A method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer
By controlling the arc plasma deposition and vacuum packaging process, using V2O5 film instead of IrO2 as an ion storage layer, solving the problem of high cost of IrO2, achieving efficient and low-cost electrochromic component preparation, achieving an optical property of ΔT%>45%.
Patent Information
- Application Number
- CN202310235331.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-03-13
- Publication Date
- 2025-08-22
- Estimated Expiration
- 2043-03-13
AI Technical Summary
Among the existing electrochromic materials, the cost of IrO2 as an ion storage layer is high, making it difficult for electrochromic products to popularize people's livelihood applications. The traditional V2O5 preparation methods are complicated, which increases the cost.
By controlling the conditions of operating current, ion bombardment treatment, working pressure, working distance and working gas/reactive gas ratio, V2O5 film was deposited using arc plasma, and the test piece was vacuum encapsulated and injected with electrolyte, to prepare electrochromic components with ΔT% up to 49%.
The cost of IrO2 was successfully reduced, and the V2O5 film was replaced by expensive IrO2 films, and the electrochromic components with high optical properties were stably produced, with ΔT%>45%.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of electrochromic materials, and in particular to a method for preparing an electrochromic component in which V2O5 replaces IrO2 as an ion storage layer. Background Art
[0002] Electrochromic materials are materials whose optical properties (reflectivity, transmittance, absorptivity, etc.) undergo a stable, reversible color change under the influence of an applied electric field. This phenomenon manifests itself as a reversible change in color and transparency. Electrochromic materials offer a high degree of user control and a wide range of visible light wavelength adjustments, blocking most visible and near-infrared light. This has made electrochromic technology a proactive, green, intelligent, and energy-saving technology that has recently gained significant attention.
[0003] The common structure of electrochromic components includes: (1) Transparent conductive layer: This layer must have two characteristics: extremely high conductivity and high visible light wavelength penetration. It is currently mostly made of ITO and plays the role of providing the electrons required for the color change process; (2) Electrochromic layer (the most important color-changing electrode layer in the component): The color change process is carried out by the electrons provided by the transparent conductive layer and the ions provided by the ion conduction layer and ion storage layer; (3) Ion conduction layer (electrolyte layer): The electrolyte is used as the ion conduction layer to provide the ions (large quantities) required for color change, with H + With Li + Two main ions; (4) ion storage layer (auxiliary electrode layer): The ions required in the color change process can also be provided by this layer (in small amounts). Materials with opposite electrical properties to the electrochromic layer can be selected, and the color addition and complementation effect can be achieved during coloring, making the coloring effect of the element more obvious.
[0004] Although electrochromic materials have been developed for some time, due to the integration of thin-film, electrochemical, and optical technologies, the technology is not yet fully mature. The production cost of commercial products is extremely high, making the consumer application of electrochromic products still relatively unpopular. For example, IrO2, like WO3, is an inorganic electrochromic material. Its electrical properties are exactly opposite to WO3, making it suitable for use as the electrochromic layer (WO3) and ion storage layer (IrO2) of an electrochromic component. This allows the production of an electrochromic component with a spectral change rate ΔT greater than 55%. This structure is also known as a complementary electrochromic component. However, IrO2 is a precious metal material, and a 3-inch, 1mm target can cost over NT$30,000 to NT$400,000. Even if the component has excellent properties, the cost alone still makes it difficult to popularize this technology for consumer applications. Researchers have attempted to use inexpensive V2O5 as an ion storage layer (a 3-inch, 12mm target costs approximately 10,000 yuan). For example, patent CN111286710A discloses a method for preparing a V2O5 multi-layer ion storage layer for electrochromic glass. However, this method requires modification of a single electrode ion storage layer. Specifically, the sol-gel method is used to prepare a nano-V2O5 porous ion storage layer, which involves complex steps and increases costs. Summary of the Invention
[0005] The purpose of the present invention is to overcome the shortcomings of the above-mentioned background technology and provide a method for preparing an electrochromic component in which V2O5 replaces IrO2 as an ion storage layer. By controlling conditions such as working current, ion bombardment treatment, working pressure, working distance, working gas / reaction gas ratio, etc., V2O5 is used as the ion storage layer to produce a component (ITO / WO3 / electrolyte / V2O5 / ITO) with a ΔT% as high as 49%, making it feasible for V2O5 film to replace expensive IrO2 film.
