A method for preparing all-solid-state inorganic electrochromic glass and a monitoring and control system

By combining APCVD and PVD processes and monitoring and control systems, the problems of high equipment and materials cost and long production in the preparation of all-solid-state inorganic electrochromic glass are solved, and efficient and uniform film deposition and low energy consumption production are achieved, which improves product quality and industrialization potential.

CN119797773BActive Publication Date: 2025-08-22ANHUI ZHIYUN NEW MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510068183.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-01-16
Publication Date
2025-08-22
Estimated Expiration
2045-01-16

AI Technical Summary

Technical Problem

The existing preparation method for all-solid-state inorganic electrochromic glass relies on PVD equipment to deposit film layers, resulting in long production time, high equipment and material costs, and problems such as large leakage, uneven color discoloration, and slow response, which limits its industrialization development.

Method used

Using a combination of APCVD and PVD, the conductive film layer, insulating layer and electrochromic layer are deposited on the glass substrate in turn, and the insulating layer is added to reduce leakage, and real-time parameter optimization is carried out in combination with the monitoring and control system to ensure the uniformity and quality of the film layer.

Benefits of technology

It has achieved a reduction in equipment and material costs, improved deposition speed and film uniformity, reduced leakage, reduced energy losses, and improved production efficiency and product quality.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a method for preparing all-solid-state inorganic electrochromic glass and a monitoring and control system, which relate to the technical field of glass preparation, including: APCVD deposition of film layers: plating a first conductive film layer on a glass substrate; plating a first insulating layer on the first conductive film layer; plating a main color-changing layer on the first insulating layer to obtain an electrochromic layer; PVD deposition of film layers: plating a second insulating layer on the electrochromic layer; plating an electrochromic storage layer on the second insulating layer; plating a second conductive layer on the electrochromic storage layer. The present invention achieves a dual reduction in equipment investment and material costs by combining the APCVD and PVD processes. By combining the precise control of the APCVD process with the high deposition rate of the PVD process, the effective deposition speed is improved, the uniformity and quality of the film layer are ensured, and by adding two insulating layers on both sides of the electrochromic layer, the leakage phenomenon is effectively reduced, the energy loss is reduced, and the aging process of the film layer is slowed down.
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Description

Technical Field

[0001] The present invention relates to the technical field of glass preparation, and in particular to a method for preparing all-solid-state inorganic electrochromic glass and a monitoring and control system. Background Art

[0002] As a smart material, all-solid-state inorganic electrochromic glass can be used in smart windows in the architectural field, dynamically controlling solar radiation and indoor lighting, thereby reducing building energy consumption. In the automotive industry, it can be applied to windows and sunroofs, enhancing the driving experience and the level of vehicle intelligence. In the electronic display field, it is expected to become a new type of display device or dimming element, expanding the application range of display technology. Therefore, its market demand is growing, which is of great significance to the improvement and innovation of its preparation process.

[0003] In existing technology, all-solid-state inorganic electrochromic glass is typically produced by sequentially depositing five nanofilm layers onto a glass substrate using PVD (physical vapor deposition) equipment. These five layers include a first conductive layer, an electrochromic layer, an ion transport layer, an electrochromic storage layer, and a second conductive layer. When a DC voltage (1-3V) is applied to the first and second conductive layers, ions migrate under the influence of the electric field. When lithium ions enter the electrochromic layer, the transmittance of the glass decreases; when lithium ions enter the electrochromic storage layer, the transmittance increases. By switching the positive and negative polarity of the DC voltage, the transmittance of the glass can be increased or decreased.

[0004] Based on the above, existing preparation methods rely on PVD equipment to deposit the film layer, which has a slow deposition speed, is time-consuming for large-scale production, and increases equipment depreciation costs. Furthermore, the materials used are expensive, which limits the industrial development of all-solid-state inorganic electrochromic glass. Furthermore, existing technologies suffer from large leakage, which leads to energy waste, film aging, and performance degradation, resulting in uneven color change and slow response of the electrochromic glass. Therefore, it is necessary to provide a method for preparing all-solid-state inorganic electrochromic glass to address the above technical issues. Summary of the Invention

[0005] The present invention provides a method for preparing all-solid-state inorganic electrochromic glass, which solves the problems raised in the above-mentioned background technology.

[0006] In order to solve the above technical problems, the present invention provides a method for preparing all-solid-state inorganic electrochromic glass, comprising the following steps:

[0007] S1, glass substrate preparation;

[0008] S2, APCVD deposition film:

[0009] S21, depositing a first conductive film layer on the glass substrate;

[0010] S22, depositing a first insulating layer on the first conductive film layer;

[0011] S23, plating a main color-changing layer on the first insulating layer to obtain an electrochromic layer;

[0012] S3, PVD deposition film:

[0013] S31, plating a second insulating layer on the electrochromic layer;

[0014] S32, depositing an electrochromic storage layer on the second insulating layer;

[0015] S33, depositing a second conductive layer on the electrochromic storage layer.

