CN103008675B - A kind of preparation method of nickel coated copper composite powder - Google Patents
A kind of preparation method of nickel coated copper composite powder Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of nickel coated copper composite powder, its processing step comprises: mantoquita and oxalates or carbonate reaction oxalic copper or copper carbonate are precipitated, filter, after pure water rinsing to neutrality, be mixed with the solution that concentration is 10-80g/L; According to the proportions nickel salt solution of copper nickel weight ratio 2:1-1:2 and required oxalates or carbonate solution, then join in above-mentioned cupric oxalate or copper carbonate solution and react generating nickel coated copper product.First the present invention uses the coated mantoquita of nickel salt, obtains nickel coated copper powder end with thermal decomposition, and production technology is simple, and be easy to operation, low production cost, can realize suitability for industrialized production.By nickel coated copper powder prepared by the present invention end or alloy pattern be spherical, class is spherical, irregular and dendroid, there is the advantages such as powder dispersion is even, segregation-free, covered effect are good, plated layer compact, granularity are controlled, can be applicable to electromagnetic shielding material and powder metallurgy pre-alloyed powder.Also can be used to prepare monel powder.
Description
Technical field
The invention belongs to metallurgical technology field, particularly relate to a kind of preparation method that can be applicable to the nickel coated copper composite powder of electromagnetic shielding material and powder metallurgy pre-alloyed powder.
Background technology
Electromagnetic screen coating can apply with it on complicated shape, cost is low, simple and practical and the advantage such as widely applicable is most popular, occupy shielding material market more than 75% share.Can effectively solve electronic product Electromagnetic Interference and shielding problem.In addition, on hyundai electronics war, warship, nuclear submarine, in order to prevent external electromagnetic interference and prevent electromagnetic wave outside radiation own, also need to adopt effective shielding measure.The raw material that current electromagnetic screen coating uses is generally fine silver powder, silver-coated copper powder, pure copper powder and nickel powder.The oxidation resistance of argent is strong, and shield effectiveness is splendid, but silver particles is easily moved in rubber matrix, and the resistance causing material raises, hydraulic performance decline, and silver powder, silver-coated copper powder high cost, hinder its development and apply simultaneously.Electric conductivity and the silver of copper powder are suitable, oxidation resistance is more weak, but ability of resisting to migration is far above silver, have good shielding action to high impedance electric field, pure nickel powder has the performance of good electromagnetic wave absorption, and magnetic conductivity is larger than silver, there is excellent anti-oxidant and corrosion resistance, there is good capability of electromagnetic shielding, be widely used military and civilian is industrial as a kind of excellent shielding material, become the main flow of the national electromagnetic shielding agent such as American-European.But pure nickel powder is not so good as copper powder in electric conductivity, cost performance etc.Therefore, at the coated one deck nickel of Copper Powder Surface, obtain the nickel coated copper powder that cost performance is higher, both can improve its oxidation resistance and the shield effectiveness to Low ESR magnetic field, the high conductivity that copper powder can be kept again excellent and ability of resisting to migration are the Main way of current electromagnetic shielding material development.
In prior art, the preparation method of metal coated composite powder mainly contains sol-gel method, chemical vapour deposition technique, electroless plating method, galvanoplastic, thermal decomposition one reducing process etc.
Electroless plating method is nickel coated copper powder preparation method conventional at present.Take electrolytic copper powder as core, adopt reducing agent reduction nickel salt, generate nickel powder and be coated on copper, form nickel coated copper powder end.In this technical process, because copper powder specific area is very large, there is larger apparent activation energy, generally need be realized the self-catalyzed reaction of copper by special process conditions and plating solution composition.Need in production to add the active material that some play catalytic action, just can obtain nickel coated copper powder.This complex process, operation easier greatly, are unfavorable for control of product quality as can be seen here.
