A high-vacuum sublimation deposition production device and method for a nano-silicon-carbon negative electrode material
Patent Information
- Application Number
- CN202510634338.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-16
- Publication Date
- 2026-10-20
- Estimated Expiration
- 2045-05-16
AI Technical Summary
现有的硅碳负极材料制备技术,大多是将纳米硅粉或者一氧化硅粉末与碳源粉末混合烧结制得,部分厂家所采用的气相沉积工艺也是直接往硅基材料的粉体内通入碳源气体来进行沉积碳的包覆,但是在通入碳源气体时容易出现 气体分布不均匀的现象,而且还容易存在硅基粉体团聚,影响纳米硅碳负极材料的性能,鉴于此,本发明提出了一种纳米硅碳负极材料的高真空升华沉积生产装置及方法,以解决上述问题
通过气体分布组件通过旋转和升降的复合运动,能够全方位覆盖沉积壳体内的空间,旋转运动使得混合气体在水平方向上均匀分布,而升降运动则确保混合气体在垂直方向上也能均匀扩散,这种双重运动方式避免了局部混合气体浓度过高或过低的问题,而且也可以对沉积壳体中的混合气体进行搅拌处理,提高混合气体的混合质量,从而为纳米硅碳负极材料的均匀沉积提供了理想的反应环境;
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Figure CN120443113B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to a high-vacuum sublimation deposition apparatus and method for producing nano-silicon-carbon anode materials. Background Technology
[0002] Lithium-ion batteries, as a highly efficient and environmentally friendly energy storage device, have been widely used in electric vehicles, consumer electronics, energy storage systems, and other fields. However, with the continuous expansion of the application fields of lithium-ion batteries, the requirements for their performance are also becoming increasingly stringent, especially in terms of energy density, cycle life, and safety.
[0003] Nano-silicon-carbon anode materials exhibit enormous application potential due to their unique physical and chemical properties. Silicon possesses a high theoretical specific capacity, significantly improving battery energy density, while carbon materials exhibit excellent conductivity and stability, effectively mitigating the volume expansion problem of silicon during charging and discharging. Existing silicon-carbon anode material preparation technologies mostly involve mixing and sintering nano-silicon powder or silicon monoxide powder with carbon source powder. Some manufacturers use vapor deposition processes that directly introduce carbon source gas into the silicon-based material powder to deposit carbon coating. However, uneven gas distribution and silicon-based powder agglomeration are prone to occur during carbon source gas introduction, affecting the performance of nano-silicon-carbon anode materials. Therefore, this invention proposes a high-vacuum sublimation deposition production apparatus and method for nano-silicon-carbon anode materials to solve the above problems. Summary of the Invention
[0004] The purpose of this invention is to provide a high-vacuum sublimation deposition production apparatus and method for nano-silicon-carbon anode materials, so as to solve the problems mentioned in the background art.
[0005] To achieve the above objectives, the present invention provides the following technical solution: A high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials includes a deposition shell, a storage shell at the bottom of the deposition shell, and a sublimation shell at the bottom of the storage shell. A sealing cap is provided on the deposition shell, a gas distribution component is provided inside the deposition shell, a guide tube is provided on the sublimation shell, a drive screw is provided on the sealing cap, the gas distribution component is provided on the drive screw, the guide tube cooperates with the drive screw, the drive screw rotates, causing the gas distribution component to rotate and rise and fall along the axis of the drive screw to uniformly distribute the gas, and causing the guide tube to rotate around the axis of the drive screw to uniformly distribute the vapor.
[0006] As an improvement to the above technical solution, a heat insulation block is provided on the sublimation shell, and the heat insulation block is disposed between the sublimation shell and the storage shell; A sublimation crucible is provided inside the sublimation shell, and a sublimation heating chamber is provided between the sublimation crucible and the sublimation shell. A feeding pipe is provided on the sublimation shell, and the feeding pipe communicates with the inner cavity of the sublimation crucible. A sealed feeding cover is provided on the feeding pipe.
[0007] As an improvement to the above technical solution, the surface of the guide tube is uniformly provided with multiple sets of guide through holes, and the heat insulation block is provided with a guide rotation groove; The guide tube is provided with a rotating tube with an inner cavity. The outer wall of the rotating tube is provided with a guide rotation protrusion ring. The guide rotation protrusion ring is rotatably disposed in the guide rotation 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. The stirring blade is adapted to the inner wall of the sublimation crucible.
[0008] As an improvement to the above technical solution, a solar rotating gear is provided at the bottom end of the drive screw, and three sets of mutually meshing planetary rotating gears are provided on the solar rotating gear. The three sets of planetary rotating gears are provided with mutually meshing internal gear rings on their outer sides, and a reinforcing rod is provided on the internal gear rings. The reinforcing rod is connected to the inner wall of the deposition shell. The planetary rotating gear is provided with planetary connecting rods, and the rotating tube is provided with a rotating bracket. All three sets of planetary connecting rods are rotatably mounted on the rotating bracket. The reinforcing rod is provided with a protective shell, which has a first protective inclined surface and a second protective inclined surface. The internal gear ring is disposed inside the protective shell, and the drive screw and the rotating bracket are rotatably and sealingly connected to the protective shell.
