CN101758230A - Method for chemical plating of metal on particle surface - Google Patents
Method for chemical plating of metal on particle surface Download PDFInfo
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- CN101758230A CN101758230A CN200910196277A CN200910196277A CN101758230A CN 101758230 A CN101758230 A CN 101758230A CN 200910196277 A CN200910196277 A CN 200910196277A CN 200910196277 A CN200910196277 A CN 200910196277A CN 101758230 A CN101758230 A CN 101758230A
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Abstract
The invention discloses a method for chemical plating of metal on the particle surface. An ultrasonic oscillation generator is put into a mechanical stirring paddle, a mechanical agitator is combined with a built-in ultrasonator, then the powder particles are fully dispersed by adding the reaction components by a liquid-phase spraying method, and the reaction in the plated area is uniform and stable, therefore, the purpose of uniformly-distributed coating powder particles is achieved. The method of combining the mechanical agitator and the built-in ultrasonator is adopted, thereby effectively improving the dispersion efficiency and solving the problem of powder particle agglomeration; and the method of adding the reaction components by liquid-phase spraying is adopted, therefore, the reaction in the chemical plating solution is uniform, and the defects of the unstable plating solution and the uneven surface plating of the powder particles can be avoided. The method has the advantages of simple and convenient operation, uniform dispersion of the powder particles, complete coating and the like, and effectively solves the problems of agglomeration, uneven surface coating and instability of the plating solution due to the excessively high plating speed during the chemical plating of the powder particles.
Description
Technical field
The present invention relates to the method in a kind of material surface modifying technology field, specifically, what relate to is a kind of method of chemical plating of metal on particle surface.
Background technology
The particle chemical plating of metal is a kind of effective surface modification means, by often improving the material surface performance on the basis that keeps original material property at pottery or surface of metal particles chemical plating of metal.For example, will make ceramic grain surface conduct electricity, and easily combine keeping changing the ceramic grain surface performance under ceramic high rigidity own, the high strength characteristics prerequisite with metal at metals such as ceramic grain surface plated copper or silver.At copper particle surface plate silver metal, will greatly increase copper particle surface electric conductivity and make the particle non-oxidizability strengthen.Therefore chemical plating of metal on particle surface has been widely used in aspects such as new material manufactures, composite material interface improvement.Yet along with improving constantly of specification requirement, now gradually need be on the particle of sub-micron or Nano grade chemical plating of metal.To the difficult point of sub-micron or nano grain surface chemical plating have following some: one, the tiny surface area that causes of particle is huge, makes particle reunite easily and be difficult for disperseing, and this just causes chemical plating inhomogeneous easily; Two, because granule surface area is huge, make the chemical plating fluid system become unstable, in the plating process, cause selfdecomposition or reaction speed too fast easily, thus cause plating do not go up or plating incomplete.Mainly as follows for the research of submicron particles surface chemistry plating both at home and abroad;
1) Qu Zhanmin; Powdered graphite chemical nickel plating and chemical silvering technology; Electroplate and finish 29 (6) 2007;
2) Shen Pei; The important process condition of plating bath stirring-chemical nickel plating; Paint spraying and plating 3 (4) 2005;
3) Cai Kefeng; At ceramic powders surface chemical plating cladding metal; Electroplate and environmental protection 14 (2) 1994;
4) Zhang Bangwei; The plating technology parameter is to the influence of electroless deposition speed; Electroplate and environmental protection 19 (5) 1999;
Have following several for the main solution of these two problems as can be known from above document: 1) chemical plating fluid, add dispersant, can reduce the generation of agglomeration traits so relatively, but can influence the adhesion of chemical plating of metal and original particle.2) adopt the way of stirring and ultrasonic concussion combination, but generally be that ultrasonic concussion places outside the container now, its concussion effect greatly weakens.3) adopt and to slow down the solution drip velocity and solve the too fast plating problem of non-uniform of reaction, but owing to there is excessive concentration gradient in reactant liquor, therefore simple is to be difficult to overcome the above problems by controlling adding speed.
Summary of the invention
The present invention is directed to deficiency and defective that above-mentioned prior art exists, a kind of method of chemical plating of metal on particle surface be provided, efficiently solve in the powder particle chemical plating reunite, coating surface is inhomogeneous, the plating excessive velocities causes the plating bath problem of unstable.
For achieving the above object, the present invention is placed on ultrasonic concussion generating means in the mechanical agitation slurry, adopts mechanical agitation to combine with built-in ultrasonic concussion; And the mode that adopts the liquid phase spraying to add reactive component, powder particle is fully disperseed, the reaction of plating zone is uniform and stable, thereby reaches the purpose that powder particle surface evenly coats.
Above-mentioned particle is applicable to all ceramic powder particles, and its particle mean size is between 0.01 μ m-100 μ m, and institute's metal lining can be realized the metal of chemical plating for all.
