CN106944322A - The electroless plating of substrate - Google Patents
The electroless plating of substrate Download PDFInfo
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- CN106944322A CN106944322A CN201610009344.8A CN201610009344A CN106944322A CN 106944322 A CN106944322 A CN 106944322A CN 201610009344 A CN201610009344 A CN 201610009344A CN 106944322 A CN106944322 A CN 106944322A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
- B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/56—Three layers or more
- B05D7/58—No clear coat specified
- B05D7/584—No clear coat specified at least some layers being let to dry, at least partially, before applying the next layer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2451/00—Type of carrier, type of coating (Multilayers)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2504/00—Epoxy polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2518/00—Other type of polymers
- B05D2518/10—Silicon-containing polymers
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Chemically Coating (AREA)
Abstract
The invention provides the product and its method that a kind of electroless plating in substrate prepares laminated coating, including epoxy based coatings, silver coating and anti-scratch coating.
Description
Technical field
It is by electroless plating the present invention relates to the coating multiple coating in substrate, especially laminated coating
Mode is deposited on substrate surface.
Background technology
A kind of processing mode on common metal surface is plating.However, plating is because generating a large amount of toxicity
Accessory substance and waste cause harm to earth environment.And the cost of plating is very high.These are limited
The development of electroplating industry.
The content of the invention
The present invention provides a kind of substrate with electroless plating, including one in the substrate surface
On adherent coating, the adherent coating include the first silicon substrate plinth coupling agent；One in the adhesion
It is lubricious on coating, it is described lubricious comprising epoxy resin；One described lubricious
On silver coating, the silver coating include silver nano-grain；And one on the silver coating
Anti-scratch coating, the anti-scratch coating includes second silicon substrate plinth coupling agent.
Another method of the present invention provides the side that a kind of electroless plating in substrate is coated with multicoat
Adherent coating comprising the first silicon substrate plinth coupling agent is coated on the table of the substrate by method, including a.
Face；B. lubricious comprising epoxy resin is coated on the adherent coating；C. it will include
The silver coating of silver nano-grain be coated on it is described it is lubricious on；D. the coupling of the second silicon substrate plinth will be included
The anti-scratch coating of agent is coated on the silver coating.
Another aspect of the invention, which provides one, is used for the suit of the electroless plating in substrate, including
Adherent coating solution containing the first silicon substrate plinth coupling agent, the lubricious solution containing epoxy resin, contain
The electroless plating solution of silver nitrate base soln and glucose base soln and containing the second silicon substrate plinth
The anti-scratch coating solution of coupling agent.
Brief description of the drawings
Accompanying drawing 1 is shown according to one embodiment of the invention gamma-aminopropyl-triethoxy-silane
(A1100) with the interaction of the adherent coating on epoxy resin basis.
Accompanying drawing 2 shows same embodiment of the invention (3- mercaptopropyis) trimethoxy silane
(A189) with the interaction of silver coating.
Accompanying drawing 3 shows the result of same embodiment decoration test of the invention.
Accompanying drawing 4 shows the result of same embodiment sample adhesion test of the invention.
Accompanying drawing 5 shows the result of the anticorrosive test of same embodiment sample of the invention.
Accompanying drawing 6 shows the result of same embodiment sample shock-testing of the invention.
Accompanying drawing 7 shows the result of same embodiment sample hardness test of the invention.
Accompanying drawing 8 shows the result of same embodiment sample UV irradiations test of the invention.
Accompanying drawing 9 shows the result of same embodiment sample waterproof test of the invention.
Accompanying drawing 10 shows the result of the antiacid test of same embodiment sample of the invention.
Accompanying drawing 11 shows the result of same embodiment sample alkali resistant test of the invention.
Embodiment
The invention provides a kind of decorative product with electroless plating multicoat (i.e. without using electricity
Plating can obtain multicoat).
In one embodiment of the present of invention, whole electroless plating method is related to three key steps：
Base coating application step, silver coating application step and anti-scratch coating application step.In one embodiment
In, the thickness of base coating is 17.5 μm.In another embodiment, the thickness of silver coating is
90nm.In another embodiment, the thickness of anti-scratch coating is 2 μm.
Each step and used material is discussed below.
