Strong-adhesion super-hydrophobic coating and preparation method thereof

Abstract

The invention belongs to the field of biomimetic materials, and discloses a strong-adhesion super-hydrophobic coating and a preparation method thereof.The strong-adhesion super-hydrophobic coating comprises flaky micro / nano structure crystal grains, the strong-adhesion super-hydrophobic coating comprises TixCyOz, X is equal to 1-1.67, y is equal to 1.33-2.33, and z is equal to 0.33-0.67. The high-adhesion super-hydrophobic coating is improved from the two aspects of the coating structure and the preparation process, the prepared high-adsorption super-hydrophobic coating material belongs to a metal oxycarbide material, bonding between crystal grains in the coating prepared through a chemical vapor deposition method belongs to metallurgical bonding, and compared with a traditional high-molecular super-hydrophobic coating material, the high-adsorption super-hydrophobic coating material has the advantages that the high-adsorption super-hydrophobic coating material is more excellent in adsorption performance; and the coating has a series of advantages of strong adhesion, strong wear resistance, low cost, large-scale and large-area production and the like.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of biomimetic materials, and particularly relates to a strong-adhesion super-hydrophobic coating and a preparation method thereof. BACKGROUND

[0002] Global biological systems can be divided into two categories according to surface properties and interactions: the first category is a low-adhesion system, and the second category is a high-adhesion system. The low-adhesion system has the smallest adhesion and wettability, and a lotus leaf is a typical example, based on which researchers prepare a biomimetic super-hydrophobic surface. The high-adhesion system has a surface with high adhesion and friction. Due to the existence of surface adhesion, when the contact angle between a water droplet and a high-adhesion super-hydrophobic surface is greater than 150°, the water droplet is still adhered to the surface even if the surface is tilted by 90° or even 180°. The micro / nano-structured surface material developed based on the "rose petal" effect has the function of super-hydrophobicity and super-adhesion, and has the function of a "mechanical hand", which can realize the controllable transfer, transmission and collection of micro-liquid droplets, and thus plays an important role in micro-fluidic systems, liquid non-destructive transfer and biological engineering technology.

[0003] The existing high-adhesion super-hydrophobic surface material is mainly based on high molecular materials, and has defects such as insufficient adhesion (<60 μN), poor wear resistance, high cost, complex process, and difficulty in large-area preparation. It has very important research significance and application value to develop a high-adhesion super-hydrophobic surface material with strong adhesion, strong wear resistance, low cost and large-area production. In view of the above problems, it is necessary to provide a strong-adhesion super-hydrophobic coating and a preparation method thereof. SUMMARY

[0004] In order to overcome the defects of the prior art, the purpose of the present application is to provide a strong-adhesion super-hydrophobic coating and a preparation method thereof.

[0005] To achieve the above purpose, in a first aspect, the present application discloses a strong-adhesion super-hydrophobic coating, which comprises flaky micro / nano-structured grains, and the components of the strong-adhesion super-hydrophobic coating comprise Ti X C y O z , wherein X = 1-1.67, y = 1.33-2.33, and z = 0.33-0.67.

[0006] Further, the flaky micro / nano-structured grains are perpendicular to the surface of the substrate and interweave with each other, the surface of the flaky micro / nano-structured grains has wrinkles, and the edges of the flaky micro / nano-structured grains are curled.

[0007] Further, the length of the flaky micro / nano-structured grains is 400-900 μm, and the thickness is 160-220 nm.

[0008] Furthermore, the contact angle of the strong adhesion superhydrophobic coating is 150°-152.6°, the adhesion force is 10-15.4mN, and the average coefficient of friction is 0.15-0.35.

[0009] Secondly, this application discloses a method for preparing a strong adhesion superhydrophobic coating, comprising:

[0010] The substrate is placed inside the first vacuum chamber;

[0011] The carbon source is pre-decomposed in the second vacuum chamber to obtain gaseous carbon pre-decomposition products;

[0012] Gaseous carbon pre-decomposition products, titanium source, and oxygen source are introduced into the first vacuum chamber and vapor-phase deposition is performed on the surface of the substrate to obtain a strong adhesion superhydrophobic coating.

[0013] Furthermore, the substrate may include metal, ceramic, or carbon materials.

