A preparation method and application of a reusable coating carrier

Abstract

The present invention belongs to the technical field of vacuum coating, and specifically discloses a method for preparing a reusable coating carrier. First, the surface of the carbon felt is etched with an acidic solution, and then the oxygen-containing functional groups such as ‑COOH and C=O on the surface are removed by alkali washing, and ultrasound is used to assist to prepare a deoxygenated carbon felt. Thereafter, a hydrophobic layer is deposited on the surface of the deoxygenated carbon felt by an electrochemical deposition method to obtain a surface-passivated hydrophobic carbon felt. The carbon felt has excellent hydrophobic and lipophilic properties and can be attached with a large amount of evaporation agents. Compared with the prior art, the prepared pills are placed in a room temperature environment for up to three months, and the coated pills can still function stably. The carrier material can still be used normally after being recycled five times, and does not affect the coating performance.

Description

Technical Field

[0001] The invention relates to the field of vacuum evaporation coating, and in particular to a preparation method and application of a reusable coating carrier. Background Art

[0002] Vacuum evaporation coating refers to a deposition technology that uses the heat energy of a film material heating device (called an evaporation source) under vacuum conditions to evaporate a certain substance and deposit it on the surface of the substrate material. Among them, the coating carrier plays a very important role. It is required to be pure and non-deteriorated, not react with the evaporation agent, and have high temperature resistance.

[0003] Patent CN114310184A provides a method for preparing a vacuum-coated pill carrier. The technology uses stainless steel micro-wire felt as a carrier and uses stamping technology to press it into a metal crucible to obtain a pill carrier, which can effectively ensure the stability of the pill properties and greatly save labor costs. However, steel wool made of low-carbon steel is very easy to absorb moisture and rust and deteriorate, which makes it difficult to reuse it after completing a coating experiment. In addition, during the production process, more or less oily compounds will adhere to the surface of the steel wool, which seriously affects the performance of the evaporation agent.

[0004] In order to solve the cleanliness problem of steel wool, patent CN111020490A discloses a method for preparing film-coated AF pills. This technology uses vacuum baking to dry and remove impurities from steel wool. The prepared AF pills can be placed at room temperature for more than 3 months, and can be placed at high temperature and high humidity of 60 ℃ / 60% for more than 1 month without reducing product performance.

[0005] However, the above technical solutions, including the existing technologies, do not solve the problem that the steel wool can be reused after the evaporation, which undoubtedly greatly increases the production cost. Therefore, it is urgent to develop a coating carrier that does not affect the evaporation agent, is reusable, and has a low cost. Summary of the invention

[0006] In view of the problems in the prior art such as poor stability and non-reusability of coating carriers, the first object of the present invention is to provide a reusable coating carrier, which material does not react with the evaporation agent, has stable properties, can be stored for a long time, and can be recovered and reused multiple times after the evaporation is completed.

[0007] The second object of the present invention is to provide a method for preparing a reusable coating carrier, which is simple and easy to implement, has low cost and is suitable for industrial production.

[0008] In order to achieve the above technical objectives, the present invention provides a method for preparing a reusable coating carrier, which specifically includes the following preparation steps:

[0009] Step 1:

[0010] The carbon felt is immersed in an acidic solution, and after being taken out, it is washed with ultrapure water until the pH of the washing solution is neutral, and then dried at 60°C; then, the surface of the carbon felt is defunctionalized with an alkaline solution, and ultrasound is used to assist, and after being taken out, it is washed with ultrapure water until the pH of the washing solution is neutral, and then dried at 60°C to obtain a surface passivated carbon felt;

[0011] Step 2:

[0012] In a dual-electrode system, the surface passivated carbon felt is fixed on the cathode electrode, electrodeposited in an electrolyte, and attached with a uniform hydrophobic layer through magnetic stirring. After completion, it is sequentially cleaned with ultrapure water, anhydrous ethanol, and acetone, and finally dried.

[0013] Preferably, the acidic solution is one of H2SO4, HNO3, and H2SO4-HNO3.

[0014] Preferably, the ratios of the acidic solutions are H2SO4: H2O = 0.5~2: 1~4, HNO3: H2O = 0.5~2: 1~4, H2SO4: HNO3: H2O = 0.5~2: 0.5~2: 1~4.

