CN1765550A - Preparation method of ultra-fine nickel powder - Google Patents
Preparation method of ultra-fine nickel powder Download PDFInfo
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- CN1765550A CN1765550A CN 200510101300 CN200510101300A CN1765550A CN 1765550 A CN1765550 A CN 1765550A CN 200510101300 CN200510101300 CN 200510101300 CN 200510101300 A CN200510101300 A CN 200510101300A CN 1765550 A CN1765550 A CN 1765550A
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Abstract
The invention relates to a method for preparing the ultra-fine nickel powder. The invention firstly mixes the solution of soluble nickel slat in the temperature of 20-80 Deg. C to be added the oxalic acid or ammonium oxalate precipitating agent whose concentration is 100-200 g/l and mol rate between oxalic acid or ammonium and nickel ion is 1.5-5 to be deposited, washed, filtered, and dried to attain the oxalic nickel powder; processes thermal decomposition on the solution at the vacuum degree of 0.2Pa-0.001MPa, the temperature of 200-600 Deg. C to keep warm for 0.5-5 hours to be added inactive gas for deactivation and attain ultra-fine nickel powder. The invention can prepare ultra-fine nickel powder with oxalic acid directly without non-oxide gas.
Description
Technical field
The present invention relates to a kind of preparation technology of submicron particle, relate in particular to a kind of preparation method of extra-fine nickel powder.
Background technology
Extra-fine nickel powder typically refers to particle diameter less than 1 micron nickel powder, has the physicochemical properties of a series of uniquenesses such as great skin effect and bulk effect because of it, all has wide practical use in many fields such as catalyst, battery material and carbide alloy binding agents.In recent years, because the fast development of mobile phone, laptop computer, computer and other telecommunication equipment, constantly rose to the demand of extra-fine nickel powder in market.
At present, a large amount of work has been carried out in the preparation of extra-fine nickel powder both at home and abroad, its main method is: evaporation-condensation method, reducing process, electrolysis, hydroxyl nickel thermal decomposition method etc.The nickel powder of this method of evaporation-condensation method preparation has advantages such as good sphericity, oxidation resistance are strong, but to the requirement height of equipment, the cost height of product costs an arm and a leg.The advantage of reducing process method is: preparation cost is very low, and equipment is simple and less demanding, and reaction is control easily, and the technological parameter that can control in the course of reaction is controlled crystalline form and particle size, but the oxidation resistance of the metal dust that this method makes is poor.The particle preparation of electrolysis and surperficial coating can be finished synchronously, particle purity height, and granularity is neat, but particle size is bigger.The nickel powder specific area of hydroxyl nickel thermal decomposition method is big, and it is good to be used as catalyst effect in battery material, but this method is because decomposition reaction is to carry out in the pyrolysis tower, along with temperature raises, the easy sintering of particle together, hydroxyl nickel is extremely toxic substance in addition, causes environmental pollution easily.
Chinese patent CN1600479A discloses a kind of method that adopts nickel oxalate thermal decomposition under nonoxidizing atmosphere to prepare fibrous nickel powder, and nonoxidizing atmosphere comprises that hydrogen, hydrogen add inert gas and pure inert gas.Because this method needs spent gas, has increased production cost.
Summary of the invention
The object of the present invention is to provide a kind of non-oxidized gas that do not need, directly prepare the method for extra-fine nickel powder preparation by nickel oxalate.
Extra-fine nickel powder preparation method of the present invention is as follows:
Soluble nickel salt is mixed with the aqueous solution that nickel ion concentration is 0.1～1.2mol/L, the control temperature is 20～80 ℃, stir down, mol ratio by oxalic acid or ammonium oxalate precipitating reagent and nickel ion is 1.5～5, adding concentration is oxalic acid or the ammonium oxalate precipitating reagent of 100～200g/L, precipitate, washing, filtration, drying precipitated, obtain the nickel oxalate powder, at vacuum 0.2Pa～0.001MPa, 200～600 ℃ of following thermal decompositions of temperature are incubated 0.5～5 hour, feed the inert gas passivation then, make extra-fine nickel powder.
Above-mentioned soluble nickel salt comprises nickelous sulfate, nickel nitrate, nickel acetate or nickel chloride.
The present invention is characterised in that nickel oxalate is carried out thermal decomposition under vacuum condition, because oxidizing atmosphere is low under the vacuum condition, so do not need nonoxidizing atmosphere can directly make nickel powder.To decompose the mechanism make nickel powder may be nickel oxalate when the vacuum thermal decomposition by direct heat, produces gases such as carbon monoxide, forms weak reducing atmosphere, and nickel ion is reduced.In addition, because the activity of nickel metal is not strong, easily reduces and be difficult for due to the oxidation.
The specific embodiment
Embodiment 1
Be made into the aqueous solution of nickel ion 0.15mol/L with nickelous sulfate, pH is about 5.1, adds in the reactor, the control temperature is 60 ℃, is 2.0 by oxalic acid and nickel ion mol ratio, under agitation adds the oxalic acid that concentration is 120g/L, get the nickel oxalate precipitation, washing, filtration, drying are put into vacuum drying oven with dried nickel oxalate, and the control temperature is 260 ℃, in vacuum is to carry out thermal decomposition under the 0.001MPa, be incubated 2 hours, feed the argon gas body then and carry out passivation, making granularity is 0.6 μ m, specific area 10m
2The extra-fine nickel powder of/g.Fig. 1 is the SEM figure of extra-fine nickel powder; Fig. 2 is the XRD figure of extra-fine nickel powder.
