CN109652787B - Pretreatment process before surface chemical plating of polyether-ether-ketone composite material - Google Patents
Pretreatment process before surface chemical plating of polyether-ether-ketone composite material Download PDFInfo
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- CN109652787B CN109652787B CN201811567655.1A CN201811567655A CN109652787B CN 109652787 B CN109652787 B CN 109652787B CN 201811567655 A CN201811567655 A CN 201811567655A CN 109652787 B CN109652787 B CN 109652787B
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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
Abstract
The invention belongs to the technical field of surface modification and electroplating of special materials, and particularly relates to a pretreatment process before surface chemical plating of a polyether-ether-ketone composite material. The method comprises the following steps: stress removal, oil removal, pretreatment, etching, regulation and activation, and dispergation chemical plating. The invention solves the problems of lower bonding strength and lower product percent of pass in the prior art, and the metal plating layer after the pretreatment process before chemical plating has high bonding strength, is not easy to fall off, has high product percent of pass and is suitable for industrial application.
Description
Technical Field
The invention belongs to the technical field of surface modification and electroplating of special materials, and particularly relates to a pretreatment process before surface chemical plating of a polyether-ether-ketone composite material.
Background
Plastics are common articles of everyday life. At present, the market commonly shows that some plastic surfaces have decorative metal layers and are bright and smooth. The surface metallization of these plastics is typically done by physical vapor deposition techniques or chemical deposition techniques. However, it is difficult to metallize the surface of the anisotropic article by physical vapor deposition techniques.
Electroplating is mainly performed on the electric conductor, and more energy is consumed. The chemical plating process is simple, the production flow is convenient, and pre-treatment is required to be carried out between plastic macromolecules to activate the surfaces of the plastic macromolecules. For example: the common pretreatment process before chemical plating of ABS plastic is stress removal → surface degreasing → cleaning → coarsening → recovery → cleaning → reduction → cleaning → sensitization → cleaning → presoaking → colloidal palladium activation → recovery → cleaning → dispergation → cleaning → chemical plating.
The polyether-ether-ketone resin is a special aromatic linear thermoplastic resin with high crystallinity. It has the heat resistance and chemical stability of aromatic thermosetting resin and easy processing of thermoplastic resin, and has excellent comprehensive performance, and is produced through injection molding, extrusion molding, compression molding, blow molding and other steps. In order to meet the requirements of manufacturing high-precision, heat-resistant, corrosion-resistant, wear-resistant, fatigue-resistant and impact-resistant parts, the polyether-ether-ketone resin is subjected to enhancement modification treatment such as blending, filling and fiber compounding to obtain the polyether-ether-ketone resin composite material with more excellent performance. The polyether-ether-ketone is a special engineering plastic prepared by high-temperature polycondensation of difluorobenzophenone and aromatic dihydric phenol, and can also be prepared by polycondensation of aromatic dihalide and 4,4' -dihydroxy benzophenone, and has high thermal-oxidative stability. High mechanical property, belonging to special engineering plastics. The polyether-ether-ketone can be made into a reinforcing material or a composite material with glass fiber or carbon fiber, and can be applied to the fields of industries such as high-temperature resistant structural materials, wear-resistant materials, electric insulating materials and the like, petroleum and petrochemical, aerospace and the like. However, with the development of science and technology, the surface metallization of the polyetheretherketone is helpful for the functionalization of materials, and the functions of conductivity, corrosion resistance, decoration and the like are satisfied. The national invention patent application No. 201410814151.0 discloses a palladium-free chemical plating method for a polyetheretherketone and polyetheretherketone/carbon nanotube composite material. The pretreatment process mainly adopts concentrated sulfuric acid as a swelling agent to carry out surface swelling treatment, then adsorbs a reducing agent on the swelled surface, and then carries out chemical plating, so that a metal plating layer is deposited on the surface of the polyetheretherketone or polyetheretherketone/carbon nanotube composite material, and the plating layer has good binding force.