1. base coating application step
Before base coating is coated on into substrate, preparation process optionally can be implemented in substrate,
Can be in the polishing of implementation surface, surface cleaning and/or surface preparation in substrate.In one embodiment
In, the substrate can be metallic substrates.
1.1 surface preparations
In a particular embodiment, substrate is pre-processed with preprocessing solution, preprocessing solution
Made by 8.64g A1100,750ml ethanol and 31.52g deionized waters in mixed at room temperature 10 minutes
Into.First, substrate and preprocessing solution contact, ultrasound is carried out 10 minutes in room temperature.Then, base
Bottom is dried 20 minutes in 100 DEG C of baking oven, is cooled to room temperature and is obtained precondition substrate.
1.2. the composition of adherent coating solution and lubricious solution
Base coating includes two former coatings：Adherent coating and lubricious.Adherent coating is applied first
Prevent in the viscosity for being used to strengthen base coating and substrate on substrate surface and being provided for the substrate that is applied
The performance of corrosion.Then by it is lubricious be applied to adherent coating on improve base coating smoothness from
And strengthen the viscosity of base coating and silver coating.
The compositing range of adherent coating solution and lubricious solution is listed in table 1A and 2A respectively.
The compositing range of table 1A adherent coating solutions
| Composition | Weight % scopes |
| Epoxy resin (Epoxy) E-51 | 28.99%-32.04% |
| BYK-361N | 0.23%-0.26% |
| Ethanol | 6.96%-7.69% |
| Acetone | 54.46%-60.19% |
| TZ-550 | 4.36%-4.81% |
The compositing range of the lubricious solution of table 2A
In a particular embodiment, the composition of adherent coating solution and lubricious solution is arranged respectively
In table 1B and 2B.
The composition of table 1B adherent coating solutions
The composition of the lubricious solution of table 2B
| Composition | Weight % |
| Epoxy resin E-51 | 44.17% |
| BYK-361N | 0.40% |
| CGE | 5.80% |
| Acetone | 4.66% |
| DAA | 24.98% |
| N-butanol | 12.49% |
| TZ-550 | 7.50% |
In one embodiment, the acetone in adherent coating solution or lubricious solution serves as solvent
And the 90% of adherent coating solution or lubricious liquor capacity can be increased to.
In addition, the difference of the solvent (i.e. acetone) in adherent coating solution and lubricious solution
Weight is than that can cause the different evaporation rates of two kinds of coating solutions.
1.2.1 the preparation of adherent coating solution
In a particular embodiment, adherent coating solution includes adhesion original solution and curing agent is molten
Liquid.First, adhesion original solution (1kg) is by by 713.05g epoxy resin E-51,171.15g
Acetone and 115.8g ethanol are made in mixed at room temperature to formation homogeneous solution.Curing agent solution
(1kg) is mixed by 33.90g BYK-361N, 636.80g TZ-550 and 329.30g ethanol in room temperature
It is bonded to form homogeneous solution and be made.
Afterwards, 342.4g adheres to original solution, 400.0g acetone and 57.6g curing agent solutions and mixed in room temperature
Close 3 minutes, then ultrasonic wave is carried out 10 minutes in water-bath, so as to obtain adherent coating solution.
1.2.2 the preparation of lubricious solution
In a particular embodiment, lubricious solution includes smooth original solution and TZ-500.It is first
First, smooth original solution (1kg) by 477.55g epoxy resin E-51,135.05g n-butanol,
270.10g DAAs, 50.35g acetone, 62.65g CGE and 4.30g BYK-361N are in room temperature
Mix to formation homogeneous solution and be made.
Afterwards, the smooth original solutions of 925.0g and 75.0g TZ-550 were in mixed at room temperature 3 minutes, then
Ultrasonic wave is carried out in water-bath 10 minutes, so as to obtain lubricious solution.
1.3 coupling agent A1100
Coupling agent A1100 is added in adherent coating solution and applied with the adhesion on reinforced epoxy basis
Bonding of the layer between substrate surface.It is this it is enhanced bonding be due to A1100 NH groups with
The O Interaction of substituents of epoxy resin causes the very strong combination of the two functional groups, such as Fig. 1 institutes
Show.
1.4 adherent coatings are coated on substrate
Ultrasonic wave degassing was first passed around more than 5 minutes by above-mentioned prepared adherent coating solution.It is viscous
Attached coating solution is coated in substrate by brush, immersion or spraying method.The substrate warp being applied
150 DEG C of heat hardenings 15 minutes.
In a particular embodiment, adherent coating solution is sprayed in substrate in the following manner.
