CN109957128B - Organic film surface roughening agent, preparation method and roughening method thereof - Google Patents

Organic film surface roughening agent, preparation method and roughening method thereof Download PDF

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CN109957128B
CN109957128B CN201711401530.7A CN201711401530A CN109957128B CN 109957128 B CN109957128 B CN 109957128B CN 201711401530 A CN201711401530 A CN 201711401530A CN 109957128 B CN109957128 B CN 109957128B
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organic film
film layer
parts
agent
surface roughening
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CN109957128A (en
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赵长涛
罗富华
王继厚
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Huizhou BYD Electronic Co Ltd
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Huizhou BYD Electronic Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
    • C09D101/08—Cellulose derivatives
    • C09D101/26—Cellulose ethers
    • C09D101/28—Alkyl ethers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
    • C09D101/08—Cellulose derivatives
    • C09D101/26—Cellulose ethers
    • C09D101/28—Alkyl ethers
    • C09D101/286—Alkyl ethers substituted with acid radicals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D171/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D191/00—Coating compositions based on oils, fats or waxes; Coating compositions based on derivatives thereof
    • C09D191/06—Waxes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2300/00—Characterised by the use of unspecified polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/08—Cellulose derivatives
    • C08J2401/26—Cellulose ethers
    • C08J2401/28—Alkyl ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2471/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2491/00—Characterised by the use of oils, fats or waxes; Derivatives thereof
    • C08J2491/06—Waxes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Abstract

The invention discloses an organic film surface roughening agent, a preparation method and a roughening method thereof. The surface of the substrate of the electronic product shell is sprayed or electrophoresed to form an organic film layer, the organic film layer can be partially dissolved by the coarsening agent of the surface of the organic film layer, and undissolved organic substances and additive coarse particles in the organic film layer can be remained on the surface of the organic film layer subjected to coarsening treatment by the coarsening agent, so that the surface roughness of the organic film layer formed by electrophoresis or spraying is increased, and the bonding force between the organic film layer formed by electrophoresis or spraying and the PVD coating layer is tighter.

Description

Organic film surface roughening agent, preparation method and roughening method thereof
Technical Field
The invention relates to a roughening agent, and particularly relates to an organic film surface roughening agent, a preparation method and a roughening method thereof.
Background
The existing electronic product shell is manufactured by directly performing PVD coating on the surface of a substrate, in order to increase the bonding force between a PVD film layer and the substrate, the surface of the substrate is usually subjected to roughening treatment, the roughening treatment method generally comprises physical roughening and chemical roughening, the physical roughening generally adopts a sand blasting or shot blasting method, the bonding force of a coating obtained by the methods is limited, and the surface of a product is completely free from gloss, which is unfavorable for decorative coating, the chemical roughening method is designed according to the fact that materials capable of reacting with acid or alkali exist in the materials, and the materials are dissolved from components after being treated by the acid or alkali, so that the surface is roughened. Chemical roughening can result in a uniformly roughened surface that bonds much better to the coating than physical roughening. The most commonly used chemical roughening solutions are strongly oxidizing roughening solutions based on chromic acid and sulfuric acid, and roughening solutions containing phosphoric acid and potassium dichromate are also available. However, the chemical roughening solution has strong corrosivity, and when the chemical roughening solution is used for roughening the surface of a substrate which is sprayed or electrophoresed to form an organic film, the chemical roughening solution can damage the surface of the organic film. Therefore, the conventional chemical roughening solution cannot be directly applied to the surface of the substrate on which the organic film layer is formed by spraying or electrophoresis. On the other hand, in order to further improve the surface decoration effect of the substrate, the PVD coating needs to be performed on the surface of the organic film layer formed by spraying or electrophoresis, and the organic film layer formed by spraying or electrophoresis is an acrylic resin or epoxy resin organic film layer, but the adhesion between the organic film layer formed by spraying or electrophoresis and the PVD coating is poor. Therefore, how to develop an electronic product casing capable of increasing the adhesion between the organic film layer formed by spraying or electrophoresis and the PVD coating layer is a problem to be solved in the field.
Disclosure of Invention
Aiming at the technical problem of poor adhesive force between an organic film layer (acrylic resin or epoxy resin organic film layer) formed by spraying or electrophoresis on a base material of an electronic product shell and a PVD (physical vapor deposition) coating layer, the invention provides a roughening agent capable of increasing the adhesive force between the organic film layer (spraying layer or electrophoresis layer) and the PVD coating layer, wherein the roughening agent is used for roughening the surface of the organic film layer formed by spraying or spraying, so that the adhesive force between the PVD coating layer and the organic film layer can be effectively increased.
