Method and device for detecting content of elements in coating material
By measuring and calibrating the attenuation data of the X-ray machine head and tail, and combining this with the X-ray attenuation law, the accuracy problem of silicon content detection in coated materials was solved, achieving higher detection precision.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ZHEJIANG SHUANGYUAN TECH CO LTD
- Filing Date
- 2025-12-18
- Publication Date
- 2026-04-10
AI Technical Summary
Existing technologies make it difficult to accurately measure the silicon content in the coating material during the lithium battery coating process. This is due to issues such as instrument differences and the nonlinear superposition of X-ray attenuation values after material stacking, which affects the accuracy of coating surface density measurement.
By measuring the attenuation data of the X-ray machine head before coating the base material and measuring the attenuation data of the X-ray machine tail after coating the material, and combining the attenuation patterns of different rays, the areal density of the main and target elements in the coating layer is analyzed, and the attenuation coefficients of the X-ray machine head and tail are calibrated to improve the accuracy of detection.
It effectively avoids the influence of coating layer material superposition on X-ray attenuation data, reduces instrument difference errors, and improves the accuracy of element content detection in coating materials.
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Figure CN121347559B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of coating material composition measurement, and particularly relates to a method and device for detecting element content in a coating material. BACKGROUND
[0002] As an advanced electrode preparation process, double-layer coating technology has great potential in improving the performance of lithium batteries. Among them, the design of the layered structure of the binder is one of the key links of the double-layer coating process, which has an important influence on the structural integrity, cycle stability and electrochemical performance of the electrode. Double-layer coating is a process of coating two different slurries on the current collector to form a double-layer structure electrode.
[0003] In the production process of lithium batteries, the consistency control of the battery is crucial, and the areal density consistency of the coated electrode sheet is an important influencing factor. Therefore, the areal density of the electrode sheet needs to be detected in real time during the coating process. In recent years, with the development of measurement technology and control technology, the areal density measurement instrument is gradually used in the industry to realize the measurement of the lithium battery electrode sheet coating. When the rays penetrate the lithium battery coated electrode sheet, the intensity attenuates, which conforms to the exponential law, is related to the coating areal density, and the measurement of the coating areal density is realized according to the attenuation of the detected rays.
[0004] Patent application CN119771699A discloses a thickness measurement device and use method of double-layer coated sheet, the core is to use a double-energy ray thickness gauge, feedback lithium battery negative electrode sheet areal density and carbon element and silicon element proportion. The difference between the measurement values before and after the silicon solidification layer is obtained by two detectors to realize the measurement of silicon content, but on the one hand, due to the instrument difference of different detectors, their no-load values are different, and there is a big instrument error between the detectors when using different detectors to detect the difference of ray attenuation; on the other hand, the ray attenuation value after the superposition of two different solidification layer materials is not the simple addition of the attenuation values of the two materials, and there is no linear superposition relationship between the attenuation values. The attenuation of X-rays penetrating a substance follows the Beer-Lambert Law, that is, the exponential attenuation law.
[0005] The patent application CN120445912A discloses a pole piece detection method, a detection device, a detection equipment and a storage medium. The method comprises the following steps: acquiring first detection data corresponding to irradiation of a first light beam on a composite coating on a pole piece, and second detection data corresponding to irradiation of a second light beam on the composite coating; determining a proportion of a target component in the composite coating based on the first detection data and the second detection data; determining a surface density of the composite coating based on the second detection data; determining a surface density of the target component based on the proportion of the target component and the surface density of the composite coating; and the correlation coefficient between the absorption coefficient of the first light beam and the atomic number is greater than the correlation coefficient between the absorption coefficient of the second light beam and the atomic number. Based on the above method, the surface density of the target component in the composite coating can be determined.
[0006] How to measure the silicon content in the coating material during the detection of lithium batteries and improve the accuracy of the silicon content measurement in the coating material is a problem to be solved at present. SUMMARY
[0007] In view of the defects in the prior art, the present application provides a method and device for detecting the content of elements in coating material. The method comprises the following steps: measuring the first ray machine head attenuation data of the base material before coating to obtain the element surface density of the base material; coating a coating layer containing target elements on the surface of the base material to form a coated material; measuring the first ray machine tail attenuation data and the second ray machine tail attenuation data of the coated material; based on the second ray machine tail attenuation data of the coated material, obtaining the total surface density of each element in the coated material; combining the total surface density of each element in the coated material, the element surface density of the base material and the first ray machine tail attenuation data to obtain the surface density of the main element and the target element in the coating layer, and the content of the target element in the coated material. By analyzing the attenuation law of each element in the coating material by different rays, the surface density of the main element and the target element in the coating layer is obtained, and then the content of the target element in the coated material is obtained, which avoids the influence of the material superposition in the coating layer on the first ray machine tail attenuation data, and improves the accuracy of the element content detection in the coated material.
[0008] In a first aspect, the present application provides a method for detecting the content of elements in coating material, which specifically comprises the following steps:
[0009] Measuring the first ray machine head attenuation data of the base material before coating to obtain the element surface density of the base material;
[0010] Coating a coating layer containing target elements on the surface of the base material to form a coated material;
[0011] Measuring the first ray machine tail attenuation data and the second ray machine tail attenuation data of the coated material;
[0012] Based on the second ray tail attenuation data of the coating material, the total area density of each element in the coating material is given;
[0013] Combined with the total area density of each element in the coating material, the substrate element area density and the first ray tail attenuation data, the main element area density and the target element area density in the coating layer are obtained, and the content of the target element in the coating material is given.
[0014] Further, the first ray head detection device is arranged at the head position before coating, and the first ray head attenuation data includes the first ray head initial intensity and the first ray head attenuation intensity;
[0015] The first ray tail detection device and the second ray tail detection device are arranged at the tail position after coating, the first ray tail attenuation data includes the first ray tail initial intensity and the first ray tail attenuation intensity, and the second ray tail attenuation data includes the second ray tail initial intensity and the second ray tail attenuation intensity.
[0016] Further, the first ray head attenuation data of the base material before coating is measured to give the substrate element area density, which specifically includes the following steps:
[0017] The first ray head initial intensity and the first ray head attenuation intensity are obtained, and the first ray head attenuation coefficient of the substrate element is determined;
[0018] The ratio of the first ray head initial intensity to the first ray head attenuation intensity is calculated by natural logarithm, and the first ray head attenuation degree is given;
[0019] Combined with the first ray head attenuation degree and the first ray head attenuation coefficient of the substrate element, the substrate element area density is given.
[0020] Further, the first ray head attenuation data of the base material before coating is measured to give the substrate element area density, which is specifically represented as:
[0021]
[0022] Wherein, μ base,f1 is the first ray head attenuation coefficient of the substrate element, T base is the substrate element area density, I init,f1 is the first ray head initial intensity, I att,f1 is the first ray head attenuation intensity.
[0023] Further, before determining the first ray head attenuation coefficient of the substrate element, the first ray head attenuation coefficient of the substrate element is calibrated, which specifically includes the following steps:
[0024] The standard substrate and the standard substrate element area density are obtained;
[0025] measuring the first ray machine head calibration initial intensity, the first ray machine head calibration decay intensity, and calculating the ratio of the first ray machine head calibration initial intensity and the first ray machine head calibration decay intensity by natural logarithm to give the first ray machine head calibration decay degree;
[0026] based on the first ray machine head calibration decay degree and the standard substrate element area density, the calibrated substrate element first ray machine head attenuation coefficient is given.
[0027] Further, based on the first ray machine head calibration decay degree and the standard substrate element area density, the calibrated substrate element first ray machine head attenuation coefficient is given, which is specifically expressed as:
[0028]
[0029] Wherein, μ cal,base,f1 is the calibrated substrate element first ray machine head attenuation coefficient, T cal,base is the standard substrate element area density, I cal,init,f1 is the first ray machine head calibration initial intensity, I cal,att,f1 is the first ray machine head calibration decay intensity.
[0030] Further, the components of the coating layer include target elements and main elements.
