JPH0474810A - Manufacture of nickel base metal fine powder - Google Patents
Manufacture of nickel base metal fine powderInfo
- Publication number
- JPH0474810A JPH0474810A JP18996290A JP18996290A JPH0474810A JP H0474810 A JPH0474810 A JP H0474810A JP 18996290 A JP18996290 A JP 18996290A JP 18996290 A JP18996290 A JP 18996290A JP H0474810 A JPH0474810 A JP H0474810A
- Authority
- JP
- Japan
- Prior art keywords
- particle shape
- reducing
- fine powder
- hydrazine
- metal fine
- 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
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 title description 2
- 239000010953 base metal Substances 0.000 title 1
- 239000002245 particle Substances 0.000 claims abstract description 13
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 150000002816 nickel compounds Chemical class 0.000 claims abstract description 4
- -1 boron compound hydride Chemical class 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910018054 Ni-Cu Inorganic materials 0.000 claims 1
- 229910018481 Ni—Cu Inorganic materials 0.000 claims 1
- 229910010277 boron hydride Inorganic materials 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000012798 spherical particle Substances 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 239000002904 solvent Substances 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- 150000004678 hydrides Chemical class 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 238000007885 magnetic separation Methods 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000012279 sodium borohydride Substances 0.000 description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
導伝性ペースト、電磁波シールド剤、電子回路リードフ
レーム用材料、粉末冶金、接合剤に利用できる。[Detailed Description of the Invention] [Industrial Application Fields] It can be used in conductive pastes, electromagnetic shielding agents, electronic circuit lead frame materials, powder metallurgy, and bonding agents.
［従来の技術］
水溶液系でニッケル化合物を次亜りん酸や水素化ほう素
ナトリウムなどの還元剤で還元する方法が知られている
が、この方法では粒子径７５を粗大になりやすく粒子−
形も不揃いで均一で高品質の製品が得られにくい、また
金属粒子と同時に水酸化物や酸化物が複製され、その分
離が龍しく純度の高い製品が得られにくい。[Prior Art] A method is known in which a nickel compound is reduced with a reducing agent such as hypophosphorous acid or sodium borohydride in an aqueous solution system.
The shape is irregular, making it difficult to obtain a uniform, high-quality product.Also, hydroxides and oxides are replicated at the same time as the metal particles, making it difficult to separate them, making it difficult to obtain a highly pure product.
［発明が解決しようとする課題］
本発明は、前項で述べたような従来法の欠点を克服する
為に遂行された６本法の特徴は、無水アルコール等の非
水溶媒系で還元速度の緩やかなヒドラジンを主還元剤に
して、還元を誘起させるために少量の還元力の強い水素
化ホウ素ナトリウムを用い２粒径２粒形の整ったサブミ
クロン粒子を製造可能にしたことにある０粒形制御剤と
して二価アルコールを添加することにより球形粒子を得
ることができる。さらに金属と水酸化物や酸化物を分離
する手段として電磁石を用いて電磁分離し。[Problems to be Solved by the Invention] The present invention is characterized by six methods carried out in order to overcome the drawbacks of the conventional methods as described in the previous section. Using mild hydrazine as the main reducing agent and a small amount of sodium borohydride with strong reducing power to induce reduction, it is possible to produce submicron particles with two particle sizes and two well-shaped particles. Spherical particles can be obtained by adding dihydric alcohol as a shape control agent. Furthermore, electromagnetic separation is performed using electromagnets as a means of separating metals from hydroxides and oxides.
高純度（９９％）の製品を得る方法を見いだした。We have found a way to obtain a product with high purity (99%).
［実施例］ 次に実施例によって２本発明をさらに詳細に説明する。[Example] Next, the present invention will be explained in more detail by way of examples.
実施例１
２００ｍ］のビーカーに１００ｍ１の無水メタノールを
太れ、これにＮ ｉ （ＮＯ３） ＝を飽和させた。Example 1 100 ml of anhydrous methanol was added to a 200 m beaker and saturated with N i (NO3) =.
