All-solid-state inorganic electrochromic glass preparation method and monitoring regulation and control system

Abstract

The invention provides an all-solid-state inorganic electrochromic glass preparation method and a monitoring regulation and control system, and relates to the technical field of glass preparation, and the method comprises the following steps: APCVD deposition of a film layer: plating a glass substrate with a first conductive film layer; 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 film layer deposition: plating a second insulating layer on the electrochromic layer; plating an electrochromic storage layer on the second insulating layer; and plating a second conductive layer on the electrochromic storage layer. By combining the APCVD and PVD processes, double reduction of equipment investment and material cost is realized, accurate control of the APCVD process and high deposition rate of the PVD process are combined, effective deposition rate is increased, uniformity and quality of a film layer are ensured, and two insulating layers are added on two sides of the electrochromic layer, so that electric leakage is effectively reduced, and the electrochromic effect is improved. The energy loss is reduced, and the aging process of the film layer is slowed down.

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 construction field to achieve dynamic regulation of sunlight radiation and indoor lighting, and reduce building energy consumption; in the automotive industry, it can be used in car windows and skylights to improve the driving experience and the intelligence level of vehicles; in the field of electronic display, it is expected to become a new type of display device or dimming element, expanding the application scope of display technology. Therefore, its market demand is growing, which is of great significance to the improvement and innovation of the preparation process.

[0003] In the prior art, the preparation of all-solid-state inorganic electrochromic glass is usually carried out by sequentially depositing five nano-film layers on a glass substrate using PVD (physical vapor deposition) equipment. These five film 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 conductive layer and the second conductive layer, the ions move under the action of the electric field. When lithium ions enter the electrochromic layer, the transmittance of the glass decreases; and when lithium ions enter the electrochromic storage layer, the transmittance increases. By switching the positive and negative poles of the DC voltage, the transmittance of the glass can be increased or decreased.

[0004] Based on the above, the existing preparation method relies on PVD equipment to deposit the film layer, which has a slow deposition speed, takes a long time for large-scale production, increases the equipment depreciation cost, and its materials are expensive, which limits the industrial development of all-solid-state inorganic electrochromic glass. In addition, the existing technology has the problem of large leakage, which will lead to energy waste and film aging, performance degradation, and make the electrochromic glass unevenly discolored and slow to respond. Therefore, it is necessary to provide a method for preparing all-solid-state inorganic electrochromic glass to solve the above technical problems. 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 an all-solid-state inorganic electrochromic glass, comprising the following steps: S1, glass substrate preparation; S2, APCVD deposition film: S21, coating a first conductive film layer on the glass substrate; S22, plating 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 deposited film: S31, plating a second insulating layer on the electrochromic layer; S32, plating an electrochromic storage layer on the second insulating layer; S33, depositing a second conductive layer on the electrochromic storage layer.

[0007] Preferably, based on step S2, when depositing the film 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.

[0008] 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; Data acquisition and transmission module, used to collect plating information in the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer; 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, respectively, to 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 and corresponding dynamic adjustment coefficients 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 ​​and film thickness influence 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; The adjustment and optimization module is used to receive dynamic adjustment parameters and perform corresponding adjustment operations according to the dynamic adjustment parameters.

[0009] 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; A time zone division unit, used for marking the initial moment of APCVD deposition or PVD equipment depositing the corresponding film layer as the first moment, and marking the time zone between the first moment and the current moment as the film layer plating time zone; A plating state analysis unit, 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 value values, preset difference image values ​​and corresponding adjustment signals of parameters in the plating information; 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; 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 signal 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 The adjustment signaling of the parameters in the plating information and the corresponding dynamic adjustment coefficient are marked as dynamic adjustment parameters.

[0010] 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.

