CN109666926A - A kind of method of simple electroless plating on powders - Google Patents
A kind of method of simple electroless plating on powders Download PDFInfo
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- CN109666926A CN109666926A CN201910082254.5A CN201910082254A CN109666926A CN 109666926 A CN109666926 A CN 109666926A CN 201910082254 A CN201910082254 A CN 201910082254A CN 109666926 A CN109666926 A CN 109666926A
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- powder
- activation
- liquid
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention discloses a kind of methods of simple electroless plating on powders to be added catalyst, powder surface modification material and low boiling point solvent, obtain functional activation liquid after including the following steps: (1) configuration silane mixture liquid;(2) functional activation liquid is sprayed on powder, preparation activation powder;(3) activation powder is immersed in chemical plating fluid, preparation metallization powder.The present invention selects low boiling point solvent configuration feature activating solution, helps to shorten the operating time;Functional activation liquid can make the active layer for activating powder firmly be coated on powder layer surface and improve active layer and powder layer surface adhesion force.The present invention does not need centrifugation, washing after quick and easy powder activation, simplifies process flow by the way that functional activation liquid and activation powder to be sufficiently mixed by spray processing;Drying is not needed after activation, the time required to substantially reducing chemical plating process, and avoids the waste of activating solution.
Description
Technical field
The invention belongs to powder surface plating technical fields, and in particular to a kind of simple electroless plating on powders
Method.
Background technique
106119818 A of Chinese invention patent CN discloses a kind of method of inorganic powder surface chemical plating, metallic cover
Inorganic particle, plating after sensitization, activation.Inorganic particle chemical plating may be implemented in this method, but can not solve powder plating process
Middle sensitization, activating process is cumbersome, time-consuming problem.
108118315 A of Chinese invention patent CN discloses a kind of silicon carbide powder surface chemistry that coating is uniform and stable
The method of nickel plating.This method introduces ultrasonic wave added during pretreatment process and plating, solves the group of powder in a liquid
Poly- phenomenon, but this method can still waste a large amount of activating solution in activation process.
Therefore, find a kind of powder do not needed after sensitization, activation centrifugation, washing, drying method be to shorten chemical plating
Time reduces operating procedure, saves the optimal method of activating solution.
Summary of the invention
The object of the present invention is to provide a kind of methods of simple electroless plating on powders, to solve prior art powder
The waste of activating solution in plating is learned, chemical plating time-consuming problem, the invention is realized by the following technical scheme.
A kind of method of simple electroless plating on powders, specific steps include the following:
(1) it is configured after obtaining silane mixture liquid with silane coupling agent, catalyst, powder surface modification material and low is added
Boiling point solvent is placed after stirring and evenly mixing to get functional activation liquid is arrived;
(2) it is sprayed on powder using spray processing by functional activation liquid is fog-like, while high-speed stirred powder, is made
Functional activation liquid and powder are sufficiently mixed uniformly, and activation powder is obtained after rapid draing;
(3) the activation powder in step (2) is immersed in chemical plating fluid, the plating under 40 ~ 60 DEG C of heating water bath
It is centrifuged and washes after 15 ~ 50min, then dry 30 ~ 45min at 90 ~ 120 DEG C to get dry, pure metallization powder is arrived
Body.
Preferably, silane mixture liquid is to be dispersed in water silane coupling agent in the step (1), the silane
Coupling agent includes 3- Mercaptopropyltriethoxysilane and 3- glycidyl ether oxypropyltrimethoxysilane.
Preferably, 3- Mercaptopropyltriethoxysilane, 3- glycydoxy three in the silane mixture liquid
Methoxy silane, water mass ratio be 3:(2-4): (2-4).
Preferably, the powder surface modification material in the step (1) include anionic surfactant, calcium stearate,
Stearic acid.It is further preferred that the anionic surfactant, calcium stearate, stearic mass ratio are (2-4): 2:(5-
6).It is further preferred that anionic surfactant is sodium alklyarylsulfonate, in sodium alkyl sulfate, Teepol
It is at least one.Anionic surfactant can make powder not reunite in the case where high-speed stirred.
Preferably, the catalyst in the step (1) is at least one of silver nitrate, palladium chloride, platinum, nickel, gold.
Preferably, the low boiling point solvent in the step (1) be at least one of ethyl alcohol, methanol, acetone, ether, it is low
Boiling point solvent facilitates powder rapid draing.