In one aspect of the invention, an organic film surface roughening agent is provided, which comprises a main solvent, an auxiliary main solvent, a nonionic surfactant, a corrosion inhibitor, a thickening agent, a film forming agent and water; the main solvent is at least one of benzyl alcohol, butyl diethylene glycol, octanol, isooctanol, hexanol, heptanol, 2-ethylhexanol, 1-methylcyclohexanol, hexanediol and 5-ethyl-2-nonanol; the auxiliary main solvent is at least one of n-butanol, isobutanol, ethanol, methanol, propanol, propylene glycol, isopropanol, butanediol and pentanol. The surface of the substrate of the electronic product shell is sprayed or electrophoresed to form an organic film layer, the organic film layer can be partially dissolved by the roughening agent on the surface of the organic film layer, the partial dissolution mainly depends on the matching use of a main solvent and an auxiliary main solvent, the dissolving capacity of the main solvent is strong, organic substances in the organic film layer can be dissolved, but when only the main solvent is used (namely the auxiliary main solvent is not matched), the roughening agent has strong roughening capacity on the organic film layer, the roughening corrosion on the organic film layer is serious, the roughening effect is not easy to control, the substrate is easy to damage, and therefore the auxiliary main solvent with volatility is needed to assist the main solvent to dissolve the organic substances. The organic film surface roughening agent prepared by the method can better control the roughening effect of the roughening agent on the surface of the organic film. The organic film surface roughened by the organic film surface roughening agent prepared by the invention can remain undissolved organic substances in the organic film and additive coarse particles contained in the organic film, so that the surface roughness of the organic film formed by electrophoresis or spraying is increased, and the binding force between the organic film formed by electrophoresis or spraying and a PVD coating layer is tighter.
In another aspect of the invention, a preparation method of the organic film surface roughening agent is provided, and the preparation method is to uniformly mix and stir the components of the organic film surface roughening agent. Therefore, the method is simple and easy to operate, low in cost and easy for industrial production.
In another aspect of the present invention, a method for roughening the surface of an organic film is provided, wherein the components of the organic film surface roughening agent are mixed and stirred uniformly to obtain the roughening agent, and a substrate having the organic film (a spray coating layer or an electrophoresis layer) is placed into the roughening agent to be roughened, wherein the roughening temperature is 50-65 ℃ and the treatment time is 15-120 s. Therefore, the PVD coating is carried out on the surface of the organic film layer subjected to roughening treatment, the adhesive force between the organic film layer and the PVD coating layer can be obviously improved, the bonding between the film layers is more compact, and the tolerance performance is also improved.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation. In the present invention, the organic film formed by spraying or electrophoresis refers to an acrylic resin or epoxy resin organic film.
The invention provides an organic film surface roughening agent, which comprises a main solvent, an auxiliary main solvent, a nonionic surfactant, a corrosion inhibitor, a thickening agent, a film forming agent and water; the main solvent is at least one of benzyl alcohol, butyl diethylene glycol, octanol, isooctanol, hexanol, heptanol, 2-ethylhexanol, 1-methylcyclohexanol, hexanediol and 5-ethyl-2-nonanol; the auxiliary main solvent is at least one of n-butanol, isobutanol, ethanol, methanol, propanol, propylene glycol, isopropanol, butanediol and pentanol. The surface of the organic film layer roughened by the organic film layer surface roughening agent prepared by the method can remain undissolved organic substances in the organic film layer and additive coarse particles contained in the organic film layer, so that the surface roughness of the organic film layer formed by electrophoresis or spraying is increased, and the bonding force between the organic film layer formed by electrophoresis or spraying and a PVD coating layer is tighter.
In the invention, the weight ratio of the main solvent to the auxiliary main solvent can be (5-15) to 1, preferably (7-12): 1. the main solvent has strong dissolving capacity and can dissolve organic substances in the organic film layer, but when only the main solvent is used (namely the auxiliary main solvent is not matched), the coarsening agent has strong coarsening capacity on the organic film layer, the coarsening corrosion on the organic film layer is serious, the coarsening effect is not easy to control, and the base material is easy to damage, so that the auxiliary main solvent with volatility is required to assist the main solvent to dissolve the organic substances. The organic film surface roughening agent prepared by the method can better control the roughening effect of the roughening agent on the surface of the organic film. The dissolution capacity of the main solvent is strong, and when the weight ratio of the main solvent to the auxiliary main solvent is too large, the coarsening process is not easy to control and the base material is easy to corrode; the secondary main solvent is volatile, and when the weight ratio of the main solvent to the secondary main solvent is too small, the coarsening effect is poor because the solubility of the coarsening agent to organic substances in the organic film layer is not enough.
