CN103008675A - Preparation method of nickel coated copper composite powder - Google Patents
Preparation method of nickel coated copper composite powder Download PDFInfo
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Abstract
The invention relates to a preparation method of nickel coated copper composite powder. The preparation method comprises the following process steps that copper salt and oxalate or carbonate take reaction to generate cupric oxalate or copper carbonate sediments, the filtering is carried out, pure water is used for flushing to be in a neutral state, and solution with the concentration being 10 to 80g/L is prepared; and nickel salt solution and the required oxalate or carbonate solution are prepared according to a proportion that the copper nickel weight ratio is 2:1 to 1:2 and are added into the cupric oxalate or copper carbonate solution for reaction to generate nickel coated copper resultants. The preparation method has the advantages that firstly, nickel salts are used for coating copper salts, then, the thermal decomposition is carried out, nickel coated copper powder is obtained, the production process is simple, the operation is easy, the production cost is low, and the industrial production can be realized. The nickel coated copper powder or alloy prepared by the method has the morphology in a spherical shape, a near-spherical shape, an irregular shape or a tree branch shape, and has the advantages that the powder dispersion is uniform, no segregation is generated, the coating effect is good, the coating is compact, the particle size is controllable, and the like. The nickel coated copper powder or alloy can be used for electromagnetic shielding materials and powder metallurgy prealloyed powder. The preparation method can be used for preparing nickel-copper alloy powder.
Description
Technical field
The invention belongs to metallurgical technology field, particularly relate to a kind of preparation method who can be applicable to the nickel clad copper composite powder of electromagnetic shielding material and powder metallurgy pre-alloyed powder.
Background technology
Electromagnetic screen coating with its can apply at complicated shape, cost is low, simple and practical and the advantage such as widely applicable is most popular, occupies shielding material market 75% above 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 to prevent electromagnetic wave outside radiation own, also need to adopt effective shielding measure.The raw material of at present electromagnetic screen coating use generally is 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 in rubber matrix, easily move, the resistance that causes material raises, hydraulic performance decline, silver powder, silver-coated copper powder high cost have hindered its development and application simultaneously.The electric conductivity of copper powder is suitable with silver, oxidation resistance a little less than, but ability of resisting to migration is far above silver, the high impedance electric field is had preferably shielding action, and pure nickel powder has the performance of good electromagnetic wave absorption, and magnetic conductivity is larger than silver, has good anti-oxidant and corrosion resistance, have good capability of electromagnetic shielding, be widely used military and civilian is industrial as a kind of good 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 at aspects such as electric conductivity, cost performances.Therefore, coat one deck nickel at Copper Powder Surface, obtain the higher nickel coated copper powder of cost performance, both can improve its oxidation resistance and to the shield effectiveness in Low ESR magnetic field, can keep again the good high conductivity of copper powder and ability of resisting to migration, be the main direction of present electromagnetic shielding material development.
In the 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 commonly used at present.Take electrolytic copper powder as core, adopt reducing agent reduction nickel salt, generate nickel powder and be coated on the copper, form the nickel coated copper powder end.In this technical process, because the copper powder specific area is very large, have larger apparent activation energy, generally need form to realize by special process conditions and plating bath the self-catalyzed reaction of copper.Need to add the active material that some play catalytic action in the production, just can obtain nickel coated copper powder.This shows that this complex process, operation easier are large, are unfavorable for control of product quality.
Patent of invention (publication number CN1988973A) provides a kind of preparation method of nickel-plated copper powder, and it is catalyst that the method adopts palladium, and hydrazine prepares nickel-plated copper powder as reducing agent.Document " technique of used in electronic industry nickel coated copper powder and performance study " employing palladium bichloride is activator, utilizes hydrazine to coat one deck nickel for reducing agent at copper powder.All there are 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 the alkali plating solution condition, nickel sulfate solution is heated to 80-90 ℃, add electrolytic copper powder and regulate PH to 11.5-13.5, adopt hydrazine to be reduction, preparation nickel coated copper powder end.Patent of invention (publication number CN1017733401A) has also been mentioned the method for preparing nickel coated copper powder under a kind of acidic bath condition, copper powder after the salt acid treatment is placed 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 ℃, plating obtains the 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 the temperature 75-90 ℃ of condition, coats nickel powder at electrolytic copper powder.Above-mentioned technique exists experiment condition harsh, is difficult for suitability for industrialized production, tests used chemical reagent many, the problems such as experimentation cost is high, complicated operation.
