Dislocation density detection method and system of single crystal diamond, terminal and storage medium
By employing a multi-dimensional collaborative detection method, including grinding and polishing, cleaning, XRD rocking curve method, Raman mapping method, and etching method, a quantitative correlation model was established, which solved the problems of low efficiency and low accuracy in single-crystal diamond dislocation density detection, and achieved rapid and high-precision detection results.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-26
- Publication Date
- 2026-03-20
AI Technical Summary
Existing technologies for detecting dislocation density in single-crystal diamond have low efficiency and low accuracy, failing to meet user needs.
A multi-dimensional collaborative detection method was adopted, including grinding and polishing, cleaning, XRD rocking curve method, Raman mapping method and etching method, to establish a quantitative correlation model of surface morphology-lattice defects-XRD peak broadening. By controlling the surface roughness and flatness of the sample, combined with XRD partitioning test and Raman stress analysis, the dislocation density measurement model was optimized.
It achieves rapid (test results take ≤ 5 days) and high-precision dislocation density detection, breaking through the limitations of single detection technology, balancing efficiency and accuracy, and meeting the needs of single-crystal diamond in multiple scenarios of research and development, production and application.
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Figure CN121703072A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of data processing, and particularly relates to a dislocation density detection method and system for single crystal diamond, a terminal and a computer readable storage medium. BACKGROUND
[0002] Single crystal diamond has irreplaceable application prospects in high-frequency power devices, quantum information and precision optical elements due to its excellent characteristics such as wide band gap, high carrier mobility, extremely high thermal conductivity and hardness. As one of the core indicators for measuring the quality of single crystal diamond crystal, dislocation density, which is a physical quantity describing the number of dislocations in the crystal structure of a material, directly affects the consistency and reliability of the electrical, thermal and mechanical properties of the material. Therefore, developing an efficient and accurate dislocation density detection technology is a key technical bottleneck for promoting the industrial application of single crystal diamond.
[0003] However, the current single crystal diamond dislocation density measurement method has the problems of low detection efficiency and low accuracy of detection results, which cannot meet the user's demand for single crystal diamond dislocation density detection.
[0004] Therefore, the prior art still needs to be improved and developed. SUMMARY
[0005] The main purpose of the present application is to provide a single crystal diamond dislocation density detection method, system, terminal and computer readable storage medium, which aims to solve the problems of low detection efficiency and low accuracy of detection results of single crystal diamond dislocation density in the prior art.
[0006] To achieve the above-mentioned purpose, the present application provides a single crystal diamond dislocation density detection method, which comprises the following steps: Obtain a single crystal diamond sample, and perform grinding and polishing treatment on the single crystal diamond sample to obtain an initial single crystal diamond sample; Perform cleaning treatment on the initial single crystal diamond sample to obtain a target single crystal diamond sample; Perform dislocation density detection treatment on the target single crystal diamond sample to obtain an initial dislocation density detection result, and construct a target dislocation density measurement model according to the initial dislocation density detection result; Obtain surface parameter data of a current single crystal diamond to be detected, and input the surface parameter data into the target dislocation density measurement model to output a target dislocation density detection result.
[0007] Optionally, the dislocation density detection method of the single crystal diamond, wherein the single crystal diamond sample is obtained, and the single crystal diamond sample is subjected to grinding and polishing treatment to obtain an initial single crystal diamond sample, specifically comprising: obtaining a single crystal diamond sample and obtaining roughness and flatness of the single crystal diamond sample; the single crystal diamond sample is subjected to grinding and polishing treatment by using a mechanical polishing technique, and when the roughness of the single crystal diamond sample reaches a preset roughness and the flatness reaches a preset flatness, it indicates that the grinding and polishing treatment is completed, and an initial single crystal diamond sample is obtained.
[0008] Optionally, the dislocation density detection method of the single crystal diamond, wherein the cleaning treatment comprises acid pickling treatment and ultrasonic cleaning treatment; the initial single crystal diamond sample is subjected to cleaning treatment to obtain a target single crystal diamond sample, specifically comprising: a preset mixed strong acid solution is determined, and the initial single crystal diamond sample is subjected to heating cleaning treatment by using the preset mixed strong acid solution to obtain a first single crystal diamond sample; wherein the preset mixed strong acid solution is a mixed solution of sulfuric acid and nitric acid; after the acid pickling treatment is completed, a preset ultrasonic cleaning solution is determined, and the first single crystal diamond sample is subjected to ultrasonic cleaning treatment by using the preset ultrasonic cleaning solution to obtain a second single crystal diamond sample; wherein the preset ultrasonic cleaning solution comprises acetone and ethanol; the second single crystal diamond sample is subjected to rinsing treatment by using deionized water, and the second single crystal diamond sample is subjected to blow-drying by using nitrogen to obtain a target single crystal diamond sample.