[0014] Furthermore, the carbon source includes methane, ethane, ethylene, propylene, or acetylene.

[0015] Furthermore, the titanium source includes titanium tetrachloride, titanium trichloride, or titanium dichloride.

[0016] Furthermore, the oxygen source includes oxygen, carbon dioxide, or carbon monoxide.

[0017] Furthermore, the carbon source is pre-decomposed, including:

[0018] At a vacuum degree of 10 -3 Pa-10 -2 In the second vacuum chamber, the resistance wire is heated to 600-800℃ at a rate of 10-30℃ / min. Then, a carbon source is introduced into the second vacuum chamber at a flow rate of 200-500 sccm for 5-20 min. During the reaction, the pressure in the second vacuum chamber is controlled at 1×10⁻⁶. 3 Pa-5×10 3 Pa yields gaseous carbon pre-decomposition products.

[0019] Further, gaseous carbon pre-decomposition products, a titanium source, and an oxygen source are introduced into the first vacuum chamber to perform vapor deposition on the surface of the substrate, including:

[0020] The first vacuum chamber was evacuated to a vacuum level of 1×10⁻⁶. -3 Pa-5×10 -3 After Pa, an inert gas is introduced;

[0021] The first vacuum chamber and the substrate are heated under inert gas conditions;

[0022] When the first vacuum chamber temperature is 550-650℃, the gaseous carbon source pre-decomposition product, the titanium source and the oxygen source are introduced into the first vacuum chamber, and the pressure of the first vacuum chamber is adjusted to 1x10Pa-8x10 2 Pa, and the vapor deposition is carried out on the substrate surface for 5-8h;

[0023] After the deposition is completed, the introduction of the gaseous carbon source pre-decomposition product, the titanium source and the oxygen source is stopped, the temperature is lowered to 400-450℃ and kept for 1-2h, and then the temperature is lowered to room temperature, thereby obtaining the strong-adhesion super-hydrophobic coating.

[0024] Further, the first vacuum chamber and the substrate are heated under the inert gas condition, including:

[0025] The temperature is raised to 500℃ at a speed of 5-10℃ / min, kept for 1-5h, and then raised to 550-650℃, kept for 0.5-2h.

[0026] Further, the gaseous carbon source pre-decomposition product, the titanium source and the oxygen source are introduced into the first vacuum chamber in sequence, including:

[0027] The flow rate of the gaseous carbon source pre-decomposition product introduced into the first vacuum chamber is controlled to be 200-500sccm;

[0028] The flow rate of the oxygen source introduced into the first vacuum chamber is controlled to be 50-100sccm;

[0029] The titanium source carried by the oxygen source is introduced into the first vacuum chamber at a flow rate of 100-200sccm.

[0030] Technical effects and advantages of the present application:

[0031] 1. The strong-adhesion super-hydrophobic coating is improved from the coating structure and the preparation process, and the prepared strong-adhesion super-hydrophobic coating material has a series of advantages such as strong adhesion, strong wear resistance, low cost and large-area production.

[0032] 2. The carbon source is pre-decomposed by the vacuum hot wire reaction method, which can improve the chemical reaction probability of the generated coating, help to further reduce the reaction temperature of the chemical vapor deposition process, and the pre-decomposed carbon source precursor has a high energy state and chemical activity, so that the energy required for the reaction is not provided by the conventional high-temperature process, thereby realizing the reaction of the titanium source and the oxygen source at a lower temperature to generate the super-hydrophobic coating material.

[0033] 3. The strong adsorption super-hydrophobic coating prepared by the application, which is composed of carbon, oxygen and titanium, belongs to metal carbon oxide material. The coating prepared by chemical vapor deposition has metallurgical combination between the crystal grains, and has significantly improved hardness and wear resistance compared with traditional polymer super-hydrophobic coating material. In addition, the strong adsorption super-hydrophobic coating material prepared by chemical vapor deposition process has the advantages of simple process, low cost and large-area preparation, which can effectively solve the defects of current polymer super-hydrophobic material such as insufficient adhesion (<60 μN), poor wear resistance, high cost, complex process and difficult large-area preparation.

