CN109652787A - Pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating - Google Patents
Pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating Download PDFInfo
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- CN109652787A CN109652787A CN201811567655.1A CN201811567655A CN109652787A CN 109652787 A CN109652787 A CN 109652787A CN 201811567655 A CN201811567655 A CN 201811567655A CN 109652787 A CN109652787 A CN 109652787A
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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
- C23C18/22—Roughening, e.g. by etching
- C23C18/24—Roughening, e.g. by etching using acid aqueous solutions
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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
- C23C18/2086—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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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
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention belongs to special material surface is modified and electroplating technology, and in particular to pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating.Include the following steps: destressing, oil removing, pre-treatment, etching, adjustment activation, dispergation chemical plating.The present invention solves the problems, such as that bond strength is lower in the prior art and product qualification rate is lower, and the coat of metal bond strength before chemical plating through the invention after pretreating process is high, not easily to fall off, product qualification rate is high and is adapted to industrial application.
Description
Technical field
The invention belongs to the modification of special material surface and electroplating technologies, and in particular to a kind of polyether-ether-ketone composite material
Pretreating process before surface chemical plating.
Background technique
Plastics are articles common in daily life.Present market is that common some frostings have decorative metal
Layer, it is bright and smooth.The surface metalation of these plastics is generally by physical gas phase deposition technology or chemical deposition technique
It is process.However, physical gas phase deposition technology is difficult to metallize for anisotropic product progress surface.
Plating consumes more energy mainly for being electroplated for electric conductor.Chemical plating process is simple, production procedure
It is convenient, but need to make its surface active to pretreatment before carrying out between plastics macromolecule.Such as: before the chemical plating of ABS plastic
Pretreatment general technology is to remove stress → surface degreasing → cleaning → roughening → recycling → cleaning → reduction → cleaning → (quick
Change) → cleaning → preimpregnation → colloid palladium activation → recycling → cleaning → dispergation → cleaning → chemical plating.
Polyether-ether-ketone resin is a kind of aromatics linear thermoplastic's Special Resin of high crystalline.It is with aromatic series thermosetting
Characteristics, the high comprehensive performances such as the easy processing of the heat resistance of property resin, chemical stability and thermoplastic resin generally use injection
The methods of molding, extrusion molding, compression molding, blow molding machine-shaping.In order to meet manufacture high-precision, it is heat-resisting, corrosion-resistant,
Wear-resistant, antifatigue and shock resistance components requirements are blended polyether-ether-ketone resin, are filled, the enhancing such as fiber composite
Modification, to obtain more excellent performance of polyether-ether-ketone resin composite material.Polyether-ether-ketone be by difluoro benzophenone with
One kind special engineering plastics made of aromatic dicarboxylic phenol high-temperature polycondensation, can also be by aromatic series dihalo object and 4,4'- dihydroxy
Benzophenone polycondensation, which becomes, generally has high thermo-oxidative stability.Strong mechanical performance belongs to special engineering plastics.Polyether-ether-ketone energy and glass
Reinforcing material or composite material is made in glass fiber or carbon fiber, can be applied to high temperature structural materials, wear-resistant material and electrical isolation
The fields such as the industry such as material, petroleum and petrochemical industry and aerospace.However, with the development of science and technology, polyether-ether-ketone surface metalation has
The functionalization for helping material meets the functions such as electric conductivity, corrosion resistance and dicoration.National inventing patent application number
201410814151.0 disclose a kind of polyether-ether-ketone and polyether-ether-ketone/carbon nano tube compound material without palladium chemical plating method.
The invention pre-treating technology mainly uses the concentrated sulfuric acid to carry out surface swelling treatment as sweller, then inhales on the surface of swelling
Then attached reducing agent carries out chemical plating, polyether-ether-ketone or polyether-ether-ketone/carbon nano tube compound material surface is made to deposit one layer of metal
Coating, binding force of cladding material are preferable.
In the prior art, that there are bond strengths is lower, product is qualified for polyether-ether-ketone composite material surface chemical metal plating
Rate is lower.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of polyether-ether-ketone composite material surface chemical platings
Preceding pretreating process solves the problems, such as that bond strength is lower in the prior art and product qualification rate is lower, through the invention
Coat of metal bond strength before chemical plating after pretreating process is high, not easily to fall off, product qualification rate is high and is adapted to industry
On application.
