CN106282979A - Chemical plating front surface modifies system and the surface modification method of organic polymer base material - Google Patents
Chemical plating front surface modifies system and the surface modification method of organic polymer base material Download PDFInfo
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- CN106282979A CN106282979A CN201610828108.9A CN201610828108A CN106282979A CN 106282979 A CN106282979 A CN 106282979A CN 201610828108 A CN201610828108 A CN 201610828108A CN 106282979 A CN106282979 A CN 106282979A
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- base material
- organic polymer
- polymer base
- dressing agent
- chemical plating
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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
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2073—Multistep pretreatment
-
- 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
- C23C18/22—Roughening, e.g. by etching
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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 chemical plating front surface and modify system and the surface modification method of organic polymer base material, relate to surface preparation technical field.Organic polymer base material after surface coarsening is carried out surface self-organization and is processed so that its surface obtains and has and the functional group of metal ion strong bonding effect by the present invention, and then realizes combining closely of coated metal and organic polymer base material.Applied widely to organic polymer base material of coupling type stromal surface dressing agent system disclosed by the invention, surface modification method is simple to operation, the equipment without expensive, low cost, the coat of metal dense uniform formed and have strong adhesion with organic polymer base material.
Description
Technical field
The present invention relates to surface preparation technical field, modify system and a kind of use particularly to a kind of chemical plating front surface
Surface modification method before organic polymer base material chemical plating.
Background technology
Organic polymer material has the processing characteristics of excellent chemical stability and excellence.At organic polymer material table
Face uses specific processing method to obtain the surface metalation of layer of metal layer, i.e. polymeric material, and its surface can be made to have gold
Belong to some character of material, such as characteristics such as conduction, magnetic conduction or heat conduction, there is again the processability being better than metal material, can be extensive
It is applied to the fields such as incrustation, surface enhanced, surface obstruct, electromagnetic shielding, printed circuit board interconnection.
The method of organic polymer material surface metalation can be divided into physics and chemical two class methods.Physical mainly has
Vacuum evaporation, vacuum sputtering etc..Chinese patent " a kind of electromagnetic shielding with the coat of metal of Publication No. CN104507301A
Film and manufacturing process thereof " in disclose a kind of by metal film layer vacuum sputtering on polymer supported thin-film layers, to obtain tool
There is the coat of metal of capability of electromagnetic shielding.Chinese patent " a kind of non-conductive plastic surface gold of Publication No. CN1730719A
Belong to film layer preparation method " in report employing metallic tin be vacuum coating material, by radio frequency-ion coating technology in plastics system
Product surface production metal finishing coating.But these methods are required in the environment of fine vacuum operate, the equipment used is held high
Expensive and processing dimension is restricted, thus limits its range of application.Chemical method is the most not limited, and it mainly includes plating
With chemical plating.The Chinese patent " ultra-thin electromagnetic screened film and production technology thereof " of Publication No. CN104853577A disclose logical
Cross electroplating technology and form the conductive metal layer with electro-magnetic screen function on a carrier layer.But need first to use vacuum to spatter in producing
Penetrate, the method such as ion implanting or coating can implement plating after forming conductive layer, and therefore galvanoplastic do not eliminate expensive device
Dependence, and there is highly energy-consuming and high pollution problem.Chemical plating, under conditions of obstructed electric current, utilizes reducing agent containing metal
In the solution of ion, reducing metal ions become metal simple-substance be deposited on substrate surface.Chemical plating is efficient as one, energy-conservation
Surface metalation treatment technology, the coating even compact formed, in terms of barrier propterty, can improve product corrosion resistance and
Service life；At functional aspect, the specific functions such as the wear-resistant conductive of workpiece, greasy property can be improved.But, due to poly-
Laminate material surface can be relatively low, and roughness is less, uses the metal level that chemical plating is formed at organic polymer surface adhesion force
Difference.