Patent of invention (publication number CN1988973A) provides a kind of preparation method of nickel-plated copper powder, and the method adopts palladium to be catalyst, and hydrazine prepares nickel-plated copper powder as reducing agent.Document " technique of used in electronic industry nickel coated copper powder and performance study " adopts palladium bichloride to be activator, utilizes hydrazine for reducing agent coated one deck nickel on copper powder.All there is the problems such as complex process, cost are high, environmental pollution in said method.
Patent of invention (publication number CN1817512A) provides a kind of production method of nickel coated copper powder, under alkali plating solution condition, nickel sulfate solution is heated to 80-90 DEG C, adds electrolytic copper powder and regulate PH to 11.5-13.5, adopt hydrazine for reduction, prepare nickel coated copper powder end.The method of nickel coated copper powder is prepared under patent of invention (publication number CN1017733401A) also refer to a kind of acidic bath condition, copper powder after HCl treatment is placed in nickel-plating liquid, described nickel-plating liquid is nickelous sulfate, inferior sodium phosphate, sodium acetate, lactic acid, propionic acid, control PH to 4-5, temperature 80-90 DEG C, plating obtains nickel coated copper powder end.Document " preparation and property of nickel-plated copper powder characterizes ", Using Sodium Hypophosphite is reducing agent, at pH value ll-13, is reduced to nickelous sulfate under temperature 75-90 DEG C of condition, coated nickel powder on electrolytic copper powder.There is experiment condition harshness in above-mentioned technique, not easily suitability for industrialized production, and it is many to test chemical reagent used, the problems such as experimentation cost is high, complicated operation.
Document " preparation of novel Ni-Cu composite deposite " describes the technique preparing nickel coated copper powder end with composite electric plating method.Copper powder is added in the nickel plating electrolyte of sulfur acid nickel, chloric acid nickel, boric acid, control the pH value 3-4 of electrolyte, temperature 45-60 DEG C, current density 2-3A/dm
2, realize nickel plating object at Copper Powder Surface.There is complex process in this technique, the problem of the high not easily suitability for industrialized production application of production cost.
Summary of the invention
It is not enough that object of the present invention is intended to overcome existing technology, provide a kind of production technology simple, be easy to operation, low production cost, can the preparation method of nickel coated copper powder of suitability for industrialized production.
The present invention adopts following technical scheme to realize:
1) preparation of copper precipitation presoma, by mantoquita and oxalates, carbonate reaction oxalic copper or copper carbonate precipitation.Reaction temperature controls at 15-60 DEG C, under stirring, react 20-40 minute, is chosen as reaction temperature further and controls at 35-50 DEG C, under stirring, react 20-30 minute.
2) 1) in step, also can as well-known to those skilled in the art, add one or more of the dispersants such as polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), absolute ethyl alcohol, stearmide and polyethylene, be no more than at most three kinds, to prevent cupric oxalate or the reunion of carbonic acid copper powder presoma in course of reaction, addition adds 20-150g with the copper of every mole and is advisable, and the copper being chosen as every mole further adds 90-150g dispersant.Dispersant can add separately also can mix and add.
3) by 1) in sedimentation and filtration, after pure water is washed till neutrality, be mixed with 10-80g/L cupric oxalate or copper carbonate solution.
4) be 2:1-1:2 ratio according to copper nickel weight ratio, preparation nickel salt solution and required oxalates, carbonate solution, 3 are added after preparing) in, reaction temperature 15-60 DEG C, 10-30 minute is reacted under stirring, being chosen as reaction temperature further controls at 35-50 DEG C, under stirring, react 20-30 minute.Realize nickel salt precipitation to be coated in mantoquita precipitation.
5) by 4) in product filter, after pure water is washed till neutrality, absolute ethyl alcohol filter post-drying.
6) by 5) in dry after material in vacuum atmosphere, be slowly warming up to 200-300 DEG C at, insulation 1-2 hour, then hydrogen is passed into, be warming up to 350-700 DEG C, insulation 1.5-7 hour, is cooled to after less than 40 DEG C (being generally room temperature state) carry out Passivation Treatment and obtains nickel coated copper powders or monel powder.