The purpose of the present invention is achieved through the following technical solutions:
Pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating, includes the following steps:
Step 1: destressing: extremely using ethanol washing surface by the polyether-ether-ketone composite material product to have completed
After 2 times few, it is put into dry 2~10h in the baking oven that temperature is 40~80 DEG C, polyether-ether-ketone composite material system is obtained after the completion of dry
Part is stand-by；
Step 2: oil removing: it is in 50~80 DEG C of Wax removal waters that polyether-ether-ketone composite material product in step 1, which is put into temperature,
It is cleaned by ultrasonic 5~30min, the polyether-ether-ketone composite material product for obtaining oil removing is stand-by；
Step 3: pre-treatment: the polyether-ether-ketone composite material product of oil removing in step 2 being washed at least 2 times, is placed into
At least 5min is impregnated in the pretreatment solution that temperature is 20~30 DEG C, it is dry after taking out washing at least 2 times, obtain the poly- of pre-treatment
Polyetherether ketone composite product is stand-by；
Step 4: etching: by the polyether-ether-ketone composite material product of pre-treatment in step 3 be put into etching solution etching 5~
30min, the polyether-ether-ketone composite material product etched are stand-by；
Step 5: adjustment activation: it is 30~50 that the polyether-ether-ketone composite material product etched in step 4, which is put into temperature,
DEG C adjustment liquid in handle 10~30min, then it is 20~30 DEG C of colloid palladium that polyether-ether-ketone composite material product, which is put into temperature,
Middle activation at least 5min, the polyether-ether-ketone composite material product activated are stand-by；
Step 6: dispergation chemical plating: by the polyether-ether-ketone composite material product activated in step 5 be put into temperature be 20~
2~5min of dispergation in 45 DEG C of strong alkali aqueous solution, then 1~5min is rinsed, finally on the surface of polyether-ether-ketone composite material product
Upper chemical plating metal makes its surface metalation.
By pretreating process before polyether-ether-ketone composite material surface chemical plating of the present invention, treated that polyether-ether-ketone is compound
Material, then after carrying out chemical plating surface metalation, the bond strength of metal layer and polyether-ether-ketone composite material product increases,
The binding force for improving metal layer and polyether-ether-ketone composite material product improves the qualification rate of product, and is suitable for anisotropic product
Surface metalation.
The process of pretreating process is simple, at low cost, high-efficient before polyether-ether-ketone composite material surface chemical plating, and technique is steady
It is fixed, it is easy for construction, it is suitable for industrial application, there is wide industrial application value；Pre-treatment use reagent cost is low, effect
It is good.
Before polyether-ether-ketone composite material surface chemical plating pretreating process first carry out destressing, oil removing, pre-treatment, etching,
Adjustment activation and dispergation chemical plating, more by the polyether-ether-ketone composite material product after destressing, oil removing, pre-treatment, etching
Easily-activated and binding force enhancing with metal layer, the metal layer that chemical plating is formed are more secured.
Further, Wax removal water is grouped as by the group of following parts by weight in the step 2: coconut oil diethanol amide 20
~30 parts, 5~8 parts of sodium alkyl benzene sulfonate, 10~15 parts of alkylolamides phosphate, 3~5 parts of sodium secondary alkyl sulfonate, anion
3~5 parts of surfactant, 20~30 parts of water.
Wax removal water the preparation method comprises the following steps: by coconut oil diethanol amide, sodium alkyl benzene sulfonate, alkylolamides phosphate,
Sodium secondary alkyl sulfonate and anionic surfactant sequentially add in water according to weight, are stirred at least under room temperature
30min to get.
Further, pretreatment solution has the group of following parts by weight to be grouped as in the step 3: 5~8 parts of sodium carbonate, phosphorus
5~8 parts of acid dihydride sodium, 3~5 parts of sodium pyrophosphate, 2~3 parts of copper sulphate, 1~2 part of nickel sulfate, 3~5 parts of tartaric acid, water 900~
1000 parts.
