Efficient continuous graphite preparation system with integrated nondestructive testing function

Abstract

The invention belongs to the technical field of graphite preparation and detection, and particularly relates to an efficient continuous graphite preparation system with an integrated nondestructive testing function, which comprises a graphite preparation unit, a nondestructive testing unit, an intelligent feedback control unit, an environment control unit and a data management and tracing unit. Continuous preparation of graphite is achieved through a chemical vapor deposition method, the nondestructive testing unit detects the quality of graphite in real time, the intelligent feedback control unit optimizes preparation parameters based on the detection result, and the consistency of product quality is ensured. The environment control unit automatically adjusts the preparation environment according to feedback control, and the data management unit is responsible for tracing and managing process data. The problems that in the prior art, the graphite preparation process cannot be continuous, the real-time performance is poor, and a detection method is damaged are solved.

Description

Technical Field

[0001] The present invention belongs to the technical field of graphite preparation and detection, and in particular relates to a high-efficiency continuous graphite preparation system with integrated non-destructive detection. Background Art

[0002] With the vigorous development of high-tech industries such as new energy, electronic information and aerospace, the application of high-performance graphite materials in various fields is becoming increasingly extensive and vital. In key applications such as lithium-ion battery negative electrode materials, semiconductor chip heat dissipation substrates, and spacecraft thermal protection systems, the quality of graphite materials directly affects the performance and reliability of end products. These cutting-edge applications place extremely stringent requirements on graphite materials, requiring not only excellent conductivity, thermal stability and chemical inertness, but also high structural integrity, surface cleanliness and batch consistency. For example, in lithium-ion batteries, high-quality graphite can significantly improve the energy density and cycle life of the battery, which is directly related to the range and service life of electric vehicles; in the semiconductor industry, high-quality graphite materials can effectively improve the heat dissipation efficiency of chips, thereby improving the operating stability and service life of equipment, which is crucial for the development of emerging technologies such as high-performance computing and 5G communications; in the aerospace field, the thermal protection performance of graphite materials directly affects the safety and reliability of spacecraft in extreme environments, and is one of the key factors in the advancement of aerospace technology. Meeting these stringent performance requirements can not only significantly improve the performance and reliability of related products, but also broaden the scope of application of graphite materials and promote technological innovation and upgrading of the entire industrial chain. For example, a stable supply of high-quality graphite materials may promote the development of new high-energy density batteries and promote innovation in the electric vehicle industry; in the semiconductor industry, it may support more advanced chip manufacturing processes and help break through the bottleneck of computing power; in the aerospace field, high-quality graphite materials may promote the development of more advanced thermal protection systems and provide possibilities for longer-distance deep space exploration. Therefore, the development of a system that can efficiently and continuously prepare high-quality graphite and monitor and evaluate the quality of graphite in real time is of great strategic significance for promoting technological progress and product upgrades in related industries. This will not only meet the current market's urgent demand for high-quality graphite materials, but will also lay a solid foundation for the research and development and application of new graphite-based composite materials in the future, thereby promoting the overall progress in the field of materials science and engineering, and making important contributions to the country's competitiveness in related high-tech fields.

[0003] Although the preparation technology of graphite materials has been continuously improved, the existing methods still have many shortcomings and cannot meet the needs of industrial large-scale production. These shortcomings are mainly reflected in the continuity of the preparation process, the real-time quality control and the non-destructiveness of the detection method, which seriously restricts the large-scale application and industrialization of high-performance graphite materials.

[0004] Insufficient continuous preparation: For example, the Chinese patent with patent number CN114608308B discloses a graphitization furnace and its preparation method, which cannot achieve continuous preparation of high-quality graphite. This batch production method is not only inefficient, but also easily leads to quality fluctuations between batches, making it difficult to meet the needs of large-scale industrial production. The quality difference between batches may lead to unstable performance of downstream products, increasing the difficulty and cost of quality control.

[0005] Insufficient real-time quality detection: The Chinese patent with patent number CN113666748A proposes a method for preparing graphite materials, but it is still unable to detect the quality of graphite in real time during the preparation process, resulting in difficulties in product quality control. This lagging quality management model not only increases production costs, but may also lead to the production of a large number of unqualified products, reducing production efficiency and material utilization.

[0006] Insufficient pollution-free testing process: Although the Chinese patent with patent number CN103733051A involves a method for testing graphite materials, there is a problem that graphite is easily contaminated by water vapor or impurities in the air during testing after preparation, which affects the accuracy of the test results. This testing method exposed to the air is difficult to ensure the original state of the sample, which may cause the test results to deviate from the actual performance, affecting the accuracy and reliability of product quality assessment.