In the invention, the nonionic surfactant is at least one of polyoxyethylene octylphenol ether and polyoxyethylene nonylphenol ether. The nonionic surfactant can be dissolved and dispersed in a solution at a very low concentration and is preferentially adsorbed on the surface of the organic film layer to reduce the surface tension of the organic film layer, so that organic substances in the organic film layer are activated, and the dissolution of the organic substances in the organic film layer is facilitated.
In the invention, the corrosion inhibitor is at least one of 1,2, 3-benzotriazole, sulfenyl benzothiazole and phosphonic carboxylic acid. The corrosion inhibitor mainly has the function of preventing or slowing down the corrosion of metal in the roughening solution.
In the invention, the thickener is at least one of sodium carboxymethyl cellulose, methyl hydrocarbon ethyl cellulose, ethyl hydrocarbon ethyl cellulose and methyl hydrocarbon propyl cellulose. The thickener can increase the viscosity of the system and keep the system in a uniform and stable suspension state or an emulsion state.
In the invention, the film forming agent is paraffin, and the film forming agent forms a film layer on the liquid surface, so that the volatile solvent is prevented from volatilizing too fast, and the coarsening effect of the coarsening agent on the organic film layer is ensured.
In the present invention, the water functions to dissolve the hydrophilic organic substance to promote the coarsening reaction.
In the invention, the organic film layer surface roughening agent also comprises an accelerant, wherein the accelerant is at least one of triethanolamine and succinic acid. The addition of the accelerator can improve the reaction rate and accelerate the coarsening reaction rate of the coarsening agent on the surface of the organic film layer.
In the invention, the organic film layer surface coarsening agent comprises the following components in parts by weight: 40-60 parts of main solvent, 3-8 parts of auxiliary main solvent, 2-6 parts of nonionic surfactant, 1-7 parts of corrosion inhibitor, 2-6 parts of thickener, 2-6 parts of film forming agent, 10-30 parts of water and 0-15 parts of accelerator.
The invention provides a preparation method of the organic film surface roughening agent, which comprises the steps of mixing all components of the organic film surface roughening agent, and then fully and uniformly stirring to obtain the organic film surface roughening agent.
The invention also provides a method for roughening the surface of the organic film, which comprises the steps of spraying or electrophoresing the base material to form the organic film, and roughening the base material with the organic film by using the roughening agent, wherein the roughening temperature is 50-65 ℃, and the roughening time is 15-120 s.
In order to further explain the technical problems, technical solutions and advantages solved by the present invention, the present invention is described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. All the raw materials in the examples of the present invention are commercially available products unless otherwise specified.
Example 1
Preparing an organic membrane layer surface roughening agent, and mixing and uniformly stirring 40 parts of benzyl alcohol, 3 parts of ethanol, 2 parts of octylphenol polyoxyethylene ether, 2 parts of mercaptobenzothiazole, 2 parts of ethyl hydrocarbon ethyl cellulose, 3 parts of paraffin and 10 parts of water by weight to obtain the organic membrane layer surface roughening agent. And (3) placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment for 60 s at the temperature of 65 ℃. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample S1.
Example 2
Preparing an organic film surface roughening agent, and mixing and uniformly stirring 50 parts by weight of butyl diglycol, 5 parts by weight of isopropanol, 4 parts by weight of octylphenol polyoxyethylene ether, 4 parts by weight of 1,2, 3-benzotriazole, 3 parts by weight of sodium carboxymethylcellulose, 5 parts by weight of triethanolamine, 4 parts by weight of paraffin and 20 parts by weight of water to obtain the organic film surface roughening agent. And (3) placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment for 90 s at the temperature of 60 ℃. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample S2.
Example 3
Preparing an organic film layer surface roughening agent, and mixing and uniformly stirring 55 parts of benzyl alcohol, 5 parts of n-butyl alcohol, 6 parts of nonylphenol polyoxyethylene ether, 6 parts of 1,2, 3-benzotriazole, 4 parts of sodium carboxymethylcellulose, 5 parts of succinic acid, 2 parts of paraffin and 30 parts of water by weight to obtain the organic film layer surface roughening agent. And (3) placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment for 90 s at the temperature of 55 ℃. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample S3.
