A silicon production reactor based on a prying integrated vapor deposition method

Abstract

The utility model discloses a kind of gas deposition method silicon reactors based on pry integrated, including pry block and integrated on the pry block reactor body, hierarchical heating module, air cooling jacket, temperature measurement component, pressure measurement component, pipeline valve instrument and electric control system, the electric control system is respectively connected with the hierarchical heating module, the temperature measurement component and the pressure measurement component and pipeline valve instrument by wire, for receiving temperature, pressure detection signal, and control the output power of the hierarchical heating module and the on-off of pipeline valve, the utility model is evenly distributed by hierarchical heating module and electric control linkage, improve equipment high temperature damage resistance, temperature and pressure control precision and operating safety.

Description

Technical Field

[0001] This invention belongs to the technical field of reactors for preparing silicon-carbon anode materials for lithium batteries, specifically relating to a silicon-preparing reactor based on skid-mounted integrated vapor deposition method. Background Technology

[0002] In the process of preparing silicon-carbon anode materials by chemical vapor deposition, the reactor (also known as a fluidized bed device) is the core device. Its working principle is as follows: solid particles (such as porous carbon skeleton powder) are placed in a container (equipment body) with a perforated distribution plate, and gas flow (such as inert gas or silane mixture) is blown in from the bottom; when the gas flow velocity increases to the point where "the drag force and the particle gravity are in balance", the particles are no longer static, the bed expands and "tumbles like a boiling liquid", forming a fluidized bed. At this time, the specific surface area of ​​the particles increases significantly, and the heat transfer, mass transfer efficiency and reaction rate are greatly improved; if the gas velocity is further increased, the bed enters a circulating fluidized state, and the particles are carried out by the gas flow and collected and returned by the separator, which can realize continuous reaction.

[0003] Currently, this type of fluidized bed equipment is widely used in the chemical vapor deposition process for silicon production. However, it mainly relies on a "single gas flow drive, simple heating and cooling structure." Its structural and functional adaptability remains at the level of basic reaction requirements, making it difficult to meet the high requirements of silicon-carbon anode material production for "high-temperature stability, temperature accuracy, and equipment lifespan." The following problems exist: 1. Severe corrosion and wear at high temperatures result in short equipment lifespan: Traditional fluidized bed heating elements (such as resistance wires) are in direct contact with the reaction atmosphere (containing silane decomposition products and doped gases) and have no protective structure. At high temperatures (500-800℃), reaction products are prone to adhere to the surface of the heating elements, leading to corrosion or mechanical wear, which in turn shortens the life of the heating elements and the overall equipment. 2. Narrow reaction temperature range, difficult temperature control (prone to overheating or underheating): Traditional equipment uses "integrated heating" (such as heating strips wrapped around the outer wall of the equipment), with no zoned design for the heating area, and poor linkage between the cooling system (mostly water-cooled jackets) and the heating system. When the reaction needs to maintain a narrow temperature range (such as ±2℃ fluctuation), integrated heating is prone to local overheating, while water cooling response lag can easily cause a sudden drop in temperature, which cannot match the precision requirements of silane pyrolysis (which needs to be stable at 500-800℃). 3. Slow response and low control precision: Traditional equipment has few temperature and pressure detection points (mostly 1-2 detection points), and the linkage between the detection signals and the heating / cooling system relies on manual or simple relay control, without integrated electronic control logic; when the reaction atmosphere (such as silane concentration, airflow speed) changes and causes temperature / pressure fluctuations, the system response time is long (>10s), making it difficult to adjust parameters in real time, resulting in poor silicon deposition uniformity and unstable product quality. Therefore, we propose a skid-mounted integrated vapor deposition method for silicon reactor fabrication. Utility Model Content