Preferably, the chemical plating fluid in the step (3) is copper plating bath and nickel-plating liquid.
Preferably, the powder in the step (3) be graphene, calcium carbonate, 12 powder of nylon, ceramic powder, in kaolin extremely
Few one kind.
Beneficial effects of the present invention:
(1) low boiling point solvent configuration feature activating solution is selected, is easily dried removal after activating powder, when helping to shorten operation
Between;Metallic ion coordination bond energy in sulfydryl and catalyst in functional activation liquid in 3- Mercaptopropyltriethoxysilane
By force, the active layer for activating powder can be made firmly to be coated on powder layer surface, 3- glycydoxy trimethoxy silicon
Ehter bond, epoxy group isopolarity group in alkane can be improved the active layer and powder layer surface adhesion force of activation powder, to make
The reactivity of obtained activation powder is more stable, promotes subsequent plating process;In addition, further including in functional activation liquid
Powder surface modification material, anionic surfactant therein, calcium stearate, stearic acid can make powder in high-speed stirred
In the case of do not reunite, be uniformly dispersed, obtain the activation powder of uniform particle diameter.
(2) present invention is by the way that functional activation liquid and activation powder to be sufficiently mixed by spray processing, quickly and easily.And powder
Centrifugation, washing are not needed after body activation, simplify process flow;Drying is not needed after activation, substantially reduces chemical plating process
Required time is 2 ~ 3h the time required to powder copper facing in the prior art, and the time of the invention is 1.5 ~ 2h, is at least shortened
0.5h;Plating solution not will cause waste.
Detailed description of the invention
The photo of 12 powder of nickel plating nylon prepared by Fig. 1 embodiment 1;
The XRD spectrum of 12 powder of nickel plating nylon prepared by Fig. 2 embodiment 1;
The SEM figure of 12 powder of nickel plating nylon prepared by Fig. 3 embodiment 1.
Specific embodiment
Below with reference to embodiment, the present invention will be further explained.Obviously, described embodiment is the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Test method described in following embodiments is unless otherwise specified conventional method;The reagent is such as without special theory
It is bright to be obtained through commercial channels.
Embodiment 1
A kind of method of simple electroless plating on powders, specific steps include the following:
(1) by 3- Mercaptopropyltriethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, water in mass ratio 3:
3:4 is placed in dispersion machine high speed stirring 5min to get silane mixture liquid;Add silver nitrate solution, powder surface modification material
(sodium alklyarylsulfonate: calcium stearate: stearic mass ratio is 3:2:5), ethyl alcohol, continue to place one section after stirring 60min
Time obtains functional activation liquid.Wherein, silane mixture liquid: silver nitrate solution: powder surface modification material: the quality of ethyl alcohol
Than for 10:1:0.2:2.
(2) functional activation liquid is sprayed onto 12 powder of nylon using spray processing, high-speed stirred powder, make solution with
12 powder of nylon is sufficiently mixed uniformly, and activation powder is obtained after rapid draing.
(3) above-mentioned activation powder is immersed in nickel-plating liquid, is cleaned after 40 DEG C of heating water bath 50min with deionized water, 90
DEG C baking oven in dry 30min to get to dry, pure 12 powder of nickel plating nylon.
Fig. 1 is the photo of 12 powder of nickel plating nylon, and 12 powder of nylon after chemical plating is in black as can be seen from Figure 1.Fig. 2 is
The XRD spectrum of 12 powder of nickel plating nylon, as shown in Fig. 2, 36oWith 40oThe peak of vicinity is the diffraction maximum of nylon powder, is in addition existed
45oWith 52oThe peak at place is the diffraction maximum of face-centered cubic nickel (111) and (200), and face-centered cubic nickel crystallite is plated in after showing chemical plating
On 12 powder of modification of nylon.Fig. 3 is that the SEM of 12 powder of nickel plating nylon schemes, as shown in figure 3, it can be observed that 12 powder table of nylon
Nickel particle is adhered in face, shows nickel particle by being deposited on 12 powder surface of nylon after chemical plating.The simple work is used in summary
Available 12 powder of nickel plating nylon of skill.
