A carbon nanotube array fabrication system and method

Abstract

This invention provides a carbon nanotube array fabrication system and method. The system includes: a multi-channel reaction module comprising at least two reaction chambers, each chamber containing a substrate and providing an independent process environment; a material transfer module for loading the substrate into each reaction chamber and removing the processed substrate from each reaction chamber; a gas supply module connected to the multi-channel reaction module for independently supplying the process gases required for the reaction to each reaction chamber; a monitoring module for monitoring the material growth process within each reaction chamber; and a control module communicatively connected to the multi-channel reaction module, material transfer module, gas supply module, and monitoring module to receive data collected by the monitoring module and independently control the process parameters of each reaction chamber. This invention achieves efficient and controllable fabrication of carbon nanotube arrays, improving both R&D efficiency and product yield, meeting the needs of rapid iteration and industrialization.

Description

Technical Field

[0001] This invention relates to the field of nanomaterial preparation technology, and in particular to a carbon nanotube array preparation system and method. Background Technology

[0002] With the rapid development of high-end fields such as global electronics and information, new energy vehicles, aerospace, and artificial intelligence, the integration of devices continues to increase and power density continues to break through. Thermal management has become a core bottleneck restricting product performance upgrades and reliability improvements. Taking advanced microelectronic packaging as an example, the heat flux density of chips with process technology of 3nm and below has exceeded 500 W / cm². Traditional thermal interface materials (such as silicone grease, metal sheets, and ceramic matrix composites) are difficult to meet the requirements of efficient heat dissipation due to defects such as low thermal conductivity, high interfacial thermal resistance, and poor mechanical compatibility, resulting in excessively high chip operating temperatures, performance degradation, and shortened lifespan. Carbon nanotubes, as a typical one-dimensional carbon nanomaterial, are regarded as an ideal candidate for the next generation of high-performance thermal interface materials due to their unique structure and excellent axial thermal conductivity (up to 3000-6600 W / (m・K)).

[0003] Currently, the fabrication of carbon nanotube arrays mainly employs chemical vapor deposition (CVD). Existing CVD equipment is typically a standalone structure, allowing only one set of process parameters to be tested at a time, with sample characterization performed offline after growth. This approach suffers from two main problems: first, it is inefficient, as process parameter optimization heavily relies on experience-driven trial-and-error methods, resulting in long development cycles, high costs, and difficulty in meeting the demands of rapid material iteration; second, it lacks process control, as the inability to obtain real-time microstructural information (such as array height, density, and crystallinity) during growth means that once process parameters are set, they cannot be adjusted according to actual conditions, leading to poor consistency in sample performance (such as thermal conductivity), low batch yield, and difficulty in achieving controllable fabrication. Summary of the Invention

[0004] To address the technical problems of low efficiency, uncontrollable processes, and poor product consistency in existing technologies, this invention provides a carbon nanotube array fabrication system and method. The technical solution is as follows:

[0005] On one hand, a carbon nanotube array fabrication system is provided, comprising: a multi-channel reaction module including at least two reaction chambers, each reaction chamber for containing a substrate and providing an independent process environment; a material transfer module for loading the substrate into each reaction chamber and removing the processed substrate from each reaction chamber; a gas supply module connected to the multi-channel reaction module for independently supplying the process gas required for the reaction to each reaction chamber; a monitoring module for monitoring the material growth process in each reaction chamber; and a control module communicatively connected to the multi-channel reaction module, the material transfer module, the gas supply module, and the monitoring module to receive data collected by the monitoring module and independently control the process parameters of each reaction chamber.

[0006] On the other hand, a method for preparing carbon nanotube arrays is provided. This method is applied to the carbon nanotube array preparation system described above. The method includes: loading the substrate and sending it into each reaction chamber, and setting independent process parameters for each reaction chamber; purging each reaction chamber with an inert gas and heating it to a set temperature; introducing process gas into each reaction chamber to start the growth of the carbon nanotube array, and performing real-time monitoring during the growth process; dynamically adjusting the process parameters of the corresponding reaction chamber according to the results of the real-time monitoring; and cooling the reaction chamber and removing the substrate after the growth is completed.

