Cesium tungsten bronze thin film for near-infrared light shielding film and preparation method and application thereof

Abstract

The embodiment of the application discloses a cesium tungsten bronze film for near-infrared shielding film and a preparation method thereof. The method comprises the following steps: taking a cesium tungsten bronze target as a sputtering target, taking a planar substrate as a base, performing sputtering film coating in a magnetron sputtering device, obtaining the cesium tungsten bronze film on the base material, and performing heat treatment on the cesium tungsten bronze film to obtain the cesium tungsten bronze film for near-infrared shielding film. The heat treatment temperature is set to 200-450 DEG C. The heat treatment is performed on the base during the sputtering film coating process, and the heat treatment process is synchronous with the sputtering film coating process. Alternatively, the obtained cesium tungsten bronze film is subjected to heat treatment after the sputtering film coating is completed. The obtained high-quality cesium tungsten bronze film has high visible light transmittance, high near-infrared light blocking rate and high ultraviolet blocking rate, and can be used as the cesium tungsten bronze film for near-infrared shielding film. The cesium tungsten bronze film can also be made into a cesium tungsten bronze film-based composite film, and has a good application prospect in the field of near-infrared shielding film.

Description

Technical Field

[0001] This invention belongs to the field of magnetron sputtering thin film technology, specifically relating to cesium tungsten bronze thin films for near-infrared light shielding films and their preparation methods. Background Technology

[0002] With the continuous development of the global economy, the situation regarding energy consumption and environmental pollution is becoming increasingly severe. Building temperature control accounts for 36% of global energy consumption, making it one of the largest contributors to global energy consumption. More than half of the energy consumed in temperature control is used for facilities such as fans, air conditioners, and heating, but only 50% of the energy consumed by these facilities is effectively utilized. It is well known that indoor temperature mainly depends on solar radiation, which is primarily distributed in the 200-2500nm range. Ultraviolet (approximately 200-380nm), visible light (approximately 380-780nm), and near-infrared light (approximately 750-2500nm) account for 5%, 45%, and 50% of the total energy, respectively. Glass windows are the main channel for heat exchange between indoors and outdoors. If a type of glass could be invented that has high visible light transmittance while blocking ultraviolet and near-infrared light, it would be possible to shield a portion of solar radiation energy, significantly reducing energy consumption for cooling and heating.

[0003] Currently, the most studied near-infrared light shielding materials include indium tin oxide (ITO), lanthanum hexaboride (LaB6), vanadium dioxide (VO2), and tungsten bronze (M). x WO3). Cesium tungsten bronze (Cs) x WO3 has excellent physical and chemical properties, a wider near-infrared absorption region, higher near-infrared absorption intensity, and a simpler production process, making it the most promising material currently recognized.

[0004] However, it is not yet possible to prepare cesium tungsten bronze-based infrared shielding films with practical application prospects. Developing glass coating materials with low cost, simple process, stable performance, high visible light transmittance and high near-infrared light blocking rate is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0005] In view of this, some embodiments disclose a method for preparing a cesium tungsten bronze thin film for near-infrared shielding films. The method involves using a cesium tungsten bronze target as a sputtering target and a planar substrate as a base, performing sputtering deposition in a magnetron sputtering apparatus to obtain a cesium tungsten bronze thin film on the substrate material, and then heat-treating the cesium tungsten bronze thin film to obtain a cesium tungsten bronze thin film for near-infrared shielding films. The heat treatment temperature is set between 200 and 450°C.

[0006] Furthermore, in some embodiments, the method for preparing cesium tungsten bronze thin films for near-infrared shielding films discloses that the substrate is heated during the sputtering deposition process at a temperature of 200–450°C, and the heat treatment process is carried out simultaneously with the sputtering deposition process.

[0007] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, in which the obtained cesium tungsten bronze thin films are subjected to heat treatment after sputtering deposition.

[0008] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, wherein the cesium tungsten bronze target material is Cs. 0.20 WO3, Cs 0.30 WO3, Cs 0.32 WO3 or Cs 0.33 WO3.