When the present invention specifically implements, carry out according to following steps:
The first step is at first carried out surface treatment with powder particle, filters afterwards and with washed with de-ionized water three times;
Described surface treatment, its mode be pickling sensitization activation processing or directly adopt pickling processes, and its objective is increases metal lining and by the adhesion between the plating powder particle surface.
In second step, disperse in the reductant solution with the adding of the powder particle after surface treatment chemical plating fluid;
Described dispersion, the method that it adopts built-in ultrasonic concussion to combine with mechanical agitation, ultrasonic rocking equipment places in the mechanical agitation slurry; Control the powder degree of scatter by adjusting mechanical agitation speed, ultrasonic concussion frequency.Mixing speed is 50-500 rev/min, and ultrasonic concussion frequency is 15KHz-100KHz.
The 3rd goes on foot, and the main salting liquid in the chemical plating fluid system is added into carry out plating in the reductant solution;
Described interpolation, its mode are the liquid phase spraying, and spray velocity is adjustable, and spray velocity was at 5ml-100ml/ minute.
The 4th step, the powder particle filtration drying that chemistry is covered to complete.
Particle surface chemical plating method of the present invention, because the method that has adopted mechanical agitation to combine with built-in ultrasonic concussion, thereby effectively improved dispersion efficiency, solved the problem that powder is reunited.And method by adopting the liquid phase spraying to add reactive component; make that reaction evenly in the chemical plating fluid system; can avoid plating bath instability, the uneven shortcoming of powder particle surface plating; have easy and simple to handle, particle is uniformly dispersed, coat advantages such as complete, efficiently solve in the powder particle chemical plating reunite, coating surface is inhomogeneous, the plating excessive velocities causes the plating bath problem of unstable.
Description of drawings
Fig. 1 is mechanical agitation and ultrasonic concussion and a liquid phase spraying schematic diagram in the embodiment of the invention
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are done one and describe in detail, following embodiment as the usefulness of understanding technical solution of the present invention, is not to be used to limit scope of the present invention just.
As shown in Figure 1, be used to illustrate the operating process of following examples of the present invention.
As shown in Figure 2, mechanical agitation and ultrasonic concussion and liquid phase spraying schematic diagram in the embodiment of the invention, wherein: 1,2-stirring arm positive and negative electrode; 12,13-spraying apparatus positive and negative electrode; 10, the ultrasonic concussion equipment of 11-positive and negative electrode; The 3-conduit; The 4-reductant solution; 5-whiting to be plated end; 6-master's salting liquid; Built-in ultrasonic concussion hole on the 7-stirring arm; The 8-stirring arm; The 9-sprayer unit.At first whiting to be plated end and reductant solution are packed in the use in the container, connect positive and negative electrode running stirring arm and built-in Vltrasonic device thereof afterwards, then main salting liquid is imported from conduit, and the unlatching sprayer unit, main salting liquid joined with vaporific form carry out chemical plating in the reductant solution.
Embodiment one
With average grain diameter is that to coat the Ag metal be example for the WC powder particle surface of 0.01 μ m
At first 5gWC powder particle (granularity is 0.01 μ m) is placed 5% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.
Powder particle behind the suction filtration is poured in the hydrazine hydrate solution of 500ml, its concentration is 3ml/L, and regulating pH value with ammoniacal liquor is 8, and mixing speed is 500 rev/mins, and ultrasonic concussion frequency is 100KHz, stirs ultrasonic concussion 15 minutes.
Be that 10g/L liquor argenti nitratis ophthalmicus 500ml adds with Sprayable then with concentration, liquor argenti nitratis ophthalmicus adding speed is 5ml/min, treat that chemical plating fully after, suction filtration obtains the good WC powder particle of plating, and with deionized water rinsing three times.
Afterwards that plating is good WC powder particle places vacuum, 100 ℃ of dryings 24 hours.The WC powder particle that is obtained coats evenly, and the Ag coating thickness is 0.5-0.6 μ m, bath stability in the plating process.
Embodiment two
With average grain diameter is that to coat the Ag metal be example for the WC powder particle surface of 1 μ m
At first 15g WC powder particle (granularity is 1 μ m) is placed 5% salpeter solution, stirring and washing 5 minutes adopts suction filtration after the washed with de-ionized water three times then.
Powder particle behind the suction filtration is poured in the 500ml hydrazine hydrate solution, its concentration is 6ml/L, regulating pH value with ammoniacal liquor is 10, stir ultrasonic concussion, the 500ml liquor argenti nitratis ophthalmicus that with concentration is 30g/L then adds with Sprayable, silver nitrate adds speed at 30ml/L, and mixing speed is 200 rev/mins, and ultrasonic concussion frequency is 15KHz.
After treating that chemical plating is fully, suction filtration obtains the good WC powder particle of plating, and with deionized water rinsing three times.