[0031] Further, based on the second ray machine tail decay data of the coating material, the total area density of each element in the coating material is given, which specifically includes the following steps:
[0032] determining the second ray machine tail absorption coefficient and the second ray machine tail translation coefficient;
[0033] calculating the ratio of the second ray machine tail initial intensity and the second ray machine tail decay intensity by natural logarithm to give the second ray machine tail decay degree;
[0034] combining the second ray machine tail decay degree, the second ray machine tail absorption coefficient and the second ray machine tail translation coefficient, the total area density of each element in the coating material is given.
[0035] Further, combining the second ray machine tail decay degree, the second ray machine tail absorption coefficient and the second ray machine tail translation coefficient, the total area density of each element in the coating material is given, which is specifically expressed as:
[0036]
[0037] Wherein, μ l2 is the second ray machine tail absorption coefficient, T all is the total area density of each element in the coating material, I init,l2 is the second ray machine tail initial intensity, I att,l2is a second tail attenuation intensity of the second ray, B l2 is a second tail translation coefficient of the second ray.
[0038] Further, before determining the second tail absorption coefficient and the second tail translation coefficient, the method further comprises calibrating the second tail absorption coefficient and the second tail translation coefficient, and specifically comprises the following steps:
[0039] obtaining a first standard coating material and a second standard coating material, determining the substrate element area density, the main element area density and the target element area density in the first standard coating material and the second standard coating material respectively, and giving the total element area density in the first standard coating material and the total element area density in the second standard coating material;
[0040] measuring the second ray tail first standard initial intensity, the second ray tail first standard attenuation intensity, the second ray tail second standard initial intensity and the second ray tail second standard attenuation intensity of the first standard coating material and the second standard coating material respectively;
[0041] calculating the second ray tail first standard initial intensity and the second ray tail first standard attenuation intensity by natural logarithm, and giving the second ray tail first standard attenuation degree;
[0042] calculating the ratio of the second ray tail second standard initial intensity and the second ray tail second standard attenuation intensity by natural logarithm, and giving the second ray tail second standard attenuation degree;
[0043] combining the second ray tail first standard attenuation degree, the total element area density in the first standard coating material and the second ray tail second standard attenuation degree, the total element area density in the second standard coating material, and based on the linear relationship, giving the calibrated second tail absorption coefficient and the second tail translation coefficient.
[0044] Further, combining the second ray tail first standard attenuation degree, the total element area density in the first standard coating material and the second ray tail second standard attenuation degree, the total element area density in the second standard coating material, and based on the linear relationship, giving the calibrated second tail absorption coefficient and the second tail translation coefficient, which is specifically expressed as:
[0045]
[0046] wherein, μ cal,l2 is the calibrated second tail absorption coefficient, T all,sta1 is the total element area density in the first standard coating material, T all,sta2 is the total element area density in the second standard coating material, I init,l2,sta1 is the second ray tail first standard initial intensity, Iatt,l2,sta1 is the first standard intensity of the second ray tail, I init,l2,sta2 is the second standard initial intensity of the second ray tail, I att,l2,sta2 is the second standard decay intensity of the second ray tail, B cal,l2 is the calibrated second ray tail translation coefficient.
[0047] Further, the main element surface density and the target element surface density in the coating layer are obtained in combination with the total surface density of each element in the coating material, the substrate element surface density, and the first ray tail decay data, and specifically include the following steps:
[0048] The first ray tail decay coefficient of the substrate element, the first ray tail decay coefficient of the main element, and the first ray tail decay coefficient of the target element are determined.
[0049] The first ray tail decay degree is given by calculating the ratio of the first ray tail initial intensity to the first ray tail decay intensity in natural logarithm.
[0050] The main element surface density and the target element surface density in the coating layer are obtained in combination with the first ray tail decay degree, the first ray tail decay coefficient of the substrate element, the first ray tail decay coefficient of the main element, the first ray tail decay coefficient of the target element, the total surface density of each element in the coating material, and the substrate element surface density.
[0051] Further, the main element surface density and the target element surface density in the coating layer are obtained in combination with the first ray tail decay degree, the first ray tail decay coefficient of the substrate element, the first ray tail decay coefficient of the main element, the first ray tail decay coefficient of the target element, the total surface density of each element in the coating material, and the substrate element surface density, and specifically represented as:
[0052]
[0053] wherein μ base,l1 is the first ray tail decay coefficient of the substrate element, μ main,l1 is the first ray tail decay coefficient of the main element, μ obj,l1 is the first ray tail decay coefficient of the target element, μ l2 is the second ray tail absorption coefficient, T base is the substrate element surface density, T main is the main element surface density in the coating layer, T obj is the target element surface density, T all is the total surface density of each element in the coating material, I init,l1 is the first ray tail initial intensity, I att,l1 is the first ray tail decay intensity, I init,l2 is the second ray tail initial intensity, I att,l2B is a second ray tail attenuation intensity of the substrate element l2 B is a second ray tail translation coefficient of the substrate element.
[0054] Further, before determining the first ray tail attenuation coefficient of the substrate element, the first ray tail attenuation coefficient of the main element, and the first ray tail attenuation coefficient of the target element, the first ray tail attenuation coefficient of the substrate element, the first ray tail attenuation coefficient of the main element, and the first ray tail attenuation coefficient of the target element are calibrated, specifically including the following steps:
[0055] The standard substrate and the standard substrate element surface density are obtained, and based on the detection of the standard substrate by the first ray tail detection device, the calibrated first ray tail attenuation coefficient of the substrate element is given.
[0056] A main element coating layer is coated on the surface of the standard substrate to obtain a main element standard coating material, and a standard main element surface density is given.
[0057] Based on the detection of the main element standard coating material by the first ray tail detection device, and combined with the first ray tail attenuation coefficient of the substrate element, the calibrated first ray tail attenuation coefficient of the main element is given.
[0058] A target element coating layer is coated on the surface of the main element standard coating material to obtain a composite element standard coating material, and a standard target element surface density is given.
[0059] Based on the detection of the composite element standard coating material by the first ray tail detection device, and combined with the first ray tail attenuation coefficient of the substrate element and the first ray tail attenuation coefficient of the main element, the calibrated first ray tail attenuation coefficient of the target element is given.
[0060] Further, the standard substrate and the standard substrate element surface density are obtained, and based on the detection of the standard substrate by the first ray tail detection device, the calibrated first ray tail attenuation coefficient of the substrate element is given, specifically including the following steps:
[0061] The standard substrate and the standard substrate element surface density are obtained.
[0062] The first ray tail primary calibration initial intensity and the first ray tail primary calibration attenuation intensity for the standard substrate are measured, and the ratio of the first ray tail primary calibration initial intensity to the first ray tail primary calibration attenuation intensity is calculated by natural logarithm to give the first ray tail primary calibration attenuation degree.
[0063] Based on the first ray tail primary calibration attenuation degree and the standard substrate element surface density, the calibrated first ray tail attenuation coefficient of the substrate element is given.
[0064] Further, based on the detection of the standard substrate by the first-ray tail detection device, a calibrated substrate element first-ray tail attenuation coefficient is given, which is specifically represented as:
[0065]
[0066] wherein μ cal,base,l1 is the calibrated substrate element first-ray tail attenuation coefficient, T cal,base is the standard substrate element surface density, I cal,init,l1,pri is the first-ray tail primary calibration initial intensity, I cal,att,l1,pri is the first-ray tail primary calibration decay intensity.
[0067] Further, based on the detection of the standard substrate by the first-ray tail detection device, a calibrated substrate element first-ray tail attenuation coefficient is given, which is specifically represented as:
[0068] The first-ray tail secondary calibration initial intensity and the first-ray tail secondary calibration decay intensity for the standard coating material of the main element are measured, and the ratio of the first-ray tail secondary calibration initial intensity to the first-ray tail secondary calibration decay intensity is calculated in natural logarithm to give the first-ray tail secondary calibration decay degree;
[0069] The first-ray tail secondary calibration decay degree of the substrate element is given in combination with the substrate element first-ray tail attenuation coefficient and the standard substrate element surface density;
[0070] The calibrated main element first-ray tail attenuation coefficient is given in combination with the first-ray tail secondary calibration decay degree, the first-ray tail secondary calibration decay degree of the substrate element, and the standard main element surface density.
