Xrd-based online analysis system for copper foil crystal structure

Abstract

This invention relates to the field of online monitoring and control technology in materials manufacturing, and discloses an XRD-based online analysis system for the crystal structure of copper foil. The system includes a construction module, a monitoring module, a focusing module, and a strategy formulation module. The system establishes a sample-specific diffraction behavior profile, compares historical spectra in real time to identify dynamic changes in intensity and full width at half maximum (FWHM), and generates a structural state vector quantifying the real-time state. This vector is then analyzed to locate the diffraction angle range corresponding to crystal structure anomalies and mapped to the specific physical location of the copper foil. Based on historical intervention data of the anomaly coordinates, targeted structural control commands are automatically generated. This system achieves highly sensitive online monitoring of the dynamic evolution of the copper foil crystal structure and can directly correlate microstructural anomalies to physical locations and drive precise process intervention, thereby improving the level of intelligent control in the production process.

Description

Technical Field

[0001] This invention relates to the field of online monitoring and control technology in materials manufacturing, specifically to an online analysis system for the crystal structure of copper foil based on XRD. Background Technology

[0002] In the fields of high-end electronic circuits and lithium battery manufacturing, the uniformity and stability of the crystal structure of copper foil are key factors determining its mechanical properties, conductivity, and subsequent processing quality. Currently, industry monitoring of copper foil crystal structure mainly relies on offline sampling inspection using laboratory X-ray diffractometers. This method is static and lagging, only obtaining phase composition information for a specific sample at a certain point in time. The production process is a continuous and dynamic process, and the crystal structure evolves in real time with fluctuations in process parameters. Offline sampling inspection cannot capture this dynamic change process, cannot record the complete structural evolution history of a specific production line or material batch, and has serious monitoring blind spots.

[0003] Structural anomaly conclusions obtained from offline analysis are typically presented in the form of inspection reports. These reports only indicate that the material "has a problem," but cannot quickly and accurately pinpoint the specific physical location of the anomaly on continuously produced copper foil rolls. After an anomaly is discovered, process adjustments heavily rely on the engineer's experience. Engineers need to work backward from macroscopic quality feedback to deduce possible adjustments to process parameters. This "post-mortem correction" approach is inefficient, and the adjustment process lacks direct data support specific to the type of structural anomaly, potentially leading to over-adjustment or under-adjustment, resulting in additional quality and cost losses. Summary of the Invention

[0004] The purpose of this invention is to provide an online analysis system for copper foil crystal structures based on XRD, so as to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides an online analysis system for the crystal structure of copper foil based on XRD, the system comprising:

[0006] The diffraction profile construction module acquires raw diffraction signals from an online XRD detector, performs waveform purification, performs baseline calibration, and establishes a diffraction behavior profile for copper foil samples through pattern standardization.

[0007] The dynamic spectrum monitoring module compares the current diffraction pattern with the historical patterns in the archive in real time based on the diffraction behavior archive, identifies the intensity drift at a specific angle in the pattern, tracks the change trajectory of the full width at half maximum (FWHM), determines the real-time state of the crystal structure, and generates a structure state vector.

[0008] The anomaly focusing module analyzes the structural state vector, locates the diffraction angle interval where intensity drift and half-width change occur simultaneously, calculates the structural instability index of the diffraction angle interval, maps it to the physical spatial location of the copper foil, and outputs the coordinates of the anomaly region.

[0009] The intervention strategy formulation module retrieves historical intervention records corresponding to the coordinates of the abnormal area, evaluates the prior effects of different intervention parameters, and generates customized structural intervention instructions for the current abnormal area.

[0010] Preferably, the diffraction behavior profile includes at least purified diffraction waveform data, calibrated baseline reference, standardized spectral template, and historical diffraction feature set; the structural state vector includes real-time intensity drift, half-width at half-maximum change trajectory descriptor, and crystal state determination label; the abnormal region coordinates include diffraction angle range, physical location mapping information, and structural instability index; and the customized structural intervention instructions include intervention parameter combinations, execution sequence, and expected adjustment targets.

[0011] Preferably, the diffraction profile construction module specifically performs the following steps:

[0012] Receive the raw diffraction signal stream from the online XRD detector;

[0013] The original diffraction signal stream is subjected to waveform purification processing to remove noise and equipment artifacts;

[0014] Baseline calibration is performed on the purified waveform to eliminate the long-term drift effect of background scattering;

[0015] The calibrated diffraction pattern was compared with the standard sample pattern, and the pattern was standardized to unify the intensity and angle scales.

[0016] The purified waveform, calibration baseline, and standardized spectra are integrated to construct and update the diffraction behavior profile.

[0017] Preferably, the dynamic spectrum monitoring module specifically performs the following steps:

[0018] Retrieve historical map templates and historical diffraction feature sets from the diffraction behavior archive;

[0019] The current real-time diffraction pattern is compared point by point with the historical pattern template to calculate the intensity difference in the angular dimension.

[0020] Identify specific diffraction angles where the intensity difference continuously exceeds a threshold and mark them as intensity drift regions;

[0021] Simultaneously analyze the diffraction peak shape in the intensity drift region and trace the change trajectory of its full width at half maximum (FWHM) over time;

[0022] By combining the intensity drift and the half-width at half-maximum variation trajectory, the real-time state of the crystal structure is determined, and the structure state vector is encapsulated and generated.