7) for eliminating particle adhesion, by 6) the nickel coated copper powders that obtains or monel powder carry out dispersion treatment.
Above-mentioned nickel salt and mantoquita can be their sulfate, chlorate and nitrate and hickelous nydroxide, copper sulfide, basic copper carbonates etc.
Above-mentioned carbonate can be sodium carbonate, potash, ammonium carbonate, carbonic hydroammonium etc., and oxalates is ammonium oxalate etc.
First the present invention uses the coated mantoquita of nickel salt, obtains nickel coated copper powder end with thermal decomposition, and production technology is simple, and be easy to operation, low production cost, can realize suitability for industrialized production.By nickel coated copper powder prepared by the present invention end or alloy pattern be spherical, class is spherical, irregular and dendroid, there is the advantages such as powder dispersion is even, segregation-free, covered effect are good, plated layer compact, granularity are controlled, can be applicable to electromagnetic shielding material and powder metallurgy pre-alloyed powder.Also can be used to prepare monel powder.
Detailed description of the invention
The present invention is further illustrated for the following examples.But the present invention is not by any restriction of these embodiments.
embodiment 1
By 40 DEG C containing 1.0mol/L copper sulphate, 130g/L absolute ethyl alcohol mixed aqueous solution at the uniform velocity add 40 DEG C containing 0.75mol/L ammonium oxalate, 80g/L absolute ethyl alcohol mixed aqueous solutions stirring reactor in, uniform stirring, add reaction after 20 minutes, after reacting completely, obtain cupric oxalate precipitation.
Cupric oxalate filtration pure water is washed till neutrality, by 10g/L concentration preparation cupric oxalate solution, temperature is adjusted to 40 DEG C.
Then, will with copper nickel part by weight for 2:1 takes nickelous sulfate, be dissolved in pure water and make 40 DEG C, the nickel sulfate solution of 2mol/l, and 40 DEG C, the ammonium oxalate aqueous solution of 1.0mol/L stoichiometrically at the uniform velocity adds in reaction vessel, add rear reaction 30 minutes, then use pure water cyclic washing 2 times, 150 DEG C of oven dry in electric dry oven after filtering with absolute ethyl alcohol, obtain the cupric oxalate being enclosed with nickel oxalate.
Then, the cupric oxalate being enclosed with nickel oxalate is slowly warmed up in vacuum atmosphere 250 DEG C of insulations and passes into hydrogen after 1.5 hours, be warmed up to 500 DEG C of insulation 2h, be cooled to less than 40 DEG C subsequently and carry out Passivation Treatment, obtaining spherical nickel coated copper powder.Powder is loaded ball mill for dry grinding, obtains epigranular good dispersion, the nickel coated copper powders of particle mean size 3.4 μm.
embodiment 2
By 45 DEG C containing 1.75mol/L copper sulphate, 100g/L absolute ethyl alcohol mixed aqueous solution at the uniform velocity add 45 DEG C containing 0.75mol/L ammonium oxalate, 100g/L absolute ethyl alcohol mixed aqueous solutions stirring reactor in, at the uniform velocity stir, add reaction after 25 minutes, obtain cupric oxalate precipitation.
Cupric oxalate filtration pure water is washed till neutrality, by 25g/L concentration preparation cupric oxalate solution, temperature is adjusted to 45 DEG C.
Then, will with copper nickel part by weight for 1:1 takes nickelous sulfate, be dissolved in pure water and make 45 DEG C, the nickel sulfate solution of 1.5mol/l and 45 DEG C, the aqueous sodium carbonate of 1.5mol/L stoichiometrically at the uniform velocity adds in reaction vessel, adds rear reaction 25 minutes, then uses pure water cyclic washing 2 times, 120 DEG C of oven dry in electric dry oven after filtering with absolute ethyl alcohol, obtain the cupric oxalate being enclosed with nickelous carbonate.