[0009] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films. The parameters of the magnetron sputtering apparatus include: sputtering power of 40–120 W, sputtering time of 600–1200 s, target-substrate distance of 20–80 mm, substrate rotation speed of 20–30 r / min, and a vacuum level below 5.4 × 10⁻⁶. -4 Pa.

[0010] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, wherein sputtering deposition is carried out in a protective atmosphere, which is a mixture of inert gas and oxygen at a pressure of 0.3 to 1 Pa; wherein the flow ratio of inert gas to oxygen is 40:0.5 to 5.

[0011] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, wherein the heat treatment temperature is 250–550°C, the heat treatment atmosphere is a reducing gas, and the heat treatment time is 60–120 min.

[0012] On the other hand, some embodiments disclose cesium tungsten bronze films for near-infrared shielding films, obtained by a method for preparing cesium tungsten bronze films for near-infrared shielding films.

[0013] On the other hand, some embodiments disclose the application of cesium tungsten bronze thin films for near-infrared shielding films, which are used to prepare near-infrared shielding films.

[0014] Some embodiments disclose the application of cesium tungsten bronze thin films for near-infrared shielding films, wherein the infrared shielding film is a cesium tungsten bronze thin film-based composite film.

[0015] The present invention discloses a cesium tungsten bronze thin film for near-infrared shielding films and its preparation method. The cesium tungsten bronze thin film is obtained by magnetron sputtering using a cesium tungsten bronze sputtering target, and then heat-treated to obtain a high-quality cesium tungsten bronze thin film with high visible light transmittance, high near-infrared light blocking rate, and high ultraviolet light blocking rate. This film can be used as a cesium tungsten bronze thin film for near-infrared shielding films, and can further be used to fabricate cesium tungsten bronze thin film-based composite films. Moreover, the preparation method is simple, low-cost, and conducive to mass production; it has good application prospects in the field of near-infrared shielding films.

[0016] The following examples illustrate the technical details. Attached Figure Description

[0017] Figure 1 The transmittance diagrams for UV-Vis-NIR in Examples 1 and 2 are shown.

[0018] Figure 2 This is the UV-Vis-NIR transmittance diagram for Example 5;

[0019] Figure 3 The graphs show the ultraviolet blocking rate, visible light transmittance, and near-infrared light blocking rate for Examples 6, 7, 8, and 9.

[0020] Figure 4 The graphs show the visible light transmittance, infrared blocking rate, and ultraviolet blocking rate of Examples 7 and 10.

[0021] Figure 5 The images show the XRD patterns of different annealing temperatures in Examples 6, 7, and 8.

[0022] Figure 6 The images show the UV-Vis-NIR transmittance of films of different thicknesses after annealing in Examples 11, 12, and 13. Detailed Implementation

[0023] The term "embodiment" used herein, as an example, is not necessarily to be construed as superior to or better than other embodiments. Performance testing in these embodiments of the invention, unless otherwise specified, employs conventional testing methods in the art. It should be understood that the terminology used in these embodiments is merely for describing particular implementations and is not intended to limit the scope of the disclosure of these embodiments.

[0024] Unless otherwise stated, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the embodiments of this invention pertain; other experimental methods and technical means not specifically noted in the embodiments of this invention refer to experimental methods and technical means commonly used by one of ordinary skill in the art.

[0025] The terms “basic” and “approximately” used in this document are to describe small fluctuations. For example, they can mean less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. Numerical data presented or expressed in range format in this document are used for convenience and brevity only, and should therefore be flexibly interpreted to include not only the explicitly listed values ​​that define the range, but also all independent values ​​or subranges contained within that range. For example, a numerical range of “1–5%” should be interpreted to include not only the explicitly listed values ​​from 1% to 5%, but also the independent values ​​and subranges within the indicated range. Thus, this numerical range includes independent values ​​such as 2%, 3.5%, and 4%, and subranges such as 1%–3%, 2%–4%, and 3%–5%, etc. This principle also applies to ranges that list only one value. Furthermore, this interpretation applies regardless of the width of the range or the characteristics described.

[0026] In this document, including in the claims, conjunctions such as "comprising," "including," "with," "having," "containing," "involving," and "accommodating" are understood to be open-ended, meaning "including but not limited to." Only the conjunctions "consisting of" and "composed of" are closed conjunctions.

