Process and device for preparing silicon-carbon negative electrode material by using low-temperature plasma

Abstract

The invention provides a process and a device for preparing a silicon-carbon negative electrode material by using low-temperature plasma, which are characterized in that an organic silicon precursor is easy to form plasmas of silicon and silicon oxide in a plasma state, and in the adsorption process of porous carbon, the silicon-based plasmas are subjected to chemical reaction with carbon at a lower energy level so as to be tightly combined with the carbon. Proper reaction conditions and precursor concentration are controlled, so that the diffusion speed of molecules into the porous carbon and the silicon-carbon combination speed are adjustable, the silicon and the carbon can be tightly combined in the porous carbon, and micropores of the carbon are not blocked. The key to form the optimal silicon-carbon ratio without influencing the expansion coefficient is to select the proper pore size of the porous carbon and control the adsorption rate and the reaction rate. According to the device, the boiling bed and the low-temperature plasma are integrated, so that continuous and large-scale production is realized. The process solves the problems encountered by the conventional process, and realizes low cost, low power consumption, and controllable and adjustable product microstructure and components. In order to realize the target of the process, the invention also provides a preparation device.

Description

Technical Field

[0001] This invention relates to a process and apparatus for plasma-assisted preparation of silicon-carbon anode materials under low-temperature conditions, belonging to the field of lithium-ion battery material technology development. Background Technology

[0002] Improving energy density is one of the key directions in the development of lithium battery materials. Silicon-carbon anode materials have two times or more higher energy density than pure carbon anodes, making them ideal anode materials without altering existing processes, and they are also suitable for solid-state batteries. Currently, the industry has developed multiple technical routes for the preparation of silicon-carbon anode materials. The following are some common existing preparation methods:

[0003] Chemical vapor deposition (CVD): Currently a mainstream commercially available technology. It involves depositing silane (SiH4) gas inside porous carbon materials to form uniform nano-silicon particles, which are then coated with a carbon layer. Silicon-carbon anode materials prepared using this method have advantages such as high specific capacity, high initial efficiency, and excellent cycle performance; however, CVD suffers from high energy consumption and cost, complex processes, safety hazards, and environmental pollution.

[0004] Physical mixing method: One of the traditional methods, which involves mixing silicon powder with carbon powder (such as graphite) through physical means such as ball milling and grinding. However, this method is difficult to guarantee the uniformity of silicon particle size and has relatively poor cycle performance.

[0005] Sol-gel method and electrospinning method: These methods can produce silicon-carbon composite fibers or particles with more controllable structures, but the process is relatively complex and the cost is high.

[0006] Physical mixing is simple and low-cost, but it is limited by the expansion of silicon and cannot achieve a higher silicon-to-carbon ratio. Chemical vapor deposition (CVD) produces high-performance products but is expensive. Catalytic cracking has the advantages of high efficiency and low cost, but it brings great trouble to the purification of products. The low-temperature plasma method involved in this invention can realize the preparation of silicon-carbon anode materials with low cost and low energy consumption, and the microstructure and composition ratio are easy to control. Summary of the Invention

[0007] The main objective of this invention is to prepare silicon-carbon anode materials using low-temperature plasma technology, achieving low energy consumption, low investment, and a higher silicon-to-carbon ratio.

[0008] The proportions of silicon oxide, silicon suboxide, silicon carbide, and silicon can be adjusted under different operating conditions and using different precursors.

[0009] As attached Figure 1The process shown is as follows: 1. Material tank; 2. Processing device for low-temperature plasma preparation of silicon-carbon anode materials; 3. Cyclone separator; 4. Tail gas spray device; 5. Spray water circulation treatment device; 6. Cyclone separator discharge; 7. Slag discharge port of plasma processing device; 8. Ultrasonic vibration device; 9. Cooling circulation system; 10. Plasma generating device; 8 / 9 / 10 Low-temperature plasma generator fixing bracket; 11. Pneumatic distribution device; 12. Negative pressure gauge and thermometer; 13. Top cover plate of equipment; 14. Main body of equipment; 15. Ceramic filter plate or polymer material filter plate; 16. Viewing window; 17. Insulating partition; 18. Feed port; 19. Discharge port; 20. Flange; 21. Cavity; 22. Bottom cover plate of equipment; 23. Low-temperature plasma tube; 24. Outer shell of low-temperature plasma generating tube assembly; 25. External electrode of low-temperature plasma generator; 26. External quartz tube of low-temperature plasma generator; 27. Generation and material gap of low-temperature plasma generator; 28. Internal quartz tube of low-temperature plasma generator; 29. ​​Internal electrode of low-temperature plasma generator; 30. Quartz bracket of low-temperature plasma generator; 31. Flange of low-temperature plasma generator.