Then, the cupric oxalate being enclosed with nickelous carbonate is slowly warmed up in vacuum atmosphere 230 DEG C of insulations and passes into hydrogen after 2 hours, be warmed up to 550 DEG C of insulation 1.5h, cooled less than 40 DEG C subsequently and carry out Passivation Treatment, obtaining class spherical nickel coated copper powder.Powder is loaded ball mill for dry grinding, obtains epigranular, good dispersion, the nickel coated copper powders of particle mean size 2.9 μm.
embodiment 3
By 38 DEG C containing 2mol/L copper nitrate, 90g/LPVP mixed aqueous solution at the uniform velocity add 38 DEG C containing 1.25mol/L ammonium oxalate, 50g/LPVP mixed aqueous solutions stirring reactor in, at the uniform velocity stir, add reaction after 30 minutes, obtain cupric oxalate precipitation.
Cupric oxalate filtration pure water is washed till neutrality, by 30g/L concentration preparation cupric oxalate solution, temperature is adjusted to 38 DEG C.
Then, will with copper nickel part by weight for 1:1.5 takes nickelous sulfate, be dissolved in pure water and make 38 DEG C, the nickel sulfate solution of 2mol/l and 38 DEG C, the ammonium carbonate solution of 1.0mol/L stoichiometrically at the uniform velocity adds in reaction vessel, adds rear reaction 30 minutes, then uses pure water cyclic washing 2 times, 120 DEG C of oven dry in electric dry oven after filtering with absolute ethyl alcohol, obtain the cupric oxalate being enclosed with nickelous carbonate.
Then, the cupric oxalate being enclosed with nickelous carbonate is slowly warmed up in vacuum atmosphere 200 DEG C of insulations and passes into hydrogen after 2 hours, be warmed up to 350 DEG C of insulation 3h, cooled room temperature subsequently, and carry out Passivation Treatment, obtain class spherical nickel coated copper powder.Loaded by powder in ball mill and add absolute ethyl alcohol wet-milling, discharging is dried.Obtain epigranular, good dispersion, the nickel coated copper powders of particle mean size 1.68 μm.
embodiment 4
By 35 DEG C containing 2.5mol/L copper sulphate, 100g/LPVP mixed aqueous solution at the uniform velocity add 35 DEG C containing 2mol/L ammonium oxalate, 75g/LPVP mixed aqueous solutions stirring reactor in, at the uniform velocity stir, add reaction after 30 minutes, obtain cupric oxalate precipitation.
Cupric oxalate filtration pure water is washed till neutrality, by 40g/L concentration preparation cupric oxalate solution, temperature is adjusted to 30 DEG C.
Then, will with copper nickel part by weight for 1:2 takes nickelous sulfate, the oxalic acid aqueous solution being dissolved in pure water nickel sulfate solution and the 30 DEG C of 2mol/L making 30 DEG C of 1.75mol/l stoichiometrically at the uniform velocity adds in reaction vessel, add rear reaction 30 minutes, then use pure water cyclic washing 2 times, 120 DEG C of oven dry in electric dry oven after filtering with ethanol, obtain the cupric oxalate being enclosed with nickel oxalate.
Then, the cupric oxalate being enclosed with nickel oxalate is slowly warmed up in vacuum atmosphere 280 DEG C of insulations and passes into hydrogen after 1.5 hours, be warmed up to 450 DEG C of insulation 3h, cooled room temperature subsequently, and carry out Passivation Treatment, obtain irregular shape nickel coated copper powders.Powder is impacted dispersion in gas shock mill.Obtain epigranular, good dispersion, the nickel coated copper powders of particle mean size 4.39 μm.
embodiment 5
By 50 DEG C containing 2.0mol/L copper sulphate, 150g/L absolute ethyl alcohol mixed aqueous solution at the uniform velocity add 50 DEG C containing 2mol/L ammonium oxalate, 75g/L absolute ethyl alcohol mixed aqueous solutions stirring reactor in, at the uniform velocity stir, add reaction after 30 minutes, obtain cupric oxalate precipitation.
