CN115524271A - Gas permeability measuring method, device, equipment and medium - Google Patents

Gas permeability measuring method, device, equipment and medium Download PDF

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CN115524271A
CN115524271A CN202110714636.2A CN202110714636A CN115524271A CN 115524271 A CN115524271 A CN 115524271A CN 202110714636 A CN202110714636 A CN 202110714636A CN 115524271 A CN115524271 A CN 115524271A
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gas
air pressure
detection
chamber
pressure data
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陈蓉
陈志平
单斌
曹坤
吴润卿
刘晨曦
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Huazhong University of Science and Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
    • G01N15/082Investigating permeability by forcing a fluid through a sample
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials
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Abstract

The invention discloses a method, a device, equipment and a medium for measuring gas permeability of a film, wherein the method comprises the following steps: acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, wherein the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber; performing regression processing on the air pressure data based on a Gaussian process regression algorithm to obtain predicted air pressure data; controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is within a preset air pressure range; and acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and the permeability calculation formula, wherein the valve is positioned between the accumulation chamber and the detection chamber. By using the gas permeability measuring method of the film, the detection error of an instrument can be effectively reduced, and the accuracy of a detection signal is improved.

Description

Gas permeability measuring method, device, equipment and medium
Technical Field
The present disclosure relates to permeability detection technologies, and particularly to a method, an apparatus, a device, and a medium for measuring gas permeability of a thin film.
Background
With the continuous development of flexible display panels, organic Light-Emitting Diode (OLED) display devices are widely used due to their advantages of self-luminescence, short response time, high contrast, wide viewing angle, and low power consumption. However, a significant factor restricting the development is that the organic light emitting layer is sensitive to water vapor and oxygen in the air, and a barrier film is required to prevent water and oxygen in the air from corroding the organic light emitting layer. Therefore, for OLED production, the production of high barrier films is a key technology among them. "high-end manufacturing is not performed without high-precision measurement", and a high-precision measurement means is required for preparing a film with high barrier property. Mass spectrometers are the most sophisticated devices for gas molecular measurements and are currently used in gas permeation measurements in many laboratories.
However, the barrier film has a long water oxygen permeability measurement period, the ionization efficiency of the mass spectrometer is gradually reduced along with the increase of the service time, and the final water oxygen permeability measurement is influenced by the fluctuation of the ambient temperature. Therefore, a measurement error occurs in actual measurement. The conventional detection technology is to accumulate gas permeating a film for a fixed time to achieve the function of signal amplification.
However, this method is not effective in improving the accuracy of the measurement signal, and in addition, the measurement signal is further distorted because the filament of the mass spectrometer reacts with oxygen and water vapor.
Disclosure of Invention
In view of the foregoing, it is necessary to provide a method, an apparatus, a device and a medium for measuring gas permeability of a thin film, which can effectively improve the accuracy of a measurement signal of gas permeability detected by a mass spectrometer.
In order to solve the above technical problem, a first aspect of the present application provides a method for measuring gas permeability of a membrane, the membrane to be measured divides the test cavity into an inlet chamber and an accumulation chamber, and test gas in the inlet chamber permeates through the membrane and enters the accumulation chamber, the method including:
acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, wherein the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber;
performing regression processing on the air pressure data based on a Gaussian process regression algorithm to obtain predicted air pressure data;
controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is within a preset air pressure range;
and acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and the permeability calculation formula, wherein the valve is positioned between the accumulation chamber and the detection chamber.
In the gas permeability measurement method in the above embodiment, the predicted gas pressure data is obtained by obtaining the gas pressure data of the gas pressure sensor and performing regression processing on the gas pressure data by using a gaussian process regression algorithm, so that the valve opening and closing time is controlled, the gas pressure value of the gas in the test chamber is kept within a preset range, and the gas permeability measurement value of the film to be measured is obtained according to the valve opening time and the permeability calculation formula. By using the gas permeability measuring method of the film, the detection error of an instrument can be effectively reduced, and the accuracy of a detection signal is improved.