その後エチレングリコールを添力１比な、マグネチック
スターラーで攪伴しながら５０ｍ１のヒドラジンを加え
た。その後少量の水素化ホウ素ナトリウム粉末を振りか
ける。攪伴を停止し暫くするとビーカーの上部から還元
反応が進行しやがて激しく反応が進み、水素とアンモニ
アガスを発生しながらビーカーの低部まで反応が進む、
熟成させて反応が終わった後ビーカーごと電磁石の上に
載せ電磁分離する。その後遠心分１ｉｌｌ器で同液分離
した。沈澱を冷凍乾燥器で乾燥させた。Thereafter, 50 ml of hydrazine was added with ethylene glycol added at a ratio of 1 while stirring with a magnetic stirrer. Then sprinkle a small amount of sodium borohydride powder. After stopping stirring for a while, the reduction reaction proceeds from the top of the beaker, and soon the reaction progresses violently, and the reaction progresses to the bottom of the beaker while generating hydrogen and ammonia gas.
After aging and reaction, the whole beaker is placed on an electromagnet for electromagnetic separation. Thereafter, the same liquid was separated using a centrifugal 1ill device. The precipitate was dried in a freeze dryer.
実施例２ Ｎｉ基合金微粉末の製造例を述べる。Example 2 An example of manufacturing Ni-based alloy fine powder will be described.
基本操作は実施例１で述べた方法と同じである。The basic operation is the same as the method described in Example 1.
所定の濃度比に成るように調整したＮｉ （ＮＯ３）
２とＣｕＮＯ３を無水メタノールに溶かした飽和溶液を
作り、その後の操作は実施例１で述べた通りの方法°誕
った。Ｎｉ−Ｐｄ、Ｎｉ−Ａｇ系の合金粉末も同様にし
て製造される。Ni (NO3) adjusted to a predetermined concentration ratio
A saturated solution of 2 and CuNO3 in anhydrous methanol was prepared, and the subsequent operations were as described in Example 1. Ni-Pd and Ni-Ag alloy powders are also produced in the same manner.
［発明の効果］ 本発明は、非水溶媒系で行う還元法であるので。[Effect of the invention] The present invention is a reduction method performed in a non-aqueous solvent system.
水分の影響を軽）威して物質の表面にコートする場合に
有効な方法である。たとえば、非酸化物系のセラミック
粉末を使う複合材ｆ↓、カーボン繊維の酸化防１のため
の表面処理、導電性を要求する材第１図は９本発明で作
られたニッケル粉末のＸ線回折図である。横軸は角度（
ＣｕＫα）、縦軸は強度である。This is an effective method for coating the surface of substances by reducing the influence of moisture. For example, composite materials f↓ that use non-oxide ceramic powder, surface treatment of carbon fiber to prevent oxidation, and materials that require electrical conductivity are shown in Figure 1. It is a diffraction diagram. The horizontal axis is the angle (
CuKα), and the vertical axis is the intensity.
第２図は、ニッケル粉末の粒度分布図である。FIG. 2 is a particle size distribution diagram of nickel powder.
第３図は、ニッケル粉末の粒子構造を示すＳＥＭ写真で
ある。FIG. 3 is a SEM photograph showing the particle structure of nickel powder.
指定代理人 工業技術院名古屋工業技術試験所長 富山朔太部 ン９ｕｃ。designated agent Director, Nagoya Industrial Technology Testing Institute, Agency of Industrial Science and Technology Toyama Sakuta N9uc.