[0006] To achieve the purpose of the present invention, the present invention provides a method for preparing an electrochromic component in which V2O5 replaces IrO2 as an ion storage layer, comprising arc plasma deposition of a V2O5 thin film, and vacuum packaging of the test piece and injection of an electrolyte. The arc plasma deposition of the V2O5 thin film comprises the following steps:
[0007] (1) First, clean the ITO glass and blow dry the surface;
[0008] (2) Stick the ITO glass on the substrate with heat-resistant tape, adjust the working distance between the substrate and the target, close the chamber door, start the instrument, and vacuum until the vacuum reaches 1x10 -5 below torr;
[0009] (3) When the vacuum degree reaches 1x10 -5After the temperature drops below torr, the current for depositing the V2O5 film is set, and appropriate amounts of argon and oxygen are introduced. After the chamber is filled with gas, the V2O5 film deposition begins.
[0010] (4) After the film deposition is completed, turn off the power supply, argon and oxygen valves, and shut down the machine, waiting for the V2O5 specimen to slowly cool to room temperature in the vacuum chamber.
[0011] Furthermore, in some embodiments of the present invention, the ITO glass is cleaned by placing the ITO glass in alcohol and vibrating it with an ultrasonic vibrator. After the vibrating is completed, nitrogen is used to blow the surface of the test piece until it is completely dry, and ensure that no water marks are generated on the surface.
[0012] Furthermore, in some embodiments of the present invention, the working distance between the substrate and the target is 32-36 cm, preferably 33-35 cm, and more preferably 34 cm.
[0013] Furthermore, in some embodiments of the present invention, the current for depositing the V2O5 thin film is set to 55-100A, preferably 55-65A, and more preferably 60-65A.
[0014] Furthermore, in some embodiments of the present invention, the V2O5 thin film deposition working pressure is 1.2x10 - 2 torr-2.0x10 -2 torr, preferably 2.0x10 -2 torr.
[0015] Furthermore, in some embodiments of the present invention, the volume ratio of argon to oxygen is 1:1-3, preferably 1:3.
[0016] Furthermore, in some embodiments of the present invention, the V2O5 film is first deposited at a higher working pressure of 1.8x10 -2 torr to deposit V2O5 thin films for 10 seconds.
[0017] Furthermore, in some embodiments of the present invention, the test piece packaging includes the following steps:
[0018] (a) After the V2O5 specimen has slowly cooled to room temperature, open the air valve, break the vacuum, and remove the specimen;
[0019] (b) Remove the thermal insulation tape securing the ITO glass specimen to expose the ITO glass where V2O5 is not deposited. If there is any residual adhesive, gently wipe it with alcohol. This area will serve as the current-carrying electrode.
[0020] (c) Use isolation tape to form a tape frame around the outer frame of the test piece, avoiding the ITO glass (electrode) to form a circle (this is to prevent direct contact between the electrochromic layer and the ion storage layer during vacuum packaging, which could cause a short circuit, and to allow space for electrolyte injection). A small hole is exposed as the electrolyte injection hole during vacuum packaging;
[0021] (d) Setting up an automatic glue dispensing machine to apply UV curing glue around the tape frame for bonding and packaging;
[0022] (e) Place the WO3 electrochromic layer test piece on the V2O5 ion storage layer obtained in steps (a)-(d), with the ITO electrodes of the two layers offset to facilitate subsequent bonding of conductive copper adhesive for device optical property testing.
[0023] (f) irradiating the test piece obtained in step (e) with UV light to cure the UV adhesive;
[0024] (g) The test piece that has completed step (f) is injected with electrolyte using a vacuum infusion machine. After the electrolyte injection is completed, the component is removed and the small hole is sealed with UV glue. Finally, the UV glue is cured to complete the packaging step.
[0025] Furthermore, in some embodiments of the present invention, the UV curing adhesive avoids the electrolyte injection hole, and the edges of the two test pieces need to be cut evenly, so that the vacuum injection process of the electrolyte is smoother.
[0026] Furthermore, in some embodiments of the present invention, the WO3 and V2O5 test pieces are separated by an isolation tape and fixed with UV adhesive, leaving only a small hole for injecting electrolyte.