[0034] Other features and advantages of the present application will be set forth in the following description, and in part will become apparent from the description, or can be learned by practice of the present application. The objects and other advantages of the present application will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings. BRIEF DESCRIPTION OF DRAWINGS

[0035] Figure 1 SEM (scanning electron microscope) test chart of the strong adhesion super-hydrophobic coating prepared for Example 1;

[0036] Figure 2 EDS (X-ray energy spectrum analysis) test chart of the strong adhesion super-hydrophobic coating prepared for Example 1;

[0037] Figure 3 Average friction coefficient test chart of the strong adhesion super-hydrophobic coating prepared for Example 1;

[0038] Figure 4 Static contact angle test chart of the strong adhesion super-hydrophobic coating prepared for Example 1;

[0039] Figure 5 Photo of the adhesion effect of the strong adhesion super-hydrophobic coating prepared for Example 1 on water droplets;

[0040] Figure 6 Test chart of the adhesion force between the strong adhesion super-hydrophobic coating prepared for Example 1 and water droplets. DETAILED DESCRIPTION

[0041] The technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0042] In a first aspect, the present application discloses a strong-adhesion super-hydrophobic coating, comprising flaky micro / nano-structured grains, the flaky micro / nano-structured grains being perpendicular to the surface of a substrate and interwoven with each other, the surface of the flaky micro / nano-structured grains being corrugated, the edge of the flaky micro / nano-structured grains being curled, the length of the flaky micro / nano-structured grains being 400-900 μm, for example, 400 μm, 500 μm, 600 μm, 700 μm, 800 μm, 900 μm, and the thickness of the flaky micro / nano-structured grains being 160-220 nm, for example, 160 nm, 170 nm, 180 nm, 190 nm, 200 nm, 210 nm, 220 nm. The components of the strong-adhesion super-hydrophobic coating comprise Ti X C y O z , wherein X = 1-1.67, y = 1.33-2.33, and z = 0.33-0.67, preferably, X = 1.17-1.33, y = 1.5-1.67, and z = 0.4-0.6. The contact angle of the strong-adhesion super-hydrophobic coating is 150°-152.6°, for example, 150.5°, 151°, 151.5°, 152°, or 152.6°, the adhesion is 10-15.4 mN, for example, 10 mN, 11 mN, 12 mN, 13 mN, 14 mN, 15 mN, or 15.4 mN, and the average friction coefficient is 0.15-0.35, for example, 0.15, 0.2, 0.25, 0.3, or 0.35.

[0043] In a second aspect, the present application discloses a method for preparing a strong-adhesion super-hydrophobic coating, comprising:

[0044] 1. Placing a substrate in a first vacuum chamber:

[0045] The first vacuum chamber is used as a reaction site for chemical vapor deposition, and a metal, ceramic, or carbon material substrate surface is polished, impurity-removed, cleaned, and dried before being placed in the first vacuum chamber for standby.

[0046] 2. Pre-decomposing a carbon source in a second vacuum chamber to obtain a gaseous carbon pre-decomposition product;

[0047] The vacuum degree is 10 -3 Pa-10 -2The resistance wire in the second vacuum chamber of Pa is heated at a rate of 10-30℃ / min (for example, 10℃ / min, 15℃ / min, 20℃ / min, 25℃ / min or 30℃ / min) to 600-800℃ (for example, 600℃, 650℃, 700℃, 750℃ or 800℃), and then methane, ethane, ethylene, propylene or acetylene is introduced into the second vacuum chamber at a flow rate of 200-500sccm (for example, 200sccm, 300sccm, 400sccm or 500sccm) for 5-20min (for example, 5min, 8min, 10min, 15min, 18min or 20min), preferably methane or propylene, and the pressure in the second vacuum chamber during the reaction is 1×10 3 Pa-5×10 3 to obtain gaseous carbon pre-decomposition products.

