CN1319685C - Production for nanometer nickel powder - Google Patents
Production for nanometer nickel powder Download PDFInfo
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- CN1319685C CN1319685C CNB2005100381019A CN200510038101A CN1319685C CN 1319685 C CN1319685 C CN 1319685C CN B2005100381019 A CNB2005100381019 A CN B2005100381019A CN 200510038101 A CN200510038101 A CN 200510038101A CN 1319685 C CN1319685 C CN 1319685C
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 74
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 69
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 claims abstract description 27
- 239000002184 metal Substances 0.000 claims abstract description 27
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 23
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 235000011837 pasties Nutrition 0.000 claims abstract description 17
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 15
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 claims description 6
- XGZRAKBCYZIBKP-UHFFFAOYSA-L disodium;dihydroxide Chemical compound [OH-].[OH-].[Na+].[Na+] XGZRAKBCYZIBKP-UHFFFAOYSA-L 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 150000002815 nickel Chemical class 0.000 abstract description 10
- 229910052759 nickel Inorganic materials 0.000 abstract description 8
- 230000009467 reduction Effects 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 41
- 239000012153 distilled water Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 229910001453 nickel ion Inorganic materials 0.000 description 8
- 230000018044 dehydration Effects 0.000 description 7
- 238000006297 dehydration reaction Methods 0.000 description 7
- 238000006073 displacement reaction Methods 0.000 description 7
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 7
- 238000006722 reduction reaction Methods 0.000 description 6
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 241000080590 Niso Species 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001868 cobalt Chemical class 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- -1 this Chemical class 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The present invention provides a method for preparing nanometer metal nickel powder. The present invention is characterized in that a small amount of sodium borohydride solution is added into an alcohol water solution of nickel chloride, induced reaction is generated, and sodium hydroxide and hydrazine hydrate pasty mixtures are added; after reaction, products can be made into nanometer nickel powder after being separated, washed and dried. The quality of sodium borohydride is 0.2/1000 to 1% of the quality of nickel salts, the quality of the sodium hydroxide is 0.5 to 2 times of the quality of the nickel salts, and the amount of hydrazine hydrate substances is 1.5 to 4.8 times of the amount of nickel salt substances. The present invention has the advantages that the purity of the obtained nanometer nickel powder is high; the percentage content of nickel quality is larger than 98%; the grain diameters of the products are homogeneous and controllable, and BET specific surface area which is high can achieve 129m<2>/g; equipment and technology are simple, reaction is rapid and efficient, reaction at room temperature does not need heating, and the percent reduction of the nickel is larger than 99.7%; raw materials are cheap in price and are easily obtained, and the dosages of hydrazine hydrate and the sodium hydroxide are few.
Description
One. technical field
The present invention relates to the preparation method of nano metal nickel powder, belong to field of nanometer technology.
Two. background technology
Characteristics are widely used in aspects such as catalyst, electrocondution slurry, sintering activator, battery, carbide alloy to nano-nickel powder because particle is little, specific area is big, reactivity is high, electric conductivity and thermal conductivity are good etc.The main method of preparation nano-nickel powder has at present: carbonyl nickel thermal decomposition method, evaporation-condensation method, alloyage, gas reduction method, electrolysis, mechanical crushing method and liquid phase reduction.Liquid phase reduction in these methods is easy to get, forms advantages such as being easy to control, little, the controllable granularity of product particle diameter owing to have raw material, becomes the important synthetic method of preparation nano-nickel powder one class.In the method, often select for use hydrazine as reducing agent.
CN 1302709A has announced a kind of preparation method of nm-class Ni powder, and feature is the ratio N according to amount of substance
2H
4H
2O: X: NiSO
46H
2O=(1.5~2.5): (0.75~1): 1 ratio, get N respectively
2H
4H
2O, X, NiSO
46H
2Three kinds of raw materials of O, wherein X is KOH, any one or two kinds of mixtures with arbitrary proportion among the NaOH are then with NiSO
46H
2O adds distilled water and is made into the aqueous solution and fully stirs adding N
2H
4H
2O fully stirs, and obtains mixed system A, then with the X wiring solution-forming and join among the system A, be heated to 56~99 ℃, and be incubated 10~120 minutes, and stir simultaneously, product.This method reaction needed heating, gained nickel powder granularity is 30~100 nanometers.