Document " preparation of novel Ni-Cu composite deposite " has been introduced the technique for preparing the 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 the pH value 3-4 of control electrolyte, temperature 45-60 ℃, current density 2-3A/dm
2, realize the nickel plating purpose at Copper Powder Surface.There is complex process in this technique, the high problem that is difficult for the suitability for industrialized production application of production cost.
Summary of the invention
It is not enough that purpose of the present invention is intended to overcome existing technology, provides that a kind of production technology is simple, easy operating, low production cost, but the nickel of suitability for industrialized production coats the preparation method of copper powder.
The present invention adopts following technical scheme to realize:
1) preparation of copper precipitation presoma is with mantoquita and oxalates, carbonate reaction oxalic copper or copper carbonate precipitation.Reaction temperature is controlled at 15-60 ℃, and reaction is 20-40 minute under stirring, further is chosen as reaction temperature and is controlled at 35-50 ℃, and reaction is 20-30 minute under stirring.
2) 1) in the step, also can be as well-known to those skilled in the art, one or more of the dispersants such as adding 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 is advisable with every mole copper adding 20-150 g, and the copper that further is chosen as every mole adds the 90-150g dispersant.Dispersant can add separately also can mix adding.
3) with 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 the 2:1-1:2 ratio according to copper nickel weight ratio, preparation nickel salt solution and required oxalates, carbonate solution, prepare rear adding 3) in, reaction temperature 15-60 ℃, reaction is 10-30 minute under stirring, further be chosen as reaction temperature and be controlled at 35-50 ℃, reaction is 20-30 minute under stirring.Realize that the nickel salt precipitation is coated on the mantoquita precipitation.
5) with 4) in product filter, after pure water was washed till neutrality, absolute ethyl alcohol filtered post-drying.
6) with 5) in the oven dry after material in vacuum atmosphere, slowly be warming up under 200-300 ℃, be incubated 1-2 hour, then pass into hydrogen, be warming up to 350-700 ℃, be incubated 1.5-7 hour, be cooled to and (be generally room temperature state) below 40 ℃ and carry out obtaining nickel coated copper powder or monel powder after the Passivation Treatment.
7) for eliminating particle adhesion, with 6) the nickel coated copper powder or the monel powder that obtain carry out dispersion treatment.
Above-mentioned nickel salt and mantoquita can be their sulfate, chlorate and nitrate and hickelous nydroxides, copper sulfide, basic copper carbonate etc.
Above-mentioned carbonate can be sodium carbonate, potash, ammonium carbonate, carbonic hydroammonium etc., and oxalates is ammonium oxalate etc.
The present invention at first uses nickel salt to coat mantoquita, and subsequently thermal decomposition obtains the nickel coated copper powder end, and production technology is simple, easy operating, and low production cost can be realized suitability for industrialized production.Nickel coated copper powder end or the alloy pattern prepared by the present invention is sphere, class is spherical, irregular and dendroid, have the advantages such as powder is uniformly dispersed, segregation-free, covered effect is good, coating is fine and close, granularity is controlled, can be applicable to electromagnetic shielding material and powder metallurgy pre-alloyed powder.Also can be used to prepare the monel powder.
The specific embodiment
The present invention is further illustrated for the following examples.But the present invention is not subjected to any restriction of these embodiment.
Embodiment 1
40 ℃ of mixed aqueous solutions that contain 1.0mol/L copper sulphate, 130g/L absolute ethyl alcohol are at the uniform velocity added in the stirring reactor of 40 ℃ of mixed aqueous solutions that contain 0.75mol/L ammonium oxalate, 80g/L absolute ethyl alcohol, uniform stirring, add reaction after 20 minutes, obtain the cupric oxalate precipitation after reacting completely.
Cupric oxalate filtered be washed till neutrality with pure water, press 10g/L concentration and prepare cupric oxalate solution with adjustment to 40 ℃.
Then, to take by weighing nickelous sulfate take copper nickel part by weight as 2:1, be dissolved in and make 40 ℃ in the pure water, the nickel sulfate solution of 2mol/l, and 40 ℃, the ammonium oxalate aqueous solution of 1.0mol/L at the uniform velocity adds in the reaction vessel by stoichiometric proportion, added afterreaction 30 minutes, then use the pure water cyclic washing 2 times, filter rear 150 ℃ of oven dry in electric dry oven with absolute ethyl alcohol, obtain being enclosed with the cupric oxalate of nickel oxalate.