[0016] Preferably, based on step S2, during APCVD film deposition, the first conductive film layer, the first insulating layer and the electrochromic layer are deposited in the first thin film reaction chamber of the float line, the second thin film reaction chamber of the float line and the third thin film reaction chamber of the float line respectively.

[0017] A monitoring and control system for the preparation of all-solid-state inorganic electrochromic glass, the monitoring and control system comprising a data acquisition and transmission module, a data analysis and control module, and an adjustment and optimization module;

[0018] Data acquisition and transmission module, used to collect plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer;

[0019] A data analysis and control module is used to perform plating analysis on the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer, and obtain plating analysis results; wherein the plating analysis results include the preset difference value, preset difference mean value, preset fluctuation value, preset extreme value, preset difference value and corresponding adjustment signal and corresponding dynamic adjustment coefficient of the parameters in the plating information; analyze the film thickness and optical characteristics of any film layer during APCVD deposition and PVD deposition to obtain the film thickness influence value and the optical characteristic comprehensive value; perform weighted processing on the preset difference value and film thickness influence value of the parameters in the plating information to obtain the mutual influence coefficient; when generating the adjustment signal corresponding to the parameter, calculate the dynamic adjustment coefficient corresponding to the parameter; mark the adjustment signal of the parameter in the plating information and the corresponding dynamic adjustment coefficient as dynamic adjustment parameters;

[0020] The adjustment and optimization module is used to receive dynamic adjustment parameters and perform corresponding adjustment operations according to the dynamic adjustment parameters.

[0021] Preferably, the data analysis and control module includes a time zone division unit, a plating state analysis unit, a thickness and optical change analysis unit, and an information summary analysis and processing unit;

[0022] A time zone division unit is used to mark the initial moment of APCVD deposition or PVD deposition of the corresponding film layer as the first moment, and mark the time zone between the first moment and the current moment as the film layer deposition time zone;

[0023] A plating state analysis unit is used to perform plating analysis on the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer, and obtain plating analysis results; wherein the plating analysis results include preset difference values, preset difference mean values, preset fluctuation values, preset extreme values, preset difference shadow values ​​and corresponding adjustment signals of the parameters in the plating information;

[0024] Thickness and optical change analysis unit, used to analyze the film thickness and optical characteristics of any film layer during APCVD deposition and PVD deposition, and obtain the film thickness impact value and optical characteristic comprehensive shadow value;

[0025] The information summary analysis processing unit is used to perform weighted processing on the preset differential value, film thickness influence value, and optical characteristic comprehensive value of the parameters in the plating information to obtain the mutual influence coefficient; when receiving the adjustment signal corresponding to the parameter, the preset differential value and mutual influence coefficient are used to calculate the dynamic adjustment coefficient of the parameter

[0026] The parameter adjustment signaling in the plating information and the corresponding dynamic adjustment coefficient are marked as dynamic adjustment parameters.

[0027] Preferably, the monitoring and control system also includes a monitoring setting module, which is used to respectively set a temperature sensor, a gas flow sensor and a film thickness monitor in the reaction chambers for APCVD deposition of the first conductive film layer, the first insulating layer and the electrochromic layer; and is also used to set a sputtering rate monitor, a vacuum monitor and a thin film optical property analyzer in the equipment corresponding to the PVD deposition of the second insulating layer, the electrochromic storage layer and the second conductive layer.

[0028] Preferably, the plating information of the corresponding reaction chamber or equipment during the APCVD deposition and PVD deposition of any film layer is analyzed separately, specifically:

[0029] According to the preset value of any parameter in the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer; performing difference calculation between any parameter in the plating information and the preset value of the parameter to obtain a preset difference; identifying the preset difference values ​​of all acquisition moments within the film layer plating time zone, performing mean, standard deviation, maximum and minimum calculation on the preset difference values ​​within the film layer plating time zone, and obtaining a preset difference mean, a preset fluctuation value and a preset range value;

[0030] Perform weighted calculation on the preset difference value, the preset difference mean value, the preset fluctuation value, and the preset extreme value to obtain the preset difference value;

[0031] Set the allowable variation range of any parameter in the plating information, match the preset difference value of the parameter in the plating information with the allowable variation range corresponding to the parameter, if the preset difference value is within its allowable variation range, it indicates that the parameter is in a normal state; if the preset difference value is not within its allowable variation range, it indicates that the parameter is in a deviated state, and generate an adjustment signaling corresponding to the parameter;

[0032] The preset difference value, preset difference mean value, preset fluctuation value, preset range value, preset difference value and corresponding adjustment signaling and corresponding dynamic adjustment coefficient of the parameters in the plating information are marked as plating analysis results.