First, by deionized water with 22mL/min speed, 3bar air spraying in substrate.So
Afterwards, acetone is sprayed in substrate, sprayed afterwards in substrate adherent coating solution 30 seconds and spray gun away from
From substrate about 15cm.The substrate being applied was through 150 DEG C of heat hardenings 15 minutes.
1.5 lubricious are coated on are attached the substrate that coating is coated with
Ultrasonic wave degassing was first passed around more than 10 minutes by above-mentioned prepared lubricious solution.Light
Sliding coating solution is coated on adherent coating by brush, immersion or spraying method.The substrate being applied
It is coated with 3-6 hours through 80 DEG C.
In a particular embodiment, in the following manner by lubricious solution spraying in substrate.
First, by deionized water with 55mL/min speed, 3bar air spraying in substrate.So
Afterwards, acetone is sprayed in substrate, lubricious solution 30 seconds is sprayed in substrate afterwards and spray gun away from
From substrate about 15cm.The substrate being applied is handled 3-6 hours through 80 DEG C of heat hardenings.
2 silver coating application steps
In this step, it is coated on by redox reaction silver by electroless plating on base coating, wherein
Silver-colored ammonium compound [Ag (NH3)2]+With the glucose response as reducing agent.
2.1 electroless plating solution
Electroless plating solution includes two solution, and silver nitrate base soln and glucose basis are molten
Liquid, the scope of its composition is as shown in table 3.
The composition of the silver nitrate base soln of table 3 and glucose base soln
In one embodiment, concentration range of the silver nitrate in silver nitrate base soln is
7.5-20g/L.In another embodiment, concentration range of the glucose in glucose base soln
For 5-20g/L.
2.1.1 the preparation of silver nitrate base soln
In a specific embodiment, silver nitrate base soln is prepared by following manner.6.00g hydrogen
Sodium oxide molybdena and 20mL deionized waters are in mixed at room temperature until all solids dissolve, so as to obtain hydrogen-oxygen
Change sodium solution.10g silver nitrates and 100mL deionized waters mixed at room temperature to all solids dissolve from
And obtain silver nitrate solution.Sodium hydroxide solution is added in silver nitrate solution until brown precipitate life
Into.30mL 28% ammoniacal liquor is obtained by mixing ammonia spirit with 60mL deionized waters.Ammonia spirit
NaOH and mixture of silver nitrate are added dropwise to until all brown precipitates are redissolved to obtain just
Obtain settled solution.It is molten so as to obtain nitric acid silver base that settled solution is finally diluted to 1L by deionized water
Liquid.
2.1.2 the preparation of glucose base soln
In a specific embodiment, glucose base soln by by 8.00g glucose,
0.54g citric acids, 20mL ethanol and 980mL water mix at room temperature until formed homogeneous solution and
Prepare.
2.1.3 the preparation of sensitizing solution
In a specific embodiment, mixing 4.00g SnCl2(stannous chloride) and 4mL 37%
Hydrochloric acid, then heats mixture 10 minutes until forming settled solution at 60 DEG C.Will in room temperature
800mL deionized waters add into settled solution and obtain sensitizing solution.
2.2 silver coatings are coated in the substrate of base coating
2.2.1 clean
It is coated with the acetone and ethanol (volume ratio 1 of the substrate flowing of base coating：1) washed
1 minute, then it is washed with deionized 1 minute.The cleaning of the base coating on epoxy resin basis is not only
Remove unreacted epoxy resin residue, and make epoxy resin surface roughening so as to improve Sn from
Son and silver it is mechanical interlocked and can be below the step of in adhere to epoxy resin surface.
2.2.2 it is sensitized
In this step, contacted after cleaning with dried substrate with stannous chloride solution, Ran Houyong
The deionized water washing substrate of flowing, in 90 DEG C of dryings of baking oven, is cooled to room temperature in atmosphere.
Stannous chloride strengthens the adhesion of the epoxy resin surface of silver and base coating as sensitizer.One
In individual embodiment, stannous chloride is applying first oxidized (such as oxidation by air 1 before substrate
My god).Inventor is had found once through peroxidating (or aging), some Sn2+Sn will be oxidized to4+,
Produced Sn2+And Sn4+Mixture Sn is comprised only to silver and the sticking ratio of epoxy resin2+'s
" fresh stannous chloride " has more preferable enhancing effect.