[0027] Furthermore, in some embodiments of the present invention, the vacuum filling machine sucks the electrolyte by means of a pressure difference between the test piece and the vacuum chamber.
[0028] The present invention greatly improves the optical properties of V2O5 thin films by controlling conditions such as working current, ion bombardment treatment, working pressure, working distance, and the working gas / reactive gas ratio. This makes it possible for V2O5 thin films to replace expensive IrO2 thin films. V2O5 can be used as an ion storage layer to stably produce components with a ΔT% greater than 45% (ITO / WO3 / electrolyte / V2O5 / ITO). DETAILED DESCRIPTION
[0029] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. Additional aspects and advantages of the present invention will be partially given in the following description, partially become apparent from the following description, or be understood through practice of the present invention. It should be understood that the following description is only used to explain the present invention and is not intended to limit the present invention.
[0030] As used herein, the terms "comprises," "including," "having," "containing" or any other variations thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a listed element is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
[0031] The conjunction "consisting of" excludes any unspecified element, step, or component. If used in a claim, this phrase renders the claim closed, excluding materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of" appears in a clause of the body of a claim, rather than immediately following the subject matter, it limits only the elements described in that clause; other elements are not excluded from the claim as a whole.
[0032] When amount, concentration or other value or parameter is represented with range, preferred range or the range that a series of upper preferred value and lower preferred value limit are expressed, this should be understood as specifically disclosing all ranges formed by any pairing of any range upper limit or preferred value and any range lower limit or preferred value, no matter whether this range is disclosed separately.For example, when disclosing scope "1 to 5", described scope should be interpreted as including scope "1 to 4", "1 to 3", "1 to 2", "1 to 2 and 4 to 5", "1 to 3 and 5" etc.When numerical range is described in this article, unless otherwise stated, otherwise this scope is intended to include its end value and all integers and fractions within this range.
[0033] The singular includes plural references unless the context clearly dictates otherwise. "Optional" or "either" means that the subsequently described event or incident can or cannot occur, and that the description includes instances where the event occurs and instances where it does not.
[0034] The indefinite articles "a" and "an" before the elements or components of the present invention do not limit the quantity requirement (i.e. the number of times they appear). Therefore, "a" or "an" should be interpreted as including one or at least one, and elements or components in the singular also include plural forms, unless the quantity clearly refers to only the singular form.
[0035] In addition, the terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples" described below mean that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic descriptions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the technical features involved in the various embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
[0036] The present invention aims to fabricate electrochromic components using inexpensive V2O5 instead of expensive IrO2 as the ion storage layer. In a specific embodiment of the present invention, to increase experimental accuracy and reduce other factors that may cause experimental error, the present invention uses procured ITO glass instead of self-deposited ITO thin film as the transparent conductive layer of the electrochromic component.
[0037] The experimental method can be simply divided into two steps: arc plasma deposition of V2O5 thin film, vacuum packaging of the test piece and injection of electrolyte. The experimental steps of arc plasma deposition of V2O5 thin film are as follows:
[0038] (1) First, place the ITO glass in alcohol and use an ultrasonic vibrator to vibrate for 15 minutes to remove dirt on the surface. After the vibration is completed, use nitrogen to blow the surface until it is completely dry and ensure that there are no water marks on the surface;
[0039] (2) Glue the ITO glass to the substrate with heat-resistant tape, adjust the distance between the substrate and the target (working distance), close the chamber door, start the instrument, and start vacuuming after the oil pump heat engine is completed. Wait until the vacuum reaches 1x10 -5 below torr;
[0040] (3) When the background vacuum reaches 1x10 -5 After reaching 0.1 torr, set the current for V2O5 film deposition and introduce appropriate amounts of argon and oxygen. Wait 3-5 minutes for the chamber to be filled with gas before starting V2O5 film deposition.
[0041] (4) After the film deposition is completed, turn off the power supply, argon and oxygen valves, and shut down the machine, waiting for the specimen to slowly cool to room temperature in the vacuum chamber.
