A coating process for improving the wear resistance of microcrystalline glass

Abstract

The application discloses a kind of coating processes for improving the wear resistance of microcrystalline glass, belongs to the technical field of microcrystalline glass processing, including AF silk printing process and AF coating process, characterized by including: before AF silk printing process, it also includes substrate surface pretreatment process, ICP etching treatment process, substrate surface finishing process;The beneficial effects of the application are: the surface of microcrystalline glass substrate is pretreated, the wear resistance of microcrystalline glass is improved, a two-step deposition method is used to obtain a coating microcrystalline glass with superior firmness, Mohs hardness, water drop angle and daun value;Two-step ICP etching treatment with specific gas fraction is used to improve the wear resistance of microcrystalline glass after polishing surface finishing and coating.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of microcrystalline glass processing, and more particularly to a film plating process for improving the wear resistance of microcrystalline glass. BACKGROUND

[0002] Nanocrystalline glass is a kind of high-strength glass newly developed in recent years, which has obvious advantages in physical properties and mechanical properties compared with ordinary high-aluminum glass. As a CG cover plate, it is a good substrate selection. However, due to the differences in manufacturing process and inherent properties of nanocrystalline glass, the surface of the nanocrystalline glass substrate has greater roughness and microcracks compared with other glasses, thereby greatly reducing the AF performance. In order to better improve the performance of AF on this substrate, a new film plating treatment method is developed to enhance the wear resistance of nanocrystalline glass AF. SUMMARY

[0003] To solve the above problems and overcome the shortcomings of the prior art, the application provides a film plating process for improving the wear resistance of microcrystalline glass, which can effectively solve the problem of greater roughness and microcracks on the surface of the nanocrystalline glass substrate compared with other glasses.

[0004] The specific technical solution of the application to solve the above technical problems is: a film plating process for improving the wear resistance of microcrystalline glass, comprising an AF silk printing process and an AF film plating process, characterized by comprising: a substrate surface pretreatment process, an ICP etching treatment process, and a substrate surface finishing process before the AF silk printing process.

[0005] The substrate surface pretreatment process is: using a two-step deposition method, depositing 3-7nm of a first layer of primer material on the substrate surface by PVD, and then depositing 20-30nm of a second layer of primer material on the first layer of primer material.

[0006] The ICP etching treatment process is: under the protection of an inert protective gas, using an etching gas source and a catalytic gas, and using ICP to etch the surface of the film layer.

[0007] The substrate surface finishing process is: using a polishing material to polish the surface of the etched film layer.

[0008] Further, the film layer after polishing surface finishing is subjected to AF silk printing and AF film plating.

[0009] Further, the first layer of primer material is nitride, and the second layer of primer material is SiO2.

[0010] Further, the first layer of primer material is nitride, and the nitride is Si3N4.

[0011] Further, the ICP etching treatment process is as follows: Ar gas is used as inert protective gas, N2 is used as main etching gas source, O2 and H2 are used as catalytic gas, and ICP is used to etch the surface of the film layer.

[0012] Further, the ICP etching treatment process is a two-step process, including:

[0013] ICP Step 1: gas ratio: Ar=700-900sccm, N2=50-150sccm, H2=20-40sccm, power: 2-3KW, etching: 120-150s.

[0014] ICP Step 2: gas ratio: Ar=150-250sccm, O2=300-500sccm, power: 2-3KW, etching: 150-180s.

[0015] ICP Step 2: gas ratio: Ar=150-250sccm, O2=300-500sccm, power: 2-3KW, etching: 150-180s.

[0016] Further, the polishing material is any one of polyurethane, sponge and carpet.

[0017] The beneficial effects of the present application are:

[0018] The present application creatively pretreats the surface of the microcrystalline glass substrate before AF screen printing and AF film plating, improves the wear resistance of the microcrystalline glass, and avoids the roughness and microcracks of the substrate surface compared with other glasses due to the difference between the manufacturing process and the inherent characteristics of the microcrystalline glass, thereby greatly reducing the AF characteristics.