In a particular embodiment, sensitizing solution is sprayed in substrate in the following manner.First,
By deionized water with 10mL/min speed, 3bar air spraying in substrate.Then, it is sensitized
Liquid is sprayed 30 seconds in substrate and spray gun is apart from substrate about 5cm.
2.2.3 silver coating is coated on substrate
After sensitization, intersection is sprayed on simultaneously in room temperature for silver nitrate base soln and glucose base soln
0.5 minute in substrate after sensitization.When intersecting spraying, silver nitrate base soln and glucose basis
The particle of solution will form fine evaporated form before the surface of the substrate of contact sensitization.Therefore,
Silver nano-grain conforming layer (about 30-150nm granular size) can be sprayed on base by intersecting
On bottom, produced product has identical or more preferable brightness effect than the product of electroplated coating silver.It
Afterwards, substrate is washed with deionized, and is then dried at least 15 minutes in 100 DEG C of baking ovens.
In one embodiment, the spray rate of silver nitrate base soln and glucose base soln is
3：2 to 1：3 (such as 12mL/min:8mL/min,8mL/min:8mL/min,8mL/min:
12mL/min,8mL/min:16mL/min,or 8mL/min:24mL/min etc.).
In another embodiment, the concentration of silver nitrate base soln is 10g/L；Glucose basis
The concentration of solution is 8g/L；The spray rate of silver nitrate base soln is 10mL/min；Glucosyl group
The spray rate of plinth solution is 20mL/min.
In another particular embodiment, silver nitrate base soln and glucose base soln are with following
Method is sprayed in substrate.The substrate being sensitized first deionized water rinsing 1 minute, is then used
Double head spray gun, deionized water sprays substrate by first shower nozzle with 10mL/min speed, goes
Ionized water sprays substrate by second shower nozzle with 20mL/min speed, and double spray guns are apart from substrate
About 40cm.Silver nitrate base soln and glucose base soln pass through first and second respectively afterwards
Shower nozzle is sprayed in substrate 60 seconds simultaneously, and first shower nozzle sprays base with 10mL/min speed
Bottom, second shower nozzle sprays substrate with 20mL/min speed, double spray guns apart from substrate about
40cm.The substrate of coating is cleaned 1 minute with deionized water, is dried 30 seconds in compressed air,
100 DEG C of heat hardenings 15 minutes, are cooled to room temperature.
2.2.4 anti-oxidant treatment
The substrate of silver coating optionally can be processed to strengthen antioxidant effect.In this step,
Substrate is in contact 5 minutes with anti-oxidant solution at 40 DEG C, and then substrate, which is washed with deionized, exceedes
3 times and in drying at room temperature.
2.3 glucose are reducing agent
It is unstable in the use of electroless plating that US4,737,188 (188 patent) described reducing agent
Fixed, wherein hydrogen can discharge and/or reduced sugar is degraded to sediment or other accessory substances.In addition, turning
Change sugar needs higher temperature to make silver-colored effective deposition as reducing agent.For example, 188 patents are begged for
Effect is bad when having discussed deposition of silver below 43-54 DEG C and high cost.
In the present invention, inventor successfully uses glucose as reducing agent effectively by silver nano-grain
Conforming layer is deposited on the epoxy resin surface of substrate.And the deposition process (i.e. spraying process) of silver layer
It is to be carried out in room temperature, it is more much lower than temperature required for 188 patents.
3 anti-scratch coating application steps
In this step, siliceous anti-scratch coating is coated on silver coating is applied substrate to improve
Anti-scratch performance.
The composition of 3.1 anti-scratch coating solutions
The compositing range of anti-scratch coating solution is listed in table 4A.
The compositing range of the anti-scratch coating solutions of table 4A
In a particular embodiment, the composition of anti-scratch coating solution is listed in table 4B.