In the prior art, the surface chemical plating metal of the polyetheretherketone composite material has lower bonding strength and lower product percent of pass.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a pretreatment process before chemical plating of a surface of a polyetheretherketone composite material, solves the problems of low bonding strength and low product percent of pass in the prior art, and has the advantages of high bonding strength of a metal plating layer, difficult falling, high product percent of pass and suitability for industrial application after the pretreatment process before chemical plating.
The purpose of the invention is realized by the following technical scheme:
a pretreatment process before surface chemical plating of a polyetheretherketone composite material comprises the following steps:
step one, stress removal: washing the surface of the prepared polyether-ether-ketone composite material part for at least 2 times by using ethanol, then drying the part in an oven at the temperature of 40-80 ℃ for 2-10 h, and obtaining the polyether-ether-ketone composite material part for later use after drying;
step two, oil removal: putting the polyether-ether-ketone composite material part obtained in the step one into de-waxing water at the temperature of 50-80 ℃, and ultrasonically cleaning for 5-30 min to obtain a de-oiled polyether-ether-ketone composite material part for later use;
step three, pretreatment: washing the deoiled polyether-ether-ketone composite material part in the step two for at least 2 times, then soaking the part in a pretreatment solution at the temperature of 20-30 ℃ for at least 5min, taking out the part, washing the part for at least 2 times, and drying the part to obtain a pretreated polyether-ether-ketone composite material part for later use;
step four, etching: placing the polyether-ether-ketone composite material part pretreated in the third step into an etching solution for etching for 5-30 min to obtain an etched polyether-ether-ketone composite material part for later use;
step five, adjusting and activating: placing the polyether-ether-ketone composite material part etched in the fourth step into a regulating solution with the temperature of 30-50 ℃ for treatment for 10-30 min, and then placing the polyether-ether-ketone composite material part into colloidal palladium with the temperature of 20-30 ℃ for activation for at least 5min to obtain an activated polyether-ether-ketone composite material part for later use;
sixthly, dispergation chemical plating: and D, putting the activated polyether-ether-ketone composite material part in the step five into a strong alkali aqueous solution at the temperature of 20-45 ℃ for glue dissolving for 2-5 min, rinsing for 1-5 min, and finally chemically plating metal on the surface of the polyether-ether-ketone composite material part to metalize the surface of the polyether-ether-ketone composite material part.
After the surface of the polyetheretherketone composite material part is subjected to chemical plating and surface metallization, the bonding strength between the metal layer and the polyetheretherketone composite material part is increased, the bonding force between the metal layer and the polyetheretherketone composite material part is improved, the product yield is improved, and the surface metallization method is suitable for surface metallization of anisotropic parts.
The pretreatment process before surface chemical plating of the polyether-ether-ketone composite material has the advantages of simple flow, low cost, high efficiency, stable process and convenient construction, is suitable for industrial application, and has wide industrial application value; the reagent used for pretreatment has low cost and good effect.
The pretreatment process before the surface chemical plating of the polyetheretherketone composite material is to perform stress removal, oil removal, pretreatment, etching, adjustment activation and dispergation chemical plating, and the polyetheretherketone composite material workpiece after the stress removal, the oil removal, the pretreatment and the etching is easier to activate and the bonding force with the metal layer is enhanced, so that the metal layer formed by the chemical plating is firmer.
Further, the wax removing water in the second step consists of the following components in parts by weight: 20-30 parts of coconut oil diethanolamide, 5-8 parts of sodium alkyl benzene sulfonate, 10-15 parts of alkyl alkylamide phosphate, 3-5 parts of secondary alkyl sodium sulfonate, 3-5 parts of an anionic surfactant and 20-30 parts of water.
The preparation method of the wax removing water comprises the following steps: sequentially adding coconut oil diethanolamide, sodium alkyl benzene sulfonate, alkylolamide phosphate, secondary alkyl sodium sulfonate and an anionic surfactant into water according to the weight part ratio, and stirring and mixing for at least 30min at normal temperature to obtain the coconut oil diethanolamide.
Further, the pretreatment solution in the third step comprises the following components in parts by weight: 5-8 parts of sodium carbonate, 5-8 parts of sodium dihydrogen phosphate, 3-5 parts of sodium pyrophosphate, 2-3 parts of copper sulfate, 1-2 parts of nickel sulfate, 3-5 parts of tartaric acid and 900-1000 parts of water.