[0048] It should be noted that, on the one hand, if the carbon source is not pre-decomposed, under the subsequent oxygen source introduction condition, the oxygen source will first react with the undecomposed carbon source to generate CO2 and be discharged, reducing the reaction probability and degree with the titanium source, thereby resulting in the inability to form a strong adsorption super-hydrophobic coating material composed of a certain proportion of carbon, oxygen and titanium elements. Pre-decomposing the carbon source gas by the hot wire reaction method can improve the chemical reaction probability of generating the coating. On the other hand, the pre-decomposed carbon source precursor has a high energy state and chemical activity, which helps to further reduce the reaction temperature of the chemical vapor deposition process, thereby realizing the reaction with the titanium source and the oxygen source to generate the super-hydrophobic coating material at a lower temperature.

[0049] 3. Introducing the gaseous carbon pre-decomposition products, the titanium source and the oxygen source into the first vacuum chamber to perform vapor deposition on the surface of the substrate to obtain a strong adhesion super-hydrophobic coating:

[0050] The first vacuum chamber is evacuated to 1×10 -3 Pa-5×10 -3After the Pa, inert gas is introduced at 100-300 seem (for example, 100 seem, 150 seem, 200 seem, 250 seem or 300 seem) for 100-300 seconds, the first vacuum chamber and the substrate are heated under the condition of inert gas, heated to 500°C at a rate of 5-10°C / min (for example, 5°C / min, 6°C / min, 8°C / min, 9°C / min or 10°C / min), and kept for 1-5 hours, then heated to 550-650°C (for example, 550°C, 580°C, 600°C, 630°C or 650°C), and kept for 0.5-2 hours. When the temperature of the first vacuum chamber is 550-650°C, the gaseous carbon source pre-decomposition product is introduced into the first vacuum chamber at a flow rate of 200-500 seem, the flow rate of the oxygen source (oxygen, carbon dioxide and carbon monoxide) introduced into the first vacuum chamber is controlled at 50-100 seem (for example, 50 seem, 60 seem, 70 seem, 80 seem, 90 seem or 100 seem), and at the same time, the titanium source (heated titanium tetrachloride, titanium trichloride or titanium dichloride to be vaporized as the titanium source) is introduced into the first vacuum chamber at a flow rate of 100-200 seem (for example, 100 seem, 120 seem, 140 seem, 160 seem, 180 seem or 200 seem) through the oxygen source, and the pressure of the first vacuum chamber is adjusted to 1x10 Pa-8x10 2 Pa (for example, 10 Pa, 100 Pa, 200 Pa, 300 Pa, 400 Pa, 500 Pa, 600 Pa, 700 Pa or 800 Pa), and vapor deposition is carried out on the surface of the substrate for 5-8 hours. After the deposition is completed, the introduction of the gaseous carbon source pre-decomposition product, the titanium source and the oxygen source is stopped, the temperature is lowered to 400-450°C (for example, 400°C, 410°C, 420°C, 430°C, 440°C or 450°C) and kept for 1-2 hours, and then lowered to room temperature, thereby obtaining the strong adhesion super-hydrophobic coating.

[0051] It should be noted that, unlike the traditional polymer super-hydrophobic coating material, the strong adhesion super-hydrophobic coating composed of carbon, oxygen and titanium prepared by the chemical vapor deposition method belongs to the metal carbon oxide material, the combination between the crystal grains of the coating belongs to metallurgical combination, and the hardness and wear resistance of the coating are significantly improved. In addition, the chemical vapor deposition method for preparing the coating has the advantages of simple process, low cost and large-area preparation, which can effectively solve the defects of the current polymer super-hydrophobic material, such as insufficient adhesion (<60 μN), poor wear resistance, high cost, complex process and difficult large-area preparation. Furthermore, the oxygen source is introduced in the process of preparing the coating by the chemical vapor deposition method, the oxygen content in the coating is increased, which helps to improve the binding force between the coating and water molecules, thereby improving the adhesion of the super-hydrophobic coating to water and obtaining the strong adhesion effect.

[0052] To better illustrate the present scheme, the following examples and comparative examples are provided.

[0053] Example 1

[0054] S1: The substrate of ceramic, metal, carbon-based material, etc. is polished and cleaned, the surface is sandblasted with quartz sand, then polished, and then ultrasonic cleaned with alcohol. The cleaned substrate is dried in an oven and then placed in a chemical vapor deposition furnace for standby.

