CN105463454A - Ceramic surface multi-layer composite coating film and preparing method thereof - Google Patents
Ceramic surface multi-layer composite coating film and preparing method thereof Download PDFInfo
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- CN105463454A CN105463454A CN201510855219.4A CN201510855219A CN105463454A CN 105463454 A CN105463454 A CN 105463454A CN 201510855219 A CN201510855219 A CN 201510855219A CN 105463454 A CN105463454 A CN 105463454A
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/20—Metallic material, boron or silicon on organic substrates
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/46—Electroplating: Baths therefor from solutions of silver
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Electroplating Methods And Accessories (AREA)
- Chemically Coating (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention discloses a ceramic surface multi-layer composite coating film and a preparing method thereof. The multi-layer composite coating film comprises three-layer structures including an organic coating, a pre-plated middle metal layer and an electroplated layer. The preparing method of the multi-layer composite coating film comprises the steps that dry method cleaning and activating are carried out on the ceramic material surface; the activated ceramic material is coated with the organic coating; and then the ceramic material is placed in a physical vapor deposition furnace, the middle metal layer is pre-plated, finally, the ceramic material is placed in electroplate liquid to be subjected to constant-current electroplating, and the ceramic surface multi-layer composite coating film is obtained. The binding force among the layers of the multi-layer composite coating film is good, and especially, the binding force with a ceramic material base body is superior. The composite coating film is high in surface glassiness, and the electroplated layer is even and bright in color. The electroplating method is simple in technology and good in repeatability.
Description
Technical field
The present invention relates to surface multi-layer composite film coating field, be specifically related to a kind of ceramic surface MULTILAYER COMPOSITE plated film and preparation method thereof.
Background technology
Carry out metallizing process at ceramic surface, usually first electroless plating method or sputtering method are adopted to ceramic surface, vapour deposition method carries out preplating one deck intermediate metal layer, then electroplate on the basis of intermediate metal layer.But when some ceramic material surfaces exists the problems such as coarse, defect, between the intermediate metal layer of preplating and ceramic surface matrix, bonding force is bad, and glossiness also needs further raising.
Summary of the invention
Goal of the invention: for deficiency of the prior art, the invention provides a kind of method at ceramic surface MULTILAYER COMPOSITE plated film.The method technique is simple, and favorable reproducibility, the product bonding force of preparation is good, glossiness is high.
Technical scheme: for achieving the above object, the present invention by the following technical solutions:
In a method for ceramic surface MULTILAYER COMPOSITE plated film, comprise the following steps:
(1) pre-treatment: dry clean and activation are carried out to ceramic material surfaces;
(2) organic coating is coated with: the stupalith after activation is coated with organic coating;
(3) preplating: step (2) is coated with the stupalith after organic coating and puts into physical vapor deposition stove, pre-metal cladding in shielding gas atmosphere;
(4) electroplate: after the stupalith cleaning after pre-for step (3) metal cladding, put into electroplate liquid, platinized platinum is cooked electrode, and adopt continuous current plating mode to electroplate, current density is 0.5 – 3A/dm
2, the distance of negative electrode and positive electrode is 10 – 15cm, and temperature is 20 – 50 DEG C, and electroplating time is 0.1 – 50min, and after having electroplated, ceramic surface MULTILAYER COMPOSITE plated film adopts washed with de-ionized water 2 times, then cleans 1 time with ultrapure water, naturally dries or N
2dry up.
Further, in step (1), the concrete grammar of dry clean is as follows: first by dry cloth wiping ceramic material surfaces, remove grease and dust, then the grease of high-temperature flame treatment ceramic material surfaces is utilized, reach the object of oil removing grease removal, then by electrostatic precipitation, remove the particle of dust and the burning generation being adsorbed on ceramic material surfaces; The concrete grammar of described activation is as follows: adopt methane gas as combustion gases, thermal-flame flame envelope contact ceramic material surfaces 5 – 30s, make it reach the high temperature of 1000 DEG C instantaneously, thus make ceramic material outer surface have a large amount of polar link, be easy to form good combination power with organic coating.