In order to improve metal level that chemical plating the formed adhesive force on organic polymer surface, at surface of polymer material
Need before metallization first it to be carried out surface moditied processing." one is used for the Chinese patent of Publication No. CN101126156A
The technique of ABS plastic base material chemical plating pre-treatment " in utilize the Chitosan-phospholipid complex chelation to palladium catalyst, with change
Learn bonding action and replace the tradition non-conductive substrate surface chemistry treatment before plating physical bond effect to palladium catalyst.But, shell
Polysaccharide is only soluble in partially acidic solution, and under different pH value and temperature conditions, its molecular structure can occur bigger change, leads
Cause its SOLUTION PROPERTIES unstable, which has limited chitosan use on organic polymer base material.Publication No.
The Chinese patent " a kind of method in PolytetrafluoroethylFilm Film chemical plating " of CN101974741A is penetrated by Co 60 gamma
The mode that line irradiates carries out pre-irradiation process to polytetrafluoroethylene film, is reacted with polyamine compounds by base material afterwards, at thin film
Amine groups on surface self-organization, utilizes amine groups bond wire catalyst, then obtains gold by the method deposition of chemical plating
Belong to film.The technique that Co 60 gamma ray required for the method irradiates requires height to equipment and reaction environment, is unfavorable for its low one-tenth
Promoting the use of of this.
In the case, in order to low cost, realize the surface metalation of organic polymer material efficiently, one is found
Kind of technological process is simple, without process equipment with high costs, applied widely, surface metal-layer is attached with organic polymer base material
Put forth effort strong chemical plating front surface method of modifying to be particularly important.
Summary of the invention
To achieve these goals, the invention provides a kind of chemical plating front surface modify system and use this chemical plating
Front surface is modified system and organic polymer base material is carried out surface modification method.The present invention is by the organic polymer base material after roughening
Chemical plating front surface modification system carries out being processed so that the high forces that its surface has bond wire ion, to realize
Coated metal is combined closely with organic polymer base material；The chemical plating front surface of the present invention modifies system and surface modification method
There is advantage simple, efficient, energy saving, environmental protection, applied widely.
The technical scheme that the present invention provides is as follows:
Technical scheme 1:
A kind of chemical plating front surface modifies system, including coupling type stromal surface dressing agent, and organic solvent and deionized water,
Each component molar is than for coupling type stromal surface dressing agent: organic solvent: deionized water=1: 20～100: 0～6；Described coupling
Type stromal surface dressing agent be mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane, aminopropyl trimethoxysilane and
Any one or its combination in any in aminopropyl triethoxysilane, described organic solvent is ethanol, ethylene glycol, normal propyl alcohol, different
Any one or its in propanol, butanol, ethylene glycol monomethyl ether, ethylene glycol, ethyl acetate, butyl acetate, acetone, acetylacetone,2,4-pentanedione
The mutual solution of arbitrary proportion.
Technical scheme 2:
The surface modification method of a kind of organic polymer base material, utilizes chemical plating front surface to modify system organic to be roughened
Polymeric substrate carries out surface moditied processing so that stromal surface dressing agent is self-assembled to organic polymer base material；Described substrate
Coating material system includes stromal surface dressing agent, organic solvent and deionized water, and wherein, stromal surface dressing agent is coupling
Type, each component molar is than for coupling type stromal surface dressing agent: organic solvent: deionized water=1: 20～100: 0～6.
Organic polymer base material also should carry out surface coarsening before carrying out surface moditied processing and process bigger to obtain
Roughness, and then make base material have bigger contact area to react with stromal surface dressing agent；One concrete reality of the present invention
Execute the surface coarsening of organic polymer base material in example and process that organic polymer base material is specifically soaked in temperature is 40～80 DEG C
Coarsening solution in process 5～20 minutes；
Preferably, described coarsening solution is sodium hydroxide solution, potassium hydroxide solution or its mixed liquor, and coarsening solution concentration is
1～5mol/L.