The preparation method of the pretreatment solution comprises the following steps: sequentially adding sodium carbonate, sodium dihydrogen phosphate, sodium pyrophosphate, copper sulfate, nickel sulfate and tartaric acid into water according to the weight part ratio, and stirring and mixing at normal temperature for at least 30min to obtain the sodium phosphate-nickel-tartrate composite material.
Further, in the third step, the drying temperature is 95-105 ℃, and the drying time is 1-2 hours.
Furthermore, the etching solution in the fourth step comprises the following components in parts by weight: 20-50 parts of sodium hydrofluoride, 500-800 parts of a sulfuric acid solution with the volume fraction of 20-30% and 2-3 parts of thiourea.
The preparation method of the etching solution comprises the following steps: and adding sodium hydrofluoride and thiourea into a sulfuric acid solution with the volume fraction of 20-30%, and stirring and mixing at normal temperature for at least 30min to obtain the sodium hydrofluoride-thiourea-containing aqueous solution.
Further, in the fifth step, the adjusting solution is a solution A, a solution B, a solution C and a solution D according to the ratio of 1: (0.6-0.7): (0.6-0.8): (1.0-1.2) uniformly mixing to obtain a regulating solution, wherein the solution A is a 0.5-100 mM hydrochloric acid solution, the solution B is a 0.01-30 mM copper sulfate solution, the solution C is a 20-30% sulfuric acid solution in volume fraction, and the solution D is a 2-10 g/L quaternary ammonium salt solution of a cationic surface active wetting agent.
Further, the preparation method of the colloidal palladium in the fifth step comprises the following steps: dissolving 10-200 parts by weight of stannous chloride in 100-500 parts by weight of a 30-35% hydrochloric acid solution under stirring, adding 2-10 parts by weight of sodium stannate, and stirring to obtain a milky white solution, which is marked as solution E; and then adding 0.5-3 parts by weight of palladium chloride into a mixed solution of 100-500 parts by weight of a hydrochloric acid solution with the mass fraction of 30-35% and 200-600 parts by weight of deionized water in another container, heating and dissolving completely, adding 0.5-5 parts by weight of stannous chloride at 25-40 ℃, stirring for 1-5 min to obtain a solution F, pouring the solution F into the solution E, adding 200-300 parts by weight of deionized water, and preserving heat for 4-6 h at 50-75 ℃ to obtain the colloidal palladium.
Further, the strong alkali aqueous solution in the sixth step is 180-220 mg/L sodium hydroxide aqueous solution.
Further, the metal chemically plated in the sixth step is nickel, copper or silver,
the invention has the beneficial effects that:
1. after the surface of the polyetheretherketone composite material part is subjected to chemical plating and surface metallization, the bonding strength between the metal layer and the polyetheretherketone composite material part is increased, the bonding force between the metal layer and the polyetheretherketone composite material part is improved, the product yield is improved, and the method is suitable for surface metallization of anisotropic parts;
2. the pretreatment process before surface chemical plating of the polyether-ether-ketone composite material has the advantages of simple flow, low cost, high efficiency, stable process and convenient construction, is suitable for industrial application, and has wide industrial application value; reagents used for pretreatment have low cost and good effect; the surface tension of the polyether-ether-ketone composite material workpiece treated by the pretreatment solution and the adjusting solution is higher, the workpiece is easier to activate, and the bonding force between the workpiece and the metal layer after activation is stronger;
3. the pretreatment process before the surface chemical plating of the polyetheretherketone composite material is to perform stress removal, oil removal, pretreatment, etching, adjustment activation and dispergation chemical plating, and the polyetheretherketone composite material workpiece after the stress removal, the oil removal, the pretreatment and the etching is easier to activate and the bonding force with the metal layer is enhanced, so that the metal layer formed by the chemical plating is firmer.
Drawings
FIG. 1 is a schematic structural diagram of a heterogeneous part of a PEEK composite part;
FIG. 2 is a schematic structural diagram of a PEEK composite product after chemical plating;
in the figure: 1-polyether-ether-ketone composite material part and 2-metal layer.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following.
