CN1586773A - Nano structure nickel powde and its preparing method - Google Patents
Nano structure nickel powde and its preparing method Download PDFInfo
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- CN1586773A CN1586773A CN 200410050999 CN200410050999A CN1586773A CN 1586773 A CN1586773 A CN 1586773A CN 200410050999 CN200410050999 CN 200410050999 CN 200410050999 A CN200410050999 A CN 200410050999A CN 1586773 A CN1586773 A CN 1586773A
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Abstract
The present invention provides one kind of nano structure nickel powder and its preparation process. The nano structure nickel powder is barbed spherical nickel powder with distributed barbs in nano size in the surface. The barbs have length adjustable in 20-800 nm and diameter adjustable in 10-200 nm, and nano structure nickel powder has average granularity adjustable in 50-3000 nm. The nano structure barbed spherical nickel powder with narrow size distribution is prepared through mixing the water solution of nickel salt and the water solution containing alkali, reductant, two kinds of surfactant, additive A and sodium dodecyl benzene sulfonate, reaction at 50-98 deg.c for 5-390 min, cooling, washing, and stoving.
Description
Technical field
The present invention relates to the nickel powder and the manufacture method thereof of nanostructured.
Background technology
Extra-fine nickel powder has good anticorrosive, catalytic performance and has very big specific area and bulk effect, can use more and more widely at aspects such as aerospace, electronics, chemical industry, metallurgy, military affairs as the catalyst of chemical engineering industry, magnetic recording material, electromagnetic shielding material, hydrogen storage material, conducting resinl or the like.Especially the metal dust of special appearance, its application aspect high-tech is more extensive.Because electronic structure depends on the state at interface, and particle morphology is a key factor that influences interfacial structure.Therefore, the preparation of the nano metal particles that the size pattern is controlled has been subjected to researchers' extensive attention.
The method of existing manufacturing metal nickel powder is a lot, as: mechanical crushing method, method for constructing, electrolysis, pulp High Pressure Hydrogen reducing process, liquid phase reduction or the like.Adopt the nickel powder of these method preparations, pattern is single, mostly is dendrite or near-spherical metal dust.Adopt hydrazine hydrate to make reducing agent and prepare extra-fine nickel powder, many patent documentations and non-patent literature report has been arranged.As the patent application 98124035.6 of Japanese Chengdu high-energy chemistry Industrial Co., Ltd, the patent application 99101538.X of China Science ﹠ Technology University, the patent application 02148673.5 of University of Science ﹠ Technology, Beijing, the patent application 01107728.X of Shandong University, patent application 01144702.8 of Beijing Non-Ferrous Metal Research General Academy etc., all reported the preparation method of nickel powder, the nickel powder of gained all is a near-spherical, and performances such as its electric conductivity, formability are good not enough in some application.
Summary of the invention
The purpose of this invention is to provide a kind of spherical superfine nano structure nickel powder and preparation method thereof that stings.
For reaching above-mentioned purpose, the feature of nanostructured nickel powder of the present invention is: the powder surface is covered with nanometer thorn-like structure, and the length of thorn is between 20nm～800nm, and the diameter of thorn is between 10nm～200nm, and the powder particle mean size is between 50nm～3 μ m.
The method for preparing above-mentioned nickel powder is as follows: in the normal temperature mechanical agitation or/and add under the condition of ultrasonic field, after the mixed aqueous solution that is added with alkali, reducing agent, surfactant additive A and neopelex and nickel salt aqueous solution mixed, 50 ℃～98 ℃ down reaction 5～390 minutes to solution become black, cooling, washing, oven dry get spherical nickel powder.
Described surfactant additive A is any in water soluble polymer polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), the polyethylene glycol (PEG), and mean molecule quantity is not less than 20,000, and concentration is 0.1～20g/L.
The concentration of described neopelex is 0.001～20g/L.
Described nickel salt is one or more the mixture in nickel chloride, nickelous sulfate, the nickel acetate, and nickel concentration is 0.05～0.6mol/L.
Described reducing agent is hydrazine or hydrazine hydrate, and its concentration is 2～10: 1 with the nickel ion concentration ratio.