[0004] The purpose of this invention is to provide a skid-mounted integrated chemical vapor deposition reactor for silicon fabrication, in order to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, this utility model provides the following technical solution: a skid-mounted integrated chemical vapor deposition reactor for silicon fabrication, comprising a skid and a reactor body integrated on the skid, a staged heating module, an air-cooled jacket, a temperature measurement component, a pressure measurement component, pipeline valves and instruments, and an electrical control system; The staged heating module, the air-cooled jacket, the temperature measuring component, and the pressure measuring component are all mounted on the reactor body; The electrical control system is electrically connected to the graded heating module, the temperature measurement component, the pressure measurement component, and the pipeline valve instrument via wires, and is used to receive temperature and pressure detection signals and control the output power of the graded heating module and the on / off state of the pipeline valve.

[0006] Preferably, the reactor body is a closed cavity, and the reactor body has multiple sets of interfaces, including: a displacement gas port for introducing displacement gas, a powder feed port for inputting porous carbon skeleton powder, multiple gas inlets for inputting gas, a jacket cooling inlet and jacket cooling outlet for cooling gas inlet and outlet, a vacuum exhaust outlet for vacuum extraction and exhaust gas discharge, a high-level venting port for depressurization, and a product outlet for outputting products.

[0007] Preferably, the staged heating module includes six independent electric heating modules, which are evenly distributed along the axial and circumferential directions of the outer wall of the reactor body and are in close contact with the outer wall of the reactor body.

[0008] Preferably, the surface of each group of electric heating modules is coated with a ceramic coating with a thickness of 0.3-0.8 mm.

[0009] Preferably, the air-cooled jacket is an annular structure, fitted onto the outer wall of the reactor body, and located between the six electric heating modules. The two ends of the air-cooled jacket are respectively connected to the jacket cooling inlet and the jacket cooling outlet.

[0010] Preferably, the temperature measurement component includes three temperature gauges, which are respectively installed in the top, middle and bottom regions of the reactor body, and the detection probes extend into the reactor body.

[0011] Preferably, the pressure measurement assembly includes five pressure gauges, each of which is installed on the reactor body.

[0012] Preferably, the electrical control system includes a PLC controller, a touch screen, relays, and a power regulator; The temperature sensor, the pressure sensor, and the touch screen are all connected to the PLC controller. The PLC controller is connected to the pipeline valve instrument via the relay; The PLC controller is connected to the graded heating module via the power regulator. The PLC controller is used to receive signals from the temperature and pressure monitoring gauges and process the data. The power regulator is used to adjust the output power of each stage heating module, with an adjustment range of 0-30KW.

[0013] Compared with the prior art, the beneficial effects of this utility model are: 1. More precise temperature control and cooling: The uniform distribution of the staged heating modules replaces the traditional integral heating, allowing for independent adjustment of the temperature requirements of different reaction zones at the top, middle, and bottom of the reactor, thus avoiding incomplete silane pyrolysis or excessive decomposition caused by uneven local temperatures. The linkage between the air-cooled jacket and the heating module can quickly respond to temperature fluctuations. Compared with traditional water-cooled jackets, it is easier to achieve uniform cooling and there is no risk of condensation. This avoids the agglomeration of carbon skeleton powder caused by condensation on the cavity wall and ensures fluidization stability. Multiple temperature sensors capture the temperature in the core reaction zone of the reactor in real time, providing a precise basis for temperature control and ensuring that the reaction temperature remains stable within the reasonable range required for silane pyrolysis, thereby improving the consistency of the silicon deposition process. 2. Improve equipment durability under high-temperature conditions and extend service life: By coating the surface of the staged heating module with a ceramic coating, which has the characteristics of high temperature resistance and chemical inertness, the high temperature reaction gas in the reactor body can be directly isolated from the direct contact between the heating element and the heating element. This effectively solves the problem of corrosion and wear that often occurs in traditional fluidized bed heating elements due to direct exposure to the high temperature reaction environment. It also avoids power attenuation or failure of the heating element due to surface damage, significantly extends the service life of the heating module and the overall equipment, reduces the frequency and cost of maintenance during long-term operation, and ensures production continuity. 3. Full-process monitoring and automatic control: Pressure monitoring instruments enable full-process pressure monitoring from material feeding to product discharge, avoiding process interruptions or safety hazards caused by local pressure anomalies (such as overpressure or negative pressure). After receiving temperature and pressure detection signals, the electronic control system can automatically adjust the heating power and control the valve opening and closing (such as starting the air-cooled jacket when the temperature is too high and opening the high-level venting when the pressure is too high), replacing the traditional manual control, shortening the response time of parameter fluctuations, and reducing product quality fluctuations caused by human operation delays. Given the toxic and flammable nature of silanes, the end-to-end monitoring and automatic shut-off functions effectively reduce leakage risks, improve equipment operational safety, and meet the safety standards of industrial production. Attached Figure Description