[0007] Insufficient non-destructive testing methods: For example, the graphite quality testing method in the Chinese patent with patent number N118347858A often requires destructive testing, which not only causes material waste, but also fails to ensure comprehensive quality control of each batch of products. The limitations of destructive testing make it impossible to conduct comprehensive testing of all products, increasing quality risks and causing unnecessary waste of resources.

[0008] The existence of the above technical bottlenecks makes the large-scale production of high-quality graphite materials face many challenges and it is difficult to meet the growing market demand. Therefore, how to provide an innovative system that can integrate continuous preparation and real-time non-destructive testing to break through the limitations of existing technologies and achieve efficient and stable production of high-quality graphite materials is a technical problem that needs to be solved urgently. Summary of the invention

[0009] The purpose of the present invention is to provide an efficient continuous graphite preparation system with integrated non-destructive testing, so as to solve the technical problems that the prior art cannot realize continuous graphite preparation, realize efficient and stable production of high-quality graphite materials, and graphite is easily contaminated by water vapor or impurities in the air during post-preparation testing, making it impossible to realize non-destructive testing of graphite quality.

[0010] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:

[0011] A high-efficiency continuous graphite preparation system with integrated non-destructive testing, comprising a graphite preparation unit, a non-destructive testing unit, an intelligent feedback control unit, an environmental control unit, and a data management and tracing unit, wherein the graphite preparation unit is connected to the non-destructive testing unit, the non-destructive testing unit is connected to the intelligent feedback control unit, the intelligent feedback control unit is respectively connected to the environmental control unit and the graphite preparation unit, and the data management and tracing unit is respectively connected to the graphite preparation unit and the non-destructive testing unit;

[0012] The graphite preparation unit is a roll-to-roll chemical vapor deposition preparation unit, which is used for continuous graphite preparation by chemical vapor deposition;

[0013] The nondestructive testing unit is used to perform nondestructive testing on the graphite prepared by the graphite preparation unit;

[0014] The intelligent feedback control unit is used to optimize the preparation parameters based on the detection results of the nondestructive testing unit and the preset algorithm, and control the graphite preparation unit and the environmental control unit based on the optimized preparation parameters;

[0015] The environmental control unit is used to control the environmental parameters during the graphite preparation process and to control the environmental parameters based on the optimized parameters of the intelligent feedback control unit;

[0016] The data management and traceability unit is arranged in the server and is provided with a product number generating unit. The product number generating unit associates production parameters and quality data to generate a production number of the graphite product, and stores the preparation parameters corresponding to the production number in the preparation process of the graphite preparation unit and the detection data obtained by the non-destructive detection unit.

[0017] Preferably, the graphite preparation unit comprises a feeding unit, a preheating unit, a reaction unit, a gas supply unit, a cooling unit and a receiving unit, wherein the feeding unit is connected to the preheating unit, the reaction unit is connected to the preheating unit and the gas supply unit, and the cooling unit is connected to the receiving unit;

[0018] The feeding unit is provided with a base material supply reel, a tension controller and a guide roller, the preheating unit is provided with a heating device and a temperature monitoring device, the heating device is an infrared heating device or a resistance heating device; the reaction unit includes a reaction chamber, the reaction chamber is made of a high temperature resistant material, the high temperature resistant material is quartz, a gas distribution device and a temperature equalization device are provided inside the reaction chamber, the gas distribution device is used to achieve uniform distribution of the introduced gas in the entire reaction chamber, the temperature equalization device is used to achieve temperature balance in the entire reaction chamber; the gas supply unit is used to realize gas supply in the reaction chamber, the cooling unit realizes cooling of the prepared graphite by a gradient cooling device and a low temperature inert gas injection system; the material collecting device continuously collects the cooled graphite material.

[0019] Preferably, the graphite preparation process of the graphite preparation unit is as follows: a base material made of copper foil or nickel foil is released from a supply reel, passes through a tension controller and a guide roller and enters a preheating unit, the preheating unit heats the base material to a specified temperature range to prepare for graphite growth, the heated base material enters a reaction chamber, and simultaneously a carbon source gas and a carrier gas are mixed in a preset proportion and introduced into the reaction chamber, under high temperature and a specific atmosphere, carbon atoms are deposited and reorganized on the surface of the base, and grow into a graphite structure, the grown graphite material enters a cooling zone, and is protected by a gradient cooling device and a low-temperature inert gas injection system to ensure the integrity of the graphite structure, and the cooled graphite material is continuously collected by a collecting device.

