Preparation method of coating film system with electrically-driven infrared shielding thermal regulation and control function

Abstract

The invention discloses a preparation method of a coating film system with an electrically-driven infrared shielding heat regulation function, and relates to the technical field of functional film preparation glass deep processing, and the preparation method comprises the following steps: S1, coating by adopting a magnetron sputtering method, vacuumizing a magnetron sputtering equipment background to 10 <-6 > Torr, coating at 500-4000 W power, controlling Ar flow to be 100-500 sccm, introducing O2 with the flow of 2-15 sccm, and controlling the temperature to be 20-30 DEG C; preparing an ITO thin film by taking glass as a substrate, wherein the thickness of the prepared film is 50-600nm; according to the preparation method of the coating film system with the electrically-driven infrared shielding heat regulation and control function, the prepared film system can be intelligently regulated and controlled through direct-current voltage according to human needs, so that the film system has the transmission and shielding effects on visible light, and meanwhile, the infrared band can be effectively cut off, so that heat conduction is regulated and controlled, and the heat conduction efficiency is improved. And the method has a huge application prospect in the fields of green buildings and intelligent automobiles.

Description

Technical Field

[0001] The present invention relates to the technical field of glass deep processing for preparing functional thin films, and in particular to a method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function. Background Art

[0002] Smart cars are developing towards electronic and intelligent directions, and the industry will continue to develop towards further high intelligence and modernization. However, smart cars still face some problems, such as a significant decrease in cruising range in summer and winter, insufficient charging infrastructure, and the sun shining through car windows in summer, making the car hot. The thermal management of the car cabin still needs to be improved. Smart cars have a great demand for controllable adjustment of cabin light and heat. Therefore, glass components that can perform light and heat regulation have become an important part of automotive intelligence and automotive energy conservation and emission reduction. The present invention provides a film system preparation technology with infrared light shielding and thermal regulation functions in the face of glass components for building energy conservation and automotive intelligence and energy conservation, which has important application value and prospects in the above-mentioned fields. Summary of the invention

[0003] In view of the deficiencies in the prior art, the present invention provides a method for preparing a coating film system with an electrically driven infrared shielding and thermal regulation function, which solves the problems in the above-mentioned background technology.

[0004] To achieve the above objectives, the present invention is implemented through the following technical solutions: A method for preparing a coating film system with an electrically driven infrared shielding heat regulation function, comprising the following steps:

[0005] S1. Use magnetron sputtering method to coat the film. The background vacuum of magnetron sputtering equipment is pumped to 10 -6 Torr, with a coating power of 500-4000W, an Ar flow rate of 100-500sccm, and an O2 flow rate of 2-15sccm, an ITO film is prepared on a glass substrate with a film thickness of 50-600nm;

[0006] S2. A WO3 thin film is further prepared on the ITO film layer prepared above, using metal W as a sputtering target, adopting a reactive sputtering method, with a sputtering power of 600-3000 W, an Ar flow rate of 100-500 sccm, and an O2 flow rate of 10-60 sccm, to prepare a film with a thickness of 100-600 nm;

[0007] S3, on the basis of the WO3 prepared in the above step, continue to prepare an ITO film in the same manner as step S1, with a thickness of 10-100 nm to obtain the desired film system;

[0008] S4. Placing the film system prepared in step S3 in a liquid electrolyte, using ITO as an electrode, and applying a certain voltage to obtain a coating film system with infrared heat shielding properties.

[0009] Preferably, the ITO film is prepared in step S1 by using ceramic ITO as a sputtering target, using direct current or radio frequency sputtering, and heating at room temperature or substrate, with a heating temperature of 100-400°C.

[0010] Preferably, in step S4, the voltage is a direct current of 0.5-5V, and the liquid electrolyte is one of a LiClO4 solution, a NaCl solution and a KOH solution.

[0011] Preferably, the magnetron sputtering equipment in step S1 includes an electrical control box and a sputtering tube, a sealing cover is provided on the top of the sputtering tube, and a target electrode is fixedly provided on the bottom of the sealing cover, convex plates are fixedly connected to both sides of the target electrode, and the bottom of the target electrode is connected to the sputtering target material through a locking assembly.