[0014] Figure 1 This is a cross-sectional view of the reactor of this utility model.

[0015] In the diagram: 1. Reactor body; 101. Replacement gas port; 102. Powder feed port; 103. Gas inlet; 104. Jacket cooling inlet; 105. Jacket cooling outlet; 106. Vacuum exhaust outlet; 107. High-level vent; 108. Product outlet; 2. Staged heating module; 3. Air-cooled jacket; 4. Temperature gauge; 5. Pressure gauge. Detailed Implementation

[0016] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0017] Please see Figure 1 The present invention provides a skid-mounted integrated chemical vapor deposition reactor for silicon production, comprising a skid and a reactor body 1 integrated on the skid, a staged heating module 2, an air-cooled jacket 3, a temperature measurement component, a pressure measurement component, pipeline valves and instruments, and an electrical control system. The staged heating module 2, the air-cooled jacket 3, the temperature measurement component and the pressure measurement component are all installed on the reactor body 1; The reactor body 1 is a closed cavity. The reactor body 1 has multiple sets of interfaces, including: a displacement gas port 101 for introducing displacement gas, a powder feed port 102 for inputting porous carbon skeleton powder, multiple gas inlets 103 for inputting gas, a jacket cooling inlet 104 and a jacket cooling outlet 105 for cooling gas inlet and outlet, a vacuum exhaust outlet 106 for vacuum extraction and exhaust gas discharge, a high-level vent 107 for pressure relief, and a product outlet 108 for outputting the product. The vacuum exhaust outlet and the high-level vent 107 respectively realize exhaust gas treatment and pressure safety control, avoiding process interruption caused by insufficient interfaces of traditional equipment. The staged heating module 2 includes six independent electric heating modules. The six electric heating modules are evenly distributed along the axial and circumferential directions of the outer wall of the reactor body 1 and are tightly attached to the outer wall of the reactor body 1. This replaces the traditional whole heating, realizes zoned temperature control, solves the problem of uneven local temperature, and improves heat transfer efficiency and shortens the heating time by being tightly attached to the body. The surface of each group of electric heating modules is coated with a ceramic coating with a thickness of 0.3-0.8mm, which isolates the high-temperature reaction gas from direct contact with the heating element, reduces corrosion and wear, and extends the life of the heating module. The air-cooled jacket 3 is a ring structure, fitted on the outer wall of the reactor body 1 and located between the six electric heating modules. The two ends of the air-cooled jacket 3 are connected to the jacket cooling inlet 104 and the jacket cooling outlet 105 respectively, replacing the traditional water-cooled jacket. The cooling gas flows uniformly along the body, the cooling response time is <3s, there is no risk of condensation, and the powder inside the cavity is avoided from clumping, solving the problem of lag in traditional water cooling. The temperature measurement component includes three temperature gauges 4, which are installed at the top, middle and bottom of the reactor body 1 respectively. The detection probes extend into the reactor body 1, covering the core reaction area of ​​the reactor, avoiding the local data deviation of traditional single-point detection, ensuring that the detection data is the accurate temperature inside the cavity, and providing a precise basis for temperature control. The pressure measurement component includes five pressure monitoring gauges 5, which are installed on the reactor body 1 to monitor the pressure throughout the process in real time, thus avoiding the safety risks caused by pressure runaway in traditional equipment. The electrical control system is electrically connected to the staged heating module 2, the temperature measurement component, the pressure measurement component, and the pipeline valve instruments via wires. It is used to receive temperature and pressure detection signals and control the output power of the staged heating module and the opening and closing of the pipeline valves. The electrical control system includes a PLC controller, a touch screen, relays, and a power regulator; temperature sensor 4, pressure sensor 5, and the touch screen are all connected to the PLC controller; the PLC controller is connected to pipeline valve instruments via relays; the PLC controller is connected to the staged heating module 2 via the power regulator. The PLC controller is used to receive signals from the temperature sensor and pressure sensor and process the data. The power regulator is used to adjust the output power of each staged heating module, with an adjustment range of 0-30KW, to achieve fully automatic control and solve the problem of slow response in traditional manual control (the control logic and signal transmission of the electrical control system are existing technologies well known in the field and will not be described in detail here).