[0009] Optionally, the dislocation density detection method of the single crystal diamond, wherein the initial dislocation density detection result comprises a first measurement result, a second measurement result and a third measurement result; the target single crystal diamond sample is subjected to dislocation density detection treatment to obtain an initial dislocation density detection result, and a target dislocation density measurement model is constructed according to the initial dislocation density detection result, specifically comprising: the target single crystal diamond sample is subjected to first dislocation density detection treatment by using an XRD rocking curve method to obtain a first measurement result; the target single crystal diamond sample is subjected to second dislocation density detection treatment by using a Raman mapping method to obtain a second measurement result; sample surface parameter data of the target single crystal diamond sample is obtained, and an initial dislocation density measurement model is constructed according to the sample surface parameter data, the first measurement result and the second measurement result; The target single-crystal diamond sample is subjected to a third dislocation density detection process using an etching method to obtain a third measurement result. Based on the third measurement result, the initial dislocation density measurement model is optimized to obtain the target dislocation density measurement model.
[0010] Optionally, the method for detecting dislocation density in single-crystal diamond, wherein the first dislocation density detection processing of the target single-crystal diamond sample using the XRD rocking curve method to obtain a first measurement result specifically includes: The target single-crystal diamond sample is divided into regions to obtain multiple sample sub-regions of equal area; XRD rocking curve tests were performed on each of the sample sub-regions to obtain multiple XRD rocking curves, and a first measurement result was obtained based on the multiple XRD rocking curves.
[0011] Optionally, the method for detecting dislocation density in single-crystal diamond, wherein the third dislocation density detection processing of the target single-crystal diamond sample using an etching method to obtain a third measurement result specifically includes: The target single-crystal diamond sample is placed in an MPCVD device, and hydrogen and oxygen of a preset concentration are introduced into the MPCVD device. The target single-crystal diamond sample is subjected to hydrogen-oxygen etching treatment using hydrogen and oxygen at a preset concentration in the MPCVD equipment to obtain the etching result. The number of dislocation etching pits within a preset area in the target single-crystal diamond sample is calculated based on the etching results, and a third measurement result is obtained based on the number of dislocation etching pits. The third measurement result is the ratio of the number of dislocation etch pits to the preset area.
[0012] Optionally, the method for detecting dislocation density in single-crystal diamond, wherein acquiring surface parameter data of the single-crystal diamond to be detected, inputting the surface parameter data into the target dislocation density measurement model, and outputting the target dislocation density detection result specifically includes: Acquire the surface parameter data of the single crystal diamond to be tested, wherein the surface parameter data includes surface morphology data and lattice defect data; The surface morphology data and the lattice defect data are input into the target dislocation density measurement model. The target dislocation density measurement model is used to perform dislocation density detection processing on the surface morphology data and the lattice defect data to obtain the target dislocation density detection result.
[0013] Furthermore, to achieve the above objectives, the present invention also provides a dislocation density detection system for single-crystal diamond, wherein the dislocation density detection system for single-crystal diamond comprises: The sample polishing module is used to acquire single-crystal diamond samples and perform polishing treatment on the single-crystal diamond samples to obtain initial single-crystal diamond samples. The sample cleaning module is used to clean the initial single-crystal diamond sample to obtain the target single-crystal diamond sample. The model building module is used to perform dislocation density detection processing on the target single-crystal diamond sample, obtain the initial dislocation density detection result, and build the target dislocation density measurement model based on the initial dislocation density detection result. The dislocation density output module is used to acquire the surface parameter data of the single crystal diamond to be tested, input the surface parameter data into the target dislocation density measurement model, and output the target dislocation density detection result.
[0014] Furthermore, to achieve the above objectives, the present invention also provides a terminal, wherein the terminal includes: a memory, a processor, and a single-crystal diamond dislocation density detection program stored in the memory and executable on the processor, wherein when the single-crystal diamond dislocation density detection program is executed by the processor, it implements the steps of the single-crystal diamond dislocation density detection method as described above.
[0015] Furthermore, to achieve the above objectives, the present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a dislocation density detection program for single-crystal diamond, and when the dislocation density detection program for single-crystal diamond is executed by a processor, it implements the steps of the dislocation density detection method for single-crystal diamond as described above.
[0016] In this invention, a single-crystal diamond sample is obtained and polished to obtain an initial single-crystal diamond sample; the initial single-crystal diamond sample is then cleaned to obtain a target single-crystal diamond sample; dislocation density detection is performed on the target single-crystal diamond sample to obtain an initial dislocation density detection result, and a target dislocation density measurement model is constructed based on the initial dislocation density detection result; surface parameter data of the single-crystal diamond to be tested is acquired and input into the target dislocation density measurement model, and the target dislocation density detection result is output. This invention, by controlling the surface parameters of the single-crystal diamond and establishing a dislocation density measurement model based on the initial dislocation density detection result, can effectively improve the detection efficiency and accuracy of single-crystal diamond dislocation density detection. Attached Figure Description
[0017] Figure 1This is a flowchart of a preferred embodiment of the method for detecting dislocation density in single-crystal diamond according to the present invention; Figure 2 This is a structural diagram of a preferred embodiment of the dislocation density detection system for single-crystal diamond of the present invention; Figure 3 This is a structural diagram of a preferred embodiment of the terminal of the present invention. Detailed Implementation
[0018] To make the objectives, technical solutions, and advantages of this invention clearer and more explicit, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
[0019] Single-crystal diamond possesses excellent properties such as a wide bandgap, high carrier mobility, extremely high thermal conductivity, and high hardness, making it irreplaceable in applications such as high-frequency power devices, quantum information, and precision optical components. Dislocation density (a physical quantity describing the number of dislocations in a material's crystal structure; dislocations are defects in the crystal structure and significantly affect material properties; higher dislocation density generally leads to better strength and toughness, but can also affect plasticity) is one of the core indicators for evaluating the quality of single-crystal diamond crystals, directly impacting the consistency and reliability of its electrical, thermal, and mechanical properties. Therefore, developing efficient and accurate dislocation density characterization techniques is a key technological bottleneck in promoting the industrial application of single-crystal diamond.