In one embodiment, before acquiring the air pressure data detected by the air pressure sensor, the method includes:
acquiring a signal-to-noise ratio and detection time of real-time detection data detected by a mass spectrometer, wherein the mass spectrometer is positioned in the detection chamber; and if the signal-to-noise ratio is greater than or equal to a first preset threshold value and/or the detection time is greater than or equal to a second preset threshold value, acquiring air pressure data detected by the air pressure sensor.
In one embodiment, the method for measuring gas permeability of a membrane further comprises:
acquiring a gas permeability prediction value of the film to be tested based on the temperature data, the air pressure data and an ideal state equation;
and filtering the gas permeability measured value based on a Kalman filtering algorithm and the gas permeability prediction value to obtain the gas permeability of the film to be measured.
In one embodiment, said controlling the valve opening and closing time according to the predicted air pressure data to make the air pressure data within a preset air pressure range includes:
if the predicted air pressure data is larger than or equal to a third preset threshold value, shortening the opening time of the valve;
and if the predicted air pressure data is smaller than a third preset threshold value, increasing the opening time of the valve.
In one embodiment, the obtaining a gas permeability measurement value of the membrane to be measured based on the valve on-off time and the permeability calculation formula includes:
acquiring the cumulative time of valve opening;
calculating a gas permeability measurement based on the valve opening integration time, the temperature data, and the gas pressure data detected by the gas pressure sensor according to the following formula:
Figure BDA0003134388900000031
in the above formula, J S As permeability,. DELTA.p s For the gas pressure, Δ p, in the detection chamber o Detecting the gas pressure in the chamber for the initial state, V the volume of the chamber, A the surface area of the film to be detected, R the gas state constant, T the temperature data detected by the temperature sensor, T a Accumulating time for the valve opening.
In one embodiment, the ideal gas state equation is:
PV=nRT;
in the above formula, P is the air pressure data detected by the air pressure sensor, V is the detection chamber volume, n is the amount of the substance of the detection gas, R is the gas state constant, and T is the temperature data detected by the temperature sensor.
In one embodiment, the obtaining a predicted value of the gas permeability of the film to be measured based on the temperature data, the pressure data and the ideal gas state equation includes:
calculating a mass of the detected gas based on the temperature data, the pressure data, and an ideal gas equation of state;
and obtaining a gas permeability prediction value of the film to be detected based on the amount of the substance of the detection gas, wherein the gas permeability prediction value of the film to be detected = the amount of the substance of the detection gas/(detection time ×. Surface area of the film to be detected).
This application second aspect provides a water oxygen permeability measuring device of film, the film that awaits measuring will the test cavity separates for admitting air room and accumulation room, the test gas infiltration in the admitting air room the film gets into the accumulation room, the device includes:
the detection data acquisition module is used for acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, and the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber;
the valve switching time control module is used for carrying out regression processing on the air pressure data based on a Gaussian process regression algorithm so as to obtain predicted air pressure data; controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is in a preset air pressure range;
and the water oxygen permeability numerical value acquisition module is used for acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and the permeability calculation formula, and the valve is positioned between the accumulation chamber and the detection chamber.
Among the water oxygen permeability measuring device in above-mentioned embodiment, through setting up detection data acquisition module, valve on-off time control module and water oxygen permeability value acquisition module and mutually supporting, carry out regression processing to the atmospheric pressure data who obtains based on gaussian process regression algorithm to obtain prediction atmospheric pressure data, thereby control valve on-off time, make atmospheric pressure data be located and predetermine the atmospheric pressure within range, improve water oxygen permeability measurement process's the degree of accuracy, reduced the detection and set up the influence of self.
A third aspect of the application proposes a computer device comprising a memory storing a computer program and a processor implementing the steps of the method described above when executing the computer program.