[0042] After completing the above steps, proceed to test piece packaging:
[0043] (5) After the V2O5 specimen is slowly cooled to room temperature, open the air valve, break the vacuum and remove the specimen;
[0044] (6) Tear off the thermal insulation tape that fixes the ITO glass test piece to expose the ITO glass without the V2O5 film deposited. If there is any residual adhesive, gently wipe it with alcohol. This area is intended to be used as the electrode for power supply.
[0045] (7) Use 0.5mm isolation tape to form a circle around the outer frame of the test piece, avoiding the ITO glass (electrode) (the purpose is to prevent the electrochromic layer and the ion storage layer from directly contacting each other during vacuum packaging, causing a short circuit of the component, and to allow space for the electrolyte to be injected), and expose a small hole as the electrolyte suction point during vacuum packaging;
[0046] (8) Set up an automatic dispensing machine to apply UV curing glue around the tape frame for bonding and packaging;
[0047] (9) Take the WO3 electrochromic layer test piece and gently place it on the V2O5 ion storage layer that has completed steps (1)-(4), and stagger the ITO electrodes of the two to facilitate the subsequent adhesion of conductive copper glue for component optical property testing; (Note: Do not cover the reserved electrolyte injection hole with UV curing glue, and the edges of the two test pieces must be cut evenly to allow the vacuum injection process of the electrolyte to be smoother.)
[0048] (10) Irradiate the test piece after step (5) with UV light to cure the UV adhesive. (At this point, the WO3 and V2O5 thin film test pieces are separated by isolation tape and fixed with UV adhesive, leaving only one small hole for injecting electrolyte.)
[0049] (11) The test piece that has completed step (6) is injected with electrolyte using a vacuum filling machine. After the electrolyte injection is completed, the component is taken out and the small hole is sealed with UV glue. Finally, the packaging step is completed after the UV glue is cured. Among them, the vacuum filling machine absorbs the electrolyte into the component by means of the pressure difference between the test piece and the vacuum chamber.
[0050] Example 1
[0051] Study on the effects of working distance and ion bombardment on V2O5 thin films
[0052] This experimental parameter design references the experimental design for a WO3 electrochromic layer. The optimal working distance for WO3 thin film deposition is 34cm. The optical properties of the film are highly sensitive to working distance, and even small changes in working distance significantly affect them. Under identical process conditions, this experiment used a 34cm working distance as the median and deposited V2O5 thin films at three different working distances (32, 34, and 36cm). Because working distance affects plasma concentration, which in turn affects the number of ionized ions, this indirectly alters the film's microstructure and properties. This experiment investigated the effects of depositing V2O5 thin films at different working distances on their optical properties. The process parameters and measured optical properties of the V2O5 films are detailed in Table 1.
[0053] The three test pieces exhibited significant differences in optical properties. While the ΔT% values for V2O5#2 (34cm) and V2O5#3 (36cm) were identical, significant bubbles were observed during the measurement of V2O5#3 (36cm). Based on past experience with WO3 thin film production, bubbles are often caused by the reaction between metal particles on the film surface and the electrolyte. The presence of bubbles significantly reduces component reliability. To mitigate this issue, a two-stage process was subsequently implemented, depositing the V2O5 film at a higher pressure for 10 seconds before the actual deposition process.
[0054] Table 1 Experimental parameters and optical properties of V2O5 films affected by working distance
[0055]
[0056]
[0057] In various plasma processes, in order to increase film adhesion or help form the desired microstructure, the substrate is continuously bombarded with energetic particles (ions) at the beginning of the process. Before the film is formed, the substrate is continuously bombarded to remove contaminants (surface oxides) on the substrate surface, thereby increasing the adhesion between the film layer and the substrate.
[0058] Previous experience with WO3 thin film deposition has shown that WO3 films deposited at lower operating pressures are prone to generating bubbles in the electrolyte during optical property measurement of packaged components, resulting in reduced component reliability. However, WO3 films deposited at higher operating pressures do not exhibit this phenomenon. SEM images show a much higher number of surface particles on WO3 films deposited at lower operating pressures than those deposited at higher operating pressures. These particles are mostly spherical tungsten metal. This suggests that the electrolyte reacts with the tungsten metal particles on the surface of the WO3 film to generate the large number of bubbles.