[0009] As an improvement to the above technical solution, a deposition heating chamber is provided inside the deposition shell, and two sets of guide grooves are symmetrically opened on the inner wall of the deposition shell, and the guide grooves are arranged in the deposition heating chamber; The gas distribution assembly includes a lifting ring, with two sets of guide protrusions symmetrically arranged on the outer wall of the lifting ring. The two sets of guide protrusions are slidably arranged in two sets of guide grooves. A rotating ring is arranged inside the lifting ring, and multiple sets of distribution pipes are evenly arranged inside the rotating ring. A driving ring is arranged at the center of the rotating ring, and the driving ring is threaded onto the outer wall of the driving screw. The multiple sets of distribution pipes are all connected to the driving ring, and multiple sets of distribution through holes are evenly opened on the distribution pipes. The rotating ring and the lifting ring work together to allow the lifting ring to move up and down in two sets of guide grooves.
[0010] As an improvement to the above technical solution, a movable ring groove is provided inside the lifting ring, and the rotating ring is rotatably disposed in the movable ring groove; Two sets of blocking rods are symmetrically arranged in the movable ring groove, and two sets of contact protrusions are symmetrically arranged on the outer wall of the rotating ring. The contact protrusions contact the blocking rods, so that the rotating ring does not rotate around the axis of the driving screw.
[0011] As an improvement to the above technical solution, a connecting sleeve is rotatably sleeved on the outer wall of the drive ring, and a gas connecting pipe is provided on the connecting sleeve. A distribution cavity is provided inside the drive ring. Multiple sets of first connecting through holes and multiple sets of second connecting through holes are opened on the outer wall of the drive ring. The multiple sets of first connecting through holes are matched with the positions of multiple sets of distribution pipes. The distribution pipes are connected to the distribution cavity through the first connecting through holes. The multiple sets of second connecting through holes are matched with the positions of the connecting sleeve. The gas connecting pipes are connected to the distribution cavity through the second connecting through holes.
[0012] As an improvement to the above technical solution, the storage shell is frustum-shaped, the heat insulation block is provided with a heat insulation slope, a storage cavity is provided between the storage shell and the heat insulation block, a recycling pipe is provided at the bottom of the storage shell, and a recycling sealing plate is provided at the port of the recycling pipe. The sealing cover is equipped with a drive servo motor, which is connected to a drive screw. The sealing cover is also equipped with a gas inlet pipe, and a high-temperature resistant alloy corrugated pipe is installed between the gas inlet pipe and the gas connection pipe. The sealing cover is also equipped with an outlet pipe, which is connected to the inside of the sealing cover.
[0013] A method for using a high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials includes the following steps: S10, Loading: Silicon powder and silicon dioxide are fed into the sublimation crucible through a feeding pipe in the specified proportions. The gas source is connected to the gas feed pipe, and the vacuum pump is connected to the gas outlet pipe. The deposition shell, storage shell, and sublimation shell are kept in a sealed state. S20, Stirring: The feeding pipe is sealed, and the drive servo motor is turned on, so that the drive screw reciprocates and drives the stirring blade to rotate and stir in the sublimation crucible, and heats the deposition heating chamber and the sublimation heating chamber. S30, Vacuum treatment: The recovery pipe and the feeding pipe are sealed, and the deposition shell, storage shell and sublimation shell are kept 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, Gas delivery: The mixed gas is introduced into the deposition heating chamber through the gas feed pipe, and the servo motor is continuously turned on, so that the rotating ring switches between rotating and lifting states, so that the mixed gas fills the deposition heating chamber. S50, Insulation: After S40 starts, the deposition heating chamber and sublimation heating chamber are kept warm, and the servo motor is continuously turned on, so that the rotating ring switches between rotating and lifting states, so that the mixed gas fills the deposition heating chamber, and at the same time, the vapor in the sublimation crucible fills the deposition heating chamber through the distribution pipe. S60, Collection: After the vapor in the sublimation crucible in S50 has reacted with the mixed gas, the product is collected and processed through the outlet pipe.
[0014] As an improvement to the above technical solution, after S60 is completed, the drive servo motor is continuously turned on, so that the rotating ring is in a lifting state, which drives the lifting ring to rise and fall on the inner wall surface of the deposition shell to scrape off the residual material. At the same time, the residual material that falls into the storage shell is recycled through the recycling pipe.