A fourth aspect of the present application proposes a computer-readable storage medium having stored thereon a computer program which, when being executed by a processor, carries out the steps of the method as described above.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to make the technical solutions of the present invention practical in accordance with the contents of the specification, the following detailed description is given of preferred embodiments of the present invention with reference to the accompanying drawings.
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In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain drawings of other embodiments without creative efforts based on the drawings.
FIG. 1 is a schematic view of a gas permeation detection system as provided herein;
FIG. 2 is a schematic diagram of a detection system for measuring gas permeability by a mass spectrometer provided in the present application;
FIG. 3 is a schematic diagram of a detection principle of gas permeability measurement by a mass spectrometer based on a fixed accumulation time provided in the present application;
FIG. 4 is a schematic diagram of a permeability measurement signal of a sample to be measured as a function of measurement time provided in the present application;
FIG. 5 is a schematic diagram of a mass spectrometer measurement signal as a function of accumulation time as provided herein;
FIG. 6 is a schematic flow chart of a gas permeability measurement method provided in an embodiment of the present application;
FIG. 7 is a schematic diagram of a Gaussian process regression algorithm provided herein;
FIG. 8 is a schematic flow chart of a gas permeability measurement method provided in another embodiment of the present application;
FIG. 9 is a schematic diagram of a Kalman filtering algorithm provided in the present application;
FIG. 10 is a schematic diagram of a gas permeability detection system based on adjustable accumulation time as provided herein;
fig. 11 is a schematic diagram illustrating the use effect of a gas permeability measurement method provided in the present application.
Detailed Description
To facilitate an understanding of the present application, the present application will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present application are shown in the drawings. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Where the terms "comprising," "having," and "including" are used herein, another component may be added unless a specific limiting term is used, such as "only," "consisting of 8230; \8230composition," etc. Unless mentioned to the contrary, singular terms may include the plural and are not to be construed as being one in number.
It will be understood that, although the terms first, second, etc. may be used herein to describe various elements, these elements should not be limited by these terms. These terms are only used to distinguish one element from another. For example, a first element could be termed a second element, and, similarly, a second element could be termed a first element, without departing from the scope of the present application.
In this application, unless otherwise expressly stated or limited, the terms "connected" and "connecting" are used broadly and encompass, for example, direct connection, indirect connection via an intermediary, communication between two elements, or interaction between two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as the case may be.
The gas permeation detection system is basically characterized in that a sample material is arranged between an upper chamber and a lower chamber, the upper chamber and the lower chamber are close to a vacuum state at the beginning, high-pressure water vapor or other gases are introduced into the upper chamber after the detection is started to form a large pressure difference between the upper chamber and the lower chamber, so that the gases slowly permeate through the material to enter the lower chamber, the gas permeation reaches a stable state after a period of time, and the steady state permeation rate is J at the moment S Permeability of material is P, upper chamber pressure is P u D is the thickness of the material, and the relationship between the permeation flux and the pressure is as follows:
Figure BDA0003134388900000071
i.e. the gas permeability P of the sample material can pass through the gas steady state permeability J in the steady state S And pressure intensity P u The corresponding relationship of (a) is obtained. Based on this principle, gas permeability measurements of the sample material can be achieved.