[0023] Preferably, the anomaly focusing module specifically performs the following steps:

[0024] The real-time intensity drift and half-width variation trajectory descriptor contained in the structural state vector are analyzed.

[0025] In the diffraction angle space, locate those continuous intervals that simultaneously exhibit significant intensity shifts and changes in full width at half maximum (FWHM).

[0026] Based on the severity and spatial continuity of the drift and change trajectory, the structural instability index of the continuous interval is calculated;

[0027] Based on the spatial geometric relationship between the XRD detector and the copper foil sample, the diffraction angle range is mapped to the physical position coordinates of the copper foil surface;

[0028] The coordinates of the abnormal region are formed by combining the structural instability index with the physical location coordinates.

[0029] Preferably, the intervention strategy formulation module specifically performs the following steps:

[0030] Receive the coordinates of the abnormal area and extract the physical location mapping information therein;

[0031] In the historical intervention record database, retrieve all prior intervention cases associated with the physical location mapping information;

[0032] Analyze the combination of intervention parameters used in each prior intervention case and their actual adjustment effect on the crystal structure;

[0033] Based on the structural instability index of the current anomalous region, the most suitable intervention parameters are screened and evaluated from prior cases;

[0034] By integrating the selected intervention parameters and the process timing requirements of the copper foil production line, the customized structural intervention instructions are generated.

[0035] Preferably, the system further includes a spectrum depth analysis module, which receives the structure state vector generated by the dynamic spectrum monitoring module, performs deconvolution fitting on the marked abnormal diffraction peaks therein, separates overlapping peak components, extracts the precise angular position, integral intensity and micro-strain parameters of each sub-peak, and generates a lattice distortion depth report.

[0036] Preferably, the map depth analysis module specifically performs the following steps:

[0037] Extract diffraction peak data containing anomalous changes from the structural state vector;

[0038] An iterative approximation method is used to fit the peak shape function of the diffraction peak segments to achieve the separation of overlapping peaks;

[0039] Extract precise Bragg angle, integral intensity, and peak width parameters from the separated sub-peaks;

[0040] Based on the peak shape and width parameter of the sub-peak, the micro-strain value characterizing the degree of micro-lattice distortion is calculated;

[0041] The parameters and microstrain values ​​of all sub-peaks are summarized to generate the lattice distortion depth report.

[0042] Preferably, the system further includes a strategy optimization module, which simultaneously receives the coordinates of the abnormal region output by the anomaly focusing module and the lattice distortion depth report generated by the map depth analysis module, cross-validates the physical location of the abnormal region and the lattice distortion type, adjusts the weights of the intervention parameters according to the distortion type, and outputs the optimized structural intervention command.

[0043] Preferably, the system further includes a closed-loop execution verification module, which receives customized structural intervention instructions generated by the intervention strategy formulation module, sends the instructions to the production line control system, and triggers a new round of diffraction signal acquisition after the instructions are executed. By comparing the differences in diffraction behavior files before and after the intervention, the intervention effect is verified, and the verification results are fed back to the historical intervention record database of the intervention strategy formulation module.

[0044] Compared with the prior art, the beneficial effects of the present invention are:

[0045] By establishing a dedicated diffraction behavior archive reflecting the evolution history of the crystal structure of copper foil from a specific production line or batch, and dynamically comparing and analyzing the trends of real-time acquired diffraction patterns with historical pattern sequences in the archive, subtle features such as the trend drift of X-ray diffraction intensity at specific diffraction angles and the continuous variation trajectory of the full width at half maximum (FWHM) of diffraction peaks can be identified. This relative change monitoring mode based on its own historical data improves the detection sensitivity and early identification capability of changes in the microscopic state of the crystal structure. The identified multi-dimensional change features are fused and quantified into a structural state vector, achieving continuous and digital characterization of the health and stability of the copper foil crystal structure, providing a precise quantitative basis for real-time assessment of the structural state.

[0046] By analyzing the structural state vector using algorithms, the system locates a specific angular range where diffraction intensity and half-width at half-maximum (FWHM) change synergistically. It then calculates the structural instability index for this range and maps the anomaly of the diffraction signal to the physical spatial coordinates of the copper foil strip, directly outputting the location information of the anomaly region. Based on these anomaly coordinates, the system automatically retrieves and correlates historical anomalies of the same type or location stored in the database, along with all corresponding process intervention records. By evaluating the historical effects of different combinations of intervention parameters, it generates customized process adjustment instructions for the current anomaly pattern and location. This process achieves an automated closed loop, from detecting microscopic diffraction anomalies to accurately locating macroscopic physical positions and generating targeted process intervention strategies, transforming offline analysis conclusions into online control actions. Attached Figure Description

[0047] Figure 1 This is a timing diagram of the XRD-based online analysis system for copper foil crystal structures described in this invention.