The composition of the anti-scratch coating solutions of table 4B
| Composition | Weight % |
| MTMS | 34.57% |
| A189 | 4.00% |
| N-butanol | 12.04% |
| Acetic acid | 1.21% |
| Deionized water | 13.65% |
| 3% silica gel | 1.21% |
| DAA | 33.32% |
| Crystal violet | 0.01% |
3.1.1 the preparation of anti-scratch coating solution
In a particular embodiment, 36.0g A189,311.2g MTMS, 122.9g deionizations
Water, 10.8g acetic acid, 108.3g n-butanols and the silica gel of 10.8g 3% are in mixed at room temperature 15 minutes, institute
Solution ultrasonic wave 45 minutes in a water bath are obtained, is heated 10 hours at 70 DEG C and is cooled to room temperature.So
Add 0.11g crystal violets and 300g DAAs molten so as to obtain anti-scratch coating in the solution of cooling afterwards
Liquid.
3.2 coupling agent A189
A189, shown in the chemical constitution such as following formula (I) of (3- mercaptopropyis) trimethoxy silane
(I)
When anti-scratch coating is applied on silver coating, coupling agent A189 and the anti-scratch coating of silicon substrate plinth
Solution mixing is applied on silver coating strengthen the adhesion of the anti-scratch coating of silicon substrate plinth and silver coating.It is this
Enhanced adhesion is due to that A189 SH groups and the silver surface of silver coating interact to form strong
With reference to and formed, as shown in Figure 2.
3.3 crystal violets
The outer of product is applied if it is desired, can add in anti-scratch coating solution and improve by crystal violet
See.Especially, micro- yellow secondary effect that crystal violet can remove the silver surface of silver coating is added.
3.4 anti-scratch coatings are coated on the substrate of silver coating
The substrate for being coated with silver coating is contacted more than 1 minute with above-mentioned anti-scratch coating solution, and substrate exists
100 DEG C are heated beyond 18 hours, then are handled 3 hours at 150 DEG C, so as to obtain with multicoat
Substrate.
In a specific embodiment, anti-scratch coating solution is sprayed in substrate in the following manner.First
By deionized water with 8mL/min speed, 3bar air spraying in substrate, then in substrate
The anti-scratch coating solution of upper spraying 35 seconds, spray gun is apart from substrate about 15cm, and the substrate of spraying is at 150 DEG C
Heat hardening 3 hours.
4 sample tests
The decoration product (electroless plating sample) prepared by the above method and plating mode silver coating
Product (electroplated sample) is compared test.Metallic substrates are used for electroless plating sample and electroplated sample
Be steel Q-195A and/or kirsite #3.
4.1 decoration tests
Electroless plating sample and electroplated sample are in 45 degree of 380-780nm corner reflection UV-Vis light splitting
Photometer measurement.As shown in figure 3, electroless plating sample has higher corner reflection than electroplated sample.Nothing
The reflective surface area of electroplated sample is 26,264 and the reflective surface area of electroplated sample is 17,911.Therefore
Electroless plating sample has more preferable decorative effect than electroplated sample.
4.2 adhesion tests
With reference to ISO2409:2007 lacquer paintings and clear picture measure the ASTM of adhesion with adhesive tape test
D3359-08 standard method of test is used (cross cut test).Result shows as shown in Figure 4, nothing
Electroplated sample does not have fragment to come off, and reaches 5B standards (0% test area comes off), shows test
Area does not come off, than 4B standard more preferably (having the test area less than 5% to come off).Therefore this
A little coating, especially silver coatings are not easy to come off from electroless plating sample.
4.3 anticorrosive tests
With reference to ISO 9227:2006 in manual adjustment air corrosion test, operation salt spray (Fog)
The ASTM B117-07 standard methods of instrument are used (salt spray test -72 hours corrosion-free).Such as
Result shown in Fig. 5 shows that electroless plating sample does not change visually.Therefore electroless plating sample shows to resist
Corrosivity.
4.4 shock-testings
ASTM D2794-93 (2004) the standard method of test quilt deformed for organic coating resistance to rapid
Using (steel ball impact-without visible slight crack).As shown in fig. 6, electroless plating sample is without visible slight crack.
Therefore show that electroless plating sample is unlikely to deform.
4.5 hardness tests
With reference to ISO 15184:1998 lacquer paintings and clear picture test the ASTM of hardness of film with pencil
D3363-05 standard method of test is used (pencil test->=2 hours).Result as shown in Figure 7
Show this sustainable test of electroless plating sample 3-4 hours.Therefore show that electroless plating sample surfaces are resistant to
Scrape.
