CN103611931A - Method for preparing nickel-coated copper composite powder in laboratory through electroplating - Google Patents
Method for preparing nickel-coated copper composite powder in laboratory through electroplating Download PDFInfo
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- CN103611931A CN103611931A CN201310697472.2A CN201310697472A CN103611931A CN 103611931 A CN103611931 A CN 103611931A CN 201310697472 A CN201310697472 A CN 201310697472A CN 103611931 A CN103611931 A CN 103611931A
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Abstract
The invention relates to the technical field of electroplating, in particular to a method for preparing nickel-coated copper composite powder in a laboratory through electroplating. The method is characterized in that by the utilization of a cathode nickel net or a cathode nickel plate and the cooperation of magnetic stirring, the nickel-coated copper powder is quickly and efficiently prepared in the laboratory. The method has the advantages that the problems that under a traditional electroplating condition, when the surface of conductive powder is electroplated, the powder difficultly gathers on a cathode or the plated power is difficultly used as the cathode are solved, through the method, the nickel-coated copper composite powder can be prepared in the laboratory, dispersibility of the powder is very good, nickel coating is complete, and a plating layer is dense and is in a crystalline state.
Description
Technical field
The present invention relates to electroplating technology field, refer in particular to a kind of method that nickel clad copper composite powder is prepared in plating that is applicable to laboratory.
Background technology
Along with developing rapidly of modern science and technology, at metallurgy, machinery; navigation, electronics, the numerous areas such as communication and material protection; homogenous material has been difficult to meet some special requirement, causes the research of composite day by day come into one's own and obtained development rapidly.Metal coated composite powder is as one type of composite, has clad metal concurrently and as the characteristic that is wrapped by two or more material of powder of core, thereby all becomes requisite material at above-mentioned numerous areas.
Rare due to nonferrous metal resource, restricted non-ferrous metal production and application in a lot of fields, so non-ferrous metal cladded type composite powder is as a class substituted type material, there is good researching value and application prospect, conventional nickel in Powder Metallurgy Industry, copper is as metal carbonyl coat, coated comparatively cheap metal dust, replace pure nickel powder, copper powder, reaches with this object that reduces production costs and save the energy.
Use electric plating method, can on the powder of electric conductivity, carry out plating having, but directly will be wrapped by powder and on its surface, form uniform nickel clad as negative electrode, there is certain difficulty, so have special requirement to producing electronickelling composite powder experimental provision, to thering is the powder surface nickel plating of electric conductivity, can select the method for thermopnore to carry out electronickelling, but this device is not suitable for being used in laboratory research, also has and propose to have designed a kind of Special electric plating appts: anode is the insoluble anode that graphite or stainless steel etc. are made, the composite cathode of negative electrode for needing coated electroconductive powder and carrier to be grouped into, the also mechanical driving part of guaranteed anode and cathode relative motion---feed flow and feed part, adopt this special electroplanting device to be coated electroconductive powder: along with the relative motion of anode and cathode, powder and electroplate liquid enter between anode and cathode together, electroplate liquid flows in the gap of powder, under electric field action, anode ion deposits the surface-discharge at powder, obtain homogeneous coating, this is a kind of good method, by this special device, can realize powder surface quantitatively coated, and the clad forming is even, and the present invention makes negative electrode with nickel plate and nickel screen respectively, by the homodisperse electroplate liquid of copper powder, Copper Powder Surface is carried out the coated processing of nickel under vigorous stirring, successfully realized in use for laboratory galvanoplastic and prepared the coated copper powder of nickel, do not introduce impurity element, hydrogen loss, phosphorus content, mobility and apparent density all meet the requirement of high-performance monel powdered metallurgical material, and its processing performance and physical property meet national standard.
Nickel copper-clad composite powder, its core is copper powder particle, outer surface is coated one deck nickel, this composite powder can replace pure nickel powder, the mechanical impurity of copper powder, can significantly improve that conventional method obtains that the mobility of mixed-powder of nickel, copper is low, homogenieity (not forming segregation) and non-oxidizability, corrosion resistance and the problem that wears no resistance, can also reduce costs, improve productivity effect, there is good application prospect, thereby preparation technology and the powder metallurgy behavior thereof of research nickel copper-clad composite powder there are important market value and realistic meaning.
