A method for effectively adjusting optical modulation of amorphous WO3 thin films

Abstract

The present invention discloses a method for effectively regulating the optical modulation of an amorphous WO3 thin film. The two ends of the prepared WO3 thin film are connected to a DC regulated power supply, and the optical modulation of the amorphous WO3 thin film product is regulated by changing the operating voltage. The method is simple and has low preparation cost. At the same time, the method can achieve effective regulation of the optical modulation without adversely affecting the surface morphology and microstructure of the amorphous WO3 thin film, and has broad application prospects.

Description

Technical Field

[0001] The invention belongs to the technical field of electrochromic thin film materials, and in particular relates to a method for effectively regulating optical modulation of an amorphous WO3 thin film. Background Art

[0002] WO3 is an important electrochromic material that can be used in architecture, transportation, aerospace and other fields. In practical applications, amorphous or non-crystalline WO3 thin films have better color change efficiency than crystalline WO3 thin films due to their loose structure, and therefore have been widely studied and applied.

[0003] Generally, the main indicators for evaluating the electrochromic performance of a material include color change efficiency, color change response time, color storage time, cycle life, etc. Among them, color change efficiency is the most important indicator of electrochromic materials. It can be described by the difference in transmittance between the maximum colored state and the faded state at a certain wavelength in the visible light band, namely optical modulation (OM). In addition to being related to its microstructure, the color change efficiency or optical modulation of the material is also closely related to the material's preparation process and post-processing methods. Therefore, it is very necessary to find an effective process method to effectively adjust the optical modulation or color change efficiency of amorphous WO3 thin films. Summary of the Invention

[0004] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of this application to avoid obscuring the purpose of this section, the abstract and the title of the invention, and such simplifications or omissions should not be used to limit the scope of the present invention.

[0005] In view of the above problems and / or the problems existing in the prior art, the present invention is proposed.

[0006] Therefore, the purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for effectively regulating the optical modulation of amorphous WO3 thin films.

[0007] In order to solve the above technical problems, the present invention provides the following technical solutions: comprising:

[0008] Amorphous WO3 thin films were prepared by magnetron sputtering using high-purity W target as target material and ITO conductive glass as substrate.

[0009] The two ends of the amorphous WO3 film are clamped with alligator clips of a DC regulated power supply, and power is applied. The optical modulation of the amorphous WO3 film is effectively adjusted by changing the working voltage of the power supply.

[0010] As a preferred embodiment of the method for effectively regulating the optical modulation of the amorphous WO3 thin film of the present invention, the amorphous WO3 thin film prepared by the magnetron sputtering method is realized by using a magnetron sputtering coating system, comprising:

[0011] The chamber of the magnetron sputtering coating system was vacuumed to 5.0×10 -3 After Pa, high-purity argon gas is introduced, the chamber pressure is adjusted through a high valve, and then the RF power supply is turned on and the power is adjusted, and sputtering deposition is carried out at room temperature.

[0012] As a preferred solution of the method for effectively regulating optical modulation of amorphous WO3 thin films according to the present invention, the gas pressure in the regulating chamber is adjusted to 0.3 Pa, the power is 100 W, and the deposition time is 1.5 h.

[0013] As a preferred solution of the method for effectively regulating optical modulation of amorphous WO3 thin film of the present invention, wherein: the amorphous WO3 thin film prepared by the magnetron sputtering method has an amorphous structure and a thickness of 100 nm.

[0014] As a preferred solution of the method for effectively regulating the optical modulation of the amorphous WO3 thin film of the present invention, the voltage resolution of the DC regulated power supply is 0.01V.

[0015] As a preferred solution of the method for effectively regulating the optical modulation of the amorphous WO3 thin film of the present invention, the current resolution of the DC regulated power supply is 0.001A.

[0016] As a preferred solution of the method for effectively regulating the optical modulation of the amorphous WO3 thin film of the present invention, the duration of the power-on treatment is 0.5 to 1.5 hours.

[0017] As a preferred solution of the method for effectively regulating the optical modulation of the amorphous WO3 thin film of the present invention, wherein: the operating voltage is 0-7V.

[0018] As a preferred solution of the method for effectively adjusting the optical modulation of the amorphous WO3 thin film of the present invention, the method for adjusting the optical modulation of the amorphous WO3 thin film is achieved by changing the optical transmittance of the amorphous WO3 thin film in the colored state and the faded state.

[0019] As a preferred solution of the method for effectively regulating optical modulation of amorphous WO3 thin films of the present invention, the method can achieve effective regulation of optical modulation without adversely affecting the surface morphology and microstructure of the amorphous WO3 thin film.