[0059] Based on the above analysis, the following experimental design was developed to (a) prevent the formation of bubbles from metallic particles reacting with the electrolyte; (b) enhance the adhesion of the V2O5 film by ion bombardment before the start of the process to facilitate microstructure formation; and (c) observe the effects of deposition at different plasma concentrations on the V2O5 film:
[0060] Under the same process conditions, before the formal V2O5 process, control the process working pressure:
[0061] (1) First, use a higher working pressure of 1.8x10 -2 torr to deposit V2O5 thin films for 10 seconds.
[0062] Purpose: Similar to ion bombardment treatment, in addition to cleaning the specimen surface and improving film adhesion, previous experience in producing WO3 thin films shows that when deposited at higher working pressures, the number of particles is smaller and the metallicity is lower. Therefore, using this layer as a buffer layer in contact with the ITO glass should reduce bubble generation when encapsulating the device and measuring its optical properties.
[0063] (2) V2O5 process was performed at three different working distances.
[0064] Purpose: Because plasma concentration varies with working distance, an effect similar to changes in working pressure, plasma concentration affects the number of dissociated ions and the resistance between ions and the substrate. Drawing on previous WO3 thin film experiments, three different working distances were designed to observe their effects on the properties of V2O5 films.
[0065] Table 3-2 below details the experimental process parameters and optical quality data for V2O5 thin films. While the optical properties of the three test pieces declined slightly, none of the three groups exhibited blistering during optical property measurements, demonstrating that the dual-stage process is effective in improving device reliability (reducing blistering). However, the ΔT% remains relatively low. Further research will be conducted on the process gas / reactant gas ratio and operating pressure to identify the optimal process window for V2O5 thin films.
[0066] Table 2 Experimental parameters and optical properties of V2O5 films affected by ion bombardment
[0067]
[0068]
[0069] Example 2
[0070] Study on the influence of working pressure on V2O5 thin film
[0071] Since working pressure affects plasma concentration, and the concentration in the plasma area affects the number of ionized ions and the resistance between ions and the substrate, which in turn causes the substrate bias to change, the electric field size also changes accordingly, affecting the film microstructure. In this experiment, three different working pressures will be designed based on the parameters of the WO3 electrochromic layer to observe the impact on the properties of the V2O5 film.
[0072] The optimal deposition conditions for WO3 thin films are a pressure of 1.5x10 -2 torr, under the same process conditions, this experiment used 1.5x10 -2 torr working pressure is the middle value, and three different working pressures (1.2x10 -2 , 1.5x10 -2 , 2.0x10 - 2Torr-free (1000 torr) V2O5 thin films were deposited. The effect of working pressure on plasma concentration is similar to that of working distance, directly or indirectly causing changes in the film's microstructure and properties. Furthermore, referring to the results of Experiment 1, the working distance was set to 34 cm. The process parameters and measured optical properties of the V2O5 films are summarized in Table 3 below.
[0073] The optical properties of the three groups of test pieces are obviously different. -2 When measuring optical properties in 10 torr (100 torr), bubbles still occur. It is expected that the introduction of a two-stage process will improve this phenomenon, but the ΔT% is too low and will be ignored. The subsequent discussion will focus on the products with better optical properties.
[0074] Table 3 Experimental parameters and optical properties of V2O5 films in which working pressure is affected
[0075]
[0076]
[0077] Example 3
[0078] Study on the effect of working gas / reactive gas ratio on V2O5 thin film
[0079] We all know that when reactive gases dissociate, they react with target ions, attracting them to the substrate bias and depositing them into a thin film. When the reactive gas ratio is too low, the film will contain metallic bonds. Past experience shows that when WO3 thin films are deposited at relatively low reactive gas ratios, bubbles are more likely to form during packaging and optical property measurement. This indicates that the particles on the film surface are mostly metallic tungsten, and the bubbles are generated by the reaction between the metal particles and the electrolyte. If the reactive gas ratio is too high, chemical reactions will occur on the target surface, causing target poisoning, reduced coating efficiency, or arc instability. Therefore, the reactive gas ratio is a key factor in determining the stability of the arc plasma process during long-term coating operations.
