High-vacuum sublimation deposition production device and method for nano silicon-carbon negative electrode material

Abstract

The invention discloses a high-vacuum sublimation deposition production device and method for a nanometer silicon carbon negative electrode material, the device comprises a deposition shell, the bottom end of the deposition shell is provided with a storage shell, and the bottom end of the storage shell is provided with a sublimation shell; a sealing cover is arranged on the deposition shell, a gas distribution assembly is arranged in the deposition shell, a guide pipe is arranged on the sublimation shell, a driving screw rod is arranged on the sealing cover, the gas distribution assembly is arranged on the driving screw rod, and the guide pipe is matched with the driving screw rod; the gas distribution device has the technical effects that the space in the deposition shell can be covered in all directions through the gas distribution assembly through the compound motion of rotation and lifting, mixed gas is evenly distributed in the horizontal direction through the rotation motion, it is guaranteed that the mixed gas can be evenly diffused in the vertical direction through the lifting motion, and the gas distribution efficiency is improved. The double motion mode avoids the problem that the concentration of local mixed gas is too high or too low.

Description

Technical Field

[0001] The invention relates to a high vacuum sublimation deposition production device and method for nano silicon carbon negative electrode materials. Background Art

[0002] As a highly efficient and environmentally friendly energy storage device, lithium-ion batteries have been widely used in electric vehicles, consumer electronics, energy storage systems, and other fields. However, as the application of lithium-ion batteries continues to expand, the requirements for their performance are becoming increasingly stringent, especially in terms of energy density, cycle life, and safety.

[0003] Nano silicon carbon negative electrode materials have shown great application potential due to their unique physical and chemical properties. Silicon has a high theoretical specific capacity and can significantly improve the energy density of the battery, while carbon materials have good conductivity and stability, which can effectively alleviate the volume expansion problem of silicon during the charging and discharging process. The existing silicon carbon negative electrode material preparation technology is mostly to mix and sinter nano silicon powder or silicon monoxide powder with carbon source powder. The vapor deposition process adopted by some manufacturers is also to directly introduce carbon source gas into the powder of silicon-based materials to deposit carbon coating. However, when the carbon source gas is introduced, the gas distribution is prone to unevenness, and silicon-based powder is prone to agglomeration, which affects the performance of nano silicon carbon negative electrode materials. In view of this, the present invention proposes a high vacuum sublimation deposition production device and method for nano silicon carbon negative electrode materials to solve the above problems. Summary of the Invention

[0004] The purpose of the present invention is to provide a high vacuum sublimation deposition production device and method for nano silicon carbon negative electrode materials to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solutions: A high vacuum sublimation deposition production device for nano silicon carbon negative electrode materials, comprising a deposition shell, a storage shell provided at the bottom end of the deposition shell, and a sublimation shell provided at the bottom end of the storage shell; A sealing cover is provided on the deposition shell, a gas distribution assembly is provided in the deposition shell, a guide tube is provided on the sublimation shell, a driving screw is provided on the sealing cover, the gas distribution assembly is provided on the driving screw, the guide tube cooperates with the driving screw, and the driving screw rotates, driving the gas distribution assembly to rotate and rise and fall along the axis of the driving screw to evenly distribute the gas, and driving the guide tube to rotate with the axis of the driving screw to evenly distribute the steam.

[0006] As an improvement of the above technical solution, a heat insulation block is provided on the sublimation shell, and the heat insulation block is provided between the sublimation shell and the storage shell; A sublimation crucible is provided in the sublimation shell, a sublimation heating chamber is provided between the sublimation crucible and the sublimation shell, a feeding pipe is provided on the sublimation shell, the feeding pipe is communicated with the inner cavity of the sublimation crucible, and a sealed feeding cover is provided on the feeding pipe.

[0007] As an improvement to the above technical solution, a plurality of guide through holes are evenly provided on the surface of the guide tube, and a guide rotation groove is provided on the heat insulation block; The guide tube is provided with a rotating tube connected to the inner cavity, the outer wall of the rotating tube is provided with a guiding rotating protrusion ring, the guiding rotating protrusion ring is rotatably set in the guiding rotating groove, the rotating tube is provided with a conical guide cover, the conical guide cover is connected to the inner cavity of the rotating tube, the bottom end of the conical guide cover is provided with a stirring blade, and the stirring blade is adapted to the inner wall of the sublimation crucible.

[0008] As an improvement to the above technical solution, a sun rotating gear is provided at the bottom end of the driving screw, and three sets of planetary rotating gears that mesh with each other are provided on the sun rotating gear. The outsides of the three sets of planetary rotating gears are provided with inner gear rings that mesh with each other, and a reinforcement rod is provided on the inner gear ring, and the reinforcement rod is connected to the inner wall of the deposition shell; The planetary rotating gear is provided with a planetary connecting rod, the rotating tube is provided with a rotating bracket, and the three groups of planetary connecting rods are all rotatably provided on the rotating bracket; The reinforcing rod is provided with a protective shell, the protective shell is provided with a first protective bevel and a second protective bevel, the inner gear ring is provided in the protective shell, and the driving screw and the rotating bracket are both rotationally sealed with the protective shell.

[0009] As an improvement of the above technical solution, a deposition heating chamber is provided in the deposition shell, and two groups of guide grooves are symmetrically opened on the inner wall of the deposition shell, and the guide grooves are provided in the deposition heating chamber; The gas distribution assembly includes a lifting ring, the outer wall of the lifting ring is symmetrically provided with two groups of guide protrusions, the two groups of guide protrusions are respectively slidably arranged in two groups of guide grooves, a rotating ring is provided in the lifting ring, a plurality of distribution pipes are evenly arranged in the rotating ring, a driving ring is provided in the center of the rotating ring, the driving ring is threadedly sleeved on the outer wall of the driving screw, the plurality of distribution pipes are connected to the driving ring, and the distribution pipes are evenly provided with a plurality of distribution through holes; The rotating ring cooperates with the lifting ring so that the lifting ring can be lifted and lowered in the two sets of guide grooves.