[0033] Preferably, the film thickness and optical properties of any film layer deposited by APCVD and PVD are analyzed, specifically:

[0034] Obtain the film thickness of any film layer during APCVD deposition or PVD deposition at all acquisition moments within the film coating time zone; perform difference calculation on the film thickness at adjacent acquisition moments to obtain the film thickness change value;

[0035] The film thickness variation value within the film coating time zone is calculated by the mean and standard deviation to obtain the film thickness variation mean and film thickness fluctuation value;

[0036] Obtaining a preset thickness of the film layer, identifying the maximum thickness of the film layer in the film layer plating zone, and performing difference calculation between the maximum thickness and the preset thickness to obtain an expected thickness difference;

[0037] The film thickness influence value is obtained by weighted calculation of the current film thickness change value, the film thickness change mean value, the film thickness fluctuation value, and the expected thickness difference value;

[0038] Obtain optical property information of APCVD and PVD deposited films at all acquisition moments within the film coating time zone; optical property information includes the light transmittance, reflectivity, and absorptivity of the film at a specific wavelength;

[0039] Construct a graph showing how light transmittance, reflectance, and absorptance vary with wavelength, identify the corresponding light transmittance, reflectance, and absorptance curves in the graph, and calculate the smoothness of the curves using numerical analysis methods.

[0040] Identify the smoothness of the curves corresponding to the light transmittance, reflectivity, and absorptivity at all acquisition moments within the film coating time zone; calculate statistical indicators of the smoothness of the curve corresponding to any parameter in the optical characteristic information within the film coating time zone, including the average value, variance, maximum value, and minimum value; set a smoothing qualified value for the curve corresponding to any parameter in the optical characteristic information, and perform a difference calculation between the smoothness of the curve corresponding to any parameter in the optical characteristic information and its smoothing qualified value to obtain a smoothing qualified difference;

[0041] The smoothing influence value is obtained by weighting the smoothing qualified difference and the statistical index of smoothness;

[0042] Then, the characteristic peak in the curve is identified by the peak detection algorithm, and the peak position movement and intensity increase and decrease of the characteristic peak in the film coating time zone are analyzed to obtain the peak position movement rate and peak position intensity impact value;

[0043] Perform weighted calculation on the smoothing influence value, peak position moving rate and peak position intensity influence value to obtain the parameter comprehensive value corresponding to the parameter in the optical characteristic information;

[0044] Then, the weighted calculation of the comprehensive shadow values ​​of all parameters in the optical characteristic information is performed to obtain the comprehensive shadow value of the optical characteristic.

[0045] Preferably, corresponding adjustment operations are performed according to the dynamic adjustment parameters, specifically:

[0046] When receiving the temperature adjustment signal corresponding to any film layer deposited by APCVD, the device supporting the reaction chamber of the corresponding film layer is adjusted according to the dynamic adjustment coefficient;

[0047] When receiving the adjustment signal of the gas flow corresponding to any film layer deposited by APCVD, the valve opening of the gas supply device of the reaction chamber is adjusted according to the dynamic adjustment coefficient;

[0048] When receiving the adjustment signal of the target material sputtering rate or film layer composition corresponding to any film layer deposited by PVD, the sputtering power of the PVD equipment is adjusted according to the dynamic adjustment coefficient.

[0049] Preferably, the data acquisition and transmission module adopts a redundant design and is provided with a main data transmission line and an auxiliary data transmission line; the data acquisition and transmission module also includes a line fault monitoring unit, which is used to perform a fault assessment on the data transmission line corresponding to the plating information to obtain a line assessment value;

[0050] Set a line fault threshold. If the line evaluation value is greater than its line fault threshold, it means that the data transmission route has a fault, and then switch to the auxiliary data transmission line to transmit the plating information.

[0051] Preferably, a fault assessment is performed on the data transmission line corresponding to the plating information, specifically:

[0052] Obtaining fault impact information on data transmission lines, including electrical characteristics, signal quality information for transmitted data, and line physical status and characteristics. Electrical characteristics include line resistance, capacitance, and inductance; signal quality information includes signal strength, signal-to-noise ratio, and bit error rate; and line physical status and characteristics include line temperature, connection status, transmission delay, and packet loss rate.

[0053] A normal value is set for any parameter in the fault impact information, and the difference between the numerical value of any parameter in the fault impact information and the normal value of the parameter is calculated to obtain a normal difference; the normal differences of all parameters in the fault impact information are weighted to obtain a line evaluation value.

[0054] Compared with related technologies, the method for preparing all-solid-state inorganic electrochromic glass and the monitoring and control system provided by the present invention have the following beneficial effects:

[0055] By combining APCVD and PVD processes, the present invention achieves a dual reduction in equipment investment and material costs. By combining the precise control of the APCVD process with the high deposition rate of the PVD process, the effective deposition speed is improved, ensuring the uniformity and quality of the film layer. By adding two insulating layers on both sides of the electrochromic layer, the leakage phenomenon is effectively reduced, the energy loss is reduced, and the aging process of the film layer is slowed down. In addition, the structural design also achieves uniform color change over a large area, improving the visual effect and application value.