[0007] The beneficial effects of the technical solution provided by the embodiments of the present invention include at least the following: First, by constructing a multi-channel reaction module and independent material transfer, gas supply, and monitoring modules, multiple reaction chambers can operate in parallel and independently. A single batch of experiments can simultaneously explore multiple sets of differentiated process parameters, completely changing the limitation of low efficiency in parameter optimization of traditional preparation systems. This improves process development efficiency by more than 80% and supports large-scale synchronous preparation, increasing production efficiency by more than 5 times compared to traditional processes, thus meeting the needs of rapid material iteration and industrialization. Second, the invention creatively integrates in-situ optical monitoring and Raman spectroscopy monitoring, enabling real-time and synchronous acquisition of morphological and crystal quality information of carbon nanotube arrays during growth, solving the problem that traditional offline characterization cannot reflect the dynamic growth process. Finally, the control module achieves centralized coordination and closed-loop control of each module, enabling dynamic adjustment of process parameters based on real-time monitoring data, thereby precisely controlling the growth state of the array. This significantly improves the consistency of performance of samples in the same batch, increasing the product qualification rate from less than 60% in traditional processes to over 95%, providing a reliable system solution for the controllable preparation of high-performance, highly consistent carbon nanotube array thermal interface materials. Attached Figure Description

[0008] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0009] Figure 1 This is a schematic diagram of a carbon nanotube array fabrication system provided in an embodiment of the present invention;

[0010] Figure 2 This is a schematic block diagram of a multi-channel reaction module provided in an embodiment of the present invention;

[0011] Figure 3 This is a schematic diagram of the structure of a reaction chamber body, a base positioning crucible, and a linear motion unit provided in an embodiment of the present invention;

[0012] Figure 4 This is a schematic block diagram of a material transfer module provided in an embodiment of the present invention;

[0013] Figure 5 This is a schematic block diagram of a gas supply module provided in an embodiment of the present invention;

[0014] Figure 6 This is a schematic diagram of a monitoring module provided in an embodiment of the present invention;

[0015] Figure 7 This is a flowchart of a carbon nanotube array fabrication method provided in an embodiment of the present invention.

[0016] Explanation of reference numerals in the attached drawings: 100, Multi-channel reaction module; 101, Reaction chamber body; 102, Reaction chamber; 103, Heating unit; 104, Cooling unit; 105, Temperature sensor; 106, Observation window; 107, Gas passage; 200, Material transfer module; 201, Base positioning crucible; 202, Loading execution unit; 203, Linear motion unit; 300, Gas supply module; 301, Multi-channel mass flow controller; 302, Gas mixing distributor; 303, Multi-channel reversing valve group; 304, Pressure sensor; 400, Monitoring module; 401, In-situ optical monitoring unit; 402, Raman spectrometer; 500, Control module. Detailed Implementation

[0017] The technical solution of the present invention will now be described with reference to the accompanying drawings.

[0018] In embodiments of the present invention, words such as "exemplarily," "for example," etc., are used to indicate that something is an example, illustration, or description. Any embodiment or design described as "exemplary" in the present invention should not be construed as being more preferred or advantageous than other embodiments or designs. Specifically, the use of the word "exemplary" is intended to present the concept in a concrete manner. Furthermore, in embodiments of the present invention, the meaning expressed by "and / or" can be both, or either one.

[0019] In the embodiments of this invention, the terms "image" and "picture" may sometimes be used interchangeably. It should be noted that, without emphasizing the distinction between them, they convey the same meaning. Similarly, the terms "of," "corresponding (relevant)," and "corresponding" may sometimes be used interchangeably. It should be noted that, without emphasizing the distinction between them, they convey the same meaning.

[0020] In this embodiment of the invention, sometimes a subscript such as W1 may be written in a non-subscript form such as W1. When the difference is not emphasized, the meaning they express is the same.

[0021] To make the technical problems, technical solutions and advantages of the present invention clearer, a detailed description will be given below in conjunction with the accompanying drawings and specific embodiments.

[0022] Please see Figure 1 This invention provides a carbon nanotube array fabrication system, comprising a multi-channel reaction module 100, a material transfer module 200, a gas supply module 300, a monitoring module 400, and a control module 500. The multi-channel reaction module 100 includes at least two reaction chambers 102, each chamber 102 accommodating a substrate and providing an independent process environment. The material transfer module 200 loads the substrate into each reaction chamber 102 and removes the processed substrate from each chamber 102. The gas supply module 300 is connected to the multi-channel reaction module 100 and independently supplies the process gases required for the reaction to each reaction chamber 102. The monitoring module 400 monitors the material growth process within each reaction chamber 102. The control module 500 is communicatively connected to the multi-channel reaction module 100, the material transfer module 200, the gas supply module 300, and the monitoring module 400 to receive data collected by the monitoring module 400 and independently control the process parameters of each reaction chamber 102.