[0080] With reference to the optimal process conditions for WO3 thin films, the working gas / reactive gas ratio (Ar / O2) is 1 / 3. Due to the limitation of the machine's pumping rate, the maximum working gas / reactive gas ratio can only be set to 1 / 3 in this experiment. Under the premise that other process conditions are the same, V2O5 thin films are deposited with four different working gas / reactive gas ratios (1 / 1, 1 / 1.5, 1 / 2, and 1 / 3). In addition, referring to the results of Experiments 1 and 2, the working distance and working pressure are set to 34cm, 2.0x10 -2 The detailed process parameters and the measured optical properties of the V2O5 thin films are listed in Table 4.
[0081] The four test pieces had a ΔT% > 40%, and no bubbles were generated during optical property measurements. The arc plasma was stable during deposition, and no arc extinction occurred, indicating that a suitable process window for V2O5 thin film deposition has been initially found.
[0082] Although there is still some distance between (ITO / WO3 / electrolyte / V2O5 / ITO)ΔT%=49% and the current ΔT%>55% of this group of components (ITO / WO3 / electrolyte / IrO2 / ITO), it is undeniable that if we only consider the optical properties of the components, V2O5 film can replace the expensive IrO2 film.
[0083] Table 4 Experimental parameters and optical properties of V2O5 films in which Ar / O2 ratio is affected
[0084]
[0085] Example 4
[0086] Study on the effect of working current on V2O5 thin film
[0087] The working current has the most direct impact on the ion concentration in the arc plasma and the target surface temperature. The larger the working current, the higher the arc plasma concentration. In addition, a higher target surface temperature will increase the formation of film particles, resulting in larger particles and defects, and increasing the roughness of the film.
[0088] Based on past experience in arc plasma thin film deposition, a higher operating current (>75A) is used for deposition unless the deposition rate is too slow, a film of sufficient thickness (>1μm) needs to be deposited, or non-optical thin films are being deposited. Otherwise, surface particles will increase the surface roughness of the film, resulting in a hazy appearance and affecting the optical properties of the film.
[0089] Although adjusting the operating current was not expected to be of much help in finding the V2O5 thin film process window, adhering to the spirit of experimentation, a series of experiments were designed to deposit V2O5 thin films at different operating currents. V2O5 thin films were deposited at two different operating currents (75A and 100A). Reference was made to previous experience with optical thin film deposition at high operating currents: particle size significantly reduces visible light transmittance of the film and creates a rough surface morphology. Because larger particles were expected, the working distance was adjusted to the experimental machine's maximum value of 57cm (larger particles, affected by gravity, would fall before reaching the substrate, preventing deposition on the substrate). The pressure was also adjusted to 5.0x10 -3torr (increasing the probability of inter-ion collisions and reducing particle flight distance) to reduce the chance of large particles depositing on the V2O5 film surface, thereby minimizing the impact on optical properties. Experimental results showed that both optical property measurements generated bubbles, with a low ΔT%, and prolonged film coloration and decolorization reaction times. Detailed process parameters and V2O5 film optical quality data are listed in Table 5.
[0090] Table 5 Experimental parameters and optical properties of V2O5 films investigated by working current
[0091]
[0092] The above experimental results show that the film coloring and decolorization reaction time is relatively long. According to the previous experience of WO3 film production process, it means that the film microstructure at this time is not conducive to the Li + This phenomenon can only be improved by changing the microstructure through the inflow and outflow of ions. After the film deposition is completed, the surface appears foggy, which is caused by particles and thus results in poor ΔT%.
[0093] Subsequent experiments, referring to the results of Experiment 3, modified the experimental parameters in Table 5, adjusting the working gas / reactant gas ratios of Ar / O2. V2O5 thin films were deposited using two different working gas / reactant gas ratios (0 / 1 and 1 / 1). Experiment #17, in which the parameters were designed without the introduction of Ar, used only the reactive gas O2 to produce the V2O5 film. Under these extreme conditions, the film was deposited using a stable arc plasma. No bubbles were generated during measurement, and visual inspection revealed a smooth, non-hazy film surface, indicating that the particle problem had been resolved. However, the film's coloration and decolorization reaction times remained relatively long, clearly outside the V2O5 thin film process window. Furthermore, the film's optical properties were not particularly outstanding. Therefore, subsequent experiments with higher currents for V2O5 thin film deposition were discontinued.