At present, gas steady state permeability J s There are many measurement methods, for example: weighing method, storage experiment method, mass spectrometer method, etc. The mass spectrometer is the most precise device for measuring gas molecules and is very suitable for being used as a device for measuring gas permeability. Taking the process of measuring the steady state permeability of a gas by a mass spectrometer as an example, please refer to fig. 2, the apparatus includes: the device comprises an air inlet chamber, an accumulation chamber and a detection chamber, wherein the air inlet chamber, the accumulation chamber and the detection chamber are connected with a vacuum pump through respective valves, and the accumulation chamber is communicated with the detection chamber through the valvesThe spectrometer is connected with the detection chamber, can measure the pressure data of the interior gas of detection chamber, and each cavity can set up baroceptor (barometer) and temperature sensor as required in order to obtain corresponding data. Before the detection experiment begins, the sample film is placed between the air inlet chamber and the accumulation chamber, each chamber is pumped to a vacuum state, the detection experiment begins, gas to be detected is sent into the air inlet chamber through a certain buffer device, the gas permeates the sample film to enter the accumulation chamber, and the process is carried out t a After the time is accumulated, the gas enters a detection chamber to be detected by a mass spectrometer, the detection output is the gas pressure p, and the gas pressure p passes through t d After the time is checked, evacuating the accumulation chamber and the detection chamber to detect gas, wherein the evacuation time is t e And after the evacuation is finished, the next cycle is carried out, namely each signal acquisition comprises three processes of vacuumizing, accumulating and detecting and the like, and each step in each cycle adopts consistent time period setting. The output is shown in FIG. 3, where Δ p is the gas pressure jump detected by the mass spectrometer, at which time the gas steady state permeability is
Figure BDA0003134388900000081
Wherein t is a And the valve opening accumulation time is, V is the volume of the detection chamber, A is the surface area of the film to be detected, R is a gas state constant, and T is temperature data detected by the temperature sensor.
However, in actual measurement, the process of measuring gas permeability by the mass spectrometer lasts for a long time (up to 60 days), the mass spectrometer has a condition that ionization efficiency decreases with time, and environmental temperature fluctuation also affects final water oxygen permeability measurement, so that a detection signal is inaccurate, as shown in fig. 4, a solid line represents a curve of gas pressure in a detection chamber changing with time in an ideal state, and as time increases, the gas permeability of a film tends to be stable, and the gas pressure in the detection chamber also tends to be stable. The dotted line represents a curve of the change of the gas pressure in the detection chamber with time in the detection state, and since the mass spectrometer can generate the condition of the reduction of the ionization efficiency with time, the detection of the same pressure can generate the condition of signal fluctuation, namely, the corresponding relation between the measured signal and the actual signal is not fixed. In addition, since the filament of the mass spectrometer reacts with oxygen and water vapor, the measurement signal cannot be linearly corresponding to the gas pressure concentration in the chamber, as shown in fig. 5, a straight line represents the variation of the mass spectrometer detection signal with the accumulation time in an ideal state, and a dotted broken line represents the variation of the mass spectrometer detection signal with the accumulation time in a detection state. Therefore, in order to improve the reliability of the signal, the measured signal of the mass spectrometer should be in a linear section, i.e. the gas pressure in the detection chamber should be kept at a high level, however, the gas accumulation time in the existing mass spectrometer measurement method is always fixed, and the method based on time integration cannot control the gas pressure entering the mass spectrometer, so that a large measurement error is generated.
Based on the method, the gas permeability measuring method of the film can effectively control the pressure of gas entering a mass spectrometer and reduce measuring errors. In order to illustrate the technical solution of the water oxygen permeability measurement method of the present application, the following description will be given by way of specific examples.
In one embodiment, as shown in fig. 6, there is provided a gas permeability measurement method of a membrane dividing a test chamber into an inlet chamber and an accumulation chamber, a test gas in the inlet chamber permeating through the membrane into the accumulation chamber, the method comprising the steps of:
step S10: acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, wherein the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber;
wherein, the temperature data and the air pressure data can be detected by the detection device shown in fig. 2, and specifically, the description of the process can be found above.
Step S20: performing regression processing on the air pressure data based on a Gaussian process regression algorithm to obtain predicted air pressure data;
the Gaussian process regression is a nonparametric model for performing regression analysis on data by using Gaussian process priors, and comprises two parts, namely noise (regression residual) and the Gaussian process priors, and the solution is performed according to Bayesian inference. Without limiting the form of the kernel function, gaussian process regression is theoretically a general approximation of any continuous function in a compact space. In step S20, the regression processing is performed on the obtained air pressure data, which is a process of obtaining a predicted value similar to an actual value by using the algorithm, performing regression processing on an existing data point by gaussian process regression as shown in fig. 7, and outputting a prediction curve, and the predicted air pressure data is obtained by using the prediction curve.
