Inert carbon fiber felt coating carrier as well as preparation method and application thereof
By using carbon fiber felt and performing calcination passivation and hydrophobic layer adhesion, the problem of easy oxidation of steel wool coated carrier at high temperatures is solved, and the stability and reusability of carbon fiber felt coated carrier is achieved, reducing production costs and improving Coating performance.
Patent Information
- Application Number
- CN202411208321.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-30
- Publication Date
- 2024-12-06
AI Technical Summary
The existing steel wire wool coating carriers are prone to oxidation at high temperatures, resulting in chemical reactions, attenuation of performance, low production efficiency, high cost, and difficult to reuse.
Carbon fiber felt is used as the substrate, and the combination of carbon fiber felt and vapor deposition agent is improved through calcination passivation and hydrophobic layer adhesion, and an inert carbon fiber felt coating carrier is prepared to ensure its stability and reusability.
The carbon fiber felt coating carrier exhibits excellent stability and wear resistance in vacuum evaporation coating, with an initial contact angle of 115 to 118°, and remains above 110° after multiple frictions, and can be reused, reducing production costs.
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Figure CN119082663A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a carbon fiber felt coating carrier, in particular to an inert carbon fiber felt coating carrier and a preparation method and application thereof, belonging to the technical field of vacuum evaporation coating. Background Art
[0002] Vacuum coated pills are composed of two main parts: a specific potion and a carrier that can absorb the potion. The properties of the potion itself determine the wear resistance and weather resistance of the relevant coating, while the carrier directly determines the stability of the potion performance during the shelf life. Generally speaking, the pill carrier is prepared by a one-step pressing method using steel wool and a metal shell. Among them, steel wool is made by cutting steel. In the production process, in order to avoid oxidation of the steel wool material surface and cool the cutting knife under high temperature operation, some oil-containing emulsions are inevitably used. However, if this type of emulsion component cannot be well removed during the high-temperature impurity removal process, the emulsion may react uncontrollably with the potion during the storage of the product, resulting in the performance of the pills attenuation or even failure. In addition, due to the characteristics of steel wool, it is very easy to make the cotton cake uneven during the crucible pressing of the pills, affecting the film performance and resulting in low production efficiency. At the same time, the material of steel wool is low-carbon steel, which is prone to rust during storage. Importantly, after the evaporation is completed, the steel wool cannot be reused due to factors such as incomplete evaporation of the potential solution and deterioration of the steel wool, resulting in high production costs. Therefore, the market is in urgent need of a stable and reusable coating material carrier. Summary of the invention
[0003] In view of the problems existing in the prior art, the first object of the present invention is to provide an inert carbon fiber felt coating carrier. The coating carrier uses carbon fiber felt as a substrate, and effectively improves the bonding between the carbon fiber felt and the evaporation agent by passivation and attachment of a hydrophobic layer. The carbon fiber felt is stable in nature, not easily oxidized, and does not chemically react with the evaporation agent, which is convenient for long-term storage of the agent.
[0004] The second object of the present invention is to provide a method for preparing an inert carbon fiber felt coating carrier. The method modifies the carbon fiber felt by calcination passivation and over-volume impregnation, and greatly improves the bonding effect between the carbon fiber felt and the evaporation agent while ensuring the chemical properties of the carbon fiber felt are stable; the method has the advantages of simple process, low cost and high yield, and is convenient for large-scale industrial production.
[0005] The third purpose of the present invention is to provide an application of an inert carbon fiber felt coating carrier, which is used as a coating carrier for vacuum evaporation coating. Based on the excellent physical and chemical properties of the above-mentioned carbon fiber felt coating carrier, while ensuring the coating performance, the stability and reusability of the coating carrier are greatly improved; after testing, when the carbon fiber felt coating carrier provided by the present invention is used for vacuum evaporation, the initial contact angle of the coating substrate is 115-118°, and the contact angle is ≥110° when rubbed with rubber 8000 times and steel wool 5000 times, showing excellent technical effects, and after three cycles of use, the contact angle of the obtained coating substrate is still maintained above 110° when rubbed with rubber 8000 times and steel wool 5000 times.
