CN103752842A - Substitution and chemistry deposition compound preparation method for nano silver coated copper powder - Google Patents
Substitution and chemistry deposition compound preparation method for nano silver coated copper powder Download PDFInfo
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- CN103752842A CN103752842A CN201310552029.6A CN201310552029A CN103752842A CN 103752842 A CN103752842 A CN 103752842A CN 201310552029 A CN201310552029 A CN 201310552029A CN 103752842 A CN103752842 A CN 103752842A
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Abstract
The invention discloses a method for preparing nano silver coated copper powder for conductive filler through reduction for a plurality of components; the method comprises the steps of preparing nano-copper powder through hydrate reduction method, adding Tollens' reagent and formaldehyde into the reaction system without separation and purification, and plating the silver on the surface of copper for preparing silver coated copper powder for electrocondution slurry through substitution-chemistry reduction compound method. The copper powder prepared by the invention can be plated with silver without separation and purification condition, so the pickling and sensitization process can be saved, the ammonium hydroxide is used for adjusting the pH of the solution as well as chelating agent for fitting the copper and silver, and the second type chelating agent is not needed, so the synthetic process is simplified and the cost is reduced. The silver coated copper powder is good in dispersibility, oxidation resistance and thermal stability, the electrical resistivity is 1*10<6> to 1*10<4>ohm*m, the nano silver coated copper powder is the spherical particle with core/shell structure, the core is copper and the shell is silver, the grain size is 20-100nm, the plating layer is even and compact and the silver content is 25-60%.
Description
Technical field
The present invention relates to a kind of method of utilizing multicomponent reduction to prepare conductive filler Nano Silver copper-clad powder.
Background technology
The development of nanometer technology, realized dispersed in macromolecule resin of conducting metal, form conductive filler, can be made into conducting resinl, electrically-conducting paint, conductive rubber etc., it is widely used in the fields such as the conduction, electromagnetic shielding of all departments such as electronics, electromechanics, communication, printing, Aero-Space, weapons.Conductive phase is main mainly with platinum, palladium, gold and the noble metal powder such as silver-colored greatly, and wherein the research of Nano Silver is the most deep, but its self-defect expensive and silver-colored migration has limited its application in some field.For this problem, people have researched and developed electrical-conductive nanometer copper powder, but its antioxygenic property is poor, and conductance significantly declines, and can not meet the needs of higher-end businesses.At coated with uniform one deck silver of copper powder, the silver-colored copper-clad particle of this core/shell structure has not only kept physics and the chemical property of original metallic copper core, there is the good metallic character of silver coating simultaneously, improve non-oxidizability and heat endurance, received gradually in recent years the concern of researcher.
The preparation method of Nano Silver copper-clad mainly contains: displacement method, chemical reduction method, displacement and chemical deposition composite algorithm, electrochemical process, atomized molten method, vapor phase method, pulsed laser deposition etc.Displacement method is that copper powder larger current potential is directly inserted to silver-colored solution, and due to the electromotive force existing between the two, silver ion is reduced at Copper Powder Surface, forms coating.Displacement method is because cuprammonium ion is in the absorption of Copper Powder Surface, and the silver-coated copper powder of structure is interspersed in normal formation.Reducing process is that to utilize reducing agent be silver-colored simple substance by the silver ion reduction in silver-colored solution, and is deposited on Copper Powder Surface, forms coating.Reducing process need be carried out pickling by copper powder, after sensitization, activation, inserts reductant solution, complex process again.Replaced with the set of chemical deposition composite algorithm the feature of displacement method and reducing process, first with copper powder replacement ag plating, be equivalent to activation process, recycling reducing process is silver-plated to powder.Chemical method is silver-plated because reaction speed comparatively fast can cause the unstable of plating solution, generally by main salting liquid and reductant solution separate configuration, in order to make silver plating reaction velocity-stabilization, obtains the coating of coated even compact, and the adding technology that feeds intake is particularly crucial.
Summary of the invention
The present invention adopts displacement and chemical deposition composite algorithm to utilize multicomponent reduction to prepare Nano Silver copper-clad.First copper ammon solution is prepared to copper nanoparticle with hydrazine hydrate reduction, under the condition of not separation and purification, in system, add silver ammino solution, now copper-Yin displacement reaction and excess hydrazine hydrate reduction is silver-plated to be carried out simultaneously, then adds formaldehyde reduction further to improve silver content, impels coating even compact.