[0056] 2. The monitoring and control system proposed in the present invention can perform real-time monitoring and adjustment according to the characteristics of the membrane layer, ensuring parameter optimization during the production process, reducing rework and waste, and ensuring a high product qualification rate. Through the intelligent monitoring and control mechanism, the production process is made more flexible and can quickly respond to different production needs, thereby improving production efficiency and the market competitiveness of products. BRIEF DESCRIPTION OF THE DRAWINGS

[0057] Figure 1 A flowchart of a method for preparing all-solid-state inorganic electrochromic glass provided by the present invention;

[0058] Figure 2 This is a system block diagram of a monitoring and control system for the preparation of all-solid-state inorganic electrochromic glass provided by the present invention. DETAILED DESCRIPTION

[0059] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. 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 making creative efforts are within the scope of protection of the present invention.

[0060] The terms used in this disclosure are for the purpose of describing specific embodiments only and are not intended to limit the disclosure. As used in this disclosure and the appended claims, the singular forms "group," "class," and "the" are intended to include the plural forms, unless the context clearly indicates otherwise. It should also be understood that the term "and / or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.

[0061] It should be understood that although the terms first, second, third, etc. may be used in this disclosure to describe various information, such information should not be limited to these terms. These terms are only used to distinguish information of the same type from each other. For example, without departing from the scope of this disclosure, first information may also be referred to as second information, and similarly, second information may also be referred to as first information. Depending on the context, the word "if" as used herein may be interpreted as "at the time of" or "when" or "in response to determining."

[0062] Please refer to Figure 1-Figure 2 A method for preparing all-solid-state inorganic electrochromic glass comprises the following steps:

[0063] S1, glass substrate preparation;

[0064] S2, APCVD deposition film:

[0065] S21, depositing a first conductive film layer on the glass substrate; it should be noted that when depositing the first conductive film layer on the glass substrate, in the first thin film reaction chamber of the float line, when the glass substrate passes at a stable speed, a source material (TEOS or SiH4) is first introduced into the reaction chamber, and a chemical reaction occurs at a high temperature to generate SIO2, wherein SIO2 serves as an intermediate transition layer, effectively preventing other metal ions (such as Na+ and Ca2+) from migrating from the glass substrate to the conductive film (such as the first conductive layer FTO), avoiding corrosion or performance impact on the conductive film, improving the flatness of the glass surface to a certain extent, and providing a better substrate for subsequent thin film deposition; then, tin tetrachloride and hydrogen fluoride gases are introduced, and a chemical reaction occurs in a high temperature environment to generate a fluorine-doped tin oxide thin film (FTO) and uniformly deposited on the glass substrate;

[0066] S22, forming a first insulating layer on the first conductive film layer. It should be noted that, after the glass substrate enters the second thin film reaction chamber of the float line, a specific precursor compound gas such as Si, Ti, Sn, or Al is introduced into the reaction chamber, where a chemical reaction occurs at a high temperature to generate a SiO2, TiO2, SnO2, or Al2O3 thin film, which is then deposited on the first conductive film layer to form the first insulating layer.

[0067] S23, coating a main color-changing layer on the first insulating layer to obtain an electrochromic layer. It should be noted that the glass substrate enters the third thin-film reaction chamber of the float line, into which an appropriate amount of tungsten compound gas (such as tungsten hexachloride (WCL6) or tungsten hexafluoride (WF6)) is introduced, where a chemical reaction occurs at high temperature to generate a WO3 thin film which is deposited on the first insulating layer to form the electrochromic layer.

[0068] S3, PVD deposition film:

[0069] S31, forming a second insulating layer on the electrochromic layer; it should be noted that PVD deposition technology is used to deposit tungsten oxide, tungsten oxynitride, or other materials on the electrochromic layer as the second insulating layer; in a vacuum environment, target material atoms or molecules are deposited onto the glass surface by sputtering or evaporation; parameters such as sputtering power, vacuum level, deposition time, and temperature are precisely controlled to ensure the quality and uniformity of the second insulating layer;

[0070] S32, depositing an electrochromic storage layer on the second insulating layer. It should be noted that a metal oxide such as nickel-tungsten, nickel-tungsten-tantalum, nickel-tungsten-niobium, or nickel-tungsten-tin is deposited on the second insulating layer using PVD technology as the electrochromic storage layer.

[0071] S33, depositing a second conductive layer on the electrochromic storage layer; it should be noted that indium tin oxide (ITO) is deposited on the electrochromic storage layer by PVD as the second conductive layer.

[0072] It should be noted that when the first conductive film layer is plated on the glass substrate, in the first thin film reaction chamber of the float line, when the glass substrate passes at a stable speed, tin tetrachloride and hydrogen fluoride gases are precisely introduced into the reaction chamber, and a chemical reaction occurs in a high-temperature environment to generate a fluorine-doped tin oxide thin film (FTO) and evenly deposited on the glass substrate.

[0073] In the present application, based on step S2, when depositing the film layer by APCVD, the first conductive film layer, the first insulating layer and the electrochromic layer are respectively deposited in the first thin film reaction chamber of the float line, the second thin film reaction chamber of the float line and the third thin film reaction chamber of the float line.