[0023] The aforementioned system architecture integrates traditionally isolated material preparation, transport, monitoring, and control functions into a cohesive whole. The multi-channel reaction module 100 provides a parallel experimental platform, the material transfer module 200 and the gas supply module 300 ensure the precision and independence of process execution, while the monitoring module 400 and the control module 500 endow the system with the ability to "sense" and "think." This integrated and modular design not only lays the foundation for high-throughput experiments but, more importantly, provides the physical architecture for realizing real-time sensing and intelligent control of the growth process, making intelligent material preparation, moving from "experience-based trial and error" to "data-driven" methods, possible.

[0024] This embodiment overcomes the bottleneck of high-throughput preparation, significantly improving R&D and production efficiency. Employing a distributed gas path design of "main pipeline - multiple branch pipelines" and at least two reaction chambers 102, multiple sets of differentiated process parameters can be explored simultaneously in a single batch, increasing R&D efficiency by over 80%. Simultaneously, it supports the large-scale simultaneous preparation of multiple samples in the same batch, improving production efficiency by more than 5 times compared to traditional processes, meeting the needs of rapid material iteration and industrial mass production.

[0025] Please see Figure 2 and Figure 3 Optionally, the multi-channel reaction module 100 includes several independent reaction chamber bodies 101. Each reaction chamber body 101 is provided with a reaction chamber 102, a heating unit 103, a cooling unit 104, a temperature sensor 105, at least one observation window 106, and a gas passage 107. The reaction chamber body 101 can be integrally molded, for example, and the molding material can be selected according to the temperature resistance requirements. The molding material can be, for example, quartz glass, which has a maximum temperature resistance of 1200°C.

[0026] In this embodiment, the heating unit 103 is used to heat the reaction environment in the reaction chamber 102. It can be a resistance heating wire or heating strip surrounding the outer wall of the reaction chamber 102, or an infrared heater set at the bottom of the reaction chamber 102. Its power can be precisely adjusted by the control module 500 according to the feedback of the temperature sensor 105, so as to achieve rapid rise and fall and high-precision stable control of the temperature field in the reaction chamber.

[0027] The cooling unit 104 is used to cool the reaction chamber body 101. For example, water cooling can be used to cool the reaction chamber body 101. A circulating water path is set inside the reaction chamber body 101 and an interface for the circulating water path is set on it. The cooling unit 104 ensures that the temperature of the outer wall of the reaction chamber body 101 is lower than a set threshold (e.g., 40°C) to ensure operational safety.

[0028] Temperature sensor 105 is used to monitor the temperature of reaction chamber 102. To achieve controllable initial temperature in the reaction chamber, the temperature sensor 105 can monitor the temperature in real time, and based on the monitoring results and process requirements, control heating unit 103 and / or cooling unit 104 to achieve precise temperature adjustment within reaction chamber 102. Monitoring module 400 monitors the material growth process within reaction chamber 102 through observation window 106. Observation window 106 is made of high-transmittance glass and can be integrally machined during the processing of reaction chamber body 101. Gas passage 107 connects gas supply module 300 and reaction chamber 102, thereby allowing gas to be introduced into reaction chamber 102.

[0029] In this embodiment, the heating unit 103, cooling unit 104, temperature sensor 105, and gas passage 107 are disposed inside the reaction chamber body 101, therefore... Figure 3 The figure does not show the interface. The cooling unit 104, being water-cooled, has its interface A, the interface of the circulating water path, exposed on the outer wall of the reaction chamber body 101, visible in the figure. The gas passage 107 can also be configured as follows: a gas passage 107 is provided on the support that holds the base positioning crucible 201 (described below), allowing the reaction gas to be introduced from the end of the reaction chamber 102; the gas interface B, exposed on the support of the base positioning crucible 201, is visible in the figure.

[0030] Please see Figure 4 Optionally, the material transfer module 200 includes a base positioning crucible 201, a loading execution unit 202, and a linear motion unit 203. Structural diagrams of the base positioning crucible 201 and the linear motion unit 203 can be found in [reference needed]. Figure 3 .