The present invention relates to following course of reaction altogether: 1, hydrazine hydrate reduction cuprammonium 2, copper powder reduce silver-colored ammonia 3, excess hydrazine hydrate and reduce silver-colored ammonia 4, formaldehyde and reduce silver-colored ammonia.By adjusting synthetic technological condition, obtain target product, the most at last its requirement of ITO conductive film serigraphy that has been dispersed in epoxide-resin glue success reality.
Reaction equation is as follows:
2Cu(NH
3)
4 2++N
2H
4+4OH
-→2Cu+8NH
3+N
2+4H
2O.....................................(1)
2Ag(NH
3)
2 ++Cu→2Ag+Cu(NH
3)
4 2+......................................................(2)
4Ag(NH
3)
2 +N
2H
4+4OH
-→4Ag+8NH
3+N
2+4H
2O....................................(3)
4Ag(NH
3)
2 +HCHO+6OH
-→4Ag+8NH
3+4H
2O+CO
3 2-.................................(4)
Concrete implementation step is as follows:
(1) preparation of copper powder
Dispersant and Tong Yuan are dissolved in deionized water, with concentrated ammonia liquor, are adjusted to pH=9～12 and obtain copper ammon solution I; Dispersant and reducing agent I are dissolved in deionized water obtaining to reducing solution II; Under oxygen free condition, solution II is slowly dropped in solution I, 15～50 ℃ of reaction temperatures, reaction 1～4h finishes; Obtain aubergine copper powder suspension.
(2) preparation of silver-coated copper powder
Dispersant and Yin Yuan are dissolved in deionized water, with concentrated ammonia liquor regulate pH=10～12 silver ammino solution III; Under oxygen free condition, solution III is slowly splashed in (1) reacted solution, 15～50 ℃ of reaction temperatures, inject reducing agent II in the backward reaction system of reaction 1～4h, continue reaction 1～4h, and solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
(3) step (1), (2) described dispersant are one or more in polyvinylpyrrolidone, softex kw, dodecyl sodium sulfate, neopelex, and consumption is 0～25g;
(4) the described copper source of step (1) comprises copper sulphate, copper nitrate, one or more in copper chloride;
(5) the described silver-colored source of step (2) comprises silver nitrate, silver oxide, and one or more in silver chlorate, the mol ratio in Tong Yuan and silver-colored source is 1:1～5;
(6) the described reducing agent I of step (1) is 80% hydrazine hydrate, and the mol ratio of copper source and hydrazine hydrate is 1:10～30;
(7) the described reducing agent II of step (2) is 30% formaldehyde, and the mol ratio of silver-colored source and formaldehyde is 1:1～5.
The present invention makes copper powder by oneself can be silver-plated under the condition of not separation and purification, saved pickling, activation process, and ammoniacal liquor, not only for regulator solution pH but also serve as chelating agent and coordinate with copper silver ion, is not introduced the second chelating agent, has simplified synthesis technique, reduces costs.
Gained silver-coated copper powder of the present invention end good dispersion, has good anti-oxidant and thermal stability, resistivity 1 × 10
-6～1 × 10
-4Ω m, core/shell structure spheric granules, kernel is copper, shell be silver, particle diameter between 20-100nm, coating even compact, silver content is 25%～60%.By Fig. 1 copper nanoparticle and nanometer silver-coated copper powder XRD collection of illustrative plates and Fig. 2 silver-coated copper powder end SEM figure and the known products obtained therefrom of partial enlarged drawing, be silver-colored copper-clad thing phase, other impurity peaks appearance such as oxide-free, powder is uniformly dispersed, the smooth densification of coating surface.
Accompanying drawing explanation
Fig. 1 is copper nanoparticle and nanometer silver-coated copper powder XRD spectra.
Fig. 2 is silver-coated copper powder end SEM figure and partial enlarged drawing.