Cupric oxalate filtration pure water is washed till neutrality, by 30g/L concentration preparation cupric oxalate solution, temperature is adjusted to room temperature.
Then, will with copper nickel part by weight for 1:1 takes nickelous sulfate, be dissolved in pure water and make 50 DEG C, the nickel sulfate solution of 2mol/l and 50 DEG C, the oxalic acid aqueous solution of 2mol/L stoichiometrically at the uniform velocity adds in reaction vessel, adds rear reaction 30 minutes, then uses pure water cyclic washing, 100 DEG C of oven dry in electric dry oven after filtering with absolute ethyl alcohol, obtain the cupric oxalate being enclosed with nickel oxalate.
Then, the cupric oxalate being enclosed with nickel oxalate is slowly warmed up in vacuum atmosphere 300 DEG C of insulations and passes into hydrogen after 2 hours, be warmed up to 700 DEG C of insulation 7h, cooled room temperature subsequently, and carry out Passivation Treatment, obtain spherical nickel copper alloy powder.Powder is impacted dispersion in gas shock mill.Obtain epigranular, good dispersion, the monel powder of particle mean size 3.82 μm.
Embodiment 6
By 38 DEG C containing 2mol/L copper nitrate, 100g/LPVP mixed aqueous solution at the uniform velocity add 38 DEG C containing 1.25mol/L potash, 80g/LPVP mixed aqueous solutions stirring reactor in, at the uniform velocity stir, add reaction after 30 minutes, obtain copper carbonate precipitation.
Cupric oxalate filtration pure water is washed till neutrality, by 30g/L concentration preparation copper carbonate solution, temperature is adjusted to 40 DEG C.
Then, will with copper nickel part by weight for 1:1.5 takes nickelous sulfate, be dissolved in pure water and make 40 DEG C, the nickel sulfate solution of 2mol/l and 40 DEG C, the ammonium carbonate solution of 1.0mol/L stoichiometrically at the uniform velocity adds in reaction vessel, adds rear reaction 30 minutes, then uses pure water cyclic washing 2 times, 120 DEG C of oven dry in electric dry oven after filtering with absolute ethyl alcohol, obtain the cupric oxalate being enclosed with nickelous carbonate.
Then, the cupric oxalate being enclosed with nickelous carbonate is slowly warmed up in vacuum atmosphere 200 DEG C of insulations and passes into hydrogen after 2 hours, be warmed up to 350 DEG C of insulation 3h, cooled room temperature subsequently, and carry out Passivation Treatment, obtain dendroid nickel coated copper powders.Loaded by powder in ball mill and add absolute ethyl alcohol wet-milling, discharging is dried.Obtain epigranular, good dispersion, the nickel coated copper powders of particle mean size 2.13 μm.
Claims (4)
1. the preparation method of a nickel coated copper composite powder, its processing step comprises: mantoquita and oxalates or carbonate stirring reaction 20-30 minute oxalic copper or copper carbonate under the situation existed by dispersant are precipitated, control reaction temperature 35-50 DEG C, filter, after pure water rinsing to neutrality, be mixed with the solution that concentration is 10-80g/L; According to the proportions nickel salt solution of copper nickel weight ratio 2:1-1:2 and required oxalates or carbonate solution, then join stirring reaction 20-30 minute generating nickel coated copper product in above-mentioned cupric oxalate or copper carbonate solution, control reaction temperature 35-50 DEG C; By above-mentioned nickel coated copper product after filtration, with pure water to neutral, absolute ethyl alcohol filters post-drying, then in vacuum atmosphere, be slowly warming up to 200-300 DEG C, insulation 1-2 hour, then passes into hydrogen, be warming up to 350-700 DEG C, continue insulation 1.5-7 hour, be then cooled to after room temperature-40 DEG C carries out Passivation Treatment and obtain nickel coated copper powders, finally adopt the mode of gas shock or ball milling to carry out dispersion treatment the nickel coated copper powders of gained;
Above-mentioned dispersant is one or more in polyvinylpyrrolidone, polyethylene glycol, absolute ethyl alcohol, stearmide and polyethylene, and its addition adds 20-150g with the copper of every mole.