トーーイ
／ＡＴＩ
手続補正書彷即
平成２年１１月２６日
１、事件の表示
平成２年特許顕第１８９９６２号
２、発明の名称
ニッケル基金属微粉末の製造法
３、補正をする者
事件との関係 特許出願人
住 所 東京都千代田区霞が関１丁目３番１号（１１
４）名 称 工業技術院長 杉 浦 賢４、指
定代理人TOI/ATI Procedural amendment immediately November 26, 1990 1. Indication of the case 1990 Patent Publication No. 189962 2. Name of the invention Method for producing nickel-based metal fine powder 3. Person making the amendment Related patent applicant address: 1-3-1 Kasumigaseki, Chiyoda-ku, Tokyo (11
4) Name Ken Sugiura, Director of the Agency of Industrial Science and Technology 4, Designated Agent
Claims (1)
形制御剤に二価アルコールを用いて、ニッケル化合物を
還元してＮｉ金属微粉末を製造する方法。 ２ 請求項１記載の方法で、Ｎｉ−Ｐｄ、Ｎｉ−Ａｇ、
Ｎｉ−Ｃｕ系の合金微粉末を製造する方法。[Scope of Claims] 1. A method for producing fine Ni metal powder by reducing a nickel compound using hydrazine and a boron hydride compound as chemical reducing agents and a dihydric alcohol as a particle shape control agent. 2. In the method according to claim 1, Ni-Pd, Ni-Ag,
A method for producing Ni-Cu based alloy fine powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18996290A JPH0474810A (en) | 1990-07-18 | 1990-07-18 | Manufacture of nickel base metal fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18996290A JPH0474810A (en) | 1990-07-18 | 1990-07-18 | Manufacture of nickel base metal fine powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0474810A true JPH0474810A (en) | 1992-03-10 |
Family
ID=16250105
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18996290A Pending JPH0474810A (en) | 1990-07-18 | 1990-07-18 | Manufacture of nickel base metal fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0474810A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0985474A3 (en) * | 1998-09-11 | 2000-03-29 | Murata Manufacturing Co., Ltd. | Metal powder, method for producing the same by reduction of metallic salt, and conductive pastes containing this metal powder |
| JP2008525640A (en) * | 2004-12-28 | 2008-07-17 | 成都▲開▼▲飛▼高能化学工▲業▼有限公司 | High tap density ultrafine spherical metallic nickel powder and wet manufacturing method thereof |
| CN100436008C (en) * | 2007-04-10 | 2008-11-26 | 北京科技大学 | Chemical production of metal nickel nano-line |
| JP2013253296A (en) * | 2012-06-07 | 2013-12-19 | Osaka Gas Co Ltd | Method for producing alloy particle |
| CN104289724A (en) * | 2014-09-15 | 2015-01-21 | 童东革 | Preparing method of sea-urchin-shaped amorphous Ni-B alloy nanometer materials |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63125605A (en) * | 1986-11-14 | 1988-05-28 | Daido Steel Co Ltd | Production of fine metal powder |
-
1990
- 1990-07-18 JP JP18996290A patent/JPH0474810A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63125605A (en) * | 1986-11-14 | 1988-05-28 | Daido Steel Co Ltd | Production of fine metal powder |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0985474A3 (en) * | 1998-09-11 | 2000-03-29 | Murata Manufacturing Co., Ltd. | Metal powder, method for producing the same by reduction of metallic salt, and conductive pastes containing this metal powder |
| US6156094A (en) * | 1998-09-11 | 2000-12-05 | Murata Manufacturing Co., Ltd. | Method for producing metal powder |
| JP2008525640A (en) * | 2004-12-28 | 2008-07-17 | 成都▲開▼▲飛▼高能化学工▲業▼有限公司 | High tap density ultrafine spherical metallic nickel powder and wet manufacturing method thereof |
| JP4837675B2 (en) * | 2004-12-28 | 2011-12-14 | 成都▲開▼▲飛▼高能化学工▲業▼有限公司 | High tap density ultrafine spherical metallic nickel powder and wet manufacturing method thereof |
| CN100436008C (en) * | 2007-04-10 | 2008-11-26 | 北京科技大学 | Chemical production of metal nickel nano-line |
| JP2013253296A (en) * | 2012-06-07 | 2013-12-19 | Osaka Gas Co Ltd | Method for producing alloy particle |
| CN104289724A (en) * | 2014-09-15 | 2015-01-21 | 童东革 | Preparing method of sea-urchin-shaped amorphous Ni-B alloy nanometer materials |
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