[0010] As an improvement to the above technical solution, a movable ring groove is provided in the lifting ring, and the rotating ring is rotatably provided in the movable ring groove; Two groups of blocking rods are symmetrically arranged in the movable ring groove, and two groups of contact protrusions are symmetrically arranged on the outer wall of the rotating ring. The contact protrusions are in contact with the blocking rods, so that the rotating ring does not rotate around the axis of the driving screw.

[0011] As an improvement of the above technical solution, a connecting sleeve is provided on the rotating sleeve of the outer wall of the driving ring, a gas connecting pipe is provided on the connecting sleeve, a distribution cavity is provided in the driving ring, and multiple groups of first connecting holes and multiple groups of second connecting holes are provided on the outer wall of the driving ring. The multiple groups of first connecting holes match the positions of multiple groups of distribution pipes, and the distribution pipes are connected to the distribution cavity through the first connecting holes, and the multiple groups of second connecting holes match the positions of the connecting sleeve, and the gas connecting pipes are connected to the distribution cavity through the second connecting holes.

[0012] As an improvement to the above technical solution, the storage shell is in a truncated cone shape, the insulation block is provided with an insulation slope, a storage cavity is provided between the storage shell and the insulation block, a recovery pipe is provided at the bottom end of the storage shell, and a recovery sealing plate is provided at the port of the recovery pipe; The sealing cover is provided with a driving servo motor, which is transmission-connected to the driving screw. The sealing cover is provided with a gas feed pipe, and a high-temperature resistant alloy bellows is provided between the gas feed pipe and the gas connecting pipe. The sealing cover is also provided with an air outlet pipe, which is connected to the inside of the sealing cover.

[0013] A method for using a high vacuum sublimation deposition production device for nano silicon carbon negative electrode materials comprises the following steps: S10, loading: Introduce the silicon powder and silicon dioxide into the sublimation crucible through the feeding pipe, connect the gas source to the gas feeding pipe, connect the vacuum pump to the gas outlet pipe, and keep the deposition shell, storage shell and sublimation shell sealed; S20, stirring: The feeding pipe is sealed, and the driving servo motor is turned on to make the driving screw reciprocate to drive the stirring blade to rotate and stir in the sublimation crucible, and heat the deposition heating chamber and the sublimation heating chamber; S30, vacuum treatment: The recovery pipe and the feeding pipe are sealed, and the deposition housing, the storage housing, and the sublimation housing are placed in a vacuum state. At the same time, the deposition heating chamber and the sublimation heating chamber are continuously heated, and the temperature of the deposition heating chamber is lower than that of the sublimation heating chamber. S40, air supply: The mixed gas is introduced into the deposition heating chamber through the gas feed pipe, and the servo motor is driven to be continuously turned on, so that the rotating ring is continuously switched between the rotating state and the lifting state, so that the mixed gas is filled in the deposition heating chamber; S50, insulation: After S40 starts, the deposition heating chamber and the sublimation heating chamber are kept warm, and the servo motor is driven to be continuously turned on, so that the rotating ring is continuously switched between a rotating state and a lifting state, so that the mixed gas is filled in the deposition heating chamber, and at the same time, the steam in the sublimation crucible is filled in the deposition heating chamber through the distribution pipe; S60, Collection: After the steam in the sublimation crucible and the mixed gas have completed contact reaction in S50, the product is collected and processed through the gas outlet pipe.