4.6RoHS instruction testings
The general detection certification Co., Ltd IEC62321 in this test reference Hong Kong:2008 perform.Such as
Shown in table 5, electroless plating sample does not detect Cd, Pb, Hg, Cr (VI), PBBs, PBDE.Without electricity
Plating sample does not detect toxic heavy metal or hydrocarbon thing yet, therefore is environmentally friendly.
The RoHS instruction testings of the electroless plating sample of table 5
4.7UV irradiation tests
With reference to the ASTM of ISO4892-3, the UV for nonmetallic materials the fluorescent lamp instrument irradiated
G154-04 standard methods and exposed mode 1/2 is used.Electroless plating sample as shown in Figure 8 can not
See color change.Therefore the coating of electroless plating sample is presented with anti-UV photoprotections.
4.8 waterproof tests
In this test, electroless plating sample is immersed in 40 DEG C of water 24 hours.Nothing as shown in Figure 9
Electroplated sample is without visual color change.Therefore show that electroless plating sample is waterproof.
4.9 antiacid tests
In this test, electroless plating sample is immersed in room temperature 0.1N sulfuric acid 24 hours.As schemed
Electroless plating sample shown in 10 is without visual color change.Therefore show that electroless plating sample is antiacid.
4.10 alkali resistants are tested
In this test, electroless plating sample is immersed in room temperature 0.1N NaOH 24 hours.
Electroless plating sample as shown in figure 11 is without visual color change.Therefore show that electroless plating sample is alkali resistant
's.
Therefore the exemplary of the present invention is fully described.Although specification is mentioned
Specific embodiment, it will be evident to those skilled in the art that can with the change of these details come
Implement the present invention.Therefore the present invention should not be construed as limited to embodiments set forth herein.
For example, acetone can be used in the process of the present invention as solvent, but those skilled in the art know it
For example methanol, benzene, triethylamine, acetic acid, chlorobenzene, phenol and quinolone can also for his chemical reagent
Use.
Moreover, those skilled in the art are appreciated that spray time can change and become according to different factors
Change, such as the substrate and painting environments that are sprayed-on.
Claims (16)
1. a kind of substrate with electroless plating, including one the adhesion on the substrate surface
Coating, the adherent coating includes the first silicon substrate plinth coupling agent；One on the adherent coating
It is lubricious, it is described lubricious comprising epoxy resin；One it is described it is lubricious on silver apply
Layer, the silver coating includes silver nano-grain；And an anti-scratch coating on the silver coating,
The anti-scratch coating includes second silicon substrate plinth coupling agent.
2. the substrate described in claim 1, wherein the first silicon substrate plinth coupling agent is γ-aminopropyl
Triethoxysilane；The second silicon substrate plinth coupling agent is (3- mercaptopropyis) trimethoxy silane.
3. a kind of method that electroless plating in substrate is coated with multicoat, including：
A., adherent coating comprising the first silicon substrate plinth coupling agent is coated on to the surface of the substrate；
B. lubricious comprising epoxy resin is coated on the adherent coating；
C. by the silver coating comprising silver nano-grain be coated on it is described it is lubricious on；
D. the anti-scratch coating comprising the second silicon substrate plinth coupling agent is coated on the silver coating.
4. the method described in claim 3, the first silicon substrate plinth coupling agent is the second of γ-aminopropyl three
TMOS；The second silicon substrate plinth coupling agent is (3- mercaptopropyis) trimethoxy silane.
5. the method described in claim 3, step a further comprises
I. by deionized water with 22mL/min speed, 3bar air spraying in substrate；
Ii. acetone is sprayed in substrate, adherent coating solution 30 seconds and spray gun is sprayed in substrate afterwards
Apart from substrate about 15cm；And
Iii. in the substrate being applied obtained by 150 DEG C of heat hardening step ii 15 minutes, so that described
The adherent coating is formed in substrate.
6. the method described in claim 3, step b further comprises
I. by deionized water with 55mL/min speed, 3bar air spraying in substrate；
Ii. acetone is sprayed in substrate, lubricious solution 30 seconds and spray gun is sprayed in substrate afterwards
Apart from substrate about 15cm；
Iii. in the substrate being applied obtained by 80 DEG C of heat hardening step ii 3-6 hours, so that described
Form described lubricious on the adherent coating of substrate.