[0010] In the equipment system, product quality control and large-scale production can be achieved by connecting multiple power sources (multiple discharge tubes) in parallel and series.

[0011] This invention provides a process for preparing silicon-carbon anode materials using low-temperature plasma, and also provides an apparatus for preparing silicon-carbon anode materials using low-temperature plasma.

[0012] One of the processes for preparing silicon-carbon anode materials by low-temperature plasma mainly includes a material tank, a processing device for preparing silicon-carbon anode materials by low-temperature plasma, a cyclone separator, a spray system and other devices.

[0013] In some embodiments, raw materials are placed in a material tank and fed into a processing device for preparing silicon-carbon anode materials by a screw conveyor.

[0014] In some embodiments, the distribution of plasma states is more stable and uniform under vacuum conditions. The processing device for preparing silicon-carbon anode materials by low-temperature plasma is in a vacuum state throughout the process. The positive and negative electrodes are connected to an external plasma generating device through a pipeline to ensure that a stable plasma (field) state is formed between the positive and negative electrodes.

[0015] In some embodiments, the tank is equipped with a pneumatic distribution device. After the raw material enters the device, it is blown into the internal channel by the pneumatic distribution device. Silicon-carbon bonding is formed by the plasma electric field. After controlling the appropriate time, it enters the cyclone separator.

[0016] In some embodiments, the material is processed in a circulating manner to achieve the boiling (bed) effect in the equipment. Due to the layout of the equipment and the characteristics of the raw materials, there may be a problem that the material cannot be circulated. Therefore, an ultrasonic vibration device is provided to vibrate for a long time or at regular intervals so that the material can continue to circulate.

[0017] In some embodiments, the release of plasma from the electrode generates heat, so a cooling circulation device is installed to reduce electrode heating and reduce the impact on materials.

[0018] In some embodiments, in order to prevent blockage of a single pipe and maximize cooling effect and output, the electrodes are arranged in a three- or multiple triangular or various polygonal layouts.

[0019] In some embodiments, the cyclone separator not only releases the finished product but also separates and discharges exhaust gas. After separation, the finished product is packaged and shipped out after passing inspection, while the exhaust gas enters the spray system for treatment.

[0020] In some embodiments, the spraying system is provided with an exhaust gas spraying device and a spray water circulation treatment device. The exhaust gas enters the exhaust gas spraying device and is mixed with a preset solvent through the spray head to meet the standard before being recycled or treated.

[0021] In some embodiments, the spray water recycling treatment device is responsible for collecting the mixed solution in the exhaust gas spray device for treatment, while purifying the solution. After the waste liquid is separated, the qualified solution is recycled, while the waste liquid is discharged for treatment.

[0022] One type of equipment for preparing silicon-carbon anode materials by low-temperature plasma includes a low-temperature plasma generator, a discharge medium, a coolant, a vacuum container, a container cover, a low-temperature plasma generator fixing bracket, an ultrasonic vibration device, a ceramic filter plate or a polymer filter plate, a gas distribution device, a negative pressure gauge, a temperature gauge, and other sensors.

[0023] The low-temperature plasma generator consists of a positive electrode tube and a negative electrode tube, a quartz dielectric tube, an insulating partition, a cooling circulation device, a coolant, a material chamber, and electrode leads.

[0024] In some embodiments, the electrodes are inserted in a tube-like manner, with two quartz dielectric tubes inserted as a material cavity, allowing the material to pass through the gap in the middle of the quartz dielectric tubes, ensuring normal plasma release and normal material passage. The two quartz dielectric tubes should be placed in a concentric circle-like position.

[0025] In some embodiments, multiple support columns are used to fix the two quartz media tubes to ensure stability and form a material channel.

[0026] In some embodiments, the positive and negative electrodes are composed of two mirrored stainless steel tubes, with the outer electrode of the low-temperature plasma generator being the inner wall mirror of the tube and the inner electrode being the outer wall mirror of the tube.

[0027] In some embodiments, the outer pipe wall is provided with multiple flanges for connecting insulating partitions;

[0028] In some embodiments, the positive and negative electrode groups consist of three or more groups. Multiple electrode groups are connected by insulating partitions and stainless steel pipe flanges. At the same time, the insulating partitions serve as coolant isolation plates to isolate coolant from materials. To ensure maximum coolant efficiency, the electrode tubes adopt a triangular or polygonal layout.

[0029] In some embodiments, to prevent material from adhering to the electrodes, all electrode tubes are cut at a 45-degree angle to ensure the smooth drop of material, and ultrasonic vibration (timed or continuous operation) is added.