[0020] Preferably, the nondestructive testing unit comprises a laser emission source, an optical path module, a spectrometer, a detection probe and a data acquisition module, wherein the laser emission source is connected to the optical path module, the optical path module is connected to the spectrometer, the spectrometer is connected to the detection probe, and the detection probe is connected to the data acquisition and analysis module;

[0021] The laser emission source is a solid-state laser, and the wavelength of the laser emitted by the solid-state laser is 532nm or 633nm; the optical path module includes a focusing lens, a spectroscope, a collecting lens and a fiber coupler; the spectrometer is a Raman spectrometer, and the detection probe is an online movable Raman probe installed at the reaction unit outlet and the cooling unit outlet; the data acquisition and analysis module realizes the acquisition and analysis of the Raman spectrum formed by the spectrometer decomposing the scattered light.

[0022] Preferably, the specific working process of the nondestructive testing unit is as follows: the laser emission source emits a laser of a specific wavelength, which is irradiated onto the prepared graphite sample through the optical path module; the graphite sample generates Raman scattered light, which is transmitted to the spectrometer through the collection lens and the optical fiber; the spectrometer decomposes the scattered light to form a Raman spectrum; the data acquisition module collects Raman spectrum data in real time and performs rapid analysis; the data acquisition and analysis module is based on the G peak (~1580cm -1 ), 2D peak (~2700cm -1 ) and D peak (~1350cm -1 ) to evaluate graphite quality.

[0023] Preferably, the intelligent feedback control unit includes a central processing unit, a control module and an execution module, the central processing unit is connected to the control module, the control module is connected to the execution module, the control module sends a control command to the execution module, and the execution module performs corresponding actions according to the control command.

[0024] Preferably, the specific working process of the intelligent feedback control unit is: the central processing unit receives the Raman spectroscopy analysis results transmitted by the non-destructive testing unit, the control unit optimizes the graphite preparation parameters based on a preset algorithm, and sends adjustment control commands to the execution module based on the optimized graphite preparation parameters, including adjustment control commands for temperature parameters, gas flow parameters, and substrate movement speed parameters.

[0025] Preferably, the environmental control unit includes an atmosphere protection module, a temperature control system and an anti-vibration system. The atmosphere protection module includes an inert gas supply device and an airflow controller. The inert gas supply device continuously delivers inert gas to the detection area to form a protective atmosphere. The inert gas is nitrogen or argon. The anti-vibration system is provided with an active vibration isolation platform and a shock-absorbing bracket for absorbing environmental vibrations in real time.

[0026] Preferably, two detection probes are provided, including a first detection probe and a second detection probe, and the overall preparation process of graphite is as follows: the base material is released from the supply reel and enters the preheating module to be heated to a predetermined temperature; the preheated base material enters the reaction chamber, and the mixed gas is introduced at the same time to start the graphite growth process; at the outlet of the reaction module, the first detection probe performs real-time detection of the growing graphite; the intelligent feedback control unit adjusts and optimizes the preparation parameters in real time according to the detection results; the grown graphite material enters the cooling module for gradient cooling; at the outlet of the cooling module, the second detection probe performs final quality detection on the cooled graphite; the environmental control unit maintains a stable environment in the detection area throughout the process; the prepared graphite material is continuously collected in real time by the material receiving device; the data management and traceability module records the entire process data of graphite preparation, and generates a unique production number identification for each batch of products.

[0027] The beneficial effects of the present invention include:

[0028] The present invention provides an efficient continuous graphite preparation system with integrated nondestructive testing, including a graphite preparation unit, a nondestructive testing unit, an intelligent feedback control unit, an environmental control unit, and a data management and traceability unit. The graphite preparation unit performs continuous graphite preparation by chemical vapor deposition; the nondestructive testing unit performs nondestructive testing on the graphite prepared by the graphite preparation unit; the intelligent feedback control unit optimizes the preparation parameters based on the test results of the nondestructive testing unit and a preset algorithm, and controls the graphite preparation unit and the environmental control unit based on the optimized preparation parameters; the environmental control unit is used to control the environmental parameters in the graphite preparation process and to control the environmental parameters based on the optimized parameters of the intelligent feedback control unit.

[0029] First, by setting up a graphite preparation unit including a feeding unit, a preheating unit, a reaction unit, a gas supply unit, a cooling unit and a collecting unit, the preheated substrate enters the reaction chamber, and the carbon source gas and the carrier gas are mixed in a preset proportion and introduced into the reaction chamber. Under high temperature and a specific atmosphere, carbon atoms are deposited and reorganized on the surface of the substrate to form a graphite structure. The grown graphite material is cooled, and gradient cooling and inert gas protection are used to make the final graphite structure complete, and the cooled graphite material is continuously collected by a collecting device, thereby realizing continuous production, real-time quality monitoring and non-destructive testing in the graphite preparation process, so as to achieve efficient and stable production of high-quality graphite materials.