[0012] Preferably, the locking assembly includes a first bent plate and a second bent plate fixed on the top of the sputtering target, the first bent plate passes through to the outside of the convex plate and is provided with a movable groove on one side, and a spring is fixedly connected to the inner wall of the movable groove, one end of the spring is fixedly connected to a fixing rod, and the second bent plate passes through to the outside of the convex plate and is provided with a slot matching the fixing rod on one side.

[0013] Preferably, a fixing seat is fixedly connected to the bottom of the sputtering cylinder, and a motor is fixedly connected to the bottom of the inner wall of the fixing seat, and a coating seat is provided at the output end of the motor.

[0014] Preferably, clamping assemblies are provided on both sides of the top of the coating seat, and the clamping assemblies include an L-shaped clamping plate slidably arranged on the top of the coating seat, and the top of the L-shaped clamping plate is threadedly connected with an adjusting bolt.

[0015] Preferably, a threaded hole matching the adjusting bolt is formed on the top of the coating seat.

[0016] The present invention provides a method for preparing a coating film system with an electrically driven infrared shielding and heat regulation function. It has the following beneficial effects:

[0017] (1) The method for preparing a coating film system with an electrically driven infrared shielding and heat regulation function can intelligently regulate the film system through a DC voltage according to human needs, so that it can produce a transparent and shielding effect on visible light, and can effectively cut off the infrared band, thereby regulating heat conduction. It has great application prospects in the fields of green buildings and smart cars.

[0018] (2) In the method for preparing a coating film system with an electrically driven infrared shielding thermal regulation function, when magnetron sputtering is performed on the film system, the sputtering target is connected to the target electrode through a locking assembly. The installation is simple and quick, and the sputtering target can be quickly disassembled and replaced, thereby improving the work efficiency during film preparation.

[0019] (3) In the method for preparing a coating film system with an electrically driven infrared shielding and heat regulation function, the glass substrate is limited on the coating seat by a clamping assembly, and the clamping assembly can adjust the position according to glass substrates of different sizes by setting an adjusting bolt. The coating seat is flexible to use, and the glass substrate can be driven to rotate to ensure uniform deposition of the thin film. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A schematic diagram of the structure of the magnetron sputtering equipment of the present invention;

[0021] Figure 2 It is a cross-sectional view of the sputtering tube structure of the present invention;

[0022] Figure 3 It is a schematic diagram of the installation of the locking assembly structure of the present invention;

[0023] Figure 4 is a cross-sectional view of the locking assembly structure of the present invention;

[0024] Figure 5 The SEM scanning cross-sectional morphology of a typical sample prepared in the present invention;

[0025] Figure 6 Spectral transmittance graphs of typical samples in the transmission state and light shielding state are prepared for the present invention.

[0026] In the figure: 1. magnetron sputtering equipment; 101. electric control box; 102. sputtering tube; 2. sputtering target; 3. sealing cover; 4. target electrode; 5. convex plate; 6. first bending plate; 7. second bending plate; 8. movable groove; 9. spring; 10. fixing rod; 11. slot; 12. fixing seat; 13. motor; 14. coating seat; 15. L-shaped clamp; 16. adjusting bolt; 17. threaded hole. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] Embodiment 1

[0029] The present invention provides a method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function, comprising the following steps:

[0030] S1. Use magnetron sputtering method to coat the film. The background vacuum of magnetron sputtering equipment 1 is pumped to 10 -6 Torr, using a DC room temperature sputtering method, with a coating power of 500-4000W, an Ar flow rate of 100-500sccm, and an O2 flow rate of 2-15sccm, using glass as a substrate and ceramic ITO as a sputtering target to prepare an ITO film with a film thickness of 50-600nm;

[0031] S2, further preparing a WO3 thin film on the above-prepared ITO film layer, using metal W as the sputtering target 2, adopting a reactive sputtering method, with a sputtering power of 600-3000W, an Ar flow rate of 100-500sccm, and introducing O2 with a flow rate of 10-60sccm, to prepare a film with a thickness of 100-600nm;

[0032] S3, on the basis of the WO3 prepared in the above step, continue to prepare an ITO film in the same manner as step S1, with a thickness of 10-100 nm to obtain the desired film system;

[0033] S4. Place the film system prepared in step S3 in a LiClO4 liquid electrolyte, use ITO as an electrode, and apply a 0.5-5V DC voltage to obtain a coating film system with infrared heat shielding properties.

