CN111748806A - Roughening liquid for polyphenylene sulfide and composite material thereof, preparation method and use method thereof - Google Patents
Roughening liquid for polyphenylene sulfide and composite material thereof, preparation method and use method thereof Download PDFInfo
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- CN111748806A CN111748806A CN202010705472.2A CN202010705472A CN111748806A CN 111748806 A CN111748806 A CN 111748806A CN 202010705472 A CN202010705472 A CN 202010705472A CN 111748806 A CN111748806 A CN 111748806A
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- roughening
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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
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
- C25D5/56—Electroplating of non-metallic surfaces of plastics
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- ing And Chemical Polishing (AREA)
- Chemically Coating (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a roughening liquid for polyphenylene sulfide and a composite material thereof, which comprises the following components in parts by weight: 10-100ml/L hydrofluoric acid, 10-300ml/L sulfuric acid, 10-100ml/L nitric acid, 0.1-5g/L sodium chloride, 1-30g/L ferric nitrate nonahydrate, and the balance of water. The coarsening liquid adopts a chemical coarsening mode, can permeate into the small holes and the grooves, and can realize uniform microcosmic coarsening even aiming at the base material with a complex structure.
Description
Technical Field
The invention relates to the technical field of electroplating pretreatment of plastic products, in particular to a roughening liquid for polyphenylene sulfide and a composite material thereof, and a preparation method and a use method thereof.
Background
Compared with the 3G/4G era, the 5G era with high frequency and high speed has higher requirements and challenges on a plurality of related devices and materials, and the antenna element is one of the devices and the materials. As an important component inside the 5G base station, the number of antenna elements increases sharply, and excellent performance is required to meet the requirement of 5G communication transmission. Compared with the traditional metal antenna oscillator, the 3D plastic antenna oscillator has great advantages in the aspects of loss, cost, weight and the like, and has already obtained the authentication of a base station terminal client. In the following 5G base station construction scheme, the 3D plastic antenna oscillator can comprehensively replace the traditional metal antenna, and the use amount and the output value can meet a peak period.
Polyphenylene sulfide (PPS for short) has good high resistivity and low dielectric constant, and its electric insulation property is less changed with temperature, and can retain good electric insulation property even under the condition of high-temp. And secondly, the PPS has excellent chemical stability, can resist various acid and alkali corrosion, and has corrosion resistance close to that of Polytetrafluoroethylene (PTFE). The excellent comprehensive performance of the PPS makes the PPS the first choice of the mainstream high-frequency communication material at present, and for example, the antenna element adopts the scheme greatly at present.
It is known that the larger the specific surface area, the larger the roughness and the better the bonding force. If the surface of the plastic is required to have a desired roughness, the surface of the material must be roughened. For example, chromic acid is adopted for roughening ABS plastic electroplating, and some polycarbonate common plastics and the like can be subjected to bite roughening by using strong alkali. However, polyphenylene sulfide has excellent corrosion resistance, and therefore, roughening of the surface is difficult. Patent CN109640539A mentions that the roughening method is physical sand blasting, but the roughening method can only roughen the surface of a flat or simpler structure material, and the grain size of the sand is large, so that micro-roughening cannot be achieved, and the bonding force with the surface coating is not ideal.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a roughening solution for polyphenylene sulfide and composite materials thereof, wherein the roughening solution adopts a chemical roughening mode, can permeate into pores and grooves, and can realize uniform micro-roughening even aiming at a base material with a complex structure. In addition, the invention also provides a preparation method and a use method of the roughening liquid for the polyphenylene sulfide and the composite material thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, a roughening solution for polyphenylene sulfide and composite materials thereof is provided, wherein the roughening solution comprises the following components in amounts: 10-100ml/L hydrofluoric acid, 10-300ml/L sulfuric acid, 10-100ml/L nitric acid, 0.1-5g/L sodium chloride, 1-30g/L ferric nitrate nonahydrate, and the balance of water.
Wherein, the coarsening liquid comprises the following components in parts by weight: 30-80ml/L hydrofluoric acid, 50-200ml/L sulfuric acid, 30-100ml/L nitric acid, 0.5-2g/L sodium chloride, 5-20g/L ferric nitrate nonahydrate, and the balance of water.
Wherein the mass concentration of the hydrofluoric acid is 55%, the mass concentration of the sulfuric acid is 98%, and the mass concentration of the nitric acid is 68%.
In a second aspect of the present invention, a preparation method of the above roughening solution for polyphenylene sulfide and composite material thereof is provided, wherein hydrofluoric acid, sulfuric acid, nitric acid, sodium chloride and ferric nitrate nonahydrate are sequentially dissolved in water according to a certain proportion to form an aqueous solution.
Adding sulfuric acid into water, cooling to room temperature, adding hydrofluoric acid and nitric acid into the sulfuric acid aqueous solution according to the steps, adding sodium chloride and ferric nitrate nonahydrate, and mixing uniformly to obtain the coarsening liquid.