[0048] Figure 2 A flowchart illustrating the work involved in building the diffraction archive module;

[0049] Figure 3 A flowchart illustrating the operation of the exception focusing module;

[0050] Figure 4 Thermal distribution of structural instability index in abnormal regions of copper foil;

[0051] Figure 5 The composite spectrum of XRD diffraction intensity and full width at half maximum (FWHM) anomaly during the verification stage of copper foil. Detailed Implementation

[0052] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0053] Please see Figure 1This invention provides an online analysis system for copper foil crystal structures based on XRD. The system integrates multiple functional modules to achieve real-time monitoring, anomaly diagnosis, and intervention strategy generation for copper foil crystal structures. The core of the system includes a diffraction profile construction module, a dynamic spectrum monitoring module, an anomaly focusing module, and an intervention strategy formulation module. These modules work together to complete the entire process from raw signal acquisition to intervention command generation. The diffraction profile construction module processes the raw diffraction signals from the online XRD detector, establishing a diffraction behavior profile of the copper foil sample through waveform purification, baseline calibration, and spectrum standardization. The dynamic spectrum monitoring module compares the current and historical diffraction patterns in real time based on this profile, identifies intensity drift and changes in full width at half maximum (FWHM), and generates a structural state vector. The anomaly focusing module analyzes this vector, locates the abnormal diffraction angle range, calculates the structural instability index, and maps it to the physical space to output the coordinates of the abnormal region. The intervention strategy formulation module retrieves historical intervention records based on the coordinates, evaluates the effectiveness of intervention parameters, and generates customized structural intervention commands.

[0054] In one embodiment of the present invention, the diffraction behavior archive includes at least purified diffraction waveform data, calibrated baseline reference, standardized spectral template, and a set of historical diffraction features. These data are continuously acquired and standardized to form a complete archive. The structural state vector consists of real-time intensity drift, a half-width at half-maximum (FWHM) change trajectory descriptor, and a crystal state determination label, used to quantify the dynamic changes in the crystal structure. The coordinates of the anomalous region include diffraction angle ranges, physical location mapping information, and a structural instability index, which spatially map diffraction anomalies to specific locations on the copper foil. Customized structural intervention instructions cover intervention parameter combinations, execution sequence, and expected adjustment targets, ensuring precise matching between intervention measures and anomaly types.

[0055] In practice, the diffraction behavior archive includes at least purified diffraction waveform data, a calibrated baseline reference, a standardized spectral template, and a historical diffraction feature set. The purified diffraction waveform data comes from the waveform purification process, the calibrated baseline reference originates from the baseline calibration operation, the standardized spectral template is generated by comparing it with standard sample spectra, and the historical diffraction feature set is a summary of features extracted from a series of historical standardized spectra. In practice, the diffraction behavior archive serves as a dynamically updated database, continuously integrating the processing results from the diffraction archive construction module.

[0056] In practical implementation, the structural state vector includes real-time intensity drift, a half-width at half-maximum (HWHM) change trajectory descriptor, and a crystal state determination label. The real-time intensity drift is calculated through real-time comparison by the dynamic spectrum monitoring module. The HWHM change trajectory descriptor records the sequence data of the HWHM evolution of a specific diffraction peak over time. The crystal state determination label is a classification identifier for the stability of the crystal structure based on the combination of intensity drift and HWHM change trajectory. Optionally, the crystal state determination label can adopt a three-level classification: "stable," "metastable," and "instable."

[0057] In practical implementation, the coordinates of the anomalous region include the diffraction angle range, physical location mapping information, and structural instability index. The diffraction angle range is determined by the anomalous focusing module's positioning in the diffraction angle space. The physical location mapping information is calculated based on the spatial geometric calibration relationship between the XRD detector and the copper foil sample. The structural instability index is a numerical value used to quantify the degree of anomalousness. In practical implementation, the structural instability index is calculated jointly by the intensity drift and the half-width at half-maximum variation trajectory within the diffraction angle range, and its calculation formula is expressed as follows:

[0058]

[0059] in: This represents a structural instability index. The normalized intensity shift, The normalized half-width variation trajectory descriptor statistics represent the statistical values. and These are preset weighting factors that correspond to the intensity and peak shape changes, respectively.

[0060] In practical implementation, customized structural intervention instructions include intervention parameter combinations, execution sequence, and expected adjustment targets. The intervention parameter combinations are a set of process parameters selected from historical cases. The execution sequence specifies the order and timing of each parameter's actions in production line control. The expected adjustment targets clarify the desired crystal structure state after the instructions are executed. Optionally, the intervention parameter combinations may involve annealing temperature, rolling force, or tension values. It can be understood that the diffraction behavior profile, structural state vector, abnormal region coordinates, and customized structural intervention instructions together constitute the core carrier of data flow within the system. Their clear composition and structure define the norms for information interaction between modules, ensuring the consistency of analysis logic and the clarity of the execution path.