Example 4
Preparing an organic film surface roughing agent, and mixing and uniformly stirring 56 parts of heptanol, 8 parts of propylene glycol, 4 parts of nonylphenol polyoxyethylene ether, 5 parts of 1,2, 3-benzotriazole, 4 parts of methyl hydrocarbon propyl cellulose, 10 parts of triethanolamine, 3 parts of paraffin and 30 parts of water by weight to obtain the organic film surface roughing agent. And (3) placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment for 120 s at the temperature of 55 ℃. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample S4.
Example 5
Preparing an organic film layer surface roughening agent, and mixing and uniformly stirring 60 parts of benzyl alcohol, 4 parts of n-butyl alcohol, 6 parts of nonylphenol polyoxyethylene ether, 7 parts of 1,2, 3-benzotriazole, 6 parts of sodium carboxymethylcellulose, 13 parts of triethanolamine, 5 parts of paraffin and 30 parts of water by weight to obtain the organic film layer surface roughening agent. And (3) placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment for 60 s at the temperature of 55 ℃. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample S5.
Example 6
Preparing an organic film surface roughening agent, and uniformly mixing and stirring 60 parts of 2-ethylhexanol, 3 parts of isobutanol, 5 parts of octylphenol polyoxyethylene ether, 6 parts of phosphine carboxylic acid, 5 parts of methyl hydrocarbon ethyl cellulose, 10 parts of succinic acid, 5 parts of paraffin and 30 parts of water by weight to obtain the organic film surface roughening agent. And (3) placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment for 30 s at the temperature of 55 ℃. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample S6.
Comparative example 1
And (3) cleaning the substrate on which the organic film layer is formed by spraying or electrophoresis without roughening, and directly putting the substrate into a vacuum coating machine for coating to obtain a sample D1.
Comparative example 2
Preparing a commonly used strong oxidizing coarsening agent, and mixing 6 g/L of methyl ethyl ketone peroxide, 100 g/L of m-nitrobenzenesulfonate, 300 g/L of sulfuric acid and 80 g/L of potassium permanganate by weight and stirring uniformly to prepare the coarsening agent. And placing the matrix on which the organic film layer is formed by spraying or electrophoresis in a coarsening agent for coarsening treatment. And cleaning the coarsened base material, and then putting the base material into a vacuum coating machine for coating to obtain a sample D2.
And (3) performance testing: the following tests were carried out according to the national standard GB/T15844-2-1995.
1. And (3) testing the hundred-lattice adhesive force: before testing, the appearance of the sample is checked to be abnormal, and no color change, air bubbles, cracks, falling off and the like exist, and the surface of the base material is wiped clean by using dust-free cloth; the sample surface was uniformly forced (with force such that the blade edge just penetrated through the film layer to the substrate) using a cutting knife to form 10X 10 consecutive 1X 1 mm2A square cell of (2); brushing the fragments of the test area with a dust-free cloth, uniformly pulling out a section of NICIBAN CT405AP-24 tape, removing the foremost section, then cutting off about 55 mm of tape, placing the center point of the tape above the grid in a direction parallel to a set of cutting lines, and then flattening the tape at the position above the grid area with a fingernail to ensure that the tape is in good contact with the film layer, the tape length at least exceeding 20 mm of the grid; sticking an adhesive tape, standing for 90 s, holding one suspended end of the adhesive tape, and quickly pulling down the adhesive tape within 0.5-1.0 s at an angle as close to 60 degrees as possible; the film peeling condition is checked, and the specific evaluation criteria are as follows:
5B: the cutting edge is completely smooth without falling off;
4B: a little coating falls off at the intersection of the cuts, and the affected cross cutting area is not more than 5%;
3B: the coating is stripped at the intersection of the cuts and/or along the edges of the cuts, and the affected cross cutting area is more than 5 percent but not more than 15 percent;
2B: the film layer partially or totally falls off in large fragments along the cut edges and/or partially or totally falls off on different parts of the grid, the affected cross cut area is more than 15% but not more than 35%;
1B: the coating is peeled off along large fragments of the cutting edge, and/or some squares are partially or completely peeled off, and the affected cross cutting area is more than 35 percent but not more than 65 percent;
0B: the degree of exfoliation exceeded 1B.