Further, in step (2), the thickness of organic coating is 5 – 60 μm; Organic coating is colourless or have color, and described color is the one in gold, silver color, coppery, nickel look, black, redness or green.Organic coating is coated in the ceramic material surfaces activated, and can reach levelling, hide the defect of ceramic surface and coarse, and then lay the foundation for follow-up raising glossiness.
Further, in step (2), described organic coating is that ultraviolet light polymerization is crosslinked or thermofixation is crosslinked; The time that described ultraviolet light polymerization is cross-linked is 30 – 90s; The temperature that described thermofixation is cross-linked is 70 – 180 DEG C, and the time that described thermofixation is cross-linked is 10 – 60min.
Further, the thickness of the described pre-metal cladding of step (3) is 0.05 – 5 μm; Described metal adopts one or more of copper, nickel and chromium.
Further, the shielding gas in described step (3) is N
2or Ar.
Further, the electroplate liquid in described step (4) is cyanide-free gold electroplating plating solution or cyanideless electro-plating silver plating solution.Wherein, cyanide-free gold electroplating crosses liquid and comprises: sulfurous acid gold or citric acid gold 2 – 50g/L, 2-sulfo--5,5-T10 10 – 120g/L, succimide 10 – 50g/L, Tripotassium Citrate 40 – 100g/L, citric acid 10 – 40g/L, antimonypotassium tartrate 1 – 3g/L, polyoxyethylene glycol 0.5 – 2g/L, S-WAT 20 – 150g/L, γ-picolinic acid 2 – 10g/L, this cyanide-free gold electroplating crosses liquid and adopts lemon acid for adjusting pH 5 ± 0.5, and keeps cyanogen-less gold liquid temp at 50 ± 3 DEG C; Cyanideless electro-plating silver plating solution comprises: Silver Nitrate 2 – 50g/L, 2-sulfo--5,5-T10 10 – 120g/L, succimide 10 – 50g/L, potassium hydroxide 10 – 50g/L, ethylene diamine tetra methylene phosphonic acid sodium 40 – 100g/L, ammonium molybdate 1 – 3g/L, polyoxyethylene glycol 0.5 – 2g/L, S-WAT 20 – 150g/L, γ-picolinic acid 5 – 20g/L, this non-cyanide plating silvering solution adopts potassium hydroxide to regulate pH at 8 – 10, and keeps non-cyanide silver coating liquid temp 25 – 45 DEG C.
Another object of the present invention is to provide a kind of ceramic surface MULTILAYER COMPOSITE plated film, this MULTILAYER COMPOSITE plated film adopts aforesaid method to be prepared from.
Beneficial effect: the ceramic surface MULTILAYER COMPOSITE plated film prepared by the present invention, this composite film coating includes organic coating, preplating intermediate metal layer and electrolytic coating three-decker, between each layer, bonding force is good, especially bonding force is excellent and between ceramic matrix, this composite film coating surface gloss is high, electrolytic coating color even light.Electro-plating method technique of the present invention is simple, favorable reproducibility.
Embodiment
The present invention is further described below, and the description of specific embodiment is only example in essence, instead of intend to limit content disclosed by the invention and application thereof or use.