[0074] In the present application, a monitoring and control system for the preparation of all-solid-state inorganic electrochromic glass is provided, wherein the monitoring and control system includes a data acquisition and transmission module, a data analysis and control module, and an adjustment and optimization module;

[0075] The data acquisition and transmission module is used to collect the plating information of any film layer deposited by APCVD or PVD in the corresponding reaction chamber or equipment. The plating information of the APCVD deposited film layer includes parameter information related to the deposited film, such as temperature and gas flow rate. The plating information of the PVD deposited film layer includes parameter information related to the deposited film, such as target sputtering power, gas flow rate, and film layer characteristics.

[0076] A data analysis and control module is used to perform plating analysis on the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer, and obtain plating analysis results; wherein the plating analysis results include preset difference values, preset difference mean values, preset fluctuation values, preset extreme values, preset difference values ​​and corresponding adjustment signals of the parameters in the plating information; analyze the film thickness and optical properties of any film layer during APCVD deposition and PVD deposition to obtain film thickness influence values ​​and optical characteristic comprehensive shadow values; perform weighted processing on the preset difference values, film thickness influence values ​​and optical characteristic comprehensive shadow values ​​of the parameters in the plating information to obtain mutual influence coefficients; when generating adjustment signals corresponding to the parameters, calculate the dynamic adjustment coefficients corresponding to the parameters; mark the adjustment signals of the parameters in the plating information and the corresponding dynamic adjustment coefficients as dynamic adjustment parameters;

[0077] The adjustment and optimization module is used to receive dynamic adjustment parameters and perform corresponding adjustment operations according to the dynamic adjustment parameters.

[0078] In this application, the data analysis and control module includes a time zone division unit, a plating status analysis unit, a thickness and optical change analysis unit, and an information summary analysis and processing unit;

[0079] A time zone division unit is used to mark the initial moment of APCVD deposition or PVD deposition of the corresponding film layer as the first moment, and mark the time zone between the first moment and the current moment as the film layer deposition time zone;

[0080] A plating state analysis unit is used to perform plating analysis on the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer, and obtain plating analysis results; wherein the plating analysis results include preset difference values, preset difference mean values, preset fluctuation values, preset extreme values, preset difference shadow values ​​and corresponding adjustment signals of the parameters in the plating information;

[0081] Thickness and optical change analysis unit, used to analyze the film thickness and optical characteristics of any film layer during APCVD deposition and PVD deposition, and obtain the film thickness impact value and optical characteristic comprehensive shadow value;

[0082] The information summary analysis processing unit is used to perform weighted processing on the preset differential value, film thickness influence value, and optical characteristic comprehensive value of the parameters in the plating information to obtain the mutual influence coefficient X; when receiving the adjustment signaling corresponding to the parameter, the preset differential value and mutual influence coefficient are used to calculate the dynamic adjustment coefficient K of the parameter, which is expressed by the formula: ; Wherein, k represents the adjustment proportional coefficient corresponding to the parameter in the plating information;

[0083] The parameter adjustment signaling in the plating information and the corresponding dynamic adjustment coefficient are marked as dynamic adjustment parameters.

[0084] In the present application, the monitoring and control system also includes a monitoring setting module, which is used to respectively set a temperature sensor, a gas flow sensor and a film thickness monitor in the reaction chamber for APCVD deposition of the first conductive film layer, the first insulating layer and the electrochromic layer; and is also used to set a sputtering rate monitor, a vacuum monitor and a thin film optical property analyzer in the equipment corresponding to the PVD deposition of the second insulating layer, the electrochromic storage layer and the second conductive layer.

[0085] In this application, the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer is analyzed separately, specifically:

[0086] According to the preset value of any parameter in the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer; performing difference calculation between any parameter in the plating information and the preset value of the parameter to obtain a preset difference value YD1; identifying the preset differences of all acquisition moments within the film layer plating time zone, and performing mean, standard deviation, maximum and minimum calculation on the preset differences within the film layer plating time zone to obtain a preset difference mean value YD2, a preset fluctuation value YD3, and a preset extreme difference value YD4;

[0087] The preset difference value YD is obtained by weighted calculation of the preset difference value, the preset difference mean value, the preset fluctuation value, and the preset extreme value. The formula is: ; Among them, d1, d2, d3, and d4 represent the weight influence factors corresponding to the preset difference, preset difference mean, preset fluctuation value, and preset extreme value respectively;

[0088] Set the allowable variation range of any parameter in the plating information, match the preset difference value of the parameter in the plating information with the allowable variation range corresponding to the parameter, if the preset difference value is within its allowable variation range, it indicates that the parameter is in a normal state; if the preset difference value is not within its allowable variation range, it indicates that the parameter is in a deviated state, and generate an adjustment signaling corresponding to the parameter;

[0089] The preset difference value, preset difference mean value, preset fluctuation value, preset range value, preset difference value and corresponding adjustment signaling and corresponding dynamic adjustment coefficient of the parameters in the plating information are marked as plating analysis results.