2. RCA paper tape wear resistance test: a175 g load was applied to a special NORMAN RCA abrasion tester (model 7-IBB) and a special paper tape (11/16 inch wide 6) made by NORMAN, and the tape was continuously rubbed on the surface of the specimen. And setting the number of friction turns, starting the instrument, observing the surface of the sample after the test, increasing the number of friction turns to test again until the substrate is exposed (starting from 0 turn and increasing 50 turns every time) if the substrate is not exposed, and recording the number of turns of the substrate exposed for the first time.
3. And (3) steel wool testing: a250 gf load was applied with special STEEL WOOL (STEEL WOOL type: #0000, manufacturer: Bon Star STEEL WOOL), and the area of the indenter was measured 2X 2 cm2The sample was rubbed back and forth on the surface at a speed of 40 cycles/min with a stroke of about 40 mm. And setting the number of friction turns, starting the instrument, observing the surface of the sample after the test, increasing the number of friction turns to test again until the substrate is exposed (starting from 0 turn and increasing 10 turns every time) if the substrate is not exposed, and recording the number of turns of the substrate exposed for the first time.
4. Newton's pen test: a Newton pen (Model: ERICHSEN, Hardness Test Pencil Model 318) is adopted, a proper spring is selected according to different requirements, pressure is selected and fixed, the Newton pen is vertically placed on a Test surface, is pressed downwards and is used for drawing 35 mm straight lines on the surface at the speed of 5 mm/second, the surface is observed after being lightly wiped by dust-free cloth, if no scratch occurs, the pressure is increased until the scratch occurs on the surface of a sample (from 0N, 1N is increased every time), and the pressure when the scratch occurs for the first time is recorded.
5. Chemical resistance test: the cosmetics (lipstick, foundation liquid and hand cream) are uniformly smeared on a sample, placed in a constant temperature and humidity cabinet with the temperature of 70 ℃ and the humidity of 90% for 24 hours, then placed at normal temperature for 4 hours, and the product is wiped by alcohol, so that no obvious residual trace exists, and the product is qualified.
6. And (3) temperature impact test: before testing, visually inspecting a sample, putting the product into a temperature impact testing machine, placing the product at minus 40 ℃ for 2 h, then transferring the product to 85 ℃ for 2 h for 1 cycle, and placing the product at normal temperature for 4 h after 5 cycles, wherein before/after testing, the product has no adverse phenomena such as corrosion, spots, fading, discoloration, cracks, foaming, distortion and the like, and is qualified.
7. And (3) testing the damp-heat cycle: the sample is placed in a constant temperature and humidity box with the temperature of 50 ℃ and the humidity of 95 percent for 72 h. Before/after the test, the test shows that the steel plate is qualified without adverse phenomena such as corrosion, spots, fading, discoloration, cracks, bubbling, distortion and the like.
8. And (3) salt spray testing: placing the sample into a salt fog chamber according to an actual installation mode, continuously spraying for 2 h (spraying solution: 5% NaCl solution, pH 6.5-7.2) at 35 +/-2 ℃, then placing the sample into a constant temperature and humidity box, placing the constant temperature and humidity box at 50 ℃ and 95% for 22 h for 1 cycle, performing 3 cycles in total, and performing visual and mechanical property inspection on the sample in a laboratory environment recovery period. The product surface should not have the abnormality such as rust, discoloration, bubbling and the like, and the 3M610 adhesive tape is used for adhesion test (drawing for 4 times), and the product is qualified if the product does not fall off.
The test results of the above examples and comparative examples are shown in table 1:
TABLE 1
Adhesion test RCA wear resistance Steel wool test Newton's pen test Chemical resistance test Temperature shock test Damp and heat cycle test Salt spray test
S1 3B 250 turns 120 circles 4N OK OK OK OK
S2 4B 250 turns 120 circles 4N OK OK OK OK
S3 5B 300 circles 150 circles 5N OK OK OK OK
S4 4B 250 turns 120 circles 4N OK OK OK OK
S5 3B 250 turns 110 circles 4N OK OK OK OK
S6 3B 150 circles 110 circles 3N OK OK OK OK
D1 0B 50 circles 50 circles 1N OK NG NG NG
D2 2B 150 circles 100 circles 2N OK NG NG OK
Examples 1 to 6 samples S1 to S6 were prepared by roughening an organic film with the organic film surface roughening agent prepared according to the present invention and then performing PVD coating. From the test results in Table 1, it can be seen that the adhesion, abrasion resistance and various environmental tests of samples S1-S6 are significantly better than those of comparative samples D1 and D2. Wherein, the weight ratio of the main solvent to the auxiliary main solvent in the embodiment 1-5 is (5-15):1, and the weight ratio of the main solvent to the auxiliary main solvent in the embodiment 6 is 20: 1, the performance of the sample prepared in the example 6 is slightly poor, but is still better than that of the samples prepared in the comparative examples 1 and 2, which shows that the coarsening treatment of the organic film surface coarsening agent prepared by the invention on the organic film can effectively increase the binding force between the organic film and the PVD coating layer.