[0071] Further, based on the detection of the standard substrate by the first-ray tail detection device, a calibrated substrate element first-ray tail attenuation coefficient is given, which is specifically represented as:
[0072]
[0073] wherein μ cal,base,l1 is the calibrated substrate element first-ray tail attenuation coefficient, T cal,base is the standard substrate element surface density, μ cal,main,l1 is the calibrated main element first-ray tail attenuation coefficient, T cal,main is the standard main element surface density, I cal,init,l1,sec is the first-ray tail secondary calibration initial intensity, I cal,att,l1,sec is the first-ray tail secondary calibration decay intensity.
[0074] Further, based on the detection of the composite element standard coated material by the first-ray tail detection device, and in combination with the substrate element first-ray tail attenuation coefficient and the main element first-ray tail attenuation coefficient, a calibrated target element first-ray tail attenuation coefficient is given, which specifically includes the following steps:
[0075] The first-ray tail final-stage calibration initial intensity and the first-ray tail final-stage calibration decay intensity for the composite element standard coated material are measured, and the ratio of the first-ray tail final-stage calibration initial intensity to the first-ray tail final-stage calibration decay intensity is calculated in natural logarithm to give the first-ray tail final-stage calibration decay degree;
[0076] In combination with the substrate element first-ray tail attenuation coefficient and the standard substrate element area density, the substrate element first-ray tail final-stage calibration decay degree is given;
[0077] In combination with the main element first-ray tail attenuation coefficient and the standard main element area density, the main element first-ray tail final-stage calibration decay degree is given;
[0078] In combination with the first-ray tail final-stage calibration decay degree, the substrate element first-ray tail final-stage calibration decay degree, the main element first-ray tail final-stage calibration decay degree, and the standard target element area density, the calibrated target element first-ray tail attenuation coefficient is given.
[0079] Further, based on the detection of the composite element standard coated material by the first-ray tail detection device, and in combination with the substrate element first-ray tail attenuation coefficient and the main element first-ray tail attenuation coefficient, a calibrated target element first-ray tail attenuation coefficient is given, which is specifically represented as:
[0080]
[0081] Wherein, μ cal,base,l1 is the calibrated substrate element first-ray tail attenuation coefficient, T cal,base is the standard substrate element area density, μ cal,main,l1 is the calibrated main element first-ray tail attenuation coefficient, T cal,main is the standard main element area density, μ cal,obj,l1 is the calibrated target element first-ray tail attenuation coefficient, T cal,obj is the standard target element area density, I cal,init,l1,ter is the first-ray tail final-stage calibration initial intensity, I cal,att,l1,ter is the first-ray tail final-stage calibration decay intensity.
[0082] Further, the content of the target element in the coated material is given, which specifically includes: according to the main element area density and the target element area density, the proportion of the target element in the coating layer is calculated to give the content of the target element in the coated material.
[0083] Further, the content of the target element in the coated material is given, which is specifically represented as:
[0084]
[0085] Wherein, τ obj is the content of the target element in the coated material, T obj is the surface density of the target element, T main is the surface density of the main element.
[0086] In a second aspect, the present application also provides a device for detecting the content of elements in a coated material, which adopts the method for detecting the content of elements in a coated material according to any one of the above, comprising:
[0087] a measuring unit, comprising a first ray head detection device, a first ray tail detection device and a second ray tail detection device, the first ray head detection device is used to measure the first ray head attenuation data of the base material before coating, the first ray tail detection device is used to measure the first ray tail attenuation data of the coated material, and the second ray tail detection device is used to measure the second ray tail attenuation data of the coated material;
[0088] a coating unit, used to coat a paint layer containing the target element on the surface of the base material to form a coated material;
[0089] an analysis unit, used to give the surface density of the base material elements, and based on the second ray tail attenuation data of the coated material, to give the total surface density of each element in the coated material; combined with the total surface density of each element in the coated material, the surface density of the base material elements and the first ray tail attenuation data, the surface density of the main element in the paint layer and the surface density of the target element are obtained, and the content of the target element in the coated material is given.
[0090] The present application provides a method and device for detecting the content of elements in a coated material, which at least has the following beneficial effects:
[0091] (1) By analyzing the attenuation law of each element in the coated material by different rays, the surface density of the main element in the paint layer and the surface density of the target element are obtained, and then the content of the target element in the coated material is given, which avoids the influence of the material superposition in the paint layer on the first ray tail attenuation data, and improves the accuracy of detecting the content of elements in the coated material.
[0092] (2) By calibrating the first ray machine tail attenuation coefficient of the base material element, the first ray machine tail attenuation coefficient of the main element, and the first ray machine tail attenuation coefficient of the target element, on the one hand, the negative influence of the instrument difference of different detection equipment on the detection of the element content in the coating material can be reduced, and on the other hand, the influence of the superposition of different materials in the base material and the coating layer on the ray attenuation value and then the influence on the data of the element content in the coating material can be avoided, thereby improving the accuracy of the detection of the element content in the coating material. BRIEF DESCRIPTION OF DRAWINGS
[0093] Figure 1 The flow chart of the detection method of the element content in the coating material provided by the embodiment of the present application is provided.
[0094] Figure 2 The production process chart of coating the coating layer on the surface of the base material provided by the embodiment of the present application is provided.
[0095] Figure 3 The flow chart of determining the surface density of the base material element provided by the embodiment of the present application is provided.
[0096] Figure 4 The structural schematic diagram of the coating material provided by the embodiment of the present application is provided.
[0097] Figure 5 The flow chart of determining the total surface density of each element in the coating material provided by the embodiment of the present application is provided.
[0098] Figure 6 The flow chart of determining the surface density of the main element and the surface density of the target element provided by the embodiment of the present application is provided.
[0099] Figure 7 The structural schematic diagram of the main element standard coating material provided by the embodiment of the present application is provided.
[0100] Figure 8 The structural schematic diagram of the composite element standard coating material provided by the embodiment of the present application is provided.
[0101] Figure 9 The structural block diagram of the detection device of the element content in the coating material provided by the embodiment of the present application is provided.
[0102] Among them, 10, the first ray machine head detection equipment; 20, the first ray machine tail detection equipment and the second ray machine tail detection equipment; 201, the measurement unit; 202, the coating unit; 203, the analysis unit; 301, the coating layer; 302, the base material; 303, the standard base material; 304, the main element coating layer; 305, the target element coating layer. DETAILED DESCRIPTION
[0103] For better understanding of the above technical solutions, the above technical solutions will be described in detail below in combination with the drawings of the specification and specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor are within the scope of protection of the present application.
[0104] The terms used in the embodiments of the present application are only for the purpose of describing specific embodiments, and are not intended to limit the present application. The singular forms "a", "said" and "the" used in the embodiments of the present application and the appended claims are also intended to include the plural forms, unless the context clearly indicates otherwise. "Multiple" generally includes at least two.
[0105] It should also be noted that the term "include", "contain" or any other variant thereof is intended to cover non-exclusive inclusion, so that the goods or devices including a series of elements not only include those elements, but also include other elements not explicitly listed, or include elements inherent to such goods or devices. Without more limitation, the element defined by the sentence "including a" does not exclude the presence of other identical elements in the goods or devices including the element.
[0106] The specific capacity of the conventional graphene negative electrode is only 372 mAh / g, while the theoretical mass specific capacity and the theoretical volume specific capacity of the silicon negative electrode are as high as 4200 mAh / g and 9786 mAh / cm 3 , respectively. In addition, the silicon negative electrode has an ultra-negative potential of -3.04 V, and the natural reserves of silicon are high and the price is low, so it is considered to be one of the most promising negative electrode materials for lithium batteries.
[0107] The lithium ion battery electrode generally adopts a die extrusion multi-layer coating method. For the silicon negative electrode, a typical production process is to coat a slurry containing carbon black on the copper foil substrate, and to coat a slurry containing silicon on the bottom layer. In the actual production process, due to the instability of the die extrusion, the coating extrusion amount has a certain fluctuation, and the silicon-containing slurry has the phenomenon of uneven stirring, so that the theoretical calculation of the silicon content after the mixing of the upper and lower layers of coating is not accurate, which causes great difficulty in the quality control of the lithium battery negative electrode sheet.