Example 1
A pretreatment process before surface chemical plating of a polyetheretherketone composite material comprises the following steps:
step one, stress removal: washing the surface of the prepared polyether-ether-ketone composite material part for at least 2 times by using ethanol, then drying the part in an oven at the temperature of 40-80 ℃ for 2-10 h, and obtaining the polyether-ether-ketone composite material part for later use after drying;
step two, oil removal: putting the polyether-ether-ketone composite material part obtained in the step one into de-waxing water at the temperature of 50-80 ℃, and ultrasonically cleaning for 5-30 min to obtain a de-oiled polyether-ether-ketone composite material part for later use;
step three, pretreatment: washing the deoiled polyether-ether-ketone composite material part in the step two for at least 2 times, then soaking the part in a pretreatment solution at the temperature of 20-30 ℃ for at least 5min, taking out the part, washing the part for at least 2 times, and drying the part to obtain a pretreated polyether-ether-ketone composite material part for later use;
step four, etching: placing the polyether-ether-ketone composite material part pretreated in the third step into an etching solution for etching for 5-30 min to obtain an etched polyether-ether-ketone composite material part for later use;
step five, adjusting and activating: placing the polyether-ether-ketone composite material part etched in the fourth step into a regulating solution with the temperature of 30-50 ℃ for treatment for 10-30 min, and then placing the polyether-ether-ketone composite material part into colloidal palladium with the temperature of 20-30 ℃ for activation for at least 5min to obtain an activated polyether-ether-ketone composite material part for later use;
sixthly, dispergation chemical plating: and D, putting the activated polyether-ether-ketone composite material part in the step five into a strong alkali aqueous solution at the temperature of 20-45 ℃ for glue dissolving for 2-5 min, rinsing for 1-5 min, and finally chemically plating metal on the surface of the polyether-ether-ketone composite material part to metalize the surface of the polyether-ether-ketone composite material part.
Specifically, the wax removing water in the second step consists of the following components in parts by weight: 20-30 parts of coconut oil diethanolamide, 5-8 parts of sodium alkyl benzene sulfonate, 10-15 parts of alkyl alkylamide phosphate, 3-5 parts of secondary alkyl sodium sulfonate, 3-5 parts of an anionic surfactant and 20-30 parts of water.
Specifically, the pretreatment solution in the third step comprises the following components in parts by weight: 5-8 parts of sodium carbonate, 5-8 parts of sodium dihydrogen phosphate, 3-5 parts of sodium pyrophosphate, 2-3 parts of copper sulfate, 1-2 parts of nickel sulfate, 3-5 parts of tartaric acid and 900-1000 parts of water.
Specifically, in the third step, the drying temperature is 95-105 ℃, and the drying time is 1-2 hours.
Specifically, the etching solution in the fourth step comprises the following components in parts by weight: 20-50 parts of sodium hydrofluoride, 500-800 parts of a sulfuric acid solution with the volume fraction of 20-30% and 2-3 parts of thiourea.
Specifically, the adjusting solutions in the step five are solution A, solution B, solution C and solution D according to the ratio of 1: (0.6-0.7): (0.6-0.8): (1.0-1.2) uniformly mixing to obtain a regulating solution, wherein the solution A is a 0.5-100 mM hydrochloric acid solution, the solution B is a 0.01-30 mM copper sulfate solution, the solution C is a 20-30% sulfuric acid solution in volume fraction, and the solution D is a 2-10 g/L quaternary ammonium salt solution of a cationic surface active wetting agent.
Specifically, the preparation method of the colloidal palladium in the fifth step comprises the following steps: dissolving 10-200 parts by weight of stannous chloride in 100-500 parts by weight of a 30-35% hydrochloric acid solution under stirring, adding 2-10 parts by weight of sodium stannate, and stirring to obtain a milky white solution, which is marked as solution E; and then adding 0.5-3 parts by weight of palladium chloride into a mixed solution of 100-500 parts by weight of a hydrochloric acid solution with the mass fraction of 30-35% and 200-600 parts by weight of deionized water in another container, heating and dissolving completely, adding 0.5-5 parts by weight of stannous chloride at 25-40 ℃, stirring for 1-5 min to obtain a solution F, pouring the solution F into the solution E, adding 200-300 parts by weight of deionized water, and preserving heat for 4-6 h at 50-75 ℃ to obtain the colloidal palladium.