[0034] Embodiment 2

[0035] S1. Use magnetron sputtering method to coat the film. The background vacuum of magnetron sputtering equipment 1 is pumped to 10 -6 Torr, using DC sputtering method, coating with 500-4000W power, Ar flow rate of 100-500sccm, O2 flow rate of 2-15sccm, glass as substrate, substrate heated to 100-400℃, ceramic ITO as sputtering target, prepare ITO film, the prepared film thickness is 50-600nm;

[0036] S2, further preparing a WO3 thin film on the above-prepared ITO film layer, using metal W as the sputtering target 2, adopting a reactive sputtering method, with a sputtering power of 600-3000W, an Ar flow rate of 100-500sccm, and introducing O2 with a flow rate of 10-60sccm, to prepare a film with a thickness of 100-600nm;

[0037] S3, on the basis of the WO3 prepared in the above step, continue to prepare an ITO film in the same manner as step S1, with a thickness of 10-100 nm to obtain the desired film system;

[0038] S4. Place the film system prepared in step S3 in a KOH liquid electrolyte, use ITO as an electrode, and apply a 0.5-5V DC voltage to obtain a coating film system with infrared heat shielding properties.

[0039] By the attached Figure 5 It can be seen that the film system prepared by the present invention has a clear film structure, the bottom layer 162nm and the upper layer 25nm are ITO thin films, and the middle layer is WO3. The film system is tested by spectrum, as shown in the attached Figure 6 As shown, the visible film system is in a cut-off state for both visible light and infrared parts in the light-shielding state, and in the film-transmitting state, that is, without affecting the visible light transmittance of the glass, it also has an obvious cut-off effect on the infrared band, which is of great significance for the subsequent preparation of thermal control devices based on this invention, such as green building energy-saving and emission-reduction glass, and thermal control glass components for new energy vehicles, which have potential demands for this invention.

[0040] Embodiment 3

[0041] In conjunction with Example 1 and Example 2, please refer to Figures 1 to 4 As shown, the specific improvements are as follows: the magnetron sputtering equipment 1 in step S1 includes an electric control box 101 and a sputtering tube 102 fixed on the top of the electric control box 101, a pipeline is also provided on the side of the sputtering tube 102, which can be connected to an external vacuum system for vacuuming the inside of the sputtering tube 102, a sealing cover 3 is provided on the top of the sputtering tube 102, and a target electrode 4 is fixedly provided at the bottom of the sealing cover 3, and convex plates 5 are fixedly connected to both sides of the target electrode 4, and the bottom of the target electrode 4 is connected to the sputtering target 2 through a locking assembly;

[0042] The locking assembly includes a first bent plate 6 and a second bent plate 7 fixed on the top of the sputtering target 2. The two sections of the first bent plate 6 and the second bent plate 7 are hinged and can rotate. The first bent plate 6 passes through one side of the outside of the convex plate 5 and is provided with a movable groove 8, and the inner wall of the movable groove 8 is fixedly connected with a spring 9, and one end of the spring 9 is fixedly connected with a fixing rod 10. The second bent plate 7 passes through one side of the outside of the convex plate 5 and is provided with a slot 11 that matches the fixing rod 10.

[0043] Through the setting of the above structure, the sputtering target 2 is connected to the target electrode 4 through the locking assembly. By pulling the fixing rod 10, the fixing rod 10 moves into the movable groove 8, squeezing the spring 9, and then the fixing rod 10 moves out of the slot 11, and then the first bending plate 6 and the second bending plate 7 are rotated upward by ninety degrees to move downward out of the convex plate 5. The sputtering target 2 and the target electrode 4 can be separated, which is convenient for quickly replacing different sputtering target materials 2 according to needs, thereby improving the work efficiency during film preparation.

[0044] Embodiment 4

[0045] In conjunction with Embodiments 1 to 3, please refer to Figure 2 As shown, the specific improvements are as follows: the bottom of the sputtering tube 102 is fixedly connected with a fixing seat 12, and the bottom of the inner wall of the fixing seat 12 is fixedly connected with a motor 13, and the output end of the motor 13 is provided with a coating seat 14;

[0046] Clamping assemblies are provided on both sides of the top of the coating seat 14, and the clamping assemblies include an L-shaped clamping plate 15 slidably arranged on the top of the coating seat 14, and the shape is adapted to the glass substrate. The top of the L-shaped clamping plate 15 is threadedly connected with an adjusting bolt 16, and the top of the coating seat 14 is provided with a threaded hole 17 adapted to the adjusting bolt 16. There are multiple threaded holes 17, which are convenient for the adjusting bolt 16 to fix the L-shaped clamping plate 15 at different positions.