[0061] In one embodiment of the present invention, see [reference] Figure 2The diffraction profile construction module receives the raw diffraction signal stream from the online XRD detector and performs waveform purification to remove noise and equipment artifacts. The purified waveform undergoes baseline calibration to eliminate the long-term drift effects of background scattering. The calibrated diffraction pattern is compared with the standard sample pattern and standardized to unify intensity and angle scales. The purified waveform, calibration baseline, and standardized pattern are then integrated to construct and update the diffraction behavior profile. The dynamic spectrum monitoring module retrieves historical spectrum templates and historical diffraction feature sets from the diffraction behavior profile. It compares the currently acquired real-time diffraction pattern with the historical spectrum templates point-by-point, calculating the intensity difference in the angular dimension. Specific diffraction angles where the intensity difference continuously exceeds a threshold are identified and marked as intensity drift regions. The diffraction peak shape in these intensity drift regions is analyzed simultaneously, and the trajectory of their full width at half maximum (FWHM) changes over time is tracked. The real-time state of the crystal structure is determined by combining the intensity drift and the FWHM change trajectory, and a structure state vector is generated.

[0062] In practice, the diffraction profile construction module receives the raw diffraction signal stream from the online X-ray diffraction detector. This raw signal stream is a continuous angle-intensity data sequence containing background noise and device artifacts. Waveform purification removes noise and artifacts by applying digital filters and thresholding, such as using wavelet transform to separate high-frequency noise and morphological filtering to suppress pulse artifacts. In the implementation, a baseline calibration operation is performed on the purified waveform. Baseline calibration is achieved by fitting the background scattering curve and subtracting its long-term drift component. The calibrated diffraction pattern is then compared with a reference pattern from a standard copper foil sample to perform pattern standardization. Pattern standardization unifies the intensity and angle scales of patterns acquired from different batches or detection locations. Finally, the purified waveform data, the calibrated baseline reference, and the standardized pattern template are integrated to construct and continuously update the diffraction behavior profile.

[0063] In some embodiments, the dynamic spectrum monitoring module retrieves historical spectrum templates and historical diffraction feature sets from the diffraction behavior archive. The historical spectrum template is a standardized diffraction pattern representing the average state of a stable process stage. The historical diffraction feature set contains the precise angular positions, peak intensities, and full width at half maximum (FWHM) characteristic values ​​of the main diffraction peaks in the template. The dynamic spectrum monitoring module compares the currently acquired real-time diffraction pattern with the historical spectrum template point by point, calculating the intensity difference at each diffraction angle point. The formula for calculating the intensity difference is expressed as:

[0064]

[0065] in: Represents the angle Normalized difference values ​​at the location, This represents the current real-time diffraction pattern at the angle. Strength at that location, Representing historical atlas templates at angles Strength at that location, It is a confidence weight factor that is related to the angle.

[0066] Taking the production monitoring of a certain batch of 12μm lithium battery copper foil as an example, the historical spectrum template of the stable process stage in the diffraction behavior archive is called up, and the diffraction angle is... Location, historical strength The intensity of the diffraction pattern currently acquired in real time at this angle Based on prior calibration, the confidence weight factor corresponding to this angle is... Since this angle is the main diffraction peak position of the copper foil, its confidence level is higher than that of other angles. Substituting it into the formula, we can obtain the result. The intensity difference threshold was set to 2000. The calculated result, 2646, exceeded the threshold for three consecutive acquisition cycles. Therefore, θ... The region was marked as an intensity drift region. Simultaneous analysis of the diffraction peak shape in this region revealed that the full width at half maximum (FWHM) increased from an initial 0.15° to 0.18° at a rate of 0.01° / s, exceeding the FWHM change rate threshold of 0.005° / s. Based on this, the crystal state was determined to be "metastable," and a structural state vector was generated containing the real-time intensity drift of 2450, the FWHM change trajectory descriptor [0.15°, 0.16°, 0.18°], and the "metastable" label.

[0067] Optionally, the diffraction peak shape in the intensity drift region can be analyzed simultaneously, tracking the change trajectory of its half-width at half-maximum (HWHM) over time. This involves fitting the peak shape of the diffraction peaks in this region and recording their HWHM values ​​for each acquisition cycle, thus forming a time series. By combining the calculated intensity drift with the observed HWHM change trajectory, the dynamic spectrum monitoring module determines the real-time state of the crystal structure according to preset judgment rules. For example, when the intensity drift exceeds a first threshold and the HWHM change rate exceeds a second threshold, it is judged as "abnormal." Finally, the real-time intensity drift, HWHM change trajectory descriptor, and crystal state judgment label are encapsulated to generate a structure state vector. In specific implementations, the filter parameters used for waveform purification and the model parameters for baseline calibration can be configured according to the specific model of the online X-ray diffraction detector and the copper foil production line environment. In some embodiments, the spectrum normalization process uses rigid transformation or nonlinear stretching algorithms to ensure precise alignment of the current spectrum with the standard sample spectrum at the characteristic peak positions.