[0055] S2: Vacuumize the hot-wire chemical reaction vacuum chamber to a vacuum degree of 5x10 -3 Pa, turn on the power, heat the resistance wire to 770℃ at a heating rate of 15℃ / min, pass in propylene at 300sccm, and perform carbon source pre-decomposition reaction for 15min, controlling the pressure in the hot-wire chemical reaction vacuum chamber to be 3x10 3 Pa during the reaction.

[0056] S3: During the carbon source pre-decomposition reaction, keep the flow meter and valve between the hot-wire chemical reaction vacuum chamber and the chemical vapor deposition furnace chamber closed. Use a two-stage vacuum pump group to vacuumize the chemical vapor deposition furnace to 1x10 -3 Pa, then pass in argon at 200sccm, and start the furnace heating program, set the heating rate to 8℃ / min, heat to 500℃, and keep for 2 hours, then heat to 630℃ again, and keep for 1 hour.

[0057] S4: After the heat preservation is completed, open the one-way valve between the hot-wire chemical reaction vacuum chamber and the chemical vapor deposition chamber, control the gaseous carbon source pre-decomposition product gas flow from the hot-wire chemical reaction vacuum chamber to the chemical vapor deposition chamber to be 300sccm through the flow meter, and pass in carbon dioxide gas carrying 150sccm of vaporized titanium trichloride at 80sccm, adjust the reaction pressure in the chemical vapor deposition chamber to be 5x10 2 Pa by the vacuum pump, and the reaction time is 6h and the reaction temperature is 630℃.

[0058] S5: After the low-temperature chemical vapor deposition is completed, the chemical vapor deposition device enters the controllable cooling mode, stops passing in all gases, and cools down at a rate of 3℃ / min to 450℃, and keeps for 1.5h. After the heat preservation at 400-450℃ is completed, turn off the power, and automatically cool down to room temperature to obtain the strong adhesion super-hydrophobic coating material Ti 1.27 C 1.41 O 0.528 .

[0059] Figure 1 The SEM test diagram of the strong adhesion super-hydrophobic coating prepared in this example is shown inFigure 1 It can be seen that the strong-adhesion super-hydrophobic coating grains of Example 1 are sheet-shaped micro / nano structures perpendicular to the substrate surface, the sheet-shaped micro / nano grains interweave with each other, the length direction of the grains is in a crumpled shape, and the length is 600-700 μm; the thickness direction of the grains is in a curled shape, and the thickness is 180-200 nm; Figure 2 The EDS test result graph of the strong-adhesion super-hydrophobic coating prepared in this example is shown in Figure 4. Figure 2 It can be seen that the strong-adhesion super-hydrophobic coating of Example 1 contains carbon, oxygen and titanium elements. The molar content of carbon element is 42.20%, the molar content of oxygen element is 15.84%, and the molar content of titanium element is 38.09%; Figure 3 The average friction coefficient test graph of the strong-adhesion super-hydrophobic coating prepared in this example is shown in Figure 5. Figure 3 It can be seen that the average friction coefficient of the strong-adhesion super-hydrophobic coating of Example 1 is 0.15; Figure 4 The static contact angle test graph of the strong-adhesion super-hydrophobic coating prepared in this example is shown in Figure 6. Figure 4 It can be seen that the static contact angle of the strong-adhesion super-hydrophobic coating of Example 1 is 152.6°; Figure 5 The photo of the water droplet adhesion effect of the strong-adhesion super-hydrophobic coating prepared in this example is shown in Figure 7. Figure 6 The test result graph of the adhesion force between the strong-adhesion super-hydrophobic coating prepared in this example and the water droplet is shown in Figure 8. Figure 5 , 6 It can be seen that the strong-adhesion super-hydrophobic coating prepared in Example 1 has strong adsorption capacity to water droplets, and the adhesion force is 15.4 mN.

[0060] Example 2

[0061] The method is the same as that of Example 1, except that in step S2, the resistance wire is heated to 600°C.

[0062] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.32, the static contact angle is 150.6°, and the adhesion force to water droplets is 12.8 mN.

[0063] Example 3

[0064] The method is the same as that of Example 1, except that in step S2, the resistance wire is heated to 800°C.

[0065] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.28, the static contact angle is 151.2°, and the adhesion force to water droplets is 13.1 mN.