Pretreatment solution the preparation method comprises the following steps: by sodium carbonate, sodium dihydrogen phosphate, sodium pyrophosphate, copper sulphate, nickel sulfate and wine
Stone acid sequentially adds in water according to weight, be stirred under room temperature at least 30min to get.
Further, drying temperature is 95~105 DEG C in the step 3, and drying time is 1~2h.
Further, etching solution has the group of following parts by weight to be grouped as in the step 4: 20~50 parts of hydrofluoric acid sodium, body
Fraction is 500~800 parts of sulfuric acid solution, 2~3 parts of thiocarbamide of 20~30%.
Etching solution the preparation method comprises the following steps: hydrofluoric acid sodium and thiocarbamide are added in the sulfuric acid solution that volume fraction is 20~30%,
Be stirred under room temperature at least 30min to get.
Further, in the step 5 adjust liquid be solution A, solution B, solution C and solution D according to 1:(0.6~
0.7): (0.6~0.8): (1.0~1.2) are uniformly mixed into liquid is adjusted, and wherein solution A is the hydrochloric acid of 0.5~100mM
Solution, solution B are the copper-bath of 0.01~30mM, and solution C is the sulfuric acid solution that volume fraction is 20~30%, solution D
For the cation surface activating wetting agent quaternary ammonium salt solution of 2~10g/L.
Further, in the step 5 colloid palladium the preparation method comprises the following steps: the stannous chloride of 10~200 parts by weight is being stirred
In the hydrochloric acid solution that the mass fraction for being dissolved in 100~500 parts by weight under the conditions of mixing is 30~35%, 2~10 parts by weight are added
Sodium stannate stirs to get milky white solution, is denoted as solution E；0.5~3 parts by weight palladium chloride is added 100 in another container again
In the mixed liquor of hydrochloric acid solution and 200~600 parts by weight of deionized water that the mass fraction of~500 parts by weight is 30~35%,
After dissolving by heating completely, 0.5~5 parts by weight stannous chloride is added at 25~40 DEG C, obtains solution F after stirring 1~5min, then
Solution F is poured into solution E, 200~300 parts by weight of deionized water are added, keeps the temperature 4~6h at 50~75 DEG C to get colloid
Palladium.
Further, the sodium hydrate aqueous solution that strong alkali aqueous solution is 180~220mg/L in the step 6.
Further, in the step 6 chemical plating metal be nickel, copper or silver,
The beneficial effects of the present invention are:
1. by pretreating process before polyether-ether-ketone composite material surface chemical plating of the present invention, treated that polyether-ether-ketone is answered
Condensation material product, then after carrying out chemical plating surface metalation, the bond strength of metal layer and polyether-ether-ketone composite material product increases
Greatly, the binding force for improving metal layer and polyether-ether-ketone composite material product improves the qualification rate of product, and is suitable for anisotropic system
The surface metalation of part；
2. the process of pretreating process is simple before polyether-ether-ketone composite material surface chemical plating of the present invention, at low cost, efficiency
Height, process stabilizing is easy for construction, is suitable for industrial application, has wide industrial application value；Pre-treatment use reagent at
This is low, effect is good；By pretreatment solution and adjustment liquid, treated that polyether-ether-ketone composite material article surface tension is bigger, more
It is easily-activated, it is stronger with the binding force of metal layer after activation；
3. pretreating process first carries out destressing, oil removing, pre-treatment, erosion before polyether-ether-ketone composite material surface chemical plating
It carves, adjust activation and dispergation chemical plating, pass through the polyether-ether-ketone composite material product after destressing, oil removing, pre-treatment, etching
More easily-activated and binding force enhancing with metal layer, the metal layer that chemical plating is formed are more secured.
Detailed description of the invention
Fig. 1 is the anisotropic product structural schematic diagram of polyether-ether-ketone composite material product；
Fig. 2 is structural schematic diagram after polyether-ether-ketone composite material product chemical plating；
In figure: 1- polyether-ether-ketone composite material product, 2- metal layer.
Specific embodiment
Technical solution of the present invention is described in further detail combined with specific embodiments below, but protection scope of the present invention is not
It is confined to as described below.