[0094] The present invention investigates the effects of operating current, ion bombardment, operating pressure, operating distance, and the ratio of working gas to reactive gas on the optical properties of V2O5 thin films. Through these experiments, it has been possible to stably fabricate devices (ITO / WO3 / electrolyte / V2O5 / ITO) with a ΔT% > 45%, using V2O5 as an ion storage layer.
[0095] The current optimal condition, ΔT% = 49% (ITO / WO3 / electrolyte / V2O5 / ITO), is still some distance away from the current ΔT% > 55% of this group of components (ITO / WO3 / electrolyte / IrO2 / ITO). However, it is undeniable that, judging solely by the optical properties of the components, V2O5 thin film has the potential to replace the expensive IrO2 thin film.
[0096] It will be easily understood by those skilled in the art that the above description is merely an embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer, characterized in that: The preparation method includes two steps: arc plasma deposition of a V2O5 thin film, and vacuum packaging of a V2O5 test piece and injection of an electrolyte. The arc plasma deposition of a V2O5 thin film includes the following steps: (1) First clean the ITO glass and blow dry the surface; (2) Stick the ITO glass on the substrate with heat-resistant tape, adjust the working distance between the substrate and the target, close the chamber door, start the instrument, and vacuum until the vacuum degree reaches 1x10 -5 torr below; (3) When the vacuum degree reaches 1x10 -5 After the temperature drops below torr, the current for depositing the V2O5 film is set, and appropriate amounts of argon and oxygen are introduced. After the chamber is filled with gas, the V2O5 film deposition begins. (4) After the film deposition is completed, turn off the power supply, argon and oxygen valves, and shut down the machine, waiting for the V2O5 specimen to slowly cool to room temperature in the vacuum chamber; The working distance between the substrate and the target is 34 cm; the current for depositing the V2O5 film is set to 60-65A; the working pressure for depositing the V2O5 film is 2.0x10 -2 torr.
2. The method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer according to claim 1, characterized in that: The ITO glass is cleaned by placing the ITO glass in alcohol and using an ultrasonic vibrator to vibrate and clean it. After the vibrating and cleaning is completed, nitrogen is used to blow the surface of the test piece until it is completely dry, and it is ensured that no water marks are generated on the surface.
3. The method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer according to claim 1, characterized in that: The volume ratio of the argon gas to the oxygen gas is 1:1-3.
4. The method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer according to claim 1, characterized in that: The volume ratio of the argon gas to the oxygen gas is 1:
3.
5. The method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer according to claim 1, characterized in that: The V2O5 test piece packaging includes the following steps: (a) After the V2O5 specimen is slowly cooled to room temperature, open the air valve, break the vacuum and remove the specimen; (b) Remove the thermal insulation tape securing the ITO glass specimen to expose the ITO glass not deposited with V2O5. Gently wipe any residual adhesive with alcohol to use as the current-carrying electrode. (c) Use isolation tape to form a tape frame around the outer frame of the test piece, avoiding the ITO glass and leaving a small hole as the electrolyte injection hole for vacuum packaging; (d) Setting up an automatic glue dispensing machine to apply UV curing glue around the tape frame for bonding and packaging; (e) Place the WO3 electrochromic layer test piece on the V2O5 ion storage layer (prepared for steps (a)-(d)). Stagger the ITO electrodes between the two layers to facilitate subsequent bonding of conductive copper adhesive for device optical property testing. (f) irradiating the test piece obtained in step (e) with UV light to cure the UV adhesive; (g) The test piece that has completed step (f) is injected with electrolyte using a vacuum infusion machine. After the electrolyte injection is completed, the component is removed and the small hole is sealed with UV glue. Finally, the UV glue is cured to complete the packaging step.
6. The method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer according to claim 5, characterized in that: The WO3 and V2O5 test pieces are separated by isolation tape and fixed with UV glue, leaving only a small hole for injecting electrolyte.
7. The method for preparing an electrochromic component using V2O5 instead of IrO2 as an ion storage layer according to claim 1, characterized in that: The vacuum filling machine sucks the electrolyte by means of the pressure difference between the test piece and the vacuum chamber.
Citation Information
Patent Citations
Method for fabricating electrochromic device
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Electrochromic device comprising protective inorganic solid electrolyte film and manufacturing method thereof
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