Specifically, the strong alkali aqueous solution in the sixth step is 180-220 mg/L sodium hydroxide aqueous solution.
Specifically, the metal electroless-plated in the sixth step is nickel, copper or silver.
Specific parameters of examples 1 to 6 are shown in table 1, examples 1 to 4 are technical parameters defined in the present invention, examples 5 were pretreated without using a pretreatment liquid, and examples 6 were treated without using a conditioning liquid, wherein examples 5 to 6 are comparative examples.
TABLE 1
Specific performance parameters of examples 1 to 6 are shown in table 2, examples 1 to 4 are technical parameters defined in the present invention, examples 5 were pretreated without using a pretreatment liquid, and examples 6 were treated without using a conditioning liquid, wherein examples 5 to 6 are comparative examples.
And (3) according to the method B in ASTM D3359-83, the binding force of the metal coating and the polyether-ether-ketone composite material part is measured by a grid scratch tape method: the test procedure was as follows: after the sample is processed as required, the sample is placed on a fixed base and then placed under a magnifying glass with a light source together with the base; respectively scribing 6 nicks in two vertical directions by using a blade to form 25 grids, wherein the nicks are 1mm in distance, the nicks are required to reach the base material, and slightly brushing loose film fragments by using a soft brush; then, cutting a pressure-sensitive adhesive tape with the length of 75mm, and completely covering the scored area, wherein the adhesive tape is required to be in full contact with and bonded with the coating, and no air bubble is left in the middle; after 90 + -30 s of retention, the tape is quickly and uniformly pulled off at 180 degrees in the opposite direction, and then the number and area of the films stuck off by the tape are checked under a magnifier.
The evaluation was made with reference to the following criteria. The binding force is classified into 6 grades, the grade 5B (the cut edge is smooth and has no square grid separation) is optimal, the grade 4B (the cut edge has small coating separation at the square grid intersection and has less than 5% of the area affected) is qualified, the grade 3B (the cut edge has small coating separation at the square grid intersection and has 5-15% of the area affected), the grade 2B (the cut edge has partial separation, the cut edge has large coating separation or partial whole grid separation at the square grid intersection and has 15-35% of the area affected), the grade 1B (the cut edge has large coating separation, some square grids have partial or whole separation and has 35-65% of the area affected), and the grade 0B (the cut edge has large coating separation at the square grid intersection and has more than 65% of the area affected).
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| Grade | 5B | 5B | 5B | 5B | 4B | 4B |
TABLE 2
As can be seen from the data in table 2, the grades of examples 1 to 4 are significantly better than the comparative examples, and the bonding strengths of examples 5 to 6 are lower than those of examples 1 to 4.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A pretreatment process before surface chemical plating of a polyetheretherketone composite material is characterized by comprising the following steps:
step one, stress removal: washing the surface of the prepared polyether-ether-ketone composite material part for at least 2 times by using ethanol, then drying the part in an oven at the temperature of 40-80 ℃ for 2-10 h, and obtaining the polyether-ether-ketone composite material part for later use after drying;
step two, oil removal: putting the polyether-ether-ketone composite material part obtained in the step one into de-waxing water at the temperature of 50-80 ℃, and ultrasonically cleaning for 5-30 min to obtain a de-oiled polyether-ether-ketone composite material part for later use;
step three, pretreatment: washing the deoiled polyether-ether-ketone composite material part in the step two for at least 2 times, then soaking the part in a pretreatment solution at the temperature of 20-30 ℃ for at least 5min, taking out the part, washing the part for at least 2 times, and drying the part to obtain a pretreated polyether-ether-ketone composite material part for later use; the pretreatment solution comprises the following components in parts by weight: 5-8 parts of sodium carbonate, 5-8 parts of sodium dihydrogen phosphate, 3-5 parts of sodium pyrophosphate, 2-3 parts of copper sulfate, 1-2 parts of nickel sulfate, 3-5 parts of tartaric acid and 900-1000 parts of water;