Embodiment 2
A kind of method of simple electroless plating on powders, specific steps include the following:
(1) by 3- Mercaptopropyltriethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, water in mass ratio 4:
3:3 is placed in dispersion machine high speed stirring 5min to get silane mixture liquid;Add palladium chloride solution, powder surface modification material
(sodium alklyarylsulfonate: calcium stearate: stearic ratio be 2:2:6), ether, continue stir 60min after place one section when
Between, obtain functional activation liquid.Wherein, silane mixture liquid: silver nitrate solution: powder surface modification material: the mass ratio of ethyl alcohol
For 10:0.5:0.01:1.
(2) functional activation liquid is sprayed onto calcium carbonate powder using spray processing, high-speed stirred powder, make solution with
Calcium carbonate powder is sufficiently mixed uniformly, and activation powder is obtained after rapid draing.
(3) above-mentioned activation powder is immersed in copper plating bath, is cleaned after 60 DEG C of heating water bath 15min with deionized water, 120
DEG C baking oven in dry 45min to get to dry, pure copper facing calcium carbonate powder.
Embodiment 3
A kind of method of simple electroless plating on powders, specific steps include the following:
(1) by 3- Mercaptopropyltriethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, water in mass ratio 3:
3:4 is placed in dispersion machine high speed stirring 5min to get silane mixture liquid;Add silver nitrate solution, powder surface modification material
(sodium alkyl sulfate: calcium stearate: stearic ratio is 3:2:5), ethyl alcohol, continue to place a period of time after stirring 60min, obtain
To functional activation liquid.Wherein, silane mixture liquid: silver nitrate solution: powder surface modification material: the mass ratio of ethyl alcohol is 10:
1.5:0.7:5.
(2) functional activation liquid is sprayed onto nylon powder using spray processing, high-speed stirred powder makes solution and Buddhist nun
Imperial powder is sufficiently mixed uniformly, and activation powder is obtained after rapid draing.
(3) above-mentioned activation powder is immersed in copper plating bath, is cleaned after 40 DEG C of heating water bath 50min with deionized water, 90
DEG C baking oven in dry 30min to get to dry, pure copper facing nylon powder.
Embodiment 4
A kind of method of simple electroless plating on powders, specific steps include the following:
(1) by 3- Mercaptopropyltriethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, water in mass ratio 3:
3:4 is placed in dispersion machine high speed stirring 5min to get silane mixture liquid;The silver nitrate solution added, powder surface modifier
Matter (sodium alkyl sulfate: calcium stearate: stearic ratio is 3:2:5), ethyl alcohol, continue to place a period of time after stirring 60min,
Obtain functional activation liquid.Wherein, silane mixture liquid: silver nitrate solution: powder surface modification material: the mass ratio of ethyl alcohol is
10:0.8:0.4:4.
(2) functional activation liquid is sprayed onto ceramic powder using spray processing, high-speed stirred powder, makes solution and pottery
Porcelain powder is sufficiently mixed uniformly, and activation powder is obtained after rapid draing.
(3) above-mentioned activation powder is immersed in copper plating bath, is cleaned after 40 DEG C of heating water bath 15min with deionized water, 90
DEG C baking oven in dry 30min to get to dry, pure copper facing ceramic powder.
Embodiment 5
A kind of method of simple electroless plating on powders, specific steps include the following:
(1) by 3- Mercaptopropyltriethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, water in mass ratio 2:
4:4 is placed in after dispersion machine high speed stirring 5min to get silane mixture liquid;Add palladium chloride solution, powder surface modifier
Matter (Teepol: calcium stearate: stearic ratio be 3:2:5), acetone, continue stir 60min after place one section when
Between, obtain functional activation liquid.Wherein, silane mixture liquid: silver nitrate solution: powder surface modification material: the mass ratio of ethyl alcohol
For 10:1.2:0.6:3.
(2) functional activation liquid is sprayed onto kaolin powder using spray processing, high-speed stirred powder, make solution with
Kaolin powder is sufficiently mixed uniformly, and activation powder is obtained after rapid draing.
(3) above-mentioned activation powder is immersed in copper plating bath, is cleaned after 60 DEG C of heating water bath 50min with deionized water, 120
DEG C baking oven in dry 45min to get to dry, pure copper facing kaolin powder.
Claims (10)
1. a kind of method of simple electroless plating on powders, characterized by the following steps:
It is configured after obtaining silane mixture liquid with silane coupling agent, catalyst, powder surface modification material and low boiling point solvent is added,
It is placed after stirring and evenly mixing to get functional activation liquid is arrived;
It is sprayed on powder using spray processing by functional activation liquid is fog-like, while high-speed stirred powder, makes functional work
Change liquid and powder is sufficiently mixed uniformly, activation powder is obtained after rapid draing;
By in step (2) activation powder immerse chemical plating fluid in, under 40 ~ 60 DEG C of heating water bath after 15 ~ 50min of plating from
The heart is simultaneously washed, and dries 30 ~ 45min at 90 ~ 120 DEG C to get metallization powder is arrived.