[0030] In some embodiments, the low-temperature plasma generator is placed at the center of the container and fixed to the center of the container using three or more low-temperature plasma generator fixing brackets. Positive and negative power lines, one or more inlet and outlet pipes, inlet and outlet coolant pipes, sampling pipes, and ultrasonic vibration devices are inserted into the corresponding low-temperature plasma generator fixing brackets.

[0031] In some embodiments, the raw materials of silicon-carbon anode material are micron-sized to prevent the raw materials of silicon-carbon anode material from being sucked out during the vacuum process. A ceramic filter plate or a polymer filter plate is placed between the container and the container cover to achieve gas-solid separation and remove by-product exhaust gas.

[0032] In some embodiments, silicon-carbon anode material raw materials are blown into the low-temperature plasma generator by a pneumatic distribution device, with one or more pneumatic distribution devices installed at the bottom of the container.

[0033] In some embodiments, multiple sensors, such as negative pressure gauges and temperature gauges, are designed to observe the vacuum level and temperature inside the device. Attached Figure Description

[0034] Figure 1 A process flow diagram for the low-temperature plasma preparation of silicon-carbon anode materials.

[0035] Figure 2 A processing device for preparing silicon-carbon anode materials by low-temperature plasma.

[0036] Figure 3 A cross-sectional view of a processing apparatus for preparing silicon-carbon anode materials by low-temperature plasma.

[0037] Figure 4 A schematic diagram of an electrode for a processing device used in low-temperature plasma preparation of silicon-carbon anode materials. Detailed Implementation

[0038] The raw materials are placed in a material tank 1, and a screw conveyor is used to make the raw materials enter the processing device for low-temperature plasma preparation of silicon-carbon anode materials through the feed port 18. The processing device for low-temperature plasma preparation of silicon-carbon anode materials is equipped with an ultrasonic vibration device 8, a cooling circulation system 9, a plasma generator 10, and a pneumatic distribution device 11.

[0039] Since the materials are fused by plasma, and since the 10 plasma generator is too large, the processing device for preparing silicon-carbon anode materials by low-temperature plasma in the 2 low-temperature plasma is only equipped with 23 low-temperature plasma tubes for releasing plasma. The internal part is connected to the external part by wiring, and the wiring is accessed by the 8 / 9 / 10 low-temperature plasma generator fixing bracket.

[0040] 8. Ultrasonic vibration devices mainly prevent materials from getting stuck by long-term or timed vibration;

[0041] Since plasma release requires a vacuum environment, vacuum pumping and venting interfaces are provided on the cover plate of device 13; instruments such as a negative pressure gauge and a temperature gauge are also provided on the main body of device 14; at the same time, in order to observe the material in chamber 21, a viewing window is added to the main body of device 14.

[0042] The top cover plate of equipment 13 and the bottom cover plate of equipment 22 are connected to the main body of equipment 14 by flanges. Since the silicon-carbon anode material is micron-sized, in order to prevent the material from being drawn away during vacuuming, venting, or exhausting, a ceramic filter plate or a polymer filter plate is placed between the top cover plate of equipment 13 and the main body of equipment 14.

[0043] The low-temperature plasma tube assembly consists of an insulating partition (17), a low-temperature plasma tube (23), a flared end (20), and a shell (24). The low-temperature plasma tube (23) is composed of an external electrode (25), an external quartz tube (26), a material gap (27), an internal quartz tube (28), and an internal electrode (29). The low-temperature plasma generator uses two insulating partitions (17) to fix the low-temperature plasma tube (23). Two positions of the insulating partitions (17) are located near the top and bottom of the low-temperature plasma tube (23). The shell (24) encloses both the insulating partitions (17) and the low-temperature plasma tube (23). The insulating partitions (17) and the low-temperature plasma tube (23) are connected by bolts via a flange (31). Similarly, the shell (24) has a similar structure for fixing the insulating partitions (17).