Embodiment 1
Pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating, includes the following steps:
Step 1: destressing: extremely using ethanol washing surface by the polyether-ether-ketone composite material product to have completed
After 2 times few, it is put into dry 2~10h in the baking oven that temperature is 40~80 DEG C, polyether-ether-ketone composite material system is obtained after the completion of dry
Part is stand-by；
Step 2: oil removing: it is in 50~80 DEG C of Wax removal waters that polyether-ether-ketone composite material product in step 1, which is put into temperature,
It is cleaned by ultrasonic 5~30min, the polyether-ether-ketone composite material product for obtaining oil removing is stand-by；
Step 3: pre-treatment: the polyether-ether-ketone composite material product of oil removing in step 2 being washed at least 2 times, is placed into
At least 5min is impregnated in the pretreatment solution that temperature is 20~30 DEG C, it is dry after taking out washing at least 2 times, obtain the poly- of pre-treatment
Polyetherether ketone composite product is stand-by；
Step 4: etching: by the polyether-ether-ketone composite material product of pre-treatment in step 3 be put into etching solution etching 5~
30min, the polyether-ether-ketone composite material product etched are stand-by；
Step 5: adjustment activation: it is 30~50 that the polyether-ether-ketone composite material product etched in step 4, which is put into temperature,
DEG C adjustment liquid in handle 10~30min, then it is 20~30 DEG C of colloid palladium that polyether-ether-ketone composite material product, which is put into temperature,
Middle activation at least 5min, the polyether-ether-ketone composite material product activated are stand-by；
Step 6: dispergation chemical plating: by the polyether-ether-ketone composite material product activated in step 5 be put into temperature be 20~
2~5min of dispergation in 45 DEG C of strong alkali aqueous solution, then 1~5min is rinsed, finally on the surface of polyether-ether-ketone composite material product
Upper chemical plating metal makes its surface metalation.
Specifically, Wax removal water is grouped as by the group of following parts by weight in the step 2: coconut oil diethanol amide 20~
30 parts, 5~8 parts of sodium alkyl benzene sulfonate, 10~15 parts of alkylolamides phosphate, 3~5 parts of sodium secondary alkyl sulfonate, anion table
3~5 parts of face activating agent, 20~30 parts of water.
Specifically, pretreatment solution has the group of following parts by weight to be grouped as in the step 3: 5~8 parts of sodium carbonate, phosphoric acid
5~8 parts of sodium dihydrogen, 3~5 parts of sodium pyrophosphate, 2~3 parts of copper sulphate, 1~2 part of nickel sulfate, 3~5 parts of tartaric acid, water 900~
1000 parts.
Specifically, drying temperature is 95~105 DEG C in the step 3, and drying time is 1~2h.
Specifically, etching solution has the group of following parts by weight to be grouped as in the step 4: 20~50 parts of hydrofluoric acid sodium, volume
Score is 500~800 parts of sulfuric acid solution, 2~3 parts of thiocarbamide of 20~30%.
Specifically, it is solution A, solution B, solution C and solution D according to 1:(0.6~0.7 that liquid is adjusted in the step 5):
(0.6~0.8): (1.0~1.2) are uniformly mixed into liquid is adjusted, and wherein solution A is the hydrochloric acid solution of 0.5~100mM,
Solution B is the copper-bath of 0.01~30mM, and solution C is the sulfuric acid solution that volume fraction is 20~30%, solution D is 2~
The cation surface activating wetting agent quaternary ammonium salt solution of 10g/L.
Specifically, in the step 5 colloid palladium the preparation method comprises the following steps: the stannous chloride of 10~200 parts by weight is being stirred
Under the conditions of be dissolved in 100~500 parts by weight mass fraction be 30~35% hydrochloric acid solution in, add 2~10 parts by weight tin
Sour sodium, stirs to get milky white solution, is denoted as solution E；Again in another container by 0.5~3 parts by weight palladium chloride be added 100~
In the mixed liquor of hydrochloric acid solution and 200~600 parts by weight of deionized water that the mass fraction of 500 parts by weight is 30~35%, add
After heat of solution is complete, 0.5~5 parts by weight stannous chloride is added at 25~40 DEG C, obtains solution F after stirring 1~5min, then will
Solution F is poured into solution E, and 200~300 parts by weight of deionized water are added, and keeps the temperature 4~6h at 50~75 DEG C to get colloid palladium.