In a third aspect of the present invention, a method for using the above roughening solution for polyphenylene sulfide and composite material thereof is provided, which comprises placing a workpiece made of polyphenylene sulfide material or composite material thereof into the roughening solution to perform chemical immersion type roughening.
Wherein, when the coarsening liquid is used, the coarsening time is 5-30 min.
Wherein, when the coarsening liquid is used, the coarsening temperature is 20-40 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention compounds three strong acids (hydrofluoric acid, sulfuric acid and nitric acid) with strong oxidizing property and strong corrosivity to form a solution with strong oxidizing property, which can carry out corrosion coarsening on fillers such as polyphenylene sulfide, glass fiber and the like, can swell a high molecular chain segment and further carry out corrosion, improves the specific surface area of a base material, can further improve the oxidation corrosion capability of the coarsening solution by adding ferric nitrate nonahydrate, and further accelerates the corrosion speed of the coarsening solution on the base material by adding sodium chloride salt substances.
Compared with the traditional physical roughening, the roughening solution disclosed by the invention can permeate into small holes and grooves on the base material, even the base material with a complex structure can realize uniform micro roughening, the chemical roughening greatly improves the direct bonding force of the coating and the base material, and the roughening solution can be applied to the metallization requirements of polyphenylene sulfide and composite materials thereof, such as chemical plating, electroplating or magnetron sputtering.
Detailed Description
Example 1
The roughening solution in this example comprises 30ml/L hydrofluoric acid (55 wt%), 200ml/L sulfuric acid (98 wt%), 40ml/L nitric acid (68 wt%), 1g/L sodium chloride, 7g/L ferric nitrate nonahydrate, and the balance water.
The preparation process of the roughening solution is as follows:
adding sulfuric acid into water, cooling to room temperature, adding hydrofluoric acid into the sulfuric acid aqueous solution, cooling to room temperature, adding nitric acid, adding sodium chloride and ferric nitrate nonahydrate, and mixing to obtain the roughening solution.
Example 2
The roughening solution in this example comprises 100ml/L hydrofluoric acid (55 wt%), 10ml/L sulfuric acid (98 wt%), 100ml/L nitric acid (68 wt%), 1.5g/L sodium chloride, 15g/L ferric nitrate nonahydrate, and the balance water.
The preparation process of the roughening solution in this example was the same as in example 1.
Example 3
The roughening solution in this example comprises 60ml/L hydrofluoric acid (55 wt%), 90ml/L sulfuric acid (98 wt%), 70ml/L nitric acid (68 wt%), 2g/L sodium chloride, 30g/L ferric nitrate nonahydrate, and the balance water.
The preparation process of the roughening solution in this example was the same as in example 1.
Example 4
The roughening solution in this example comprises 35ml/L hydrofluoric acid (55 wt%), 300ml/L sulfuric acid (98 wt%), 10ml/L nitric acid (68 wt%), 0.1g/L sodium chloride, 1g/L ferric nitrate nonahydrate, and the balance water.
The preparation process of the roughening solution in this example was the same as in example 1.
Example 5
The roughening solution in this example comprises 70ml/L hydrofluoric acid (55 wt%), 170ml/L sulfuric acid (98 wt%), 30ml/L nitric acid (68 wt%), 0.5g/L sodium chloride, 5g/L ferric nitrate nonahydrate, and the balance water.
The preparation process of the roughening solution in this example was the same as in example 1.
Example 6
The roughening solution in this example comprises 80ml/L hydrofluoric acid (55 wt%), 50ml/L sulfuric acid (98 wt%), 50ml/L nitric acid (68 wt%), 5g/L sodium chloride, 20g/L ferric nitrate nonahydrate, and the balance water.
The preparation process of the roughening solution in this example was the same as in example 1.
Comparative example 1
Comparative example 1 is a comparative example of example 4, in comparative example 1, hydrofluoric acid was not added, and the contents of the remaining components and the preparation method were the same as those of example 4.
Comparative example 2
Comparative example 2 is a comparative example of example 4, in comparative example 2, nitric acid was not added, and the contents of the remaining components and the preparation method were the same as those of example 4.
The roughening liquid prepared in the examples 1 to 6, the comparative examples 1 and the comparative examples 2 is subjected to a roughening capability test, a workpiece made of polyphenylene sulfide or a composite material thereof is completely immersed into the roughening liquid to be roughened in a chemical immersion manner, the temperature is controlled to be 20-40 ℃, the roughening time is 5-30min, the subsequent process electroplating is carried out after the workpiece is roughened, the binding force of the workpiece is tested by a one-grid test at intervals of 1mm, and the binding force condition of a plating layer and a substrate is observed to judge the roughening effect of the roughening liquid.