[0031] The substrate positioning crucible 201 is used to support and position the substrate, and one or two substrate positioning crucibles 201 are provided for each reaction chamber 102. Generally, one substrate positioning crucible is provided for each reaction chamber 102 to ensure an independent process environment; however, in some scenarios where efficiency is desired, multiple crucibles can be used. Figure 2 The structure includes two base positioning crucibles 201 for each reaction chamber 102, which can further increase the number of products generated in a single run. The specific number can be selected as needed.

[0032] The loading execution unit 202 is used to transfer the substrate onto or remove it from the substrate positioning crucible 201. The execution unit is primarily used for transferring the substrate positioning crucible 201. Optionally, the loading execution unit 202 is a multi-axis manipulator, and the end effector of the multi-axis manipulator is a vacuum suction head. The multi-axis manipulator includes an X-axis drive module, a Y-axis drive module, and a Z-axis conventional module, enabling movement in any direction within space; combined with the vacuum suction head, it facilitates the transfer of the substrate positioning crucible 201.

[0033] The linear motion unit 203 is used to drive the base positioning crucible 201 to move linearly, so as to send the base positioning crucible 201 into or out of the reaction chamber 102. To achieve more precise linear movement, the linear motion unit 203 may optionally be a lead screw and nut transmission mechanism, which drives the lead screw to rotate through a servo motor, thereby driving the base positioning crucible 201 fixed on the nut to move precisely to a designated position in the reaction chamber 102 or out.

[0034] Optionally, the process gases include at least a carbon source gas, hydrogen, and an inert gas. The carbon source gas provides carbon atoms for carbon nanotube growth and can be, for example, methane (CH4), ethylene (C2H4), or acetylene (C2H2). Hydrogen (H2) is mainly used to reduce catalyst precursors, activate catalyst particles, and process amorphous carbon generated during the etching reaction, which is crucial for improving the crystallinity of carbon nanotubes. The inert gas, such as argon (Ar), mainly serves as a carrier gas, dilution gas, and protective gas, used to purge air before the reaction, maintain stable reaction pressure, and protect the sample from cooling after the reaction.

[0035] Please see Figure 5 The gas supply module 300 includes a multi-channel mass flow controller 301, a gas mixing distributor 302, a multi-channel reversing valve assembly 303, and a pressure sensor 304. The multi-channel mass flow controller 301 is used for independent flow control of multiple process gases; the input of the gas mixing distributor 302 is connected to the output of the multi-channel mass flow controller 301, and it is used to mix multiple controlled gases to form a mixed gas; the input of the multi-channel reversing valve assembly 303 is connected to the output of the gas mixing distributor 302, and its multiple outputs are respectively connected to each reaction chamber 102, used to selectively deliver the mixed gas to the target reaction chamber 102; the pressure sensor 304 is installed in the pipeline of the gas supply module 300, and is used to monitor gas pressure.

[0036] The aforementioned gas path structure enables "centralized control and independent distribution" from the gas source to each reaction chamber 102. The multi-channel mass flow controller 301 acts as a "precise metering hand," setting precise flow rates for each gas. The gas mixing distributor 302 ensures thorough and uniform mixing of various gases, forming a stable reaction gas source. The multi-channel reversing valve assembly 303 functions as a "smart switch," distributing the mixed gas independently and on demand to designated reaction chambers 102. The pressure sensor 304 monitors pipeline pressure in real time, providing feedback for safe operation and closed-loop flow control. This system collectively ensures that each reaction chamber 102 receives an independent, stable, and precisely controllable gas atmosphere, which is crucial for multi-parameter high-throughput screening and controllable preparation.

[0037] Optionally, the gas supply module 300 may also include a switch for controlling the on / off state of the gas supply, a gas filter, etc. The switch can be used to directly control the on / off state of the gas supply; the gas filter is used to pre-treat the gas, filtering out minute impurities or moisture from the gas source. If the gas source itself has already been treated, this component is not required.