[0018] The beneficial effects of this utility model are as follows: 1. More precise temperature control and cooling: The uniform distribution of the staged heating modules replaces the traditional integral heating, allowing for independent adjustment of the temperature requirements of different reaction zones at the top, middle, and bottom of the reactor, thus avoiding incomplete silane pyrolysis or excessive decomposition caused by uneven local temperatures. The linkage between the air-cooled jacket and the heating module can quickly respond to temperature fluctuations. Compared with traditional water-cooled jackets, it is easier to achieve uniform cooling and there is no risk of condensation. This avoids the agglomeration of carbon skeleton powder caused by condensation on the cavity wall and ensures fluidization stability. Multiple temperature sensors capture the temperature in the core reaction zone of the reactor in real time, providing a precise basis for temperature control and ensuring that the reaction temperature remains stable within the reasonable range required for silane pyrolysis, thereby improving the consistency of the silicon deposition process. 2. Improve equipment durability under high-temperature conditions and extend service life: By coating the surface of the staged heating module with a ceramic coating, which has the characteristics of high temperature resistance and chemical inertness, the high temperature reaction gas in the reactor body can be directly isolated from the direct contact between the heating element and the heating element. This effectively solves the problem of corrosion and wear that often occurs in traditional fluidized bed heating elements due to direct exposure to the high temperature reaction environment. It also avoids power attenuation or failure of the heating element due to surface damage, significantly extends the service life of the heating module and the overall equipment, reduces the frequency and cost of maintenance during long-term operation, and ensures production continuity. 3. Full-process monitoring and automatic control: Pressure monitoring instruments enable full-process pressure monitoring from material feeding to product discharge, avoiding process interruptions or safety hazards caused by local pressure anomalies (such as overpressure or negative pressure). After receiving temperature and pressure detection signals, the electronic control system can automatically adjust the heating power and control the valve opening and closing (such as starting the air-cooled jacket when the temperature is too high and opening the high-level venting when the pressure is too high), replacing the traditional manual control, shortening the response time of parameter fluctuations, and reducing product quality fluctuations caused by human operation delays. Given the toxic and flammable nature of silanes, the full-process monitoring and automatic shut-off function can effectively reduce the risk of leakage, improve the safety of equipment operation, and meet the safety standards of industrial production.