[0020] However, current methods for measuring dislocation density in single-crystal diamond suffer from low detection efficiency and low accuracy, failing to meet users' needs for single-crystal diamond dislocation density detection.
[0021] To address the aforementioned issues, this invention proposes a multi-dimensional collaborative method for detecting diamond dislocation density. This method controls sample surface roughness and smoothness, and employs a combination of XRD zonal testing and Raman stress analysis to determine defect distribution, thereby establishing a quantitative correlation model of "surface morphology-lattice defects-XRD peak broadening." Furthermore, the experimental results are corrected using dislocation density etching. Ultimately, this achieves rapid (detection time ≤ 5 days) and high-precision diamond dislocation density detection. This invention overcomes the limitations of single detection technologies, balancing efficiency and accuracy. It enables rapid screening, precise counting, and microscopic analysis across multiple scenarios, solving the problem that single detection methods cannot cover all needs, and meeting the diverse requirements of single-crystal diamond in research, development, production, and application.
[0022] The method for detecting dislocation density in single-crystal diamond according to a preferred embodiment of the present invention, such as... Figure 1As shown, the dislocation density detection method for single-crystal diamond includes the following steps: Step S10: Obtain a single-crystal diamond sample and perform grinding and polishing treatment on the single-crystal diamond sample to obtain an initial single-crystal diamond sample.
[0023] Before conducting formal dislocation density testing on single-crystal diamond, the single-crystal diamond sample needs to be ground and polished to reduce interference from surface morphology and processing defects, so that the roughness and flatness of the single-crystal diamond sample meet the preset requirements.
[0024] Specifically, a single-crystal diamond sample is obtained, and the roughness and flatness of the single-crystal diamond sample are obtained; the single-crystal diamond sample is polished using mechanical polishing technology. When the roughness of the single-crystal diamond sample reaches a preset roughness and the flatness reaches a preset flatness, the polishing process is completed, and an initial single-crystal diamond sample is obtained.
[0025] The processing procedure for single-crystal diamond samples is as follows: After the single-crystal diamond sample is cut and leveled by laser, it is polished by mechanical polishing until Ra (Arithmetic Average Roughness, i.e., roughness in this invention) < 10nm (i.e., the preset roughness in this invention) and macroscopic flatness (i.e., flatness in this invention) < 0.06mm (i.e., the preset flatness in this invention).
[0026] Understandably, to reduce the interference of surface morphology and processing defects on XRD testing, the following pretreatment steps need to be performed on single-crystal diamond samples before XRD testing: 1. Surface polycrystalline treatment: First, laser cutting is used to remove the polycrystalline material on the surface and edge of the single-crystal diamond sample. The cutting is considered complete only when there is no obvious polycrystalline material under the microscope. This is to reduce the interference of the broadening of the diffraction peaks of the amorphous phase on the dislocation signal. 2. Cutting surface control: A single-blade cutting process is adopted (using laser cutting, the cutting process is completed in one go, and it is necessary to cut without multiple obvious planes) to avoid the introduction of multiple planes by multi-blade cutting, which would lead to substandard flatness. It is necessary to ensure that the surface roughness Ra≤10nm. 3. Polishing process: It is necessary to ensure that the surface of the single crystal diamond sample is smooth with only a single crystal facet after polishing and without multiple facets.
[0027] Step S20: Clean the initial single-crystal diamond sample to obtain the target single-crystal diamond sample. The cleaning process includes acid washing and ultrasonic cleaning.
[0028] For the pretreatment of single-crystal diamond samples, in addition to the grinding and polishing process, it is also necessary to clean the initial single-crystal diamond samples obtained after grinding and polishing. The cleaning process includes acid washing and ultrasonic cleaning. The purpose is to remove impurities on the initial single-crystal diamond samples to ensure the accuracy of subsequent dislocation density detection.
[0029] Specifically, a preset mixed strong acid solution is determined, and the initial single-crystal diamond sample is subjected to heating and cleaning treatment using the preset mixed strong acid solution to obtain a first single-crystal diamond sample; wherein, the preset mixed strong acid solution is a mixed solution of sulfuric acid and nitric acid; after the acid washing treatment is completed, a preset ultrasonic cleaning solution is determined, and the first single-crystal diamond sample is subjected to ultrasonic cleaning treatment using the preset ultrasonic cleaning solution to obtain a second single-crystal diamond sample; wherein, the preset ultrasonic cleaning solution includes acetone and ethanol; the second single-crystal diamond sample is rinsed with deionized water, and the second single-crystal diamond sample is dried with nitrogen gas to obtain a target single-crystal diamond sample.