[0038] Please see Figure 6 Optionally, the monitoring module 400 includes an in-situ optical monitoring unit 401 and a Raman spectrometer 402. The in-situ optical monitoring unit 401 is used for real-time optical imaging of the material growth process within the reaction chamber 102; the Raman spectrometer 402 is used for real-time Raman spectral acquisition of the material growth process within the reaction chamber 102. The in-situ optical monitoring unit 401 and the Raman spectrometer 402 constitute a comprehensive in-situ monitoring system covering both macroscopic morphology and microstructure. The in-situ optical monitoring unit 401 acts like an "eye," observing the morphological evolution of the array's height, density, and uniformity in real time to determine whether the growth rate is normal. The Raman spectrometer 402 acts like a "stethoscope," analyzing the vibrational spectra of carbon atoms to diagnose the intrinsic structural information of carbon nanotubes, such as crystal quality and defect density, in real time. The synchronous operation of both allows for comprehensive capture of growth dynamics, providing a comprehensive and in-depth decision-making basis for subsequent intelligent feedback control, and is the core of realizing "structure-performance" correlation modeling.

[0039] Please see Figure 7 The present invention also provides a method for preparing a carbon nanotube array, which is applied to the above-mentioned carbon nanotube array preparation system and specifically includes steps S701 to S705.

[0040] Step S701: After loading the substrate, send it into each reaction chamber 102 and set independent process parameters for each reaction chamber 102.

[0041] In this step, the substrate can be prepared first. For example, a coated silicon wafer can be used as the substrate. It is first placed in an acetone solution for ultrasonic cleaning for 10 minutes to remove surface oil and impurities, and then transferred to an ethanol solution for ultrasonic cleaning for 10 minutes to further purify the substrate surface. After cleaning, it is placed in a 60°C constant temperature oven for drying for 30 minutes to ensure that there is no residual solvent on the substrate surface. Then, the dried substrate is placed on a substrate placement stage, which is similar to a transfer station for temporarily placing the dried substrate or the substrate that has participated in the growth reaction.

[0042] After loading the substrate, it is sent into each reaction chamber 102. For example, it may include: first, using the cooperation of a multi-axis manipulator and a vacuum suction head, picking up the substrate and transferring it to the substrate positioning crucible 201, and then using a linear motion unit 203 to send the substrate positioning crucible 201 and the substrate together into the reaction chamber 102.

[0043] Independent process parameters can be set for each reaction chamber 102. For example, the operator can set the process parameters of each reaction chamber 102 (such as reaction temperature, flow rate of each reaction gas, growth time, etc.) on the control unit through the human-machine interface.

[0044] Step S702: Purge each reaction chamber 102 with inert gas and heat it to the set temperature. The purpose of purging is to remove air, especially oxygen and water vapor, from the reaction chamber 102 to prevent them from oxidizing the substrate or catalyst at high temperatures or introducing unnecessary side reactions. Specifically, the control module 500 controls the gas supply module 300 to open the argon gas pipeline and continuously purge each reaction chamber 102 with argon gas at a set flow rate (e.g., 100 sccm) for 5 minutes. At the same time, the heating unit 103 starts working and heats each reaction chamber 102 to the target reaction temperature (e.g., 800℃) according to the preset heating rate. Purging and heating can be performed simultaneously to improve efficiency; until the temperature stabilizes and purging is completed.

[0045] Step S703: Process gas is introduced into each reaction chamber 102 to initiate the growth of carbon nanotube arrays, and real-time monitoring is performed during the growth process. According to preset parameters, the control system controls the gas supply module 300 to introduce carbon source gas (such as methane) and hydrogen in a set ratio while maintaining argon gas. For example, the methane flow rate is set to 30 sccm, and the hydrogen flow rate is set to 100 sccm. At this time, the carbon source gas begins to decompose and grow carbon nanotube arrays under the action of high temperature and catalyst. Simultaneously, the monitoring module 400 starts working: the in-situ optical monitoring unit 401 captures high-resolution images of the samples in the chamber at a fixed frequency (e.g., every 5 minutes); the Raman spectrometer 402 irradiates the growing array with laser light through a fiber optic probe and observation window 106 and collects its Raman scattering signal. Both monitoring data are collected synchronously and transmitted to the control module 500.

[0046] Step S704: Based on the real-time monitoring results, dynamically adjust the process parameters of the corresponding reaction chamber 102. The algorithm built into the control module 500 compares and analyzes the real-time monitoring data with the preset "target range". This process is repeated cyclically during the growth period, realizing dynamic, closed-loop process control based on real-time status.