[0066] Example 4

[0067] The method is the same as that of Example 1, except that in step S2, the pressure in the hot wire reaction vacuum chamber during the reaction is controlled to be 1×10 3 Pa.

[0068] The strong adhesion superhydrophobic coating prepared in this embodiment has a friction coefficient of 0.20, a static contact angle of 151.2°, and an adhesion force to water droplets of 13.4 mN.

[0069] Example 5

[0070] The method is the same as in Example 1, except that in step S2, the pressure inside the hot filament reaction vacuum chamber is controlled to be 5 × 10⁻⁶. 3 Pa.

[0071] The strong adhesion superhydrophobic coating prepared in this embodiment has a friction coefficient of 0.17, a static contact angle of 152.2°, and an adhesion force to water droplets of 15.2 mN.

[0072] Example 6

[0073] The method is the same as in Example 1, except that in step S2, the carbon source is methane.

[0074] The strong adhesion superhydrophobic coating prepared in this embodiment has a friction coefficient of 0.28, a static contact angle of 150.1°, and an adhesion force to water droplets of 11.3 mN.

[0075] Example 7

[0076] The method is the same as in Example 1, except that in step S2, the carbon source pre-decomposition time is 5 min.

[0077] The strong adhesion superhydrophobic coating prepared in this embodiment has a friction coefficient of 0.20, a static contact angle of 150.4°, and an adhesion force to water droplets of 13.5 mN.

[0078] Example 8

[0079] The method is the same as in Example 1, except that in step S2, the carbon source pre-decomposition time is 20 min.

[0080] The strong adhesion superhydrophobic coating prepared in this embodiment has a friction coefficient of 0.18, a static contact angle of 151.8°, and an adhesion force to water droplets of 14.7 mN.

[0081] Example 9

[0082] The method is the same as in Example 1, except that: in step S3, when heated to 500°C, the temperature is held for 2 hours, and then the temperature is raised to 650°C again and held for 1 hour; in step S4, the reaction temperature of chemical vapor deposition is 650°C.

[0083] The strong adhesion superhydrophobic coating prepared in this embodiment has a friction coefficient of 0.20, a static contact angle of 151.5°, and an adhesion force to water droplets of 13.5 mN.

[0084] Example 10

[0085] The method is the same as example 1, except that in step S3, the temperature is heated to 500℃, and the temperature is kept for 2 hours, then the temperature is heated to 550℃ again, and the temperature is kept for 1 hour; in step S4, the reaction temperature of chemical vapor deposition is 550℃.

[0086] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.31, the static contact angle is 150.3°, and the adhesion force to water droplets is 11.5 mN.

[0087] Example 11

[0088] The method is the same as example 1, except that in step S4, the reaction pressure of chemical vapor deposition is 8x10 2 Pa.

[0089] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.23, the static contact angle is 151.4°, and the adhesion force to water droplets is 13.2 mN.

[0090] Example 12

[0091] The method is the same as example 1, except that in step S4, the reaction pressure of chemical vapor deposition is 1x10 2 Pa.

[0092] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.28, the static contact angle is 150.5°, and the adhesion force to water droplets is 12.3 mN.

[0093] Example 13

[0094] The method is the same as example 1, except that in step S3, the temperature is kept for 5 hours at 500℃.

[0095] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.18, the static contact angle is 152.2°, and the adhesion force to water droplets is 14.9 mN.

[0096] Example 14

[0097] The method is the same as example 1, except that in step S3, the temperature is kept for 1 hour at 500℃.

[0098] The friction coefficient of the strong-adhesion super-hydrophobic coating prepared in this example is 0.24, the static contact angle is 151.5°, and the adhesion force to water droplets is 13.3 mN.

[0099] Example 15

[0100] The method is the same as that in Example 1, except that in step S3, the holding time at 630℃ is 2h.

[0101] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.17, a static contact angle of 152.3°, and an adhesion to water droplets of 14.7mN.

[0102] Example 16

[0103] The method is the same as that in Example 1, except that in step S3, the holding time at 630℃ is 0.5h.

[0104] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.21, a static contact angle of 151.6°, and an adhesion to water droplets of 14.2mN.

[0105] Example 17

[0106] The method is the same as that in Example 1, except that in step S4, the oxygen source is oxygen.

