese Patent Publication No. 56-46641. On the other hand, as a method for producing metallic nickel powder used as this kind of internal electrode material, for example, Japanese Patent Laid-Open No. 53-9 is used.
Japanese Patent No. 5165 proposes a method in which a hydrazine or a hydrazine compound is added to and mixed with a nickel-containing solution containing any one of nickel chloride, nickel carbonate and nickel acetate, and the mixture is heated at a temperature of 100 ° C. or lower.

【０００３】[0003]

【発明が解決しようとする課題】しかしながら、この方
法では、微細な粒径のニッケル粉末を得るためには、ニ
ッケル塩１モル当たりヒドラジン又はその化合物を約１
４モル以上と多量添加しなければならず、しかも、生成
したニッケル粉末は粒度分布幅が広くバインダに対する
分散性が悪いため、積層コンデンサの内部電極材料とし
て使用した場合、内部欠陥や電気特性の劣化を招くとい
う問題があった。However, in this method, in order to obtain a nickel powder having a fine particle size, about 1 hydrazine or its compound is added per mol of the nickel salt.
It must be added in a large amount of 4 mol or more, and the generated nickel powder has a wide particle size distribution and poor dispersibility in the binder. Therefore, when it is used as an internal electrode material of a multilayer capacitor, internal defects and deterioration of electrical characteristics are caused. There was a problem of inviting.

【０００４】従って、本発明は、分散性が良く、粒径が
小さく粒度分布幅の極めて狭い金属ニッケル微粉末を得
ることを目的とするものである。Therefore, an object of the present invention is to obtain a fine metal nickel powder having a good dispersibility, a small particle size and an extremely narrow particle size distribution width.

【０００５】[0005]

【課題を解決するための手段】本発明は、前記課題を解
決するため、水溶性ニッケル(II)塩の水溶液に強アルカ
リを加えて水酸化ニッケル(II)を生成させ、該水酸化ニ
ッケル(II)を強アルカリ下にて還元剤で還元するように
したものである。[Means for Solving the Problems] In order to solve the above-mentioned problems, a strong alkali is added to an aqueous solution of a water-soluble nickel (II) salt to form nickel (II) hydroxide, II) is reduced with a reducing agent in a strong alkali.

【０００６】前記水溶性ニッケル(II)としては、例え
ば、塩化ニッケル（ＮiＣl2）、硫酸ニッケル（ＮiＳＯ
4）、硝酸ニッケル（Ｎi（ＮＯ3）2）、酢酸ニッケルな
どが挙げられるが、これらに限定されるものではない。
また、強アルカリとしては、水酸化カリウム及び水酸化
ナトリウムのいずれかを使用すれば良い。還元剤として
は、ヒドラジン及びヒドラジン化合物のうちの一種が使
用されるが、ヒドラジン又はヒドラジン水化物が好適で
ある。この還元剤、例えば、ヒドラジン水化物の添加量
は、一般的には、理論量の２〜３倍で十分である。Examples of the water-soluble nickel (II) include nickel chloride (NiCl 2 ) and nickel sulfate (NiSO).
4 ), nickel nitrate (Ni (NO 3 ) 2 ), nickel acetate and the like, but not limited thereto.
As the strong alkali, either potassium hydroxide or sodium hydroxide may be used. As the reducing agent, one of hydrazine and a hydrazine compound is used, and hydrazine or hydrazine hydrate is preferable. The reducing agent, for example, the amount of hydrazine hydrate added is generally sufficient to be 2 to 3 times the theoretical amount.

【０００７】前記還元は強アルカリ下で行われるが、ｐ
Ｈ１０以上が好ましく、また、温度５５〜７０℃、ニッ
ケルイオン濃度２.０mol／ｌ以下の条件下で行うのが好
適である。更に、微細で粒度分布幅の狭い微粉末を得る
ためには、４０分以内の還元を完了させるように温度及
びニッケルイオン濃度を調整するのが望ましい。The reduction is carried out under strong alkali, but p
H10 or more is preferable, and it is suitable to carry out under conditions of a temperature of 55 to 70 ° C. and a nickel ion concentration of 2.0 mol / l or less. Further, in order to obtain a fine powder having a fine particle size distribution width, it is desirable to adjust the temperature and the nickel ion concentration so as to complete the reduction within 40 minutes.