step four, etching: placing the polyether-ether-ketone composite material part pretreated in the third step into an etching solution for etching for 5-30 min to obtain an etched polyether-ether-ketone composite material part for later use;
step five, adjusting and activating: placing the polyether-ether-ketone composite material part etched in the fourth step into a regulating solution with the temperature of 30-50 ℃ for treatment for 10-30 min, and then placing the polyether-ether-ketone composite material part into colloidal palladium with the temperature of 20-30 ℃ for activation for at least 5min to obtain an activated polyether-ether-ketone composite material part for later use; the adjusting solution is a solution A, a solution B, a solution C and a solution D according to the volume ratio of 1: (0.6-0.7): (0.6-0.8): (1.0-1.2) uniformly mixing to obtain a regulating solution, wherein the solution A is a 0.5-100 mM hydrochloric acid solution, the solution B is a 0.01-30 mM copper sulfate solution, the solution C is a 20-30% sulfuric acid solution in volume fraction, and the solution D is a 2-10 g/L quaternary ammonium salt solution of a cationic surface active wetting agent;
sixthly, dispergation chemical plating: and D, putting the activated polyether-ether-ketone composite material part in the step five into a strong alkali aqueous solution at the temperature of 20-45 ℃ for glue dissolving for 2-5 min, rinsing for 1-5 min, and finally chemically plating metal on the surface of the polyether-ether-ketone composite material part to metalize the surface of the polyether-ether-ketone composite material part.
2. The pretreatment process before surface chemical plating of the polyetheretherketone composite material according to claim 1, wherein the drying temperature in the third step is 95-105 ℃ and the drying time is 1-2 h.
3. The pretreatment process before surface chemical plating of the polyetheretherketone composite material according to claim 1, wherein the etching solution in the fourth step comprises the following components in parts by weight: 20-50 parts of sodium hydrofluoride, 500-800 parts of a sulfuric acid solution with the volume fraction of 20-30% and 2-3 parts of thiourea.
4. The pretreatment process before surface chemical plating of the polyetheretherketone composite material according to claim 1, wherein the preparation method of the colloidal palladium in the fifth step comprises: dissolving 10-200 parts by weight of stannous chloride in 100-500 parts by weight of a 30-35% hydrochloric acid solution under stirring, adding 2-10 parts by weight of sodium stannate, and stirring to obtain a milky white solution, which is marked as solution E; and then adding 0.5-3 parts by weight of palladium chloride into a mixed solution of 100-500 parts by weight of a hydrochloric acid solution with the mass fraction of 30-35% and 200-600 parts by weight of deionized water in another container, heating and dissolving completely, adding 0.5-5 parts by weight of stannous chloride at 25-40 ℃, stirring for 1-5 min to obtain a solution F, pouring the solution F into the solution E, adding 200-300 parts by weight of deionized water, and preserving heat for 4-6 h at 50-75 ℃ to obtain the colloidal palladium.
5. The pretreatment process before surface chemical plating of the polyetheretherketone composite material according to claim 1, wherein the aqueous strong alkali solution in the sixth step is 180-220 mg/L aqueous sodium hydroxide solution.
6. The pretreatment process before chemical plating on the surface of the polyetheretherketone composite material according to claim 1 or 5, wherein the metal chemically plated in the sixth step is nickel, copper or silver.
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| CN112962126A (en) * | 2021-02-01 | 2021-06-15 | 宁波劳伦斯表面技术有限公司 | Alkaline double-color electroplating debonder and preparation process thereof |
| CN113186522B (en) * | 2021-05-26 | 2022-01-28 | 西南科技大学 | Tin salt sensitization activation method for titanium alloy surface chemical plating |
| CN113913800B (en) * | 2021-11-12 | 2024-03-26 | 中航光电科技股份有限公司 | Electroplating pretreatment process for carbon fiber reinforced polyether-ether-ketone composite material |
| CN114107985A (en) * | 2021-11-12 | 2022-03-01 | 中航光电科技股份有限公司 | Plating process of marine environment resistant composite material plating layer |
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