[0019] In summary, the method of using the skid-mounted integrated silicon fabrication reactor based on vapor deposition provided in this embodiment is as follows: Atmosphere replacement: The electrical control system controls the valve of the replacement gas port 101 to open, and the replacement gas (high-purity nitrogen or argon) enters the reactor body 1. After the air is purged, the valve is closed. Material introduction: The porous carbon skeleton enters from the powder feed inlet 102, and silane and media 2-4 are introduced from the corresponding gas inlets 103; Temperature control: The PLC controls the power of the graded heating module 2 through the power regulator based on the signal from the temperature detection table 4, raising the temperature to 500-800℃; when the temperature exceeds the limit, the air-cooling jacket 3 is activated, and cooling gas enters from the jacket cooling inlet 104 to quickly cool down the temperature. Pressure control: The PLC controls the high-level vent valve 107 to release pressure or adjust the displacement air flow to replenish pressure based on the signal from pressure monitoring table 5, maintaining a slight positive pressure of 0.05-0.1MPa. Product processing: After the reaction is completed, the product enters the storage tank from the product outlet 108, and the tail gas enters the processing device from the vacuum tail gas outlet 106.

[0020] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A silicon-producing reactor based on skid-mounted integrated vapor deposition method, characterized in that, Includes a skid and a reactor body (1) integrated on the skid, a staged heating module (2), an air-cooled jacket (3), a temperature measurement assembly, a pressure measurement assembly, pipeline valves and instruments, and an electrical control system; The staged heating module (2), the air-cooled jacket (3), the temperature measuring component and the pressure measuring component are all mounted on the reactor body (1); The electrical control system is electrically connected to the graded heating module (2), the temperature measurement component, the pressure measurement component, and the pipeline valve instrument via wires, respectively, to receive temperature and pressure detection signals and control the output power of the graded heating module and the on / off state of the pipeline valve.

2. The silicon fabrication reactor based on skid-mounted integrated vapor deposition method according to claim 1, characterized in that: The reactor body (1) is a closed cavity. The reactor body (1) has multiple sets of interfaces, including: a displacement gas port (101) for introducing displacement gas, a powder feed port (102) for inputting porous carbon skeleton powder, multiple gas inlets (103) for inputting gas, a jacket cooling inlet (104) and a jacket cooling outlet (105) for cooling gas inlet and outlet, a vacuum exhaust outlet (106) for vacuum extraction and exhaust gas discharge, a high-level venting port (107) for depressurization, and a product outlet (108) for outputting products.

3. A skid-mounted integrated silicon production reactor based on vapor deposition according to claim 2, characterized in that: The graded heating module (2) includes six independent electric heating modules. The six electric heating modules are evenly distributed along the axial and circumferential directions of the outer wall of the reactor body (1) and are closely attached to the outer wall of the reactor body (1).

4. A skid-mounted integrated silicon production reactor based on vapor deposition according to claim 3, characterized in that: Each of the electric heating modules is coated with a ceramic coating with a thickness of 0.3-0.8 mm.

5. A skid-mounted integrated silicon production reactor based on vapor deposition according to claim 3, characterized in that: The air-cooled jacket (3) is a ring structure, sleeved on the outer wall of the reactor body (1), and located between the six electric heating modules. The two ends of the air-cooled jacket (3) are respectively connected to the jacket cooling inlet (104) and the jacket cooling outlet (105).

6. A skid-mounted integrated silicon production reactor based on vapor deposition according to claim 2, characterized in that: The temperature measurement assembly includes three temperature gauges (4), which are respectively installed in the top, middle and bottom regions of the reactor body (1), and the detection probes extend into the reactor body (1).

7. A skid-mounted integrated silicon production reactor based on vapor deposition according to claim 6, characterized in that: The pressure measurement assembly includes five pressure monitoring gauges (5), which are respectively installed on the reactor body (1).

8. A skid-mounted integrated silicon production reactor based on vapor deposition according to claim 7, characterized in that: The electrical control system includes a PLC controller, a touch screen, relays, and a power regulator; The temperature sensor (4), the pressure sensor (5), and the touch screen are all connected to the PLC controller; The PLC controller is connected to the pipeline valve instrument via the relay; The PLC controller is connected to the graded heating module (2) via the power regulator. The PLC controller is used to receive signals from the temperature and pressure monitoring gauges and process the data. The power regulator is used to adjust the output power of each stage heating module, with an adjustment range of 0-30KW.

Images