CN113957421A - PET (polyethylene terephthalate) surface roughening liquid and preparation method thereof - Google Patents
PET (polyethylene terephthalate) surface roughening liquid and preparation method thereof Download PDFInfo
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- CN113957421A CN113957421A CN202111225262.4A CN202111225262A CN113957421A CN 113957421 A CN113957421 A CN 113957421A CN 202111225262 A CN202111225262 A CN 202111225262A CN 113957421 A CN113957421 A CN 113957421A
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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
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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
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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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Abstract
The invention provides PET surface roughening liquid which is prepared from the following components: 30-35 g/L of potassium permanganate, 20-25 g/L of sodium hydroxide, 2-4 g/L of 4-methylimidazole, 5-6 g/L of tetramethyl fluorourea hexafluorophosphate, 3-4 g/L of an auxiliary agent and the balance of water. The invention also provides a preparation method of the PET surface roughening liquid. The PET surface roughening liquid provided by the invention has a good roughening effect.
Description
Technical Field
The invention relates to a roughening liquid, in particular to a PET (polyethylene terephthalate) surface roughening liquid and a preparation method thereof.
Background
The plastic electroplating generally adopts the following process methods: the method comprises the following steps of degreasing, coarsening, sensitizing, activating, chemically depositing nickel (or copper), wherein coarsening is an important link, the coarsening directly affects the binding force and brightness of a plating layer and the integrity of the plating layer, and the coarsening can enable the surface of a plated part to have hydrophilicity and form proper roughness or enable the surface to form a micropore shape, so that the adsorption of colloidal palladium and the good adhesive force of the plating layer are ensured.
At present, most of roughening solution used for plastics is mixed solution containing chromic anhydride, and although the roughening solution containing the chromic anhydride formula can obtain good roughening effect on the surfaces of ABS and PC, high-temperature heating is needed in the using process, great harm is brought to the environment and operators, and the roughening effect is not good when the roughening solution is applied to the surface of PET.
The PET is named as polyethylene terephthalate and is prepared by exchanging dimethyl terephthalate with ethylene glycol or esterifying terephthalic acid with ethylene glycol to synthesize dihydroxy ethyl terephthalate, and then performing polycondensation reaction. The surface of the PET is smooth, the hydrophobicity is strong, the improvement effect of the existing roughening liquid containing the chromic anhydride formula on the roughness of the surface of the PET is not strong, and the formed pits are not too many, so that the roughening effect is poor.
Chinese patent application CN201610507429.9 discloses a roughening solution for special engineering plastics, wherein each liter of roughening solution for special engineering plastics comprises the following components: 250g/L NaPS 150, 15-80g/L benzene, 30-60g/L tetrahydrofuran and 40-100ml/L sulfuric acid. Although the components of the roughening solution do not contain chromic acid, the environment pollution is less, but the roughening effect is poor when the roughening solution is applied to the surface of PET.
Disclosure of Invention
The invention aims to provide PET surface roughening liquid with a good roughening effect.
In order to solve the technical problems, the technical scheme of the invention is as follows:
PET surface roughening liquid is prepared from the following components: 30-35 g/L of potassium permanganate, 20-25 g/L of sodium hydroxide, 2-4 g/L of 4-methylimidazole, 5-6 g/L of tetramethyl fluorourea hexafluorophosphate, 3-4 g/L of an auxiliary agent and the balance of water.
Further, the invention is prepared from the following components: 32g/L of potassium permanganate, 21g/L of sodium hydroxide, 3g/L of 4-methylimidazole, 5.5g/L of tetramethyl fluorourea hexafluorophosphate, 3.5g/L of an auxiliary agent and the balance of water.
Furthermore, the auxiliary agent is N, N-dimethylformamide.
Further, the water is deionized water.
The invention also provides a preparation method of the PET surface roughening liquid.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of PET surface roughening liquid comprises the following steps:
s1, adding potassium permanganate into water with the weight being 20 times that of the potassium permanganate, and stirring for 10-20 minutes to obtain a solution A;
s2, adding sodium hydroxide into water with the weight being 20 times that of the sodium hydroxide, and stirring for 10-20 minutes to obtain a solution B
S3, adding 4-methylimidazole, tetramethyl fluorourea hexafluorophosphate and an auxiliary agent into the rest water, and stirring until the mixture is uniformly mixed to obtain a solution C;
and S4, mixing the solution A obtained in the step S1, the solution B obtained in the step S2 and the solution C obtained in the step S3, and stirring for 20-30 minutes to obtain the PET surface roughening solution.