[0015] In the present invention, the particularly preferred acidic solution is a mixed acid solution of H2SO4-HNO3. Studies have found that when the H2SO4-HNO3 mixed acid solution is used for treatment, it helps to synergistically improve the reusability of the subsequently prepared coating carrier.

[0016] Preferably, in the present invention, the ratio of the particularly preferred mixed acid solution is 1-1.5:0.7-1.1:3-3.5, and the treatment time and temperature can be adjusted according to the preparation requirements. Considering the convenient operability of the technical solution, the time can be 1-3 hours and the temperature can be 20-50°C. Studies have found that when the above concentration is used for treatment, it helps to further improve the reusability of the coating carrier.

[0017] Preferably, the alkaline solution is one of NaOH and KOH.

[0018] Preferably, the concentration of the alkaline solution is 1 mol / L to 5 mol / L.

[0019] In the present invention, the particularly preferred concentration of the alkaline solution is 2.7-3.1 mol / L. Studies have found that when the particularly preferred concentration of the alkaline solution is used for treatment, it is beneficial to improve the reusability of the coating carrier.

[0020] The time and temperature of the alkaline solution treatment can be adjusted according to the preparation requirements. Considering the convenient operability of the technical solution, the treatment time can be 1~3 h and the temperature can be 20~50°C.

[0021] Preferably, the anode in the dual-electrode system is one of metal nickel, iron, and cobalt, depending on the cations in the electrolyte, and the cathode is metal titanium.

[0022] Preferably, the electrolyte is an acidic salt solution of metals such as Ni, Fe, and Co.

[0023] Preferably, the acidic salt solution is a sulfate or hydrochloride solution of metal Ni, Fe, or Co. In the present invention, a mixed acidic solution of NiSO4 and CoSO4 is particularly preferred, and its concentration is preferably 0.1-1.5 mol / L and 0.1-1.5 mol / L, and particularly preferably 0.8-1.2 mol / L and 0.3-0.5 mol / L, which can effectively improve the adsorption and stability of the coating carrier to the evaporation agent and improve the reusability of the coating carrier.

[0024] The current density of the mixed acid solution can be adjusted according to the preparation requirements. Considering the convenient operation of the technical solution, the current density can be -50 ~ -150 mA / cm 2 .

[0025] Preferably, the drying treatment in step 2 refers to drying at 60° C. for 6 to 18 hours.

[0026] In the present invention, the particularly preferred drying time is 10 to 12 h, which helps to improve the hydrophobicity of the coating carrier and improve the reusability of the coating carrier.

[0027] The beneficial effects of the present invention are:

[0028] 1. Through the preparation method provided by the present invention, especially the initial acidic and alkaline solution modification treatment steps, the surface of the carbon felt is successfully passivated, and the active functional groups are effectively removed, thereby significantly improving the retention capacity of the coating carrier for the evaporation agent. This modification treatment not only enables the evaporation agent to effectively adhere to the carrier surface for a long time, but also ensures the stability of the performance during the coating process, avoiding coating quality problems caused by agent loss or performance degradation.

[0029] 2. The preparation method of the present invention endows the coating carrier with excellent stability and durability. After repeated use, the coating carrier can still maintain good physical and chemical properties and continue to be used as an effective carrier for evaporation operation. This feature not only reduces production costs, but also reduces the generation of waste, which is in line with the development trend of green environmental protection.

[0030] 3. The preparation method of the present invention has clear steps and is easy to operate. It can realize the preparation of the film-coated carrier without complicated equipment and expensive raw materials. This simple and easy-to-use preparation method greatly reduces the production cost and improves the production efficiency, so that the film-coated carrier has a wide application prospect and market competitiveness in industrial production.