[0014] As an improvement to the above technical solution, after S60 is completed, the driving servo motor is continuously turned on, so that the rotating ring is in a lifting state, driving the lifting ring to lift and lower on the inner wall surface of the deposition shell to scrape off the residual material, and at the same time, the residual material dropped in the storage shell is recovered through the recovery pipe.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The gas distribution assembly can fully cover the space inside the deposition shell through the combined motion of rotation and lifting. The rotational motion makes the mixed gas evenly distributed in the horizontal direction, while the lifting motion ensures that the mixed gas can also be evenly diffused in the vertical direction. This dual motion mode avoids the problem of local mixed gas concentration being too high or too low, and can also stir the mixed gas in the deposition shell to improve the mixing quality of the mixed gas, thereby providing an ideal reaction environment for the uniform deposition of nano-silicon-carbon negative electrode materials. The combined motion of rotation and lifting can also precisely control the lifting and rotation speed of the gas distribution component, enabling precise regulation of gas flow and distribution. This not only improves reaction efficiency but also ensures sufficient contact and reaction between the mixed gas and steam during the reaction process, thereby improving the performance and consistency of the nano-silicon-carbon negative electrode material. By rotating the guide tube, the steam generated in the sublimation shell can be evenly guided into the deposition shell. This evenly distributed steam is fully in contact with the mixed gas, avoiding the problem of excessively high or low local steam concentration, thereby improving the uniformity and consistency of the reaction. It can also promote the dynamic mixing of steam in the deposition shell to accelerate the reaction rate, effectively improving production efficiency and reducing reaction time. By driving the screw to simultaneously drive the gas distribution assembly and the guide tube to rotate, the coordinated movement of the two is achieved, which can ensure that the distribution process of the mixed gas and vapor in the deposition shell is highly synchronized, avoiding uneven distribution caused by asynchronous movement. At the same time, a single driving screw drives the gas distribution assembly and the guide tube at the same time, reducing the complexity of the driving system. This design not only reduces the manufacturing cost of the device, but also reduces the system failure points, improves the reliability and maintenance convenience of the device, and uses a single driving screw to drive multiple components to reduce energy loss during the transmission process. This efficient power transmission method improves the overall energy efficiency of the device, and the rotation speed of the driving screw can be adjusted according to process requirements, thereby accurately controlling the distribution speed and range of the mixed gas and vapor. This flexibility enables the device to adapt to different reaction conditions and optimize the reaction process. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 It is a schematic diagram of the structure of the present invention; Figure 2 For the present invention Figure 1 Cross-sectional view of AA; Figure 3 This is a schematic structural diagram of the deposition shell of the present invention; Figure 4 For the present invention Figure 3 Cross-sectional view of the middle BB; Figure 5 Schematic diagram of the three-dimensional structure of the deposited shell of the present invention; Figure 6 This is a schematic diagram of the positions of the drive screw and gas distribution components of the present invention; Figure 7 For the present invention Figure 6 Schematic diagram of the enlarged structure at C in the middle; Figure 8 This is a schematic diagram of the positions of the lifting ring and the rotating ring of the present invention; Figure 9 It is a structural schematic diagram of the lifting ring of the present invention; Figure 10 For the present invention Figure 9 Schematic diagram of the enlarged structure at D in the middle; Figure 11 It is a structural schematic diagram of the rotating ring of the present invention; Figure 12 It is a front view of the lifting ring of the present invention; Figure 13 For the present invention Figure 12 Cross-sectional view of EE; Figure 14 is a cross-sectional schematic diagram of the drive ring of the present invention; Figure 15 This is a schematic diagram of the positions of the conical guide cover and the stirring blades of the present invention; Figure 16 For the present invention Figure 15 Schematic diagram of the enlarged structure at F in the middle; Figure 17 This is a schematic diagram of the structure inside the protective housing of the present invention; Figure 18 For the present invention Figure 17 Schematic diagram of the enlarged structure at G in the middle.

[0017] In the figure: 10, deposition shell; 11, deposition heating chamber; 12, guide groove; 20, storage shell; 21, recovery pipe; 22, storage chamber; 30, sublimation shell; 31, feeding pipe; 32, sublimation heating chamber; 33, sublimation crucible; 34, conical guide cover; 341, rotating tube; 3411, guiding rotating raised ring; 342, rotating bracket; 343, guide tube; 3431, guiding through hole; 344, stirring blade; 35, insulation block; 351, insulation slope; 36, rotating groove; 40, sealing cover; 41, gas outlet pipe; 42, driving servo motor; 43, gas feeding pipe; 44, driving screw; 4 5. High-temperature resistant alloy bellows; 50. Gas distribution assembly; 51. Drive ring; 511. First connecting through-hole; 512. Distribution cavity; 513. Second connecting through-hole; 52. Connecting sleeve; 521. Gas connecting pipe; 53. Distribution pipe; 54. Distribution through-hole; 55. Rotating ring; 551. Contact protrusion; 56. Lifting ring; 561. Movable ring groove; 562. Blocking rod; 563. Guide protrusion; 60. Sun rotating gear; 61. Planetary rotating gear; 62. Planetary connecting rod; 63. Reinforcement rod; 64. Inner ring; 65. Protective shell; 651. First protective slope; 652. Second protective slope. DETAILED DESCRIPTION

[0018] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0019] Example: like Figure 1-18 As shown, this embodiment provides a high vacuum sublimation deposition production device for nano silicon carbon negative electrode materials, comprising a deposition housing 10, a storage housing 20 is provided at the bottom end of the deposition housing 10, and a sublimation housing 30 is provided at the bottom end of the storage housing 20; A sealing cover 40 is provided on the deposition shell 10, a gas distribution assembly 50 is provided in the deposition shell 10, a guide tube 343 is provided on the sublimation shell 30, a driving screw 44 is provided on the sealing cover 40, the gas distribution assembly 50 is provided on the driving screw 44, the guide tube 343 cooperates with the driving screw 44, and the driving screw 44 rotates, driving the gas distribution assembly 50 to rotate and rise and fall along the axis of the driving screw 44 to evenly distribute the gas, and driving the guide tube 343 to rotate with the axis of the driving screw 44 to evenly distribute the steam.