[0019] The present application creatively adopts a two-step deposition method to obtain a film-coated microcrystalline glass with superior firmness, Mohs hardness, water drop angle and da Vinci value.

[0020] The present application creatively adopts a two-step ICP etching treatment with specific gas ratio to improve the wear resistance of the microcrystalline glass after the film-coated film layer on the polished surface is treated. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 is an electron microscope scanning image of the untreated surface of the microcrystalline glass substrate of the present application; Figure 1 Figure 2 is an electron microscope scanning image of the surface of the microcrystalline glass substrate after the pretreatment process of the present application;

[0022] Figure 2 Figure 3 is an electron microscope scanning image of the surface of the microcrystalline glass substrate after the ICP etching treatment process of the present application;

[0023] Figure 3 is an electron microscope scanning image of the surface of the microcrystalline glass substrate after the ICP etching treatment process of the present application; Figure 3 Figure 3 is an electron microscope scanning image of the surface of the microcrystalline glass substrate after the ICP etching treatment process of the present application;

[0024] Figure 4 ​​is a microcrystalline glass substrate surface treatment process after the appearance of the electron microscope scanning graph; DETAILED DESCRIPTION

[0025] In the description of the present application, specific details are merely to enable a full understanding of the embodiments of the present application, but as a person skilled in the art should know that the implementation of the present application is not limited to these details. In addition, well-known structures and functions are not described or shown in detail to avoid obscuring the essential points of the embodiments of the present application. For those skilled in the art, the specific meaning of the above terms in the present application can be understood in specific circumstances.

[0026] DETAILED DESCRIPTION

[0027] In order to better understand the present application, specific examples are described, it is worth emphasizing that the effect of the embodiment and various embodiments within the scope of the present application, including the respective reagents and the content of the reagent ratio, there is no substantial difference, can realize the effect described in the present application and solve the above problems, other combinations are not listed here;

[0028] The specific steps are as follows:

[0029] First step: using two-step deposition method for substrate surface pretreatment; through PVD method on the substrate surface deposition 3-7nm first layer of bottoming material, then on the first layer of bottoming material again deposition 20-30nm second layer of bottoming material;

[0030] Specifically: the vacuum degree of magnetron sputtering coating machine reaches 2.0E-3pa, ICP gas (when Si3N4 is deposited, N2 is needed, and SiO2 needs O2), ICP (oxidation source) starts to work, clean the glass surface for 2min, and then the target gas is filled with Ar. In this process, first, the first layer of bottoming material film layer is deposited (according to the film system program setting) 5nm Si3N4 layer as the bottom layer, and then the second layer of bottoming material film layer is deposited (according to the film system program setting) 25nm SiO2,

[0031] Among them, the film system program setting of the first layer of bottoming material film layer deposition is: when 5nm Si3N4 layer is deposited, the double target power is 12KW, the target Ar flow is 300sccm, the ICP power is 2KW, and the O2, N2 of ICP (oxidation source) is filled in the ratio of 50sccm:600sccm;

[0032] The film system program setting of the second layer of bottoming material film layer deposition is: when 25nm SiO2 layer is deposited, the single target power is 6KW, and special attention is paid to the slow speed (≈1 angstrom / s) of the outermost Si02; the target Ar flow is 300sccm, the ICP power is 2KW, and the Ar, O2 flow ratio of ICP gas is 50sccm:200sccm;

[0033] Second step: ICP etching treatment on the surface of the two-step deposited film layer, the specific parameters are as follows:

[0034] ICP Step 1: gas ratio: Ar = 700-900sccm, N2 = 50-150sccm, H2 = 20-40sccm, power: 2-3KW etching: 120-150s;

[0035] Step 2: gas ratio: Ar = 150-250sccm, O2 = 300-500sccm, power: 2-3KW etching: 150-180s;

[0036] Third step: single-sided polishing treatment, the specific parameters are as follows:

[0037] The polishing material is selected from any one of polyurethane, sponge and carpet, the upper disc rotation speed is 55-65, the lower disc rotation speed is 16-19, the pressure control current is 9-11, and the polishing time is 250-350s;

[0038] After the polishing surface finishing of the film layer, Figure 4 According to the prior art, AF silk screen printing and AF film plating are carried out on the film layer after polishing surface finishing, specifically:

[0039] Fourth step: After the product is returned to the grinding, it is cleaned on the flat plate, the back frame ink is printed, it is baked at 150℃ / 30min, and then it is cleaned in the flat plate cleaning machine to ensure that the film plating surface is clean OK, and then the film (two-side film, the bottom film is high-temperature PET film, and the surface film is PE anti-static protective film) is coated. After the PET high-temperature film on the back of the coated product is firmly pasted to the film plating machine drum by high-temperature double-sided adhesive, the PE anti-static protective film is torn off, the film plating machine door is closed, and vacuum is extracted;

[0040] Fifth step: AF plating, when the film plating vacuum reaches ≤3.0E-3pa,

[0041] a). Plasma: argon 650-750sccm, power 650-800W, cleaning 8-10min;

[0042] b). Preheat the evaporation resistance (AF film material) to start the evaporation resistance energy: 20% / 30s;

[0043] c). Evaporation resistance energy: 34% to start evaporation AF film material ≥350s to form a film.

[0044] In order to more intuitively show the process advantages of the present application, the film plating process of the present application and the equivalent replacement method of the same process are compared,

[0045] Comparative example 1:

[0046] The preparation method is the same as that of the example, except that in the preparation process of the present comparative example, the substrate surface pretreatment is as follows: using one-step deposition method, and the primer material is nitride, and the total film thickness is consistent with the present application.

[0047] Comparative Example 2

[0048] The preparation method is the same as that of the example, except that in the preparation process of the present comparative example, the substrate surface pretreatment is as follows: using one-step deposition method, and the primer material is SiO2, and the total film thickness is consistent with the present application.

[0049] Comparative Example 3

[0050] The preparation method is the same as that of the example, except that in the preparation process of the present comparative example, the substrate surface pretreatment is not used.

[0051] And the product is tested for firmness DOE, wherein the firmness test standard is as follows:

[0052] Test conditions: 80℃±2℃ pure water, water boiling of the sample for 30min / 60min / 90min / 120min / 150min; after standing at room temperature for 2 hours, the adhesion test is carried out;

[0053] Test method and judgment: after the same time, use an art knife to draw a 1*1mm grid on the surface of the product to be tested according to the hundred grid tool, select 3M CT-18 special film pulling adhesive tape, completely adhere to the hundred grid surface, press without air bubbles, and then observe the surface of the adhesive tape, if there is no film layer, it is judged as NG, if there is no film layer, it is judged as OK.

[0054] And the product is tested for hardness, wherein the hardness test standard is as follows:

[0055] Test conditions: using a specified hardness Mitsubishi test pencil core or a corresponding hardness Mohs hardness pen tip, with a pressure of 1kgf, the angle between the pencil core or pen tip and the surface to be tested is 45°, and 3 lines are drawn on the front surface of the lens to be tested, each line being 5mm long.

[0056] Test method and judgment: the test substrate is fixed with the test surface facing up, the angle and range are adjusted, the test pen core or pen tip is in contact with the test surface, the weight is increased by 1000g, the feed speed is 1cm / min, the switch is started to begin testing, and the test is repeated three times for different positions, if the surface is scratched, it is judged as NG, if not, it is judged as OK (note: the initial position is considered as OK if there is a scratch).