Afterwards that plating is good WC powder particle places vacuum, 150 ℃ of dryings 24 hours.The WC powder particle that is obtained coats evenly, and the Ag coating thickness is 0.8-1 μ m, bath stability in the plating process.
Embodiment three
With average grain diameter is that to coat the Ag metal be example for the SiC powder particle surface of 2 μ m
At first 8g SiC powder particle (granularity is 2 μ m) is placed 10% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.Powder particle behind the suction filtration is carried out the sensitization activation processing, adopt 15%SnCl
2Solution sensitization and 20%PdCl solution activation processing are used washed with de-ionized water three times afterwards.
Afterwards the above-mentioned powder particle of handling well is poured in the 500ml hydrazine hydrate solution, its concentration is 4.5ml/L, and regulating pH value with ammoniacal liquor is 9, stirs ultrasonic concussion.Be that the 15g/L liquor argenti nitratis ophthalmicus adds with Sprayable then with 500ml concentration, silver nitrate adds speed at 45ml/min, and mixing speed is 100 rev/mins, and ultrasonic concussion frequency is 30KHz.
After treating that chemical plating is fully, suction filtration obtains the good SiC powder particle of plating, and with deionized water rinsing three times.
Afterwards that plating is good SiC powder particle places vacuum, 100 ℃ of dryings 24 hours.The SiC powder particle that is obtained coats evenly, and the Ag coating thickness is 0.8-1 μ m, bath stability in the plating process.
Embodiment four
With average grain diameter is that to coat the Ag metal be example for the diamond dust particle surface of 10 μ m
At first 5g diamond dust particle (granularity is 100 μ m) is placed 5% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.Powder particle behind the suction filtration is carried out the sensitization activation processing, adopt 15%SnCl
2Solution sensitization and 20%PdCl solution activation processing are used washed with de-ionized water three times afterwards.
Afterwards the above-mentioned powder particle of handling well is poured in the hydrazine hydrate solution of 500ml, its concentration is 3ml/L, regulating pH value with ammoniacal liquor is 8, stir ultrasonic concussion, be that 10g/L liquor argenti nitratis ophthalmicus 500ml adds with Sprayable then with concentration, silver nitrate adds speed at 100ml/min, and mixing speed is 50 rev/mins, and ultrasonic concussion frequency is 100KHz.
After treating that chemical plating is fully, suction filtration obtains the good diamond dust particle of plating, and with deionized water rinsing three times.
Afterwards that plating is good diamond dust particle places vacuum, 110 ℃ of dryings 24 hours.
The diamond dust particle surface that is obtained coats evenly, and coating thickness is 2-3 μ m, bath stability in the plating process.
Embodiment five
With average grain diameter is that to coat the Cu metal be example for the diamond dust particle surface of 100 μ m
At first 10g diamond dust particle (granularity is 100 μ m) is placed 20% salpeter solution, stirring and washing 30 minutes adopts suction filtration after the washed with de-ionized water three times then.
After the sensitization activation processing, pour into the powder behind the suction filtration in the 500ml formalin, its concentration is 3ml/L, regulating pH value with sodium hydroxide solution is 10, stir ultrasonic concussion, the 500ml copper-bath that with concentration is 45g/L then adds with Sprayable, copper sulphate adds speed at 5ml/min, and mixing speed is 150 rev/mins, and ultrasonic concussion frequency is 50KHz.
After treating that chemical plating is fully, suction filtration obtains the good diamond dust particle of plating, and with deionized water rinsing three times.
Afterwards that plating is good diamond dust particle places vacuum, 150 ℃ of dryings 24 hours.The diamond dust particle surface plating that obtains even, coating layer thickness is 3-5 μ m, bath stability in the plating process.
Embodiment six
With average grain diameter is that to coat the Cu metal be example for the SiC powder particle surface of 30 μ m
At first 10g SiC powder particle (granularity is 30 μ m) is placed 10% salpeter solution, stirring and washing 10 minutes adopts suction filtration after the washed with de-ionized water three times then.
Powder particle behind the suction filtration is poured in the 500ml formalin after the sensitization activation, and its concentration is 4.5ml/L, and regulating pH value with NaOH is 9, stirs ultrasonic concussion.Be that the 35g/L copper-bath adds with Sprayable then with 500ml concentration, silver nitrate adds speed at 15ml/min, and mixing speed is 250 rev/mins, and ultrasonic concussion frequency is 50KHz.
After treating that chemical plating is fully, suction filtration obtains the good SiC powder particle of plating, and with deionized water rinsing three times.
Afterwards that plating is good SiC powder particle places vacuum, 120 ℃ of dryings 24 hours.The SiC powder particle surface that obtains coat evenly, coating thickness is 1-2 μ m, bath stability in the plating process.