There is at present the method for much preparing nickel cladded type composite powder to have a lot, preparation method's patent of typical metal cladded type composite powder has at present: the patent of invention that publication number is CN1988973A provides a kind of preparation method of nickel-plated copper powder, it is catalyst that the method adopts palladium, and diamine (hydrazine) is prepared 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 diamine (hydrazine) on copper powder, to be coated one deck nickel for reducing agent; The patent of invention that publication number is 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 ℃, add electrolytic copper powder to regulate pH to 11.5-13.5, adopting diamine (hydrazine) is reducing agent, prepares nickel coated copper powder end; Above-mentioned several document is all used diamine (hydrazine) to make reducing agent to prepare nickel coated copper powder when end, and the sedimentation rate of this method nickel is relatively low, and complex process, cost be high, have the problems such as environmental pollution; Publication number is that the patent of invention of CN101733401A has also been mentioned a kind of prepare nickel coated copper powder under acidic bath condition method, copper powder after salt acid treatment is placed in to 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 nickel phosphorus copper-clad powder; Document " preparation of novel Ni-Cu composite deposite " has been introduced the technique of 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 ℃, current density 2-3A/dm
2but, at Copper Powder Surface, realize nickel plating object experiment condition harsh, the problem such as cost is high, complicated operation; Easy according to experimental implementation, the aspect considerations such as test efficiency raising, the present invention makes negative electrode with nickel plate and nickel screen respectively, by the homodisperse electroplate liquid of copper powder, Copper Powder Surface is carried out the coated processing of nickel under vigorous stirring, successfully realized in use for laboratory galvanoplastic and prepared the coated copper powder of nickel.Do not introduce impurity element, hydrogen loss, phosphorus content, mobility and apparent density all meet the requirement of high-performance monel powdered metallurgical material, its processing performance and physical property meet national standard, by SEM (comprising EDS), XRD analysis is electroplated the nickel copper-clad composite powder of producing, and finds that the coating of nickel copper-clad composite powder is pure nickel, and nickel is crystalline state, clad is even, in plating process, does not introduce impurity element.And gained powder is carried out to the test of chemistry and processing performance, and result shows: electroplate the nickel copper-clad composite powder of producing, the covering amount of its nickel is controlled, the requirement that is all up to state standards of the content of impurity element and hydrogen loss, and powder quality is good.
Summary of the invention
The method that the present invention selects plating to prepare nickel clad copper composite powder realizes by following scheme:
(1) electroplanting device
The experimental provision of electroplating mainly consists of the following components: electric source for electroplating, anode: select square nickel plate, negative electrode: select square nickel plate or the nickel screen of comparable size, electroplate liquid, magnetic stirring apparatus, pH test paper, electronic balance, 1000ml beaker.
(2) electro-plating method
The electroplate liquid that this experiment is used is a watt nickel (sulfate-chloride type) solution.Solution composition and technological specification are as shown in table 1 below:
Table 1 electroplate liquid is a watt nickel (sulfate-chloride type) solution ratio
In above-mentioned plating solution, nickelous sulfate is the main component of plating solution, it is the source of nickel ion, when the content of nickelous sulfate is low, solution dispersibility is good, and coating crystallization is careful, but cathode efficiency and limiting current density are low, deposition velocity is slow, and the content of nickelous sulfate is when high, allows the current density used large, deposition velocity is fast, but dispersibility is slightly poor; In plating solution, add appropriate nickel chloride and can effectively prevent anodic passivity; Owing to there being the side reaction of liberation of hydrogen in plating solution, therefore add boric acid to play cushioning effect to bath pH value, keep the pH value of plating solution relatively stable; In plating solution, add SDS(lauryl sodium sulfate) can be adsorbed on the tension force that cathode surface reduces interface between electrode and solution, thus make bubble easily leave electrode surface, prevent that pin hole from appearring in coating.
(3) preparation of plating solution
1, electronic balance accurately takes required chemical reagent, is accurate to 0.01g.