[0108] The application provides a detection method and device for element content in coated material, and the method comprises the following steps: measuring first ray head attenuation data of base material before coating to obtain element area density of the base material; coating a coating layer containing target elements on the surface of the base material to form coated material; measuring first ray tail attenuation data and second ray tail attenuation data of the coated material; obtaining total area density of each element in the coated material based on the second ray tail attenuation data of the coated material; combining the total area density of each element in the coated material, the element area density of the base material and the first ray tail attenuation data to obtain area density of main elements and area density of target elements in the coating layer, and then obtaining the content of the target elements in the coated material. The area density of main elements and the area density of target elements in the coating layer are obtained by analyzing the attenuation law of each element in the coated material by different rays, and then the content of the target elements in the coated material is obtained, which avoids the influence of the material superposition in the coating layer on the first ray tail attenuation data and improves the accuracy of the element content detection in the coated material.
[0109] The face density of the base material (for example, copper) at the same point before and after coating is unchanged, which avoids the difference in ray attenuation between different machines, theoretically eliminates the interference of the difference between different machines, and makes the content of the target elements which are difficult to directly measure measurable.
[0110] As shown in FIG. 1, the embodiment of the application provides a detection method for element content in coated material, and the specific steps are as follows: Figure 1 S101: measuring first ray head attenuation data of base material before coating to obtain element area density of the base material.
[0111] Further, the first ray head detection device is arranged at the head position before coating, and the first ray head attenuation data comprises first ray head initial intensity and first ray head attenuation intensity.
[0112] The first ray tail detection device and the second ray tail detection device are arranged at the tail position after coating, the first ray tail attenuation data comprises first ray tail initial intensity and first ray tail attenuation intensity, and the second ray tail attenuation data comprises second ray tail initial intensity and second ray tail attenuation intensity.
[0113]
[0114] In the embodiments provided by the present application, the first ray head detection device and the first ray tail detection device are devices that measure the degree of attenuation of the first ray in the object, and the second ray tail detection device is a device that measures the degree of attenuation of the second ray in the object. The first ray and the second ray are of different types. In this example, the first ray is an X-ray, and the second ray is a beta ray. In other examples, other rays can be used to complete the relevant measurement tasks, and the present application is not limited in this regard. Generally, the attenuation of the ray follows certain rules. For example, when an X-ray penetrates a substance, it attenuates according to the Beer-Lambert law, which describes the relationship between the absorption of the X-ray and the concentration and path length of the medium when the X-ray passes through a uniform medium.
[0115] It should be understood that the first ray tail detection device and the second ray tail detection device are devices defined by function. The first ray tail detection device and the second ray tail detection device can be two devices. If the devices can simultaneously meet the measurement tasks of the first ray tail detection device and the second ray tail detection device, the first ray tail detection device and the second ray tail detection device can be one device, and the present application is not limited in this regard. In this example, the first ray head detection device is an X-ray thickness gauge, and the first ray tail detection device and the second ray tail detection device are X / β-ray thickness gauges. The ray thickness gauge is an instrument that uses a ray to penetrate an object and measures the degree of attenuation of the ray in the object to measure the object.
[0116] Reference Figure 2In a specific example, during the production process of lithium battery double-layer coating, an X-ray thickness gauge (first radiation head detection device 10) and an X / β-ray thickness gauge (first radiation tail detection device and second radiation tail detection device 20) are required. First, after the copper foil (base material) is unwound at the head of the coating unit 202, an X-ray thickness gauge (first radiation head detection device 10) is placed immediately to measure the copper surface density of the copper foil (i.e., to measure the first radiation head attenuation data of the base material before coating, and to give the base material element surface density), then enter the coating unit 202 for double-layer coating and perform pole piece baking in the oven, and after exiting the oven, an X / β-ray thickness gauge is set at the tail of the coating unit 202, the β-ray is used to measure the surface density of the pole piece (the total surface density of each element in the coating material), i.e., to give the second radiation tail attenuation data, the X-ray is used to measure the surface density of the pole piece, i.e., to give the first radiation tail attenuation data, and finally to wind up, completing the production process of lithium battery double-layer coating. Among them, the head is the beginning of the coating process in the coating equipment, and the tail is the end of the coating process in the coating equipment. In this example, the copper foil is double-layer coated, and the first coating layer containing carbon elements and the second coating layer containing carbon and silicon elements are coated in turn, and the pole piece is obtained by coating double-layer coating on the copper foil (i.e., coating material).
[0117] Further, the first radiation head attenuation data of the base material before coating is measured, and the base material element surface density is given, as described in Figure 3 , which specifically includes the following steps:
[0118] The first radiation head initial intensity and the first radiation head attenuation intensity are obtained, and the base material element first radiation head attenuation coefficient is determined;
[0119] The ratio of the first radiation head initial intensity to the first radiation head attenuation intensity is calculated in natural logarithm, and the first radiation head attenuation degree is given;
[0120] The base material element surface density is given in combination with the first radiation head attenuation degree and the base material element first radiation head attenuation coefficient.
[0121] Further, the first radiation head attenuation data of the base material before coating is measured, and the base material element surface density is given, which is specifically represented as:
[0122]
[0123] Wherein, μ base,f1 is the base material element first radiation head attenuation coefficient, T base is the base material element surface density, I init,f1 is the first radiation head initial intensity, and I att,f1 is the first radiation head attenuation intensity.
[0124] It can be understood that when the base material is determined, the attenuation degree of the first ray to the base material is determined, that is, there is a theoretical value of the attenuation degree of the first ray to the base material, which conforms to the attenuation law of the first ray. At this time, the first ray head detection equipment is used to detect the base material, and the first ray head attenuation data including the first ray head initial intensity and the first ray head attenuation intensity are obtained. The first ray head attenuation data is substituted into the formula conforming to the first ray attenuation law, and the base material element first ray head attenuation coefficient can adopt the theoretical value or the calibrated value, which is not limited.
[0125] Further, before determining the base material element first ray head attenuation coefficient, the base material element first ray head attenuation coefficient is calibrated, specifically including the following steps:
[0126] The standard base material and the standard base material element surface density are obtained.
[0127] The first ray head calibration initial intensity and the first ray head calibration attenuation intensity for the standard base material are measured, and the ratio of the first ray head calibration initial intensity to the first ray head calibration attenuation intensity is calculated by natural logarithm to give the first ray head calibration attenuation degree.
[0128] Based on the first ray head calibration attenuation degree and the standard base material element surface density, the calibrated base material element first ray head attenuation coefficient is given.
[0129] Further, based on the first ray head calibration attenuation degree and the standard base material element surface density, the calibrated base material element first ray head attenuation coefficient is given, which is specifically expressed as:
[0130]
[0131] Wherein, μ cal,base,f1 is the calibrated base material element first ray head attenuation coefficient, T cal,base is the standard base material element surface density, I cal,init,f1 is the first ray head calibration initial intensity, and I cal,att,f1 is the first ray head calibration attenuation intensity.
[0132] In a specific embodiment, taking copper as an example, the standard base material of copper element is obtained, and the standard base material is weighed to obtain the standard base material element surface density. Then the first ray head detection equipment is used to measure the standard base material to obtain the first ray head calibration initial intensity and the first ray head calibration attenuation intensity. Then the measured data is substituted into the formula conforming to the first ray attenuation law of the standard base material to obtain the calibrated base material element first ray head attenuation coefficient.
[0133] By calibrating the attenuation coefficient of the first ray machine head of the base material element, measurement errors caused by instrument differences of the first ray machine head detection device itself are avoided, thereby improving the accuracy of the data and providing a data basis for the detection of the target element content in the coating material.
[0134] S102: A coating layer containing a target element is coated on the surface of the base material to form a coated material.
[0135] Further, the components of the coating layer include the target element and the main element.
[0136] It should be understood that the coating layer 301 is a general term for the coating material on the base material 302, and the coating layer 301 can be one layer or multiple layers. In this example, the structure of the coated material is shown in Figure 4 The target element in the coating layer 301 is the silicon element, and the main element in the coating layer 301 is the carbon element. After coating, the coated material including the base material 302 and the coating layer 301 is obtained.