[0047] Step S705: After growth is complete, the reaction chamber 102 is cooled and the substrate is removed. In this step, the electromagnetic reversing valve corresponding to the carbon source gas in the gas supply module 300 is first closed to stop the carbon source supply; at the same time, argon gas is continuously supplied to provide an inert protective atmosphere for the reaction chamber. The heating unit 103 reduces its power until it is turned off, and is gradually cooled to room temperature under argon protection. During the cooling process, the pressure sensor 304 and the flow monitoring unit continue to work to ensure that the pressure in the reaction chamber 102 is stable and to avoid pressure fluctuations damaging the array structure.

[0048] After cooling to room temperature, the action of removing the substrate is exactly the opposite of the action of placing it in. First, the substrate is removed from the reaction chamber 102 by the linear motion unit 203, and then the substrate is transferred to the designated position (e.g., substrate placement stage) by the multi-axis robot.

[0049] Optionally, real-time monitoring includes real-time optical imaging of the growth process via in-situ optical monitoring unit 401; and dynamic adjustment of the process parameters of the corresponding reaction chamber 102, including adjusting the carbon source gas flow rate and / or reaction temperature of the corresponding reaction chamber 102 based on the optical imaging information. The optical imaging information directly reflects the macroscopic kinetics of the array growth. Through image processing techniques (such as edge detection), the average height of the array and its rate of change over time (growth rate) can be calculated in real time. When the system determines that the growth rate of a certain chamber is below the lower limit of the target range, it indicates insufficient carbon atom supply or reaction activation energy. At this time, the control module 500 will prioritize fine-tuning the carbon source gas flow rate of that chamber to directly increase the reactant concentration; if adjusting the flow rate is ineffective, it may be due to insufficient catalyst activity caused by a low temperature, and the system will further slightly increase the set temperature of that chamber. This direct feedback based on morphology effectively ensures the uniformity of array growth and the target height.

[0050] Optionally, real-time monitoring includes real-time Raman spectral acquisition of the growth process using a Raman spectrometer 402; and dynamic adjustment of the process parameters of the corresponding reaction chamber 102, including adjusting the hydrogen flow rate of the corresponding reaction chamber 102 based on the Raman spectral information. The G peak (approximately 1580 cm⁻¹) in the Raman spectrum corresponds to the in-plane vibration of sp² hybridization of carbon atoms, and the D peak (approximately 1350 cm⁻¹) is associated with defects and disordered structures. The intensity ratio of the G peak to the D peak (Ig) is... G / I DRaman spectroscopy is a key indicator for evaluating the degree of graphitization and crystallinity quality of carbon nanotubes. When the real-time acquired Raman spectrum shows I... G / I D When the ratio is lower than the preset target (e.g., <1.8), it indicates that the carbon nanotubes grown in the reaction channel have more defects and the crystal quality is reduced. This is usually related to excessive amorphous carbon byproducts generated during the reaction. In response, the control module 500 will increase the hydrogen flow rate in the chamber, because hydrogen can effectively etch amorphous carbon, purify the growth environment, and thus guide carbon atoms to arrange themselves more orderly, improving the crystal quality of the product.

[0051] Optionally, the process parameters of the corresponding reaction chamber 102 are dynamically adjusted, including: comparing the information obtained from real-time monitoring with a preset target range; when the information deviates from the preset target range, adjusting the process parameters according to the preset adjustment range. To ensure the accuracy and safety of the control, the dynamic adjustment of this system is not unlimited. The control module 500 provides settings for each monitoring parameter (such as growth rate, I...). G / I D Each adjustable process parameter (such as gas flow rate and temperature) has a preset "target range" and "adjustment range". For example, the target range for the growth rate is 5-10 μm / min, and the single increase in carbon source flow rate during adjustment should not exceed 10 sccm. When the monitoring information deviates from the target range, the system does not abruptly adjust to the limit value, but calculates and executes the optimal adjustment amount within the preset adjustment range. This avoids process instability caused by over-adjustment, ensures the smoothness, reliability, and repeatability of the closed-loop control process, and is an important guarantee for achieving stable and consistent preparation.

[0052] In the three embodiments described above, the first embodiment uses an optical monitoring unit to monitor and regulate the growth process; the second embodiment uses a ray spectrometer to monitor and regulate the growth process; and the third embodiment demonstrates that during the regulation process, adjustments can be made according to some preset parameters, thus avoiding the introduction of complex algorithms and making the regulation process faster.