[0015] Compared with the prior art, the beneficial effects of the present invention are: The gas distribution component, through a combination of rotation and lifting motion, can cover the space inside the deposition shell in all directions. The rotational motion ensures that the mixed gas is evenly distributed in the horizontal direction, while the lifting motion ensures that the mixed gas is also evenly diffused in the vertical direction. This dual motion method avoids the problem of excessively high or low local mixed gas concentrations, and can also stir the mixed gas in the deposition shell to improve the mixing quality of the mixed gas, thus providing an ideal reaction environment for the uniform deposition of nano-silicon-carbon anode materials. The combined motion of rotation and lifting can also precisely control the lifting and rotation speed of the gas distribution component, enabling precise control of gas flow and distribution. This not only improves reaction efficiency but also ensures full contact and reaction between the mixed gas and steam during the reaction process, thereby enhancing the performance and consistency of the nano-silicon-carbon anode material. By rotating the guide tube, the vapor generated in the sublimation shell can be uniformly guided to the deposition shell. This uniformly distributed vapor comes into full contact with the mixed gas, avoiding the problem of excessively high or low local vapor concentration, thereby improving the uniformity and consistency of the reaction. Moreover, it can promote the dynamic mixing of vapor in the deposition shell, accelerate the reaction rate, effectively improve production efficiency, and reduce reaction time. By simultaneously driving the gas distribution component and the guide tube with a drive screw, their coordinated movement is achieved. This ensures a highly synchronized distribution of the mixed gas and vapor within the deposition shell, avoiding uneven distribution caused by asynchronous movement. Furthermore, driving both the gas distribution component and the guide tube with a single drive screw reduces the complexity of the drive system. This design not only lowers manufacturing costs but also reduces potential failure points, improving reliability and ease of maintenance. Using a single drive screw to drive multiple components reduces energy loss during transmission, enhancing the overall energy efficiency of the device. The rotational speed of the drive screw can be adjusted according to process requirements, precisely controlling the distribution speed and range of the mixed gas and vapor. This flexibility allows the device to adapt to different reaction conditions and optimize the reaction process. Attached Figure Description
[0016] Figure 1 This is a schematic diagram of the structure of the present invention; Figure 2 For the present invention Figure 1 Sectional view of AA; Figure 3 This is a schematic diagram of the deposition shell structure of the present invention; Figure 4 For the present invention Figure 3 Sectional view of BB; Figure 5 This is a three-dimensional structural schematic diagram of the deposition shell of the present invention; Figure 6 This is a schematic diagram showing the positions of the drive screw and gas distribution assembly of the present invention; Figure 7 For the present invention Figure 6 Enlarged structural diagram at point C; Figure 8 This is a schematic diagram showing the positions of the lifting ring and the rotating ring of the present invention; Figure 9 This is a schematic diagram of the lifting ring structure of the present invention; Figure 10 For the present invention Figure 9 Enlarged structural diagram at point D; Figure 11 This is a schematic diagram of the rotating ring structure of the present invention; Figure 12 This is a front view of the lifting ring of the present invention; Figure 13 For the present invention Figure 12 Sectional view of EE; Figure 14 This is a cross-sectional schematic diagram of the drive ring of the present invention; Figure 15 This is a schematic diagram showing the positions of the conical guide cover and the stirring blade of the present invention; Figure 16 For the present invention Figure 15 Enlarged structural diagram at point F; Figure 17 This is a schematic diagram of the internal structure of the protective housing of the present invention; Figure 18 For the present invention Figure 17 A magnified structural diagram of point G in the middle.
[0017] In the diagram: 10. Deposition shell; 11. Deposition heating chamber; 12. Guide groove; 20. Storage shell; 21. Recovery pipe; 22. Storage cavity; 30. Sublimation shell; 31. Feed pipe; 32. Sublimation heating chamber; 33. Sublimation crucible; 34. Conical guide shroud; 341. Rotating tube; 3411. Guide rotation protrusion ring; 342. Rotating support; 343. Guide tube; 3431. Guide through hole; 344. Stirring blade; 35. Heat insulation block; 351. Heat insulation slope; 36. Rotating groove; 40. Sealing cap; 41. Gas outlet pipe; 42. Drive servo motor; 43. Gas feed pipe; 44. Drive 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 connection pipe; 53. Distribution pipe; 54. Distribution through hole; 55. Rotating ring; 551. Contact protrusion; 56. Lifting ring; 561. Movable ring groove; 562. Barrier rod; 563. Guide protrusion; 60. Sun rotating gear; 61. Planetary rotating gear; 62. Planetary connecting rod; 63. Reinforcing rod; 64. Internal gear ring; 65. Protective shell; 651. First protective inclined surface; 652. Second protective inclined surface. Detailed Implementation
[0018] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0019] Example: like Figure 1-18 As shown, this embodiment proposes a high-vacuum sublimation deposition production device for nano-silicon-carbon anode materials, including a deposition shell 10, a storage shell 20 at the bottom end of the deposition shell 10, and a sublimation shell 30 at the bottom end of the storage shell 20. A sealing cap 40 is provided on the deposition shell 10, a gas distribution assembly 50 is provided inside the deposition shell 10, a guide tube 343 is provided on the sublimation shell 30, a drive screw 44 is provided on the sealing cap 40, the gas distribution assembly 50 is provided on the drive screw 44, the guide tube 343 cooperates with the drive screw 44, the drive screw 44 rotates, causing the gas distribution assembly 50 to rotate and rise and fall along the axis of the drive screw 44 to uniformly distribute the gas, and causing the guide tube 343 to rotate around the axis of the drive screw 44 to uniformly distribute the vapor.