[0011] Preferably, plating analysis is performed on the plating information of the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer, specifically: 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 of all acquisition moments in the film layer plating time zone, performing mean, standard deviation, maximum and minimum calculation on the preset difference in the film layer plating time zone, and obtaining a preset difference mean, a preset fluctuation value and a preset extreme value; The preset difference value, the preset difference mean value, the preset fluctuation value, and the preset extreme value are weightedly calculated to obtain the preset difference image value; Set the allowable variation range of any parameter in the plating information, match the preset differential image value of the parameter in the plating information with the allowable variation range corresponding to the parameter, if the preset differential image value is within its allowable variation range, it indicates that the parameter is in a normal state; if the preset differential image value is not within its allowable variation range, it indicates that the parameter is in a deviated state, and generate an adjustment signal corresponding to the parameter; The preset difference value, preset difference mean value, preset fluctuation value, preset extreme value, preset difference value of the parameters in the plating information and the corresponding adjustment signaling and the corresponding dynamic adjustment coefficient are marked as plating analysis results.

[0012] Preferably, the film thickness and optical properties of any film layer deposited by APCVD and PVD are analyzed, 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 value and film thickness fluctuation value; Obtaining the preset thickness of the film layer, identifying the maximum value of the film layer thickness in the film layer plating time zone and performing difference calculation with the preset thickness to obtain an expected thickness difference; The film thickness change value at the current moment is weightedly calculated with the film thickness change mean value, the film thickness fluctuation value, and the expected thickness difference value to obtain the film thickness influence value; Obtain the optical property information of APCVD deposited and PVD deposited films at all acquisition moments within the film coating time zone; the optical property information includes the light transmittance, reflectivity and absorptivity of the film at a specific wavelength; Construct a graph of light transmittance, reflectance and absorptance as a function of wavelength, identify the corresponding light transmittance, reflectance and absorptance curves in the graph; calculate the smoothness of the curve using a numerical analysis method; Identify the smoothness of the curves corresponding to the light transmittance, reflectivity and absorptivity at all acquisition moments in the film coating time zone; calculate the statistical indicators of the smoothness of the curve corresponding to any parameter in the optical characteristic information in the film coating time zone, including the average value, variance, maximum value and minimum value; set the smoothness qualified value of the curve corresponding to any parameter in the optical characteristic information, and perform difference calculation between the smoothness of the curve corresponding to any parameter in the optical characteristic information and its smoothness qualified value to obtain the smoothness qualified difference; The smoothing influence value is obtained by weighted calculation of 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 influence value; The smoothing influence value, the peak position moving rate and the peak position intensity influence value are weightedly calculated to obtain the parameter comprehensive value corresponding to the parameter in the optical characteristic information; Then, the comprehensive image values ​​of all parameters in the optical characteristic information are weightedly calculated to obtain the comprehensive image value of the optical characteristic.

[0013] Preferably, corresponding adjustment operations are performed according to the dynamic adjustment parameters, specifically: When receiving the adjustment signal of the temperature corresponding to any film layer deposited by APCVD, the device supporting the reaction chamber controlling 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 matched with the reaction chamber is adjusted according to the dynamic adjustment coefficient; When receiving an adjustment signal of a target material sputtering rate or a 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.

[0014] 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; Set a line fault threshold. If the line evaluation value is greater than its line fault threshold, it means that the data transmission route is faulty, then switch to the auxiliary data transmission line to transmit the plating information.

[0015] Preferably, a fault assessment is performed on the data transmission line corresponding to the plating information, specifically: Obtaining fault impact information of the data transmission line, including electrical characteristic information, signal quality information of the transmitted data, and line physical state and characteristic information; wherein the electrical characteristic information includes the resistance value, capacitance value, and inductance value of the line, the signal quality information includes the signal strength, signal-to-noise ratio, bit error rate, and the line physical state and characteristic information includes the line temperature, connection status, transmission delay, and data packet loss rate; A normal value of a parameter is set for any parameter in the fault impact information, and a difference is calculated between the numerical value of any parameter in the fault impact information and the normal value of the parameter to obtain a normal difference; and the normal differences of all parameters in the fault impact information are weighted to obtain a line evaluation value.