[0020] In this embodiment, when producing nano-silicon-carbon negative electrode materials, mixed powder is placed in the sublimation shell 30 and the entire shell is vacuumed. At the same time, the deposition shell 10 and the sublimation shell 30 are heated, and the temperature in the sublimation shell 30 is made higher than the temperature in the deposition shell 10. Then, the mixed gas is injected into the deposition shell 10 through the gas distribution assembly 50, and the screw 44 is driven to rotate, driving the gas distribution assembly 50 to rotate and rise and fall along the axis of the drive screw 44, so that the mixed gas is evenly distributed in the deposition shell 10. At the same time, the steam generated by the heated mixed powder in the sublimation shell 30 is evenly distributed in the deposition shell 10 through the rotating guide pipe 343 and reacts in the deposition shell 10. The reaction product can then be collected. The gas distribution assembly 50 can fully cover the space within the deposition housing 10 through a combined rotational and lifting motion. The rotational motion uniformly distributes the mixed gas in the horizontal direction, while the lifting motion ensures uniform diffusion of the mixed gas in the vertical direction. This dual motion mode avoids the problem of excessively high or low concentrations of the mixed gas in a local area, and can also stir the mixed gas in the deposition housing 10, improving the mixing quality of the mixed gas, thereby providing an ideal reaction environment for the uniform deposition of nano-silicon-carbon negative electrode materials. The combined motion of rotation and lifting can also precisely control the lifting and rotation speed of the gas distribution assembly 50, which can achieve precise regulation of gas flow and distribution. This not only improves the reaction efficiency, but also ensures sufficient contact and reaction between the mixed gas and steam during the reaction process, thereby improving the performance and consistency of the nano-silicon-carbon negative electrode material. By rotating the guide tube 343, the steam generated in the sublimation housing 30 can be evenly guided into the deposition housing 10. This evenly distributed steam is fully in contact with the mixed gas, avoiding the problem of excessively high or low local steam concentration, thereby improving the uniformity and consistency of the reaction. It can also promote dynamic mixing of the steam in the deposition housing 10 and accelerate the reaction rate, which can effectively improve production efficiency and reduce reaction time. By driving the screw 44 to simultaneously drive the gas distribution assembly 50 and the guide tube 343 to rotate, the coordinated movement of the two is achieved, which can ensure that the distribution process of the mixed gas and steam in the deposition shell 10 is highly synchronized, avoiding uneven distribution caused by asynchronous movement. At the same time, a single driving screw 44 drives the gas distribution assembly 50 and the guide tube 343 at the same time, reducing the complexity of the driving system. This design not only reduces the manufacturing cost of the device, but also reduces the system failure points, improves the reliability and maintenance convenience of the device, and uses a single driving screw 44 to drive multiple components to reduce energy loss during the transmission process. This efficient power transmission method improves the overall energy efficiency of the device, and the rotation speed of the driving screw 44 can be adjusted according to process requirements, thereby accurately controlling the distribution speed and range of the mixed gas and steam. This flexibility enables the device to adapt to different reaction conditions and optimize the reaction process.

[0021] Specifically, the sublimation housing 30 is provided with a heat insulation block 35 , and the heat insulation block 35 is provided between the sublimation housing 30 and the storage housing 20 ; A sublimation crucible 33 is provided in the sublimation shell 30 , a sublimation heating chamber 32 is provided between the sublimation crucible 33 and the sublimation shell 30 , a feeding pipe 31 is provided on the sublimation shell 30 , the feeding pipe 31 is communicated with the inner cavity of the sublimation crucible 33 , and a sealed feeding cover is provided on the feeding pipe 31 .

[0022] In this embodiment, the insulation block 35 is made of insulation material, and the mixed powder is fed into the sublimation crucible 33 through the feeding pipe 31. After the mixed powder is fed in, the feeding pipe 31 is sealed by the feeding cover. Of course, when the sublimation shell 30 is heated, the heating position is located in the sublimation heating chamber 32 to heat the sublimation crucible 33 .

[0023] Specifically, a plurality of guide through holes 3431 are evenly formed on the surface of the guide tube 343, and a guide rotation groove 36 is formed on the heat insulation block 35; The guide tube 343 is provided with a rotating tube 341 connected to the inner cavity. The outer wall of the rotating tube 341 is provided with a guiding rotating protrusion ring 3411. The guiding rotating protrusion ring 3411 is rotatably set in the guiding rotating groove 36. The rotating tube 341 is provided with a conical guide cover 34. The conical guide cover 34 is connected to the inner cavity of the rotating tube 341. The bottom end of the conical guide cover 34 is provided with a stirring blade 344. The stirring blade 344 is adapted to the inner wall of the sublimation crucible 33.

[0024] In this embodiment, when the mixed powder is heated, the driving screw 44 drives the rotating tube 341 to rotate, thereby causing the guide tube 343 to rotate, so that the steam is evenly distributed in the inner cavity of the deposition shell 10, which can promote the full mixing of the steam and the gas in the deposition shell, accelerate the reaction rate, and improve the production efficiency and quality of the nano-silicon-carbon negative electrode material. The conical guide cover 34 can evenly guide the steam generated in the sublimation crucible 33 into the deposition shell 10 through rotation. Its conical structure itself has good guiding performance. Combined with the rotational motion, it can effectively avoid local accumulation of steam and ensure uniform distribution of steam in the deposition shell 10. Of course, when the rotating tube 341 rotates, the conical guide cover 34 and the stirring blade 344 are driven to rotate, which can effectively prevent the mixed powder in the sublimation crucible 33 from accumulating or clogging during the sublimation process, ensuring the continuity and stability of the sublimation process. In addition, the mixed powder in the sublimation crucible 33 can be stirred to be fully mixed, avoiding accumulation or uneven distribution of nano-scale materials, thereby improving the uniformity of the sublimation process. At the same time, the mixed powder is more fully in contact with the inner wall of the sublimation crucible 33, accelerating heat transfer, and improving the heating efficiency of the material.

[0025] Specifically, a sun rotating gear 60 is provided at the bottom end of the driving screw 44, and three sets of planetary rotating gears 61 that mesh with each other are provided on the sun rotating gear 60. The outsides of the three sets of planetary rotating gears 61 are provided with inner rings 64 that mesh with each other. A reinforcement rod 63 is provided on the inner ring 64, and the reinforcement rod 63 is connected to the inner wall of the deposition shell 10; The planetary connecting rod 62 is provided on the planetary rotating gear 61, and the rotating bracket 342 is provided on the rotating tube 341. The three sets of planetary connecting rods 62 are all rotatably provided on the rotating bracket 342. A protective shell 65 is provided on the reinforcement rod 63 , and the protective shell 65 is provided with a first protective bevel 651 and a second protective bevel 652 . The inner gear ring 64 is provided in the protective shell 65 , and the drive screw 44 and the rotating bracket 342 are both rotationally sealed and connected to the protective shell 65 .