[0053] Taking the in-situ optical monitoring unit 401 as an example, data can be collected synchronously at a frequency of once every 5 minutes. The in-situ optical monitoring unit 401 captures growth images through the observation window 106 and compares the monitored values ​​with preset thresholds. If the array height growth rate is lower than the preset value, it is determined that the carbon source supply is insufficient or the temperature is too low. The control system sends a command to the gas supply module 300 to increase the carbon source gas flow rate of the corresponding channel by 5%-10%, or sends a temperature command to the heating unit 103 to raise the temperature by 5-10°C, until the height growth rate returns to the target range.

[0054] Taking the Raman spectrometer 402 as an example, data can be collected synchronously at a frequency of once every 5 minutes. The Raman spectrometer captures the Raman spectrum emitted during the growth of the carbon nanotube array through the observation window 106. If the intensity ratio of the G peak to the D peak in the Raman spectrum is <1.8, it indicates insufficient crystallinity and is determined to be due to an unstable reaction atmosphere. Hydrogen flow compensation is then activated to increase the hydrogen flow rate by 3%-5%, and the etching effect of hydrogen is used to improve the crystal quality. At the same time, the heating unit 103 is finely adjusted to maintain a stable temperature field.

[0055] In summary, this invention successfully integrates high-throughput parallel fabrication technology with in-situ real-time monitoring and feedback technology through modular integration of hardware systems and intelligent closed-loop control of software algorithms. This not only significantly improves the R&D and production efficiency of carbon nanotube arrays but also fundamentally changes their fabrication mode from "open-loop, experience-driven" to "closed-loop, data-driven." This approach can accurately establish the mapping relationship between "process parameters - microstructure - macroscopic performance," enabling proactive and precise control of the material growth process and final performance. It provides a new and powerful technological platform for the rapid development and large-scale manufacturing of high-performance, highly consistent carbon nanotube array thermal interface materials.

[0056] It should be understood that the term "and / or" in this article is merely a description of the relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, A and B existing simultaneously, or B existing alone. A and B can be singular or plural. Additionally, the character " / " in this article generally indicates an "or" relationship between the preceding and following related objects, but it can also represent an "and / or" relationship. Please refer to the context for a more accurate understanding.

[0057] In this invention, "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of a single item or a plurality of items. For example, at least one of a, b, or c can represent: a, b, c, ab, ac, bc, or abc, where a, b, and c can be a single item or multiple items.

[0058] It should be understood that, in various embodiments of the present invention, the order of the above-mentioned process numbers does not imply the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present invention.

[0059] Those skilled in the art will recognize that the units and algorithm steps of the various examples described in conjunction with the embodiments disclosed herein can be implemented in electronic hardware, or a combination of computer software and electronic hardware. Whether these functions are implemented in hardware or software depends on the specific application and design constraints of the technical solution. Those skilled in the art can use different methods to implement the described functions for each specific application, but such implementations should not be considered beyond the scope of this invention.

[0060] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the specific working processes of the devices, apparatuses, and units described above can be referred to the corresponding processes in the foregoing method embodiments, and will not be repeated here.

[0061] In the several embodiments provided by this invention, it should be understood that the disclosed devices, apparatuses, and methods can be implemented in other ways. For example, the apparatus embodiments described above are merely illustrative; for instance, the division of units is only a logical functional division, and in actual implementation, there may be other division methods. For example, multiple units or components may be combined or integrated into another device, or some features may be ignored or not executed. Furthermore, the coupling or direct coupling or communication connection shown or discussed may be through some interfaces; the indirect coupling or communication connection between devices or units may be electrical, mechanical, or other forms.

[0062] The units described as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of this embodiment according to actual needs.

[0063] In addition, the functional units in the various embodiments of the present invention can be integrated into one processing unit, or each unit can exist physically separately, or two or more units can be integrated into one unit.

[0064] If the aforementioned functions are implemented as software functional units and sold or used as independent products, they can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of this invention, or the part that contributes to the prior art, or a part of the technical solution, can be embodied in the form of a software product. This computer software product is stored in a storage medium and includes several instructions to cause a computer device (which may be a personal computer, server, or network device, etc.) to execute all or part of the steps of the methods described in the various embodiments of this invention. The aforementioned storage medium includes various media capable of storing program code, such as USB flash drives, portable hard drives, read-only memory (ROM), random access memory (RAM), magnetic disks, or optical disks.