The organic film surface roughening agent prepared by the invention can dissolve part of the organic film through the matching use of the main solvent, the auxiliary main solvent, the nonionic surfactant and other components, and undissolved organic substances in the organic film and additive coarse particles contained in the organic film can be remained on the surface of the organic film subjected to roughening treatment by the organic film surface roughening agent prepared by the invention, so that the surface roughness of the organic film formed by electrophoresis or spraying is increased, and the binding force between the organic film formed by electrophoresis or spraying and a PVD coating layer is tighter.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (9)

1. An organic film surface roughening agent is characterized by comprising 40-60 parts of main solvent, 3-8 parts of auxiliary main solvent, 2-6 parts of nonionic surfactant, 1-7 parts of corrosion inhibitor, 2-6 parts of thickening agent, 2-6 parts of film forming agent and 10-30 parts of water by weight; the main solvent is at least one of benzyl alcohol, butyl diethylene glycol, octanol, hexanol, heptanol, 2-ethylhexanol, 1-methylcyclohexanol, hexanediol and 5-ethyl-2-nonanol; the auxiliary main solvent is at least one of n-butyl alcohol, isobutyl alcohol, ethanol, methanol, propanol, propylene glycol, butanediol and amyl alcohol; the weight ratio of the main solvent to the auxiliary main solvent is (5-15) to 1, and the organic film layer is an acrylic resin or epoxy resin organic film layer.
2. The organic film surface roughening agent as claimed in claim 1, wherein the nonionic surfactant is at least one of polyoxyethylene octylphenol ether and polyoxyethylene nonylphenol ether.
3. The organic film surface roughening agent as recited in claim 1, wherein said corrosion inhibitor is at least one of 1,2, 3-benzotriazole, mercaptobenzothiazole, and phosphonocarboxylic acid.
4. The organic film layer surface roughening agent according to claim 1, wherein said thickener is at least one of sodium carboxymethyl cellulose, methyl hydrocarbon ethyl cellulose, ethyl hydrocarbon ethyl cellulose, and methyl hydrocarbon propyl cellulose.
5. The organic film layer surface roughening agent as recited in claim 1, wherein said film forming agent is paraffin.
6. The organic film layer surface roughening agent according to claim 1, further comprising a promoter: the accelerant is at least one of triethanolamine and succinic acid.
7. The organic film layer surface roughening agent as claimed in any one of claims 1 to 6, wherein the organic film layer surface roughening agent includes 0 to 15 parts by weight of an accelerator.
8. A method for preparing an organic film surface roughening agent, characterized in that the components of the organic film surface roughening agent according to any one of claims 1 to 7 are mixed and stirred uniformly.
9. A method for roughening the surface of an organic film layer, which is characterized in that a substrate with the organic film layer is placed in the organic film layer surface roughening agent of any one of claims 1 to 7 to be roughened, wherein the roughening temperature is 50-65 ℃, the roughening time is 15-120 s, and the organic film layer is an acrylic resin or epoxy resin organic film layer.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000282246A (en) * 1999-04-01 2000-10-10 Nippon Kayaku Co Ltd Preetching agent
CN1823557A (en) * 2003-09-29 2006-08-23 揖斐电株式会社 Interlayer insulating layer for printed wiring board, printed wiring board and method for manufacturing same
CN101260257A (en) * 2008-04-28 2008-09-10 嘉纳尔科技（北京）有限公司 Low volatility paint remover
CN107337956A (en) * 2016-12-27 2017-11-10 深圳市新合富力科技有限公司 Magnesium alloy paint stripper

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000282246A (en) * 1999-04-01 2000-10-10 Nippon Kayaku Co Ltd Preetching agent
CN1823557A (en) * 2003-09-29 2006-08-23 揖斐电株式会社 Interlayer insulating layer for printed wiring board, printed wiring board and method for manufacturing same
CN101260257A (en) * 2008-04-28 2008-09-10 嘉纳尔科技（北京）有限公司 Low volatility paint remover
CN107337956A (en) * 2016-12-27 2017-11-10 深圳市新合富力科技有限公司 Magnesium alloy paint stripper

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