[0047] Through the arrangement of the above structure, when in use, the sealing cover 3 is opened, and the glass substrate is placed on the coating seat 14. By moving the L-shaped clamping plate 15 to both sides of the glass substrate and screwing the adjusting bolts 16 into the corresponding threaded holes 17, the glass substrates of different sizes can be limited. The use is flexible. During magnetron sputtering, the motor 13 is started, and the coating seat 14 is driven to rotate through the rotating shaft. The coating seat 14 can drive the glass substrate to rotate to ensure uniform deposition of the thin film.

[0048] Meanwhile, the contents not described in detail in this specification belong to the prior art known to those skilled in the art, and the model parameters of each electrical appliance are not specifically limited, and conventional equipment compatible with the equipment can be used.

[0049] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function, characterized in that: The following steps are involved: S1. Use magnetron sputtering method to coat the film. The background vacuum of magnetron sputtering equipment (1) is evacuated to 10 -6 Torr, with a coating power of 500-4000W, an Ar flow rate of 100-500sccm, and an O2 flow rate of 2-15sccm, an ITO film is prepared on a glass substrate with a film thickness of 50-600nm; S2, further preparing a WO3 thin film on the above-prepared ITO film layer, using metal W as the sputtering target (2), adopting a reactive sputtering method, with a sputtering power of 600-3000W, an Ar flow rate of 100-500sccm, and an O2 flow rate of 10-60sccm, to prepare a film with a thickness of 100-600nm; S3, on the basis of the WO3 prepared in the above step, continue to prepare an ITO film in the same manner as step S1, with a thickness of 10-100 nm to obtain the desired film system; S4. Placing the film system prepared in step S3 in a liquid electrolyte, using ITO as an electrode, and applying a certain voltage to obtain a coating film system with infrared heat shielding properties.

2. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 1, characterized in that: In the step S1, the ITO film is prepared by using ceramic ITO as a sputtering target, using direct current or radio frequency sputtering, and heating at room temperature or substrate, with a heating temperature of 100-400°C.

3. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 1, characterized in that: In the step S4, the voltage is a direct current of 0.5-5V, and the liquid electrolyte is one of a LiClO4 solution, a NaCl solution and a KOH solution.

4. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 1, characterized in that: The magnetron sputtering equipment (1) in step S1 comprises an electric control box (101) and a sputtering tube (102), the top of the sputtering tube (102) is provided with a sealing cover (3), and the bottom of the sealing cover (3) is fixedly provided with a target electrode (4), both sides of the target electrode (4) are fixedly connected with a convex plate (5), and the bottom of the target electrode (4) is connected to the sputtering target material (2) through a locking assembly.

5. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 4, characterized in that: The locking assembly comprises a first bent plate (6) and a second bent plate (7) fixed on the top of the sputtering target (2); the first bent plate (6) is provided with a movable groove (8) on one side extending through the outside of the convex plate (5); a spring (9) is fixedly connected to the inner wall of the movable groove (8); one end of the spring (9) is fixedly connected to a fixing rod (10); the second bent plate (7) is provided with a slot (11) matching the fixing rod (10) on one side extending through the outside of the convex plate (5).

6. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 4, characterized in that: The bottom of the sputtering cylinder (102) is fixedly connected to a fixing seat (12), and the bottom of the inner wall of the fixing seat (12) is fixedly connected to a motor (13), and the output end of the motor (13) is provided with a coating seat (14).

7. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 6, characterized in that: Clamping assemblies are arranged on both sides of the top of the coating seat (14), and the clamping assembly comprises an L-shaped clamping plate (15) slidably arranged on the top of the coating seat (14), and an adjusting bolt (16) is threadedly connected to the top of the L-shaped clamping plate (15).

8. The method for preparing a coating film system with an electrically driven infrared shielding and heat regulating function according to claim 7, characterized in that: A threaded hole (17) adapted to the adjusting bolt (16) is provided on the top of the coating seat (14).

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