【０００８】[0008]

【作用】ニッケル源として塩化ニッケルを用い、還元剤
としてヒドラジン水化物を用いた場合について、下記反
応式を参照しながら説明すると、塩化ニッケルを水に溶
かして水溶液とし（反応式（１））、これに水酸化ナト
リウム溶液を加えて強アルカリ性にすると、水酸化ニッ
ケル（II）、Ｎｉ(ＯＨ)2、が沈澱する（反応式
（２））。これにヒドラジン水化物を加えると、ヒドラ
ジンが分解し（反応式（３））、その分解により生じた
アンモニアと水酸化ニッケル（II）とが反応してニッケ
ル錯塩を生成し（反応式（４））、これに更にヒドラジ
ン水化物を加えるとニッケル錯塩が還元され、ニッケル
が析出する（反応式（５））。The case where nickel chloride is used as the nickel source and hydrazine hydrate is used as the reducing agent will be described with reference to the following reaction formula. Nickel chloride is dissolved in water to form an aqueous solution (reaction formula (1)), When sodium hydroxide solution is added to this to make it strongly alkaline, nickel (II) hydroxide and Ni (OH) 2 are precipitated (reaction formula (2)). When hydrazine hydrate is added to this, hydrazine decomposes (reaction formula (3)), and ammonia generated by the decomposition reacts with nickel (II) hydroxide to form a nickel complex salt (reaction formula (4)). ), And when hydrazine hydrate is further added thereto, the nickel complex salt is reduced and nickel is deposited (reaction formula (5)).

【０００９】（１）ＮiＣl2・６Ｈ2Ｏ→Ｎi2+＋２Ｃl-
＋６Ｈ2Ｏ （２）Ｎi2+＋２ＯＨ-→Ｎi(ＯＨ)2↓ 強アルカリ下 （３）２Ｎ2Ｈ4・Ｈ2Ｏ→２ＮＨ3＋Ｎ2＋２ｅ-＋２Ｈ3
Ｏ+ （４）Ｎi(ＯＨ)2＋６ＮＨ3→［Ｎi(ＮＨ3)6］2+＋２Ｏ
Ｈ- （５）［Ｎi(ＮＨ3)6］2+＋２ｅ-→Ｎi↓＋ＮＨ3 (1) NiCl2・ 6H2O → Ni2+＋ 2Cl-
+ 6H2O (2) Ni2++ 2OH-→ Ni (OH)2↓ Under strong alkali (3) 2N2HFour・ H2O → 2NH3+ N2+ 2e-+ 2H3
O+  (4) Ni (OH)2+6 NH3→ [Ni (NH3)6]2++20
H-  (5) [Ni (NH3)6]2++ 2e-→ Ni ↓ + NH3

【００１０】前記還元反応により生成されるニッケル粉
末の一次粒子の粒径及びその粒度分布は、一般に、その
反応速度、従って、還元剤（ここではヒドラジン水化
物）の投入開始時から反応系中のニッケルイオンが全て
ニッケルに還元されるまでの時間に依存するが、還元が
４０分以内で完了するようにニッケルイオン濃度及び反
応温度を調節すれば、１次粒子の平均粒径０.３μｍ、
粒度範囲０.１７〜５.２７μｍと粒度分布幅が極めて狭
くサブミクロンオーダーの球形のニッケル微粉末が得ら
れる。通常、ニッケルイオン濃度２.０mol以下、反応温
度５５〜７０℃の条件下で還元を行うのが好適である。The particle size and the particle size distribution of the primary particles of nickel powder produced by the above reduction reaction are generally determined by the reaction rate, and therefore, from the start of the introduction of the reducing agent (here, hydrazine hydrate) in the reaction system. Although it depends on the time until all the nickel ions are reduced to nickel, if the nickel ion concentration and reaction temperature are adjusted so that the reduction is completed within 40 minutes, the average particle size of the primary particles is 0.3 μm,
Spherical nickel fine powder of submicron order with a very narrow particle size distribution range of 0.17 to 5.27 μm is obtained. Usually, it is preferable to carry out the reduction under the condition that the nickel ion concentration is 2.0 mol or less and the reaction temperature is 55 to 70 ° C.

【００１１】以下、実施例について説明する。Examples will be described below.