the specific embodiment
Embodiment 1
By polyvinylpyrrolidone (5g) and copper sulphate (0.8g, 5mmol) be dissolved in 500ml ionized water, with concentrated ammonia liquor, be adjusted to pH=12 and obtain solution I, polyvinylpyrrolidone (5g) and 80% hydrazine hydrate (3.125g, 0.05mol) are dissolved in 500ml deionized water obtaining to solution II, under oxygen free condition, solution II are slowly dropped in solution I, 15 ℃ of reaction temperatures, magnetic agitation, 1h dropwises, and continues reaction 3h and obtains aubergine copper powder suspension.By polyvinylpyrrolidone (25g) and silver nitrate (1.7g, 0.01mol) be dissolved in 500ml deionized water, with concentrated ammonia liquor adjusting, pH=10 obtains silver ammino solution III, under oxygen free condition, solution III is slowly splashed in above-mentioned copper powder suspension, in the backward reaction system of reaction 2h, inject 30% formaldehyde (0.5g, 5mmol), continue reaction 2h, solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
Embodiment 2
By softex kw (15g) and copper chloride (1.35g, 0.01mol) be dissolved in 500ml deionized water, with concentrated ammonia liquor, be adjusted to pH=9 and obtain copper ammon solution I, by softex kw (15g) and 80% hydrazine hydrate (12.5g, 0.2mol) be dissolved in 500ml deionized water obtaining reducing solution II, under oxygen free condition, solution II is slowly dropped in solution I, 45 ℃ of reaction temperatures, magnetic agitation, 2h dropwises, and continues reaction 2h and obtains aubergine copper powder suspension.By softex kw (15g) and silver oxide (2.32g, 0.01mol) add in 500ml deionized water, with concentrated ammonia liquor adjusting, pH=11 obtains silver ammino solution III, under oxygen free condition, solution III is slowly splashed in above-mentioned copper powder suspension, in the backward reaction system of reaction 1h, inject 30% formaldehyde (5g, 0.05mol), continue reaction 1h, solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
By dodecyl sodium sulfate (15g) and copper nitrate (1.88g, 0.01mol) be dissolved in 500ml ionized water, with concentrated ammonia liquor, be adjusted to pH=10 and obtain copper ammon solution I, by dodecyl sodium sulfate (15g) and 80% hydrazine hydrate (18.75g, 0.3mol) be dissolved in 500ml deionized water obtaining reducing solution II, under oxygen free condition, solution II is slowly dropped in solution I, 35 ℃ of reaction temperatures, magnetic agitation, 2h dropwises, and continues reaction 2h and obtains aubergine copper powder suspension.By dodecyl sodium sulfate (15g) and silver oxide (4.64g, 0.02mol) add in 500ml deionized water, with concentrated ammonia liquor adjusting, pH=11.5 obtains silver ammino solution III, under oxygen free condition, solution III is slowly splashed in above-mentioned copper powder suspension, in the backward reaction system of reaction 2h, inject 30% formaldehyde (5g, 0.05mol), continue reaction 2h, solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
Embodiment 4
By polyvinylpyrrolidone (25g) and copper chloride (2.7g, 0.02mol) be dissolved in 500ml ionized water, with dense water, be adjusted to pH=11 and obtain copper ammon solution I, by polyvinylpyrrolidone (25g) and 80% hydrazine hydrate (31.25g, 0.5mol) be dissolved in 500ml deionized water obtaining reducing solution II, under oxygen free condition, solution II is slowly dropped in solution I, 50 ℃ of reaction temperatures, magnetic agitation, 2h dropwises, and continues reaction 2h and obtains aubergine copper powder suspension.By silver chlorate (14.35g, 0.1mol) add in 500ml deionized water, with concentrated ammonia liquor adjusting, pH=12 obtains silver ammino solution III, under oxygen free condition, solution III is slowly splashed in above-mentioned reacted solution, in the backward reaction system of reaction 1h, inject 30% formaldehyde (3g, 0.03mol) continue reaction 4h, solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
Embodiment 5
By dodecyl sodium sulfate (10g), neopelex (10g) and copper sulphate (3.2g, 0.02mol) be dissolved in 500ml ionized water, with concentrated ammonia liquor, be adjusted to pH=11.5 and obtain copper ammon solution I, by dodecyl sodium sulfate (10g), neopelex (10g) and 80% hydrazine hydrate (25g, 0.4mol) be dissolved in 500ml deionized water obtaining reducing solution II, under oxygen free condition, solution II is slowly dropped in solution I, 30 ℃ of reaction temperatures, magnetic agitation, 3h dropwises, continue reaction 1h and obtain aubergine copper powder suspension.By dodecyl sodium sulfate (10g), neopelex (10g) and silver nitrate (10.2g, 0.06mol) add in 500ml deionized water, with concentrated ammonia liquor adjusting, pH=11.5 obtains silver ammino solution III, under oxygen free condition, solution III is slowly splashed in above-mentioned reacted solution, in the backward reaction system of reaction 2h, inject 30% formaldehyde (2.5g, 0.025mol), continue reaction 2h, solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
Embodiment 6
By polyvinylpyrrolidone (10g), dodecyl sodium sulfate (5g) and copper sulphate (2g, 0.0125mol) be dissolved in 500ml ionized water, with concentrated ammonia liquor, be adjusted to pH=10.5 and obtain copper ammon solution I, by polyvinylpyrrolidone (10g), dodecyl sodium sulfate (5g) and 80% hydrazine hydrate (12.5g, 0.2mol) be dissolved in 500ml deionized water obtaining reducing solution II, under oxygen free condition, solution II is slowly dropped in solution I, 30 ℃ of reaction temperatures, magnetic agitation, 3h dropwises, and continues reaction 1h and obtains aubergine copper powder suspension.By polyvinylpyrrolidone (10g), dodecyl sodium sulfate (5g) and silver nitrate (6.8g, 0.04mol) add in 500ml deionized water, with concentrated ammonia liquor adjusting, pH=11 obtains silver ammino solution III, under oxygen free condition, solution III is slowly splashed in above-mentioned reacted solution, in the backward reaction system of reaction 1h, inject 30% formaldehyde (2.5g, 0.025mol) continue reaction 3h, solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
Claims (7)
1. utilize displacement and chemical deposition composite algorithm to prepare the method for Nano Silver copper-clad powder, it is characterized in that: comprise following course of reaction: 1, hydrazine hydrate reduction cuprammonium 2, copper powder reduce silver-colored ammonia 3, excess hydrazine hydrate and reduce silver-colored ammonia 4, formaldehyde and reduce silver-colored ammonia.