[0027] To better illustrate the content of this invention, numerous specific details are provided in the following detailed embodiments. Those skilled in the art should understand that the invention can be practiced even without certain specific details. In the embodiments, some methods, means, instruments, and devices well-known to those skilled in the art are not described in detail, in order to highlight the main points of the invention.

[0028] Without conflict, the technical features disclosed in the embodiments of the present invention can be combined arbitrarily, and the resulting technical solution belongs to the content disclosed in the embodiments of the present invention.

[0029] In some embodiments, the method for preparing a cesium tungsten bronze thin film for near-infrared shielding film involves using a cesium tungsten bronze target as a sputtering target and a planar substrate as a substrate, performing sputtering deposition in a magnetron sputtering apparatus to obtain a cesium tungsten bronze thin film on the substrate material, and then heat-treating the cesium tungsten bronze thin film to obtain the cesium tungsten bronze thin film for near-infrared shielding film, wherein the heat treatment temperature is set between 200 and 450°C.

[0030] In some embodiments, the near-infrared shielding film of the cesium tungsten bronze film prepared by the method of near-infrared shielding film has a near-infrared light blocking rate of more than 80%; in some preferred embodiments, the near-infrared light blocking rate is greater than 90%; more preferably, the near-infrared light blocking rate is greater than 98%.

[0031] In some embodiments, the visible light transmittance of the cesium tungsten bronze film of the near-infrared shielding film is greater than 60%; in some preferred embodiments, the visible light transmittance is greater than 70%; and in some even more preferred embodiments, the visible light transmittance is greater than 80%.

[0032] In some embodiments, the cesium tungsten bronze film of the near-infrared shielding film prepared by the method of preparing the near-infrared shielding film has an ultraviolet blocking rate of more than 70%; in some preferred embodiments, the ultraviolet blocking rate is greater than 80%; and more preferably, the ultraviolet blocking rate is greater than 90%.

[0033] In some embodiments, the cesium tungsten bronze film of the near-infrared shielding film has a visible light transmittance greater than 60%, a near-infrared light blocking rate greater than 70%, and an ultraviolet light blocking rate greater than 70%. More preferably, the cesium tungsten bronze film of the near-infrared shielding film has a visible light transmittance greater than 60%, a near-infrared light blocking rate greater than 90%, and an ultraviolet light blocking rate greater than 80%.

[0034] Some embodiments disclose methods for preparing cesium tungsten bronze thin films for near-infrared shielding films. During sputtering deposition, the substrate is heated to a temperature of 200–450°C, and the heat treatment process is performed simultaneously with the sputtering deposition process. Typically, heating the substrate to a set temperature and then performing sputtering on the heated substrate allows for heat treatment of the cesium tungsten bronze thin film sputtered and self-assembled on the substrate during sputtering. Heating at higher temperatures is beneficial for forming a fine-grained, highly intact microstructure of the cesium tungsten bronze thin film. A heating temperature of 200–450°C is generally conducive to obtaining the desired heat treatment effect and achieving an ideal cesium tungsten bronze thin film.

[0035] In some embodiments, thermocouple heating is used, and the temperature control power supply consists of a temperature controller, a phase-shifting trigger module, a thyristor, and an external circuit. The heating temperature of the sample is controllable from room temperature to 500°C to 800°C.

[0036] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, in which the obtained cesium tungsten bronze thin films are heat-treated after sputtering deposition. Typically, the sputtered cesium tungsten bronze thin films are heat-treated in a reducing atmosphere to complete the annealing process, adjust oxygen vacancy defects, and improve the near-infrared blocking rate. Furthermore, the microstructure can be improved at a set temperature, resulting in fine, complete, and uniform grains in the film. Heating temperatures of 200–450°C are generally favorable for achieving the desired annealing heat treatment effect, yielding ideal cesium tungsten bronze thin films.

[0037] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, wherein the heat treatment temperature is 250–550°C, the heat treatment atmosphere is a reducing gas, and the heat treatment time is 60–120 min.