Step S30: controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is in a preset air pressure range;
specifically, as shown in fig. 2, the valve is located between the accumulation chamber and the detection chamber, the valve opening and closing time is controlled to control the gas pressure in the detection chamber, and the valve opening and closing time is controlled based on the predicted gas pressure data in step S20, so that the gas pressure data is within the preset gas pressure range.
Step S40: and acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and a permeability calculation formula, wherein the valve is positioned between the accumulation chamber and the detection chamber.
Specifically, based on the valve switching time and the permeability calculation formula, the permeability of the gas in a stable state can be obtained, and the gas permeability measurement value of the film to be measured can be calculated by combining gas pressure data detected by the gas pressure sensor.
In the gas permeability measuring method in the above embodiment, the predicted gas pressure data is obtained by obtaining the gas pressure data of the gas pressure sensor and performing regression processing on the gas pressure data by using a gaussian process regression algorithm, so that the valve opening and closing time is controlled, the gas pressure value of the gas in the test chamber is kept within a preset range, and the gas permeability measurement value of the film to be measured is obtained according to the valve opening time and the permeability calculation formula. By using the gas permeability measuring method of the film, the detection error of an instrument can be effectively reduced, and the accuracy of a detection signal is improved.
In one embodiment, before acquiring the air pressure data detected by the air pressure sensor, the method includes:
acquiring a signal-to-noise ratio and detection time of real-time detection data detected by a mass spectrometer, wherein the mass spectrometer is positioned in the detection chamber; and if the signal-to-noise ratio is greater than or equal to a first preset threshold value and/or the detection time is greater than or equal to a second preset threshold value, acquiring air pressure data detected by the air pressure sensor.
Specifically, the mass spectrometer is a detection instrument that qualitatively and quantitatively determines the mass and intensity of gas particles by mass spectrometry to obtain the real-time detection data. The signal-to-noise ratio is the ratio of the signal to the noise at the maximum undistorted output power of the instrument, and is usually not measured directly but is converted by measuring the amplitude of the noise signal. According to the method for measuring the gas permeability of the film, the gas permeability of the film is finally obtained through a predicted value and an algorithm, and only a certain amount of real-time detection data need to be obtained, so that the signal-to-noise ratio of the detection data and the detection time can be used as data obtaining conditions, wherein the detection time comprises the total detection time and the interval time between the obtained signals. As an example, if the first preset threshold is set to 2 and the second preset threshold is set to 1 hour, when the signal-to-noise ratio of the acquired detection data is greater than 2 (the signal-to-noise ratio is greater than 2, 1), and/or the interval time is greater than 1 hour, the acquired real-time monitoring data amount meets the requirement, and a detection data sample can be established based on the real-time detection data.
In the method for measuring the gas permeability of the thin film in the embodiment, the detection data sample is determined by setting the first preset threshold and the second preset threshold, so that the erroneous judgment of the system is avoided to a great extent, and the reliability of the system is improved.
In one embodiment, as shown in fig. 8, the method for measuring gas permeability of a membrane further includes the steps of:
step S50: acquiring a gas permeability prediction value of the film to be tested based on the temperature data, the air pressure data and an ideal state equation;
the temperature data and the air pressure data are obtained through detection of a temperature sensor and an air pressure sensor which are located in a detection chamber.
Step S60: and filtering the gas permeability measured value based on a Kalman filtering algorithm and the gas permeability prediction value to obtain the gas permeability of the film to be measured.