[0030] Secondly, by setting up a nondestructive testing unit including a laser emission source, an optical path module, a spectrometer, a detection probe and a data acquisition module, nondestructive testing of graphite is achieved during the preparation process. There is no need to perform destructive testing on the prepared graphite, which avoids the waste of graphite materials, reduces the production cost of graphite, and achieves comprehensive control of graphite preparation.

[0031] Again, the laser emission source uses a laser with a wavelength of 532nm or 633nm to ensure sensitivity to the graphite structure, so as to achieve non-destructive and rapid detection of graphite. The number of layers, defect density and crystal quality of graphite are evaluated based on the intensity, position and half-width of the G peak (~1580cm^-1), 2D peak (~2700cm^-1) and D peak (~1350cm^-1) of the spectrum, further achieving high efficiency and continuity in graphite production.

[0032] Finally, by setting up an intelligent feedback control unit including a central processing unit, a control module and an execution module, the Raman detection results are associated with the preparation parameters to achieve real-time optimization of the preparation process and further improve the quality of the prepared graphite. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 The figure is a structural diagram of the high-efficiency continuous graphite preparation system with integrated non-destructive testing according to the present invention.

[0034] Figure 2 This is a composition structure diagram of the graphite preparation unit of the present invention.

[0035] Figure 3 It is a composition structure diagram of the nondestructive testing unit of the present invention.

[0036] Figure 4 A schematic diagram of the Raman spectrum of graphite prepared by the efficient continuous graphite preparation system with integrated non-destructive testing of the present invention.

[0037] Figure 5 Schematic diagram of the Raman spectrum of graphene. DETAILED DESCRIPTION

[0038] The following is combined with Figure 1 to Figure 5 The present invention is further described in detail:

[0039] Example 1

[0040] See attached Figure 1 As shown, a high-efficiency continuous graphite preparation system with integrated non-destructive testing includes a graphite preparation unit, a non-destructive testing unit, an intelligent feedback control unit, an environmental control unit, and a data management and tracing unit. The graphite preparation unit is connected to the non-destructive testing unit, the non-destructive testing unit is connected to the intelligent feedback control unit, the intelligent feedback control unit is respectively connected to the environmental control unit and the graphite preparation unit, and the data management and tracing unit is respectively connected to the graphite preparation unit and the non-destructive testing unit.

[0041] The graphite preparation unit is a roll-to-roll chemical vapor deposition preparation unit that performs continuous graphite preparation by chemical vapor deposition. The continuous preparation of graphite is achieved by the roll-to-roll chemical vapor deposition preparation unit. High-purity metal foil (such as copper foil or nickel foil) is used as the growth substrate, and it is continuously delivered into the system through a precisely controlled feeding mechanism. The preheating unit uses infrared heating or resistance heating to uniformly heat the substrate material to a suitable temperature (approximately a specified temperature range) to prepare for subsequent graphite growth. The reaction unit uses a precision gas flow control system to mix the carbon source gas (such as methane) and the carrier gas (such as hydrogen, argon) in a specific proportion and then introduce them. The reaction chamber uses quartz tubes or special alloy materials to ensure stability in high temperature environments. The graphite growth conditions are optimized by precisely controlling the temperature, gas flow and pressure. The cooling unit uses gradient cooling technology to ensure the integrity and uniformity of the graphite structure. Inert gases (such as nitrogen) are used to assist the cooling process, further achieving the integrity and uniformity of the graphite structure.

[0042] The non-destructive testing unit sets up detection points at the exit of the reaction zone and the exit of the cooling zone to achieve real-time and non-destructive monitoring of graphite quality, monitor the growth quality and structural integrity of graphite, and perform non-destructive testing on the graphite prepared by the graphite preparation unit. A laser with a wavelength of 532nm or 633nm is used to ensure sensitivity to the graphite structure, and high-precision optical components, including focusing lenses, spectroscopes, and collection lenses, are used to achieve fast and accurate spectrum acquisition.

[0043] The intelligent feedback control unit associates the Raman detection results with the preparation parameters to achieve real-time optimization of the preparation process. Based on the detection results of the nondestructive testing unit and the preset algorithm, the preparation parameters are optimized, and the graphite preparation unit and the environmental control unit are controlled based on the optimized preparation parameters; the environmental control unit controls the environmental parameters in the graphite preparation process and controls the environmental parameters based on the optimized parameters of the intelligent feedback control unit; the data management and traceability unit is set in the server, and is provided with a product number generation unit, which associates the production parameters and quality data to generate the production number of the graphite product, and stores the preparation parameters corresponding to the production number in the preparation process of the graphite preparation unit and the detection data obtained by the nondestructive testing unit.