[0006] In order to solve the above technical problems, the present invention provides a method for preparing an inert carbon fiber felt coating carrier, comprising: cleaning the carbon fiber felt, calcining and passivating it, and performing hydrophobic treatment in a reducing atmosphere in sequence to obtain the obtained product.
[0007] As a preferred solution, the carbon fiber felt is at least one of graphite-based carbon fiber felt, polyacrylonitrile-based carbon fiber felt and viscose-based carbon fiber felt.
[0008] As a preferred solution, the calcination passivation process is carried out in a mixed atmosphere of hydrogen and protective gas.
[0009] As a preferred solution, the protective atmosphere is at least one of argon, nitrogen and helium.
[0010] As a preferred solution, the volume fraction of hydrogen in the mixed atmosphere is 5-35%.
[0011] As a preferred solution, the calcination passivation conditions are: calcination temperature is 400-800°C, and calcination time is 1-3h.
[0012] As a preferred solution, the hydrophobic solution is 4-(heptadecafluorooctyl)aniline ethanol solution and / or hexadecyltrimethoxysilane ethanol solution.
[0013] As a preferred solution, the concentration of the 4-(heptadecafluorooctyl)aniline ethanol solution is 5-20 mM.
[0014] As a preferred solution, the mass percentage concentration of the hexadecyltrimethoxysilane ethanol solution is 2 to 20 wt %.
[0015] As a preferred solution, the process of impregnation with the hydrophobic solution is: immerse the calcined and passivated carbon fiber felt in the hydrophobic solution for 12 to 48 hours, then clean it with ethanol and dry it.
[0016] The present invention also provides an inert carbon fiber felt coating carrier obtained by any one of the preparation methods described above.
[0017] The present invention also provides an application of an inert carbon fiber felt coating carrier as a coating carrier for vacuum evaporation coating.
[0018] As a preferred solution, the process parameters of the vacuum evaporation coating include: plasma treatment for 1 to 5 minutes, voltage 65 to 68V, current 2.5 to 3A; electron gun preheating power 10% to 15%, silicon plating 10 to 14nm, turntable rotation 99.9%. Further preferably, the process parameters of the vacuum evaporation coating include: plasma treatment for 3 minutes, voltage 65 to 68V, current 2.5 to 3A; electron gun preheating power 10% to 15%, silicon plating 12nm, turntable rotation 99.9%.
[0019] As a preferred solution, in the vacuum evaporation coating process, the voltage ratio of the three sections A:B:C is 20.5%:22.1%:22.1%.
[0020] Compared with the prior art, the beneficial technical effects of the technical solution of the present invention are:
[0021] 1) The coating carrier provided by the present invention uses carbon fiber felt as a matrix, and effectively improves the bonding effect between the carbon fiber felt and the evaporation agent by passivation and attachment of a hydrophobic layer. The carbon fiber felt is stable in nature, not easily oxidized, and does not chemically react with the evaporation agent, which is convenient for long-term storage of the agent;
[0022] 2) In the preparation method provided by the present invention, the carbon fiber felt is modified by calcination passivation and over-volume impregnation, and the bonding effect between the carbon fiber felt and the evaporation agent is greatly improved under the premise of ensuring the chemical properties of the carbon fiber felt are stable; the method has the advantages of simple process, low cost and high yield, and is convenient for large-scale industrial production;
[0023] 3) In the technical solution provided by the present invention, based on the excellent physical and chemical properties of the above-mentioned carbon fiber felt coating carrier, while ensuring the coating performance, the stability and reusability of the coating carrier are greatly improved; after testing, when the carbon fiber felt coating carrier provided by the present invention is used for vacuum evaporation, the initial contact angle of the coating substrate is 115-118°, and the contact angle is ≥110° when rubbed with rubber 8000 times and steel wool 5000 times, showing excellent technical effects, and after three cycles of use, the contact angle of the obtained coating substrate is still maintained above 110° when rubbed with rubber 8000 times and steel wool 5000 times. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] Figure 1 This is the SEM image of the film-coated carrier prepared in Example 1;
[0025] Figure 2 The XRD pattern of the film-coated carrier prepared in Example 1;
[0026] Figure 3 A schematic diagram of the cycle experiment results of the coating carrier prepared in Example 6;
[0027] Figure 4 This is a schematic diagram of the cycle test results of the steel wool crucible in Comparative Example 4. DETAILED DESCRIPTION
[0028] 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.