[0137] S103: Measure the first ray machine tail attenuation data and the second ray machine tail attenuation data of the coated material.
[0138] In combination with the process flow chart of Figure 2 , the first ray machine tail detection device and the second ray machine tail detection device are used to measure the coated material to obtain the first ray machine tail attenuation data corresponding to the first ray machine tail detection device and the second ray machine tail attenuation data corresponding to the second ray machine tail detection device.
[0139] S104: Based on the second ray machine tail attenuation data of the coated material, the total area density of each element in the coated material is given.
[0140] Further, based on the second ray machine tail attenuation data of the coated material, the total area density of each element in the coated material is given, referring to Figure 5 , specifically including the following steps:
[0141] Determine the second ray machine tail absorption coefficient and the second ray machine tail translation coefficient;
[0142] Calculate the ratio of the second ray machine tail initial intensity to the second ray machine tail attenuation intensity in natural logarithm, and give the second ray machine tail attenuation degree;
[0143] In combination with the second ray machine tail attenuation degree, the second ray machine tail absorption coefficient and the second ray machine tail translation coefficient, the total area density of each element in the coated material is given.
[0144] Further, in combination with the second ray machine tail attenuation degree, the second ray machine tail absorption coefficient and the second ray machine tail translation coefficient, the total area density of each element in the coated material is given, which is specifically represented as:
[0145]
[0146] wherein μ l2 is the second ray tail absorption coefficient, T all is the total area density of each element in the coating material, I init,l2 is the second ray tail initial intensity, I att,l2 is the second ray tail decay intensity, B l2 is the second ray tail translation coefficient, T base is the substrate element area density, T main is the main element area density in the coating layer, T obj is the target element area density.
[0147] It should be understood that the attenuation effect of the second ray on each element in the coating material can be considered the same, which is represented by μ l2 . The above formula is the second ray attenuation law formula of the coating material, B l2 can be understood as a coefficient in the attenuation law, and under the premise that each element in the coating material is determined, the theoretical value of B l2 is also determined. In this example, the attenuation effect of the beta ray as the second ray on the copper element, the carbon element, and the silicon element can be considered the same. T base can be measured by the first ray head detection device, I init,l2 and I att,l2 are measured by the second ray tail detection device. Therefore, the unknowns are the main element area density and the target element area density, i.e., the area density of the carbon element and the area density of the silicon element.
[0148] Further, before determining the second ray tail absorption coefficient and the second ray tail translation coefficient, the second ray tail absorption coefficient and the second ray tail translation coefficient are calibrated, specifically including the following steps:
[0149] A first standard coating material and a second standard coating material are obtained, the substrate element area density, the main element area density, and the target element area density in the first standard coating material and the second standard coating material are determined, and the total area density of each element in the first standard coating material and the total area density of each element in the second standard coating material are given;
[0150] The second ray tail first standard initial intensity, the second ray tail first standard decay intensity, the second ray tail second standard initial intensity, and the second ray tail second standard decay intensity for the first standard coating material and the second standard coating material are measured, respectively;
[0151] The second ray tail first standard initial intensity and the second ray tail first standard decay intensity are calculated by natural logarithm, and the second ray tail first standard decay degree is given;
[0152] The ratio of the second ray tail second standard initial intensity and the second ray tail second standard decay intensity is calculated by natural logarithm, and the second ray tail second standard decay degree is given;
[0153] The calibrated second ray tail absorption coefficient and the second ray tail translation coefficient are given by combining the second ray tail first standard decay degree, the total area density of each element in the first standard coating material, the second ray tail second standard decay degree, the total area density of each element in the second standard coating material, and based on the linear relationship.
[0154] In a specific embodiment, the standard substrate is coated with the target element and the main element, and the standard substrate needs to be coated twice to obtain the first standard coating material and the second standard coating material. It can be understood that the selection of the standard substrate and the coating of the target element and the main element are set according to the calibration requirements, that is, the area density of the substrate element, the area density of the main element and the area density of the target element in the first standard coating material and the second standard coating material are known. Then the first standard coating material and the second standard coating material are measured by using the second ray tail detection equipment respectively, and the second ray tail first standard initial intensity corresponding to the first standard coating material, the second ray tail first standard decay intensity and the second ray tail second standard initial intensity corresponding to the second standard coating material, and the second ray tail second standard decay intensity are obtained. The relevant data corresponding to the first standard coating material and the relevant data corresponding to the second standard coating material are substituted into the formula conforming to the second ray decay law respectively, and a binary linear equation set about the second ray tail absorption coefficient and the second ray tail translation coefficient is obtained, and the calibrated second ray tail absorption coefficient and the second ray tail translation coefficient are obtained by solving.
[0155] It should be noted that the area density of at least one element in the first standard coating material and the second standard coating material obtained by coating the standard substrate twice is different, and then the corresponding second ray tail first standard decay degree and the second ray tail second standard decay degree are different, so as to realize the solving of the second ray tail absorption coefficient and the second ray tail translation coefficient, and complete the calibration.
[0156] By calibrating the second ray tail absorption coefficient and the second ray tail translation coefficient, the measurement error caused by the instrument difference of the second ray tail detection equipment itself is avoided, and the accuracy of the data is improved, which provides a data basis for the detection of the content of the target element in the coating material.
[0157] Further, combined with the first standard attenuation degree of the second ray tail, the total area density of each element in the first standard coating material, and the second standard attenuation degree of the second ray tail, the total area density of each element in the second standard coating material, and based on the linear relationship, the calibrated second ray tail absorption coefficient and the second ray tail translation coefficient are given, which is specifically represented as:
[0158]
[0159] Wherein, μ cal,l2 is the calibrated second ray tail absorption coefficient, T all,sta1 is the total area density of each element in the first standard coating material, T all,sta2 is the total area density of each element in the second standard coating material, I init,l2,sta1 is the first standard initial intensity of the second ray tail, I att,l2,sta1 is the first standard attenuation intensity of the second ray tail, I init,l2,sta2 is the second standard initial intensity of the second ray tail, I att,l2,sta2 is the second standard attenuation intensity of the second ray tail, B cal,l2 is the calibrated second ray tail translation coefficient.
[0160] S105: Combined with the total area density of each element in the coating material, the substrate element area density and the first ray tail attenuation data, the main element area density and the target element area density in the coating layer are obtained, and the content of the target element in the coating material is given.
[0161] Further, combined with the total area density of each element in the coating material, the substrate element area density and the first ray tail attenuation data, the main element area density and the target element area density in the coating layer are obtained, and the content of the target element in the coating material is given. Figure 6 , specifically including the following steps:
[0162] Determine the first ray tail attenuation coefficient of the substrate element, the first ray tail attenuation coefficient of the main element and the first ray tail attenuation coefficient of the target element;
[0163] Calculate the ratio of the first ray tail initial intensity to the first ray tail attenuation intensity by natural logarithm, and give the first ray tail attenuation degree;
[0164] Combined with the first ray tail attenuation degree, the first ray tail attenuation coefficient of the substrate element, the first ray tail attenuation coefficient of the main element, the first ray tail attenuation coefficient of the target element, and the total area density of each element in the coating material, the substrate element area density, the main element area density and the target element area density in the coating layer are obtained.
[0165] In a specific embodiment, the first ray tail attenuation coefficient of the substrate element, the first ray tail attenuation coefficient of the main element, the first ray tail attenuation coefficient of the target element, the substrate element area density, the first ray tail initial intensity and the first ray tail attenuation intensity ratio are substituted into the corresponding first ray attenuation law of the coating material to obtain a first relationship about the main element area density and the target element area density. The total area density of each element in the coating material, the substrate element area density, the second ray tail absorption coefficient and the second ray tail translation coefficient are substituted into the corresponding second ray attenuation law of the coating material to obtain a second relationship about the main element area density and the target element area density. The first relationship and the second relationship are combined to obtain the main element area density and the target element area density.