[0030] After the grinding and polishing of the single-crystal diamond sample is completed to obtain the initial single-crystal diamond sample, further sample cleaning is required. The specific process is as follows: After obtaining the first single-crystal diamond sample by chemical acid washing, such as heating and cleaning with strong acid solutions such as sulfuric acid, nitric acid or the above-mentioned mixed acids, the sample is then ultrasonically cleaned with acetone and ethanol for 10 minutes in sequence, followed by rinsing with deionized water and drying with nitrogen gas. This process removes contaminants from the surface of the first single-crystal diamond sample, resulting in a clean sample (i.e., the second single-crystal diamond sample in this invention) to avoid interference with the test.
[0031] Step S30: Perform dislocation density detection processing on the target single-crystal diamond sample to obtain the initial dislocation density detection result, and construct the target dislocation density measurement model based on the initial dislocation density detection result.
[0032] This invention employs three methods for dislocation density detection: XRD rocking curve method, Raman mapping method, and etching method. Specifically, this invention constructs an initial dislocation density measurement model based on the first measurement result obtained by the XRD rocking curve method and the second measurement result obtained by the Raman mapping method. The initial dislocation density measurement model is then optimized based on the third measurement result obtained by the etching method to establish a quantitative correlation model of surface morphology-lattice defects-XRD peak broadening (i.e., the target dislocation density measurement model in this invention), which enables accurate measurement of dislocation density in single-crystal diamond.
[0033] Specifically, the target single-crystal diamond sample is divided into multiple sample sub-regions of equal area; XRD rocking curve tests are performed on each sample sub-region to obtain multiple XRD rocking curves, and a first measurement result is obtained based on the multiple XRD rocking curves.
[0034] XRD stands for X-ray Diffraction.
[0035] After grinding, polishing, and cleaning the single-crystal diamond sample to obtain the target single-crystal diamond sample, formal testing can be carried out based on the target single-crystal diamond sample. The testing process is as follows: 1. Surface morphology test: The surface roughness of the target single crystal diamond sample is tested again using a white light interferometer to see if it is within the range of 100*100μm and whether Ra is <10nm.
[0036] 2. XRD Partition Testing: XRD partition testing (meaning testing different locations within a single target single-crystal diamond sample) is performed on seed crystals (i.e., the target single-crystal diamond sample) with different surface conditions to obtain multiple sample sub-regions of equal area. The FWHM value (Full Width at Half Maximum) is obtained by acquiring the XRD rocking curves of each sample sub-region. By performing XRD rocking curve tests on different samples before and after polishing, and before and after edge trimming, the interference of surface morphology on XRD can be eliminated. After the XRD rocking curve test is completed, a curve is obtained, and the half-width at half-maximum (FWHM) value of the curve is obtained.
[0037] Understandably, XRD (X-ray diffraction) is a powerful analytical technique primarily used to study the crystal structure of substances. It determines the structure and properties of a crystal by measuring the diffraction of X-rays within it. XRD testing can provide detailed information about the crystal structure, including interplanar spacing, lattice parameters, and crystallinity. In XRD testing, "zonal testing" typically refers to targeted testing of different regions of the sample (usually by cutting the crystal into three equal-area pieces) to obtain more detailed information about the crystal structure.
[0038] This invention, by testing the full width at half maximum (FWHM) of the crystal facets, can quickly obtain information on the overall lattice distortion of a sample and correlate it with the total number of dislocations. Simultaneously, it can effectively improve the efficiency of subsequent dislocation density detection, adapting to the high-throughput detection requirements of single-crystal diamond. Furthermore, the XRD rocking curve method is also applicable to scenarios requiring batch quality screening before seed crystal warehousing, rapid sampling inspection of mass production batches, and quantitative correlation analysis between macroscopic quality and total dislocations.
[0039] The target single-crystal diamond sample was subjected to a second dislocation density detection process using Raman mapping to obtain a second measurement result.
[0040] The technical principle of Raman mapping is to perform spatially resolved scanning through Raman spectroscopy and to invert dislocation density by utilizing the broadening or displacement of Raman peaks caused by dislocations.
[0041] The testing process for Raman spectroscopy mapping is as follows: Raman mapping scanning is performed on samples of different density grades (seed crystals grown using process formulas or seed crystals cultivated using HPHT (High Pressure High Temperature) method) (i.e., the target single crystal diamond sample in this invention). The test range is 500*500μm, which is used to output the Raman peak position, full width at half maximum (FWHM), and stress distribution map (i.e., the second measurement result in this invention).
[0042] Furthermore, this invention maps parameters such as Raman peak shift and full width at half maximum (FWHM) broadening to the defect distribution of single-crystal diamond through spatial resolution scanning (step size ≤ 0.5 μm), achieving a resolution of sub-micron level and revealing the spatial aggregation characteristics of microscopic defects.
[0043] In addition, the Raman mapping technology in this invention can also be applied to scenarios such as dislocation analysis at the interface of spliced samples, identification of local defects in samples with low dislocation density, and characterization of microscopic defects in complex structures.
[0044] This invention utilizes X-ray diffraction, laser Raman spectroscopy, and other detection technologies to rapidly and non-destructively determine the crystal quality of diamond as a whole and in localized areas.