[0068] In one embodiment of the present invention, see [reference] Figure 3The anomaly focusing module analyzes the real-time intensity drift and half-width at half-maximum (HWHM) change trajectory descriptors contained in the structural state vector, locating continuous intervals in the diffraction angle space that simultaneously exhibit significant intensity drift and HWHM changes. Based on the severity and spatial continuity of the drift and trajectory changes, the structural instability index of the continuous interval is calculated. The diffraction angle interval is mapped to the physical position coordinates of the copper foil surface according to the spatial geometric relationship between the XRD detector and the copper foil sample. The structural instability index and physical position coordinates are combined to form the anomaly region coordinates. The intervention strategy formulation module receives the anomaly region coordinates and extracts the physical position mapping information. It retrieves all prior intervention cases associated with the physical position mapping information from the historical intervention record database. It analyzes the combination of intervention parameters used in each prior intervention case and its actual adjustment effect on the crystal structure. Based on the structural instability index of the current anomaly region, it selects and evaluates the most suitable intervention parameters from the prior cases. The selected intervention parameters and the process timing requirements of the copper foil production line are integrated to generate customized structural intervention instructions.

[0069] In practical implementation, the anomaly focusing module parses the real-time intensity drift and half-width at half-maximum (HWHM) change trajectory descriptor contained in the structural state vector. The real-time intensity drift is a data sequence distributed along the diffraction angle dimension, and the HWHM change trajectory descriptor records the HWHM values ​​at specific angles at multiple historical time points. In practice, continuous intervals exhibiting both significant intensity drift and HWHM changes are located in the diffraction angle space. This is achieved by traversing the diffraction angles and applying a dual threshold judgment logic: a diffraction angle point must satisfy both an intensity drift greater than threshold A and its corresponding HWHM change greater than threshold B, and adjacent angle points meeting these conditions are aggregated into a continuous interval.

[0070] In some embodiments, a structural instability index for a continuous interval is calculated based on the severity of the drift and the trajectory of change, as well as spatial continuity. Severity is assessed by quantifying the magnitude of the intensity drift and the rate of change of the full width at half maximum (FWHM), while spatial continuity considers the angular range covered by the continuous interval. The formula for calculating the structural instability index is expressed as follows:

[0071]

[0072] in: This represents a structural instability index. This represents the severity of the drift in the normalized average intensity. This represents the severity of the change in the half-width at half-maximum after normalization. and These are preset combination factors corresponding to two different levels of severity. It is a spatial continuity multiplier that is positively correlated with the continuous angular range. In practice, the diffraction angle range is mapped to the physical position coordinates of the copper foil surface based on the spatial geometric relationship between the X-ray diffraction detector and the copper foil sample. The spatial geometric relationship is pre-calibrated by the incident angle of the detector, the position of the sample stage, and the sample size. The mapping process is completed by solving the geometric transformation equation.

[0073] Optionally, the intervention strategy formulation module receives the coordinate data packet of the abnormal region and extracts the physical location mapping information, which exists in the form of two-dimensional coordinates or partition numbers. It retrieves all prior intervention cases associated with the physical location mapping information from the historical intervention record database. This database records the location of each past anomaly, the combination of intervention parameters used, and the adjustment effect data of the crystal structure after execution. It analyzes the combination of intervention parameters used in each prior intervention case and its actual adjustment effect on the crystal structure. The actual adjustment effect on the crystal structure is quantified by comparing the changes in diffraction pattern characteristics before and after the intervention. Based on the structural instability index of the current abnormal region, it selects and evaluates the most suitable intervention parameters from the prior cases. The selection process involves similarity calculations, such as calculating the Euclidean distance between the current instability index and the anomaly index in historical cases. In specific implementations, the values ​​of threshold A and threshold B can be dynamically configured according to the process specifications of different copper foil products. In some embodiments, the design of the spatial continuity multiplier M allows for a higher instability index in anomaly regions with a wider coverage angle.

[0074] In one embodiment of the present invention, the system adds a spectrum depth analysis module. This module receives the structure state vector generated by the dynamic spectrum monitoring module and performs deconvolution fitting on the marked abnormal diffraction peaks to separate overlapping peak components. The precise angular position, integral intensity, and micro-strain parameters of each sub-peak are extracted from the separated sub-peaks to generate a lattice distortion depth report. The spectrum depth analysis module extracts diffraction peak segment data containing abnormal changes from the structure state vector and uses an iterative approximation method to fit the peak shape function to achieve the separation of overlapping peaks. The precise Bragg angle, integral intensity, and peak width parameters of the separated sub-peaks are extracted, and the micro-strain value characterizing the degree of micro-lattice distortion is calculated based on the peak width parameter of the sub-peaks. The parameters and micro-strain values ​​of all sub-peaks are summarized to generate a lattice distortion depth report.

[0075] In practical implementation, the spectral depth analysis module receives the structural state vector generated by the dynamic spectral monitoring module. This vector contains information on anomalous diffraction peak segments marked by crystal state determination tags. Specifically, diffraction peak segment data containing anomalous changes is extracted from the structural state vector. This data typically encompasses the intensity distribution data within a specific angular range extending outwards from the anomalous diffraction peak. An iterative approximation method is used to fit the peak shape function to separate overlapping peaks. Examples of iterative approximation methods include the Levenberg-Marquardt algorithm, which continuously adjusts the parameters of multiple peak shape functions to minimize the residual between the fitted curve and the original data. Commonly used peak shape functions include the Pseudo-Voigt function or the Pearson VII function. In practical implementation, precise Bragg angle, integral intensity, and peak width parameters are extracted from the separated sub-peaks. The precise Bragg angle corresponds to the angle value at the sub-peak apex. The integral intensity is obtained by calculating the area under the sub-peak's peak shape curve. The peak width parameter typically refers to the full width at half maximum (FWHM) of the sub-peak.