[0031] In summary, the preparation method of the reusable coating carrier provided by the present invention shows significant beneficial effects in improving the retention capacity of the evaporation agent, enhancing the stability and durability of the coating carrier, simplifying the preparation process, and reducing production costs, and has important practical application value and market promotion prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is the SEM image of the reusable coating carrier prepared in Example 1;

[0033] Figure 2 This is an enlarged SEM image of the reusable coating carrier prepared in Example 1;

[0034] Figure 3 The XRD pattern of the reusable coating carrier prepared in Example 1;

[0035] Figure 4 The results of the recycling experiment of the reusable coating carrier prepared in Example 1;

[0036] Figure 5 The coating performance results of the reusable coating carrier prepared in Example 1 after being stored for different time periods. DETAILED DESCRIPTION

[0037] The present invention is further described below in conjunction with the embodiments, which can enable those skilled in the art to more fully understand the present invention, but does not limit the present invention in any way. Embodiment 1:

[0038] The present invention provides a method for preparing a reusable coating carrier, which specifically comprises the following preparation steps:

[0039] Step 1:

[0040] The carbon felt was immersed in a mixed acid solution of H2SO4-HNO3, H2SO4: HNO3: H2O = 1.2:0.9:3.4, the treatment time was 1h, and the temperature was room temperature. After taking it out, it was washed with ultrapure water until the pH of the washing solution was neutral, and then dried at 60°C. Then, the surface of the carbon felt was defunctionalized with a NaOH solution with a concentration of 3 mol / L, and assisted by ultrasound, the treatment time was 1h, and the temperature was room temperature. After taking it out, it was washed with ultrapure water until the pH of the washing solution was neutral, and then dried at 60°C to obtain a surface passivated carbon felt;

[0041] Step 2:

[0042] The surface passivated carbon felt was fixed on the cathode titanium electrode. The electrolyte was a mixed acidic solution of NiSO4 and CoSO4 with concentrations of 0.9 mol / L and 0.4 mol / L, respectively. The anode was a nickel electrode with a current density of -90 mA / cm 2 , turn on magnetic stirring. After completion, wash with ultrapure water, anhydrous ethanol, and acetone in turn, and finally dry. The drying temperature is 60°C and the time is 12 h. A reusable coating carrier is prepared.

[0043] Coating performance test steps: After the coated substrate is left to stand and cleaned and dried, the initial test of the water contact angle is performed and the result is recorded as the initial angle. Then, the friction resistance test is performed using rubber and steel wool respectively. The number of rubber frictions is 8k times, and the number of steel wool frictions is 5k (steel wool is replaced after 1k frictions). After the test is completed, the water contact angle is recorded again. The test results show that compared with the traditional steel wool carrier, the coating carrier does not affect the coating performance.

[0044] The film-coated carrier obtained in Example 1 was used in the evaporation experiment. The initial contact angle of the film-coated substrate and the contact angle after being rubbed with rubber for 8000 times and steel wool for 5000 times are shown in Table 1:

[0045] Table 1. Contact angles of coated substrates under different experimental conditions

[0046]

[0047] The surface morphology and surface crystal structure of the above-mentioned coated carrier were analyzed by SEM and XRD, and the results are as follows: Figure 1 , Figure 2 and Figure 3 As shown. Figure 1 and Figure 2 It can be seen that the coating carrier shows a three-dimensional fiber mesh structure, and a dense metal layer is evenly loaded on its surface. Figure 3It can be seen that the coating carrier successfully loaded the Ni-Co alloy layer. Embodiment 2:

[0048] Compared with Example 1, the only difference is that the mixed acid solution of H2SO4-HNO3 is replaced by H2SO4 solution, H2SO4: H2O = 2.1:3.4, and then the same steps are used to prepare the coating carrier.

[0049] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1. Embodiment 3:

[0050] Compared with Example 1, the only difference is that the 3 mol / L NaOH solution is replaced by a 3 mol / L KOH solution, and then the coating carrier is prepared by the same steps.

[0051] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1. Embodiment 4:

[0052] Compared with Example 1, the only difference is that the electrolyte, which is a mixed acidic solution of NiSO4 and CoSO4, is replaced with a mixed acidic solution of NiSO4 and FeSO4, and then the same steps are used to prepare the coating carrier.

[0053] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1. Embodiment 5:

[0054] Compared with Example 1, the only difference is that the drying time is adjusted from 12 h to 6 h, and then the coating carrier is prepared by the same steps.