[0090] In this application, the film thickness and optical properties of any film layer deposited by APCVD and PVD are analyzed, specifically:

[0091] Obtain the film thickness of any film layer during APCVD deposition or PVD deposition at all acquisition moments within the film coating time zone; calculate the difference between the film thicknesses at adjacent acquisition moments to obtain the film thickness change value MH1;

[0092] The film thickness variation value within the coating time zone is calculated by the mean and standard deviation to obtain the film thickness variation mean MH2 and film thickness fluctuation value MH3;

[0093] Obtaining the preset thickness of the film layer, identifying the maximum thickness of the film layer in the film layer plating zone, and performing difference calculation between the maximum thickness and the preset thickness to obtain an expected thickness difference MH4;

[0094] The film thickness influence value MH is obtained by weighted calculation of the current film thickness change value, the mean film thickness change value, the film thickness fluctuation value, and the expected thickness difference. The formula is: ; Among them, m1, m2, m3, and m4 represent the weighted influencing factors corresponding to the film thickness change value, the film thickness change mean value, the film thickness fluctuation value, and the expected thickness difference value, respectively;

[0095] Obtain optical property information of APCVD and PVD deposited films at all acquisition moments within the film coating time zone; optical property information includes the light transmittance, reflectivity, and absorptivity of the film at a specific wavelength;

[0096] Construct a graph showing how light transmittance, reflectance, and absorptance vary with wavelength, identify the corresponding light transmittance, reflectance, and absorptance curves in the graph, and calculate the smoothness of the curves using numerical analysis methods.

[0097] Identify the smoothness of the curves corresponding to the light transmittance, reflectivity, and absorptivity at all acquisition moments within the film coating time zone; calculate statistical indicators of the smoothness of the curve corresponding to any parameter in the optical characteristic information within the film coating time zone, including the average value, variance, maximum value, and minimum value; set a smoothing qualified value for the curve corresponding to any parameter in the optical characteristic information, and perform a difference calculation between the smoothness of the curve corresponding to any parameter in the optical characteristic information and its smoothing qualified value to obtain a smoothing qualified difference;

[0098] The smoothing influence value is obtained by weighting the smoothing qualified difference and the statistical index of smoothness;

[0099] Then, the characteristic peaks in the curve are identified by the peak detection algorithm, and the movement of the peak position and the increase and decrease of the intensity of the characteristic peaks in the film coating time zone are analyzed. Specifically:

[0100] The acquisition time in the film coating time zone is numbered as i, and the number of the characteristic peak is represented as j; the peak position wavelength value of the characteristic peak at the i-th acquisition time in the film coating time zone is represented as ; Count the number of characteristic peaks in the film coating time zone to represent m; calculate the difference between the peak wavelength values ​​of the characteristic peaks at different acquisition times to obtain the peak position shift , the formula is: ;in, Indicates the peak wavelength value of the jth characteristic peak at the initial acquisition time;

[0101] The peak movement rate v is calculated based on the peak movement amount, and the formula is: , where ti and t0 represent the i-th acquisition time and the initial acquisition time in the film coating time zone, respectively;

[0102] Obtain the intensity value of the characteristic peak at any collection time within the film coating time zone, construct a line graph of the change of the intensity value of the characteristic peak with the peak intensity at the collection time, input the collection time and the intensity value of the characteristic peak into the peak change line graph, mark the position of the intensity value of the characteristic peak in the line graph as the peak point, connect adjacent peak points to obtain a peak line; calculate the slope of the peak line, mark the slope with a positive value as a positive slope value, and mark the slope with a negative value as a negative slope value; sum up all the positive slope values ​​and negative slope values ​​in the peak change line graph to obtain a positive slope total value and a negative slope total value, and perform weighted calculation on the positive slope total value and the negative slope total value to obtain a peak intensity influence value;

[0103] Perform weighted calculation on the smoothing influence value, peak position moving rate and peak position intensity influence value to obtain the parameter comprehensive value corresponding to the parameter in the optical characteristic information;

[0104] Then, the weighted calculation of the comprehensive shadow values ​​of all parameters in the optical characteristic information is performed to obtain the comprehensive shadow value of the optical characteristic.

[0105] In this application, corresponding adjustment operations are performed according to the dynamic adjustment parameters, specifically:

[0106] When receiving the temperature adjustment signal corresponding to any film layer deposited by APCVD, the device supporting the reaction chamber of the corresponding film layer is adjusted according to the dynamic adjustment coefficient;

[0107] When receiving the adjustment signal of the gas flow corresponding to any film layer deposited by APCVD, the valve opening of the gas supply device of the reaction chamber is adjusted according to the dynamic adjustment coefficient;

[0108] When receiving the adjustment signal of the target material sputtering rate or film layer composition corresponding to any film layer deposited by PVD, the sputtering power of the PVD equipment is adjusted according to the dynamic adjustment coefficient.

[0109] In the present application, the data acquisition and transmission module adopts a redundant design and is provided with a main data transmission line and an auxiliary data transmission line; the data acquisition and transmission module also includes a line fault monitoring unit, which is used to perform a fault assessment on the data transmission line corresponding to the plating information to obtain a line assessment value;

[0110] Set a line fault threshold. If the line evaluation value is greater than its line fault threshold, it means that the data transmission route has a fault, and then switch to the auxiliary data transmission line to transmit the plating information.