[0029] Example 1
[0030] Step 1): The polyacrylonitrile-based carbon fiber felt is first soaked in anhydrous ethanol for cleaning to remove surface dust and unadhered carbon fibers, and then dried;
[0031] Step 2): Place the carbon felt in a tube furnace and place in an argon / hydrogen atmosphere (VAr / VH2 = 90 mL min -1 / 10mL·min -1 ) atmosphere at 700°C for 1.5h, and then washed and dried with anhydrous ethanol to obtain a passivated carbon fiber felt;
[0032] Step 3): The passivated carbon fiber felt is immersed in an ethanol solution of 4-(heptadecafluorooctyl)aniline at a concentration of 15 mM to attach a hydrophobic layer. The immersion time is 16 hours. After being taken out, it is washed with anhydrous ethanol and dried to prepare a new coating carrier.
[0033] Then, the above-mentioned new coating carrier was used for evaporation experiment, and the evaporation process parameters were: plasma treatment for 3 minutes, voltage 65-68V, current 2.5-3A; electron gun preheating power 10%-15%, silicon plating 12nm, turntable rotation 99.9%, evaporation A: B: C three-stage voltage ratio of 20.5%: 22.1%: 22.1%. After completion, 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 Table 1.
[0034] Example 2
[0035] This embodiment is exactly the same as the embodiment 1, the difference being that only the polyacrylonitrile carbon fiber felt is changed to a viscose-based carbon fiber felt.
[0036] 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.
[0037] Example 3
[0038] This example is exactly the same as Example 1, except that only argon / hydrogen (VAr / VH2 = 90 mL·min -1 / 10mL·min -1 ) was changed to nitrogen / hydrogen (VAr / VH2=90mL·min -1 / 10mL·min -1 ).
[0039] 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.
[0040] Example 4
[0041] This example is exactly the same as Example 1, except that only argon / hydrogen (VAr / VH2 = 90 mL·min -1 / 10mL·min -1 ) was changed to argon / hydrogen (VAr / VH2 = 80 mL min -1 / 20mL·min -1 ).
[0042] 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.
[0043] Example 5
[0044] This example is exactly the same as Example 1, except that the 15 mM 4-(heptadecafluorooctyl)aniline ethanol solution is replaced with a 10 wt % hexadecyltrimethoxysilane ethanol solution, and the immersion time is 24 h.
[0045] 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.
[0046] Example 6
[0047] The material of Example 1 was recovered, rinsed with anhydrous ethanol and dried, and the coating experiment was carried out again in the same manner as in Example 1, and this was repeated twice to explore its cyclic stability. 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 3 shown.
[0048] Comparative Example 1
[0049] This embodiment is exactly the same as the embodiment 1, except that the high-temperature calcination treatment is not performed in a pure argon atmosphere containing hydrogen, and the subsequent preparation is performed according to the same steps.
[0050] 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.
[0051] Comparative Example 2
[0052] This example is exactly the same as Example 1, except that the immersion treatment in the 15 mM 4-(heptadecafluorooctyl)aniline ethanol solution is not performed, but the immersion is directly performed in anhydrous ethanol solution, and the subsequent preparation is performed according to the same steps.
[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.
[0054] Comparative Example 3
[0055] A conventional steel wool crucible was used to replace the inert carbon fiber felt crucible, and a coating experiment was performed 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.
[0056] Comparative Example 4
[0057] The steel wool crucible in Comparative Example 3 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 twice to explore its cyclic stability. 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.