2, first measure half the water yield of required plating solution volume, add the nickelous sulfate, the nickel chloride that quantitatively take, stir lower until dissolve completely, obtain solution 1.
3, in other container, add suitable quantity of water, dissolve boric acid, after boric acid all dissolves, under stirring, added in solution 1.
4, with hydrochloric acid, regulate bath pH value to setting; Solution is poured into the volumetric flask of certain volume, then added the SDS quantitatively taking, with distilled water, regulate plating solution volume to setting; NiSO in plating solution now
4.6H
2o is 320g.L
-1, NiCl
2.6H
2o50g.L
-1, H
2bO
345g.L
-1, SDS0.1g.L
-1.
5, in plating solution, insert negative electrode nickel screen or nickel plate, anode nickel plates, add copper powder, in every liter of plating solution, add 30g copper powder, regulate electroplating parameter to desirable value, start plating, in plating process, use magnetic agitation always, guarantee that copper powder fully mixes, guarantee the even of plating.
6, after plating certain hour, powered-down, takes out cathode and anode, treats in beaker, after composite powder precipitation, to pour out plating solution, collects powder.
7, with distilled water, clean to neutral, with acetone, clean composite powder, dry.
(4) select different negative electrodes to produce nickel copper-clad composite powder
1, negative electrode is nickel plate
Negative electrode is selected nickel plate, in plating, find, only stick near the Copper Powder Surface of nickel cathode plate or minus plate and can realize the coated of nickel, copper powder color is from the initial brick-red silver gray that becomes, but because minus plate area is limited, also incomplete to the copper powder suction-operated in plating solution, so with regard to copper powder in general, plating amount is less, and plating amount reaches 5%.
2, negative electrode is nickel screen
On the basis of above-mentioned experiment, trying, it is larger to change the nickel plate as negative electrode into surface area, the nickel screen that adsorption capacity is stronger, found that in the quality of Copper Powder Surface electronickelling and greatly take on a new look, the most of color of copper powder of disperseing in plating solution after electroplating power supply is opened ten minutes all becomes grey, along with plating time lengthening, the copper powder in plating solution can be realized complete plating, and plating amount reaches 15%.
Described square nickel plate and nickel screen are of a size of 50mm*50mm*50mm, and the order number of nickel screen is 300 orders.
The inventive method adopts nickel plate first, or nickel screen is as electroplating cathode, utilize mechanical agitation to need the copper powder of plating fully to mix with electroplate liquid, in the process of electroplating, utilize nickel plate and the larger reference area of nickel screen fully to attract copper powder in electroplate liquid to negative electrode, thereby realize in Copper Powder Surface plated nickel, while having overcome traditional plating legal system for cladding powder, negative electrode is difficult to collect plated whiting or usings plating powder directly as negative electrode, be difficult to the deficiency realizing; Application this method can realize fast at the coated nickel completely of Copper Powder Surface, and ambrose alloy combination interface is pure, the composite powder of preparation is only by nickel, copper two phase compositions, nickel is crystalline state, meet the requirement of high-performance monel powdered metallurgical material, and the preparation of negative electrode is simple, with for the production of thermopnore or have the negative electrode of mechanical driving device to be more easy to realize in laboratory the preparation that galvanoplastic are prepared nickel copper-clad composite powder.
Accompanying drawing explanation
The microscopic appearance figure that Figure 1 shows that the nickel copper-clad composite powder that under ESEM, galvanoplastic are produced, (a) is starting powder; (b) be powder after electroplating; As can be seen from the figure, dendroid pattern through the composite powder particle after electroplating still retains, relatively can obviously find out with the pattern of the original copper powder of Fig. 1 (a), the passivation that becomes of the branch pattern of the powder after plating, powder particle is grown up, by the more original copper powder rough surface of powder surface after plating, there is born of the same parents' shape thing to occur; Due to stirring action violent in plating process, make original powder morphology suffer certain destruction, there is fracture and incomplete situation in powder particle as can be seen from Figure simultaneously.
Fig. 2 is copper, the nickel element face distribution scintigram that galvanoplastic are produced nickel copper-clad composite powder; The SEI figure that Fig. 2 (a) is composite powder, Fig. 2 (b) is the scanning of copper coin vegetarian noodles, Fig. 2 (c) is nickel element face scintigram.