[0111] In this application, a fault assessment is performed on the data transmission line corresponding to the plating information, specifically:

[0112] Obtaining fault impact information on data transmission lines, including electrical characteristics, signal quality information for transmitted data, and line physical status and characteristics. Electrical characteristics include line resistance, capacitance, and inductance; signal quality information includes signal strength, signal-to-noise ratio, and bit error rate; and line physical status and characteristics include line temperature, connection status, transmission delay, and packet loss rate.

[0113] A normal value is set for any parameter in the fault impact information, and the difference between the numerical value of any parameter in the fault impact information and the normal value of the parameter is calculated to obtain a normal difference; the normal differences of all parameters in the fault impact information are weighted to obtain a line evaluation value.

[0114] Other embodiments of the present invention will readily occur to those skilled in the art after considering the specification and practicing the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the present invention that follow the general principles of the invention and include common knowledge or customary techniques in the art not disclosed herein. The description and examples are to be considered as exemplary only, with the true scope and spirit of the invention being indicated by the following claims.

[0115] It should be understood that the present invention is not limited to the exact construction described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of the present invention is limited only by the appended claims.

Claims

1. A method for preparing all-solid-state inorganic electrochromic glass, characterized in that: The following steps are involved: S1, glass substrate preparation; S2, APCVD deposition film: S21, depositing a first conductive film layer on the glass substrate; S22, depositing a first insulating layer on the first conductive film layer; S23, plating a main color-changing layer on the first insulating layer to obtain an electrochromic layer; S3, PVD deposition film: S31, plating a second insulating layer on the electrochromic layer; S32, depositing an electrochromic storage layer on the second insulating layer; S33, depositing a second conductive layer on the electrochromic storage layer; Furthermore, the preparation method further comprises a monitoring and control system for controlling the preparation process, wherein the monitoring and control system comprises a data acquisition and transmission module, a data analysis and control module, and an adjustment and optimization module: Data acquisition and transmission module, used to collect plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer; Data analysis and control module, including time zone division unit, plating status analysis unit, thickness and optical change analysis unit, information summary analysis and processing unit; A time zone division unit is used to mark the initial moment of APCVD deposition or PVD deposition of the corresponding film layer as the first moment, and mark the time zone between the first moment and the current moment as the film layer deposition time zone; A plating state analysis unit is used to perform plating analysis on the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer, and obtain plating analysis results; wherein the plating analysis results include a preset difference value, a preset difference mean value, a preset fluctuation value, a preset extreme value, a preset difference value, a corresponding adjustment signaling, and a corresponding dynamic adjustment coefficient of the parameters in the plating information; The logic for obtaining the preset difference value is: According to the preset value of any parameter in the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer; performing difference calculation between any parameter in the plating information and the preset value of the parameter to obtain a preset difference; identifying the preset difference values ​​of all acquisition moments within the film layer plating time zone, performing mean, standard deviation, maximum and minimum calculation on the preset difference values ​​within the film layer plating time zone, and obtaining a preset difference mean, a preset fluctuation value and a preset range value; Perform weighted calculation on the preset difference value, the preset difference mean value, the preset fluctuation value, and the preset extreme value to obtain the preset difference value; The thickness and optical change analysis unit is used to analyze the thickness and optical characteristics of any film layer during APCVD and PVD deposition, specifically: Obtain the film thickness of any film layer during APCVD deposition or PVD deposition at all acquisition moments within the film coating time zone; perform difference calculation on the film thickness at adjacent acquisition moments to obtain the film thickness change value; The film thickness variation value within the film coating time zone is calculated by the mean and standard deviation to obtain the film thickness variation mean and film thickness fluctuation value; Obtaining a preset thickness of the film layer, identifying the maximum thickness of the film layer in the film layer plating zone, and performing difference calculation between the maximum thickness and the preset thickness to obtain an expected thickness difference; The film thickness influence value is obtained by weighted calculation of the current film thickness change value, the film thickness change mean value, the film thickness fluctuation value, and the expected thickness difference value; Obtain optical property information of APCVD and PVD deposited films at all acquisition moments within the film coating time zone; optical property information includes the light transmittance, reflectivity, and absorptivity of the film at a specific wavelength; Construct a graph showing how light transmittance, reflectance, and absorptance vary with wavelength, identify the corresponding light transmittance, reflectance, and absorptance curves in the graph, and calculate the smoothness of the curves using numerical analysis methods. Identify the smoothness of the curves corresponding to the light transmittance, reflectivity, and absorptivity at all acquisition moments within the film coating time zone; calculate statistical indicators of the smoothness of the curve corresponding to any parameter in the optical characteristic information within the film coating time zone, including the average value, variance, maximum value, and minimum value; set a smoothing qualified value for the curve corresponding to any parameter in the optical characteristic information, and perform a difference calculation between the smoothness of the curve corresponding to any parameter in the optical characteristic information and its smoothing qualified value to obtain a smoothing qualified difference; The smoothing influence value is obtained by weighting the smoothing qualified difference and the statistical index of smoothness; Then, the characteristic peak in the curve is identified by the peak detection algorithm, and the peak position movement and intensity increase and decrease of the characteristic peak in the film coating time zone are analyzed to obtain the peak position movement rate and peak position intensity impact value; Perform weighted calculation on the smoothing influence value, peak position moving rate and peak position intensity influence value to obtain the parameter comprehensive value corresponding to the parameter in the optical characteristic information; Then, the weighted calculation of the comprehensive shadow values ​​of all parameters in the optical characteristic information is performed to obtain the comprehensive shadow value of the optical characteristic; The information summary analysis processing unit is used to perform weighted processing on the preset differential image value, film thickness influence value, and optical characteristic comprehensive image value of the parameters in the plating information to obtain the mutual influence coefficient; when receiving the adjustment signaling corresponding to the parameter, the preset differential image value and the mutual influence coefficient are used to calculate the dynamic adjustment coefficient of the parameter; Marking the parameter adjustment signaling in the plating information and the corresponding dynamic adjustment coefficient as dynamic adjustment parameters; The adjustment and optimization module is used to receive dynamic adjustment parameters and perform corresponding adjustment operations according to the dynamic adjustment parameters.