[0076] In some embodiments, the micro-strain value characterizing the degree of micro-lattice distortion is calculated based on the peak shape width parameter of the separated sub-peaks. The formula for calculating the micro-strain value is expressed as follows:

[0077]

[0078] in: Represents the microstrain value expressed as a percentage. This represents the actual physical broadening value of the i-th sub-peak after instrument broadening correction. The reference peak width represents the strain-free standard sample. A structured lattice distortion depth report is generated by summarizing the Bragg angle, integral intensity, peak width parameters, and calculated microstrain values ​​of all sub-peaks separated from the anomalous diffraction peak segments.

[0079] Taking sub-peak 1, separated from an abnormal diffraction peak segment through deconvolution fitting, as an example, with a Bragg angle of 43.35°, its peak width was measured. A strain-free standard copper foil was selected as the reference sample, and the reference peak width was measured at the same diffraction angle. Specifically, after instrument broadening correction, the instrument broadening contribution of the broadening curve function at 43.35° is 0.003°, and the original measured reference peak width is 0.151°. After deducting the instrument broadening, we get... Substituting into the formula, we can obtain... Similarly, for sub-peak 2, the Bragg angle of 43.52° is calculated. , ,have to ; Sub-peak 3, Bragg angle 43.70°, , (Instrument broadening correction value 0.003°), resulting in The microscopic strain values ​​and related parameters of the three sub-peaks are summarized to generate a lattice distortion depth report, which clarifies that the region corresponding to sub-peak 2 is a high-distortion region, providing core data support for the strategy optimization module.

[0080] Optionally, when the spectrum depth analysis module performs deconvolution fitting on diffraction peak segments, the number of sub-peaks can be automatically determined using statistical criteria such as goodness of fit or residual analysis. The sub-peak parameters extracted after deconvolution fitting can be organized into a data table, see Table 1.

[0081] Table 1: Sub-peak Parameters of Deconvolution Fitting

[0082] ;

[0083] In some embodiments, the instrument broadening correction value The broadening correction value needs to be obtained by measuring the diffraction peak width of a standard sample and establishing a broadening curve function. In practice, obtaining the instrument broadening correction value relies on systematic measurement and function modeling of the strain-free standard sample. The standard sample is a calibrated copper foil with a complete crystal structure and no internal stress. Its diffraction pattern is acquired at multiple Bragg angles using an online X-ray diffraction detector, and the full width at half maximum (FWHM) of each diffraction peak is accurately measured as a reference peak width value. Based on these measurement data, a broadening curve function is established using a polynomial or spline function fitting with the diffraction angle as the independent variable and the peak width as the dependent variable. This function describes the peak broadening characteristics of the instrument itself at different angles. In actual analysis, the measured peak width of the diffraction peak of the copper foil sample to be tested is substituted into this broadening curve function for interpolation or calculation, thereby separating the broadening portion contributed by the instrument and obtaining the physical broadening value purely caused by crystal micro-distortion, providing accurate input for subsequent micro-strain calculations. It is understandable that the successful application of the iterative approximation method depends on the rationality of the initial parameter settings, which can be estimated based on standard card data or historical fitting results.

[0084] See Figure 4In stage 8 of the online analysis of the copper foil crystal structure, the heatmap visually presented the distribution of structural instability indices corresponding to different physical locations and diffraction angle ranges. Specifically, the vertical axis of the graph represents the physical location of the copper foil (including locations 1, 2, and 3), and the horizontal axis represents the diffraction angle ranges (43.2-43.4°, 43.4-43.6°, 43.6-43.8°). The color of the blocks and their numerical values ​​correspond to the structural instability index (right-side color scale). From the distribution characteristics, the region corresponding to physical location 2 and the diffraction angle of 43.4-43.6° has a structural instability index of 1.72 (significantly higher than other regions), while the indices in other regions are concentrated in the 0.85-1.02 range. This distribution result highly corresponds to the sub-peak microstrain parameters obtained by deconvolution fitting from the spectrum depth analysis module (sub-peak 2 corresponds to a microstrain of 1.72 in Table 1), reflecting the spatial mapping relationship of "diffraction angle - physical location - structural instability index," providing a visualized structural state basis for subsequent anomaly region location and intervention strategy formulation.

[0085] In one embodiment of the present invention, the system further includes a strategy optimization module and a closed-loop execution verification module. The strategy optimization module simultaneously receives the coordinates of the abnormal region output by the abnormal focusing module and the lattice distortion depth report generated by the spectral depth analysis module. It cross-verifies the physical location of the abnormal region and the type of lattice distortion, adjusts the weights of the intervention parameters according to the distortion type, and outputs the optimized structural intervention command. The closed-loop execution verification module receives the customized structural intervention command generated by the intervention strategy formulation module, sends the command to the production line control system, and triggers a new round of diffraction signal acquisition after the command is executed. The intervention effect is verified by comparing the differences in diffraction behavior records before and after the intervention, and the verification results are fed back to the historical intervention record database of the intervention strategy formulation module.