[0166] Further, in combination with the first ray tail attenuation degree, the first ray tail attenuation coefficient of the substrate element, the first ray tail attenuation coefficient of the main element, the first ray tail attenuation coefficient of the target element and the total area density of each element in the coating material, the substrate element area density, the main element area density and the target element area density in the coating layer are obtained, which is specifically expressed as:
[0167]
[0168] Wherein, μ base,l1 is the first ray tail attenuation coefficient of the substrate element, μ main,l1 is the first ray tail attenuation coefficient of the main element, μ obj,l1 is the first ray tail attenuation coefficient of the target element, μ l2 is the second ray tail absorption coefficient, T base is the substrate element area density, T main is the main element area density in the coating layer, T obj is the target element area density, T all is the total area density of each element in the coating material, I init,l1 is the first ray tail initial intensity, I att,l1 is the first ray tail attenuation intensity, I init,l2 is the second ray tail initial intensity, I att,l2 is the second ray tail attenuation intensity, B l2 is the second ray tail translation coefficient.
[0169] Further, the content of the target element in the coating material is given, which specifically includes: calculating the proportion of the target element in the coating layer according to the main element area density and the target element area density, and giving the content of the target element in the coating material.
[0170] Further, the content of the target element in the coating material is given, which is specifically expressed as:
[0171]
[0172] wherein τ obj is the content of the target element in the coating material, T obj is the target element area density, T main is the main element area density.
[0173] Further, before determining the substrate element first ray tail attenuation coefficient, the main element first ray tail attenuation coefficient and the target element first ray tail attenuation coefficient, the method further comprises calibrating the substrate element first ray tail attenuation coefficient, the main element first ray tail attenuation coefficient and the target element first ray tail attenuation coefficient, and specifically comprising the following steps:
[0174] obtaining a standard substrate and a standard substrate element area density, and based on detection of the standard substrate by the first ray tail detection device, giving a calibrated substrate element first ray tail attenuation coefficient;
[0175] coating a main element coating layer on the surface of the standard substrate to obtain a main element standard coating material, and giving a standard main element area density;
[0176] based on detection of the main element standard coating material by the first ray tail detection device, and in combination with the substrate element first ray tail attenuation coefficient, giving a calibrated main element first ray tail attenuation coefficient;
[0177] coating a target element coating layer on the surface of the main element standard coating material to obtain a composite element standard coating material, and giving a standard target element area density;
[0178] based on detection of the composite element standard coating material by the first ray tail detection device, and in combination with the substrate element first ray tail attenuation coefficient and the main element first ray tail attenuation coefficient, giving a calibrated target element first ray tail attenuation coefficient.
[0179] Further, obtaining a standard substrate and a standard substrate element area density, and based on detection of the standard substrate by the first ray tail detection device, giving a calibrated substrate element first ray tail attenuation coefficient, specifically comprising the following steps:
[0180] obtaining a standard substrate and a standard substrate element area density;
[0181] measuring a first ray tail primary calibration initial intensity and a first ray tail primary calibration decay intensity for the standard substrate, and calculating a ratio of the first ray tail primary calibration initial intensity to the first ray tail primary calibration decay intensity in natural logarithm to give a first ray tail primary calibration decay degree;
[0182] based on the first ray tail primary calibration decay degree and the standard substrate element area density, giving a calibrated substrate element first ray tail attenuation coefficient.
[0183] Further, based on the detection of the standard substrate by the first-ray tail detection device, a calibrated substrate element first-ray tail attenuation coefficient is given, which is specifically represented as:
[0184]
[0185] wherein μ cal,base,l1 is the calibrated substrate element first-ray tail attenuation coefficient, T cal,base is the standard substrate element area density, I cal,init,l1,pri is the first-ray tail primary calibration initial intensity, and I cal,att,l1,pri is the first-ray tail primary calibration decay intensity.
[0186] In a specific embodiment, first, the standard substrate and the standard substrate element area density are obtained, and the standard substrate is detected by using the first-ray tail detection device to obtain the first-ray tail primary calibration initial intensity and the first-ray tail primary calibration decay intensity. The standard substrate element area density, the first-ray tail primary calibration initial intensity, and the first-ray tail primary calibration decay intensity are substituted into the first-ray attenuation law corresponding to the standard substrate to obtain the calibrated substrate element first-ray tail attenuation coefficient.
[0187] In a specific example, the standard substrate is copper, the copper is weighed to obtain the standard copper element area density, the copper is detected by using the first-ray tail detection device to obtain the first-ray tail primary calibration initial intensity and the first-ray tail primary calibration decay intensity, and the standard substrate element area density, the first-ray tail primary calibration initial intensity, and the first-ray tail primary calibration decay intensity are substituted into the first-ray attenuation law corresponding to the standard substrate, which is specifically represented as:
[0188]
[0189] wherein μ cal,Cu,l1 is the calibrated copper element first-ray tail attenuation coefficient, T cal,Cu is the standard copper element area density, I cal,init,l1,pri is the first-ray tail primary calibration initial intensity, and I cal,att,l1,pri is the first-ray tail primary calibration decay intensity. At this time, only the calibrated copper element first-ray tail attenuation coefficient is an unknown quantity, and the solution can be obtained.
[0190] Further, based on the detection of the standard substrate by the first-ray tail detection device, a calibrated substrate element first-ray tail attenuation coefficient is given, which is specifically represented as:
[0191] The initial intensity and attenuation intensity of the secondary calibration of the first X-ray machine tail were measured for the standard coating material of the main element. The ratio of the initial intensity to the attenuation intensity of the secondary calibration of the first X-ray machine tail was calculated using the natural logarithm, and the degree of attenuation of the secondary calibration of the first X-ray machine tail was given.
[0192] Based on the attenuation coefficient of the first X-ray machine tail of the substrate element and the areal density of the standard substrate element, the secondary calibration attenuation degree of the first X-ray machine tail of the substrate element is given.
[0193] Based on the attenuation degree of the primary X-ray machine tail secondary calibration, the attenuation degree of the primary element primary X-ray machine tail secondary calibration, and the areal density of the standard principal element, the attenuation coefficient of the primary element primary X-ray machine tail is given.
[0194] Furthermore, based on the detection of the main element standard coating material using the first-ray tail-end detection device, and combined with the first-ray tail-end attenuation coefficient of the substrate element, the calibrated first-ray tail-end attenuation coefficient of the main element is given, specifically expressed as follows:
[0195]
[0196] Where, μ cal,base,l1 For the calibration of the substrate element first-ray tail attenuation coefficient, T cal,base The surface density of the standard substrate element, μ cal,main,l1 For the calibration of the primary element first-ray tail attenuation coefficient, T cal,main For the standard principal element surface density, I cal,init,l1,sec To calibrate the initial intensity of the secondary stage of the first ray machine tail, I cal,att,l1,sec The attenuation intensity of the secondary stage at the tail of the first X-ray machine is calibrated.
[0197] In one specific implementation, based on the calibrated attenuation coefficient of the first X-ray tail of the substrate element, a main element coating layer 304 is coated on the surface of a standard substrate 303 to obtain a main element standard coating material, providing the standard main element areal density. The structure of the main element standard coating material is as follows: Figure 7 As shown. It is understandable that during the calibration process, the main element coating layer 304 is applied according to the calibration requirements, meaning the standard main element areal density is known. Then, the main element standard coating material is measured using a first-ray tail-end detection device to obtain the initial intensity and attenuation intensity of the first-ray tail-end secondary calibration. Substituting the substrate element's first-ray tail-end attenuation coefficient, the initial intensity, and the attenuation intensity of the first-ray tail-end secondary calibration, the standard main element areal density, and the standard substrate element areal density into the corresponding first-ray attenuation law of the main element standard coating material, the first-ray tail-end attenuation coefficient of the main element for calibration is obtained.
[0198] In one specific example, the standard base material 303 is copper, and the main element coating layer 304 is a carbon layer, and the carbon layer is coated on the copper to obtain a main element standard coating material, and a standard carbon element area density is given. The main element standard coating material is detected by using the first-ray tail detection device to obtain a first-ray tail secondary calibration initial intensity and a first-ray tail secondary calibration decay intensity. The standard carbon element area density, the standard copper element area density, the copper element first-ray tail decay coefficient, the first-ray tail secondary calibration initial intensity, and the first-ray tail secondary calibration decay intensity are substituted into the first-ray decay law corresponding to the main element standard coating material, which is specifically expressed as:
[0199]
[0200] wherein μ cal,Cu,l1 is the calibrated copper element first-ray tail decay coefficient, T cal,Cu is the copper element area density, μ cal,C,l1 is the calibrated carbon element first-ray tail decay coefficient, T cal,C is the standard carbon element area density, I cal,init,l1,sec is the first-ray tail secondary calibration initial intensity, I cal,att,l1,sec is the first-ray tail secondary calibration decay intensity. At this time, only the calibrated carbon element first-ray tail decay coefficient is an unknown quantity, and the solution can be obtained.