2. The method for preparing all-solid-state inorganic electrochromic glass according to claim 1, characterized in that: Based on step S2, during APCVD film deposition, the first conductive film layer, the first insulating layer and the electrochromic layer are deposited in the first thin film reaction chamber of the float line, the second thin film reaction chamber of the float line and the third thin film reaction chamber of the float line respectively.

3. The method for preparing all-solid-state inorganic electrochromic glass according to claim 1, characterized in that: The monitoring and control system also includes a monitoring setting module, which is used to respectively set a temperature sensor, a gas flow sensor and a film thickness monitor in the reaction chamber for APCVD deposition of the first conductive film layer, the first insulating layer and the electrochromic layer; and is also used to set a sputtering rate monitor, a vacuum monitor and a thin film optical property analyzer in the equipment corresponding to the PVD deposition of the second insulating layer, the electrochromic storage layer and the second conductive layer.

4. The method for preparing all-solid-state inorganic electrochromic glass according to claim 1, characterized in that: The plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer is analyzed separately, specifically: Set the allowable variation range of any parameter in the plating information, and match the preset differential value of the parameter in the plating information with the allowable variation range corresponding to the parameter. If the preset differential value is within its allowable variation range, it indicates that the parameter is in a normal state; If the preset difference value is not within its allowable variation range, it indicates that the parameter is in a deviation state, and an adjustment signaling corresponding to the parameter is generated; The preset difference value, preset difference mean value, preset fluctuation value, preset range value, preset difference value and corresponding adjustment signaling and corresponding dynamic adjustment coefficient of the parameters in the plating information are marked as plating analysis results.

5. The method for preparing all-solid-state inorganic electrochromic glass according to claim 1, characterized in that: Perform corresponding adjustment operations based on dynamic adjustment parameters, specifically: When receiving the temperature adjustment signal corresponding to any film layer deposited by APCVD, the device supporting the reaction chamber of the corresponding film layer is adjusted according to the dynamic adjustment coefficient; When receiving the adjustment signal of the gas flow corresponding to any film layer deposited by APCVD, the valve opening of the gas supply device of the reaction chamber is adjusted according to the dynamic adjustment coefficient; When receiving the adjustment signal of the target material sputtering rate or film layer composition corresponding to any film layer deposited by PVD, the sputtering power of the PVD equipment is adjusted according to the dynamic adjustment coefficient.

6. The method for preparing all-solid-state inorganic electrochromic glass according to claim 1, characterized in that: The data acquisition and transmission module adopts a redundant design and is provided with a main data transmission line and an auxiliary data transmission line; the data acquisition and transmission module also includes a line fault monitoring unit, which is used to perform a fault assessment on the data transmission line corresponding to the plating information to obtain a line assessment value; Set a line fault threshold. If the line evaluation value is greater than its line fault threshold, it means that the data transmission route has a fault, and then switch to the auxiliary data transmission line to transmit the plating information.

7. The method for preparing all-solid-state inorganic electrochromic glass according to claim 6, characterized in that: Perform fault assessment on the data transmission line corresponding to the plating information, specifically: Obtaining fault impact information on data transmission lines, including electrical characteristics, signal quality information for transmitted data, and line physical status and characteristics. Electrical characteristics include line resistance, capacitance, and inductance; signal quality information includes signal strength, signal-to-noise ratio, and bit error rate; and line physical status and characteristics include line temperature, connection status, transmission delay, and packet loss rate. A normal value is set for any parameter in the fault impact information, and the difference between the numerical value of any parameter in the fault impact information and the normal value of the parameter is calculated to obtain a normal difference; the normal differences of all parameters in the fault impact information are weighted to obtain a line evaluation value.

Citation Information

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