[0057] And the product is tested for water drop angle and da Vinci value, wherein the water drop angle test specification is as follows:

[0058] The substrate plated with different thickness and different materials is placed and fixed on the test platform, 4-6ml water is dropped by the dropper and waits for 2-3s, the water source is selected as pure water, the height of the needle tube is adjusted until the surface of the substrate is contacted, then the height of the platform is lowered to make the water droplet and the needle tube separate, the height and axial distance of the platform are adjusted to make the camera display the clearest image, and the special water droplet angle tester is used to calculate the size of the water droplet angle;

[0059] Table 1: Process comparison test data of two-step deposition method of the application

[0060]

[0061] From the data analysis in Table 1, it can be seen that:

[0062] (1) The comparison between the example and Comparative Example 1 shows that although Si3N4 is used as the first layer of bottoming material, the lack of SiO2 as the outer layer of bottoming material leads to the lack of -Si bond for chemical bond reaction with AF material, which cannot be successfully prepared into a film;

[0063] (2) The comparison between the example and Comparative Example 2 shows that SiO2 is used as the first layer of bottoming material, although the scheme can be successfully prepared into a film, but there is a serious internal stress defect after the deposition of the whole film layer, which leads to the risk of film peeling;

[0064] (3) The comparison between the example and Comparative Example 3 shows that the lack of SiO2 as the outer layer of bottoming material leads to the lack of AF chemical reaction bond, which cannot be successfully prepared into a film.

[0065] In order to more intuitively show the process advantages of the application, the first layer of bottoming material of the film plating process of the application is studied and compared with the same process using equivalent replacement method,

[0066] Table 2: Comparison test data of firmness of different first layer of bottoming material of the application

[0067]

[0068] From the data analysis in Table 2, it can be seen that:

[0069] The influence of different first layer of bottoming material on firmness is studied, and it can be seen that although both use twice deposition method, the first layer of bottoming material uses Si3N4, and the second layer of bottoming material uses SiO2, compared with the first layer of bottoming material using SiO2 and NB2O5, it has superior firmness performance and better risk resistance performance.

[0070] Table 3: Comparison test data of Mohs hardness of different first layer of bottoming material of the application

[0071]

[0072]

[0073] From the data analysis of Table 3, it can be seen that:

[0074] The influence of different first layer primer materials on the Mohs hardness is studied, and it can be seen that, although both of them adopt twice deposition, the first layer primer material is Si3N4, and the second layer primer material is SiO2, which has superior Mohs hardness compared with the first layer primer material of SiO2 and NB2O5.

[0075] Table 4: Comparison test data of water drop angle and da Vinci value of different first layer primer materials of the application

[0076]

[0077] From the data analysis of Table 4, it can be seen that:

[0078] The influence of different first layer primer materials on the water drop angle and da Vinci value is studied, and it can be seen that, although both of them adopt twice deposition, the first layer primer material is Si3N4, and the second layer primer material is SiO2, which has superior water drop angle and da Vinci value compared with the first layer primer material of SiO2 and NB2O5.

[0079] Among them, the smaller the da Vinci value, the better the hydrophobicity, the larger the water drop angle, and the lower the surface relative roughness; the larger the water drop angle, the worse the hydrophobicity, the smaller the water drop angle, and the higher the surface relative roughness, so the da Vinci value and the initial water drop angle of the surface can reflect whether the surface is rough or flat from the side, as another evaluation dimension of the surface quality.

[0080] In order to more intuitively show the process advantage of the application, the application coating process and the same process are compared by using equivalent replacement method,

[0081] Comparative Example 4:

[0082] The preparation method is the same as the example, except that in the preparation process of the comparative example, the ICP etching treatment is only performed once.

[0083] Comparative Example 5:

[0084] The preparation method is the same as the example, except that in the preparation process of the comparative example, the ICP etching treatment is only performed twice.

[0085] Comparative Example 6:

[0086] The preparation method is the same as the example, except that in the preparation process of the comparative example, the ICP etching treatment is not performed.