In the present invention, organic polymer base material is polyimides, polyamide, Merlon, polyethylene terephthalate
In ester, polybutylene terephthalate (PBT), polyphenylene oxide, polyphenylene sulfide any one；
Coupling type stromal surface dressing agent in the present invention is particularly as follows: mercaptopropyl trimethoxysilane, mercapto propyl triethoxy
Any one or its combination in any in silane, aminopropyl trimethoxysilane and aminopropyl triethoxysilane.
In the embodiment of the present invention, the concrete operations that surface is modified are:
Be dissolved in the water obtained solution by described stromal surface dressing agent, is subsequently adding organic solvent and in 0～60 DEG C of ring
Stirring and dissolving 18～form homogeneous mixed solution in 24 hours under border, adds organic solvent diluting after having stirred, prepare chemistry
Plating front surface modifies system, and in described chemical plating front surface modification system, the volume fraction of organic solvent is 85～95%, substrate
The concentration of coating material is 0.05～0.4mol/L；Described organic solvent is ethanol, ethylene glycol, normal propyl alcohol, isopropanol, fourth
In alcohol, ethylene glycol monomethyl ether, ethylene glycol, ethyl acetate, butyl acetate, acetone and acetylacetone,2,4-pentanedione any one or its arbitrarily than
The mutual solution of example；
The organic polymer base material of described roughening is soaked in described chemical plating front surface modification system process 5～30 points
Clock, treatment temperature is 20～80 DEG C.
In the present invention, coupling type stromal surface dressing agent is bonded with the formation of organic polymer base material by self-assembling reaction,
Substrate surface forms one layer of self-assembled film, covalent bond and complexing adsorb follow-up metal ion, this chemical bonding
Effect makes the adhesive force of metal layer of subsequent chemistry plated deposition strong.
Preferred organic solvent in stromal surface dressing agent system of the present invention is conducive to stromal surface dressing agent organic poly-
Continuous film forming during compound substrate surface self-assembling reaction, increases organic polymer while reducing " coffee toroidal effect " further
The surface roughness of base material, provides " anchor point " of mechanical bond, it is possible to improve adhesive force further for follow-up metal deposit.
Compared with prior art, the method have the advantages that
1. the stromal surface dressing agent organic polymer applicatory base material scope of the present invention is wide, by strong complexing or
The metal ion that covalent bond absorption is follow-up, the plated layer compact of formation is uniform, and has between chemical deposit and organic polymer matrix
There is strong combination.
2. the stromal surface dressing agent system applicable base materials scope of the present invention is wide, and surface modification processes flow process is simple, cost
Cheap, be suitable to industrial application；
Accompanying drawing explanation
Fig. 1 is the surface modification method schematic flow sheet of organic polymer base material of the present invention；
Fig. 2 is to process (comparative example) without stromal surface dressing agent and modify system through chemical plating front surface of the present invention
Process polyethylene terephthalate (PET) base material obtained energy dispersion spectrum (EDS) contrast after adsorbing metal ions
Figure；
Fig. 3 is to process (comparative example) without stromal surface dressing agent and modify system through chemical plating front surface of the present invention
Process the coating light obtained after polyethylene terephthalate (PET) base material obtained carries out electroless copper under the same conditions
Learn microstructure comparison diagram.
Detailed description of the invention
Below in conjunction with specific embodiment and Figure of description, the present invention is described in detail:
As it is shown in figure 1, the surface modification method of a kind of organic polymer base material, specifically include organic polymer base material surface
It is roughened and at organic polymer base material surface self-organization stromal surface dressing agent；The present invention carries out the concrete grammar of roughening treatment also
Being not particularly limited, in a specific embodiment of the present invention, roughening treatment is that organic polymer base material is soaked in strong base solution
In (preferably concentration is sodium hydroxide or the potassium hydroxide of 1～5mol/L) and carry out heat treatment, controlling strong base solution temperature is
40～80 DEG C, process 5～20 minutes；Then take out and be soaked in stromal surface dressing agent system disclosed by the invention and (include coupling
Type stromal surface dressing agent, organic solvent and deionized water, each component molar is than for coupling type stromal surface dressing agent: You Jirong
Agent: deionized water=1: 20～100: 0～6) in carry out surface moditied processing so that stromal surface dressing agent is self-assembled to organic
Polymeric substrate.