[0038] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, wherein the cesium tungsten bronze target material is Cs. 0.20 WO3, Cs 0.30 WO3, Cs 0.32 WO3 or Cs 0.33 WO3.

[0039] In some embodiments, the cesium tungsten bronze target material has a purity greater than 99% and a density greater than 99%.

[0040] In some embodiments, a glass substrate, such as a quartz glass sheet, is used for sputtering. The glass sheet used as the substrate typically requires pretreatment to remove surface impurities, which is beneficial for obtaining a desirable sputtered film. Pretreatment usually includes washing with inorganic and organic solvents, such as ultrasonic washing with deionized water, acetone, and ethylene glycol sequentially. The quartz glass can usually be attached to the substrate with polyimide tape to facilitate the measurement of the thickness of the resulting cesium tungsten bronze film using a profilometer.

[0041] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films. The parameters of the magnetron sputtering apparatus include: sputtering power of 40–120 W, sputtering time of 600–1200 s, target-substrate distance of 20–80 mm, substrate rotation speed of 20–30 r / min, and a vacuum level below 5.4 × 10⁻⁶. -4 Pa.

[0042] Some embodiments disclose a method for preparing cesium tungsten bronze thin films for near-infrared shielding films, wherein sputtering deposition is carried out in a protective atmosphere, which is a mixture of inert gas and oxygen at a pressure of 0.3 to 1 Pa; wherein the flow ratio of inert gas to oxygen is 40:0.5 to 5.

[0043] Some embodiments disclose cesium tungsten bronze films for use in near-infrared shielding films, obtained by a method for preparing cesium tungsten bronze films for near-infrared shielding films.

[0044] Some embodiments disclose the application of cesium tungsten bronze thin films for near-infrared shielding films, which are used to prepare near-infrared shielding films.

[0045] Some embodiments disclose the application of cesium tungsten bronze thin films for near-infrared shielding films, wherein the infrared shielding film is a cesium tungsten bronze thin film-based composite film. Typically, cesium tungsten bronze thin films can be combined with other thin films to obtain cesium tungsten bronze-based thin films, which are used as near-infrared shielding films. Examples include thin film materials such as titanium oxide, tin oxide, zinc oxide, and silver. Taking titanium oxide as an example, a titanium oxide thin film is deposited on a cesium tungsten bronze thin film to obtain a cesium tungsten bronze thin film-based composite film. The near-infrared blocking rate of this composite film is superior to that of ordinary cesium tungsten bronze thin films.

[0046] The present invention discloses a cesium tungsten bronze thin film for near-infrared shielding films and its preparation method. The cesium tungsten bronze thin film is obtained by magnetron sputtering using a cesium tungsten bronze sputtering target, and then heat-treated to obtain a high-quality cesium tungsten bronze thin film with high visible light transmittance, high near-infrared light blocking rate, and high ultraviolet light blocking rate. This film can be used as a cesium tungsten bronze thin film for near-infrared shielding films, and can further be used to fabricate cesium tungsten bronze thin film-based composite films. Moreover, the preparation method is simple, low-cost, and conducive to mass production; it has good application prospects in the field of near-infrared shielding films.

[0047] The technical details are further illustrated below with reference to the embodiments.

[0048] Example 1

[0049] In Example 1, the method for preparing the cesium tungsten bronze thin film for near-infrared shielding includes:

[0050] Cesium tungsten bronze target material Cs 0.32 WO3, purity greater than 99%, density greater than 99%;

[0051] The quartz glass substrate was cleaned by placing it on a polytetrafluoroethylene cleaning rack and ultrasonically cleaning it in three solvents—deionized water, acetone, and ethylene glycol—for 10 minutes each. The cleaning rack was then removed and the substrate was dried with an N2 gun.

[0052] The quartz glass was attached to the substrate with polyimide tape (to facilitate the use of a profilometer to measure the thickness of the thin film), and then placed into the sputtering chamber, with the target-substrate distance adjusted to 75 mm.