CN 1261565A has announced the preparation method of a kind of nanometre metal cobalt powder or nickel powder, and feature is with cobalt salt (CoCl
26H
2O or CoSO
47H
2O) or nickel salt (NiCl
26H
2O) weight 2-5 NaOH doubly joins in the solution of the hydrazine hydrate of amount of substance more than 3 times of cobalt or nickel ion, alcohol-water solution with cobalt salt or nickel salt mixes again, reaction is carried out automatically, be generally and finished in 15-60 minute, the nano-cobalt powder that makes and the granule size of nickel powder are followed successively by 30-40 nanometer and<15 nanometers.The NaOH that this method is required and the amount of hydrazine hydrate are all more.
CN 1426865A has announced a kind of method for preparing nano metal nickel powder, feature is the aqueous solution that nickelous sulfate is made into 0.2-1.0mol/L, and be warming up to 50~80 ℃, and add the hydrazine hydrate aqueous solution that contains 2-5 weight ‰ potassium borohydride then, can get nano-nickel powder after the reaction.It is 8-10 that nickel sulfate solution that this method is joined needs to regulate pH value with ammoniacal liquor and dilute sulfuric acid, and will add dispersant (which kind of dispersant undeclared in the specification is), operate more loaded down with trivial detailsly, and reaction needs heat, and the nickel powder particle diameter distribution that makes is less than 100 nanometers.
CN 1552548A has announced a kind of microwave activation-aqueous solution reducing process and has prepared the method for nano-nickel powder, and feature is earlier with nickelous sulfate (NiSO
46H
2O) water-soluble, add NaOH and hydrazine solution then successively, the reduced nickel ion makes nano-nickel powder under the condition of heating using microwave.This method reaction needs to carry out under heating using microwave, and gained nickel powder average grain diameter is less than 100 nanometers.
Three. summary of the invention
The purpose of this invention is to provide a kind of fast and convenient, prepare the method for small particle diameter, high-ratio surface nano-nickel powder at normal temperatures.
Technical scheme of the present invention is as follows:
A kind of preparation method of nano metal nickel powder, it is that a spot of sodium borohydride solution is added in the alcohol solution of nickel salt, induced reaction takes place, again NaOH and hydrazine hydrate pasty mixture are joined in the above-mentioned solution fast, stir reaction down, after the reaction, product can make nano-nickel powder through separation, washing, drying.
Among the preparation method of above-mentioned nano metal nickel powder, used nickel salt is NiCl
26H
2O.
Among the preparation method of above-mentioned nano metal nickel powder, the quality (W of used sodium borohydride
NaBH4) be six water nickel chloride quality (W
NiCl26H2O) 0.2 ‰-1.6 ‰.
Among the preparation method of above-mentioned nano metal nickel powder, the quality (W of used NaOH
NaOH) with the ratio of six water nickel chloride quality be 0.5: 1-2: 1.
Among the preparation method of above-mentioned nano metal nickel powder, the amount of substance (M of used hydrazine hydrate
N2H4H2O) with the amount (M of six water nickel chlorides
NiCl26H2O) ratio be=1.5: 1-4.8: 1.
Among the preparation method of above-mentioned nano metal nickel powder, the concentration of alcohol of used alcohol solution is 95%.
Technical solution of the present invention is compared with the method for preparing nano metal nickel powder of CN 1426865A bulletin, all uses minor N aBH
4Or KBH
4As the initator of hydrazine hydrate reduction nickel ion reaction, to overcome the slow-footed defective of the independent reduced nickel ionic reaction of hydrazine hydrate.This is because NaBH
4(or KBH
4) be strong reductant, can nickel ion be reduced to metallic nickel with nickel ion reaction at normal temperatures, and the tiny nickel particles that generates thus there is catalytic action to the reaction of hydrazine hydrate and nickel ion.On the other hand, the method for preparing nano metal nickel powder of the inventive method and CN 1426865A bulletin is compared, and has technically done following improvement: the present invention is earlier with minor N aBH
4Reduction reaction takes place in the alcohol solution of adding nickel salt, make a spot of nickel ion be reduced to tiny metallic nickel particle, be distributed in the alcohol solution of nickel salt, like this, add the alcohol solution of this nickel salt when the reducing agent hydrazine hydrate after, under the catalysis of existing little metal nickel particles, in lower temperature (room temperature), hydrazine hydrate can carry out fast and equably to the reduction of nickel ion, the nano metal nickel powder particle diameter that obtains thus is tiny, even, specific area is big, and can significantly reduce the consumption of NaOH and hydrazine hydrate.