Described alkali is any in NaOH, sodium carbonate, the sodium acetate, OH
-Concentration be 0.2～7mol/L.
The gained reduzate is with the washing that hockets of deionized water and acetone.
Dry in inert gas reduzate washing back.
Adopt the inventive method to produce nickel powder, technical process is simple, easy operating, and low production cost is suitable for suitability for industrialized production.Gained nickel powder particle size distribution range is narrow, and the surface has been covered with thorn, and the length of thorn is adjustable between 20 nanometer to 800 nanometers, and the diameter of thorn is adjustable in 10 nanometer to 200 nanometers, and particle mean size is adjustable between 50nm～3 μ m.
The metal prong of a large amount of nanoscales can be avoided the reunion between the powder effectively owing to distribute in the nickel powder surface; These nanometers thorn can very effectively play the high molecular effect of pinning again in macromolecule, overcome the common metal powder and add the problem that significantly reduces material mechanical performance behind the macromolecular material, significantly improves the mechanical property of material; Simultaneously the nanometer thorn has increased the junctor meeting between the powder, identical with the conduction and the heat conductivility that can improve material under the vermicelli spare.As seen, the spherical nanostructured nickel powder of the thorn of gained of the present invention can be used widely in more technical field.
Description of drawings
Fig. 1 is that the spherical nickel powder that embodiment 1 makes amplifies 20,000 times electron scanning micrograph.
Fig. 2 is that the spherical nickel powder that embodiment 2 makes amplifies 30,000 times electron scanning micrograph.
Fig. 3 is that the spherical nickel powder surface thorn that embodiment 2 makes amplifies 250,000 times perspective electron microscope photo.
The specific embodiment
Embodiment 1
At first prepare nickel chloride aqueous solution.Prepare the mixed aqueous solution that contains NaOH, hydrazine hydrate, polyvinylpyrrolidone (PVP) and neopelex again, in stirring at normal temperature and add under the situation of ultrasonic field two kinds of solution are evenly mixed in reaction vessel, guarantee that final nickel ion concentration is 0.05mol/L, naoh concentration is 0.4mol/L, hydrazine hydrate concentration is 0.4mol/L, PVP concentration is 0.1g/L, and neopelex concentration is 0.01g/L, is warmed up to 55 ℃ of reactions then.Mixing speed is 200 rev/mins, and the reaction time is 100 minutes.After reaction finishes, solution becomes black, through depositing and be cooled to normal temperature, with deionized water and acetone hocket the washing after, dry in nitrogen, obtain nanostructured spherical nickel powder as shown in Figure 1, the length of thorn is between 20nm～50nm, the diameter of thorn is between 10nm～50nm, and powder granularity is between 50nm～150nm.
Embodiment 2
At first prepare nickel chloride aqueous solution.Prepare the mixed aqueous solution that contains NaOH, hydrazine hydrate, polyvinyl alcohol (PVA) and neopelex again, in stirring at normal temperature and add under the situation of ultrasonic field two kinds of solution are evenly mixed in reaction vessel, guarantee that final nickel ion concentration is 0.6mol/L, naoh concentration is 0.5mol/L, hydrazine hydrate concentration is 6mol/L, and PVA concentration is 10g/L, and neopelex concentration is 1g/L, be warmed up to 90 ℃ of reactions after mixing, mixing speed is 200 rev/mins.Reaction time is 250 minutes.Reaction finishes after deposit, cool off, after deionized water, acetone washing, heat drying in nitrogen, obtain as Fig. 2, nanostructured spherical nickel powder shown in Figure 3, the length of thorn is between 150nm～800nm, the diameter of thorn is between 15nm～200nm, and the powder particle mean size is between 1 μ m～3 μ m.
Embodiment 3
At first prepare nickel chloride aqueous solution.Prepare the mixed aqueous solution that contains NaOH, hydrazine hydrate, polyethylene glycol (PEG) and neopelex again, under condition of stirring, two kinds of solution are evenly mixed in reaction vessel, guarantee that final nickel ion concentration is 0.1mol/L, naoh concentration is 7mol/L, hydrazine concentration is 0.5mol/L, and PEG concentration is 4g/L, and neopelex concentration is 0.3g/L, be warmed up to 70 ℃ of reactions after mixing, mixing speed is 200 rev/mins.Reaction time is 50 minutes.React end after deposit, after alternately washing with deionized water and acetone, heat drying in argon gas, obtain the nanostructured spherical nickel powder, the length of thorn is between 50nm～100nm, and the diameter of thorn is between 50nm～100nm, and the powder particle mean size is between 120nm～300nm.