Then, the cupric oxalate that is enclosed with nickel oxalate slowly is warmed up to 250 ℃ of insulations passes into hydrogen after 1.5 hours in vacuum atmosphere, be warmed up to 500 ℃ of insulation 2h, subsequently it is cooled to below 40 ℃ and carries out Passivation Treatment, obtain spherical nickel coated copper powder.With the powder ball mill for dry grinding of packing into, obtain the epigranular good dispersion, the nickel coated copper powder of particle mean size 3.4 μ m.
Embodiment 2
45 ℃ of mixed aqueous solutions that contain 1.75mol/L copper sulphate, 100g/L absolute ethyl alcohol are at the uniform velocity added in the stirring reactor of 45 ℃ of mixed aqueous solutions that contain 0.75mol/L ammonium oxalate, 100g/L absolute ethyl alcohol, at the uniform velocity stir, add reaction after 25 minutes, obtain the cupric oxalate precipitation.
Cupric oxalate filtered be washed till neutrality with pure water, press 25g/L concentration and prepare cupric oxalate solution with adjustment to 45 ℃.
Then, to take by weighing nickelous sulfate take copper nickel part by weight as 1:1, be dissolved in and make 45 ℃ in the pure water, 1.5mol/l nickel sulfate solution and 45 ℃, 1.5mol/L aqueous sodium carbonate at the uniform velocity add in the reaction vessel by stoichiometric proportion, added afterreaction 25 minutes, then use the pure water cyclic washing 2 times, filter rear 120 ℃ of oven dry in electric dry oven with absolute ethyl alcohol, obtain being enclosed with the cupric oxalate of nickelous carbonate.
Then, the cupric oxalate that is enclosed with nickelous carbonate slowly is warmed up to 230 ℃ of insulations passes into hydrogen after 2 hours in vacuum atmosphere, be warmed up to 550 ℃ of insulation 1.5h, subsequently its cooling below 40 ℃ and carry out Passivation Treatment, is obtained the spherical nickel coated copper of class powder.With the powder ball mill for dry grinding of packing into, obtain epigranular, good dispersion, the nickel coated copper powder of particle mean size 2.9 μ m.
Embodiment 3
38 ℃ of mixed aqueous solutions that contain 2mol/L copper nitrate, 90g/L PVP are at the uniform velocity added in the stirring reactor of 38 ℃ of mixed aqueous solutions that contain 1.25mol/L ammonium oxalate, 50g/L PVP, at the uniform velocity stir, add reaction after 30 minutes, obtain the cupric oxalate precipitation.
Cupric oxalate filtered be washed till neutrality with pure water, press 30g/L concentration and prepare cupric oxalate solution with adjustment to 38 ℃.
Then, to take by weighing nickelous sulfate take copper nickel part by weight as 1:1.5, be dissolved in and make 38 ℃ in the pure water, the nickel sulfate solution of 2mol/l and 38 ℃, 1.0mol/L ammonium carbonate solution at the uniform velocity add in the reaction vessel by stoichiometric proportion, added afterreaction 30 minutes, then use the pure water cyclic washing 2 times, filter rear 120 ℃ of oven dry in electric dry oven with absolute ethyl alcohol, obtain being enclosed with the cupric oxalate of nickelous carbonate.
Then, the cupric oxalate that is enclosed with nickelous carbonate slowly is warmed up to 200 ℃ of insulations passes into hydrogen after 2 hours in vacuum atmosphere, be warmed up to 350 ℃ of insulation 3h, subsequently with its cooling room temperature, and carry out Passivation Treatment, obtain the spherical nickel coated copper of class powder.Powder packed into add the absolute ethyl alcohol wet-milling in the ball mill, the discharging oven dry.Obtain epigranular, good dispersion, the nickel coated copper powder of particle mean size 1.68 μ m.
Embodiment 4
35 ℃ of mixed aqueous solutions that contain 2.5mol/L copper sulphate, 100g/L PVP are at the uniform velocity added in the stirring reactor of 35 ℃ of mixed aqueous solutions that contain 2mol/L ammonium oxalate, 75g/L PVP, at the uniform velocity stir, add reaction after 30 minutes, obtain the cupric oxalate precipitation.
Cupric oxalate filtered be washed till neutrality with pure water, press 40g/L concentration and prepare cupric oxalate solution with adjustment to 30 ℃.
Then, to take by weighing nickelous sulfate take copper nickel part by weight as 1:2, being dissolved in the nickel sulfate solution of making 30 ℃ of 1.75mol/l in the pure water and the oxalic acid aqueous solution of 30 ℃ of 2mol/L at the uniform velocity adds in the reaction vessel by stoichiometric proportion, added afterreaction 30 minutes, then use the pure water cyclic washing 2 times, filter rear 120 ℃ of oven dry in electric dry oven with ethanol, obtain being enclosed with the cupric oxalate of nickel oxalate.