The specific test process is as follows:
(1) soaking a workpiece made of polyphenylene sulfide or a composite material thereof into deoiling liquid at 50 ℃, soaking for 3min, taking out and washing with water;
(2) transferring the cleaned workpiece into a roughening solution with the temperature of 20-40 ℃ for soaking for 5-30min, taking out and then washing with water;
(3) and then, carrying out subsequent electroplating treatment on the surface of the workpiece, wherein a conventional electroplating process flow is selected, and the electroplating process flow in the performance test is as follows: the work piece after the roughening treatment → presoaking (hydrochloric acid 20%, 1min, room temperature) → palladium water activation (3min, 30 ℃) → dispergation (2min, 50 ℃) → chemical nickel (3min, 30 ℃.) → copper acid (60min, 20-25 ℃, thickness 8 μm) → etching (3min, room temperature) → electrolytic tin plating (30min, 30 ℃, thickness 8 μm).
And (3) carrying out a check test at the interval of 1mm after the electroplating process is finished, detecting the specific test process according to ASTM D3002D3359 and DIN EN ISO 2409, observing the binding force condition of the plating layer and the matrix, and judging the roughening effect of the roughening solution.
And (4) judging a result:
grade: 5B, the edges of the cuts are completely smooth, and the edges of the grids are not peeled off;
grade: 4B, small pieces are peeled off at the intersection of the notches, and the actual damaged part in the grid cutting area exceeds 5 percent;
grade: 3B, the edges or the intersections of the cuts are stripped, and the area of the cuts is more than 5 percent but less than 15 percent;
grade: 2B, partial peeling or whole peeling at the edge of the cut, and/or partial cells are peeled by whole pieces, and the peeled area is more than 15 percent but less than 35 percent;
grade: 1B, the edges of the cuts are largely exfoliated and/or some or all of the cells are exfoliated, with an area greater than 35% but not more than 65% of the cross-hatched area.
TABLE 1 test results of binding force after coarsening
As shown in the test results in Table 1, the roughening solutions prepared in examples 1 to 6, compared with the roughening solutions prepared in comparative examples 1 and 2, achieve uniform micro-roughening on the surface of the substrate, and greatly improve the direct bonding force between the plating layer and the substrate.
Therefore, the solution with strong oxidizing property is formed by compounding three strong acids (hydrofluoric acid, sulfuric acid and nitric acid) with strong oxidizing property and strong corrosivity, the solution can be used for roughening the biting of fillers such as polyphenylene sulfide, glass fiber and the like, and can swell and further bite a high molecular chain segment, the specific surface area of the base material is improved, the oxidative corrosion capability of the roughening solution can be further improved by adding the ferric nitrate nonahydrate, and the corrosion speed of the roughening solution on the base material is further accelerated by adding sodium chloride salt substances; compared with the traditional physical coarsening, the coarsening liquid can permeate into small holes and grooves on the substrate, even if the substrate with a complex structure can also realize uniform microcosmic coarsening, and the chemical coarsening greatly improves the direct binding force of the plating layer and the substrate.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (8)
1. The roughening liquid for the polyphenylene sulfide and the composite material thereof is characterized by comprising the following components in parts by weight: 10-100ml/L hydrofluoric acid, 10-300ml/L sulfuric acid, 10-100ml/L nitric acid, 0.1-5g/L sodium chloride, 1-30g/L ferric nitrate nonahydrate, and the balance of water.
2. The roughening solution for polyphenylene sulfide and composite material thereof according to claim 1, wherein said roughening solution comprises the following components in amounts: 30-80ml/L hydrofluoric acid, 50-200ml/L sulfuric acid, 30-100ml/L nitric acid, 0.5-2g/L sodium chloride, 5-20g/L ferric nitrate nonahydrate, and the balance of water.
3. The roughening solution for polyphenylene sulfide and composite material thereof according to claim 1 or 2, wherein a mass concentration of said hydrofluoric acid is 55%, a mass concentration of said sulfuric acid is 98%, and a mass concentration of said nitric acid is 68%.
4. The method for preparing a roughening solution for polyphenylene sulfide and composite material thereof according to claim 1, wherein hydrofluoric acid, sulfuric acid, nitric acid, sodium chloride and ferric nitrate nonahydrate are sequentially dissolved in water in proportion to form an aqueous solution.
5. The method for preparing the roughening solution for polyphenylene sulfide and composite material thereof according to claim 4, wherein sulfuric acid is added into water, after the temperature is reduced to room temperature, hydrofluoric acid and nitric acid are added into the sulfuric acid aqueous solution according to the above steps, and finally sodium chloride and ferric nitrate nonahydrate are added and mixed uniformly to obtain the roughening solution.
6. The method for using the roughening solution for polyphenylene sulfide and composite material thereof according to claim 1, wherein the method comprises the step of placing a workpiece made of polyphenylene sulfide material or composite material thereof into the roughening solution for chemical immersion roughening.
7. The method as claimed in claim 6, wherein the roughening time is 5-30 min.
8. The method as claimed in claim 6, wherein the roughening temperature is 20-40 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (1)
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| CN111910231A (en) * | 2020-07-22 | 2020-11-10 | 东莞市百镀通五金电镀实业有限公司 | Roughening liquid for roughening glass fiber reinforced plastic and roughening method |
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| CN111748806B (en) | 2022-08-23 |
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