7. the method described in claim 3, step c further comprises
I. the substrate for being applied step b is contacted with sensitizer；
Ii. the substrate being sensitized in 90 DEG C of dryings, is cooled down by dry substrate to room temperature in atmosphere；
Iii. spraying silver nitrate base soln and glucose basis are intersected simultaneously in the substrate being sensitized
Solution is so as to one layer of silver nano-grain of formation in the substrate of the cooling；And
Iv. the substrate being coated with 100 DEG C of baking oven heat hardening step iii at least 15 minutes.
8. the method described in claim 3, step c further comprises
I. the substrate for being applied step b is contacted with sensitizer；
Ii. the substrate being sensitized in 90 DEG C of dryings, is cooled down by dry substrate to room temperature in atmosphere；
Iii. by the substrate being sensitized deionized water rinsing 1 minute；
Iv. double head spray gun is used, silver nitrate base soln is by first shower nozzle with 10mL/min speed
Rate sprays substrate, and glucose base soln sprays base by second shower nozzle with 20mL/min speed
Bottom, double spray guns are sprayed 60 seconds apart from substrate about 40cm；
V. substrate is cleaned with deionized water 1 minute, is dried 30 seconds in compressed air, at 100 DEG C
Heat hardening 15 minutes, is cooled to room temperature, so as to form one layer of silver nano-grain.
9. the method described in claim 7 or 8, wherein the sensitizer includes Sn2+And Sn4+'s
Mixture.
10. the method described in claim 7 or 8, wherein the size of the silver nano-grain is
30-150nm。
11. the method described in claim 4, wherein step d further comprises
I. by deionized water with 8mL/min speed, 3bar air spraying in substrate；
Ii. anti-scratch coating solution is sprayed in substrate 35 seconds, spray gun is apart from substrate about 15cm, spraying
Substrate in 150 DEG C of heat hardenings 3 hours, so as to form institute on the silver coating of the substrate
The anti-scratch coating stated.
12. one is used for the suit of the electroless plating in substrate, including containing the first silicon substrate plinth coupling agent
Adherent coating solution, lubricious solution, base soln containing silver nitrate and Portugal containing epoxy resin
The electroless plating solution of grape sugar base soln and the anti-scratch coating containing the second silicon substrate plinth coupling agent are molten
Liquid.
13. the suit described in claim 12, the adherent coating solution includes 28.99%-
32.04% (w/w) epoxy resin E-51,0.23%-0.26% (w/w) BYK-361N, 6.96%-
7.33% (w/w) ethanol, 54.46%-60.19% (w/w) acetone, and 4.36%-4.81% (w/w)
TZ-550。
14. the suit described in claim 12, the lubricious solution includes 41.96%-
46.38% (w/w) epoxy resin E-51,0.22%-0.57% (w/w) BYK-361N, 5.77%-
5.82% (w/w) glycidyl 2- methyl phenyl ethers, 4.39%-4.93% (w/w) acetone,
23.82%-26.15% (w/w) DAA, 9.37%-15.61% (w/w) n-butanol, and
6.56%-8.44% (w/w) TZ-550.
15. the suit described in claim 12, the silver nitrate base soln include deionized water,
NaOH, silver nitrate and 28% ammoniacal liquor；The glucose base soln includes glucose, lemon
Acid, ethanol and deionized water.
16. the suit described in claim 12, the anti-scratch coating includes 33.88%-35.26%
(w/w) trimethoxymethylsila,e, 3.92%-4.08% (w/w) (3- mercaptopropyis) trimethoxy
Silane, 11.80%-12.28% (w/w) n-butanol, 13.61%-13.69% (w/w) deionized water,
The silica gel of 1.18%-1.23% (w/w) 3%, 32.66%-33.99% (w/w) DAA, and 0.01%
- 0.02% (w/w) crystal violet.
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| CN201610009344.8A CN106944322A (en) | 2016-01-07 | 2016-01-07 | The electroless plating of substrate |
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| CN201610009344.8A CN106944322A (en) | 2016-01-07 | 2016-01-07 | The electroless plating of substrate |
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| CN103608172A (en) * | 2011-05-20 | 2014-02-26 | 泗通贸易有限公司 | Fabrication of mirror-like coatings |
| CN104772965A (en) * | 2014-01-09 | 2015-07-15 | 纳米及先进材料研发院有限公司 | Surface treatment of mirror finish |
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