[0020] In this embodiment, when producing nano-silicon-carbon anode material, mixed powder is placed in the sublimation shell 30 and the whole is vacuumed. At the same time, the deposition shell 10 and the sublimation shell 30 are heated so that the temperature in the sublimation shell 30 is higher than the temperature in the deposition shell 10. Then, mixed gas is injected into the deposition shell 10 through the gas distribution component 50, and the screw 44 is driven to rotate. The gas distribution component 50 is driven 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. Meanwhile, the mixed powder heated in the sublimation shell 30 generates vapor, which is evenly distributed in the deposition shell 10 through the rotating guide tube 343 and reacts in the deposition shell 10. After the reaction, the product is collected. The gas distribution component 50 can cover the space inside the deposition shell 10 in all directions through a combination of rotation and lifting motion. The rotational motion ensures that the mixed gas is evenly distributed in the horizontal direction, while the lifting motion ensures that the mixed gas is also evenly diffused in the vertical direction. This dual motion method avoids the problem of local mixed gas concentration being too high or too low. It can also stir the mixed gas in the deposition shell 10 to improve the mixing quality of the mixed gas, thereby providing an ideal reaction environment for the uniform deposition of nano-silicon-carbon anode materials. The combined motion of rotation and lifting can also precisely control the lifting and rotation speed of the gas distribution component 50, enabling precise control of gas flow and distribution. This not only improves reaction efficiency but also ensures full contact and reaction between the mixed gas and steam during the reaction process, thereby enhancing the performance and consistency of the nano-silicon-carbon anode material. By rotating the guide tube 343, the steam generated in the sublimation shell 30 can be uniformly guided to the deposition shell 10. This uniformly distributed steam comes into full 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. Moreover, it can promote the dynamic mixing of steam in the deposition shell 10 and accelerate the reaction rate, which can effectively improve production efficiency and reduce reaction time. By simultaneously driving the gas distribution assembly 50 and the guide pipe 343 to rotate via the drive screw 44, their coordinated movement is achieved. This ensures a highly synchronized distribution process of the mixed gas and vapor within the deposition shell 10, avoiding uneven distribution caused by asynchronous movement. Furthermore, driving both the gas distribution assembly 50 and the guide pipe 343 via a single drive screw 44 reduces the complexity of the drive system. This design not only lowers the manufacturing cost of the device but also reduces system failure points, improving reliability and ease of maintenance. Using a single drive screw 44 to drive multiple components reduces energy loss during transmission. This efficient power transmission method improves the overall energy efficiency of the device. Moreover, the rotational speed of the drive screw 44 can be adjusted according to process requirements, thereby precisely controlling the distribution speed and range of the mixed gas and vapor. This flexibility allows the device to adapt to different reaction conditions and optimize the reaction process.
[0021] Specifically, a heat insulation block 35 is provided on the sublimation shell 30, and the heat insulation block 35 is disposed between the sublimation shell 30 and the storage shell 20; A sublimation crucible 33 is provided inside the sublimation shell 30, and 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, and the feeding pipe 31 communicates with the inner cavity of the sublimation crucible 33. A sealed feeding cover plate is provided on the feeding pipe 31.
[0022] In this embodiment, the heat insulation block 35 is made of heat insulation material. The mixed powder is loaded 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 plate. Of course, when heating the sublimation shell 30, the heating position is located in the sublimation heating chamber 32 to heat the sublimation crucible 33.
[0023] Specifically, the surface of the guide tube 343 is uniformly provided with multiple sets 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 with an inner cavity. The outer wall of the rotating tube 341 is provided with a guide rotation protrusion ring 3411. The guide rotation protrusion ring 3411 is rotatably disposed in the guide rotation 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 drive 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. This promotes the full mixing of steam and gas in the deposition shell, accelerates the reaction rate, and improves the production efficiency and quality of nano-silicon-carbon anode materials. The conical guide cover 34 can evenly guide the steam generated in the sublimation crucible 33 to the deposition shell 10 by rotating. Its conical structure itself has good guiding performance. Combined with the rotational motion, it can effectively avoid local steam accumulation and ensure the uniform distribution of steam in the deposition shell 10. Of course, when the rotating tube 341 rotates, it drives the conical guide cover 34 and the stirring blade 344 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. Moreover, it can stir the mixed powder in the sublimation crucible 33 to make it fully mixed, avoiding the accumulation or uneven distribution of nano-sized materials, thereby improving the uniformity of the sublimation process. At the same time, it makes the contact between the mixed powder and the inner wall of the sublimation crucible 33 more sufficient, accelerating the heat transfer and improving the heating efficiency of the material.