Four. description of drawings
Fig. 1 is the XRD spectra of the nano-nickel powder of embodiment 1 sample of the inventive method preparation.
Fig. 2 is the TEM photo of the nano-nickel powder of embodiment 1 sample of the inventive method preparation, and particle size is the 20-30 nanometer.
Five. the specific embodiment
The invention will be further described with following embodiment:
Embodiment 1
Press W
NaOH: W
NiCl26H2O=2: 1; M
N2H4H2O: M
NiCl26H2O=4.8: 1; W
NaBH4: W
NiCl26H2O=1.6 ‰: 1.With 4.2g NiCl
26H
2O is dissolved in the ethanol water of 15.8ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 8.4g NaOH is joined the 8.5ml mass percent, stirs into pasty mixture B; With 0.3351g NaBH
4Be dissolved in (the NaBH among following each embodiment of wiring solution-forming C in the 10ml distilled water
4Solution concentration is all identical with this example).Get 0.2mlNaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
Analyze residual Ni in the filtrate with atomic absorption spectrophotometer
2+, find 99.7% Ni
2+Be reduced to Ni
0With X-ray diffraction (XRD), electronic transmission Electronic Speculum (TEM), BET specific area measuring the nano metal nickel powder that obtains is characterized.XRD figure has only the diffraction maximum of metallic nickel to exist, and shows that powder is a crystalline state nickel, is face-centred cubic structure; Transmission electron microscope photo shows that sample is made up of the granule of many almost sphericals; The BET specific area is 31m
2/ g, according to the computing formula of D (average grain diameter):
D=(6/ ρ
NiS) * 10
3Nm, S-BET specific area in the formula, m
2/ g; ρ
NiThe density of-nickel, 8.9g/cm
3, obtain: D is about 22nm.Below the D value of each embodiment sample, all computing formula is obtained according to this.
Embodiment 2
Press W
NaOH: W
NiCl26H2O=1.1: 1; M
N2H4H2O: M
NiCl26H2O=1.9: 1; W
NaBH4: W
NiCl26H2O=0.8 ‰: 1.With 4.2g NiCl
26H
2O is dissolved in the ethanol water of 13.6ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 4.5g NaOH is joined the 3.4ml mass percent, stirs into pasty mixture B.Get 0.1ml NaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
The BET specific area is 129m
2/ g, D is about 6nm.
Embodiment 3
Press W
NaOH: W
NiCl26H2O=2: 1; M
N2H4H2O: M
NiCl26H2O=4.8: 1; W
NaBH4: W
NiCl26H2O=0.8 ‰: 1.With 4.2g NiCl
26H
2O is dissolved in the ethanol water of 15.8ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 8.4g NaOH is joined the 8.5ml mass percent, stirs into pasty mixture B.Get 0.1ml NaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
The BET specific area is 49m
2/ g, D is about 14nm.
Embodiment 4
Press W
NaOH: W
NiCl26H2O=1.5: 1; M
N2H4H2O: M
NiCl26H2O=1.5: 1; W
NaBH4: W
NiCl26H2O=0.8 ‰: 1.With 4.2g NiCl
26H
2O is dissolved in the ethanol water of 15.8ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 6.3g NaOH is joined the 2.7ml mass percent, stirs into pasty mixture B.Get 0.1ml NaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
The BET specific area is 39m
2/ g, D is about 17nm.
Embodiment 5
Press W
NaOH: W
NiCl26H2O=1.1: 1; M
N2H4H2O: M
NiCl26H2O=1.9: 1; W
NaBH4: W
NiCl26H2O=1.6 ‰: 1.With 4.2gNiCl
26H
2O is dissolved in the ethanol water of 13.60ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 4.5gNaOH is joined the 3.4ml mass percent, stirs into pasty mixture B.Get 0.2ml NaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
The BET specific area is 80m
2/ g, D is about 9nm.
Embodiment 6
Press W
NaOH: W
NiCl26H2O=0.5: 1; M
N2H4H2O: M
NiCl26H2O=4.8: 1; W
NaBH4: W
NiCl26H2O=1%: 1.With 4.2g NiCl
26H
2O is dissolved in the ethanol water of 15.8ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 2.1g NaOH is joined the 8.5ml mass percent, stirs into pasty mixture B.Get 1.3ml NaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
The BET specific area is 17m
2/ g, D is about 40nm.