[0045] Obtain the sample surface parameter data of the target single-crystal diamond sample, and construct an initial dislocation density measurement model based on the sample surface parameter data, the first measurement result, and the second measurement result.
[0046] After obtaining the XRD rocking curve FWHM result (i.e., the first measurement result in this invention) and the Raman mapping dislocation distribution result (i.e., the second measurement result in this invention), conditions that interfere with the test results, such as polycrystalline edges, surface polycrystalline, and uneven test surfaces, can be eliminated based on the test results. A quantitative correlation model of surface morphology-lattice defects-XRD peak broadening (i.e., the initial dislocation density measurement model in this invention) can be established based on the XRD rocking curve FWHM result (i.e., the first measurement result in this invention) and the Raman mapping dislocation distribution result (i.e., the second measurement result in this invention).
[0047] The target single-crystal diamond sample is placed in an MPCVD device, and a preset concentration of hydrogen and oxygen is introduced into the MPCVD device. The target single-crystal diamond sample is subjected to hydrogen-oxygen etching treatment using the preset concentration of hydrogen and oxygen in the MPCVD device to obtain etching results. The number of dislocation etch pits in a preset area of the target single-crystal diamond sample is calculated based on the etching results, and a third measurement result is calculated based on the number of dislocation etch pits. The third measurement result is the ratio of the number of dislocation etch pits to the preset area.
[0048] The following is an introduction to MPCVD (Microwave Plasma Chemical Vapor Deposition): Diamond possesses extremely excellent physicochemical properties, but the reserves of natural diamond are limited. Therefore, various methods for synthesizing diamond have been developed, such as the high-pressure high-temperature (HPHT) method and hot-filament chemical vapor deposition (HFCVD). Among these, microwave plasma chemical vapor deposition (MPCVD) is considered the optimal method for preparing high-quality single-crystal diamonds because it avoids the introduction of impurities and can synthesize high-quality, large-area diamonds. It also boasts advantages such as no electrode discharge contamination, fast deposition rate, and good stability.
[0049] Furthermore, for the tested samples (i.e., the target single-crystal diamond samples that have undergone XRD rocking curve testing and Raman mapping testing), the dislocation density is tested using an etching method (i.e., the target single-crystal diamond samples are subjected to hydrogen-oxygen etching by MPCVD to preferentially expose the dislocations in the target single-crystal diamond samples). Then, the dislocation etch pit calculation method is used for statistical analysis. Generally, the number of dislocation etch pits in a specified area of the target single-crystal diamond sample is calculated, and the dislocation density is calculated based on the number of dislocation etch pits (dislocation density equals the number of dislocation etch pits divided by the specified area).
[0050] This invention exposes dislocation pits through chemical etching, allowing direct observation of dislocation morphology and density under an optical microscope. It provides intuitive evidence of "where the dislocations are" and "how many dislocations there are," thereby enabling intuitive morphology and accurate counting of dislocations on the surface of a target single-crystal diamond sample.
[0051] In addition, the etching method in this invention can also be applied independently to scenarios requiring the observation of surface dislocation distribution, failure analysis, and accurate determination of dislocation density in arbitration testing.
[0052] Based on the third measurement result, the initial dislocation density measurement model is optimized to obtain the target dislocation density measurement model.
[0053] After obtaining the third measurement result through etching, the third measurement result can be compared with the first and third measurement results to adjust the model parameters in the initial dislocation density measurement model, thereby obtaining the target dislocation density measurement model.
[0054] Step S40: Obtain the surface parameter data of the single crystal diamond to be tested, input the surface parameter data into the target dislocation density measurement model, and output the target dislocation density detection result.
[0055] Once the target dislocation density measurement model is established, the dislocation density of the single-crystal diamond to be tested can be measured using the target dislocation density measurement model. The target dislocation density measurement model can analyze the surface parameter data of the single-crystal diamond to be tested and output the target dislocation density detection results quickly and accurately.
[0056] Specifically, the surface parameter data of the single crystal diamond to be tested is obtained, wherein the surface parameter data includes surface morphology data and lattice defect data; the surface morphology data and the lattice defect data are input into the target dislocation density measurement model, and the target dislocation density measurement model is used to perform dislocation density detection processing on the surface morphology data and the lattice defect data to obtain the target dislocation density detection result.
[0057] Once the target dislocation density measurement model is constructed, the dislocation density of the single crystal diamond to be tested can be detected. Before inputting the target dislocation density measurement model, it is necessary to obtain the surface morphology data and lattice defect data of the single crystal diamond to be tested. Then, the surface morphology data and lattice defect data are input into the target dislocation density measurement model, and the target dislocation density measurement model outputs the target dislocation density detection result of the single crystal diamond to be tested.
[0058] In summary, this invention focuses on a multi-dimensional defect characterization technology system for single-crystal diamond. By integrating XRD full width at half maximum (FWHM), Raman stress, and surface morphology synergistic analysis techniques, it overcomes the challenge of suppressing XRD peak broadening interference under gradient grinding processes and establishes an evaluation method for the correlation between defect spatial distribution and crystal growth uniformity. Furthermore, this invention innovatively integrates cross-scale data fusion technology to achieve quantitative separation of surface morphology and XRD broadening effects, and dynamic analysis of Raman mapping spatial distribution and stress field, forming a complete technical solution covering "defect characterization - performance testing - data verification".