[0086] In practice, the strategy optimization module simultaneously receives the anomaly region coordinate data packet output by the anomaly focusing module and the lattice distortion depth report generated by the map depth analysis module. The strategy optimization module cross-validates the physical location of the anomaly region and the lattice distortion type. The physical location information is derived from the physical location mapping information in the anomaly region coordinate data packet. The lattice distortion type is determined by analyzing the microscopic strain value distribution pattern and sub-peak characteristics in the lattice distortion depth report, such as uniform strain, gradient strain, or local distortion. Based on the identified lattice distortion type, the weights of the pre-screened intervention parameters for the current anomaly region are adjusted. This adjustment process is based on a preset mapping relationship, which defines the adjustment coefficients for the sensitivity of different distortion types to various intervention parameters.

[0087] In some embodiments, the adjustment of the intervention parameter weights is calculated using a weighted adjustment formula, expressed as follows:

[0088]

[0089] in: This represents the corrected intervention parameter weights. The representative strategy optimization module receives the initial intervention parameter weights selected by the intervention strategy formulation module before the original intervention parameter weights are received. It is a global adjustment factor. It is a type influence factor corresponding to a specific lattice distortion type. The strategy optimization module integrates the corrected intervention parameter weights with the original intervention parameter combination, and outputs an optimized structural intervention instruction. The optimized structural intervention instruction clarifies the priority and intensity adjustment suggestions for each process parameter after considering the specific distortion type.

[0090] It is understood that the closed-loop execution verification module receives customized structural intervention instructions generated by the intervention strategy formulation module or strategy optimization module, and sends the combination of intervention parameters and execution sequence contained in the structural intervention instructions to the process control system of the copper foil production line, such as the annealing furnace temperature control unit or the rolling mill tension adjustment unit. After the structural intervention instructions are executed, the closed-loop execution verification module triggers a new round of diffraction signal acquisition, and obtains the diffraction pattern of the copper foil sample after intervention through an online X-ray diffraction detector. In specific implementation, the intervention effect is verified by comparing the differences in diffraction behavior files before and after intervention. The difference comparison includes recalculating the real-time intensity drift, half-width change trajectory descriptor, and structural instability index of the abnormal region after intervention, and comparing and analyzing them with the values ​​before intervention. The closed-loop execution verification module feeds back the verification results to the historical intervention record database of the intervention strategy formulation module. The verification results are stored as a new prior intervention case. The case record includes the coordinates of the abnormal region, the optimized structural intervention instructions executed, and the quantitative data of the crystal structure state changes before and after intervention.

[0091] See Figure 5The graph illustrates the variations in diffraction intensity (main vertical axis, counts) and full width at half maximum (FWHM, °) with diffraction angle (horizontal axis, °) during the anomaly identification and verification stages. Specifically, the blue and green solid lines represent the diffraction intensity during the anomaly identification and verification stages, respectively, while the red and orange dashed lines correspond to the FWHM of the two stages. The pink shaded area marks the anomaly diffraction range of 35-55°. Within this range, the diffraction intensity (blue) during the anomaly identification stage exhibits significant fluctuations and is generally higher than that during the verification stage (green). Simultaneously, its FWHM (red) shows dramatic fluctuations, indicating instability in the crystal structure within this angle range. The diffraction intensity and FWHM fluctuations during the verification stage are relatively gentle, reflecting the improvement in the crystal structure state after intervention. By comparing the differences in diffraction intensity and the trajectory of the full width at half maximum (FWHM) change between the two stages, the structural instability index of the abnormal region can be quantified: In the anomaly identification stage, the intensity drift and the degree of change in FWHM in the 35-55° range are significantly higher than in the verification stage, corresponding to the local distortion characteristics of the crystal structure; while the spectral characteristics in the verification stage are closer to the standardized template in the diffraction behavior archive, reflecting the regulatory effect of the intervention strategy on the crystal structure.