[0020] Beneficial effects of the present invention:

[0021] The present invention provides a method for effectively adjusting the optical modulation of an amorphous WO3 thin film. The two ends of the prepared WO3 thin film are connected to a DC regulated power supply. The optical modulation of the amorphous WO3 thin film product is adjusted by changing the operating voltage. The method is simple and the preparation cost is low.

[0022] The method of the present invention can achieve effective adjustment of optical modulation without adversely affecting the surface morphology and microstructure of the amorphous WO3 film, and has broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. Those skilled in the art can also derive other drawings based on these drawings without inventive effort. Among them:

[0024] Figure 1 This is a characterization and analysis result diagram of the optical modulation of the amorphous WO3 thin film in Example 1 of the present invention.

[0025] Figure 2 This is a characterization and analysis result diagram of the optical modulation of the amorphous WO3 thin film in Example 2 of the present invention.

[0026] Figure 3 This is a characterization and analysis result diagram of the optical modulation of the amorphous WO3 thin film in Example 3 of the present invention.

[0027] Figure 4 This is a characterization and analysis result diagram of the optical modulation of the amorphous WO3 thin film in Example 4 of the present invention.

[0028] Figure 5 These are SEM images of amorphous WO3 thin film samples processed in Examples 1 to 4 of the present invention.

[0029] Figure 6 Graph showing the optical modulation effects of amorphous WO3 thin films at different operating voltages in Examples 1 to 4 of the present invention. DETAILED DESCRIPTION

[0030] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification.

[0031] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0032] Secondly, the term "one embodiment" or "embodiment" herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in various places throughout this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive of other embodiments.

[0033] The magnetron sputtering coating system used in the present invention is a JGP500A magnetron sputtering coating system produced by Shenyang Keyou Vacuum Technology Co., Ltd.

[0034] The present invention characterizes and analyzes the optical modulation of the film through an electrochromic testing system.

[0035] The target material used in the present invention is a high-purity W target with a size of Purity 99.999%;

[0036] The substrate used in the present invention is ITO conductive glass: size 25×40×0.7 mm, resistance 3.5Ω / □.

[0037] Example 1

[0038] This embodiment provides a method for preparing an amorphous WO3 thin film. The following embodiments all use the amorphous WO3 thin film prepared in this embodiment as a research object.

[0039] Cleaning the ITO conductive glass substrate: Place the ITO conductive glass substrate in 99.5% analytical grade acetone, 99.7% analytical grade anhydrous ethanol, and deionized water with a resistivity of 18.2 MΩ-cm, respectively, and ultrasonically clean it for 15-20 minutes. Dry it and set it aside.

[0040] A high-purity W target and a cleaned ITO substrate were installed in the magnetron sputtering coating system, and the chamber was evacuated to 5.0×10 -3 After the pressure reaches 0.5 Pa, high-purity argon gas with a flow rate of 20 sccm and a purity of 99.999% is introduced, and the high valve is adjusted to maintain the chamber pressure at 0.3 Pa;

[0041] The radio frequency power supply was turned on and the power was adjusted to 100 W. The amorphous WO3 thin film sample with a thickness of 100 nm was obtained by sputtering deposition at room temperature for 1.5 h.

[0042] Figure 1 The optical modulation of the amorphous WO3 thin film obtained without power treatment in this embodiment is characterized and analyzed using an electrochromic test system. It can be seen that the optical modulation of the amorphous WO3 thin film obtained in this embodiment is 50%.

[0043] Example 2

[0044] Take the amorphous WO3 thin film sample prepared in Example 1, select a DC regulated power supply with a voltage resolution of 0.01V and a current resolution of 0.001A, use two alligator clips of the power supply to clamp the two ends of the amorphous WO3 thin film sample respectively, and power it on at a working voltage of 5V for 1h.

[0045] Figure 2 The optical modulation of the amorphous WO3 thin film obtained by the electrical treatment in this embodiment is characterized and analyzed using an electrochromic test system. It can be seen that the optical modulation of the amorphous WO3 thin film obtained in this embodiment is 15%.

[0046] Example 3

[0047] Take the amorphous WO3 thin film sample prepared in Example 1, select a DC regulated power supply with a voltage resolution of 0.01V and a current resolution of 0.001A, use two alligator clips of the power supply to clamp the two ends of the amorphous WO3 thin film sample respectively, and power it on at a working voltage of 6V for 1h.

[0048] Figure 3 The optical modulation of the amorphous WO3 thin film obtained by the electrical treatment in this embodiment is characterized and analyzed using an electrochromic test system. It can be seen that the optical modulation of the amorphous WO3 thin film obtained in this embodiment is 22%.