Embodiment 7
Press W
NaOH: W
NiCl26H2O=2: 1; M
N2H4H2O: M
NiCl26H2O=4.8: 1; W
NaBH4: W
NiCl26H2O=0.2 ‰: 1.With 4.2gNiCl
26H
2O is dissolved in the ethanol water of 15.8ml 95%, wiring solution-forming A; It is in 50% the hydrazine hydrate solution that 8.4g NaOH is joined the 8.5ml mass percent, stirs into pasty mixture B.Get 0.03mlNaBH
4Solution, join in the solution A, induced reaction takes place, and pasty mixture B is joined in the above-mentioned solution fast again, uses magnetic stirrer, reaction is carried out very soon, the black precipitate that generates in the reaction is with the distilled water washing, again with after ethanol washing, displacement, the dehydration, drying obtains nano metal nickel powder.
The BET specific area is 18m
2/ g, D is about 38nm.
Claims (4)
1. the preparation method of a nano metal nickel powder, it is characterized in that: sodium borohydride solution is added in the alcohol solution of nickel chloride, induced reaction takes place, again NaOH and hydrazine hydrate pasty mixture are joined in the above-mentioned solution, stir reaction down, after the reaction, product can make nano-nickel powder through separation, washing, drying.
2. according to the preparation method of the described nano metal nickel powder of claim 1, it is characterized in that added sodium borohydride quality (W
NaBH4) be six water nickel chloride quality (W
NiCl26H2O) 0.2 ‰-1.6 ‰.
3. according to the preparation method of the described nano metal nickel powder of claim 1, it is characterized in that the quality (W of NaOH
NaOH) be six water nickel chloride quality (W
NiCl26H2O) 0.5-2 doubly.
4. according to the preparation method of the described nano metal nickel powder of claim 1, it is characterized in that the amount of substance (M of hydrazine hydrate
N2H4H2O) with the amount of substance (M of six water nickel chlorides
NiCl26H2O) ratio be 1.5: 1-4.8: 1.
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Publication number | Priority date | Publication date | Assignee | Title |
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CN100391663C (en) * | 2006-04-10 | 2008-06-04 | 李小毛 | Process for preparing nano nickel powder |
CN102909391A (en) * | 2012-10-21 | 2013-02-06 | 吉林大学 | Method for preparing metal cobalt and nickel powder under room-temperature condition |
CN102952054B (en) * | 2012-11-09 | 2014-04-16 | 天津市安凯特催化剂有限公司 | Method for preparing m-beta-ethoxyl sulphone aniline |
CN104028780B (en) * | 2014-02-17 | 2016-04-20 | 瑞安市浙工大技术转移中心 | A kind of preparation method of amorphous nickel nano particle |
CN105081347B (en) * | 2015-09-07 | 2017-09-19 | 赣州市华新金属材料有限公司 | A kind of normal-pressure production method of low pine than high-purity spherical ultra-fine nickel powder |
CN105884605B (en) * | 2015-11-20 | 2019-02-01 | 中国科学技术大学 | A kind of method of Resources of Carbon Dioxide |
CN106493354B (en) * | 2016-10-24 | 2018-11-16 | 兰州大学 | The preparation method of the composite nano powder of oxide coated by zinc magnetic metal nano particle |
CN110340376B (en) * | 2019-07-16 | 2020-11-13 | 浙江大学 | Flower-shaped nickel wire wave-absorbing material and preparation method thereof |
CN113215608A (en) * | 2021-04-25 | 2021-08-06 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of bifunctional electrode |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS59162206A (en) * | 1983-03-08 | 1984-09-13 | Mitsui Mining & Smelting Co Ltd | Manufacture of fine nickel and cobalt powder |
CN1261565A (en) * | 1999-01-21 | 2000-08-02 | 中国科学技术大学 | Method for preparing nanometre metal cobalt powder or nickel powder |
CN1426865A (en) * | 2001-12-19 | 2003-07-02 | 北京有色金属研究总院 | Method of preparing nano metal nickel powder |
-
2005
- 2005-01-13 CN CNB2005100381019A patent/CN1319685C/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS59162206A (en) * | 1983-03-08 | 1984-09-13 | Mitsui Mining & Smelting Co Ltd | Manufacture of fine nickel and cobalt powder |
CN1261565A (en) * | 1999-01-21 | 2000-08-02 | 中国科学技术大学 | Method for preparing nanometre metal cobalt powder or nickel powder |
CN1426865A (en) * | 2001-12-19 | 2003-07-02 | 北京有色金属研究总院 | Method of preparing nano metal nickel powder |
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