Embodiment 1
(1) pre-treatment: first by dry cloth wiping ceramic material surfaces, remove grease and dust, then utilize the grease of high-temperature flame treatment ceramic material surfaces, reach the object of oil removing grease removal, again by electrostatic precipitation, remove the particle of dust and the burning generation being adsorbed on ceramic material surfaces; The concrete grammar of described activation is as follows: adopt methane gas as combustion gases, thermal-flame flame envelope contact stupalith table 20s, make it reach the high temperature of 1000 DEG C instantaneously, thus make ceramic material outer surface have a large amount of polar link, be easy to form good combination power with organic coating;
(2) organic coating is coated with: the ultraviolet-curing paint stupalith after activation being sprayed one deck 30 μm, with infrared lamps levelling (60 DEG C × 8min), then through ultra-violet lamp solidification (1000J/m
2× 40s);
(3) preplating: the stupalith after spraying ultraviolet-curing paint is put into physical vapor deposition stove, at N
2the layers of copper of preplating one deck 1 μm in atmosphere;
(4) electroplate: after the stupalith cleaning after step (3) preplating layers of copper, put into cyanide-free gold electroplating plating solution, cyanide-free gold electroplating plating solution comprises: sulfurous acid gold 35g/L, 2-sulfo--5,5-T10 90g/L, succimide 30g/L, Tripotassium Citrate 75g/L, citric acid 25g/L, antimonypotassium tartrate 1g/L, polyoxyethylene glycol 2g/L, S-WAT 100g/L, γ-picolinic acid 7g/L, pH is 5.5, platinized platinum is cooked electrode, adopt continuous current plating mode to electroplate, current density is 2A/dm
2, the distance of negative electrode and positive electrode is 15cm, and temperature is 25 DEG C, electroplating time is 10min, and after having electroplated, ceramic surface MULTILAYER COMPOSITE plated film adopts washed with de-ionized water 2 times, 1 time is cleaned again with ultrapure water, naturally dry, obtain product, product is at metallography microscope Microscopic observation, smooth surface free of pinholes, glossiness is excellent, bubbles, measure bonding force between each layer good according to standard GB/T/T5270--200X without volume skin.
Embodiment 2
(1) pre-treatment: first by dry cloth wiping ceramic material surfaces, remove grease and dust, then utilize the grease of high-temperature flame treatment ceramic material surfaces, reach the object of oil removing grease removal, again by electrostatic precipitation, remove the particle of dust and the burning generation being adsorbed on ceramic material surfaces; The concrete grammar of described activation is as follows: adopt methane gas as combustion gases, thermal-flame flame envelope contact stupalith table 20s, make it reach the high temperature of 1000 DEG C instantaneously, thus make ceramic material outer surface have a large amount of polar link, be easy to form good combination power with organic coating;
(2) organic coating is coated with: the ultraviolet-curing paint stupalith after activation being sprayed one deck 50 μm, with infrared lamps levelling (60 DEG C × 8min), then through ultra-violet lamp solidification (1000J/m
2× 40s);
(3) preplating: the stupalith after spraying ultraviolet-curing paint is put into physical vapor deposition stove, at N
2the nickel dam of preplating one deck 3 μm in atmosphere;
(4) electroplate: after the stupalith cleaning after step (3) preplating layers of copper, put into cyanide-free gold electroplating plating solution, cyanide-free gold electroplating plating solution comprises: sulfurous acid gold 20g/L, 2-sulfo--5,5-T10 50g/L, succimide 20g/L, Tripotassium Citrate 60g/L, citric acid 40g/L, antimonypotassium tartrate 2g/L, polyoxyethylene glycol 1g/L, S-WAT 70g/L, γ-picolinic acid 4g/L, pH is 5.0, platinized platinum is cooked electrode, adopt continuous current plating mode to electroplate, current density is 2A/dm
2, the distance of negative electrode and positive electrode is 10cm, and temperature is 40 DEG C, electroplating time is 20min, and after having electroplated, ceramic surface MULTILAYER COMPOSITE plated film adopts washed with de-ionized water 2 times, 1 time is cleaned again with ultrapure water, naturally dry, obtain product, product is at metallography microscope Microscopic observation, smooth surface free of pinholes, glossiness is excellent, bubbles, measure bonding force between each layer good according to standard GB/T/T5270--200X without volume skin.