[0044] Example 2

[0045] Based on Example 1, see Figure 2 The graphite preparation unit includes a feeding unit, a preheating unit, a reaction unit, a gas supply unit, a cooling unit and a receiving unit. The feeding unit is connected to the preheating unit, the reaction unit is connected to the preheating unit and the gas supply unit, and the cooling unit is connected to the receiving unit. The feeding unit is provided with a substrate material supply reel, a tension controller and a guide roller. The preheating unit is provided with a heating device and a temperature monitoring device. The heating device is an infrared heating device or a resistance heating device. The reaction unit includes a reaction chamber, which is made of a high-temperature resistant material, which is quartz. A gas distribution device and a temperature balancing device are provided inside the reaction chamber. The gas distribution device is used to achieve uniform distribution of the introduced gas in the entire reaction chamber. The temperature balancing device is used to achieve temperature balance in the entire reaction chamber. The gas supply unit is used to realize gas supply in the reaction chamber. The cooling unit cools the prepared graphite through a gradient cooling device and a low-temperature inert gas injection system. The receiving device continuously collects the cooled graphite material.

[0046] In this embodiment, the graphite preparation process of the graphite preparation unit is that a base material made of copper foil or nickel foil is released from a supply reel, passes through a tension controller and a guide roller and enters a preheating unit, the preheating unit heats the base material to a specified temperature range to prepare for graphite growth, the heated base material enters the reaction chamber, and at the same time, the carbon source gas and the carrier gas are mixed in a preset proportion and introduced into the reaction chamber, under high temperature and specific atmosphere, carbon atoms are deposited and recombined on the surface of the base, and grow into a graphite structure, the grown graphite material enters the cooling zone, and is protected by a gradient cooling device and a low-temperature inert gas injection system to ensure the integrity of the graphite structure, and the cooled graphite material is continuously collected by a collecting device.

[0047] The substrate material is heated to a specified temperature range of 900°C-1200°C, and the carbon source gas methane (CH 2 ) or acetylene (C 2 H 2 ), the carbon source gas concentration is methane 1%-5%, acetylene 0.5%-2%, and the carrier gas is hydrogen (H 2 ) and argon (Ar), hydrogen flow rate is 100-300sccm, argon flow rate is 500-1000sccm, pressure is 10-100Torr (LPCVD). The substrate material is copper foil or nickel foil, the growth time is 1-5 hours, and the cooling rate is 5-10℃ / minute.

[0048] In the process of preparing graphite by chemical vapor deposition (CVD), the selection of key process parameters is crucial to the quality of the final product. First, the substrate temperature is usually maintained between 900°C and 1200°C. Higher temperatures help reduce defects in graphite and improve interlayer bonding quality. Carbon source gas usually selects methane or acetylene, where the concentration of methane is between 1%-5% and the concentration of acetylene is between 0.5%-2% to control the carbon deposition rate and avoid too fast deposition leading to a decrease in graphite quality. Hydrogen and argon are selected as carrier gases, where the concentration of hydrogen is 5%-20%. Hydrogen helps clean the surface and control the deposition rate of carbon atoms, while argon is used as an inert gas to dilute the carbon source gas and maintain the stability of the reaction atmosphere. The hydrogen flow rate is usually 100-300sccm and the argon flow rate is 500-1000sccm. The preparation of graphite is usually carried out at a low pressure of 10-100Torr, because low pressure helps control the distribution and deposition rate of the carbon source and ensure the uniform growth of the graphite layer. The substrate material is mostly copper foil or nickel foil, and the thickness is generally 25-50μm. The selection of the substrate material and its thickness are crucial to the uniformity of carbon deposition and the stability of the preparation process. The flow rate control of the carbon source gas is also very important. The methane flow rate is usually 10-50sccm, while the acetylene flow rate is between 5-20sccm. The growth time is set according to the required graphite thickness, generally 1-5 hours. The cooling process rate is usually controlled at 5-10℃ / minute, and inert gases such as argon are used to protect the graphite from oxidation during the cooling process. In order to ensure the quality of graphite, the substrate material needs to be cleaned before preparation, such as using solvent cleaning or plasma cleaning. At the same time, during the preparation process, the quality of the graphite layer can be detected by real-time monitoring methods such as Raman spectroscopy to ensure the structural integrity of the final graphite product.