Embodiment:
The surface modification method of a kind of organic polymer base material, specifically includes following steps:
Step A: the surface coarsening of polyethylene terephthalate (PET) base material；
Preparation 300ml solute concentration be the sodium hydroxide solution of 2.5mol/L as surface coarsening liquid, by surface coarsening liquid
Heating, constant temperature is maintained at 60 DEG C, polyethylene terephthalate (PET) base material is immersed surface coarsening liquid and processes 20 minutes,
Polyethylene terephthalate (PET) surface is made to reach to be suitable to the state of self assembly；
Step B: polyethylene terephthalate (PET) substrate surface after roughening is modified；
60ml aminopropyl triethoxysilane and 20ml mercaptopropyltriethoxysilane is added in 10ml deionized water, then
Add 5ml methanol, 3ml isopropanol, 2ml acetylacetone,2,4-pentanedione and stir 18 hours under 25 DEG C of constant temperature, after having stirred, adding 650ml
Isopropanol and 250ml ethylene glycol monomethyl ether are diluted, and stirring, to mix homogeneously, obtains chemical plating front surface and modifies system；
Above-mentioned chemical plating front surface is modified system heating, and constant temperature is maintained at 50 DEG C, gathering roughened process benzene two
Formic acid glycol ester (PET) base material immerses in described chemical plating front surface modification system and reacts 30 minutes so that stromal surface is repaiied
Decorations agent is self-assembled on polyethylene terephthalate (PET) base material；Above-mentioned process is dried after completing and uses isopropyl respectively
Alcohol and deionized water rinsing base material, after drying has i.e. obtained the polyethylene terephthalate that chemical plating front surface is modified
(PET) base material.
Polyethylene terephthalate (PET) base surface roughness that the embodiment of the present invention obtains can reach
0.342 μm, far above the roughness (0.01 μm) of the base material merely through roughening treatment, this is conducive to the further of coating adhesion
Promote.
Comparative example:
Preparation 300ml solute concentration be the sodium hydroxide solution of 2.5mol/L as surface coarsening liquid, by surface coarsening liquid
Heating, constant temperature is maintained at 60 DEG C, polyimide base material immerses surface coarsening liquid and processes 20 minutes, obtain after surface coarsening
Polyethylene terephthalate (PET) base material.
Polyethylene terephthalate (PET) base material that Fig. 2 is comparative example and embodiment obtains is to adsorption of metal ions
The comparison diagram of performance: polyethylene terephthalate (PET) base material that comparative example and embodiment prepare is soaked in silver nitrate
Solution also carries out constant temperature process, carries out energy dispersion spectrum (EDS) and analyze, wherein after ultrasonic cleaning is clean the most in deionized water
Figure (a) and figure (b) are respectively energy dispersion spectrum (EDS) of comparative example and embodiment sample.It can be seen that through this
The upper silver ion of polyethylene terephthalate (PET) substrate surface bonding that bright surface is modified.
Polyethylene terephthalate (PET) base material that Fig. 3 is comparative example and embodiment obtains enters under the same conditions
The optical microphotograph pattern comparison diagram of coating is obtained: by poly terephthalic acid second prepared to comparative example and embodiment after row electroless copper
Diol ester (PET) base material is soaked in silver nitrate solution and carries out constant temperature process, and carries out chemistry under identical process conditions
Copper facing, carries out optical microphotograph (OM) morphology analysis to coating, and wherein figure (c) is respectively at comparative example and embodiment base with figure (d)
Optical microphotograph (OM) pattern of the coating obtained on material.It can be seen that on embodiment gained base material electroless copper,
The layers of copper dense uniform arrived, does not observes do not have obvious hole.