[0107] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.20, a static contact angle of 150.3°, and an adhesion to water droplets of 13.8mN.

[0108] Example 18

[0109] The method is the same as that in Example 1, except that in step S4, the titanium source is titanium tetrachloride.

[0110] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.32, a static contact angle of 150.2°, and an adhesion to water droplets of 10.5mN.

[0111] Example 19

[0112] The method is the same as that in Example 1, except that in step S4, the carbon dioxide gas is introduced at 100sccm.

[0113] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.19, a static contact angle of 151.3°, and an adhesion to water droplets of 14.6mN.

[0114] Example 20

[0115] The method is the same as that in Example 1, except that in step S4, the carbon dioxide gas is introduced at 50sccm.

[0116] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.24, a static contact angle of 150.3°, and an adhesion to water droplets of 13.3mN.

[0117] Example 21

[0118] The method is the same as example 1, except that in step S4, carbon dioxide carrying 100 sccm vaporized titanium trichloride is introduced at a flow rate of 80 sccm.

[0119] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.25, a static contact angle of 150.2°, and an adhesion force to water droplets of 13.6 mN.

[0120] Example 22

[0121] The method is the same as example 1, except that in step S4, carbon dioxide carrying 200 sccm vaporized titanium trichloride is introduced at a flow rate of 80 sccm.

[0122] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.22, a static contact angle of 151.1°, and an adhesion force to water droplets of 14.1 mN.

[0123] Example 23

[0124] The method is the same as example 1, except that in step S4, the gaseous carbon source pre-decomposition product gas is introduced at a flow rate of 200 sccm.

[0125] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.21, a static contact angle of 151.4°, and an adhesion force to water droplets of 14.5 mN.

[0126] Example 24

[0127] The method is the same as example 1, except that in step S4, the gaseous carbon source pre-decomposition product gas is introduced at a flow rate of 500 sccm.

[0128] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.20, a static contact angle of 151.5°, and an adhesion force to water droplets of 14.3 mN.

[0129] Example 25

[0130] The method is the same as example 1, except that in step S2, 200 sccm propylene is introduced.

[0131] The strong-adhesion super-hydrophobic coating prepared in this example has a friction coefficient of 0.22, a static contact angle of 151.6°, and an adhesion force to water droplets of 14.6 mN.

[0132] Example 26

[0133] The method is the same as example 1, except that in step S2, 500 sccm propylene is introduced.

[0134] The strong-adhesion super-hydrophobic coating prepared in the example has a friction coefficient of 0.23, a static contact angle of 151.7°, and an adhesion force to water droplets of 14.2 mN.

[0135] Comparative Example 1

[0136] The method is the same as in Example 5, except that in step S2, the pressure in the hot-wire reaction vacuum chamber is controlled to be 5.5 x 10 3 Pa.

[0137] The strong-adhesion super-hydrophobic coating prepared in the example has a friction coefficient of 0.23, a static contact angle of 151.7°, and an adhesion force to water droplets of 14.2 mN.

[0138] Comparative Example 2

[0139] The method is the same as in Example 9, except that in step S3, the reaction temperature of chemical vapor deposition is 640°C.

[0140] The strong-adhesion super-hydrophobic coating prepared in the example has a friction coefficient of 0.23, a static contact angle of 151.7°, and an adhesion force to water droplets of 14.2 mN.

[0141] Comparative Example 3

[0142] The method is the same as in Example 19, except that in step S3, the carbon dioxide gas is introduced at 110 seem.

[0143] The strong-adhesion super-hydrophobic coating prepared in the example has a friction coefficient of 0.23, a static contact angle of 151.7°, and an adhesion force to water droplets of 14.2 mN.

[0144] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent replacements to some technical features, as long as they are within the spirit and principles of the present application. Any modification, equivalent replacement, improvement, etc. made within the scope of the present application should be included in the protection scope of the present application.

Claims

1. A strong adhesion superhydrophobic coating, characterized in that, The strong adhesion superhydrophobic coating comprises lamellar micro / nanostructured grains, and the composition of the strong adhesion superhydrophobic coating includes Ti. X C y O z Where X = 1 - 1.67, y = 1.33 - 2.33, and z = 0.33 - 0.