Embodiment 2
Be made into the aqueous solution of nickel ion 0.35mol/L with nickel nitrate, pH is about 3.2, adds in the reactor, the control temperature is 30 ℃, is 2.5 by ammonium oxalate and nickel ion mol ratio, under agitation adds the ammonium oxalate that concentration is 150g/L, get the nickel oxalate precipitation, washing, filtration, drying are put into vacuum drying oven with dried nickel oxalate, and the control temperature is 350 ℃, in vacuum is to carry out thermal decomposition under the 100Pa, be incubated 3 hours, feed the argon gas body then and carry out passivation, making granularity is 0.8 μ m, specific area 6m
2The extra-fine nickel powder of/g.
Be made into the aqueous solution of nickel ion 0.45mol/L with nickelous sulfate, pH is about 5.3, adds in the reactor, the control temperature is 60 ℃, is 1.8 by oxalic acid and nickel ion mol ratio, under agitation adds the oxalic acid that concentration is 100g/L, get the nickel oxalate precipitation, washing, filtration, drying are put into vacuum drying oven with dried nickel oxalate, and the control temperature is 600 ℃, in vacuum is to carry out thermal decomposition under the 10Pa, be incubated 2 hours, feed nitrogen then and carry out passivation, making granularity is 1.0 μ m, specific area 2.3m
2The extra-fine nickel powder of/g.
Claims (1)
1. the preparation method of an extra-fine nickel powder, it is characterized in that soluble nickel salt is mixed with the aqueous solution that nickel ion concentration is 0.1～1.2mol/L, the control temperature is 20～80 ℃, stir down, mol ratio by oxalic acid or ammonium oxalate precipitating reagent and nickel ion is 1.5～5, adding concentration is oxalic acid or the ammonium oxalate precipitating reagent of 100～200g/L, precipitate, washing, filter, drying precipitated, obtain the nickel oxalate powder, at vacuum 0.2Pa～0.001MPa, 200～600 ℃ of following thermal decompositions of temperature, be incubated 0.5～5 hour, feed the inert gas passivation then, make extra-fine nickel powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510101300XA CN100387383C (en) | 2005-11-17 | 2005-11-17 | Preparation method of ultra-fine nickel powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510101300XA CN100387383C (en) | 2005-11-17 | 2005-11-17 | Preparation method of ultra-fine nickel powder |
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| CN1765550A true CN1765550A (en) | 2006-05-03 |
| CN100387383C CN100387383C (en) | 2008-05-14 |
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| CNB200510101300XA Expired - Fee Related CN100387383C (en) | 2005-11-17 | 2005-11-17 | Preparation method of ultra-fine nickel powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402205C (en) * | 2006-08-07 | 2008-07-16 | 黄德欢 | Process for preparing nano-nickel powder |
| CN101200424B (en) * | 2006-12-14 | 2010-04-14 | 中南大学 | Oxalate monodisperse ultra-fine powder and preparation method thereof |
| CN102531880A (en) * | 2012-01-04 | 2012-07-04 | 金川集团有限公司 | Preparation method of spherical nickel oxalate |
| CN102728853A (en) * | 2012-06-11 | 2012-10-17 | 仇晓丰 | Production technique for high-purity nanoscale metal magnesium powder |
| CN108550836A (en) * | 2018-06-02 | 2018-09-18 | 湖南科技大学 | A kind of preparation method of lithium ion battery Ni/LiF composite positive poles |
| CN108907229A (en) * | 2018-07-24 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of ellipsoid porous hollow nickel powder |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1195332C (en) * | 2002-02-04 | 2005-03-30 | 河南环宇集团有限公司 | Making process and product of sintered cadmium negative pole for cell |
| CN1206070C (en) * | 2002-10-22 | 2005-06-15 | 中南大学 | Process for preparing fibrous nickel powder |
-
2005
- 2005-11-17 CN CNB200510101300XA patent/CN100387383C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100402205C (en) * | 2006-08-07 | 2008-07-16 | 黄德欢 | Process for preparing nano-nickel powder |
| CN101200424B (en) * | 2006-12-14 | 2010-04-14 | 中南大学 | Oxalate monodisperse ultra-fine powder and preparation method thereof |
| CN102531880A (en) * | 2012-01-04 | 2012-07-04 | 金川集团有限公司 | Preparation method of spherical nickel oxalate |
| CN102728853A (en) * | 2012-06-11 | 2012-10-17 | 仇晓丰 | Production technique for high-purity nanoscale metal magnesium powder |
| CN102728853B (en) * | 2012-06-11 | 2014-11-05 | 仇晓丰 | Production technique for high-purity nanoscale metal magnesium powder |
| CN108550836A (en) * | 2018-06-02 | 2018-09-18 | 湖南科技大学 | A kind of preparation method of lithium ion battery Ni/LiF composite positive poles |
| CN108907229A (en) * | 2018-07-24 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of ellipsoid porous hollow nickel powder |
| CN108907229B (en) * | 2018-07-24 | 2021-08-27 | 安徽工业大学 | Preparation method of ellipsoidal porous hollow nickel powder |
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| CN100387383C (en) | 2008-05-14 |
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Owner name: ZHEJIANG SHENZHOU PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: GUANGZHOU RESEARCH INST. OF NON-FERROUS METALS Effective date: 20120411 |
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Effective date of registration: 20120411 Address after: 317300, Taizhou City, Zhejiang province Xianju County Chengguan wearing No. 14 South Road Patentee after: Zhejiang Shenzhou Pharmaceutical Co.,Ltd. Address before: 510651 Changxin Road, Guangzhou, Guangdong, No. 363, No. Patentee before: Guangzhou Research Institute of Non-ferrous Metals |
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