【００１２】[0012]

【実施例】純水１０００mlを５５〜７０℃範囲内の一定
温度に加熱、維持し、これに表１に示す量のＮiＣl2・
６Ｈ2Ｏを完全に溶解させる。この水溶液に３.１７mol
／Ｎｉ2+となるようにＮaＯＨ溶液を加えてｐＨを１３
〜１４に調整し、さらに分散剤として１％カルボキシメ
チルセルロース溶液を全量の１/１００加えた後、撹拌
機を１３０ｒｐｍの速度で回転させて撹拌しながら、Ｎ
ｉ2+イオンチェッカーでニッケルイオンが検出されなく
なるまで３０℃に維持したヒドラジン水化物を加えニッ
ケルを析出させる。ヒドラジン水化物の添加量は１２.
７mol／Ｎi2+である。次いで、反応液を室温まで冷却し
た後、純水を静かに加え、洗浄液のｐＨが７．０〜８．
０になるまで生成したニッケル粉末を洗浄する。次い
で、ニッケル粉末を濾別したのち、９０℃で乾燥して金
属ニッケル粉末を得る。Example: 1000 ml of pure water was heated and maintained at a constant temperature within the range of 55 to 70 ° C., and the amount of NiCl 2 ·
Dissolve 6H 2 O completely. 3.17 mol in this aqueous solution
/ Ni 2+ to adjust pH to 13 by adding NaOH solution.
To 14 and 1/100 of the total amount of 1% carboxymethyl cellulose solution was added as a dispersant, and the N was stirred while rotating the stirrer at a speed of 130 rpm.
Add hydrazine hydrate maintained at 30 ° C. until nickel ions are no longer detected by the i 2+ ion checker to precipitate nickel. The amount of hydrazine hydrate added is 12.
It is 7 mol / Ni 2+ . Then, after the reaction solution was cooled to room temperature, pure water was gently added, and the pH of the cleaning solution was 7.0 to 8.
The nickel powder produced is washed until it reaches zero. Next, the nickel powder is filtered off and dried at 90 ° C. to obtain metallic nickel powder.

【００１３】得られた金属ニッケル粉末は球形であり、
その一次粒子径（平均粒径）および粒度分布を求めたと
ころ、表１に示す結果が得られた。なお、一次粒子の平
均粒径は２次電子像写真から求めた。表１中、還元時間
はヒドラジン水化物の投入を開始した時点からニッケル
イオンが検出されなくなるまでの時間である。The metal nickel powder obtained is spherical,
When the primary particle size (average particle size) and particle size distribution were determined, the results shown in Table 1 were obtained. The average particle size of the primary particles was obtained from the secondary electron image photograph. In Table 1, the reduction time is the time from when the addition of hydrazine hydrate was started until nickel ions were not detected.

【００１４】[0014]

【表１】 番号 Ni2+濃度 温度 粒度分布 １次粒子径 還元時間 (mol/l) （℃） Ｄ10 Ｄ50 Ｄ90 （μｍ) （分) １ 0.10 70 0.58 1.53 3.50 0.3 10 ２* 0.42 40 0.73 2.20 14.27 0.7 120 ３* 〃 50 0.73 1.98 5.63 0.7 70 ４ 〃 60 0.56 1.38 3.32 0.3 30 ５* 0.70 40 0.76 2.13 8.97 0.7 60 ６ 〃 50 0.55 1.38 3.88 0.3 40 ７ 〃 60 0.57 1.44 3.30 0.3 35 8 0.80 〃 0.58 1.44 3.30 0.3 35 ９ 0.90 〃 0.57 1.41 2.93 0.3 30 １０ 1.0 〃 0.54 1.33 2.71 0.3 25
[Table 1] No. Ni 2+ concentration Temperature particle size distribution Primary particle size Reduction time (mol / l) (℃) D10 D50 D90 (μm) (min) 1 0.10 70 0.58 1.53 3.50 0.3 10 2 * 0.42 40 0.73 2.20 14.27 0.7 120 3 * 〃 50 0.73 1.98 5.63 0.7 70 4 〃 60 0.56 1.38 3.32 0.3 30 5 * 0.70 40 0.76 2.13 8.97 0.7 60 6 〃 50 0.55 1.38 3.88 0.3 40 7 〃 60 0.57 1.44 3.30 0.3 35 8 0.80 〃 0.58 1.44 3.30 0.3 35 9 0.90 〃 0.57 1.41 2.93 0.3 30 10 1.0 〃 0.54 1.33 2.71 0.3 25