[0059] Technical effects of the present invention: 1. Demand-driven hierarchical representation strategy: Clearly define three types of requirements: "rapid assessment - surface counting - microscopic analysis", construct a target dislocation density measurement model, and solve the problem that a single method cannot cover the whole scenario; 2. Standardization of XRD test preprocessing: By standardizing the three steps of "polycrystal removal, single-blade cutting, and single-sided polishing", the surface interference of single-crystal diamond samples is reduced, and the reliability of XRD test results is improved. 3. Multi-method collaborative verification logic: The initial dislocation density measurement model constructed based on "XRD quantification and Raman mapping microscopic analysis" is optimized by etching method to obtain the target dislocation density measurement model, thereby improving the credibility of the target dislocation density detection results output.
[0060] Furthermore, such as Figure 2 As shown, based on the above-described method for detecting dislocation density in single-crystal diamond, this invention also provides a system for detecting dislocation density in single-crystal diamond, wherein the system comprises: The sample polishing module 51 is used to acquire a single-crystal diamond sample and perform polishing treatment on the single-crystal diamond sample to obtain an initial single-crystal diamond sample. The sample cleaning module 52 is used to clean the initial single-crystal diamond sample to obtain the target single-crystal diamond sample. The model building module 53 is used to perform dislocation density detection processing on the target single-crystal diamond sample, obtain the initial dislocation density detection result, and build the target dislocation density measurement model based on the initial dislocation density detection result. The dislocation density output module 54 is used to acquire the surface parameter data of the single crystal diamond to be tested, input the surface parameter data into the target dislocation density measurement model, and output the target dislocation density detection result.
[0061] Furthermore, such as Figure 3As shown, based on the above-mentioned method and system for detecting dislocation density in single-crystal diamond, the present invention also provides a terminal, which includes a processor 10, a memory 20 and a display 30. Figure 3 Only some of the terminal components are shown; however, it should be understood that it is not required to implement all of the components shown, and more or fewer components may be implemented instead.
[0062] In some embodiments, the memory 20 may be an internal storage unit of the terminal, such as a hard disk or memory. In other embodiments, the memory 20 may be an external storage device of the terminal, such as a plug-in hard disk, smart media card (SMC), secure digital card (SD), flash card, etc. Further, the memory 20 may include both internal and external storage devices. The memory 20 is used to store application software and various types of data installed on the terminal, such as the program code installed on the terminal. The memory 20 can also be used to temporarily store data that has been output or will be output. In one embodiment, the memory 20 stores a single-crystal diamond dislocation density detection program 40, which can be executed by the processor 10 to implement the single-crystal diamond dislocation density detection method of this application.
[0063] In some embodiments, the processor 10 may be a central processing unit (CPU), a microprocessor, or other data processing chip, used to run program code stored in the memory 20 or process data, such as executing the dislocation density detection method for single-crystal diamond.
[0064] In some embodiments, the display 30 may be an LED display, a liquid crystal display, a touch-sensitive liquid crystal display, or an OLED (Organic Light-Emitting Diode) touchscreen. The display 30 is used to display information on the terminal and to display a visual user interface.
[0065] In one embodiment, when the processor 10 executes the dislocation density detection program 40 for single-crystal diamond in the memory 20, the following steps are performed: A single-crystal diamond sample was obtained, and the single-crystal diamond sample was ground and polished to obtain an initial single-crystal diamond sample. The initial single-crystal diamond sample was cleaned to obtain the target single-crystal diamond sample; The target single-crystal diamond sample is subjected to dislocation density detection processing to obtain initial dislocation density detection results, and a target dislocation density measurement model is constructed based on the initial dislocation density detection results. The surface parameter data of the single crystal diamond to be tested is obtained, and the surface parameter data is input into the target dislocation density measurement model to output the target dislocation density detection result.
[0066] The step of obtaining a single-crystal diamond sample and polishing the single-crystal diamond sample to obtain an initial single-crystal diamond sample specifically includes: Obtain a single-crystal diamond sample, and obtain the roughness and flatness of the single-crystal diamond sample; The single-crystal diamond sample is polished using mechanical polishing technology. When the roughness and flatness of the single-crystal diamond sample reach a preset roughness and a preset flatness, the polishing process is complete, and an initial single-crystal diamond sample is obtained.
[0067] The cleaning process includes acid washing and ultrasonic cleaning; the cleaning process of the initial single-crystal diamond sample to obtain the target single-crystal diamond sample specifically includes: A preset mixed strong acid solution is determined, and the initial single crystal diamond sample is heated and cleaned using the preset mixed strong acid solution to obtain a first single crystal diamond sample. The preset mixed strong acid solution is a mixed solution of sulfuric acid and nitric acid; After the acid washing process is completed, a preset ultrasonic cleaning solution is determined, and the first single crystal diamond sample is ultrasonically cleaned using the preset ultrasonic cleaning solution to obtain a second single crystal diamond sample. The preset ultrasonic cleaning solution includes acetone and ethanol; The second single-crystal diamond sample was rinsed with deionized water and then dried with nitrogen gas to obtain the target single-crystal diamond sample.