[0016] Compared with the related art, the all-solid-state inorganic electrochromic glass preparation method and monitoring and control system provided by the present invention have the following beneficial effects: The present invention achieves a dual reduction in equipment investment and material cost by combining 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, leakage is effectively reduced, 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, thereby improving the visual effect and application value.

[0017] 2. The monitoring and control system proposed in the present invention can perform real-time monitoring and adjustment according to the characteristics of the film layer, ensuring parameter optimization in 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 more flexible and can quickly respond to different production needs, thereby improving production efficiency and product market competitiveness. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 A flowchart of a method for preparing an all-solid-state inorganic electrochromic glass provided by the present invention; Figure 2 A system block diagram of a monitoring and control system for preparing all-solid-state inorganic electrochromic glass provided by the present invention. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] The terms used in this disclosure are for the purpose of describing specific embodiments only and are not intended to limit the disclosure. The singular forms of "group", "class" and "the" used in this disclosure and the appended claims are also intended to include plural forms unless the context clearly indicates otherwise. It should also be understood that the term "and / or" used herein refers to and includes any or all possible combinations of one or more associated listed items.

[0021] It should be understood that although the terms first, second, third, etc. may be used in the present disclosure to describe various information, such information should not be limited to these terms. These terms are only used to distinguish the same type of information from each other. For example, without departing from the scope of the present disclosure, the first information may also be referred to as the second information, and similarly, the second information may also be referred to as the 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".

[0022] Please refer to Figure 1-Figure 2 A method for preparing all-solid-state inorganic electrochromic glass comprises the following steps: S1, glass substrate preparation; S2, APCVD deposition film: S21, coating a first conductive film layer on a glass substrate; it should be noted that when coating the first conductive film layer on a glass substrate, in a first thin film reaction chamber of a 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 effects 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 gas are introduced, and a chemical reaction occurs in a high temperature environment to generate a fluorine-doped tin oxide film (FTO) and uniformly deposit it on the glass substrate; S22, coating 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 or Ti or Sn or AL is introduced into the reaction chamber, and a chemical reaction occurs at a high temperature to generate a SIO2 or TiO2 or SnO2 or AL2O3 thin film, which is deposited on the first conductive film layer to form a first insulating layer; 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, and an appropriate amount of tungsten compound (such as tungsten hexachloride (WCL6) or tungsten hexafluoride (WF6)) gas is introduced into the reaction chamber, and a chemical reaction occurs at a high temperature to generate a WO3 thin film and deposit it on the first insulating layer to form an electrochromic layer; S3, PVD deposited film: S31, plating a second insulating layer on the electrochromic layer; it should be noted that PVD deposition technology is used to deposit tungsten oxide, tungsten oxynitride and other materials on the electrochromic layer as the second insulating layer; in a vacuum environment, target atoms or molecules are deposited on the glass surface by sputtering or evaporation; parameters such as sputtering power, vacuum degree, deposition time, temperature, etc. are precisely controlled to ensure the quality and uniformity of the second insulating layer; S32, plating an electrochromic storage layer on the second insulating layer; it should be noted that the oxide of metals such as nickel-tungsten, nickel-tungsten-tantalum, nickel-tungsten-niobium, nickel-tungsten-tin, etc. is deposited on the second insulating layer using PVD technology as the electrochromic storage layer; S33, plating 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.

[0023] 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 accurately introduced into the reaction chamber, and a chemical reaction occurs in a high temperature environment to generate a fluorine-doped tin oxide film (FTO) and evenly deposited on the glass substrate.

[0024] 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 placed 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.

[0025] 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 comprises a data acquisition and transmission module, a data analysis and control module, and an adjustment and optimization module; The data acquisition and transmission module is used to collect the plating information of any film layer deposited by APCVD and 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, and the plating information of the PVD deposited film layer includes participating information related to the deposited film, such as target sputtering power, gas flow rate, and film layer characteristics; 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; The adjustment and optimization module is used to receive dynamic adjustment parameters and perform corresponding adjustment operations according to the dynamic adjustment parameters.