[0044] The gap between the 27 low-temperature plasma generator and the material in the 23 low-temperature plasma tube must be centered on the outer quartz tube of the 26 low-temperature plasma generator, ensuring an 8mm spacing (this spacing can be adjusted based on actual plasma release). To ensure normal plasma release and prevent tip discharge, the inner wall of the outer electrode of the 25 low-temperature plasma generator is mirrored, and similarly, the outer wall of the inner electrode of the 29 low-temperature plasma generator is mirrored. The gap between the 27 low-temperature plasma generator and the material in the 27 low-temperature plasma generator, in addition to accommodating normal plasma release, also allows for the passage of silicon-carbon anode material. As a material channel, to prevent direct contact between the positive and negative electrodes, which could lead to discharge and incorrect plasma release, a 26 low-temperature plasma generator is placed between the outer electrode of the 25 low-temperature plasma generator and the inner electrode of the 29 low-temperature plasma generator. The outer quartz tube of the generator and the inner quartz tube of the 28 low-temperature plasma generator are closely attached to the inner wall of the outer electrode of the 25 low-temperature plasma generator, and the inner quartz tube of the 28 low-temperature plasma generator is closely attached to the outer wall of the inner electrode of the 29 low-temperature plasma generator. The inner electrode of the 29 low-temperature plasma generator at the center of the 23 low-temperature plasma tube needs to ensure the generation of the 27 low-temperature plasma generator and the material gap, so it is fixed by the 30 low-temperature plasma generator quartz bracket. The material gap of a single 27 low-temperature plasma generator may be blocked as a material channel. At the same time, in order to maximize condensation, at least three or more triangular layouts are adopted. Since the device uses the 11 pneumatic distribution device to blow the material into the space between the electrodes, it prevents the material from being blown around in the 21 chamber due to cyclone. The 20 flared opening is installed at the bottom of the low-temperature plasma generator to effectively control the material direction.

[0045] The low-temperature plasma generator is suspended in the center of the 21-cavity chamber. To fix the low-temperature plasma generator, multiple 8 / 9 / 10 low-temperature plasma generator fixing brackets are used. The 8 / 9 / 10 low-temperature plasma generator fixing brackets contain multiple different pipes for different functions.

[0046] To prevent the 23 cryogenic plasma tube from generating heat during plasma release, which could affect discharge efficiency and the normal reaction of materials, a cooling circulation system (9) is used to add coolant between two 17 insulating partitions for heat exchange. To achieve maximum heat exchange efficiency, the 23 cryogenic plasma tube employs a triangular layout. To ensure proper coolant circulation, a circulation pipe is added, divided into inlet and outlet sections, placed within the 8 / 9 / 10 cryogenic plasma generator mounting bracket. Since the 8 / 9 / 10 cryogenic plasma generator mounting bracket is divided into upper and lower parts, the coolant inlet is located at the upper part of the bracket, and the coolant outlet is located at the lower part.

[0047] After the material reaction is complete, open outlet 19 to blow the material into cyclone separator 3. After the material enters cyclone separator 3, open slag discharge port 7 of plasma treatment device to discharge the residue.

[0048] When the material enters the 3-cyclone separator, it carries exhaust gas that is discharged along with it. The 3-cyclone separator separates the material and exhaust gas. After separation, the material is discharged through the bottom outlet.

[0049] The separated exhaust gas is fed into the 4 exhaust gas spray device, where it is neutralized by the corresponding solvent. The treated exhaust gas can be recycled or discharged in compliance with standards.

[0050] The solvent can be recycled. To reduce unnecessary waste, the solvent is sprayed into a 5-spray water circulation treatment device for treatment, separating the qualified solution from the waste liquid. The waste liquid is discharged from the circulation system for treatment, while the qualified solution continues to circulate.

[0051] In summary, the process and apparatus of this invention can significantly reduce production difficulty, effectively improve the finished product performance of silicon-carbon anode materials, and at the same time reduce emissions and minimize harm to the environment and human health.

[0052] Of course, there are other embodiments of the present invention. Without departing from the spirit and essence of the present invention, those skilled in the art can make various corresponding changes according to the present invention, but these corresponding changes should fall within the protection scope of the appended claims of this patent.

Claims

1. A process and apparatus for the production of silicon-carbon anode material by low temperature plasma, characterized in that, The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 2.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma according to claim 1, characterized in that The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 3.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma according to claim 1, characterized in that The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 4.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma according to claim 3, characterized in that The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 5.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma according to claim 3, characterized in that The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 6.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma according to claim 3, characterized in that The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 7.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma according to claim 3, characterized in that The application relates to a low-temperature plasma preparation process for a silicon-carbon negative electrode. 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The application relates to a low-temperature plasma preparation process for a silicon-car 8.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma of claim 7, characterized in that To ensure the highest efficiency of the cooling system of the processing device for preparing silicon-carbon negative electrode material by low-temperature plasma, and to prevent single pipe blockage, the positive and negative electrodes are provided with three or more triangular or polygonal layouts. 9.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma of claim 1, characterized in that The ultrasonic vibration device is used for long-time or timed vibration, the positive and negative electrodes are provided with a conical top to ensure normal circulation of the material and avoid accumulation in dead corners. 10.The process and device for preparing silicon-carbon negative electrode material by low-temperature plasma of claim 1, characterized in that To ensure normal operation of the material, the pneumatic distribution device can blow the material into the positive and negative electrodes, and the bottom of the positive and negative electrodes is provided with a flared structure.

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