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CN120413617A - Silicon negative electrode CVD and carbon coating equipment and continuous mass production method - Google Patents

Silicon negative electrode CVD and carbon coating equipment and continuous mass production method

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Publication number
CN120413617A
CN120413617A CN202510906239.3A CN202510906239A CN120413617A CN 120413617 A CN120413617 A CN 120413617A CN 202510906239 A CN202510906239 A CN 202510906239A CN 120413617 A CN120413617 A CN 120413617A
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China
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reactor
silicon
carbon
chamber
fluidization chamber
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CN202510906239.3A
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CN120413617B (en
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王雄鹰
王冬阳
黄文伟
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Foshan Junying Environmental Energy Equipment Co ltd
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Foshan Junying Environmental Energy Equipment Co ltd
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Abstract

The invention relates to a silicon cathode CVD and carbon coating device and a continuous mass production method, which relate to the field of silicon cathode production, one end of a reactor is rotationally connected and communicated with a carbon frame feeding device, the other end of the reactor extends into a fluidization chamber and is rotationally connected with the upper part of the fluidization chamber, the side wall of the other end of the reactor is provided with a plurality of fluidization holes, one end of the reactor is also provided with a suction hole, the air suction hole is communicated with the upper part of the fluidization chamber through an exhaust fan, the upper part of the fluidization chamber is provided with an upper air inlet hole, monosilane and nitrogen are introduced into the upper air inlet hole, the lower part of the fluidization chamber is provided with a lower air inlet hole, acetylene and nitrogen are introduced into the lower air inlet hole, the bottom of the fluidization chamber is provided with a discharge hole, and the heater is fixedly connected with the inner wall of the fluidization chamber. The reactor and the fluidization chamber are in a high-temperature low-oxygen environment, and can continuously produce the silicon negative electrode product in the reactor and the fluidization chamber without stopping, so that the yield of the silicon negative electrode is improved, the production cost is reduced, and the silicon negative electrode can be produced and used in a large scale.