Complex chart 2 and Fig. 3 is it follows that use the stromal surface dressing agent system that the present invention provides to organic polymer-based
After material carries out surface modification, base material successfully realizes surface self-organization and modifies, it is thus achieved that have strong bonding effect to metal ion
Group, beneficially combining closely and the even compact of chemical deposit between chemical deposit and base material.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is example
Property, it is impossible to be interpreted as limitation of the present invention, those of ordinary skill in the art is without departing from the principle of the present invention and objective
In the case of above-described embodiment can be changed within the scope of the invention, revise, replace and modification.
Claims (7)
1. a chemical plating front surface modifies system, it is characterised in that include coupling type stromal surface dressing agent, organic solvent and
Deionized water, each component molar is than for coupling type stromal surface dressing agent: organic solvent: deionized water=1: 20～100: 0～
6；Described coupling type stromal surface dressing agent is mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane, aminopropyl front three
Any one or its combination in any in TMOS and aminopropyl triethoxysilane, described organic solvent be ethanol, ethylene glycol,
Normal propyl alcohol, isopropanol, butanol, ethylene glycol monomethyl ether, ethylene glycol, ethyl acetate, butyl acetate, acetone, acetylacetone,2,4-pentanedione are appointed
The mutual solution of one or any ratio.
2. the surface modification method of an organic polymer base material, it is characterised in that utilize chemical plating front surface to modify system pair
The organic polymer base material of roughening carries out surface modification so that stromal surface dressing agent is self-assembled to organic polymer base material table
Face；Described chemical plating front surface is modified system and is included coupling type stromal surface dressing agent, organic solvent and deionized water, each component
Mol ratio is coupling type stromal surface dressing agent: organic solvent: deionized water=1: 20～100: 0～6.
The surface modification method of a kind of organic polymer base material the most according to claim 2, it is characterised in that organic polymer
The surface coarsening of thing base material processes particularly as follows: organic polymer base material is soaked in the coarsening solution that temperature is 40～80 DEG C process
5～20 minutes.
The surface modification method of a kind of organic polymer base material the most according to claim 3, it is characterised in that described roughening
Liquid is sodium hydroxide solution, potassium hydroxide solution or its mixed liquor, and coarsening solution concentration is 1～5mol/L.
The surface modification method of a kind of organic polymer base material the most according to claim 2, it is characterised in that described organic
Polymeric substrate is polyimides, polyamide, Merlon, polyethylene terephthalate, polybutylene terephthalate
In ester, polyphenylene oxide, polyphenylene sulfide any one.
The surface modification method of a kind of organic polymer base material the most according to claim 5, it is characterised in that described substrate
Coating material is coupling type stromal surface dressing agent, specially mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane,
Any one in aminopropyl trimethoxysilane and aminopropyl triethoxysilane or its combination in any.
The surface modification method of a kind of organic polymer base material the most according to claim 6, it is characterised in that described surface
The concrete operations modified are:
Be dissolved in the water obtained solution by described stromal surface dressing agent, is subsequently adding organic solvent and under 0～60 DEG C of environment
Stirring and dissolving 18～form homogeneous mixed solution in 24 hours, adds organic solvent diluting after having stirred, before preparing chemical plating
System is modified on surface, and in described chemical plating front surface modification system, the volume fraction of organic solvent is 85～95%, stromal surface
The concentration of dressing agent is 0.05～0.4mol/L；Described organic solvent is ethanol, ethylene glycol, normal propyl alcohol, isopropanol, butanol, second
Any one or its arbitrary proportion in glycol methyl ether, ethylene glycol, ethyl acetate, butyl acetate, acetone and acetylacetone,2,4-pentanedione
Solution mutually；
The organic polymer base material of described roughening is soaked in described chemical plating front surface modification system process 5～30 minutes,
Treatment temperature is 20～80 DEG C.
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| CN107988589A (en) * | 2017-11-23 | 2018-05-04 | 深圳大学 | A kind of nano metal compound and preparation method thereof |
| 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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2016
- 2016-09-18 CN CN201610828108.9A patent/CN106282979B/en active Active
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| CN107988589A (en) * | 2017-11-23 | 2018-05-04 | 深圳大学 | A kind of nano metal compound and preparation method thereof |
| 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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