Then, the cupric oxalate that is enclosed with nickel oxalate slowly is warmed up to 280 ℃ of insulations passes into hydrogen after 1.5 hours in vacuum atmosphere, be warmed up to 450 ℃ of insulation 3h, subsequently with its cooling room temperature, and carry out Passivation Treatment, obtain irregular shape nickel coated copper powder.Powder is impacted dispersion in the gas shock mill.Obtain epigranular, good dispersion, the nickel coated copper powder of particle mean size 4.39 μ m.
Embodiment 5
50 ℃ of mixed aqueous solutions that contain 2.0mol/L copper sulphate, 150g/L absolute ethyl alcohol are at the uniform velocity added in the stirring reactor of 50 ℃ of mixed aqueous solutions that contain 2mol/L ammonium oxalate, 75g/L absolute ethyl alcohol, at the uniform velocity stir, add reaction after 30 minutes, obtain the cupric oxalate precipitation.
Cupric oxalate filtered is washed till neutrality with pure water, press 30g/L concentration prepare cupric oxalate solution with adjustment to room temperature.
Then, to take by weighing nickelous sulfate take copper nickel part by weight as 1:1, be dissolved in and make 50 ℃ in the pure water, the nickel sulfate solution of 2mol/l and 50 ℃, the oxalic acid aqueous solution of 2mol/L at the uniform velocity adds in the reaction vessel by stoichiometric proportion, adds afterreaction 30 minutes, then uses the pure water cyclic washing, filter rear 100 ℃ of oven dry in electric dry oven with absolute ethyl alcohol, obtain being enclosed with the cupric oxalate of nickel oxalate.
Then, the cupric oxalate that is enclosed with nickel oxalate slowly is warmed up to 300 ℃ of insulations passes into hydrogen after 2 hours in vacuum atmosphere, be warmed up to 700 ℃ of insulation 7h, subsequently with its cooling room temperature, and carry out Passivation Treatment, obtain spherical monel powder.Powder is impacted dispersion in the gas shock mill.Obtain epigranular, good dispersion, the monel powder of particle mean size 3.82 μ m.
Embodiment 6
38 ℃ of mixed aqueous solutions that contain 2mol/L copper nitrate, 100g/L PVP are at the uniform velocity added in the stirring reactor of 38 ℃ of mixed aqueous solutions that contain 1.25mol/L potash, 80g/L PVP, at the uniform velocity stir, add reaction after 30 minutes, obtain the copper carbonate precipitation.
Cupric oxalate filtered be washed till neutrality with pure water, press 30g/L concentration and prepare copper carbonate solution with adjustment to 40 ℃.
Then, to take by weighing nickelous sulfate take copper nickel part by weight as 1:1.5, be dissolved in and make 40 ℃ in the pure water, the nickel sulfate solution of 2mol/l and 40 ℃, 1.0mol/L ammonium carbonate solution at the uniform velocity add in the reaction vessel by stoichiometric proportion, added afterreaction 30 minutes, then use the pure water cyclic washing 2 times, filter rear 120 ℃ of oven dry in electric dry oven with absolute ethyl alcohol, obtain being enclosed with the cupric oxalate of nickelous carbonate.
Then, the cupric oxalate that is enclosed with nickelous carbonate slowly is warmed up to 200 ℃ of insulations passes into hydrogen after 2 hours in vacuum atmosphere, be warmed up to 350 ℃ of insulation 3h, subsequently with its cooling room temperature, and carry out Passivation Treatment, obtain dendroid nickel coated copper powder.Powder packed into add the absolute ethyl alcohol wet-milling in the ball mill, the discharging oven dry.Obtain epigranular, good dispersion, the nickel coated copper powder of particle mean size 2.13 μ m.
Claims (10)
1. the preparation method of a nickel clad copper composite powder, its processing step comprises: with mantoquita and oxalates or carbonate reaction oxalic copper or copper carbonate precipitation, filter, to neutrality, be mixed with the solution that concentration is 10-80g/L with pure water rinsing; According to ratio preparation nickel salt solution and required oxalates or the carbonate solution of copper nickel weight ratio 2:1-1:2, then join reaction generating nickel coated copper product in above-mentioned cupric oxalate or the copper carbonate solution.