Claims (10)
1. the method for a chemical plating of metal on particle surface, it is characterized in that, ultrasonic concussion generating means is placed in the mechanical agitation slurry, adopt mechanical agitation to combine with built-in ultrasonic concussion, and the mode that adopts the liquid phase spraying to add reactive component, powder particle is fully disperseed, and the reaction of plating zone is uniform and stable, thereby realizes that powder particle surface evenly coats.
2. the method for chemical plating of metal on particle surface according to claim 1 is characterized in that, may further comprise the steps:
The first step is at first carried out surface treatment with powder particle, filters and use washed with de-ionized water afterwards;
In second step, will disperse in the reductant solution in the adding of the powder particle after the surface treatment chemical plating fluid; Described dispersing mode, its method that adopts built-in ultrasonic concussion to combine with mechanical agitation is disperseed, and the excusing from death rocking equipment places in the mechanical agitation slurry;
In the 3rd step, chemical plating is reacted main salting liquid add in the solution that second step obtained and carry out plating;
The 4th step, the powder particle filtration drying that chemistry is covered to complete.
3. the method for chemical plating of metal on particle surface according to claim 1 and 2 is characterized in that, described powder particle is all ceramic powder particles, and institute's metal lining is can be by the metal of chemical plating acquisition.
4. the method for chemical plating of metal on particle surface according to claim 1 and 2 is characterized in that, described powder particle, and its particle mean size is between 0.01 μ m-100 μ m.
5. the method for chemical plating of metal on particle surface according to claim 2 is characterized in that, described surface treatment, and its mode is pickling sensitization activation processing or directly adopts pickling processes.
6. the method for chemical plating of metal on particle surface according to claim 2 is characterized in that, described washed with de-ionized water, and its number of times is three times.
7. the method for chemical plating of metal on particle surface according to claim 1 and 2 is characterized in that, described dispersion, and its powder degree of scatter is controlled by adjusting mechanical agitation speed, ultrasonic concussion frequency.
8. the method for chemical plating of metal on particle surface according to claim 7 is characterized in that, described mechanical agitation speed is 50-500 rev/min, and described ultrasonic concussion frequency is 15KHz-100KHz.
9. the method for chemical plating of metal on particle surface according to claim 2 is characterized in that, described interpolation, and its mode is the liquid phase spraying, spray velocity is adjustable.
10. the method for chemical plating of metal on particle surface according to claim 9 is characterized in that, described spray velocity was at 5ml-100ml/ minute.
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| CN200910196277A CN101758230A (en) | 2009-09-24 | 2009-09-24 | Method for chemical plating of metal on particle surface |
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| CN200910196277A CN101758230A (en) | 2009-09-24 | 2009-09-24 | Method for chemical plating of metal on particle surface |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106270500A (en) * | 2016-09-30 | 2017-01-04 | 昆明理工大学 | A kind of carbon nano tube surface is uniformly coated with the method and device of argent |
| WO2017005132A1 (en) * | 2015-07-03 | 2017-01-12 | 王东 | Nano metal particle and preparation method thereof |
| CN108950529A (en) * | 2018-08-15 | 2018-12-07 | 林庆仁 | A kind of tungsten carbide-copper-nickle composite powder preparation method |
| CN111394715A (en) * | 2020-04-03 | 2020-07-10 | 湖南工程学院 | Silicon carbide particle and whisker mixture processing apparatus for aluminium base composite |
| CN114606482A (en) * | 2022-03-15 | 2022-06-10 | 佛山科学技术学院 | Method for preparing Cu @ ZrC core-shell complex-phase particle material by chemical plating |
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2009
- 2009-09-24 CN CN200910196277A patent/CN101758230A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017005132A1 (en) * | 2015-07-03 | 2017-01-12 | 王东 | Nano metal particle and preparation method thereof |
| US10926335B2 (en) | 2015-07-03 | 2021-02-23 | Dong Wang | Nano-metal particles and preparation process thereof |
| CN106270500A (en) * | 2016-09-30 | 2017-01-04 | 昆明理工大学 | A kind of carbon nano tube surface is uniformly coated with the method and device of argent |
| CN106270500B (en) * | 2016-09-30 | 2019-02-19 | 昆明理工大学 | A kind of carbon nano tube surface uniformly coats the method and device of metallic silver |
| CN108950529A (en) * | 2018-08-15 | 2018-12-07 | 林庆仁 | A kind of tungsten carbide-copper-nickle composite powder preparation method |
| CN111394715A (en) * | 2020-04-03 | 2020-07-10 | 湖南工程学院 | Silicon carbide particle and whisker mixture processing apparatus for aluminium base composite |
| CN114606482A (en) * | 2022-03-15 | 2022-06-10 | 佛山科学技术学院 | Method for preparing Cu @ ZrC core-shell complex-phase particle material by chemical plating |
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Open date: 20100630 |