【００１５】表１から明らかなように、Ｎｉ2+濃度が一
定でも反応温度を高くすることによって還元時間を短縮
でき、逆に反応温度が一定の場合、Ｎｉ2+濃度を高める
ことにより還元時間を短縮できる。また、還元時間が４
０分以内であれば、平均粒径が小さく粒度分布幅の狭い
ニッケル粉末が得られるが（試料番号１、４、６〜１
０）、還元時間が４０分より長くなると１次粒子の平均
粒径が約０.７μｍとなり、粒度分布の広い粉末となる
（試料番号２、３、５）。As is clear from Table 1, the reduction time can be shortened by increasing the reaction temperature even when the Ni 2+ concentration is constant. Conversely, when the reaction temperature is constant, the reduction time can be reduced by increasing the Ni 2+ concentration. Can be shortened. Also, the reduction time is 4
Within 0 minutes, nickel powder having a small average particle size and a narrow particle size distribution can be obtained (Sample Nos. 1, 4, 6 to 1).
0), when the reduction time is longer than 40 minutes, the average particle size of the primary particles becomes about 0.7 μm, and the powder has a wide particle size distribution (Sample Nos. 2, 3, 5).

【００１６】次に、各ニッケル粉末をエチルセルロース
系樹脂とテルピネオールを用いて導電ペーストを調製
し、１０μｍ厚のセラミックシート上に印刷して、１.
３μｍ厚の塗布膜を形成し試料を得た。各塗布膜の表面
荒さを求めるため、その表面に針を置き、この針を移動
させたときの針の上下移動幅を測定したところ、その平
均値は試料番号１、４、６〜１０のニッケル粉末を用い
た塗布膜ではそれぞれ１．６μｍであり、試料番号２、
３、５のニッケル粉末を用いたものではそれぞれ２．８
μｍであった。Next, a conductive paste was prepared from each nickel powder using ethylcellulose resin and terpineol, and printed on a ceramic sheet having a thickness of 10 μm.
A coating film having a thickness of 3 μm was formed to obtain a sample. In order to obtain the surface roughness of each coating film, a needle was placed on the surface, and the vertical movement width of the needle when the needle was moved was measured. The average value was nickel of sample numbers 1, 4, 6-10. The coating film using the powder has a thickness of 1.6 μm,
2.8 for each of 3 and 5 nickel powders
was μm.

【００１７】また、前記各試料をガラス板の上に置き、
下から光をあてて電子顕微鏡で光の透過写真をとったと
ころ、試料番号１、４、６〜１０のニッケル粉末を用い
たものでは、光の漏れの無い良質な印刷膜が得られた
が、試料番号２、３、５のニッケル粉末を用いたもので
は光の透過が観察され、塗布膜にピンホールが認められ
た。Further, each sample is placed on a glass plate,
When a transmission photograph of light was taken with an electron microscope by shining light from the bottom, a good quality printed film without light leakage was obtained with the nickel powders of sample numbers 1, 4, 6-10. In the sample Nos. 2, 3, and 5 using the nickel powder, light transmission was observed, and pinholes were observed in the coating film.

【００１８】[0018]

【発明の効果】以上説明したように、本発明は、ニッケ
ル錯塩を強アルカリ下で還元し、液相反応によりニッケ
ル粉末を製造するようにしたので、分散性が良く、粒径
が小さく粒度分布幅の極めて狭いニッケル微粉末を得る
ことができ、特性の劣化がなく、低価格で小型大容量の
セラミック積層コンデンサを製造することができる。As described above, according to the present invention, the nickel complex salt is reduced in a strong alkali to produce the nickel powder by the liquid phase reaction. Therefore, the dispersibility is good, the particle size is small, and the particle size distribution is small. It is possible to obtain a nickel fine powder having an extremely narrow width, without deterioration of characteristics, and to manufacture a small-sized and large-capacity ceramic laminated capacitor at low cost.

Claims (5)