2. according to the preparation method of nickel clad copper composite powder claimed in claim 1, it is characterized in that: with above-mentioned nickel coated copper product after filtration, extremely neutral with the pure water washing, absolute ethyl alcohol filters post-drying, then slowly is warming up to 200-300 ℃ in vacuum atmosphere, is incubated 1-2 hour, then pass into hydrogen, be warming up to 350-700 ℃, continue insulation 1.5-7 hour, then be cooled to room temperature-40 and ℃ carry out obtaining nickel coated copper powder or monel powder after the Passivation Treatment.
3. according to the preparation method of nickel clad copper composite powder claimed in claim 2, it is characterized in that: above-mentioned nickel coated copper powder adopts the mode of gas shock or ball milling to carry out dispersion treatment.
4. according to the preparation method of nickel clad copper composite powder claimed in claim 1, it is characterized in that: the reaction of formation temperature of above-mentioned cupric oxalate or copper carbonate precipitation is controlled at 15-60 ℃, reaction is 20-40 minute under stirring, further be chosen as reaction temperature and be controlled at 35-50 ℃, reaction is 20-30 minute under stirring.
5. according to the preparation method of claim 1 or 4 described nickel clad copper composite powders, it is characterized in that: add dispersant in the reaction of formation process of above-mentioned cupric oxalate or copper carbonate precipitation, addition is advisable with every mole copper adding 20-150g, and the copper that further is chosen as every mole adds the 90-150g dispersant.
6. according to the preparation method of nickel clad copper composite powder claimed in claim 5, it is characterized in that: above-mentioned dispersant is one or more in polyvinylpyrrolidone, polyethylene glycol, absolute ethyl alcohol, stearmide and the polyethylene.
7. according to the preparation method of nickel clad copper composite powder claimed in claim 1, it is characterized in that: reaction temperature 15-60 ℃ of above-mentioned nickel coated copper product, reaction is 10-30 minute under stirring, further be chosen as reaction temperature and be controlled at 35-50 ℃, reaction is 20-30 minute under stirring.
8. according to the preparation method of nickel clad copper composite powder claimed in claim 1, it is characterized in that: above-mentioned nickel salt and mantoquita are their sulfate, chlorate, nitrate and hickelous nydroxide, copper sulfide, basic copper carbonate.
9. according to the preparation method of nickel clad copper composite powder claimed in claim 1, it is characterized in that: above-mentioned
Carbonate is sodium carbonate, potash, ammonium carbonate or carbonic hydroammonium, and oxalates is ammonium oxalate.
10. according to the preparation method of nickel clad copper composite powder claimed in claim 2, it is characterized in that: described nickel coated copper powder or monel powder carry out dispersion treatment in ball mill ball milling or gas shock mill.
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| CN104475748A (en) * | 2014-11-21 | 2015-04-01 | 广西大学 | Method for preparing ultra-fine copper powder |
| CN104801709A (en) * | 2015-03-20 | 2015-07-29 | 邱羽 | Nickel-coated copper clad metal powder and preparation method and application thereof |
| CN108655392A (en) * | 2018-05-18 | 2018-10-16 | 有研粉末新材料（北京）有限公司 | A kind of preparation method of copper clad chromium composite powder |
| 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 |
| CN110740626A (en) * | 2018-10-29 | 2020-01-31 | 嘉兴学院 | Preparation method of composite electromagnetic shielding materials of copper and ceramic powder |
| CN111360244A (en) * | 2018-12-25 | 2020-07-03 | 上海核威实业有限公司 | Bearing alloy blank, bearing alloy, bearing material, and preparation method and application thereof |
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| CN104475748A (en) * | 2014-11-21 | 2015-04-01 | 广西大学 | Method for preparing ultra-fine copper powder |
| CN104801709A (en) * | 2015-03-20 | 2015-07-29 | 邱羽 | Nickel-coated copper clad metal powder and preparation method and application thereof |
| 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 |
| CN108655392A (en) * | 2018-05-18 | 2018-10-16 | 有研粉末新材料（北京）有限公司 | A kind of preparation method of copper clad chromium composite powder |
| CN110740626A (en) * | 2018-10-29 | 2020-01-31 | 嘉兴学院 | Preparation method of composite electromagnetic shielding materials of copper and ceramic 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 |
| CN111360244A (en) * | 2018-12-25 | 2020-07-03 | 上海核威实业有限公司 | Bearing alloy blank, bearing alloy, bearing material, and preparation method and application thereof |
| 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 |
| CN115611302A (en) * | 2022-10-22 | 2023-01-17 | 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 |
| 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 |
| CN115870492A (en) * | 2022-10-24 | 2023-03-31 | 广州大学 | Preparation method of oil-soluble amorphous nickel-boron alloy |
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