[0026] In this embodiment, the coordination between the planetary rotating gear 61, the sun rotating gear 60, and the inner ring gear 64 facilitates the control of the rotating tube 341 to rotate slowly, so that the steam can be more smoothly guided into the deposition shell 10 through the guide tube 343, thereby avoiding local accumulation or uneven distribution of steam caused by excessive rotation, thereby further improving the uniformity of the reaction and being able to adapt to different production conditions and process requirements. For example, under different temperatures, pressures, or gas flow rates, the rotation speed can be customized as needed to optimize the reaction conditions. Of course, the protective shell 65 completely wraps the inner gear ring 64 to form a closed space, blocking the steam from directly contacting the surface of the inner gear ring, fundamentally avoiding the condensation of steam on the inner gear ring due to temperature difference, and effectively solving the influence of the gear system on the steam during the high vacuum sublimation deposition process; Of course, the protective housing 65 is made of high temperature resistant insulation material, which can maintain a stable internal temperature and reduce the temperature drop caused by heat exchange; The first protective slope 651 and the second protective slope 652 form a streamlined flow-guiding structure, which allows the steam to slide along the slope, guiding the steam away from the surface of the protective shell 65, and preventing the steam from being retained or penetrating into the inner gear ring area; During the operation of the gear system, vibrations may be generated, which are then transmitted to the protective shell 65 through the reinforcement rod 63, so that the material on the protective shell 65 can be automatically shaken off and recovered for subsequent recycling and reuse.

[0027] Specifically, a deposition heating chamber 11 is provided in the deposition housing 10 , and two groups of guide grooves 12 are symmetrically opened on the inner wall of the deposition housing 10 , and the guide grooves 12 are provided in the deposition heating chamber 11 ; The gas distribution assembly 50 includes a lifting ring 56, the outer wall of which is symmetrically provided with two groups of guide protrusions 563. The two groups of guide protrusions 563 are respectively slidably disposed in two groups of guide grooves 12. A rotating ring 55 is disposed within the lifting ring 56, and multiple groups of distribution pipes 53 are evenly disposed within the rotating ring 55. A driving ring 51 is disposed at the center of the rotating ring 55. The driving ring 51 is threadedly sleeved on the outer wall of the driving screw 44. Multiple groups of distribution pipes 53 are connected to the driving ring 51, and multiple groups of distribution through holes 54 are evenly disposed on the distribution pipes 53. The rotating ring 55 cooperates with the lifting ring 56 so that the lifting ring 56 can be lifted and lowered in the two sets of guide grooves 12 .

[0028] In this case, the temperature in the deposition heating chamber 11 is kept at 600-800°C, and the temperature in the sublimation heating chamber 32 is kept at 1000-1200°C, and the temperature of the sublimation heating chamber 32 is always higher than the temperature of the deposition heating chamber 11.

[0029] Specifically, a movable ring groove 561 is provided in the lifting ring 56, and the rotating ring 55 is rotatably provided in the movable ring groove 561; Two groups of blocking rods 562 are symmetrically arranged in the movable ring groove 561, and two groups of contact protrusions 551 are symmetrically arranged on the outer wall of the rotating ring 55. The contact protrusions 551 are in contact with the blocking rods 562, so that the rotating ring 55 does not rotate around the axis of the driving screw 44.

[0030] In this embodiment, when the distribution pipe 53 in the deposition housing 10 switches between a rotating state and a lifting state, the drive screw 44 rotates. Since the drive ring 51 is threadedly sleeved on the outer wall of the drive screw 44, the drive ring 51 rotates as the drive screw 44 rotates, so that the distribution pipe 53 is adjusted in position according to the rotation of the drive screw 44. When the contact protrusion 551 contacts the blocking rod 562, the rotating ring 55 does not rotate with the rotation of the drive screw 44 due to the sliding cooperation of the guide protrusion 563 and the guide groove 12. At the same time, the rotating ring 55 is lifted and lowered along the axis of the drive screw 44, thereby changing the state. By providing a movable annular groove 561 in the lifting ring 56 and a blocking rod 562 in the movable annular groove 561, and providing a contact protrusion 551 on the outer wall of the rotating ring 55, the rotating ring 55 can achieve a combined motion of rotation and lifting when the driving screw 44 rotates. This combined motion mode enables the gas distribution assembly 50 to perform omnidirectional gas distribution within the deposition housing 10, ensuring uniform diffusion of the mixed gas in the horizontal and vertical directions. The motion state can also be flexibly adjusted according to process requirements, thereby adapting to different production conditions and process requirements. This flexibility enhances the versatility and applicability of the device. At the same time, this design reduces the complex interactions between mechanical components, reduces the risk of failure, and improves the reliability and stability of the device. Of course, during the lifting process, the lifting ring 56 contacts the inner wall of the deposition shell 10, which can effectively scrape off the residual waste or incompletely reacted substances attached to the inner wall of the deposition shell 10. Through the scraping effect of the lifting ring 56, these wastes can be removed from the inner wall, which is convenient for subsequent recycling and processing. At the same time, it can keep the interior of the deposition shell 10 clean, reduce pollution and equipment failures caused by the accumulation of residual materials, help improve the stability and reliability of the device, and extend the service life of the equipment.

[0031] Specifically, a connecting sleeve 52 is provided on the outer wall of the driving ring 51, and a gas connecting pipe 521 is provided on the connecting sleeve 52. A distribution cavity 512 is provided in the driving ring 51. Multiple groups of first connecting holes 511 and multiple groups of second connecting holes 513 are provided on the outer wall of the driving ring 51. The positions of the multiple groups of first connecting holes 511 match the positions of the multiple groups of distribution pipes 53. The distribution pipes 53 are connected with the distribution cavity 512 through the first connecting holes 511. The positions of the multiple groups of second connecting holes 513 match the positions of the connecting sleeve 52. The gas connecting pipe 521 is connected with the distribution cavity 512 through the second connecting holes 513.