[0026] In the present application, 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; A time zone division unit, used for marking the initial moment of APCVD deposition or PVD equipment depositing the corresponding film layer as the first moment, and marking the time zone between the first moment and the current moment as the film layer plating time zone; A plating state analysis unit, 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 value values, preset difference image values ​​and corresponding adjustment signals of parameters in the plating information; 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; 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 X; when receiving the adjustment signal corresponding to the parameter, the preset differential image value and the mutual influence coefficient are used to calculate the dynamic adjustment coefficient K of the parameter, and the formula is expressed as: ; Wherein, k represents the adjustment proportional coefficient corresponding to the parameter in the plating information; The adjustment signaling of the parameters in the plating information and the corresponding dynamic adjustment coefficient are marked as dynamic adjustment parameters.

[0027] 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.

[0028] 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: 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 difference values ​​of all acquisition moments within the film layer plating time zone, performing mean, standard deviation, maximum and minimum value calculation on the preset difference values ​​within the film layer plating time zone, and obtaining a preset difference mean value YD2, a preset fluctuation value YD3, and a preset extreme value YD4; The preset difference value, the preset difference mean value, the preset fluctuation value, and the preset extreme value are weighted and calculated to obtain the preset difference value YD, which is expressed by the formula: ; Wherein, d1, d2, d3, and d4 represent the weight influence factors corresponding to the preset difference, the preset difference mean, the preset fluctuation value, and the preset extreme value, respectively; Set the allowable variation range of any parameter in the plating information, match the preset differential image value of the parameter in the plating information with the allowable variation range corresponding to the parameter, if the preset differential image value is within its allowable variation range, it indicates that the parameter is in a normal state; if the preset differential image value is not within its allowable variation range, it indicates that the parameter is in a deviated state, and generate an adjustment signal corresponding to the parameter; The preset difference value, preset difference mean value, preset fluctuation value, preset extreme value, preset difference value of the parameters in the plating information and the corresponding adjustment signaling and the corresponding dynamic adjustment coefficient are marked as plating analysis results.

[0029] In this application, the film thickness and optical properties of any film layer deposited by APCVD and PVD are analyzed, specifically: Obtain the film thickness of any film layer during APCVD deposition and 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 MH1; The film thickness variation value in the film coating time zone is calculated by the mean and standard deviation to obtain the film thickness variation mean MH2 and the film thickness fluctuation value MH3; Obtaining the preset thickness of the film layer, identifying the maximum value of the film layer thickness in the film layer plating time zone and performing difference calculation with the preset thickness to obtain an expected thickness difference MH4; The film thickness change value at the current moment is weighted by the film thickness change mean, film thickness fluctuation value, and expected thickness difference to obtain the film thickness influence value MH, which is expressed by the formula: ; 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; Obtain the optical property information of APCVD deposited and PVD deposited films at all acquisition moments within the film coating time zone; the optical property information includes the light transmittance, reflectivity and absorptivity of the film at a specific wavelength; Construct a graph of light transmittance, reflectance and absorptance as a function of wavelength, identify the corresponding light transmittance, reflectance and absorptance curves in the graph; calculate the smoothness of the curve using a numerical analysis method; Identify the smoothness of the curves corresponding to the light transmittance, reflectivity and absorptivity at all acquisition moments in the film coating time zone; calculate the statistical indicators of the smoothness of the curve corresponding to any parameter in the optical characteristic information in the film coating time zone, including the average value, variance, maximum value and minimum value; set the smoothness qualified value of the curve corresponding to any parameter in the optical characteristic information, and perform difference calculation between the smoothness of the curve corresponding to any parameter in the optical characteristic information and its smoothness qualified value to obtain the smoothness qualified difference; The smoothing influence value is obtained by weighted calculation of the smoothing qualified difference and the statistical index of smoothness; 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: The acquisition time in the film coating time zone is numbered as i, and the characteristic peak is numbered as j; the peak position wavelength value of the jth 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; The peak position shift is obtained by calculating the difference between the peak position wavelength values ​​of the characteristic peaks at different acquisition times , the formula is: ;in, Indicates the peak wavelength value of the jth characteristic peak at the initial acquisition time; 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; Obtain the intensity value of the characteristic peak at any collection time in the film coating time zone, construct a line graph of the intensity value of the characteristic peak versus the peak intensity at the collection time, input the collection time and the intensity value of the characteristic peak into the peak position 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 position 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; The smoothing influence value, the peak position moving rate and the peak position intensity influence value are weightedly calculated to obtain the parameter comprehensive value corresponding to the parameter in the optical characteristic information; Then, the comprehensive image values ​​of all parameters in the optical characteristic information are weightedly calculated to obtain the comprehensive image value of the optical characteristic.