[0055] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1. Embodiment 6:

[0056] The material of Example 1 was recovered, rinsed with anhydrous ethanol and dried, and the coating experiment was carried out again in the manner of Example 1, and this was repeated 5 times to explore its cyclic stability performance. The initial contact angle of the coated substrate and the contact angle after 8000 times of rubber friction and 5000 times of steel wool friction are shown in Figure 1. Figure 4 shown. Embodiment 7:

[0057] The film-coated carrier obtained in Example 1 was stored in a room temperature environment for 1, 10, 20, 40, 60 and 90 days, and then the film-coating experiment was carried out again. After completion, the initial contact angle of the film-coated substrate and the contact angle after being rubbed with rubber for 8000 times and steel wool for 5000 times were tested. The results are as follows: Figure 5 shown.

[0058] Comparative Example 1:

[0059] Compared with Example 1, the difference is that no acid solution treatment is performed, and ultrapure water is used to clean and dry the product directly, and the same preparation steps are used for subsequent preparation.

[0060] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1.

[0061] Comparative Example 2:

[0062] Compared with Example 1, the difference is that after the acid solution treatment, no alkaline solution treatment is performed, and ultrasound is directly performed in ultrapure water for 1 hour, and then the preparation is carried out according to the same subsequent steps.

[0063] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1.

[0064] Comparative Example 3:

[0065] Compared with Example 1, the difference is that no electrodeposition operation is performed after the ultrasonic-assisted acid-base etching, and the surface is directly cleaned with ultrapure water, anhydrous ethanol, and acetone, and then dried.

[0066] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1.

[0067] Comparative Example 4:

[0068] Compared with Example 1, the difference is that after the electrodeposition is completed and the ultrapure water, anhydrous ethanol and acetone are used for cleaning, the oven drying treatment is not performed, but it is dried in a natural environment.

[0069] The coating experiment was carried out in the manner of Example 1. The initial contact angle of the coated substrate and the contact angle after being rubbed with rubber for 8000 times and with steel wool for 5000 times are shown in Table 1.

[0070] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing a reusable coating carrier, characterized in that: The following steps are involved: Step 1: The carbon felt is immersed in an acidic solution to etch the surface of the carbon felt, and then washed with ultrapure water until the pH of the washing solution is neutral, and dried at 60°C, and then the carbon felt is defunctionalized with an alkaline solution and assisted by ultrasound, and then washed with ultrapure water until the pH of the washing solution is neutral, and dried at 60°C to obtain a surface passivated carbon felt; Step 2: In a two-electrode system, the surface passivated carbon felt is fixed on the cathode electrode, and is electrodeposited in an electrolyte, and a uniform hydrophobic layer is attached under the action of magnetic stirring. After completion, it is washed with ultrapure water, anhydrous ethanol, and acetone in sequence, and finally dried; The acidic solution is one of H2SO4, HNO3, and H2SO4-HNO3; The ratios of the acidic solutions are respectively H2SO4: H2O = 0.5~2: 1~4, HNO3: H2O = 0.5~2: 1~4, H2SO4: HNO3: H2O = 0.5~2: 0.5~2: 1~4; The concentration of the alkaline solution is 1 mol / L to 5 mol / L.

2. The method for preparing a reusable coating carrier according to claim 1, characterized in that: The alkaline solution is one of NaOH and KOH.

3. The method for preparing a reusable coating carrier according to claim 1, characterized in that: The anode in the dual-electrode system is one of metal nickel, iron and cobalt, and the cathode is metal titanium.

4. The method for preparing a reusable coating carrier according to claim 1, characterized in that: The electrolyte includes an acidic salt solution of Ni, Fe and / or Co.

5. The method for preparing a reusable coating carrier according to claim 4, characterized in that: The acidic salt solution includes a sulfate and / or hydrochloride solution of metal Ni, Fe and / or Co.

6. The method for preparing a reusable coating carrier according to claim 1, characterized in that: The drying process in step 2 refers to drying at 60° C. for 6 to 18 hours.

7. Use of a reusable coating carrier prepared by the preparation method according to any one of claims 1 to 6 in vacuum evaporation coating.

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