Further, in step S3 of the present invention, the assistant is N, N-dimethylformamide.
Further, in the steps S1, S2, and S3 of the present invention, the water is deionized water.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention mainly comprises potassium permanganate, sodium hydroxide, 4-methylimidazole, tetramethyl fluoro urea hexafluorophosphate, an auxiliary agent N, N-dimethylformamide and the like, wherein the auxiliary agent N, N-dimethylformamide has a swelling effect on the surface of PET; potassium permanganate can perform the oxidation corrosion effect on the surface of the PET in an alkaline environment, so that the roughness of the surface of the PET is improved; the 4-methylimidazole can strengthen the oxidation corrosion performance of potassium permanganate, thereby further improving the roughness of the surface of the PET and the binding force between the PET and a plating layer, and simultaneously reducing the use amount of potassium permanganate and sodium hydroxide and reducing the pollution to the environment.
2) The tetramethyl thiourea hexafluorophosphate used in the invention can effectively accelerate the hydrolysis process of ester bonds in PET surface molecules, the ester bonds are hydrolyzed to obtain hydroxyl groups, pits are generated on the PET surface, the roughness is further increased, meanwhile, the hydroxyl groups generated by the ester bond hydrolysis can also effectively improve the hydrophilicity of the PET surface, so that the binding force between PET and a plating layer is further improved, and in addition, the tetramethyl thiourea hexafluorophosphate can also effectively reduce the grain size of the plating layer, so that the compactness of the plating layer is improved.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, and the exemplary embodiments and descriptions thereof herein are provided to explain the present invention but not to limit the present invention.
Example 1
The PET surface roughening liquid is prepared from the following components: 32g/L of potassium permanganate, 21g/L of sodium hydroxide, 3g/L of 4-methylimidazole, 5.5g/L of tetramethyl fluorourea hexafluorophosphate, 3.5g/L of N, N-dimethylformamide and the balance of deionized water.
The preparation method of the PET surface roughening liquid comprises the following steps:
s1, adding potassium permanganate into deionized water with the weight being 20 times that of the potassium permanganate, and stirring for 15 minutes to obtain a solution A;
s2, adding sodium hydroxide into deionized water with the weight being 20 times that of the sodium hydroxide, and stirring for 15 minutes to obtain a solution B
S3, adding 4-methylimidazole, tetramethyl fluoro urea hexafluorophosphate and N, N-dimethylformamide into the rest deionized water, and stirring until the mixture is uniformly mixed to obtain a solution C;
and S4, mixing the solution A obtained in the step S1, the solution B obtained in the step S2 and the solution C obtained in the step S3, and stirring for 25 minutes to obtain the PET surface roughening solution.
Example 2
The PET surface roughening liquid is prepared from the following components: 33g/L of potassium permanganate, 22g/L of sodium hydroxide, 4g/L of 4-methylimidazole, 5g/L of tetramethyl fluorourea hexafluorophosphate, 3.3g/L of N, N-dimethylformamide and the balance of deionized water.
The preparation method of the PET surface roughening liquid comprises the following steps:
s1, adding potassium permanganate into deionized water with the weight being 20 times that of the potassium permanganate, and stirring for 18 minutes to obtain a solution A;
s2, adding sodium hydroxide into deionized water with the weight being 20 times that of the sodium hydroxide, and stirring for 12 minutes to obtain a solution B
S3, adding 4-methylimidazole, tetramethyl fluoro urea hexafluorophosphate and N, N-dimethylformamide into the rest deionized water, and stirring until the mixture is uniformly mixed to obtain a solution C;
and S4, mixing the solution A obtained in the step S1, the solution B obtained in the step S2 and the solution C obtained in the step S3, and stirring for 30 minutes to obtain the PET surface roughening solution.
Example 3
The PET surface roughening liquid is prepared from the following components: 30g/L of potassium permanganate, 25g/L of sodium hydroxide, 2g/L of 4-methylimidazole, 6g/L of tetramethyl fluoro urea hexafluorophosphate, 3g/L of N, N-dimethylformamide and the balance of deionized water.
The preparation method of the PET surface roughening liquid comprises the following steps:
s1, adding potassium permanganate into deionized water with the weight being 20 times that of the potassium permanganate, and stirring for 10 minutes to obtain a solution A;
s2, adding sodium hydroxide into deionized water with the weight being 20 times that of the sodium hydroxide, and stirring for 20 minutes to obtain a solution B
S3, adding 4-methylimidazole, tetramethyl fluoro urea hexafluorophosphate and N, N-dimethylformamide into the rest deionized water, and stirring until the mixture is uniformly mixed to obtain a solution C;
and S4, mixing the solution A obtained in the step S1, the solution B obtained in the step S2 and the solution C obtained in the step S3, and stirring for 20 minutes to obtain the PET surface roughening solution.