Fig. 3 is the XRD figure that galvanoplastic are produced nickel copper-clad composite powder, the nickel copper-clad composite powder of galvanoplastic being produced by X diffraction carries out the analysis of phase, its diffracting spectrum can be found out by diffraction analysis as shown in Figure 3 simultaneously, in the nickel copper-clad composite powder of producing by plating, nickel, copper all exist with crystalline state, and only there are nickel, copper two phase compositions, illustrate while electroplating and do not introduce other impurity phase, and composite powder is oxidized.
The specific embodiment
Below in conjunction with example, the present invention will be described, but the present invention is not subject to any restriction of these embodiment.
Example 1: use nickel screen to make negative electrode, prepare nickel coated copper powder end.
1) electronic balance accurately takes required chemical reagent: NiSO
4.6H
2o:320g, NiCl
2.6H
2o:50g, H
2bO
3: 45g, SDS:0.1g, be accurate to 0.01g;
2), first measure half the water yield of required plating solution volume, add the nickelous sulfate, the nickel chloride that quantitatively take, under vigorous stirring until dissolve completely;
3), in other container, add suitable quantity of water, dissolve boric acid, after boric acid all dissolves, under stirring, added solution 2) in;
4), with hydrochloric acid, regulate bath pH value to setting 4; Solution is poured into the volumetric flask of certain volume, then added the SDS quantitatively taking, with distilled water, regulate plating solution volume to setting 1L, then be poured into beaker;
5), in being housed, inserts by the beaker of plating solution negative electrode nickel screen, Nickel Anode Plate, pack copper powder 30g into, use magnetic agitation, guarantee that copper powder fully mixes with plating solution, temperature rises to 50 degree maintenance, electroplating parameter is adjusted to desirable value, voltage 4.5V, current density 1A, start plating, in plating process, keep magnetic agitation always, guarantee the even of plating, 15 minutes plating time;
6), plating is after 15 minutes, powered-down, takes out cathode and anode, treats in beaker, after composite powder precipitation, to pour out plating solution, collects powder;
7), with distilled water, clean to neutral, with acetone, clean composite powder, dry, to weigh, plating amount reaches 15%.
Embodiment 2: use nickel plate to make negative electrode, prepare nickel coated copper powder end.
1) electronic balance accurately takes required chemical reagent: NiSO
4.6H
2o:320g, NiCl
2.6H
2o:50g, H
2bO
3: 45g, SDS:0.1g, be accurate to 0.01g;
2), first measure half the water yield of required plating solution volume, add the nickelous sulfate, the nickel chloride that quantitatively take, under vigorous stirring until dissolve completely;
3), in other container, add suitable quantity of water, dissolve boric acid, after boric acid all dissolves, under stirring, added solution 2) in;
4), with hydrochloric acid, regulate bath pH value to setting 4; Solution is poured into the volumetric flask of certain volume, then added the SDS quantitatively taking, with distilled water, regulate plating solution volume to setting 1L, then be poured into beaker;
5), in being housed, inserts by the beaker of plating solution cathode nickel plate, anode nickel plates, pack copper powder 30g into, use magnetic agitation, guarantee that copper powder fully mixes with plating solution, temperature rises to 50 degree maintenance, electroplating parameter is adjusted to desirable value, voltage 4.5V, current density 1A, start plating, in plating process, keep magnetic agitation always, guarantee the even of plating, 15 minutes plating time;
6), plating is after 15 minutes, powered-down, takes out cathode and anode, treats in beaker, after composite powder precipitation, to pour out plating solution, collects powder;
7), with distilled water, clean to neutral, with acetone, clean composite powder, dry, to weigh, plating amount reaches 5%.
Table 1 processing performance and chemical property index determining result
According to national standard, its performance to be tested, result is as shown in table 1; Phosphorus content, mobility and apparent density all meet the requirement of high-performance monel powdered metallurgical material.
Claims (8)
1. a method of efficiently preparing nickel clad copper composite powder that is applicable to laboratory, it is characterized in that: in the process of electroplating, negative electrode is selected nickel screen or nickel plate, in electroplate liquid, by magnetic agitation, fully mixing copper powder electroplates, guarantee the copper powder Contact cathod of trying one's best, realize at Copper Powder Surface and electroplate plated nickel.