[0092] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0093] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. An online analysis system for the crystal structure of copper foil based on XRD, characterized in that, The system includes: The diffraction profile construction module acquires raw diffraction signals from an online XRD detector, performs waveform purification, performs baseline calibration, and establishes a diffraction behavior profile for copper foil samples through pattern standardization. The dynamic spectrum monitoring module compares the current diffraction pattern with the historical patterns in the archive in real time based on the diffraction behavior archive, identifies the intensity drift at a specific angle in the pattern, tracks the change trajectory of the full width at half maximum (FWHM), determines the real-time state of the crystal structure, and generates a structure state vector. The anomaly focusing module analyzes the structural state vector, locates the diffraction angle interval where intensity drift and half-width change occur simultaneously, calculates the structural instability index of the diffraction angle interval, maps it to the physical spatial location of the copper foil, and outputs the coordinates of the anomaly region. The intervention strategy formulation module retrieves historical intervention records corresponding to the coordinates of the abnormal area based on the coordinates of the abnormal area, evaluates the prior effects of different intervention parameters, and generates customized structural intervention instructions for the current abnormal area. The anomaly focusing module specifically performs the following steps: The real-time intensity drift and half-width variation trajectory descriptor contained in the structural state vector are analyzed. In the diffraction angle space, locate those continuous intervals that simultaneously exhibit significant intensity shifts and changes in full width at half maximum (FWHM). Based on the severity and spatial continuity of the drift and change trajectory, the structural instability index of the continuous interval is calculated; Based on the spatial geometric relationship between the XRD detector and the copper foil sample, the diffraction angle range is mapped to the physical position coordinates of the copper foil surface; The coordinates of the abnormal region are formed by combining the structural instability index with the physical location coordinates; The formula for calculating the structural instability index is expressed as follows: ； in, Represents a structural instability index. This represents the severity of the drift in the normalized average intensity. This represents the severity of the change in the half-width at half-maximum after normalization. and These are preset combination factors corresponding to two different levels of severity. It is a spatial continuity multiplier that is positively correlated with the angular range of a continuous interval; The intervention strategy formulation module specifically performs the following steps: Receive the coordinates of the abnormal area and extract the physical location mapping information therein; In the historical intervention record database, retrieve all prior intervention cases associated with the physical location mapping information; Analyze the combination of intervention parameters used in each prior intervention case and their actual adjustment effect on the crystal structure; Based on the structural instability index of the current anomalous region, the most suitable intervention parameters are screened and evaluated from prior cases; By integrating the selected intervention parameters and the process timing requirements of the copper foil production line, the customized structural intervention instructions are generated.

2. The online analysis system for copper foil crystal structure based on XRD according to claim 1, characterized in that, The diffraction behavior profile includes at least the purified diffraction waveform data, the calibrated baseline reference, the standardized spectral template, and the historical diffraction feature set; the structural state vector includes the real-time intensity drift, the half-width at half-maximum change trajectory descriptor, and the crystal state determination label; the abnormal region coordinates include the diffraction angle range, physical location mapping information, and the structural instability index; and the customized structural intervention instructions include the intervention parameter combination, execution sequence, and expected adjustment target.

3. The online analysis system for copper foil crystal structure based on XRD according to claim 1, characterized in that, The diffraction profile construction module specifically performs the following steps: Receive the raw diffraction signal stream from the online XRD detector; The original diffraction signal stream is subjected to waveform purification processing to remove noise and equipment artifacts; Baseline calibration is performed on the purified waveform to eliminate the long-term drift effect of background scattering; The calibrated diffraction pattern was compared with the standard sample pattern, and the pattern was standardized to unify the intensity and angle scales. The purified waveform, calibration baseline, and standardized spectra are integrated to construct and update the diffraction behavior profile.

4. The online analysis system for copper foil crystal structure based on XRD according to claim 1, characterized in that, The dynamic spectrum monitoring module specifically performs the following steps: Retrieve historical map templates and historical diffraction feature sets from the diffraction behavior archive; The current real-time diffraction pattern is compared point by point with the historical pattern template to calculate the intensity difference in the angular dimension. Identify specific diffraction angles where the intensity difference continuously exceeds a threshold and mark them as intensity drift regions; Simultaneously analyze the diffraction peak shape in the intensity drift region and trace the change trajectory of its full width at half maximum (FWHM) over time; By combining the intensity drift and the half-width at half-maximum variation trajectory, the real-time state of the crystal structure is determined, and the structure state vector is encapsulated and generated.

5. The online analysis system for copper foil crystal structure based on XRD according to claim 1, characterized in that, The system also includes a spectrum depth analysis module, which receives the structure state vector generated by the dynamic spectrum monitoring module, performs deconvolution fitting on the marked abnormal diffraction peaks therein, separates overlapping peak components, extracts the precise angular position, integral intensity and micro-strain parameters of each sub-peak, and generates a lattice distortion depth report.

6. The online analysis system for copper foil crystal structure based on XRD according to claim 5, characterized in that, The map depth analysis module specifically performs the following steps: Extract diffraction peak data containing anomalous changes from the structural state vector; An iterative approximation method is used to fit the peak shape function of the diffraction peak segments to achieve the separation of overlapping peaks; Extract precise Bragg angle, integral intensity, and peak width parameters from the separated sub-peaks; Based on the peak shape and width parameter of the sub-peak, the micro-strain value characterizing the degree of micro-lattice distortion is calculated; The parameters and microstrain values ​​of all sub-peaks are summarized to generate the lattice distortion depth report.

7. The online analysis system for copper foil crystal structure based on XRD according to claim 5, characterized in that, The system also includes a strategy optimization module, which simultaneously receives the coordinates of the abnormal region output by the anomaly focusing module and the lattice distortion depth report generated by the map depth analysis module, cross-validates the physical location of the abnormal region and the lattice distortion type, adjusts the weights of the intervention parameters according to the distortion type, and outputs the optimized structural intervention command.

8. The online analysis system for copper foil crystal structure based on XRD according to claim 1, characterized in that, The system also includes a closed-loop execution verification module. The closed-loop execution verification module receives customized structural intervention instructions generated by the intervention strategy formulation module, sends the instructions to the production line control system, and triggers a new round of diffraction signal acquisition after the instructions are executed. By comparing the differences in diffraction behavior files before and after the intervention, the intervention effect is verified, and the verification results are fed back to the historical intervention record database of the intervention strategy formulation module.

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