[0068] The initial dislocation density detection results include a first measurement result, a second measurement result, and a third measurement result; The process of performing dislocation density detection on the target single-crystal diamond sample to obtain an initial dislocation density detection result, and constructing a target dislocation density measurement model based on the initial dislocation density detection result, specifically includes: The first dislocation density of the target single-crystal diamond sample was detected by XRD rocking curve method to obtain the first measurement result. The target single-crystal diamond sample was subjected to a second dislocation density detection process using Raman mapping to obtain a second measurement result. Obtain the sample surface parameter data of the target single-crystal diamond sample, and construct an initial dislocation density measurement model based on the sample surface parameter data, the first measurement result, and the second measurement result; The target single-crystal diamond sample is subjected to a third dislocation density detection process using an etching method to obtain a third measurement result. Based on the third measurement result, the initial dislocation density measurement model is optimized to obtain the target dislocation density measurement model.
[0069] Specifically, the first measurement result obtained by using the XRD rocking curve method to perform first dislocation density detection on the target single-crystal diamond sample includes: The target single-crystal diamond sample is divided into regions to obtain multiple sample sub-regions of equal area; XRD rocking curve tests were performed on each of the sample sub-regions to obtain multiple XRD rocking curves, and a first measurement result was obtained based on the multiple XRD rocking curves.
[0070] Specifically, the third dislocation density detection process performed on the target single-crystal diamond sample using an etching method to obtain a third measurement result includes: The target single-crystal diamond sample is placed in an MPCVD device, and hydrogen and oxygen of a preset concentration are introduced into the MPCVD device. The target single-crystal diamond sample is subjected to hydrogen-oxygen etching treatment using hydrogen and oxygen at a preset concentration in the MPCVD equipment to obtain the etching result. The number of dislocation etching pits within a preset area in the target single-crystal diamond sample is calculated based on the etching results, and a third measurement result is obtained based on the number of dislocation etching pits. The third measurement result is the ratio of the number of dislocation etch pits to the preset area.
[0071] Specifically, the step of acquiring the surface parameter data of the single-crystal diamond to be tested, inputting the surface parameter data into the target dislocation density measurement model, and outputting the target dislocation density detection result includes: Acquire the surface parameter data of the single crystal diamond to be tested, wherein the surface parameter data includes surface morphology data and lattice defect data; The surface morphology data and the lattice defect data are input into the target dislocation density measurement model. The target dislocation density measurement model is used to perform dislocation density detection processing on the surface morphology data and the lattice defect data to obtain the target dislocation density detection result.
[0072] The present invention also provides a computer-readable storage medium, wherein the computer-readable storage medium stores a dislocation density detection program for single-crystal diamond, and the dislocation density detection program for single-crystal diamond, when executed by a processor, implements the steps of the dislocation density detection method for single-crystal diamond as described above.
[0073] In summary, this invention provides a method, system, terminal, and storage medium for detecting dislocation density in single-crystal diamond. The method includes: acquiring a single-crystal diamond sample and polishing the sample to obtain an initial single-crystal diamond sample; cleaning the initial sample to obtain a target sample; performing dislocation density detection on the target sample to obtain an initial dislocation density detection result, and constructing a target dislocation density measurement model based on the initial result; acquiring surface parameter data of the single-crystal diamond to be tested, inputting the data into the model, and outputting the result. This invention, by controlling the surface parameters and establishing a dislocation density measurement model based on the initial dislocation density detection result, effectively improves the detection efficiency and accuracy of single-crystal diamond dislocation density detection.
[0074] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or terminal that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or terminal. Unless otherwise specified, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or terminal that includes that element.
[0075] Of course, those skilled in the art will understand that all or part of the processes in the above embodiments can be implemented by a computer program instructing related hardware (such as a processor, controller, etc.). The program can be stored in a computer-readable storage medium, and when executed, it can include the processes described in the above method embodiments. The computer-readable storage medium can be a memory, magnetic disk, optical disk, etc.
[0076] It should be understood that the application of the present invention is not limited to the examples above. Those skilled in the art can make improvements or modifications based on the above description, and all such improvements and modifications should fall within the protection scope of the appended claims.
Claims
1. A method for detecting dislocation density in single-crystal diamond, characterized in that, The method for detecting the dislocation density of single-crystal diamond includes: A single-crystal diamond sample was obtained, and the single-crystal diamond sample was ground and polished to obtain an initial single-crystal diamond sample. The initial single-crystal diamond sample was cleaned to obtain the target single-crystal diamond sample. The target single-crystal diamond sample is subjected to dislocation density detection processing to obtain initial dislocation density detection results, and a target dislocation density measurement model is constructed based on the initial dislocation density detection results. The surface parameter data of the single crystal diamond to be tested is obtained, and the surface parameter data is input into the target dislocation density measurement model to output the target dislocation density detection result.
2. The method for detecting dislocation density in single-crystal diamond according to claim 1, characterized in that, The process of obtaining a single-crystal diamond sample and polishing the single-crystal diamond sample to obtain an initial single-crystal diamond sample specifically includes: Obtain a single-crystal diamond sample, and obtain the roughness and flatness of the single-crystal diamond sample; The single-crystal diamond sample is polished using mechanical polishing technology. When the roughness and flatness of the single-crystal diamond sample reach a preset roughness and a preset flatness, the polishing process is complete, and an initial single-crystal diamond sample is obtained.