[0032] In this embodiment, when the mixed gas is introduced into the distribution pipe 53, the mixed gas first enters the gas connecting pipe 521. Since the driving ring 51 is in a rotating state, when the gas connecting pipe 521 is docked with the second connecting through hole 513, the mixed gas enters the distribution cavity 512 and enters the multiple groups of distribution pipes 53 respectively through the multiple groups of first connecting through holes 511, and is evenly distributed inside the deposition heating chamber 11 through the distribution pipe 53.

[0033] Specifically, the storage housing 20 is truncated cone-shaped, the insulation block 35 is provided with an insulation slope 351, a storage cavity 22 is provided between the storage housing 20 and the insulation block 35, a recovery pipe 21 is provided at the bottom end of the storage housing 20, and a recovery sealing plate is provided at the end of the recovery pipe 21; The sealing cover 40 is provided with a driving servo motor 42, which is in transmission connection with a driving screw 44. The sealing cover 40 is provided with a gas feed pipe 43, and a high-temperature resistant alloy bellows 45 is provided between the gas feed pipe 43 and the gas connecting pipe 521. The sealing cover 40 is also provided with an air outlet pipe 41, which is connected to the interior of the sealing cover 40.

[0034] In this case, the gas feed pipe 43 is connected to the mixed gas supply tank, and the gas outlet pipe 41 is connected to the powder collector. Of course, a vacuum pump is provided on the powder collector, and an exhaust gas treatment device is provided at the gas outlet of the vacuum pump. Of course, in this case, the mixed gas provided in the mixed gas supply tank is one or more of a carbon source gas, a carrier gas, and a reducing gas. Specifically, the carbon source gas is one or more of hydrocarbon gases such as natural gas, propylene gas, propane gas, and acetylene gas. The carrier gas is one of high-purity nitrogen and high-purity argon. The reducing gas is one of hydrogen and carbon monoxide. Of course, the mixed powder in this case is nano silicon powder and silicon dioxide powder mixed evenly in a molar ratio of 1:0.8 to 1; In this embodiment, when the mixed gas is provided, the mixed gas enters the high-temperature resistant alloy bellows 45 through the gas feed pipe 43 and is introduced into the gas connecting pipe 521. The mixed gas is evenly distributed by the gas distribution assembly 50. After the reaction is completed, the coated powder is captured and collected by the powder collector. The coated silicon-carbon powder is sucked into the powder collector under the action of vacuum. Of course, when the powder is not collected, the residual waste or incompletely reacted substances in the storage shell 20 can be recovered by opening the recovery cover on the recovery pipe 21, so as to reasonably recycle and reuse resources, and the insulating slope 351 can facilitate the introduction of waste or incompletely reacted substances into the storage cavity 22.

[0035] A method for using a high vacuum sublimation deposition production device for nano silicon carbon negative electrode materials comprises the following steps: S10, loading: The silicon powder and silicon dioxide are introduced into the sublimation crucible 33 through the feeding pipe 31, and the gas source is connected to the gas feeding pipe 43, and the vacuum pump is connected to the gas outlet pipe 41. The deposition housing 10, the storage housing 20 and the sublimation housing 30 are kept sealed. S20, stirring: The feeding pipe 31 is sealed, and the driving servo motor 42 is turned on to make the driving screw 44 rotate back and forth to drive the stirring blade 344 to rotate and stir in the sublimation crucible 33, thereby heating the deposition heating chamber 11 and the sublimation heating chamber 32; S30, vacuum treatment: The recovery pipe 21 and the feeding pipe 31 are sealed, and the deposition housing 10, the storage housing 20, and the sublimation housing 30 are placed in a vacuum state. At the same time, the deposition heating chamber 11 and the sublimation heating chamber 32 are continuously heated, and the temperature of the deposition heating chamber 11 is lower than that of the sublimation heating chamber 32. S40, air supply: The mixed gas is introduced into the deposition heating chamber 11 through the gas feed pipe 43, and the servo motor 42 is driven to be continuously turned on, so that the rotating ring 55 is continuously switched between the rotating state and the lifting state, so that the mixed gas is filled in the deposition heating chamber 11; S50, insulation: After S40 starts, the deposition heating chamber 11 and the sublimation heating chamber 32 are kept warm, and the servo motor 42 is driven to be continuously turned on, so that the rotating ring 55 is continuously switched between the rotating state and the lifting state, so that the mixed gas is filled in the deposition heating chamber 11, and at the same time, the steam in the sublimation crucible 33 is filled in the deposition heating chamber 11 through the distribution pipe 53; S60, Collection: After the steam in the sublimation crucible 33 and the mixed gas have completed contact reaction in S50 , the product is collected and processed through the gas outlet pipe 41 .