Specifically, kalman filtering is the application of statistics to the filtering algorithm. The core idea of the algorithm is to obtain the current optimal estimation by calculation according to the current instrument 'measurement value' and 'measurement error' and the previous moment 'pre-measurement' and 'prediction error'. The algorithm is distinguished by the idea of incorporating errors into the calculation and by the distinction between prediction errors and measurement errors, commonly referred to as noise. As an example, as shown in FIG. 9, for an example of calculating the optimal amount of the driving position of the vehicle based on the Kalman filter algorithm, assume that the currently obtained data signal is X k-1 According to X we k-1 By predicting X k At the same time, the signal we can actually measure is Y k The two signals have corresponding uncertainty, the information content is integrated, and the X is subjected to the Kalman filtering algorithm k And Y k And revising to obtain the optimal quantity of the automobile type position. Similarly, in steps S40 and S50, the gas permeability measured value and the gas permeability predicted value are known, and the data are processed based on the kalman filter algorithm, so that the optimal predicted value of the gas permeability can be obtained, and the optimal predicted value of the gas permeability is output as the gas permeability of the film to be measured.
In one embodiment, said controlling the valve opening and closing time according to the predicted air pressure data to make the air pressure data within a preset air pressure range includes:
if the predicted air pressure data is larger than or equal to a third preset threshold value, shortening the opening time of the valve;
and if the predicted air pressure data is smaller than a third preset threshold value, increasing the opening time of the valve.
Specifically, as shown in fig. 10, in order to keep the pressure data within the preset pressure range, that is, to keep the Δ p value stable during each cycle detection, a third preset threshold should be set in combination with the signal detected by the mass spectrometer and the past detection data, and when the obtained gas pressure data is greater than the third preset threshold, the valve opening time t is shortened a The gas pressure value delta p detected in the accumulation chamber at the next time is close to a third preset threshold value, and when the obtained gas pressure data is smaller than the third preset threshold value, the valve opening time t is increased a And the gas pressure value detected in the accumulation chamber at the next time is close to a third preset threshold value, and the monitoring data of the mass spectrometer fluctuate up and down at a certain height by setting the valve opening time, so that the signal is ensured to be in a linear section detected by the mass spectrometer, and the accuracy of the signal is improved.
In one embodiment, the obtaining a gas permeability measurement value of the membrane to be measured based on the valve on-off time and the permeability calculation formula includes:
acquiring the cumulative time of valve opening;
calculating a gas permeability measurement based on the valve opening integration time, the temperature data, and the gas pressure data detected by the gas pressure sensor according to the following formula:
Figure BDA0003134388900000121
in the above formula, J S For gas-stable permeability,. DELTA.p s For the gas pressure, Δ p, in the detection chamber o Detecting the gas pressure in the chamber for the initial state, V the volume of the chamber, A the surface area of the film to be detected, R the gas state constant, T the temperature data detected by the temperature sensor, T a Accumulating time for the valve opening.
Specifically, the quality detector can detect the pressure value delta p of the gas to be detected s The application controls the opening time of the valve to enable delta p s Remains substantially constant, Δ p o The gas pressure in the chamber is initially measured, so that the gas permeation measured by the mass spectrometer is related to the valve opening time t a The influence of the gas pressure on the detection of the permeability decreases as a function of the temperature T.
In one embodiment, the ideal gas state equation is:
PV=nRT;
in the above formula, P is the air pressure data detected by the air pressure sensor, V is the detection chamber volume, n is the amount of the substance of the detection gas, R is the gas state constant, and T is the temperature data detected by the temperature sensor.
In the embodiment of the present invention, P is the gas pressure data detected by the gas pressure sensor, V is the volume of the detection chamber, R is a gas state constant, T is the temperature data detected by the temperature sensor, which are known quantities, and n is the quantity of the substance of the detection gas, which is the quantity to be solved, so that the quantity of the substance of the detection gas can be solved based on the ideal gas state.
In one embodiment, the obtaining a predicted value of the gas permeability of the film to be measured based on the temperature data, the pressure data and the ideal gas state equation includes:
calculating a mass of the detected gas based on the temperature data, the pressure data, and an ideal gas equation of state;
and obtaining a gas permeability prediction value of the film to be detected based on the amount of the substance of the detection gas, wherein the gas permeability prediction value of the film to be detected = the amount of the substance of the detection gas/(detection time ×. Surface area of the film to be detected).