[0030] In this application, corresponding adjustment operations are performed according to the dynamic adjustment parameters, specifically: When receiving the adjustment signal of the temperature corresponding to any film layer deposited by APCVD, the device supporting the reaction chamber controlling 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 matched with the reaction chamber is adjusted according to the dynamic adjustment coefficient; When receiving an adjustment signal of a target material sputtering rate or a 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.

[0031] 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; Set a line fault threshold. If the line evaluation value is greater than its line fault threshold, it means that the data transmission route is faulty, then switch to the auxiliary data transmission line to transmit the plating information.

[0032] In this application, a fault assessment is performed on the data transmission line corresponding to the plating information, specifically: Obtaining fault impact information of the data transmission line, including electrical characteristic information, signal quality information of the transmitted data, and line physical state and characteristic information; wherein the electrical characteristic information includes the resistance value, capacitance value, and inductance value of the line, the signal quality information includes the signal strength, signal-to-noise ratio, bit error rate, and the line physical state and characteristic information includes the line temperature, connection status, transmission delay, and data packet loss rate; A normal value of a parameter is set for any parameter in the fault impact information, and a difference is calculated between the numerical value of any parameter in the fault impact information and the normal value of the parameter to obtain a normal difference; and the normal differences of all parameters in the fault impact information are weighted to obtain a line evaluation value.

[0033] Those skilled in the art will readily appreciate other embodiments of the present invention 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 present invention and include common knowledge or customary techniques in the art that are not disclosed in this disclosure. The specification and examples are to be considered exemplary only, and the true scope and spirit of the present invention are indicated by the following claims.

[0034] It should be understood that the present invention is not limited to the exact construction that has been 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, coating a first conductive film layer on the glass substrate; S22, plating 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 deposited film: S31, plating a second insulating layer on the electrochromic layer; S32, plating an electrochromic storage layer on the second insulating layer; S33, depositing a second conductive layer on the electrochromic storage layer.

2. The method for preparing all-solid-state inorganic electrochromic glass according to claim 1, characterized in that: Based on step S2, when depositing the film 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.

3. A monitoring and control system for preparing all-solid-state inorganic electrochromic glass, using a method for preparing all-solid-state inorganic electrochromic glass according to any one of claims 1 to 2, characterized in that: The monitoring and control system includes 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 in the corresponding reaction chamber or equipment during APCVD deposition and PVD deposition of any film layer; 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 and corresponding dynamic adjustment coefficients 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; The adjustment and optimization module is used to receive dynamic adjustment parameters and perform corresponding adjustment operations according to the dynamic adjustment parameters.

4. The method for preparing all-solid-state inorganic electrochromic glass according to claim 3, characterized in that: 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; A time zone division unit, used for marking the initial moment of APCVD deposition or PVD equipment depositing the corresponding film layer as the first moment, and marking the time zone between the first moment and the current moment as the film layer plating time zone; A plating state analysis unit, 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 value values, preset difference shadow values ​​and corresponding adjustment signals and corresponding dynamic adjustment coefficients of parameters in the plating information; 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; 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 signal 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; The adjustment signaling of the parameters in the plating information and the corresponding dynamic adjustment coefficient are marked as dynamic adjustment parameters.

5. The method for preparing all-solid-state inorganic electrochromic glass according to claim 3, 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.