[0201] Further, based on the detection of the composite element standard coating material by the first-ray tail detection device, and in combination with the base material element first-ray tail decay coefficient and the main element first-ray tail decay coefficient, the calibrated target element first-ray tail decay coefficient is given, which specifically includes the following steps:
[0202] The first-ray tail final calibration initial intensity and the first-ray tail final calibration decay intensity for the composite element standard coating material are measured, and the ratio of the first-ray tail final calibration initial intensity to the first-ray tail final calibration decay intensity is calculated by using the natural logarithm to give the first-ray tail final calibration decay degree;
[0203] In combination with the base material element first-ray tail decay coefficient and the standard base material element area density, the base material element first-ray tail final calibration decay degree is given;
[0204] In combination with the main element first-ray tail decay coefficient and the standard main element area density, the main element first-ray tail final calibration decay degree is given;
[0205] In combination with the first-ray tail final calibration decay degree, the base material element first-ray tail final calibration decay degree, the main element first-ray tail final calibration decay degree, and the standard target element area density, the calibrated target element first-ray tail decay coefficient is given.
[0206] Further, based on the detection of the composite element standard coating material by the first-ray tail detection device, and in combination with the first-ray tail attenuation coefficient of the base element, the first-ray tail attenuation coefficient of the main element, the calibrated first-ray tail attenuation coefficient of the target element is given, which is specifically expressed as:
[0207]
[0208] Wherein, μ cal,base,l1 is the calibrated first-ray tail attenuation coefficient of the base element, T cal,base is the standard base element surface density, μ cal,main,l1 is the calibrated first-ray tail attenuation coefficient of the main element, T cal,main is the standard main element surface density, μ cal,obj,l1 is the calibrated first-ray tail attenuation coefficient of the target element, T cal,obj is the standard target element surface density, I cal,init,l1,ter is the first-ray tail final-stage calibration initial intensity, I cal,att,l1,ter is the first-ray tail final-stage calibration decay intensity.
[0209] In a specific embodiment, based on the calibrated first-ray tail attenuation coefficient of the base element and the first-ray tail attenuation coefficient of the target element, a target element coating layer 305 is coated on the surface of the main element standard coating material to obtain a composite element standard coating material, and the standard target element surface density is given. The structure of the composite element standard coating material is shown in Figure 8 It can be understood that in the calibration process, the target element coating layer 305 is coated according to the calibration requirements, that is, the standard target element surface density is known. Then the first-ray tail detection device is used to measure the composite element standard coating material to obtain the first-ray tail final-stage calibration initial intensity and the first-ray tail final-stage calibration decay intensity. The first-ray tail attenuation coefficient of the base element, the first-ray tail attenuation coefficient of the target element, the first-ray tail final-stage calibration initial intensity, the first-ray tail final-stage calibration decay intensity, the standard main element surface density, the standard base element surface density and the standard target element surface density are substituted into the corresponding first-ray attenuation law of the composite element standard coating material to obtain the calibrated first-ray tail attenuation coefficient of the target element.
[0210] In one specific example, the standard base material 303 is copper, the main element coating layer 304 is a carbon layer, and the target element coating layer 305 is a silicon layer. The carbon layer is coated on the copper, and then the silicon layer is coated, to obtain a composite element standard coating material, giving a standard silicon element area density. The composite element standard coating material is detected using the first ray tail detection device, to obtain a first ray tail final stage calibration initial intensity and a first ray tail final stage calibration decay intensity. The standard carbon element area density, the standard copper element area density, the standard silicon element area density, the copper element first ray tail decay coefficient, the carbon element first ray tail decay coefficient, the first ray tail final stage calibration initial intensity, and the first ray tail final stage calibration decay intensity are substituted into the first ray decay law corresponding to the composite element standard coating material, and are specifically expressed as:
[0211]
[0212] wherein μ cal,Cu,l1 is the calibrated copper element first ray tail decay coefficient, T cal,Cu is the standard copper element area density, μ cal,C,l1 is the calibrated carbon element first ray tail decay coefficient, T cal,C is the standard carbon element area density, μ cal,Si,l1 is the calibrated silicon element first ray tail decay coefficient, T cal,Si is the standard silicon element area density, I cal,init,l1,ter is the first ray tail final stage calibration initial intensity, and I cal,att,l1,ter is the first ray tail final stage calibration decay intensity. At this time, only the calibrated silicon element first ray tail decay coefficient is an unknown, and solving it can obtain
[0213] It should be understood that, in the process of obtaining the calibrated base material element first ray tail decay coefficient, the main element first ray tail decay coefficient, and the target element first ray tail decay coefficient, the standard base material, the main element coating layer, and the target element coating layer mentioned are not necessarily the same, but the corresponding elements are the same. For example, the first copper foil is used in the process of calibrating the base material element first ray tail decay coefficient, and in the calibration process of the main element first ray tail decay coefficient and the target element first ray tail decay coefficient, the first copper foil can be used, or other copper foils can be used. The base material element only limits the copper element, and does not limit other parameters such as volume and size. The same applies to the target element coating layer and the main element coating layer.
[0214] By calibrating the first ray machine tail attenuation coefficient of the base material element, the first ray machine tail attenuation coefficient of the main element and the first ray machine tail attenuation coefficient of the target element, on the one hand, the negative influence of the instrument difference of different detection equipment on the element content detection of the coating material can be reduced, and on the other hand, the influence of the superposition of different materials in the base material and the coating layer on the ray attenuation value and the element content data in the coating material can be avoided, so that the accuracy of the element content detection in the coating material is improved.
[0215] Reference Figure 9 The embodiment of the present application provides a kind of detection device of element content in coating material, comprising:
[0216] The measurement unit 201 includes a first ray machine head detection device, a first ray machine tail detection device and a second ray machine tail detection device, the first ray machine head detection device is used to measure the first ray machine head attenuation data of base material before coating, the first ray machine tail detection device is used to measure the first ray machine tail attenuation data of coating material, and the first ray machine tail detection device is used to measure the second ray machine tail attenuation data of coating material;
[0217] The coating unit 202 is used to coat the coating layer containing target element on the surface of base material, to form coating material;
[0218] The analysis unit 203 is used to give the surface density of base material element, and based on the second ray machine tail attenuation data of coating material, the total surface density of each element in coating material is given;The total surface density of each element in coating material, the surface density of base material element and the first ray machine tail attenuation data are combined to obtain the surface density of main element and target element in coating layer, and the content of target element in coating material is given.
[0219] Those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working process of the described module can refer to the corresponding process in the foregoing method embodiment, which will not be described here.
[0220] Although the preferred embodiments of the present application have been described, those skilled in the art can make further changes and modifications to these embodiments once they know the basic creative concept. Therefore, the appended claims are intended to include the preferred embodiments and all changes and modifications falling within the scope of the present application. Obviously, those skilled in the art can make various modifications and variations to the present application without departing from the spirit and scope of the present application. Thus, if these modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application also intends to include these modifications and variations.
Claims
1. A method for detecting the content of an element in a coating material, characterized by, The method comprises the following steps: measuring first ray head attenuation data of a base material before coating to obtain element area density of the base material; coating a coating layer containing target elements on the surface of the base material to form a coated material; measuring first ray tail attenuation data and second ray tail attenuation data of the coated material; obtaining total element area density of the coated material based on the second ray tail attenuation data of the coated material; combining the total element area density of the coated material, the element area density of the base material and the first ray tail attenuation data to obtain main element area density and target element area density in the coating layer, and then obtaining the content of the target elements in the coated material; the main element area density and the target element area density in the coating layer are specifically expressed as: ; wherein μ base,l1 is the base element first ray tail attenuation coefficient, μ main,l1 is the host element first ray tail attenuation coefficient, μ obj,l1 is the target element first ray tail attenuation coefficient, μ l2 is the second ray tail absorption coefficient, T base is the base element areal density, T main is the host element areal density in the coating layer, T obj is the target element areal density, T all is the total areal density of the elements in the coating material and , I init,l1 is the first ray tail initial intensity, I att,l1 is the first ray tail decay intensity, I init,l2 is the second ray tail initial intensity, I att,l2 is the second ray tail decay intensity, B l2 is the second ray tail translation coefficient.