[0053] Open the mechanical pump and pre-evacuation valve to evacuate the chamber to below 10 Pa. Then close the pre-evacuation valve, run the molecular pump, and open the gate valve and shut-off valve to evacuate the chamber pressure to 5 × 10 Pa. -4 Pa, then Ar and O2 are introduced to 0.5 Pa, with an Ar to O2 flow rate ratio of 40:1.5, and the sputtering power is adjusted to 100 W / cm. 2 Adjust the substrate rotation speed to maintain it at 25 r / min;

[0054] The target material was pre-sputtered for 8 minutes to remove surface oxides;

[0055] After pre-sputtering, the baffle is opened, the substrate is heated to 300°C, and sputtering deposition is carried out for 15 minutes.

[0056] After sputtering, once the temperature inside the chamber has cooled to room temperature, high-purity Ar is introduced into the chamber until atmospheric pressure is reached. Finally, the chamber is opened and the thin film sample is removed. The magnetron sputtering chamber is then evacuated to 10 Pa, and the experimental instrument is shut down.

[0057] Samples of the sputtered cesium tungsten bronze thin film were taken and their visible light transmittance and near-infrared light blocking rate were tested. The test results are as follows: Figure 1 As shown, the visible light transmittance is 51.2%, the near-infrared light blocking rate is 98%, the ultraviolet light blocking rate is 87%, and the cesium tungsten bronze film thickness is 526.92 nm.

[0058] The cesium tungsten bronze thin film obtained in Example 1 has good near-infrared and ultraviolet light blocking properties, uniform film thickness, long service life, and strong practicality.

[0059] Example 2

[0060] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 2 is the same as in Example 1; wherein, the flow ratio of the protective gas Ar to O2 is 40:2, and the other parameters are the same as in Example 1.

[0061] The sample was tested immediately after collection. The results showed that the visible light transmittance was 52.7%, the near-infrared light blocking rate was 98.1%, the ultraviolet light blocking rate was 90%, and the cesium tungsten bronze film thickness was 531.9 nm.

[0062] Example 3

[0063] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 3 is the same as in Example 1; wherein, the flow ratio of the protective gas Ar to O2 is 40:2.5, and the other parameters are the same as in Example 1.

[0064] The sample was tested immediately after being removed, and the results were as follows: Figure 1 As shown, the visible light transmittance is 69.3%, the near-infrared light blocking rate is 91.6%, the ultraviolet light blocking rate is 87.6%, and the cesium tungsten bronze film thickness is 545.15 nm.

[0065] Example 4

[0066] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 4 is the same as in Example 1; wherein, the flow ratio of the protective gas Ar to O2 is 40:3.5, and the other parameters are the same as in Example 1.

[0067] The sample was tested immediately after being taken out. The test results showed that the visible light transmittance was 62.6%, the near-infrared light blocking rate was 95.8%, the ultraviolet light blocking rate was 90.6%, and the cesium tungsten bronze film thickness was 596.7 nm.

[0068] Example 5

[0069] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 5 is the same as that in Example 1; wherein, the flow ratio of the protective gas Ar to O2 is 40:1, the substrate temperature is heated to 200°C, and the other parameters are the same as those in Example 1.

[0070] The sample was tested immediately after being removed, and the results were as follows: Figure 2 As shown, the visible light transmittance is 61.6%, the near-infrared light blocking rate is 75.7%, the ultraviolet light blocking rate is 76.2%, and the cesium tungsten bronze film thickness is 451.3 nm.

[0071] Example 6

[0072] In Example 6, the method for preparing the cesium tungsten bronze thin film for near-infrared shielding includes:

[0073] Cesium tungsten bronze target material Cs 0.32 WO3, purity greater than 99%, density greater than 99%;

[0074] Clean the quartz glass substrate by placing it on a polytetrafluoroethylene cleaning rack and ultrasonically cleaning it in deionized water, acetone and ethylene glycol for 10 minutes each. Then remove the cleaning rack and dry it with an N2 gun.

[0075] The quartz glass was attached to the substrate with polyimide tape and placed into the sputtering chamber. The target-substrate distance was adjusted to 75 mm.