Embodiment 4
At first prepare nickel sulfate solution.Prepare the mixed aqueous solution that contains sodium carbonate, hydrazine hydrate, polyvinylpyrrolidone (PVP) and neopelex again, two kinds of solution are evenly mixed in reaction vessel adding under the situation of ultrasonic field, guarantee that final nickel ion concentration is 0.3mol/L, OH
-Concentration is 0.5mol/L, and hydrazine hydrate concentration is 0.6mol/L, and PVP concentration is 0.4g/L, and neopelex concentration is 0.001g/L, is warmed up to 98 ℃ of reactions then.Reaction time is 5 minutes, and mixing speed is 200 rev/mins.Reaction finishes after deposition and cooling, with deionized water and acetone alternately after the washing, and heat drying under inert gas, obtain the nanostructured spherical nickel powder, the length of thorn is between 30nm～60nm, and the diameter of thorn is between 50nm～100nm, and the powder particle mean size is between 80nm～150nm.
Embodiment 5
At first prepare nickel acetate aqueous solution.Prepare the mixed aqueous solution that contains sodium acetate, hydrazine hydrate, polyvinylpyrrolidone (PVP) and neopelex again, under condition of stirring, two kinds of solution are evenly mixed in reaction vessel, guarantee that final nickel ion concentration is 0.1mol/L, OH
-Concentration is 0.2ml/L, and hydrazine hydrate concentration is 0.5mol/L, and PVP concentration is 20g/L, and neopelex concentration is 20g/L, is warmed up to 50 ℃ of reactions then.Reaction time is 390 minutes, and mixing speed is 200 rev/mins.Reaction finishes after the deposition cooling, with deionized water and acetone alternately after the washing, and heat drying in nitrogen, obtain the nanostructured spherical nickel powder, the length of thorn is between 200nm～500nm, and the diameter of thorn is between 100nm～200nm, and the powder particle mean size is between 500nm～1.5 μ m.
Claims (9)
1, a kind of nanostructured nickel powder is characterized in that: the powder surface is covered with nanometer thorn-like structure, and the length of thorn is between 20nm～800nm, and the diameter of thorn is between 10nm～200nm, and the powder particle mean size is between 50nm～3 μ m.
2, a kind of method for preparing the described nanostructured nickel powder of claim 1, it is characterized in that: in the normal temperature mechanical agitation or/and add under the ultrasonic field condition, after the mixed aqueous solution that is added with alkali, reducing agent, surfactant additive A and neopelex and nickel salt aqueous solution mixed, 50 ℃～98 ℃ down reaction 5～390 minutes to solution become black, cooling, washing, oven dry get spherical nickel powder.
3, method according to claim 2, it is characterized in that: described surfactant additive A is that mean molecule quantity is not less than any in 20,000 water soluble polymer polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), the polyethylene glycol (PEG), and concentration is 0.1～20g/L.
4, method according to claim 2 is characterized in that: the concentration of described neopelex is 0.001～20g/L.
5, method according to claim 2 is characterized in that: described nickel salt is one or more the mixture in nickel chloride, nickelous sulfate, the nickel acetate, and the content of nickel ion is 0.05～0.6mol/L.
6, method according to claim 2 is characterized in that: described reducing agent is hydrazine or hydrazine hydrate, and its concentration and nickel ion concentration are than 2～10: 1.
7, method according to claim 2 is characterized in that: described alkali is any in NaOH, sodium carbonate, the sodium acetate, OH
-Concentration be 0.2～7mol/L.
8, according to each described method in the claim 2 to 7, it is characterized in that: reduzate is with the washing that hockets of deionized water and acetone.