2. The method of detecting the content of elements in a coating material according to claim 1, characterized by, a first ray head detection device is arranged at a head position before coating, and the first ray head attenuation data includes first ray head initial intensity and first ray head attenuation intensity; first ray tail detection equipment and second ray tail detection equipment are arranged at a tail position after coating, the first ray tail attenuation data includes first ray tail initial intensity and first ray tail attenuation intensity, and the second ray tail attenuation data includes second ray tail initial intensity and second ray tail attenuation intensity.
3. The method of detecting the content of elements in a coating material according to claim 1, wherein The first ray head attenuation data of the base material before coating is measured to obtain the element area density of the base material, which specifically includes the following steps: obtaining the first ray head initial intensity, the first ray head attenuation intensity, and determining the first ray head attenuation coefficient of the base material element; calculating the ratio of the first ray head initial intensity to the first ray head attenuation intensity by natural logarithm to obtain the first ray head attenuation degree; combining the first ray head attenuation degree and the first ray head attenuation coefficient of the base material element to obtain the element area density of the base material.
4. The method of detecting the content of elements in a coating material according to claim 3, wherein Before determining the first ray head attenuation coefficient of the base material element, the first ray head attenuation coefficient of the base material element is calibrated, which specifically includes the following steps: obtaining a standard base material and a standard base material element area density; measuring the first ray head calibration initial intensity and the first ray head calibration attenuation intensity for the standard base material, and calculating the ratio of the first ray head calibration initial intensity to the first ray head calibration attenuation intensity by natural logarithm to obtain the first ray head calibration attenuation degree; obtaining the calibrated first ray head attenuation coefficient of the base material element based on the first ray head calibration attenuation degree and the standard base material element area density.
5. The method of detecting the content of elements in a coating material according to claim 1, wherein The components of the coating layer include target elements and main elements.
6. The method of detecting the content of elements in a coating material according to claim 2, wherein Based on the second ray tail attenuation data of the coated material, the total element area density of the coated material is obtained, which specifically includes the following steps: determining the second ray tail absorption coefficient and the second ray tail translation coefficient; calculating the ratio of the second ray tail initial intensity to the second ray tail attenuation intensity by natural logarithm to obtain the second ray tail attenuation degree; combining the second ray tail attenuation degree, the second ray tail absorption coefficient and the second ray tail translation coefficient to obtain the total element area density of the coated material.
7. The method of detecting the content of elements in a coating material according to claim 6, wherein Before determining the second ray tail absorption coefficient and the second ray tail translation coefficient, the second ray tail absorption coefficient and the second ray tail translation coefficient are calibrated, which specifically includes the following steps: Obtaining the first standard coating material and the second standard coating material, respectively determining the substrate element surface density, the main element surface density and the target element surface density in the first standard coating material and the second standard coating material, and giving the total surface density of each element in the first standard coating material and the total surface density of each element in the second standard coating material; Respectively measuring the second ray tail first standard initial intensity, the second ray tail first standard decay intensity, the second ray tail second standard initial intensity and the second ray tail second standard decay intensity of the first standard coating material and the second standard coating material; Calculating the second ray tail first standard initial intensity and the second ray tail first standard decay intensity by natural logarithm, and giving the second ray tail first standard decay degree; Calculating the ratio of the second ray tail second standard initial intensity and the second ray tail second standard decay intensity by natural logarithm, and giving the second ray tail second standard decay degree; Combining the second ray tail first standard decay degree, the total surface density of each element in the first standard coating material and the second ray tail second standard decay degree, the total surface density of each element in the second standard coating material, and based on the linear relationship, giving the calibrated second ray tail absorption coefficient and the second ray tail translation coefficient.
8. The method of detecting the content of elements in a coating material according to claim 1, wherein It also includes calibrating the substrate element first ray tail decay coefficient, the main element first ray tail decay coefficient and the target element first ray tail decay coefficient, which specifically includes the following steps: Obtaining the standard substrate and the standard substrate element surface density, and based on the detection of the standard substrate by the first ray tail detection device, giving the calibrated substrate element first ray tail decay coefficient; Coating a main element coating layer on the surface of the standard substrate to obtain a main element standard coating material, and giving the standard main element surface density; Based on the detection of the main element standard coating material by the first ray tail detection device, and combining the substrate element first ray tail decay coefficient, giving the calibrated main element first ray tail decay coefficient; Coating a target element coating layer on the surface of the main element standard coating material to obtain a composite element standard coating material, and giving the standard target element surface density; Based on the detection of the composite element standard coating material by the first ray tail detection device, and combining the substrate element first ray tail decay coefficient and the main element first ray tail decay coefficient, giving the calibrated target element first ray tail decay coefficient.
9. The method of detecting the content of elements in a coating material according to claim 8, wherein Based on the detection of the composite element standard coating material by the first ray tail detection device, and combining the substrate element first ray tail decay coefficient and the main element first ray tail decay coefficient, giving the calibrated target element first ray tail decay coefficient, specifically including the following steps: Measuring the first ray tail final stage calibration initial intensity and the first ray tail final stage calibration decay intensity of the composite element standard coating material, and calculating the ratio of the first ray tail final stage calibration initial intensity and the first ray tail final stage calibration decay intensity by natural logarithm, giving the first ray tail final stage calibration decay degree; Combining the substrate element first ray tail decay coefficient and the standard substrate element surface density, giving the substrate element first ray tail final stage calibration decay degree; The first ray tail end attenuation degree of the main element is combined with the standard main element surface density to give a first ray tail end calibration attenuation degree of the main element. The first ray tail end calibration attenuation degree of the main element, the first ray tail end calibration attenuation degree of the base material element, the first ray tail end calibration attenuation degree of the main element, and the standard target element surface density are combined to give a calibrated target element first ray tail end attenuation coefficient.
10. The method of detecting the content of elements in a coating material according to claim 1, wherein The content of the target element in the coating material is given, specifically including: according to the main element surface density and the target element surface density, the proportion of the target element in the coating layer is calculated, and the content of the target element in the coating material is given.
11. An apparatus for detecting the content of an element in a coated material, characterized by The detection method for the content of elements in the coating material is adopted, specifically including: The measuring unit includes a first ray head detection device, a first ray tail end detection device, and a second ray tail end detection device, the first ray head detection device is used to measure the first ray head attenuation data of the base material before coating, the first ray tail end detection device is used to measure the first ray tail end attenuation data of the coating material, and the second ray tail end detection device is used to measure the second ray tail end attenuation data of the coating material; The coating unit is used to coat a coating layer containing the target element on the surface of the base material to form a coated material; The analysis unit is used to give the base material element surface density, and based on the second ray tail end attenuation data of the coating material, the total surface density of each element in the coating material is given; the total surface density of each element in the coating material, the base material element surface density, and the first ray tail end attenuation data are combined to obtain the main element surface density and the target element surface density in the coating layer, and the content of the target element in the coating material is given; the main element surface density and the target element surface density in the coating layer are specifically represented as: ; where μ base,l1 is the base element first ray tail attenuation coefficient, μ main,l1 is the host element first ray tail attenuation coefficient, μ obj,l1 is the target element first ray tail attenuation coefficient, μ l2 is the second ray tail absorption coefficient, T base is the base element areal density, T main is the host element areal density in the coating layer, T obj is the target element areal density, T all is the total areal density of each element in the coating material and , I init,l1 is the first ray tail initial intensity, I att,l1 is the first ray tail decay intensity, I init,l2 is the second ray tail initial intensity, I att,l2 is the second ray tail decay intensity, B l2 is the second ray tail translation coefficient.
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