[0049] Example 3

[0050] Based on Example 1 or Example 2, see Figure 3 The nondestructive testing unit includes a laser emission source, an optical path module, a spectrometer, a detection probe and a data acquisition module, wherein the laser emission source is connected to the optical path module, the optical path module is connected to the spectrometer, the spectrometer is connected to the detection probe, and the detection probe is connected to the data acquisition and analysis module;

[0051] The laser emission source is a solid-state laser, and the wavelength of the laser emitted by the solid-state laser is 532nm or 633nm; the optical path module includes a focusing lens, a spectroscope, a collecting lens and a fiber coupler; the spectrometer is a Raman spectrometer, and the detection probe is an online movable Raman probe installed at the outlet of the reaction unit and the outlet of the cooling unit. The data acquisition and analysis module realizes the acquisition and analysis of the Raman spectrum formed by the spectrometer decomposing the scattered light.

[0052] The specific working process of the nondestructive testing unit is that the laser emission source emits a laser of a specific wavelength, which is irradiated onto the prepared graphite sample through the optical path module. The graphite sample generates Raman scattered light, which is transmitted to the spectrometer through the collection lens and optical fiber. The spectrometer decomposes the scattered light to form a Raman spectrum; the data acquisition module collects Raman spectrum data in real time and performs rapid analysis. The data acquisition and analysis module evaluates the quality of graphite based on the G peak (~1580cm^-1), 2D peak (~2700cm^-1) and D peak (~1350cm^-1).

[0053] In this embodiment, the intelligent feedback control unit includes a central processing unit, a control module and an execution module, wherein the central processing unit is connected to the control module, the control module is connected to the execution module, the control module sends a control command to the execution module, the execution module performs corresponding actions according to the control command, associates the Raman detection results of the non-destructive testing unit with the preparation parameters, and automatically adjusts the key parameters such as the reaction temperature, gas flow rate, and substrate movement speed according to the Raman spectrum analysis results to achieve real-time optimization of the preparation process. And according to the preset quality standards, the continuously produced graphite materials are graded in real time to ensure the consistency of product quality. The specific working process of the intelligent feedback control unit is that the central processing unit receives the Raman spectrum analysis results transmitted by the non-destructive testing unit, the control unit optimizes the graphite preparation parameters based on the preset algorithm, and sends adjustment control commands to the execution module based on the optimized graphite preparation parameters, including adjustment control commands for temperature parameters, gas flow parameters, and substrate movement speed parameters.

[0054] The intelligent feedback control system also has an early warning module. When obvious quality abnormalities are detected, the system will promptly alarm and initiate emergency processing procedures to minimize the production of unqualified products.

[0055] The environmental control unit includes an atmosphere protection module, a temperature control system and an anti-vibration system. The atmosphere protection module includes an inert gas supply device and an airflow controller. The inert gas supply device continuously delivers inert gas to the detection area to form a protective atmosphere. The inert gas is nitrogen or argon. The anti-vibration system is equipped with an active vibration isolation platform and a shock-absorbing bracket to absorb environmental vibration in real time, ensure stability during the detection process, and improve the reliability of spectral data. By maintaining a constant temperature in the detection area, the influence of temperature fluctuations on the Raman spectrum is eliminated.

[0056] There are two detection probes, including a first detection probe and a second detection probe. The overall preparation process of graphite is as follows: the base material is released from the supply reel and enters the preheating module to be heated to a predetermined temperature; the preheated base material enters the reaction chamber, and the mixed gas is introduced at the same time to start the graphite growth process; at the outlet of the reaction module, the first detection probe performs real-time detection of the growing graphite; the intelligent feedback control unit adjusts and optimizes the preparation parameters in real time according to the detection results; the grown graphite material enters the cooling module for gradient cooling; at the outlet of the cooling module, the second detection probe performs final quality detection on the cooled graphite; the environmental control unit maintains a stable environment in the detection area throughout the process; the prepared graphite material is continuously collected in real time by the collecting device; the data management and traceability module records the entire process data of graphite preparation, and generates a unique production number identification for each batch of products.

[0057] This integrated roll-to-roll chemical vapor deposition preparation and Raman nondestructive testing system can achieve continuous production and real-time quality monitoring of high-quality graphite materials, effectively solving the technical problems faced by current graphite preparation technology. The system not only improves production efficiency and product quality consistency, but also minimizes material waste, laying a solid foundation for the large-scale application of high-performance graphite materials.