2. a kind of method of simple electroless plating on powders according to claim 1, it is characterised in that: the step
(1) silane mixture liquid is to be dispersed in water silane coupling agent in, and the silane coupling agent includes 3- mercaptopropyi three
Ethoxysilane and 3- glycidyl ether oxypropyltrimethoxysilane.
3. a kind of method of simple electroless plating on powders according to claim 2, it is characterised in that: the silane is mixed
Close liquid in 3- Mercaptopropyltriethoxysilane, 3- glycidyl ether oxypropyltrimethoxysilane, water mass ratio be 3:
(2-4): (2-4).
4. a kind of method of simple electroless plating on powders according to claim 1, it is characterised in that: the step
(1) the powder surface modification material in includes anionic surfactant, calcium stearate, stearic acid.
5. a kind of method of simple electroless plating on powders according to claim 4, it is characterised in that: the anion
Surfactant, calcium stearate, stearic mass ratio are (2-4): 2:(5-6).
6. a kind of method of simple electroless plating on powders according to claim 4 or 5, it is characterised in that: the yin
Ionic surface active agent is at least one of sodium alklyarylsulfonate, sodium alkyl sulfate, Teepol.
7. a kind of method of simple electroless plating on powders according to claim 1, it is characterised in that: the step
(1) catalyst in is at least one of silver nitrate, palladium chloride, platinum, nickel, gold.
8. a kind of method of simple electroless plating on powders according to claim 1, it is characterised in that: the step
(1) low boiling point solvent in is at least one of ethyl alcohol, methanol, acetone, ether.
9. a kind of method of simple electroless plating on powders according to claim 1, it is characterised in that: the step
(3) chemical plating fluid in is copper plating bath and nickel-plating liquid.
10. a kind of method of simple electroless plating on powders according to claim 1, it is characterised in that: the step
(3) powder in is at least one of graphene, calcium carbonate, 12 powder of nylon, ceramic powder, kaolin.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110923771A (en) * | 2019-12-16 | 2020-03-27 | 电子科技大学 | Through hole electroplating method of printed circuit board |
CN111074247A (en) * | 2020-03-04 | 2020-04-28 | 安徽江东科技粉业有限公司 | Simple inorganic powder surface chemical plating method |
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CN1966765A (en) * | 2005-11-17 | 2007-05-23 | 中国科学院金属研究所 | Activation method for chemical plating of non-metallic material and chemical plating therefor |
CN101139706A (en) * | 2007-10-17 | 2008-03-12 | 南京工业大学 | Spray activation process for chemical plating on surface of water-absorbing substrate |
CN106189375A (en) * | 2016-06-30 | 2016-12-07 | 嘉兴市高正高分子材料有限公司 | A kind of Activated Carbon Nanotubes |
CN108754461A (en) * | 2018-05-24 | 2018-11-06 | 合肥学院 | A kind of method of surface of polymer substrates selective chemical plating |
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2019
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EP1300488A2 (en) * | 2001-10-02 | 2003-04-09 | Shipley Co. L.L.C. | Plating path and method for depositing a metal layer on a substrate |
CN1966765A (en) * | 2005-11-17 | 2007-05-23 | 中国科学院金属研究所 | Activation method for chemical plating of non-metallic material and chemical plating therefor |
CN101139706A (en) * | 2007-10-17 | 2008-03-12 | 南京工业大学 | Spray activation process for chemical plating on surface of water-absorbing substrate |
CN106189375A (en) * | 2016-06-30 | 2016-12-07 | 嘉兴市高正高分子材料有限公司 | A kind of Activated Carbon Nanotubes |
CN108754461A (en) * | 2018-05-24 | 2018-11-06 | 合肥学院 | A kind of method of surface of polymer substrates selective chemical plating |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110923771A (en) * | 2019-12-16 | 2020-03-27 | 电子科技大学 | Through hole electroplating method of printed circuit board |
CN111074247A (en) * | 2020-03-04 | 2020-04-28 | 安徽江东科技粉业有限公司 | Simple inorganic powder surface chemical plating method |
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