[0058] Table 1. Contact angles of the coated substrates obtained in Examples 1 to 5 and Comparative Examples 1 to 3
[0059]
[0060] It can be seen from Table 1 that the initial angles of the evaporation experiments conducted using the inert carbon fiber felts provided in Examples 1 to 5 of the present invention are all above 115°. After being rubbed with rubber 8,000 times or rubbed with steel wool 5,000 times, the contact angles are still maintained above 110°, showing good hydrophobicity and wear resistance. Comparative Examples 1 and 2 lack the calcination treatment and the impregnation treatment with a hydrophobic solution during the preparation of the inert carbon fiber felts. When applied to the evaporation experiments, the initial angles decreased by 17% and 39%, respectively. After the friction experiment, the contact angle decreased by more than 34%, and the maximum decrease was 68%. This shows that only by strictly following the preparation method provided by the present invention and utilizing the synergistic effect of calcination passivation and impregnation with a hydrophobic solution can the corresponding technical objectives be achieved, and any changes in the process will lead to a decrease in the performance of the final product. In addition, the present invention also conducted multiple cyclic evaporation experiments using the inert carbon fiber felt in Example 1 of the present invention and the steel wool in Comparative Example 4, and the results are as follows. Figure 3 and Figure 4 shown; through Figure 3 and Figure 4 It can be seen that the contact angle retention rate of the inert carbon fiber felt provided in Example 1 is above 95% after three cycles of evaporation, while the contact angle of the steel wool provided in Comparative Example 4 shows an obvious downward trend after cyclic evaporation. After the third cycle, its contact angle is only 80% of the first cycle. This directly proves that the inert carbon fiber felt provided by the present invention has excellent recyclability and greatly reduces the comprehensive use cost of the evaporation carrier.
[0061] 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 an inert carbon fiber felt coating carrier, characterized in that: include: The carbon fiber felt is cleaned, calcined, passivated and hydrophobized in a reducing atmosphere to obtain the product.
2. The method for preparing an inert carbon fiber felt coating carrier according to claim 1, characterized in that: The carbon fiber felt is at least one of graphite-based carbon fiber felt, polyacrylonitrile-based carbon fiber felt and viscose-based carbon fiber felt.
3. The method for preparing an inert carbon fiber felt coating carrier according to claim 1, characterized in that: The calcination passivation process is carried out in a mixed atmosphere of hydrogen and protective gas; the protective atmosphere is at least one of argon, nitrogen and helium; the volume fraction of hydrogen in the mixed atmosphere is 5-35%.
4. The method for preparing an inert carbon fiber felt coating carrier according to claim 1, characterized in that: The calcination passivation conditions are: calcination temperature is 400-800° C., and calcination time is 1-3 hours.
5. The method for preparing an inert carbon fiber felt coating carrier according to claim 1, characterized in that: The hydrophobic solution is 4-(heptadecafluorooctyl)aniline ethanol solution and / or hexadecyltrimethoxysilane ethanol solution.
6. The method for preparing an inert carbon fiber felt coating carrier according to claim 5, characterized in that: The concentration of the 4-(heptadecafluorooctyl)aniline ethanol solution is 5 to 20 mM; the mass percentage concentration of the hexadecyltrimethoxysilane ethanol solution is 2 to 20 wt %.
7. The method for preparing an inert carbon fiber felt coating carrier according to claim 1, characterized in that: The process of impregnation with the hydrophobic solution is as follows: immersing the calcined and passivated carbon fiber felt in the hydrophobic solution for 12 to 48 hours, and then washing it with ethanol and drying it.
8. An inert carbon fiber felt coating carrier, characterized in that: Obtained by the preparation method according to any one of claims 1 to 7.
9. The use of an inert carbon fiber felt coating carrier according to claim 8, characterized in that: As a coating carrier, used for vacuum evaporation coating.
10. The use of an inert carbon fiber felt coating carrier according to claim 9, characterized in that: The process parameters of the vacuum evaporation coating include: plasma treatment for 1 to 5 minutes, voltage of 65 to 68V, current of 2.5 to 3A; electron gun preheating power of 10% to 15%, silicon coating of 10 to 14nm, and turntable rotation of 99.9%.