2. preparation method according to claim 1, concrete implementation step is as follows, it is characterized in that:
(1) preparation of copper powder
Dispersant and Tong Yuan are dissolved in deionized water, with concentrated ammonia liquor, are adjusted to pH=9～12 and obtain copper ammon solution I; Dispersant and reducing agent I are dissolved in deionized water obtaining to reducing solution II; Under oxygen free condition, solution II is slowly dropped in solution I, 15～50 ℃ of reaction temperatures, reaction 1～4h finishes; Obtain aubergine copper powder suspension.(2) preparation of silver-coated copper powder
Dispersant and Yin Yuan are dissolved in deionized water, with concentrated ammonia liquor regulate pH=10～12 silver ammino solution III; Under oxygen free condition, solution III is slowly splashed in (1) reacted solution, 15～50 ℃ of reaction temperatures, inject reducing agent II in the backward reaction system of reaction 1～4h, continue reaction 1～4h, and solution becomes bois de rose or grey from aubergine.Reacted solution centrifugal is separated to (13000r/min), 30ml water washing 3～4 times for gained solid, 30ml ethanol washing 3～4 times, at 45 ℃, vacuum drying 4h obtains Nano Silver copper-clad powder.
3. preparation method according to claim 2, it is characterized in that: step (1), (2) described dispersant are one or more in polyvinylpyrrolidone, softex kw, dodecyl sodium sulfate, neopelex, and consumption is 0～25g.
4. preparation method according to claim 2, is characterized in that: the described copper source of step (1) comprises copper sulphate, copper nitrate, one or more in copper chloride.
5. preparation method according to claim 2, is characterized in that: the described silver-colored source of step (2) comprises silver nitrate, silver oxide, and one or more in silver chlorate, the mol ratio in Tong Yuan and silver-colored source is 1: 1～5.
6. preparation method according to claim 2, is characterized in that: the described reducing agent I of step (1) is 80% hydrazine hydrate, and the mol ratio of copper source and hydrazine hydrate is 1: 10～30.
7. preparation method according to claim 2, is characterized in that: the described reducing agent II of step (2) is 30% formaldehyde, and the mol ratio of silver-colored source and formaldehyde is 1:1～5.
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| CN108080651A (en) * | 2017-12-14 | 2018-05-29 | 湖南兴威新材料有限公司 | The preparation method of electric slurry nanometer silver-coated copper powder |
| CN110842190A (en) * | 2019-10-11 | 2020-02-28 | 云南大学 | Preparation method of silver-coated copper powder |
| CN110842190B (en) * | 2019-10-11 | 2021-10-15 | 云南大学 | Preparation method of silver-coated copper powder |
| CN111304640A (en) * | 2020-03-10 | 2020-06-19 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Silver-coated copper powder, preparation method thereof and electronic paste |
| CN111304640B (en) * | 2020-03-10 | 2022-03-18 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Silver-coated copper powder, preparation method thereof and electronic paste |
| CN112355322A (en) * | 2020-11-18 | 2021-02-12 | 深圳市夏特科技有限公司 | Preparation device and preparation method of flaky silver-coated copper powder |
| CN112355322B (en) * | 2020-11-18 | 2023-04-07 | 深圳市夏特科技有限公司 | Preparation device and preparation method of flaky silver-coated copper powder |
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