[0076] Open the mechanical pump and pre-evacuation valve to evacuate the chamber to below 10 Pa. Then close the pre-evacuation valve, run the molecular pump, and open the gate valve and shut-off valve to evacuate the chamber pressure to 5 × 10 Pa. -4 Pa, then Ar and O2 are introduced to 0.5 Pa, and the sputtering power is adjusted to 100 W / cm. 2 Adjust the substrate rotation speed to 25 r / min;

[0077] First, the target material is pre-sputtered for 8 minutes to remove surface oxides. After the pre-sputtering is completed, the baffle is opened to perform sputtering deposition. The sputtering deposition time is 10 minutes.

[0078] After sputtering is complete, wait for the temperature inside the chamber to cool to room temperature, then introduce high-purity Ar into the chamber until atmospheric pressure is reached. Finally, open the chamber and remove the thin film sample.

[0079] The thin film samples were annealed at 350℃ in H2 atmosphere for 90 min.

[0080] The obtained cesium tungsten bronze thin film was tested, and the results are as follows: Figure 3 As shown, the visible light transmittance is 73.7%, the near-infrared light blocking rate is 72.9%, the ultraviolet light blocking rate is 62.8%, and the cesium tungsten bronze film thickness is 405.18 nm.

[0081] Example 7

[0082] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 7 is the same as that in Example 6; wherein, the annealing temperature is 400°C, and the other parameters are consistent with those in Example 6.

[0083] The obtained cesium tungsten bronze thin film was tested, and the results are as follows: Figure 3 As shown, the visible light transmittance is 64%, the near-infrared light blocking rate is 94.7%, the ultraviolet light blocking rate is 81%, and the cesium tungsten bronze film thickness is 445.06 nm.

[0084] Example 8

[0085] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 8 is the same as in Example 6; wherein the annealing temperature is 450°C, and all other parameters are consistent with those in Example 6.

[0086] The obtained cesium tungsten bronze thin film was tested, and the test results are as follows: Figure 3 As shown, the visible light transmittance is 57.7%, the near-infrared light blocking rate is 91.9%, the ultraviolet light blocking rate is 80.1%, and the cesium tungsten bronze film thickness is 409.98 nm.

[0087] Example 9

[0088] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 9 is the same as that in Example 6; wherein the annealing temperature is 375°C, and the other parameters are consistent with those in Example 6.

[0089] The obtained cesium tungsten bronze thin film was tested, and the test results are as follows: Figure 3 As shown, the visible light transmittance is 68.2%, the near-infrared light blocking rate is 88.4%, the ultraviolet light blocking rate is 74.3%, and the cesium tungsten bronze film thickness is 402.48 nm.

[0090] Example 10

[0091] The method for preparing the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 10 is the same as that in Example 6; wherein the sputtering time is 7 min, the annealing temperature is 400 °C, and the other parameters are consistent with those in Example 6.

[0092] The obtained cesium tungsten bronze thin film was tested, and the test results are as follows: Figure 4 As shown, the visible light transmittance is 70.4%, the near-infrared light blocking rate is 83.1%, the ultraviolet light blocking rate is 70.6%, and the cesium tungsten bronze film thickness is 314.16 nm.

[0093] Example 11

[0094] The preparation method of the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 11 is the same as that in Example 6; the cesium tungsten bronze thin film with a thickness of 244.86 nm after sputtering is annealed at an annealing temperature of 400°C, and the other parameters are consistent with those in Example 6.

[0095] The obtained cesium tungsten bronze thin film was tested, and the test results are as follows: Figure 6 As shown, the visible light transmittance is 81.5%, the near-infrared light blocking rate is 64.1%, and the ultraviolet light blocking rate is 64.6%.

[0096] Example 12

[0097] The preparation method of the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 12 is the same as that in Example 6; the cesium tungsten bronze thin film with a thickness of 314.16 nm after sputtering is annealed at an annealing temperature of 400°C, and all other parameters are the same as those in Example 6.

[0098] The obtained cesium tungsten bronze thin film was tested, and the test results are as follows: Figure 6 As shown, the visible light transmittance is 68.2%, the near-infrared light blocking rate is 83.1%, and the ultraviolet light blocking rate is 83.9%.

[0099] Example 13

[0100] The preparation method of the cesium tungsten bronze thin film for near-infrared shielding film disclosed in Example 13 is the same as that in Example 6; the cesium tungsten bronze thin film with a thickness of 445.06 nm after sputtering is annealed at an annealing temperature of 400°C, and the other parameters are consistent with those in Example 6.