Example 4
The PET surface roughening liquid is prepared from the following components: 35g/L of potassium permanganate, 20g/L of sodium hydroxide, 2.5g/L of 4-methylimidazole, 5.7g/L of tetramethyl fluorourea hexafluorophosphate, 4g/L of N, N-dimethylformamide and the balance of deionized water.
The preparation method of the PET surface roughening liquid comprises the following steps:
s1, adding potassium permanganate into deionized water with the weight being 20 times that of the potassium permanganate, and stirring for 20 minutes to obtain a solution A;
s2, adding sodium hydroxide into deionized water with the weight being 20 times that of the sodium hydroxide, and stirring for 10 minutes to obtain a solution B
S3, adding 4-methylimidazole, tetramethyl fluoro urea hexafluorophosphate and N, N-dimethylformamide into the rest deionized water, and stirring until the mixture is uniformly mixed to obtain a solution C;
and S4, mixing the solution A obtained in the step S1, the solution B obtained in the step S2 and the solution C obtained in the step S3, and stirring for 28 minutes to obtain the PET surface roughening solution.
Reference example 1:
the difference from example 1 is that: the 4-methylimidazole is absent from the component.
Reference example 2:
the difference from example 1 is that: the component lacks tetramethyl fluoro urea hexafluorophosphate.
Comparative example: example 1 of chinese patent application No. CN 201610507429.9.
Test example 1: roughness measurement
The PET copper plating process: cutting a PET plate into a test piece of 4cm multiplied by 4cm for horizontal copper deposition, and the steps are as follows: placing the test piece in a sodium hydroxide solution with the mass concentration of 20% to remove oil for 5 minutes at 50 ℃, taking out and washing with water; the test piece was roughened in a surface-roughening solution (surface-roughening solution prepared in examples 1 to 4, reference examples 1 to 2, comparative examples) at 50 ℃ for 10 minutes, and then taken out and washed with water; sensitizing the test piece in sensitizing solution (15g/L stannous chloride and 20ml/L hydrochloric acid) at 50 ℃ for 3 minutes, activating in activating solution (0.25g/L palladium chloride and 20ml/L hydrochloric acid) at 40 ℃ for 5 minutes, taking out and washing with water; the test piece was plated in a chemical copper plating solution (10 g/L copper sulfate, 25g/L sodium hypophosphite, 33g/L EDTA, 20g/L potassium sodium tartrate, pH 11) at 50 ℃ for 30 minutes.
The test pieces corresponding to examples 1 to 4, reference examples 1 to 2, and comparative examples were each tested for surface roughness after roughening using an atomic force microscope, and the test results are shown in table 1:
TABLE 1
As can be seen from Table 1, the surface roughness of the PET surface roughening solutions of examples 1-4 of the invention is higher than that of the comparative examples, which shows that the PET surface roughening solutions prepared by the invention have good effect of improving the PET surface roughness. The partial compositions of reference examples 1 and 2 are different from example 1, and the surface roughness of reference examples 1 and 2 is reduced compared with example 1, which shows that 4-methylimidazole and tetramethyl fluorourea hexafluorophosphate used in the invention can effectively improve the roughness of the PET surface.
Test example 2: plating adhesion test
The test pieces corresponding to examples 1 to 4, reference examples 1 to 2 and comparative example were tested for plating adhesion after electroless copper plating by reference to the ASTM D3330 standard peel test method, and the test results are shown in table 2:
TABLE 2
| Coating binding force (N/cm) | |
| Example 1 | 15.9 |
| Example 2 | 15.5 |
| Example 3 | 15.8 |
| Example 4 | 15.6 |
| Reference example 1 | 13.4 |
| Reference example 2 | 14.1 |
| Comparative example | 11.7 |
As can be seen from Table 2, the coating binding force of the PET surface roughening solution prepared by the invention in the examples 1-4 is higher than that of the comparative example, which shows that the PET surface roughening solution prepared by the invention has a good effect of improving the binding force between PET and the coating. Compared with the example 1, the plating bonding force of the reference examples 1 and 2 is reduced, which shows that the 4-methylimidazole and tetramethyl fluorourea hexafluorophosphate used in the invention can effectively improve the bonding force between PET and the plating.