[0025] Specifically, a solar rotating gear 60 is provided at the bottom end of the drive screw 44, and three sets of mutually meshing planetary rotating gears 61 are provided on the solar rotating gear 60. The three sets of planetary rotating gears 61 are provided with mutually meshing internal gear rings 64, and a reinforcing rod 63 is provided on the internal gear ring 64. The reinforcing rod 63 is connected to the inner wall of the deposition shell 10. The planetary rotating gear 61 is provided with a planetary connecting rod 62, and the rotating tube 341 is provided with a rotating bracket 342. All three sets of planetary connecting rods 62 are rotatably mounted on the rotating bracket 342. The reinforcing rod 63 is provided with a protective shell 65, which is provided with a first protective inclined surface 651 and a second protective inclined surface 652. The internal gear ring 64 is provided inside the protective shell 65. The driving screw 44 and the rotating bracket 342 are rotatably and sealingly connected to the protective shell 65.
[0026] In this embodiment, the cooperation between the planetary rotating gear 61, the sun rotating gear 60, and the internal gear ring 64 facilitates the slow rotation of the rotating tube 341, enabling it to guide steam more smoothly through the guide tube 343 into the deposition shell 10. This avoids localized accumulation or uneven distribution of steam due to excessive rotation, thereby further improving the uniformity of the reaction. Moreover, it can 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 encloses the inner gear ring 64, forming a sealed space, preventing 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 steam during the high vacuum sublimation deposition process; Of course, the protective shell 65 uses high-temperature resistant heat insulation material, which can maintain the internal temperature stability and reduce the sudden temperature drop caused by heat exchange; The first protective inclined surface 651 and the second protective inclined surface 652 form a streamlined flow guiding structure, which allows steam to slide along the inclined surface and guides the steam away from the surface of the protective shell 65, preventing steam from being trapped or penetrating into the inner tooth ring area. During the operation of the gear system, vibrations are generated, which are transmitted to the protective housing 65 through the reinforcing rod 63. This enables the automatic shaking off and recovery of materials on the protective housing 65 for subsequent recycling and reuse processes.
[0027] Specifically, a deposition heating chamber 11 is provided inside the deposition shell 10, and two sets of guide grooves 12 are symmetrically opened on the inner wall of the deposition shell 10. The guide grooves 12 are disposed in the deposition heating chamber 11. The gas distribution assembly 50 includes a lifting ring 56. Two sets of guide protrusions 563 are symmetrically arranged on the outer wall of the lifting ring 56. The two sets of guide protrusions 563 are slidably arranged in two sets of guide grooves 12. A rotating ring 55 is arranged inside the lifting ring 56. Multiple sets of distribution pipes 53 are evenly arranged inside the rotating ring 55. A driving ring 51 is arranged at the center of the rotating ring 55. The driving ring 51 is threaded onto the outer wall of the driving screw 44. Multiple sets of distribution pipes 53 are connected to the driving ring 51. Multiple sets of distribution through holes 54 are evenly opened on the distribution pipes 53. 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.
[0028] In this case, the temperature inside the deposition heating chamber 11 is kept at 600-800℃ and then kept at 1000-1200℃, and the temperature inside the sublimation heating chamber 32 is always higher than the temperature inside the deposition heating chamber 11.
[0029] Specifically, the lifting ring 56 is provided with a movable ring groove 561, and the rotating ring 55 is rotatably disposed in the movable ring groove 561; Two sets of blocking rods 562 are symmetrically arranged inside the movable ring groove 561, and two sets of contact protrusions 551 are symmetrically arranged on the outer wall of the rotating ring 55. The contact protrusions 551 contact 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 shell 10 is switched between a rotating state and a lifting state, the drive screw 44 rotates. Since the drive ring 51 is threaded on the outer wall of the drive screw 44, the drive ring 51 rotates with the drive screw 44, thereby adjusting the position of the distribution pipe 53 according to the rotation of the drive screw 44. When the contact protrusion 551 contacts the blocking rod 562, under the sliding cooperation of the guide protrusion 563 and the guide groove 12, the rotating ring 55 does not rotate with the rotation of the drive screw 44. At the same time, the rotating ring 55 moves up and down along the axis of the drive screw 44, thereby changing the state. By setting a movable ring groove 561 in the lifting ring 56 and a blocking rod 562 in the movable ring groove 561, and setting a contact protrusion 551 on the outer wall of the rotating ring 55, the rotating ring 55 can achieve a compound motion of rotation and lifting when the driving screw 44 rotates. This compound motion mode enables the gas distribution component 50 to perform all-round gas distribution in the deposition shell 10, ensuring that the mixed gas diffuses evenly in the horizontal and vertical directions. Moreover, the motion state can 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 interaction between mechanical parts, 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 unreacted substances attached to the inner wall of the deposition shell 10. Through the scraping action 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 inside of the deposition shell 10 clean, reduce pollution and equipment failure 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 rotatably sleeved on the outer wall of the drive ring 51, and a gas connecting pipe 521 is provided on the connecting sleeve 52. A distribution cavity 512 is provided inside the drive ring 51. Multiple sets of first connecting through holes 511 and multiple sets of second connecting through holes 513 are opened on the outer wall of the drive ring 51. The multiple sets of first connecting through holes 511 are matched with multiple sets of distribution pipes 53. The distribution pipes 53 are connected to the distribution cavity 512 through the first connecting through holes 511. The multiple sets of second connecting through holes 513 are matched with the connecting sleeve 52. The gas connecting pipe 521 is connected to the distribution cavity 512 through the second connecting through holes 513.