2. a kind of sonochemistry as claimed in claim 1 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that: described nickel plate and nickel screen, for square, are of a size of 50mm*50mm*0.5mm.
3. a kind of sonochemistry as claimed in claim 1 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that: select nickel screen as negative electrode, be of a size of 50mm*50mm*0.5mm, the order number of nickel screen is 300 orders.
4. a kind of sonochemistry as claimed in claim 1 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that concrete steps are as follows:
(1) first measure half the water yield of required plating solution volume, add the nickelous sulfate, the nickel chloride that quantitatively take, stir lower until dissolve completely, obtain solution 1;
(2) in other container, add suitable quantity of water, dissolve boric acid, after boric acid all dissolves, under stirring, added in solution 1;
(3) with hydrochloric acid, regulate bath pH value to setting; Solution is poured into the volumetric flask of certain volume, then added the SDS quantitatively taking, with distilled water, regulate plating solution volume to setting; NiSO in plating solution now
4.6H
2o is 320g.L
-1, NiCl
2.6H
2o50g.L
-1, H
2bO
345g.L
-1, SDS0.1g.L
-1;
(5) in plating solution, insert negative electrode nickel screen or nickel plate, anode nickel plates, add copper powder, regulate electroplating parameter to desirable value, start plating, in plating process, use magnetic agitation always, guarantee that copper powder fully mixes, guarantee the even of plating;
(6) after plating certain hour, powered-down, takes out cathode and anode, treats in beaker, after composite powder precipitation, to pour out plating solution, collects powder;
(7) with distilled water, clean to neutral, with acetone, clean composite powder, dry.
5. a kind of sonochemistry as claimed in claim 4 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that: the setting of described pH is 3.8～4.4.
6. a kind of sonochemistry as claimed in claim 4 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that: in every liter of plating solution, add 30g copper powder.
7. a kind of sonochemistry as claimed in claim 4 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that: described adjusting electroplating parameter to desirable value refers to: 45～60 ℃ of temperature, current density 1A, voltage 4～5V.
8. a kind of sonochemistry as claimed in claim 4 is efficiently prepared the method for nickel clad copper composite powder, it is characterized in that: described electroplating time is 5-30min.
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Cited By (5)
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|---|---|---|---|---|
| CN104084580A (en) * | 2014-06-16 | 2014-10-08 | 华南理工大学 | Preparation method of superfine nickel coated copper powder for electronic industry |
| CN104907581A (en) * | 2015-06-20 | 2015-09-16 | 浙江大学 | Preparation method of material in which globular micron stannic oxide is loaded with micron and nano silver particles |
| CN106312055A (en) * | 2016-08-31 | 2017-01-11 | 陕西斯瑞新材料股份有限公司 | Preparing method of copper-coated chromium alloy powder and copper-chromium contact |
| CN110802225A (en) * | 2019-10-11 | 2020-02-18 | 广州盛门新材料科技有限公司 | Preparation method of copper-coated graphene |
| CN114833339A (en) * | 2022-05-06 | 2022-08-02 | 中国铁道科学研究院集团有限公司 | High-temperature-resistant powder metallurgy friction material and temperature-resistant brake pad as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106312055A (en) * | 2016-08-31 | 2017-01-11 | 陕西斯瑞新材料股份有限公司 | Preparing method of copper-coated chromium alloy powder and copper-chromium contact |
| CN106312055B (en) * | 2016-08-31 | 2018-06-05 | 陕西斯瑞新材料股份有限公司 | Copper-clad evanohm powder and its copper chromium contact preparation method |
| CN110802225A (en) * | 2019-10-11 | 2020-02-18 | 广州盛门新材料科技有限公司 | Preparation method of copper-coated graphene |
| CN114833339A (en) * | 2022-05-06 | 2022-08-02 | 中国铁道科学研究院集团有限公司 | High-temperature-resistant powder metallurgy friction material and temperature-resistant brake pad as well as preparation method and application thereof |
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Application publication date: 20140305 |