[0058] See also Figure 4 In the Raman spectrum of graphite samples, we observed the following characteristic peaks: G peak is located at about 1580 cm -1 , corresponding to sp 2 In-plane vibration mode of hybridized carbon atoms; 2D peak is located at about 2700 cm -1 , which is the second harmonic of the D peak. In contrast, see Figure 5 The Raman spectrum of graphene shows the following characteristics: the G peak is similar to that of graphite, but the intensity is weaker; the 2D peak is sharper and the intensity is significantly higher than that of graphite. This is because the 2D peak of a few-layer graphene is usually 2 to 4 times the intensity of the G peak. Figure 4 and Figure 5 The results clearly demonstrate the effectiveness of Raman spectroscopy in distinguishing graphite from graphene and characterizing the quality and number of graphene layers.

[0059] In summary, the efficient continuous graphite preparation system with integrated nondestructive testing provided by the present invention includes a graphite preparation unit, a nondestructive testing unit, an intelligent feedback control unit, an environmental control unit, and a data management and tracing unit. By setting a graphite preparation unit including a feeding unit, a preheating unit, a reaction unit, a gas supply unit, a cooling unit, and a receiving unit, the preheated substrate enters the reaction chamber, and the carbon source gas and the carrier gas are mixed in a preset ratio and introduced into the reaction chamber. Under high temperature and a specific atmosphere, carbon atoms are deposited and reorganized on the surface of the substrate to form a graphite structure. The grown graphite material is cooled, and the final graphite structure is complete through gradient cooling and inert gas protection, and the cooled graphite material is continuously collected by the receiving device, realizing the continuous production, real-time quality monitoring and nondestructive testing in the graphite preparation process, so as to realize the efficient and stable production of high-quality graphite materials.

[0060] By setting up a nondestructive testing unit including a laser emission source, an optical path module, a spectrometer, a detection probe and a data acquisition module, nondestructive testing of graphite is achieved during the preparation process. There is no need to perform destructive testing on the prepared graphite, which avoids the waste of graphite materials, reduces the production cost of graphite, and achieves comprehensive control of graphite preparation. The laser emission source uses a laser with a wavelength of 532nm or 633nm to ensure sensitivity to the graphite structure to achieve nondestructive and rapid detection of graphite. The number of layers, defect density and crystal quality of graphite are evaluated based on the intensity, position and half-width of the G peak, 2D peak and D peak of the spectrum, further achieving high efficiency and continuity of graphite production. By setting up an intelligent feedback control unit including a central processing unit, a control module and an execution module, the Raman detection results are associated with the preparation parameters to achieve real-time optimization of the preparation process and further improve the quality of the prepared graphite.

Claims

1. An efficient continuous graphite preparation system with integrated non-destructive testing, characterized in that: It includes a graphite preparation unit, a nondestructive testing unit, an intelligent feedback control unit, an environmental control unit, and a data management and tracing unit. The graphite preparation unit is connected to the nondestructive testing unit, the nondestructive testing unit is connected to the intelligent feedback control unit, the intelligent feedback control unit is connected to the environmental control unit, and the data management and tracing unit is connected to the graphite preparation unit, the nondestructive testing unit and the environmental control unit respectively; The graphite preparation unit is a roll-to-roll chemical vapor deposition preparation unit, which is used for continuous graphite preparation by chemical vapor deposition; The nondestructive testing unit is used to perform nondestructive testing on the graphite prepared by the graphite preparation unit; The intelligent feedback control unit is used to optimize the preparation parameters based on the detection results of the nondestructive testing unit and the preset algorithm, and control the graphite preparation unit and the environmental control unit based on the optimized preparation parameters; The environmental control unit is used to control the environmental parameters during the graphite preparation process and to control the environmental parameters based on the optimized parameters of the intelligent feedback control unit; The data management and traceability unit is arranged in the server and is provided with a product number generating unit. The product number generating unit associates production parameters and quality data to generate a production number of the graphite product, and stores the preparation parameters corresponding to the production number in the preparation process of the graphite preparation unit and the detection data obtained by the non-destructive detection unit.

2. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 1, characterized in that: The graphite preparation unit comprises a feeding unit, a preheating unit, a reaction unit, a gas supply unit, a cooling unit and a receiving unit, wherein the feeding unit is connected to the preheating unit, the reaction unit is connected to the preheating unit and the gas supply unit, and the cooling unit is connected to the receiving unit; The feeding unit is provided with a base material supply reel, a tension controller and a guide roller, the preheating unit is provided with a heating device and a temperature monitoring device, the heating device is an infrared heating device or a resistance heating device; the reaction unit includes a reaction chamber, the reaction chamber is made of a high temperature resistant material, the high temperature resistant material is quartz, a gas distribution device and a temperature equalization device are provided inside the reaction chamber, the gas distribution device is used to achieve uniform distribution of the introduced gas in the entire reaction chamber, the temperature equalization device is used to achieve temperature balance in the entire reaction chamber; the gas supply unit is used to realize gas supply in the reaction chamber, the cooling unit realizes cooling of the prepared graphite by a gradient cooling device and a low temperature inert gas injection system; the material collecting device continuously collects the cooled graphite material.

3. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 2, characterized in that: The graphite preparation process of the graphite preparation unit is as follows: a base material made of copper foil or nickel foil is released from a supply reel, passes through a tension controller and a guide roller and enters a preheating unit, the preheating unit heats the base material to a specified temperature range to prepare for graphite growth, the heated base material enters a reaction chamber, and at the same time, a carbon source gas and a carrier gas are mixed in a preset ratio and introduced into the reaction chamber, under high temperature and a specific atmosphere, carbon atoms are deposited and reorganized on the surface of the base to grow into a graphite structure, the grown graphite material enters a cooling zone, and is protected by a gradient cooling device and a low-temperature inert gas injection system to ensure the integrity of the graphite structure, the cooled graphite material is continuously collected by a collecting device, wherein the carbon source gas includes methane and acetylene, and the carrier gas is hydrogen and argon.

4. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 1, characterized in that: The nondestructive testing unit comprises a laser emission source, an optical path module, a spectrometer, a detection probe, and the laser emission source is connected to the optical path module, the optical path module is connected to the spectrometer, the spectrometer is connected to the detection probe, and the detection probe is connected to the data acquisition and analysis module; The laser emission source is a solid-state laser, and the laser wavelength emitted by the solid-state laser is 532nm or 633nm; the optical path module includes a focusing lens, a spectroscope, a collecting lens and a fiber coupler; the spectrometer is a Raman spectrometer, and the detection probe is an online movable Raman probe installed at the reaction unit outlet and the cooling unit outlet; the data acquisition and analysis module realizes the acquisition and analysis of the Raman spectrum formed by the spectrometer decomposing the scattered light.

5. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 4, characterized in that: The specific working process of the nondestructive testing unit is as follows: a laser emission source emits a laser of a specific wavelength, which is irradiated onto the prepared graphite sample through an optical path module; the graphite sample generates Raman scattered light, which is transmitted to the spectrometer through a collecting lens and an optical fiber; the spectrometer decomposes the scattered light to form a Raman spectrum; the data acquisition module collects Raman spectrum data in real time and performs rapid analysis; the data acquisition and analysis module evaluates the quality of graphite based on the G peak, 2D peak and D peak.

6. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 1, characterized in that: The intelligent feedback control unit includes a central processing unit, a control module and an execution module. The central processing unit is connected to the control module, the control module is connected to the execution module, the control module sends a control command to the execution module, and the execution module performs corresponding actions according to the control command.

7. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 6, characterized in that: The specific working process of the intelligent feedback control unit is as follows: the central processing unit receives the Raman spectroscopy analysis results transmitted by the nondestructive testing unit, the control unit optimizes the graphite preparation parameters based on a preset algorithm, and sends adjustment control commands to the execution module based on the optimized graphite preparation parameters, including adjustment control commands for temperature parameters, gas flow parameters, and substrate movement speed parameters.

8. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 1, characterized in that: The environmental control unit includes an atmosphere protection module, a temperature control system and an anti-vibration system. The atmosphere protection module includes an inert gas supply device and an airflow controller. The inert gas supply device continuously delivers inert gas to the detection area to form a protective atmosphere. The inert gas is nitrogen or argon. The anti-vibration system is provided with an active vibration isolation platform and a shock-absorbing bracket for absorbing environmental vibrations in real time.

9. The high-efficiency continuous graphite preparation system with integrated non-destructive testing according to claim 1, characterized in that: There are two detection probes, including a first detection probe and a second detection probe. The overall preparation process of graphite is as follows: the base material is released from the supply reel and enters the preheating module to be heated to a predetermined temperature; the preheated base material enters the reaction chamber, and the mixed gas is introduced at the same time to start the graphite growth process; at the outlet of the reaction module, the first detection probe performs real-time detection of the growing graphite; the intelligent feedback control unit adjusts and optimizes the preparation parameters in real time according to the detection results; the grown graphite material enters the cooling module for gradient cooling; at the outlet of the cooling module, the second detection probe performs final quality detection on the cooled graphite; the environmental control unit maintains a stable environment in the detection area throughout the process; the prepared graphite material is continuously collected in real time by the collecting device; the data management and traceability module records the entire process data of graphite preparation, and generates a unique production number identification for each batch of products.

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