[0032] In this embodiment, when the mixed gas is introduced into the distribution pipe 53, the mixed gas first enters the gas connection pipe 521. Since the drive ring 51 is in a rotating state, when the gas connection pipe 521 is connected to the second connection through hole 513, the mixed gas enters the distribution cavity 512 and enters the multiple distribution pipes 53 through the multiple sets of first connection through holes 511 respectively, and is evenly distributed inside the deposition heating cavity 11 through the distribution pipes 53.
[0033] Specifically, the storage housing 20 is frustum-shaped, the heat insulation block 35 is provided with a heat insulation slope 351, a storage cavity 22 is provided between the storage housing 20 and the heat insulation block 35, a recycling pipe 21 is provided at the bottom end of the storage housing 20, and a recycling sealing plate is provided at the port of the recycling pipe 21. The sealing cover 40 is provided with a drive servo motor 42, which is connected to the drive screw 44. The sealing cover 40 is provided with a gas inlet pipe 43, and a high-temperature resistant alloy corrugated pipe 45 is provided between the gas inlet pipe 43 and the gas connection pipe 521. The sealing cover 40 is also provided with an outlet pipe 41, which is connected to the inside 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 installed on the powder collector, and a tail gas treatment device is installed at the outlet of the vacuum pump. Of course, in this case, the mixed gas supplied in the mixed gas supply tank is one or more of carbon source gas, carrier gas, and reducing gas. Specifically, the carbon source gas is one or more of hydrocarbon gases such as natural gas, propylene, propane, and acetylene; the carrier gas is one of high-purity nitrogen and high-purity argon; and the reducing gas is one of hydrogen and carbon monoxide. Of course, in this case, the mixed powder 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 alloy corrugated pipe 45 through the gas feed pipe 43 and is introduced into the gas connection pipe 521. It is uniformly distributed by the gas distribution component 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 unreacted substances in the storage shell 20 can be recycled by opening the recycling cover on the recycling pipe 21, so as to carry out reasonable recycling and reuse of resources. The heat insulation slope 351 can facilitate the introduction of waste or unreacted substances into the storage cavity 22.
[0035] A method for using a high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials includes the following steps: S10, Loading: 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 feed pipe 43, the vacuum pump is connected to the gas outlet pipe 41, and the deposition shell 10, storage shell 20 and sublimation shell 30 are kept in a sealed state. S20, Stirring: The feeding pipe 31 is sealed, and the drive servo motor 42 is turned on, so that the drive screw 44 reciprocates and drives the stirring blade 344 to rotate and stir in the sublimation crucible 33, and heats the deposition heating chamber 11 and the sublimation heating chamber 32. S30, Vacuum treatment: The recycling pipe 21 and the feeding pipe 31 are sealed, and the deposition shell 10, the storage shell 20 and the sublimation shell 30 are 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, Gas delivery: The mixed gas is introduced into the deposition heating chamber 11 through the gas feed pipe 43, and the servo motor 42 is continuously turned on, so that the rotating ring 55 continuously switches between rotating and lifting states, so that the mixed gas fills 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 continuously turned on, so that the rotating ring 55 switches between rotating and lifting states, so that the mixed gas fills the deposition heating chamber 11, and at the same time, the vapor in the sublimation crucible 33 fills the deposition heating chamber 11 through the distribution pipe 53. S60, Collection: After the vapor in the sublimation crucible 33 in S50 comes into contact with the mixed gas and reacts, 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 loading step, silicon powder and silicon dioxide are introduced into the sublimation crucible 33 according to the specified 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. This ensures a sealed state between the deposition shell 10, the storage shell 20, and the sublimation shell 30, providing stable conditions for subsequent reactions, thereby improving the loading efficiency and sealing performance. Second, in the stirring step, the drive servo motor 42 drives the drive screw 44 to reciprocate, causing the stirring blades 344 to rotate and stir in the sublimation crucible 33. At the same time, the deposition heating chamber 11 and the sublimation heating chamber 32 are heated to ensure uniform mixing and preheating of the raw materials, thereby improving the uniformity of stirring and heating efficiency. Furthermore, in the vacuum treatment step, the recovery pipe 21 and the feeding pipe 31 are sealed to put the entire system under vacuum. At the same time, the temperature of the deposition heating chamber 11 is continuously heated and controlled to be lower