2. according to the preparation method of nickel coated copper composite powder according to claim 1, it is characterized in that: the addition of described dispersant is that the copper of every mole adds 90-150g dispersant.
3., according to the preparation method of nickel coated copper composite powder according to claim 1, it is characterized in that: above-mentioned nickel salt and mantoquita be they sulfate, chlorate, nitrate and hickelous nydroxide, copper sulfide, basic copper carbonate.
4., according to the preparation method of nickel coated copper composite powder according to claim 1, it is characterized in that: above-mentioned
Carbonate is sodium carbonate, potash, ammonium carbonate or carbonic hydroammonium, and oxalates is ammonium oxalate.
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| CN104475748A (en) * | 2014-11-21 | 2015-04-01 | 广西大学 | Method for preparing ultra-fine copper powder |
| CN104801709B (en) * | 2015-03-20 | 2017-05-17 | 邱羽 | Nickel-coated copper clad metal powder and preparation method and application thereof |
| CN108655392B (en) * | 2018-05-18 | 2020-02-04 | 有研粉末新材料（北京）有限公司 | Preparation method of copper-coated chromium composite powder |
| CN110740626B (en) * | 2018-10-29 | 2020-11-03 | 嘉兴学院 | Preparation method of composite electromagnetic shielding material of copper and ceramic powder |
| CN111360244B (en) * | 2018-12-25 | 2022-06-07 | 上海核威实业有限公司 | Bearing alloy blank, bearing alloy, bearing material, and preparation method and application thereof |
| CN110039063A (en) * | 2019-05-28 | 2019-07-23 | 白银矿冶职业技术学院 | The method for preparing micron-stage sheet-like nickel coated copper powder with waste solution of copper electrolysis |
| CN113618075A (en) * | 2021-08-23 | 2021-11-09 | 孙珲 | Preparation method of filling high-purity nano material of ultralow-resistivity conductive paste |
| CN115611302B (en) * | 2022-10-22 | 2023-12-05 | 杭州富阳鸿源再生资源利用有限公司 | Preparation process of nano basic copper carbonate and nano basic copper carbonate |
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| CA1042735A (en) * | 1974-07-12 | 1978-11-21 | Sherritt Gordon Mines Limited | Copper coated composite powders and method of production thereof |
| JPH10102109A (en) * | 1996-09-30 | 1998-04-21 | Tanaka Kikinzoku Kogyo Kk | Production of nickel powder |
| JP3951449B2 (en) * | 1998-05-21 | 2007-08-01 | 堺化学工業株式会社 | Method for producing fine spherical metal nickel fine powder |
| CN1257785C (en) * | 2003-06-12 | 2006-05-31 | 中南大学 | Method for preparing nano-grade tungsten-based composite powder by sol-spray drying-thermal reduction |
| CN1817521A (en) * | 2006-03-17 | 2006-08-16 | 金川集团有限公司 | Production of composite copper powder with nickle coating |
| CN101347843B (en) * | 2008-09-12 | 2011-06-08 | 安徽工业大学 | Method for preparing metallic nickel nano powder |
| CN101745645B (en) * | 2008-12-17 | 2011-05-11 | 黑龙江大学 | Preparation method of nano-copper-nickel alloy by liquid phase method |
| CN101456078B (en) * | 2009-01-06 | 2010-08-18 | 中北大学 | Preparation method of nano nickel copper zinc ferrite powder |
| CN102728852B (en) * | 2012-07-10 | 2014-11-12 | 国家钽铌特种金属材料工程技术研究中心 | Preparation method of oxide or meta-coated nickel ultrafine powder |
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