3. The method for detecting dislocation density in single-crystal diamond according to claim 1, characterized in that, The cleaning process includes acid washing and ultrasonic cleaning; the cleaning process of the initial single-crystal diamond sample to obtain the target single-crystal diamond sample specifically includes: A preset mixed strong acid solution is determined, and the initial single crystal diamond sample is heated and cleaned using the preset mixed strong acid solution to obtain a first single crystal diamond sample. The preset mixed strong acid solution is a mixed solution of sulfuric acid and nitric acid; After the acid washing process is completed, a preset ultrasonic cleaning solution is determined, and the first single crystal diamond sample is ultrasonically cleaned using the preset ultrasonic cleaning solution to obtain a second single crystal diamond sample. The preset ultrasonic cleaning solution includes acetone and ethanol; The second single-crystal diamond sample was rinsed with deionized water and then dried with nitrogen gas to obtain the target single-crystal diamond sample.
4. The method for detecting dislocation density in single-crystal diamond according to claim 1, characterized in that, The initial dislocation density detection results include a first measurement result, a second measurement result, and a third measurement result; The process of performing dislocation density detection on the target single-crystal diamond sample to obtain an initial dislocation density detection result, and constructing a target dislocation density measurement model based on the initial dislocation density detection result, specifically includes: The first dislocation density of the target single-crystal diamond sample was detected by XRD rocking curve method to obtain the first measurement result. The target single-crystal diamond sample was subjected to a second dislocation density detection process using Raman mapping to obtain a second measurement result. Obtain the sample surface parameter data of the target single-crystal diamond sample, and construct an initial dislocation density measurement model based on the sample surface parameter data, the first measurement result, and the second measurement result; The target single-crystal diamond sample is subjected to a third dislocation density detection process using an etching method to obtain a third measurement result. Based on the third measurement result, the initial dislocation density measurement model is optimized to obtain the target dislocation density measurement model.
5. The method for detecting dislocation density in single-crystal diamond according to claim 4, characterized in that, The first measurement result obtained by using the XRD rocking curve method to detect the first dislocation density of the target single-crystal diamond sample includes: The target single-crystal diamond sample is divided into regions to obtain multiple sample sub-regions of equal area; XRD rocking curve tests were performed on each of the sample sub-regions to obtain multiple XRD rocking curves, and a first measurement result was obtained based on the multiple XRD rocking curves.
6. The method for detecting dislocation density in single-crystal diamond according to claim 4, characterized in that, The third dislocation density detection process for the target single-crystal diamond sample using an etching method yields a third measurement result, specifically including: The target single-crystal diamond sample is placed in an MPCVD device, and hydrogen and oxygen of a preset concentration are introduced into the MPCVD device. The target single-crystal diamond sample is subjected to hydrogen-oxygen etching treatment using hydrogen and oxygen at a preset concentration in the MPCVD equipment to obtain the etching result. The number of dislocation etching pits within a preset area in the target single-crystal diamond sample is calculated based on the etching results, and a third measurement result is obtained based on the number of dislocation etching pits. The third measurement result is the ratio of the number of dislocation etch pits to the preset area.
7. The method for detecting dislocation density in single-crystal diamond according to claim 1, characterized in that, The process of acquiring the surface parameter data of the single-crystal diamond to be tested, inputting the surface parameter data into the target dislocation density measurement model, and outputting the target dislocation density detection result specifically includes: Acquire the surface parameter data of the single crystal diamond to be tested, wherein the surface parameter data includes surface morphology data and lattice defect data; The surface morphology data and the lattice defect data are input into the target dislocation density measurement model. The target dislocation density measurement model is used to perform dislocation density detection processing on the surface morphology data and the lattice defect data to obtain the target dislocation density detection result.
8. A dislocation density detection system for single-crystal diamond, characterized in that, The dislocation density detection system for single-crystal diamond includes: The sample polishing module is used to acquire single-crystal diamond samples and perform polishing treatment on the single-crystal diamond samples to obtain initial single-crystal diamond samples. The sample cleaning module is used to clean the initial single-crystal diamond sample to obtain the target single-crystal diamond sample. The model building module is used to perform dislocation density detection processing on the target single-crystal diamond sample, obtain the initial dislocation density detection result, and build the target dislocation density measurement model based on the initial dislocation density detection result. The dislocation density output module is used to acquire the surface parameter data of the single crystal diamond to be tested, input the surface parameter data into the target dislocation density measurement model, and output the target dislocation density detection result.
9. A terminal, characterized in that, The terminal includes: a memory, a processor, and a single-crystal diamond dislocation density detection program stored in the memory and executable on the processor. When the single-crystal diamond dislocation density detection program is executed by the processor, it implements the steps of the single-crystal diamond dislocation density detection method as described in any one of claims 1-7.
10. A computer-readable storage medium, characterized in that, The computer-readable storage medium stores a dislocation density detection program for single-crystal diamond, which, when executed by a processor, implements the steps of the dislocation density detection method for single-crystal diamond as described in any one of claims 1-7.
Citation Information
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