67.

2. The strong adhesion superhydrophobic coating according to claim 1, characterized in that, The sheet-like micro / nanostructure grains are perpendicular to the substrate surface and interwoven with each other. The surface of the sheet-like micro / nanostructure grains is wrinkled, and the edges of the sheet-like micro / nanostructure grains are curled.

3. The strong adhesion superhydrophobic coating according to claim 1, characterized in that, The length of the sheet-like micro / nanostructure grains is 400-900 μm and the thickness is 160-220 nm.

4. A strong adhesion superhydrophobic coating according to any one of claims 1-3, characterized in that, The strong adhesion superhydrophobic coating has a contact angle of 150°-152.6°, an adhesion force of 10-15.4 mN, and an average coefficient of friction of 0.15-0.

35.

5. A method for preparing a strong adhesion superhydrophobic coating according to any one of claims 1-4, characterized in that, include: The substrate is placed inside the first vacuum chamber; The carbon source is pre-decomposed in the second vacuum chamber to obtain gaseous carbon pre-decomposition products; The gaseous carbon pre-decomposition products, titanium source, and oxygen source are introduced into the first vacuum chamber, and vapor deposition is performed on the surface of the substrate to obtain a strong adhesion superhydrophobic coating.

6. The preparation method according to claim 5, characterized in that, The substrate may be a metal, ceramic or carbon material.

7. The preparation method according to claim 5, characterized in that, The carbon source includes methane, ethane, ethylene, propylene, or acetylene.

8. The preparation method according to claim 5, characterized in that, The titanium source includes titanium tetrachloride, titanium trichloride, or titanium dichloride.

9. The preparation method according to claim 5, characterized in that, The oxygen source includes oxygen, carbon dioxide, or carbon monoxide.

10. The preparation method according to claim 5, characterized in that, The pre-decomposition of the carbon source includes: At a vacuum degree of 10 -3 Pa-10 -2 In the second vacuum chamber, the resistance wire is heated to 600-800℃ at a rate of 10-30℃ / min. Then, a carbon source is introduced into the second vacuum chamber at a flow rate of 200-500 sccm for 5-20 minutes. During the reaction, the pressure in the second vacuum chamber is controlled at 1×10⁻⁶. 3 Pa-5×10 3 Pa yields gaseous carbon pre-decomposition products.

11. The preparation method according to any one of claims 5-10, characterized in that, The step of introducing the gaseous carbon pre-decomposition products, titanium source, and oxygen source into the first vacuum chamber and performing vapor deposition on the surface of the substrate includes: The first vacuum chamber was evacuated to a vacuum level of 1×10⁻⁶. -3 Pa-5×10 -3 After Pa, an inert gas is introduced; The first vacuum chamber and the substrate are heated under inert gas conditions; When the temperature of the first vacuum chamber is 550-650℃, gaseous carbon source pre-decomposition products, titanium source, and oxygen source are introduced into the first vacuum chamber, while the pressure of the first vacuum chamber is adjusted to 1×10 Pa-8×10 Pa. 2 Pa, perform vapor deposition on the substrate surface for 5-8 hours; After deposition, the gaseous carbon source pre-decomposition products, titanium source and oxygen source are stopped. The temperature is lowered to 400-450℃ and kept at that temperature for 1-2 hours before being cooled to room temperature to obtain a strong adhesion superhydrophobic coating.

12. The preparation method according to claim 11, characterized in that, The heating of the first vacuum chamber and the substrate under inert gas conditions includes: Heat to 500℃ at a rate of 5-10℃ / min, hold for 1-5 hours, then heat to 550-650℃ and hold for 0.5-2 hours.

13. The preparation method according to claim 11, characterized in that, The process of introducing gaseous carbon source pre-decomposition products, titanium source, and oxygen source into the first vacuum chamber includes: The flow rate of the gaseous carbon source pre-decomposition products into the first vacuum chamber is controlled to be 200-500 sccm; The flow rate of oxygen source into the first vacuum chamber is controlled to be 50-100 sccm; The titanium source is carried by the oxygen source into the first vacuum chamber, and the flow rate of the titanium source carried by the oxygen source is 100-200 sccm.

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