[0065] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A carbon nanotube array fabrication system, characterized in that, The system includes: A multi-channel reaction module comprising at least two reaction chambers, each of which is used to contain a substrate and provide an independent process environment; A material transfer module is used to load the substrate into each reaction chamber and to remove the processed substrate from each reaction chamber; The gas supply module is connected to the multi-channel reaction module and is used to independently supply the process gas required for the reaction to each reaction chamber. A monitoring module is used to monitor the material growth process within each reaction chamber. The monitoring module includes an in-situ optical monitoring unit and a Raman spectrometer. The in-situ optical monitoring unit is used for real-time optical imaging of the material growth process within the reaction chamber, and the Raman spectrometer is used for real-time Raman spectral acquisition of the material growth process within the reaction chamber. The control module is communicatively connected to the multi-channel reaction module, the material transfer module, the gas supply module, and the monitoring module to receive data collected by the monitoring module and independently control the process parameters of each reaction chamber. The control module is configured as follows: Receive optical imaging information collected by the in-situ optical monitoring unit and Raman spectral information collected by the Raman spectrometer; Based on the optical imaging information, adjust the carbon source gas flow rate and / or reaction temperature of the corresponding reaction chamber; Based on the Raman spectral information, the hydrogen flow rate in the corresponding reaction chamber is adjusted.

2. The carbon nanotube array fabrication system according to claim 1, characterized in that, The multi-channel reaction module includes several independent reaction chamber bodies, each of which is equipped with: A reaction chamber; A heating unit is used to heat the reaction environment in the reaction chamber; A cooling unit is used to cool the main body of the reaction chamber; A temperature sensor is used to monitor the temperature of the reaction chamber; At least one observation window, through which the monitoring module monitors the material growth process within the reaction chamber; as well as A gas passage is provided for connecting the gas supply module and the reaction chamber.

3. The carbon nanotube array fabrication system according to claim 1, characterized in that, The material transfer module includes: A substrate positioning crucible is used to support and position the substrate, and one or two substrate positioning crucibles are provided for each reaction chamber. A loading execution unit is configured to transfer the substrate onto or remove it from the substrate positioning crucible; and A linear motion unit is used to drive the base positioning crucible to move linearly, so as to send the base positioning crucible into or out of the reaction chamber.

4. The carbon nanotube array fabrication system according to claim 3, characterized in that, The loading execution unit is a multi-axis manipulator, and the end effector of the multi-axis manipulator is a vacuum suction head; the linear motion unit is a lead screw and nut transmission mechanism.

5. The carbon nanotube array fabrication system according to claim 1, characterized in that, The process gas includes at least a carbon source gas, hydrogen, and an inert gas; The gas supply module includes: A multi-channel mass flow controller is used for independent flow control of various process gases; A gas mixing distributor, whose input is connected to the output of the multi-channel mass flow controller, is used to mix multiple controlled gases to form a mixed gas; A multi-way reversing valve assembly, with its input connected to the output of the gas mixer distributor and its multiple outputs respectively connected to each reaction chamber, is used to selectively deliver the mixed gas to the target reaction chamber; and A pressure sensor is installed in the pipeline of the gas supply module to monitor gas pressure.

6. A method for preparing a carbon nanotube array, characterized in that, The method, applied to the carbon nanotube array fabrication system as described in any one of claims 1 to 5, comprises: After the substrate is loaded, it is sent into each reaction chamber, and independent process parameters are set for each reaction chamber. Inert gas is introduced into each reaction chamber to purge it, and the chambers are heated to the set temperature. Process gases are introduced into each reaction chamber to initiate the growth of carbon nanotube arrays, and real-time monitoring is performed during the growth process. Based on the results of the real-time monitoring, the process parameters of the corresponding reaction chamber are dynamically adjusted; After growth is complete, the reaction chamber is cooled and the substrate is removed.

7. The method for preparing carbon nanotube arrays according to claim 6, characterized in that, Dynamically adjust the process parameters of the corresponding reaction chamber, including: The information obtained from real-time monitoring is compared with the preset target range; When the information deviates from the preset target range, the process parameters are adjusted according to the preset adjustment range.

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