[0087] Friction test index:

[0088] Weight: 1000g, grinding head: 1*1 cm, steel wool: BON STAR #0000, stroke: 40 mm, speed: 60 / min, 3000 times, water drop angle after test > 100°

[0089] Friction test method and determination:

[0090] The test piece was fixed on the test table with the side facing up, the test stroke of the friction rod was adjusted to 40 mm, the friction times were 3000, the friction rod with steel wool was completely contacted with the test surface and the position was fixed after adding a 1000g weight, the test was started by clicking, and after the friction times reached, the test piece was removed, the surface residual steel wool debris was wiped off with a clean silk cloth, and the measurement range was marked by blowing, 3 points were tested from top to bottom, a special water drop angle tester was used to calculate, the test results were saved, and whether it was greater than 100° was determined according to the standard, greater than OK, less than NG. (Note: the water drop angle after friction is lower than 20°, which means that the film layer is completely worn off, between 20°-60°, there is linear or point wear, between 60°-80°, the film layer has a sanding feeling, and above 80°, the film layer is relatively complete);

[0091] Table 5: Comparison test data of different etching treatments of the application

[0092]

[0093] Table 6: Comparison test data of single ICP etching treatment

[0094]

[0095] From the data in Tables 5 and 6, it can be seen that regardless of the component ratio and type of the atmosphere, after only the first etching treatment, the waterproof film is plated (the plating process and the last step AF plating parameters remain the same), and the friction peeling phenomenon occurs, the chemical reaction bond-Si of AF and the material is damaged, -Si and -OH, -F cannot be effectively combined, so this step cannot exist independently in this scheme.

[0096] Table 7: Comparison test data of single ICP etching treatment

[0097]

[0098] From the data in Tables 5 and 7, it can be seen that regardless of the component ratio and type of the atmosphere, only the second step, from the thickness change of the film layer, even if the component of the second step atmosphere is adjusted, there is no substantial optimization and improvement of the film layer itself, and there is no significant difference between groups, thereby proving the internal correlation between the two ICP etching treatments.

[0099] In summary: the application creatively adopts two-step deposition method to obtain a plated microcrystalline glass with superior firmness, Mohs hardness, water drop angle and dyne value;

[0100] The application creatively adopts two-step deposition method to obtain a plated microcrystalline glass with superior firmness, Mohs hardness, water drop angle and dyne value;

[0101] The application creatively adopts two-step ICP etching treatment of specific gas to improve the wear resistance of the microcrystalline glass after the film layer on the polished surface is treated and plated.

Claims

1. A coating process for improving the wear resistance of microcrystalline glass, comprising an AF screen printing process and an AF coating process, characterized in that... include: The process before AF screen printing also includes substrate surface pretreatment, ICP etching, and substrate surface finishing. The substrate surface pretreatment process is as follows: a two-step deposition method is used to deposit a 3-7nm first layer of base material on the surface of the microcrystalline glass substrate by PVD. The first layer of base material is Si3N4. Then, a 20-30nm second layer of base material is deposited on the first layer of base material. The second layer of base material is SiO2. The ICP etching process involves using an etching gas source and a catalytic gas under the protection of an inert protective gas to etch the film surface with ICP, thereby reducing surface roughness. The ICP etching process specifically involves using Ar gas as an inert protective gas, N2 as the etching gas source, and O2 and H2 as catalyst gases. The surface finishing process of the substrate involves using polishing materials to polish the etched film layer.

2. The coating process for improving the wear resistance of microcrystalline glass according to claim 1, characterized in that... After the surface polishing process, the film layer is subjected to AF screen printing and AF coating.

3. The coating process for improving the wear resistance of microcrystalline glass according to claim 1, characterized in that... The ICP etching process consists of two steps: Stepl inflation ratio: Ar=700-900sccm, N2=50-150sccm, H2=20-40sccm; power: 2-3KW; etching: 120-150s; Step 2 inflation ratio: Ar=150-250sccm, O2=300-500sccm, power: 2-3KW; etching: 150-180s.

4. The coating process for improving the wear resistance of microcrystalline glass according to claim 1, characterized in that... The polishing material can be any one of polyurethane, sponge, or carpet.

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