Test example 3: grain size testing of coatings
The crystal structure characterization of the plating layer after electroless copper plating of the test pieces corresponding to examples 1 to 4, reference example 2 and comparative example was respectively tested by using an X-ray diffractometer, and the crystal grain size was calculated by the Scherrer formula, and the test results are shown in table 3:
TABLE 3
| Grain size (nm) | |
| Example 1 | 13.6 |
| Example 2 | 13.9 |
| Example 3 | 14.2 |
| Example 4 | 13.8 |
| Reference example 2 | 15.7 |
| Comparative example | 17.5 |
As can be seen from Table 3, the grain sizes of inventive examples 1 to 4 were all lower than those of comparative examples, indicating that the grain size reduction effect of the coating layer formed of PET using the PET surface-roughening solution prepared according to the present invention was good. The partial composition of reference example 2 is different from that of example 1, and the grain size of reference example 2 is not increased much as compared with example 1, indicating that the tetramethylfluorourea hexafluorophosphate used in the present invention is effective in reducing the grain size of the plated layer.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (7)
1. The PET surface roughening liquid is characterized in that: the composition is prepared from the following components: 30-35 g/L of potassium permanganate, 20-25 g/L of sodium hydroxide, 2-4 g/L of 4-methylimidazole, 5-6 g/L of tetramethyl fluorourea hexafluorophosphate, 3-4 g/L of an auxiliary agent and the balance of water.
2. The PET surface roughening liquid according to claim 1, wherein: the composition is prepared from the following components: 32g/L of potassium permanganate, 21g/L of sodium hydroxide, 3g/L of 4-methylimidazole, 5.5g/L of tetramethyl fluorourea hexafluorophosphate, 3.5g/L of an auxiliary agent and the balance of water.
3. The PET surface roughening liquid according to claim 1, wherein: the auxiliary agent is N, N-dimethylformamide.
4. The PET surface roughening liquid according to claim 1, wherein: the water is deionized water.
5. The method for preparing the PET surface roughening liquid according to any one of claims 1 to 4, wherein the method comprises the following steps: the method comprises the following steps:
s1, adding potassium permanganate into water with the weight being 20 times that of the potassium permanganate, and stirring for 10-20 minutes to obtain a solution A;
s2, adding sodium hydroxide into water with the weight being 20 times that of the sodium hydroxide, and stirring for 10-20 minutes to obtain a solution B
S3, adding 4-methylimidazole, tetramethyl fluorourea hexafluorophosphate and an auxiliary agent into the rest water, and stirring until the mixture is uniformly mixed to obtain a solution C;
and S4, mixing the solution A obtained in the step S1, the solution B obtained in the step S2 and the solution C obtained in the step S3, and stirring for 20-30 minutes to obtain the PET surface roughening solution.
6. The method for preparing the PET surface roughening liquid according to claim 5, wherein the method comprises the following steps: in the step S3, the auxiliary is N, N-dimethylformamide.
7. The method for preparing the PET surface roughening liquid according to claim 5, wherein the method comprises the following steps: in the steps S1, S2, and S3, the water is deionized water.
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| CN202111225262.4A CN113957421B (en) | 2021-10-21 | 2021-10-21 | PET surface roughening liquid and preparation method thereof |
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| CN202111225262.4A CN113957421B (en) | 2021-10-21 | 2021-10-21 | PET surface roughening liquid and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0139090A1 (en) * | 1983-08-05 | 1985-05-02 | Schering Aktiengesellschaft | Process for the pre-treatment of polyimides |
| JP2000265028A (en) * | 1999-03-15 | 2000-09-26 | Ibiden Co Ltd | Resin composition for forming roughened surface and printed wiring board |
| CN101928937A (en) * | 2009-06-22 | 2010-12-29 | 比亚迪股份有限公司 | Colloid palladium activation solution, preparation method thereof and non-metal surface activation method |
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- 2021-10-21 CN CN202111225262.4A patent/CN113957421B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0139090A1 (en) * | 1983-08-05 | 1985-05-02 | Schering Aktiengesellschaft | Process for the pre-treatment of polyimides |
| JP2000265028A (en) * | 1999-03-15 | 2000-09-26 | Ibiden Co Ltd | Resin composition for forming roughened surface and printed wiring board |
| CN101928937A (en) * | 2009-06-22 | 2010-12-29 | 比亚迪股份有限公司 | Colloid palladium activation solution, preparation method thereof and non-metal surface activation method |
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