6. The method for preparing all-solid-state inorganic electrochromic glass according to claim 4, 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: 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; Identify the preset differences of all the acquisition moments in the film coating time zone, calculate the mean, standard deviation, maximum and minimum values ​​of the preset differences in the film coating time zone, and obtain the preset difference mean, preset fluctuation value and preset extreme value; The preset difference value, the preset difference mean value, the preset fluctuation value, and the preset extreme value are weightedly calculated to obtain the preset difference image value; 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 image 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 extreme value, preset difference value of the parameters in the plating information and the corresponding adjustment signaling and the corresponding dynamic adjustment coefficient are marked as plating analysis results.

7. The method for preparing all-solid-state inorganic electrochromic glass according to claim 4, characterized in that: The film thickness and optical properties of any film layer deposited by APCVD and PVD are analyzed, 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 value and film thickness fluctuation value; Obtaining the preset thickness of the film layer, identifying the maximum value of the film layer thickness in the film layer plating time zone and performing difference calculation with the preset thickness to obtain an expected thickness difference; The film thickness change value at the current moment is weightedly calculated with the film thickness change mean value, the film thickness fluctuation value, and the expected thickness difference value to obtain the film thickness influence value; Obtain the optical property information of APCVD deposited and PVD deposited films at all acquisition moments within the film coating time zone; the optical property information includes the light transmittance, reflectivity and absorptivity of the film at a specific wavelength; Construct a graph of light transmittance, reflectance and absorptance as a function of wavelength, identify the corresponding light transmittance, reflectance and absorptance curves in the graph; calculate the smoothness of the curve using a numerical analysis method; Identify the smoothness of the curves corresponding to the light transmittance, reflectivity and absorptivity at all acquisition moments in the film coating time zone; calculate the statistical indicators of the smoothness of the curve corresponding to any parameter in the optical characteristic information in the film coating time zone, including the mean value, variance, maximum value and minimum value; Setting a smooth pass value of a curve corresponding to any parameter in the optical characteristic information, performing a difference calculation between the smoothness of the curve corresponding to any parameter in the optical characteristic information and the smooth pass value thereof to obtain a smooth pass difference; The smoothing influence value is obtained by weighted calculation of 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 influence value; The smoothing influence value, the peak position moving rate and the peak position intensity influence value are weightedly calculated to obtain the parameter comprehensive value corresponding to the parameter in the optical characteristic information; Then, the comprehensive image values ​​of all parameters in the optical characteristic information are weightedly calculated to obtain the comprehensive image value of the optical characteristic.

8. The method for preparing all-solid-state inorganic electrochromic glass according to claim 3, characterized in that: Perform corresponding adjustment operations according to the dynamic adjustment parameters, specifically: When receiving the adjustment signal of the temperature corresponding to any film layer deposited by APCVD, the device supporting the reaction chamber controlling 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 matched with the reaction chamber is adjusted according to the dynamic adjustment coefficient; When receiving an adjustment signal of a target material sputtering rate or a 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.

9. The method for preparing all-solid-state inorganic electrochromic glass according to claim 3, 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 is faulty, then switch to the auxiliary data transmission line to transmit the plating information.

10. The method for preparing all-solid-state inorganic electrochromic glass according to claim 9, characterized in that: Perform fault assessment on the data transmission line corresponding to the plating information, specifically: Obtaining fault impact information of the data transmission line, including electrical characteristic information, signal quality information of the transmitted data, and line physical state and characteristic information; wherein the electrical characteristic information includes the resistance value, capacitance value, and inductance value of the line, the signal quality information includes the signal strength, signal-to-noise ratio, bit error rate, and the line physical state and characteristic information includes the line temperature, connection status, transmission delay, and data packet loss rate; A normal value of a parameter is set for any parameter in the fault impact information, and a difference is calculated between the numerical value of any parameter in the fault impact information and the normal value of the parameter to obtain a normal difference; and the normal differences of all parameters in the fault impact information are weighted to obtain a line evaluation value.

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