[0049] Example 4

[0050] Take the amorphous WO3 thin film sample prepared in Example 1, select a DC regulated power supply with a voltage resolution of 0.01V and a current resolution of 0.001A, use two alligator clips of the power supply to clamp the two ends of the amorphous WO3 thin film sample respectively, and power it on at a working voltage of 7V for 1h.

[0051] Figure 4 The optical modulation of the amorphous WO3 thin film obtained by the electrical treatment in this embodiment is characterized and analyzed using an electrochromic test system. It can be seen that the optical modulation of the amorphous WO3 thin film obtained in this embodiment is 48%.

[0052] Figure 5 These are SEM images of samples treated in Examples 1-4 of the present invention. Sample a is treated at a 5V operating voltage, sample b is treated at a 6V operating voltage, sample c is treated at a 7V operating voltage, and sample d is untreated. Compared to sample d, which is untreated, the samples treated at 5V and 6V have slightly finer particles, but no significant changes in surface morphology. The sample treated at 7V has even finer particles, and the film surface is smoother and denser.

[0053] Furthermore, the WO3 film still maintains an amorphous structure after the electrical treatment, which shows that the adjustment method of the present invention has no obvious adverse effects on the surface morphology, microstructure, etc. of the amorphous WO3 film, which is of great significance to the performance stability and service life of the amorphous WO3 film materials and devices.

[0054] Figure 6 The optical modulation effect of amorphous WO3 thin film under different working voltages in the embodiment of the present invention is shown in FIG. Figure 6 It can be seen that by adopting the adjustment method of the present invention, the optical modulation of the amorphous WO3 film can be reduced from 50% to 15%, or can be increased from 15% to 48% again, thereby achieving effective adjustment of the optical modulation.

[0055] At the same time, the effect of the galvanic treatment on the optical modulation of the amorphous WO3 thin film is not monotonic. When the voltage is less than 5V, the optical modulation decreases with increasing voltage; when the voltage is greater than 5V, the optical modulation increases with increasing voltage. This change in optical modulation is actually caused by a change in the optical transmittance between the stained and faded states. This change in optical transmittance may be due to two factors: first, the surface morphology of the film changes after the galvanic treatment, which also changes the reflectivity, absorptivity, and transmittance of the film; second, the density of the film changes after the galvanic treatment, which affects the injection and extraction of electrons and ions during electrochromism.

[0056] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.

Claims

1. A method for effectively adjusting the optical modulation of amorphous WO3 thin films, characterized by: include, Amorphous WO3 thin films were prepared by magnetron sputtering using high-purity W target as target material and ITO conductive glass as substrate. Use alligator clips of a DC regulated power supply to clamp the two ends of the amorphous WO3 film, apply power, and effectively adjust the optical modulation of the amorphous WO3 film by changing the working voltage of the power supply; The duration of the power-on treatment is 0.5 to 1.5 h, and the operating voltage is 0 to 7 V. When the operating voltage is <5 V, the optical modulation decreases with increasing voltage; When the operating voltage is >5 V, the optical modulation increases with the voltage; The method for adjusting the optical modulation of the amorphous WO3 film is achieved by changing the optical transmittance of the amorphous WO3 film in the colored state and the faded state, thereby achieving effective adjustment of the optical modulation without adversely affecting the surface morphology and microstructure of the amorphous WO3 film.

2. The method for effectively adjusting optical modulation of amorphous WO3 thin film according to claim 1, characterized in that: The magnetron sputtering method for preparing amorphous WO3 thin film is implemented by using a magnetron sputtering coating system, including: The chamber of the magnetron sputtering coating system was vacuumed to 5.0×10 -3 After Pa, high-purity argon gas is introduced, the chamber pressure is adjusted through a high valve, and then the RF power supply is turned on and the power is adjusted, and sputtering deposition is carried out at room temperature.

3. The method for effectively adjusting optical modulation of amorphous WO3 thin film according to claim 2, characterized in that: The chamber pressure was adjusted to 0.3 Pa, the power was 100 W, and the deposition time was 1.5 h.

4. The method for effectively adjusting optical modulation of an amorphous WO3 thin film according to claim 1 or 2, characterized in that: The amorphous WO3 film prepared by the magnetron sputtering method has an amorphous structure and a thickness of 100 nm.

5. The method for effectively adjusting optical modulation of amorphous WO3 thin film according to claim 1, characterized in that: The voltage resolution of the DC regulated power supply is 0.01 V.

6. The method for effectively adjusting optical modulation of amorphous WO3 thin film according to claim 1, characterized in that: The current resolution of the DC regulated power supply is 0.001 A.

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