[0036] In this embodiment, the above steps achieve multiple technical effects: First, in the charging step, silicon powder and silicon dioxide are introduced into the sublimation crucible 33 according to the ratio, and the gas source is connected to the gas feed pipe 43, and the vacuum pump is connected to the gas outlet pipe 41 to ensure the sealing state between the deposition shell 10, the storage shell 20 and the sublimation shell 30, providing stable conditions for subsequent reactions, thereby improving the efficiency of charging and the sealing performance. Secondly, in the stirring step, the driving screw 44 is driven by the driving servo motor 42 to rotate back and forth, so that the stirring blade 344 rotates and stirs in the sublimation crucible 33, and the deposition heating chamber 11 and the sublimation heating chamber 32 are heated at the same time, ensuring uniform mixing and preheating of the raw materials, thereby improving the uniformity of stirring and heating efficiency. Further, in the vacuum treatment step, the recovery pipe 21 and the feeding pipe 31 are sealed to keep the entire system in a vacuum state, while continuously heating and controlling the temperature of the deposition heating chamber 11 to be lower than that of the sublimation heating chamber 32, providing a suitable temperature gradient for the sublimation process, thereby improving the effect of vacuum treatment and the accuracy of temperature control. In addition, in the gas supply step, the mixed gas is introduced into the deposition heating chamber 11 through the gas feed pipe 43, and the drive servo motor 42 is continuously turned on to switch the rotating ring 55 between the rotating and lifting states to ensure that the mixed gas is evenly distributed in the deposition heating chamber 11, thereby improving the reaction efficiency, thereby achieving the uniformity of gas distribution and the improvement of reaction efficiency. In the heat preservation step, the deposition heating chamber 11 and the sublimation heating chamber 32 are heat-insulated, and at the same time, the rotating ring 55 is continuously switched to ensure that the steam in the sublimation crucible 33 is evenly filled in the deposition heating chamber 11 through the distribution pipe 53, promoting full contact and reaction between the steam and the mixed gas, thereby improving the heat preservation effect and the uniformity of steam distribution. Finally, in the collection step, the product is collected and processed through the gas outlet pipe 41 to ensure the continuity of the production process and the efficient recovery of the product, thereby improving the collection efficiency of the product and the continuity of the production process. In summary, the method of use of the present invention achieves efficient production and high-quality preparation of nano-silicon-carbon negative electrode materials by precisely controlling the parameters and conditions of each step, and has significant technical advantages and application value.

[0037] Specifically, after S60 is completed, the driving servo motor 42 is continuously turned on, so that the rotating ring 55 is in a lifting state, driving the lifting ring 56 to lift and lower on the inner wall surface of the deposition shell 10 to scrape off the residual material, and at the same time, the residual material dropped in the storage shell 20 is recovered through the recovery pipe 21.

[0038] In this embodiment, the servo motor 42 is driven to drive the rotating ring 55 to rise and fall, so that the lifting ring 56 moves on the inner wall surface of the deposition shell 10, effectively scraping off the residual material attached to the inner wall, ensuring the cleanliness of the interior of the deposition shell 10, avoiding the impact of residual materials on subsequent production processes, reducing the corrosion and wear of the equipment caused by material accumulation, extending the service life of the equipment, and reducing the equipment maintenance cost.

[0039] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A high vacuum sublimation deposition production device for nano silicon carbon negative electrode materials, characterized by: It comprises a deposition shell (10), a storage shell (20) is provided at the bottom end of the deposition shell (10), and a sublimation shell (30) is provided at the bottom end of the storage shell (20); The deposition shell (10) is provided with a sealing cover (40), a gas distribution assembly (50) is provided in the deposition shell (10), a guide tube (343) is provided on the sublimation shell (30), a driving screw (44) is provided on the sealing cover (40), the gas distribution assembly (50) is provided on the driving screw (44), the guide tube (343) cooperates with the driving screw (44), and the driving screw (44) rotates, driving the gas distribution assembly (50) to rotate and rise and fall along the axis of the driving screw (44) to evenly distribute the gas, and driving the guide tube (343) to rotate along the axis of the driving screw (44) to evenly distribute the steam.

2. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 1, characterized in that: A heat insulation block (35) is provided on the sublimation housing (30), and the heat insulation block (35) is provided between the sublimation housing (30) and the storage housing (20); A sublimation crucible (33) is provided in the sublimation shell (30), a sublimation heating chamber (32) is provided between the sublimation crucible (33) and the sublimation shell (30), a feeding pipe (31) is provided on the sublimation shell (30), the feeding pipe (31) is communicated with the inner cavity of the sublimation crucible (33), and a sealed feeding cover is provided on the feeding pipe (31).

3. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 2, characterized in that: The surface of the guide tube (343) is evenly provided with a plurality of guide through holes (3431), and the heat insulation block (35) is provided with a guide rotation groove (36); The guide tube (343) is provided with a rotating tube (341) whose inner cavity is connected. The outer wall of the rotating tube (341) is provided with a guiding rotating protrusion ring (3411). The guiding rotating protrusion ring (3411) is rotatably arranged in the guiding rotating groove (36). The rotating tube (341) is provided with a conical guiding cover (34). The conical guiding cover (34) is connected with the inner cavity of the rotating tube (341). The bottom end of the conical guiding cover (34) is provided with a stirring blade (344). The stirring blade (344) is adapted to the inner wall of the sublimation crucible (33).

4. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 3, characterized in that: A sun rotating gear (60) is provided at the bottom end of the driving screw (44), and three sets of planetary rotating gears (61) that mesh with each other are provided on the sun rotating gear (60), and inner gear rings (64) that mesh with each other are provided on the outside of the three sets of planetary rotating gears (61), and a reinforcing rod (63) is provided on the inner gear ring (64), and the reinforcing rod (63) is connected to the inner wall of the deposition shell (10); A planetary connecting rod (62) is provided on the planetary rotating gear (61), a rotating bracket (342) is provided on the rotating tube (341), and the three groups of planetary connecting rods (62) are all rotatably provided on the rotating bracket (342); A protective shell (65) is provided on the reinforcing rod (63), and the protective shell (65) is provided with a first protective inclined surface (651) and a second protective inclined surface (652). The inner gear ring (64) is provided in the protective shell (65), and the driving screw (44) and the rotating bracket (342) are both connected to the protective shell (65) in a rotational sealing manner.

5. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 1, characterized in that: A deposition heating chamber (11) is provided in the deposition shell (10), two groups of guide grooves (12) are symmetrically provided on the inner wall of the deposition shell (10), and the guide grooves (12) are provided in the deposition heating chamber (11); The gas distribution assembly (50) includes a lifting ring (56), the outer wall of the lifting ring (56) is symmetrically provided with two groups of guide protrusions (563), the two groups of guide protrusions (563) are respectively slidably provided in two groups of guide grooves (12), a rotating ring (55) is provided in the lifting ring (56), a plurality of distribution pipes (53) are evenly provided in the rotating ring (55), a driving ring (51) is provided at the center of the rotating ring (55), the driving ring (51) is threadedly sleeved on the outer wall of the driving screw (44), the plurality of distribution pipes (53) are connected to the driving ring (51), and the distribution pipes (53) are evenly provided with a plurality of distribution through holes (54); The rotating ring (55) cooperates with the lifting ring (56) so that the lifting ring (56) moves up and down in the two sets of guide grooves (12).

6. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 5, characterized in that: A movable ring groove (561) is provided in the lifting ring (56), and the rotating ring (55) is rotatably provided in the movable ring groove (561); Two groups of blocking rods (562) are symmetrically arranged in the movable ring groove (561), and two groups of contact protrusions (551) are symmetrically arranged on the outer wall of the rotating ring (55). The contact protrusions (551) are in contact with the blocking rods (562), so that the rotating ring (55) does not rotate around the axis of the driving screw (44).

7. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 6, characterized in that: The outer wall of the driving ring (51) is provided with a connecting sleeve (52) on which a gas connecting pipe (521) is provided. A distribution cavity (512) is provided in the driving ring (51). The outer wall of the driving ring (51) is provided with multiple groups of first connecting through holes (511) and multiple groups of second connecting through holes (513). The multiple groups of first connecting through holes (511) are matched with the multiple groups of distribution pipes (53) in position. The distribution pipes (53) are communicated with the distribution cavity (512) through the first connecting through holes (511). The multiple groups of second connecting through holes (513) are matched with the connecting sleeve (52) in position. The gas connecting pipe (521) is communicated with the distribution cavity (512) through the second connecting through holes (513).

8. The high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 2, characterized in that: The storage shell (20) is in a truncated cone shape, the heat insulation block (35) is provided with a heat insulation slope (351), a storage cavity (22) is provided between the storage shell (20) and the heat insulation block (35), a recovery pipe (21) is provided at the bottom end of the storage shell (20), and a recovery sealing plate is provided at the port of the recovery pipe (21); The sealing cover (40) is provided with a driving servo motor (42), and the driving servo motor (42) is drivingly connected to the driving screw (44). The sealing cover (40) is provided with a gas feed pipe (43), and a high-temperature resistant alloy bellows (45) is provided between the gas feed pipe (43) and the gas connecting pipe (521). The sealing cover (40) is also provided with an air outlet pipe (41), and the air outlet pipe (41) is communicated with the interior of the sealing cover (40).

9. A method for using the high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to any one of claims 1 to 8, characterized in that: The following steps are involved: S10, loading: The silicon powder and silicon dioxide are introduced into the sublimation crucible (33) in a suitable proportion through the feeding pipe (31), the gas source is connected to the gas feeding pipe (43), the vacuum pump is connected to the gas outlet pipe (41), and the deposition housing (10), the storage housing (20) and the sublimation housing (30) are kept sealed; S20, stirring: The feeding pipe (31) is sealed, and the driving servo motor (42) is turned on, so that the driving screw (44) rotates back and forth to drive the stirring blade (344) to rotate and stir in the sublimation crucible (33), and heat the deposition heating chamber (11) and the sublimation heating chamber (32); S30, vacuum treatment: The recovery pipe (21) and the feeding pipe (31) are sealed, and the deposition housing (10), the storage housing (20), and the sublimation housing (30) are placed in a vacuum state. At the same time, the deposition heating chamber (11) and the sublimation heating chamber (32) are continuously heated, and the temperature of the deposition heating chamber (11) is lower than that of the sublimation heating chamber (32); S40, air supply: The mixed gas is introduced into the deposition heating chamber (11) through the gas feed pipe (43), and the servo motor (42) is driven to be continuously turned on, so that the rotating ring (55) is continuously switched between the rotating state and the lifting state, so that the mixed gas is filled in the deposition heating chamber (11); S50, insulation: After S40 starts, the deposition heating chamber (11) and the sublimation heating chamber (32) are subjected to heat preservation treatment, and the servo motor (42) is driven to be continuously turned on, so that the rotating ring (55) is continuously switched between a rotating state and a lifting state, so that the mixed gas is filled in the deposition heating chamber (11), and at the same time, the steam in the sublimation crucible (33) is filled in the deposition heating chamber (11) through the distribution pipe (53); S60, Collection: After the steam in the sublimation crucible (33) and the mixed gas have completed contact reaction in S50, the product is collected and processed through the gas outlet pipe (41).

10. The method for using the high vacuum sublimation deposition production device for nano-silicon-carbon negative electrode materials according to claim 9, characterized in that: After S60 is completed, the driving servo motor (42) is continuously turned on, so that the rotating ring (55) is in a lifting state, driving the lifting ring (56) to lift and lower on the inner wall surface of the deposition shell (10) to scrape off the residual material, and at the same time, the residual material dropped from the storage shell (20) is recovered through the recovery pipe (21).

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