[0101] The obtained cesium tungsten bronze thin film was tested, and the test results are as follows: Figure 6 As shown, the visible light transmittance is 62.5%, the near-infrared light blocking rate is 92.5%, and the ultraviolet light blocking rate is 93.9%.

[0102] Table 1 is a list of parameters for Examples 1 to 13.

[0103] Table 1 Parameter List for Examples 1-13

[0104]

[0105]

[0106] The present invention discloses a cesium tungsten bronze thin film for near-infrared shielding films and its preparation method. The cesium tungsten bronze thin film is obtained by magnetron sputtering using a cesium tungsten bronze sputtering target, and then heat-treated to obtain a high-quality cesium tungsten bronze thin film with high visible light transmittance, high near-infrared light blocking rate, and high ultraviolet light blocking rate. This film can be used as a cesium tungsten bronze thin film for near-infrared shielding films, and can further be used to fabricate cesium tungsten bronze thin film-based composite films. Moreover, the preparation method is simple, low-cost, and conducive to mass production; it has good application prospects in the field of near-infrared shielding films.

[0107] The technical solutions and technical details disclosed in the embodiments of this invention are merely illustrative of the inventive concept of this invention and do not constitute a limitation on the technical solutions of the embodiments of this invention. Any conventional changes, substitutions, or combinations made to the technical details disclosed in the embodiments of this invention have the same inventive concept as this invention and are within the protection scope of the claims of this invention.

Claims

1. A method for preparing a cesium tungsten bronze thin film for near-infrared shielding films, characterized in that, Using a cesium tungsten bronze target as the sputtering target and a planar substrate as the substrate, sputtering deposition is performed in a magnetron sputtering apparatus to obtain a cesium tungsten bronze thin film on the substrate material. The sputtering deposition is carried out in a protective atmosphere, which is a mixture of inert gas and oxygen at a pressure of 0.3–1 Pa; the flow ratio of inert gas to oxygen is 40:0.5–5; during the sputtering deposition process, the substrate is heated to a temperature of 200–450 °C; the cesium tungsten bronze thin film is then heat-treated to obtain a cesium tungsten bronze thin film for near-infrared shielding films, wherein the heat treatment temperature is set between 200 and 450 °C; the heat treatment process is carried out simultaneously with the sputtering deposition process.

2. The method for preparing a cesium tungsten bronze thin film for near-infrared shielding film according to claim 1, characterized in that, After sputtering deposition, the resulting cesium tungsten bronze film is subjected to heat treatment.

3. The method for preparing a cesium tungsten bronze thin film for near-infrared shielding film according to claim 1 or 2, characterized in that, Cesium tungsten bronze target material is Cs 0.20 WO3, Cs 0.30 WO3, Cs 0.32 WO3 or Cs 0.33 WO3.

4. The method for preparing a cesium tungsten bronze thin film for near-infrared shielding film according to claim 1 or 2, characterized in that, The parameters of the magnetron sputtering device include: sputtering power of 40–120 W, sputtering time of 600–1200 s, target-substrate distance of 20–80 mm, substrate rotation speed of 20–30 r / min, and vacuum level below 5.4 × 10⁻⁶. -4 Pa.

5. The method for preparing a cesium tungsten bronze thin film for near-infrared shielding film according to claim 2, characterized in that, The heat treatment temperature is 250–550°C, the heat treatment atmosphere is a reducing gas, and the heat treatment time is 60–120 min.

6. A cesium tungsten bronze thin film for near-infrared shielding films, characterized in that, It is obtained by the method for preparing cesium tungsten bronze thin film for near-infrared shielding film according to any one of claims 1-5.

7. The application of the cesium tungsten bronze thin film for near-infrared shielding film as described in claim 6, characterized in that, Cesium tungsten bronze thin films are used to prepare near-infrared shielding films.

8. The application of the cesium tungsten bronze thin film for near-infrared shielding film according to claim 7, characterized in that, The infrared shielding film is a cesium tungsten bronze thin film-based composite film.

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