Embodiment 3
(1) pre-treatment: first by dry cloth wiping ceramic material surfaces, remove grease and dust, then utilize the grease of high-temperature flame treatment ceramic material surfaces, reach the object of oil removing grease removal, again by electrostatic precipitation, remove the particle of dust and the burning generation being adsorbed on ceramic material surfaces; The concrete grammar of described activation is as follows: adopt methane gas as combustion gases, thermal-flame flame envelope contact stupalith table 30s, make it reach the high temperature of 1000 DEG C instantaneously, thus make ceramic material outer surface have a large amount of polar link, be easy to form good combination power with organic coating;
(2) organic coating is coated with: the heat curing coating stupalith after activation being sprayed one deck 40 μm, with infrared lamps levelling (50 DEG C × 20min), then through ultra-violet lamp solidification (90 DEG C/m
2× 30min);
(3) preplating: the stupalith after spraying ultraviolet-curing paint is put into physical vapor deposition stove, at N
2the nickel dam of preplating one deck 2 μm in atmosphere;
(4) electroplate: after the stupalith cleaning after step (3) preplating layers of copper, put into cyanideless electro-plating silver plating solution, cyanideless electro-plating silver plating solution comprises: Silver Nitrate 40g/L, 2-sulfo--5, 5-T10 100g/L, succimide 40g/L, potassium hydroxide 35g/L, ethylene diamine tetra methylene phosphonic acid sodium 80g/L, ammonium molybdate 2g/L, polyoxyethylene glycol 1g/L, S-WAT 80g/L, γ-picolinic acid 10g/L, this cyanideless electro-plating silver plating solution adopts potassium hydroxide to regulate pH 8.5, platinized platinum is cooked electrode, continuous current plating mode is adopted to electroplate, current density is 1.0A/dm
2, the distance of negative electrode and positive electrode is 15cm, and temperature is 30 DEG C, electroplating time is 50min, and after having electroplated, ceramic surface MULTILAYER COMPOSITE plated film adopts washed with de-ionized water 2 times, 1 time is cleaned again with ultrapure water, naturally dry, obtain product, product is at metallography microscope Microscopic observation, smooth surface free of pinholes, glossiness is excellent, bubbles, measure bonding force between each layer good according to standard GB/T/T5270--200X without volume skin.
Should be understood that; above embodiment is only optimal way of the present invention; only that illustrated example effect is played to technical conceive of the present invention; can not limit the scope of the invention with this; those skilled in the art are not departing from the spirit and scope of technical solution of the present invention; modify and be equal to replacement, all should drop within protection scope of the present invention.
Claims (8)
1. a preparation method for ceramic surface MULTILAYER COMPOSITE plated film, is characterized in that, comprises the following steps:
(1) pre-treatment: dry clean and activation are carried out to ceramic material surfaces;
(2) organic coating is coated with: the stupalith after activation is coated with organic coating;
(3) preplating: step (2) is coated with the stupalith after organic coating and puts into physical vapor deposition stove, pre-metal cladding in shielding gas atmosphere;
(4) electroplate: after the stupalith cleaning after pre-for step (3) metal cladding, put into electroplate liquid, platinized platinum is cooked electrode, and adopt continuous current plating mode to electroplate, current density is 0.5 – 3A/dm
2, the distance of negative electrode and positive electrode is 10 – 15cm, and temperature is 20 – 50 DEG C, and electroplating time is 0.1 – 50min, and after having electroplated, ceramic surface MULTILAYER COMPOSITE plated film adopts washed with de-ionized water 2 times, then cleans 1 time with ultrapure water, naturally dries or N
2dry up.
2. the preparation method of ceramic surface MULTILAYER COMPOSITE plated film according to claim 1, it is characterized in that, in step (1), the concrete grammar of described dry clean is as follows: first by dry cloth wiping ceramic material surfaces, remove grease and dust, then utilize the grease of high-temperature flame treatment ceramic material surfaces, reach the object of oil removing grease removal, again by electrostatic precipitation, remove the particle of dust and the burning generation being adsorbed on ceramic material surfaces; The concrete grammar of described activation is as follows: adopt methane gas as combustion gases, and thermal-flame flame envelope contact ceramic material surfaces 5 – 30s, makes it reach the high temperature of 1000 DEG C instantaneously.