than that of the sublimation heating chamber 32, providing a suitable temperature gradient for the sublimation process, thereby improving the vacuum treatment effect and the accuracy of temperature control. Furthermore, in the gas feeding 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 activated, causing the rotating ring 55 to continuously switch between rotation and lifting states. This ensures that the mixed gas is evenly distributed in the deposition heating chamber 11, improving reaction efficiency and thus achieving uniform gas distribution and improved reaction efficiency. In the heat preservation step, the deposition heating chamber 11 and the sublimation heating chamber 32 are heat-preserved, while the rotating ring 55 continuously switches states. This ensures that the vapor in the sublimation crucible 33 is evenly filled into the deposition heating chamber 11 through the distribution pipe 53, promoting sufficient contact and reaction between the vapor and the mixed gas, thereby improving the heat preservation effect and the uniformity of vapor distribution. Finally, in the collection step, the product is collected through the gas outlet pipe 41, ensuring the continuity of the production process and the efficient recovery of the product, thereby improving the product collection efficiency and the continuity of the production process. In summary, the method of the present invention, by precisely controlling the parameters and conditions of each step, achieves efficient production and high-quality preparation of nano-silicon-carbon anode materials, possessing significant technical advantages and application value.
[0037] Specifically, after S60 is completed, the drive 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. At the same time, the residual material that falls into the storage shell 20 is recycled through the recycling pipe 21.
[0038] In this embodiment, the servo motor 42 drives 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 inside of the deposition shell 10, avoiding the impact of residual material on the subsequent production process, 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] Although embodiments of the 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 invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials, characterized in that: It includes 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). A sealing cap (40) is provided on the deposition shell (10), a gas distribution assembly (50) is provided inside the deposition shell (10), a guide tube (343) is provided on the sublimation shell (30), a drive screw (44) is provided on the sealing cap (40), the gas distribution assembly (50) is provided on the drive screw (44), the guide tube (343) cooperates with the drive screw (44), the drive screw (44) rotates, causing the gas distribution assembly (50) to rotate and rise and fall along the axis of the drive screw (44) to uniformly distribute the gas, and causing the guide tube (343) to rotate around the axis of the drive screw (44) to uniformly distribute the steam.
2. The high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to claim 1, characterized in that: A heat insulation block (35) is provided on the sublimation shell (30), and the heat insulation block (35) is disposed between the sublimation shell (30) and the storage shell (20); A sublimation crucible (33) is provided inside 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 connected to the inner cavity of the sublimation crucible (33). A sealed feeding cover is provided on the feeding pipe (31).
3. The high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to claim 2, characterized in that: The surface of the guide tube (343) is uniformly provided with multiple sets 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) with an inner cavity connected. The outer wall of the rotating tube (341) is provided with a guide rotating protrusion ring (3411). The guide rotating protrusion ring (3411) is rotatably disposed in the guide 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).
4. The high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to claim 3, characterized in that: The bottom end of the drive screw (44) is provided with a solar rotating gear (60), and the solar rotating gear (60) is provided with three sets of mutually meshing planetary rotating gears (61). The three sets of planetary rotating gears (61) are provided with mutually meshing internal gear rings (64), and the internal gear rings (64) are provided with reinforcing rods (63). The reinforcing rods (63) are connected to the inner wall of the deposition shell (10). The planetary rotating gear (61) is provided with planetary connecting rods (62), and the rotating tube (341) is provided with a rotating bracket (342). All three sets of planetary connecting rods (62) are rotatably mounted on the rotating bracket (342). The reinforcing rod (63) is provided with a protective shell (65), the protective shell (65) is provided with a first protective inclined surface (651) and a second protective inclined surface (652), the internal gear ring (64) is provided inside the protective shell (65), and the driving screw (44) and the rotating bracket (342) are rotatably and sealingly connected to the protective shell (65).