Specifically, by acquiring the temperature data of the temperature sensor and the gas pressure data of the gas pressure sensor, the mass (moles) of the detection gas can be acquired based on an ideal state equation, and since the gas permeability is the amount of the substance flowing through the gas per unit area per unit time, the gas permeability at a steady state can be calculated and used as a predicted value, specifically, the predicted value of the gas permeability of the film under test = the amount of the substance of the detection gas/(detection time × surface area of the film under test).
In the method for measuring the gas permeability of the film in the embodiment, the sensor is arranged in the detection device to obtain corresponding parameter data, the predicted value of the gas permeability of the sample film can be calculated based on the parameter data and the ideal state equation, and the predicted value is used as correction data to correct a mass spectrometer detection signal and improve the accuracy of the mass spectrometer detection signal.
This application second aspect provides a water oxygen permeability measuring device of film, the film that awaits measuring will the test cavity separates for air inlet chamber and accumulation chamber, the test gas infiltration in the air inlet chamber the film gets into the accumulation chamber, the device includes:
the detection data acquisition module is used for acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, and the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber;
the valve switching time control module is used for carrying out regression processing on the air pressure data based on a Gaussian process regression algorithm so as to obtain predicted air pressure data; controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is within a preset air pressure range;
and the water oxygen permeability numerical value acquisition module is used for acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and the permeability calculation formula, and the valve is positioned between the accumulation chamber and the detection chamber.
In the water oxygen permeability measuring device in the above embodiment, the detection data acquisition module, the valve on-off time control module and the water oxygen permeability value acquisition module are arranged to cooperate with each other, and the regression processing is performed on the acquired air pressure data based on the gaussian process regression algorithm to acquire predicted air pressure data, so that the valve on-off time is controlled, the air pressure data is located in a preset air pressure range, and the accuracy of the water oxygen permeability measuring process is improved.
A third aspect of the application proposes a computer device comprising a memory storing a computer program and a processor implementing the steps of the method described above when executing the computer program.
A fourth aspect of the present application proposes a computer-readable storage medium having stored thereon a computer program which, when being executed by a processor, carries out the steps of the method as described above.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
It will be understood by those skilled in the art that all or part of the processes of the methods of the embodiments described above can be implemented by hardware instructions of a computer program, which can be stored in a non-volatile computer-readable storage medium, and when executed, can include the processes of the embodiments of the methods described above. Any reference to memory, storage, database or other medium used in the embodiments provided herein can include at least one of non-volatile and volatile memory. Non-volatile Memory may include Read-Only Memory (ROM), magnetic tape, floppy disk, flash Memory, optical Memory, or the like. Volatile Memory can include Random Access Memory (RAM) or external cache Memory. By way of illustration and not limitation, RAM can take many forms, such as Static Random Access Memory (SRAM) or Dynamic Random Access Memory (DRAM), among others.
It should be noted that the above-mentioned embodiments are only for illustrative purposes and are not meant to limit the present invention.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, and these are all within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A method of measuring gas permeability of a membrane, wherein the membrane to be tested separates the test chamber into an inlet chamber and an accumulation chamber, and test gas in the inlet chamber permeates through the membrane into the accumulation chamber, the method comprising:
acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, wherein the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber;
performing regression processing on the air pressure data based on a Gaussian process regression algorithm to obtain predicted air pressure data;
controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is in a preset air pressure range;
and acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and a permeability calculation formula, wherein the valve is positioned between the accumulation chamber and the detection chamber.
2. The method for measuring gas permeability of a membrane according to claim 1, wherein the step of obtaining the gas pressure data detected by the gas pressure sensor comprises:
acquiring a signal-to-noise ratio and detection time of real-time detection data detected by a mass spectrometer, wherein the mass spectrometer is positioned in the detection chamber;
and if the signal-to-noise ratio is greater than or equal to a first preset threshold value and/or the detection time is greater than or equal to a second preset threshold value, acquiring air pressure data detected by the air pressure sensor.