3. the preparation method of ceramic surface MULTILAYER COMPOSITE plated film according to claim 1, is characterized in that, in step (2), the thickness of described organic coating is 5 – 60 μm; Described organic coating is colourless or have color, and described color is the one in gold, silver color, coppery, nickel look, black, redness or green.
4. the preparation method of ceramic surface MULTILAYER COMPOSITE plated film according to claim 1, is characterized in that, in step (2), described organic coating is that ultraviolet light polymerization is crosslinked or thermofixation is crosslinked; The time that described ultraviolet light polymerization is cross-linked is 30 – 90s; The temperature that described thermofixation is cross-linked is 70 – 180 DEG C, and the time that described thermofixation is cross-linked is 10 – 60min.
5. the preparation method of ceramic surface MULTILAYER COMPOSITE plated film according to claim 1, is characterized in that, in described step (3), the thickness of pre-metal cladding is 0.05 – 5 μm; Described metal adopts one or more of copper, nickel and chromium.
6. the preparation method of ceramic surface MULTILAYER COMPOSITE plated film according to claim 1, is characterized in that, the shielding gas in described step (3) is N
2or Ar.
7. the preparation method of ceramic surface MULTILAYER COMPOSITE plated film according to claim 1, it is characterized in that, in described step (4), electroplate liquid is cyanide-free gold electroplating plating solution or cyanideless electro-plating silver plating solution, wherein, cyanide-free gold electroplating crosses liquid and comprises: sulfurous acid gold or citric acid gold 2 – 50g/L, 2-sulfo--5, 5-T10 10 – 120g/L, succimide 10 – 50g/L, Tripotassium Citrate 40 – 100g/L, citric acid 10 – 40g/L, antimonypotassium tartrate 1 – 3g/L, polyoxyethylene glycol 0.5 – 2g/L, S-WAT 20 – 150g/L, γ-picolinic acid 2 – 10g/L, this cyanide-free gold electroplating plating solution adopts lemon acid for adjusting pH 5 ± 0.5, and keep cyanide-free gold electroplating bath temperature at 50 ± 3 DEG C, cyanideless electro-plating silver plating solution comprises: Silver Nitrate 2 – 50g/L, 2-sulfo--5,5-T10 10 – 120g/L, succimide 10 – 50g/L, potassium hydroxide 10 – 50g/L, ethylene diamine tetra methylene phosphonic acid sodium 40 – 100g/L, ammonium molybdate 1 – 3g/L, polyoxyethylene glycol 0.5 – 2g/L, S-WAT 20 – 150g/L, γ-picolinic acid 5 – 20g/L, this non-cyanide plating silvering solution adopts potassium hydroxide to regulate pH at 8 – 10, and keeps non-cyanide silver electroplating bath temperature 25 – 45 DEG C.
8. a ceramic surface MULTILAYER COMPOSITE plated film, is characterized in that: adopt the method described in any one of claim 1 – 7 to be prepared from.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107299367A (en) * | 2017-08-24 | 2017-10-27 | 重庆立道表面技术有限公司 | Non-cyanide bright plate silver plating solution |
| CN111732456A (en) * | 2020-06-30 | 2020-10-02 | 苏州蓝晶研材料科技有限公司 | Ceramic conductive material and preparation method and application thereof |
| CN112593263A (en) * | 2020-12-14 | 2021-04-02 | 上海华友金裕微电子有限公司 | Preparation method of silver plating additive on wafer |
| CN112746295A (en) * | 2020-12-30 | 2021-05-04 | 苏州禾川化学技术服务有限公司 | Silver plating solution and ceramic surface silver plating method |
| CN113402306A (en) * | 2021-05-27 | 2021-09-17 | 江苏濠玥电子科技有限公司 | Preparation method of ceramic surface full-covered metal layer |
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| CN112746295A (en) * | 2020-12-30 | 2021-05-04 | 苏州禾川化学技术服务有限公司 | Silver plating solution and ceramic surface silver plating method |
| CN113402306A (en) * | 2021-05-27 | 2021-09-17 | 江苏濠玥电子科技有限公司 | Preparation method of ceramic surface full-covered metal layer |
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