5. The high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to claim 1, characterized in that: The deposition shell (10) is provided with a deposition heating chamber (11), and two sets of guide grooves (12) are symmetrically opened on the inner wall of the deposition shell (10). The guide grooves (12) are arranged in the deposition heating chamber (11). The gas distribution assembly (50) includes a lifting ring (56), and two sets of guide protrusions (563) are symmetrically arranged on the outer wall of the lifting ring (56). The two sets of guide protrusions (563) are slidably arranged in two sets of guide grooves (12). A rotating ring (55) is arranged inside the lifting ring (56). Multiple sets of distribution pipes (53) are evenly arranged inside the rotating ring (55). A driving ring (51) is arranged at the center of the rotating ring (55). The driving ring (51) is threaded onto the outer wall of the driving screw (44). Multiple sets of distribution pipes (53) are all connected to the driving ring (51). Multiple sets of distribution through holes (54) are evenly opened on the distribution pipes (53). 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 apparatus for nano-silicon-carbon anode materials according to claim 5, characterized in that: The lifting ring (56) is provided with a movable ring groove (561), and the rotating ring (55) is rotatably disposed in the movable ring groove (561); Two sets of blocking rods (562) are symmetrically arranged in the movable ring groove (561), and two sets of contact protrusions (551) are symmetrically arranged on the outer wall of the rotating ring (55). The contact protrusions (551) contact 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 apparatus for nano-silicon-carbon anode materials according to claim 6, characterized in that: The outer wall of the drive ring (51) is rotatably fitted with a connecting sleeve (52), and a gas connecting pipe (521) is provided on the connecting sleeve (52). A distribution cavity (512) is provided inside the drive ring (51). Multiple sets of first connecting through holes (511) and multiple sets of second connecting through holes (513) are opened on the outer wall of the drive ring (51). The multiple sets of first connecting through holes (511) are matched with multiple sets of distribution pipes (53). The distribution pipes (53) are connected to the distribution cavity (512) through the first connecting through holes (511). The multiple sets of second connecting through holes (513) are matched with the connecting sleeve (52). The gas connecting pipe (521) is connected to the distribution cavity (512) through the second connecting through holes (513).
8. The high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to claim 2, characterized in that: The storage housing (20) is frustum-shaped, the heat insulation block (35) is provided with a heat insulation slope (351), a storage cavity (22) is provided between the storage housing (20) and the heat insulation block (35), a recycling pipe (21) is provided at the bottom of the storage housing (20), and a recycling sealing plate is provided at the port of the recycling pipe (21). A drive servo motor (42) is provided on the sealing cover (40), and the drive servo motor (42) is connected to the drive screw (44). A gas feed pipe (43) is provided on the sealing cover (40), and a high-temperature resistant alloy corrugated pipe (45) is provided between the gas feed pipe (43) and the gas connection pipe (521). An exhaust pipe (41) is also provided on the sealing cover (40), and the exhaust pipe (41) is connected to the inside of the sealing cover (40).
9. A method of using a high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to any one of claims 1-8, characterized in that: Includes the following steps: S10, Loading: Silicon powder and silicon dioxide are introduced into the sublimation crucible (33) through the feeding pipe (31) according to the ratio, and the gas source is connected to the gas feed pipe (43), the vacuum pump is connected to the gas outlet pipe (41), and the deposition shell (10), storage shell (20) and sublimation shell (30) are kept in a sealed state. S20, Stirring: The feeding pipe (31) is sealed and the drive servo motor (42) is turned on, so that the drive screw (44) reciprocates and drives the stirring blade (344) to rotate and stir in the sublimation crucible (33), and heats the deposition heating chamber (11) and the sublimation heating chamber (32); S30, Vacuum treatment: The recycling pipe (21) and the feeding pipe (31) are sealed, and the deposition shell (10), the storage shell (20) and the sublimation shell (30) are 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, Gas delivery: The mixed gas is introduced into the deposition heating chamber (11) through the gas feed pipe (43), and the servo motor (42) is continuously turned on, so that the rotating ring (55) switches between rotating and lifting states, so that the mixed gas fills the deposition heating chamber (11); S50, Insulation: After S40 starts, the deposition heating chamber (11) and sublimation heating chamber (32) are kept warm, and the servo motor (42) is continuously turned on, so that the rotating ring (55) switches between rotating and lifting states, so that the mixed gas fills the deposition heating chamber (11), and at the same time, the vapor in the sublimation crucible (33) fills the deposition heating chamber (11) through the guide pipe (343); S60, Collection: After the vapor in the sublimation crucible (33) in S50 comes into contact with the mixed gas and reacts, the product is collected and processed through the gas outlet pipe (41).
10. The method of using the high-vacuum sublimation deposition production apparatus for nano-silicon-carbon anode materials according to claim 9, characterized in that: After S60 is completed, the drive servo motor (42) is continuously turned on, so that the rotating ring (55) is in a lifting state, and the lifting ring (56) is driven to lift and lower on the inner wall surface of the deposition shell (10) to scrape off the residual material. At the same time, the residual material falling into the storage shell (20) is recycled through the recycling pipe (21).
Citation Information
Patent Citations
Nanometer silicon-carbon anode material production device and production process thereof
CN110137446A
Device and preparation method for improving deposition efficiency of silicon-carbon negative electrode prepared by CVD (Chemical Vapor Deposition)
CN119685796A