3. The method for measuring gas permeability of a membrane according to claim 2, further comprising:
acquiring a gas permeability prediction value of the film to be tested based on the temperature data, the air pressure data and an ideal state equation;
and filtering the gas permeability measured value based on a Kalman filtering algorithm and the gas permeability prediction value to obtain the gas permeability of the film to be measured.
4. The method of measuring gas permeability of a membrane according to claim 3, wherein said controlling valve opening and closing times based on said predicted gas pressure data to bring said gas pressure data within a predetermined gas pressure range comprises:
if the predicted air pressure data is larger than or equal to a third preset threshold value, shortening the opening time of the valve;
and if the predicted air pressure data is smaller than a third preset threshold value, increasing the opening time of the valve.
5. The method of claim 4, wherein the obtaining a gas permeability measurement value of the membrane to be tested based on the valve on-off time and permeability calculation formula comprises:
acquiring accumulated valve opening time;
calculating a gas permeability measurement based on the valve opening integration time, the temperature data, and the pressure data detected by the pressure sensor according to the following formula:
Figure FDA0003134388890000021
in the above formula, J S As permeability,. DELTA.p s For the gas pressure, Δ p, in the detection chamber o Detecting the gas pressure in the chamber for the initial state, V the volume of the chamber, A the surface area of the film to be detected, R the gas state constant, T the temperature data detected by the temperature sensor, T a Accumulating time for the valve opening.
6. The method for measuring gas permeability of a membrane according to any one of claims 1 to 5, wherein the ideal gas state equation is:
PV=nRT;
in the above formula, P is the air pressure data detected by the air pressure sensor, V is the detection chamber volume, n is the amount of the substance of the detection gas, R is the gas state constant, and T is the temperature data detected by the temperature sensor.
7. The method for measuring gas permeability of a membrane according to any one of claims 1 to 5, wherein the obtaining a predicted value of gas permeability of the membrane to be measured based on the temperature data, the gas pressure data and the ideal gas state equation comprises:
calculating a mass of the detected gas based on the temperature data, the pressure data, and an ideal gas equation of state;
and obtaining a gas permeability prediction value of the film to be detected based on the amount of the substance of the detection gas, wherein the gas permeability prediction value of the film to be detected = the amount of the substance of the detection gas/(detection time) × the surface area of the film to be detected).
8. A gas permeability measuring device for a membrane, wherein the membrane to be tested separates the test chamber into an inlet chamber and an accumulation chamber, and test gas in the inlet chamber permeates through the membrane into the accumulation chamber, the device comprising:
the detection data acquisition module is used for acquiring temperature data detected by a temperature sensor and air pressure data detected by an air pressure sensor, and the temperature sensor and the air pressure sensor are positioned in a detection chamber communicated with the accumulation chamber;
the valve switching time control module is used for carrying out regression processing on the air pressure data based on a Gaussian process regression algorithm so as to obtain predicted air pressure data; controlling the valve opening and closing time according to the predicted air pressure data so that the air pressure data is in a preset air pressure range;
and the water oxygen permeability numerical value acquisition module is used for acquiring a gas permeability measurement value of the film to be detected based on the valve switching time and the permeability calculation formula, and the valve is positioned between the accumulation chamber and the detection chamber.
9. A computer device comprising a memory and a processor, the memory storing a computer program, characterized in that the processor, when executing the computer program, implements the steps of the method of any of claims 1 to 7.
10. A computer-readable storage medium, on which a computer program is stored, which, when being executed by a processor, carries out the steps of the method of any one of claims 1 to 7.
CN202110714636.2A 2021-06-25 2021-06-25 Gas permeability measuring method, device, equipment and medium Pending CN115524271A (en)

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