9, according to each described method in the claim 2 to 7, it is characterized in that: dry in inert gas reduzate washing back.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431750C (en) * | 2005-12-30 | 2008-11-12 | 中山大学 | Liquid phase preparation process of nano nickle powder |
| CN100448574C (en) * | 2005-09-29 | 2009-01-07 | 江苏大学 | Method for preparing nano nickel |
| CN100450676C (en) * | 2006-03-09 | 2009-01-14 | 兰州大学 | Method for preparing nano nickel powder in emulsion system |
| CN102554259A (en) * | 2012-02-07 | 2012-07-11 | 宇辰新能源材料科技无锡有限公司 | Method for preparing spherical submicron nickel powder with controllable particle size |
| CN102728851A (en) * | 2012-06-26 | 2012-10-17 | 湖南省娄底维亚科技有限公司 | Preparation method of hexagonal phase-containing nano nickel powder |
| CN102837003A (en) * | 2012-09-07 | 2012-12-26 | 中国科学院深圳先进技术研究院 | Nano silver particles with multilevel structure and preparation method thereof |
| CN105018029A (en) * | 2014-04-25 | 2015-11-04 | 南京理工大学 | Metallic nickel/graphene composite wave-absorbing material and preparation method thereof |
| CN108311710A (en) * | 2018-02-28 | 2018-07-24 | 深圳市航天新材科技有限公司 | A kind of preparation method of the anti-oxidant nanoscale nickel powder of monodisperse |
| CN110947979A (en) * | 2019-11-08 | 2020-04-03 | 上海交通大学 | Method for synthesizing superfine single crystal nickel powder by solvothermal method |
| CN115740437A (en) * | 2022-11-23 | 2023-03-07 | 哈尔滨师范大学 | Universal Ni @ C core-shell structure and preparation method and application thereof |
-
2004
- 2004-08-06 CN CN 200410050999 patent/CN1273251C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100448574C (en) * | 2005-09-29 | 2009-01-07 | 江苏大学 | Method for preparing nano nickel |
| CN100431750C (en) * | 2005-12-30 | 2008-11-12 | 中山大学 | Liquid phase preparation process of nano nickle powder |
| CN100450676C (en) * | 2006-03-09 | 2009-01-14 | 兰州大学 | Method for preparing nano nickel powder in emulsion system |
| CN102554259B (en) * | 2012-02-07 | 2015-03-18 | 宇辰新能源材料科技无锡有限公司 | Method for preparing spherical submicron nickel powder with controllable particle size |
| CN102554259A (en) * | 2012-02-07 | 2012-07-11 | 宇辰新能源材料科技无锡有限公司 | Method for preparing spherical submicron nickel powder with controllable particle size |
| CN102728851A (en) * | 2012-06-26 | 2012-10-17 | 湖南省娄底维亚科技有限公司 | Preparation method of hexagonal phase-containing nano nickel powder |
| CN102728851B (en) * | 2012-06-26 | 2015-07-08 | 湖南省娄底维亚科技有限公司 | Preparation method of hexagonal phase-containing nano nickel powder |
| CN102837003A (en) * | 2012-09-07 | 2012-12-26 | 中国科学院深圳先进技术研究院 | Nano silver particles with multilevel structure and preparation method thereof |
| CN105018029A (en) * | 2014-04-25 | 2015-11-04 | 南京理工大学 | Metallic nickel/graphene composite wave-absorbing material and preparation method thereof |
| CN108311710A (en) * | 2018-02-28 | 2018-07-24 | 深圳市航天新材科技有限公司 | A kind of preparation method of the anti-oxidant nanoscale nickel powder of monodisperse |
| CN110947979A (en) * | 2019-11-08 | 2020-04-03 | 上海交通大学 | Method for synthesizing superfine single crystal nickel powder by solvothermal method |
| CN110947979B (en) * | 2019-11-08 | 2021-10-15 | 上海交通大学 | Method for synthesizing superfine single crystal nickel powder by solvothermal method |
| CN115740437A (en) * | 2022-11-23 | 2023-03-07 | 哈尔滨师范大学 | Universal Ni @ C core-shell structure and preparation method and application thereof |
| CN115740437B (en) * | 2022-11-23 | 2023-12-05 | 哈尔滨师范大学 | Universal Ni@C core-shell structure and preparation method and application thereof |
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