【特許請求の範囲】[Claims] 【請求項１】 水溶性ニッケル(II)塩の水溶液に強アル
カリを加えて水酸化ニッケル(II)を生成させ、該水酸化
ニッケル(II)を強アルカリ下にて還元剤で還元すること
を特徴とするニッケル微粉末の製造方法。1. A strong alkali is added to an aqueous solution of a water-soluble nickel (II) salt to form nickel (II) hydroxide, and the nickel (II) hydroxide is reduced with a reducing agent in a strong alkali. A method for producing a fine nickel powder characterized by the above. 【請求項２】 前記還元剤がヒドラジン又はヒドラジン
水化物である請求項１に記載の方法。2. The method according to claim 1, wherein the reducing agent is hydrazine or hydrazine hydrate. 【請求項３】 還元をｐＨ１０〜１４の強アルカリ下で
行う請求項１又は２に記載の方法。3. The method according to claim 1, wherein the reduction is carried out in a strong alkali having a pH of 10-14. 【請求項４】 還元を温度５５〜７０℃、ニッケルイオ
ン濃度２.０mol／ｌ以下の条件下で行う請求項１〜３の
いずれか一に記載の方法。4. The method according to claim 1, wherein the reduction is carried out under conditions of a temperature of 55 to 70 ° C. and a nickel ion concentration of 2.0 mol / l or less. 【請求項５】 還元を４０分以内に完了するように温度
及びニッケルイオン濃度を調節する請求項１〜４のいず
れか一に記載の方法。5. The method according to claim 1, wherein the temperature and the nickel ion concentration are adjusted so that the reduction is completed within 40 minutes.
JP3207872A 1991-08-20 1991-08-20 Method for producing nickel fine powder Expired - Lifetime JP2900650B2 (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6120576A (en) * 1997-09-11 2000-09-19 Mitsui Mining And Smelting Co., Ltd. Method for preparing nickel fine powder
WO2001034327A1 (en) * 1999-11-10 2001-05-17 Mitsui Mining And Smelting Co., Ltd. Nickel powder, method for preparation thereof and conductive paste
WO2001036131A1 (en) * 1999-11-12 2001-05-25 Mitsui Mining And Smelting Co., Ltd. Nickel powder and conductive paste
KR100399716B1 (en) * 2001-06-07 2003-09-29 한국과학기술연구원 The Manufacturing Method Of Fine Powder Of Nickel
KR100415491B1 (en) * 1997-12-12 2004-01-31 미츠이 긴조쿠 고교 가부시키가이샤 Nickel fine powder and process for producing the same
JP2005248198A (en) * 2004-03-01 2005-09-15 Toho Titanium Co Ltd Nickel powder, and electrically conductive paste and laminated ceramic capacitor using the same
CN1299863C (en) * 2005-03-31 2007-02-14 上海交通大学 Method for preparing hollow or clad nickel alloy spherical powder
CN100402205C (en) * 2006-08-07 2008-07-16 黄德欢 Process for preparing nano-nickel powder
JP2010185112A (en) * 2009-02-12 2010-08-26 Noritake Co Ltd Nickel particulate and production method therefor
CN103464781A (en) * 2013-09-06 2013-12-25 浙江大学 Method of producing nickel microspheres
CN103706804A (en) * 2013-12-25 2014-04-09 南昌航空大学 Environment-friendly preparing method of nickel nanocrystalline
JP2018070941A (en) * 2016-10-27 2018-05-10 住友金属鉱山株式会社 Method for producing nickel powder

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6120576A (en) * 1997-09-11 2000-09-19 Mitsui Mining And Smelting Co., Ltd. Method for preparing nickel fine powder
KR100415491B1 (en) * 1997-12-12 2004-01-31 미츠이 긴조쿠 고교 가부시키가이샤 Nickel fine powder and process for producing the same
WO2001034327A1 (en) * 1999-11-10 2001-05-17 Mitsui Mining And Smelting Co., Ltd. Nickel powder, method for preparation thereof and conductive paste
WO2001036131A1 (en) * 1999-11-12 2001-05-25 Mitsui Mining And Smelting Co., Ltd. Nickel powder and conductive paste
KR100399716B1 (en) * 2001-06-07 2003-09-29 한국과학기술연구원 The Manufacturing Method Of Fine Powder Of Nickel
JP2005248198A (en) * 2004-03-01 2005-09-15 Toho Titanium Co Ltd Nickel powder, and electrically conductive paste and laminated ceramic capacitor using the same
CN1299863C (en) * 2005-03-31 2007-02-14 上海交通大学 Method for preparing hollow or clad nickel alloy spherical powder
CN100402205C (en) * 2006-08-07 2008-07-16 黄德欢 Process for preparing nano-nickel powder
JP2010185112A (en) * 2009-02-12 2010-08-26 Noritake Co Ltd Nickel particulate and production method therefor
CN103464781A (en) * 2013-09-06 2013-12-25 浙江大学 Method of producing nickel microspheres
CN103706804A (en) * 2013-12-25 2014-04-09 南昌航空大学 Environment-friendly preparing method of nickel nanocrystalline
JP2018070941A (en) * 2016-10-27 2018-05-10 住友金属鉱山株式会社 Method for producing nickel powder

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