Specifically, the sodium hydrate aqueous solution that strong alkali aqueous solution is 180~220mg/L in the step 6.
Specifically, the metal of chemical plating is nickel, copper or silver in the step 6.
The design parameter of 1~embodiment of embodiment 6 is as shown in table 1, and 1~embodiment of embodiment 4 is the skill that the present invention limits
Art parameter does not use in embodiment 5 pretreatment liquid to carry out pre-treatment, and adjustment liquid is not used to be handled in embodiment 6, wherein real
Applying 5~embodiment of example 6 is comparative examples.
Table 1
The specific performance parameter of 1~embodiment of embodiment 6 is as shown in table 2, and 1~embodiment of embodiment 4 is that the present invention limits
Technical parameter, do not use in embodiment 5 pretreatment liquid to carry out pre-treatment, adjustment liquid do not used to be handled in embodiment 6,
Middle 5~embodiment of embodiment 6 is comparative examples.
Referring to the B method in ASTM D3359-83, the coat of metal is measured with grid scratch tape method and polyether-ether-ketone is compound
The binding force of material: testing procedure is as follows: after sample is disposed as required, sample being placed on a fixed pedestal
On, then it is put into togerther under the magnifying glass with light source together with pedestal；Respectively mark 6 quarters in two perpendicular directions with blade
Trace forms 25 grids, and indentation spacing is 1mm, and indentation will reach basis material, and the film for gently brushing away loosening with soft brush is broken
Piece；Then the pressure sensitive adhesive tape of the long 75mm of clip, is all covered on scored areas, it is desirable that adhesive tape come into full contact with coating it is Nian Jie, in
Between do not stay bubble；Adhesive tape is uniformly firmly quickly pulled in 180 ° as far as possible in opposite direction after retaining 90 ± 30s, is then existed
The quantity and area of the film sticked out by adhesive tape are checked under magnifying glass.
It is assessed referring to following standard.Binding force is divided into 6 grades, and with 5B grades, (edge of notch is very smooth, without grid point
From) be it is best, 4B grades (having the coating segregation of very little in grid infall, the region less than 5% is affected) for qualification, 3B grades
(having small coating segregation in grid infall, 5~15% region is affected), 2B grades (marginal portion of notch separates, in side
Lattice infall has large stretch of coating segregation or the separation of partial grid full wafer, and 15~35% region is affected), 1B grades (notch
The separation of edge sheet, some grids partly or entirely separate, and 35~65% region is affected), 0B grades (grid infall is in blocks
Coating segregation, the region greater than 65% is affected).
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
| Grade | 5B | 5B | 5B | 5B | 4B | 4B |
Table 2
As can be seen that the grade of 1~embodiment of embodiment 4 is substantially better than comparative example from the data of table 2, embodiment 5~
The bond strength of embodiment 6 is lower than 1~embodiment of embodiment 4.
The above is only a preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form should not be regarded as an exclusion of other examples, and can be used for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection scope of appended claims of the present invention
It is interior.
Claims (9)
1. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating, which comprises the steps of:
Step 1: destressing: the polyether-ether-ketone composite material product to have completed is used ethanol washing surface at least 2 times
Afterwards, it is put into dry 2 ~ 10h in the baking oven that temperature is 40 ~ 80 DEG C, it is stand-by to obtain polyether-ether-ketone composite material product after the completion of dry；
Step 2: oil removing: it is that ultrasound is clear in 50 ~ 80 DEG C of Wax removal waters that polyether-ether-ketone composite material product in step 1, which is put into temperature,
5 ~ 30min is washed, the polyether-ether-ketone composite material product for obtaining oil removing is stand-by；
Step 3: pre-treatment: the polyether-ether-ketone composite material product of oil removing in step 2 being washed at least 2 times, temperature is placed into
It is dry after taking out washing at least 2 times to impregnate at least 5min in 20 ~ 30 DEG C of pretreatment solutions, obtain the polyethers ether of pre-treatment
Ketone composite product is stand-by；
Step 4: etching: by the polyether-ether-ketone composite material product of pre-treatment in step 3 be put into etching solution etching 5 ~
30min, the polyether-ether-ketone composite material product etched are stand-by；
Step 5: adjustment activation: the polyether-ether-ketone composite material product etched in step 4 is put into the tune that temperature is 30 ~ 50 DEG C
Handle 10 ~ 30min in whole liquid, then by polyether-ether-ketone composite material product be put into temperature be activated in 20 ~ 30 DEG C of colloid palladium to
Few 5min, the polyether-ether-ketone composite material product activated are stand-by；
Step 6: dispergation chemical plating: it is 20 ~ 45 DEG C that the polyether-ether-ketone composite material product activated in step 5, which is put into temperature,
2 ~ 5min of dispergation in strong alkali aqueous solution, then rinse 1 ~ 5min, the finally chemical plating on the surface of polyether-ether-ketone composite material product
Metal makes its surface metalation.
2. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1, feature exist
In Wax removal water is grouped as by the group of following parts by weight in the step 2: 20 ~ 30 parts of coconut oil diethanol amide, benzene sulfonamide
5 ~ 8 parts of sour sodium, 10 ~ 15 parts of alkylolamides phosphate, 3 ~ 5 parts of sodium secondary alkyl sulfonate, 3 ~ 5 parts of anionic surfactant, water
20 ~ 30 parts.
3. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1, feature exist
In pretreatment solution has the group of following parts by weight to be grouped as in the step 3: 5 ~ 8 parts of sodium carbonate, 5 ~ 8 parts of sodium dihydrogen phosphate,
3 ~ 5 parts of sodium pyrophosphate, 2 ~ 3 parts of copper sulphate, 1 ~ 2 part of nickel sulfate, 3 ~ 5 parts of tartaric acid, 900 ~ 1000 parts of water.
4. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1 or 3, feature
It is, drying temperature is 95 ~ 105 DEG C in the step 3, and drying time is 1 ~ 2h.
5. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1, feature exist
In etching solution has the group of following parts by weight to be grouped as in the step 4: 20 ~ 50 parts of hydrofluoric acid sodium, volume fraction is 20 ~ 30%
500 ~ 800 parts of sulfuric acid solution, 2 ~ 3 parts of thiocarbamide.
6. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1, feature exist
In adjusting liquid in the step 5 is solution A, solution B, solution C and solution D according to 1:(0.6 ~ 0.7): (0.6 ~ 0.8): (1.0
~ 1.2) it is uniformly mixed into liquid is adjusted, wherein solution A is the hydrochloric acid solution of 0.5 ~ 100mM, and solution B is 0.01 ~ 30mM's
Copper-bath, solution C are the sulfuric acid solution that volume fraction is 20 ~ 30%, and the cation surface activating that solution D is 2 ~ 10g/L moistens
Humectant quaternary ammonium salt solution.
7. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1 or 6, feature
It is, colloid palladium the preparation method comprises the following steps: stannous chloride of 10 ~ 200 parts by weight is dissolved under agitation in the step 5
In the hydrochloric acid solution that the mass fraction of 100 ~ 500 parts by weight is 30 ~ 35%, 2 ~ 10 parts by weight sodium stannates are added, cream is stirred to get
White solution is denoted as solution E；0.5 ~ 3 parts by weight palladium chloride is added to the quality point of 100 ~ 500 parts by weight in another container again
In the mixed liquor of hydrochloric acid solution and 200 ~ 600 parts by weight of deionized water that number is 30 ~ 35%, after dissolving by heating completely, 25 ~ 40
0.5 ~ 5 parts by weight stannous chloride is added at DEG C, obtains solution F after stirring 1 ~ 5min, then solution F is poured into solution E, is added
200 ~ 300 parts by weight of deionized water keep the temperature 4 ~ 6h at 50 ~ 75 DEG C to get colloid palladium.
8. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1, feature exist
In strong alkali aqueous solution is the sodium hydrate aqueous solution of 180 ~ 220mg/L in the step 6.
9. pretreating process before a kind of polyether-ether-ketone composite material surface chemical plating according to claim 1 or 8, feature
It is, the metal of chemical plating is nickel, copper or silver in the step 6.
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