Description

Silicon cathode CVD and carbon cladding equipment and continuous mass production method
Technical Field
The invention relates to the field of silicon cathode production, in particular to silicon cathode CVD and carbon cladding equipment and a continuous mass production method.
Background
The gram capacity of the traditional graphite cathode is only about 370mAh/g, and the layered structure limits the adsorption capacity of lithium ions, so that the charging speed is low. In addition, graphite negative pole still has the potential safety hazard of easily starting to fire. Silicon-carbon anodes, by contrast, exhibit significant advantages in that the gram capacity of silicon can be as high as 4200mAh/g, and in that the porous structure of carbon-based materials makes it faster to charge than graphite. However, silicon expands more than 3 times in volume after charging, and when used alone, there is a risk of explosion, and the porous structure of the carbon matrix can alleviate this problem to some extent. The silicon-carbon negative electrode takes a porous carbon frame structure (or called a carbon base frame, a carbon skeleton and the like) as a matrix, and can provide a porous expandable space, so that the structural stability and the performance of a negative electrode material are ensured. Wherein the carbon skeleton can be made of resin, coconut shell and other materials.
Currently, the industrialized application of silicon carbon cathodes presents challenges. The silicon-based material has low yield and higher cost, and affects the large-scale application.
CVD (chemical vapor deposition) is one of the main methods for preparing silicon carbon anode materials in terms of production process. The process takes monosilane (SiH 4) as a raw material, and decomposes the monosilane into elemental silicon by heating, so that the elemental silicon is deposited on a carbon frame to obtain a deposited product, and a layer of elemental carbon (carbon coating) is also required to be coated on the outer side of the deposited product so as to protect the deposited product inside.
The choice of CVD production facilities is usually made from both rotary kilns and fluidised beds. 1. The rotary kiln is suitable for large production, but only 1kg can be produced in one production, which takes 8 hours, and the silane has inflammable and explosive properties in an aerobic environment, so that the production risk exists, and the rotary kiln needs to be carried out under the condition of sealing and pressurizing, so that continuous production cannot be realized. Meanwhile, the rotary kiln has the problems of dead angle, uneven reaction and the like, and the yield is difficult to improve through amplifying equipment. 2. Fluidized bed equipment has obvious advantages in aspects of product quality uniformity and the like, but has the bottleneck that continuous production is not possible and mass production is difficult. The fluidized bed CVD process needs to premix raw materials, then carries out a heating and cooling process to complete one-time CVD (commonly called as one pot), takes 6 to 8 hours, and the single machine yield is currently less than 10 Kg/pot.
In addition, in the prior art, the CVD and carbon coating processes are implemented by two sets of independent equipment, and because the CVD production equipment cannot realize continuous production, the sealed CVD production equipment needs to be opened after each CVD production equipment produces a deposited product, and the deposited product is taken out and then put into the carbon coating production equipment, so that the production time and cost are greatly increased, and the production cost of a silicon-carbon anode (hereinafter referred to as a silicon anode) is high, so that the silicon-carbon anode is difficult to apply on a large scale.
Disclosure of Invention
The invention aims to solve the technical problem of how to continuously produce a silicon anode.
The technical scheme includes that the silicon cathode CVD and carbon coating equipment comprises a carbon frame feeding device, a reactor, a fluidization chamber, a heater and an exhaust fan, wherein one end of the reactor is rotationally connected and communicated with the carbon frame feeding device, the other end of the reactor stretches into the fluidization chamber and is rotationally connected with the upper part of the fluidization chamber, a plurality of fluidization holes are formed in the side wall of the other end of the reactor, one end of the reactor is also provided with an air suction hole, the air suction hole is communicated with the upper part of the fluidization chamber through the exhaust fan, an upper air inlet hole is formed in the upper part of the fluidization chamber and is used for introducing monosilane and nitrogen, a lower air inlet hole is formed in the lower part of the fluidization chamber and is used for introducing acetylene and nitrogen, a discharge hole is formed in the bottom of the fluidization chamber, and the heater is fixedly connected with the inner wall of the fluidization chamber.
The invention has the advantages that the porous carbon frame is fed into the reactor through the carbon frame feeding device, a high-temperature environment is formed in the fluidization chamber by utilizing the heater, monosilane and nitrogen are introduced from the upper air inlet hole, and the monosilane is heated and cracked into silicon simple substance and hydrogen. The exhaust fan provides power to enable gas and silicon simple substance at the upper part of the fluidization chamber to enter the reactor through the fluidization hole, and then return to the fluidization chamber through the exhaust hole. The silicon simple substance and the carbon frame are in countercurrent contact in the reactor, the contact is sufficient, and the silicon simple substance is deposited in the pores of the carbon frame to obtain a deposited product, thereby realizing chemical vapor deposition. Subsequently, as the reactor rotates, the deposited product is fluidized from fluidization Kong Paosa to the upper portion of the fluidization chamber, and is fully fluidized. At this time, since the concentration of the silicon simple substance in the upper part of the fluidization chamber is higher than that in one end of the reactor, if a part of the carbon frame does not finish depositing with the silicon simple substance, the silicon simple substance can be fully contacted and deposited in the upper part of the fluidization chamber. The deposited product directly enters the lower part of the fluidization chamber under the action of gravity, acetylene and nitrogen are introduced from a lower air inlet hole, the acetylene is heated and cracked into carbon simple substance and hydrogen, the carbon simple substance is coated on the outer side of the deposited product, a carbon coating process is realized, a silicon negative electrode product is obtained, and the silicon negative electrode product is discharged from a discharge hole.
The reactor and the fluidization chamber are in a high-temperature low-oxygen environment, the two devices complement each other, no external air or only a small amount of air is introduced in the production process, and the oxygen content in the reactor and the fluidization chamber can be controlled below 5 ppm. By feeding the carbon skeleton feeding device, no oxygen or only a small amount of oxygen can be ensured to enter the carbon skeleton feeding device. Therefore, the silicon anode product can be continuously produced in the reactor and the fluidization chamber without stopping, the yield of the silicon anode is improved, the production cost is reduced, and the silicon anode can be produced and used in a large scale.
On the basis of the technical scheme, the invention can be improved as follows.
Further, the silicon anode CVD and carbon cladding apparatus further comprises a terminal feeding barrel, one end of the terminal feeding barrel is fixedly arranged outside the fluidization chamber and is provided with a terminal feeding port, and the other end of the reactor is rotatably connected with the other end of the terminal feeding barrel.
The beneficial effect of adopting the further scheme is that monosilane and nitrogen can be introduced from the other end of the reactor through the terminal feeding cylinder, so that the introduction efficiency of monosilane is increased, and the yield is improved.
Further, the silicon anode CVD and carbon cladding apparatus further comprises a filter, and the suction hole, the filter, the suction fan and the upper portion of the fluidization chamber are sequentially communicated through a pipeline.
The further scheme has the beneficial effects that the filter is arranged at the inlet of the exhaust fan, so that carbon frames or deposited products are prevented from entering the exhaust fan, and the carbon frames or deposited products can only be discharged from the fluidization holes.
Further, the silicon cathode CVD and carbon cladding equipment further comprises an upper circulation assembly and a lower circulation assembly, wherein the upper circulation assembly comprises a first heat exchanger, a first dehydrogenator and a first induced draft fan which are sequentially communicated, and an inlet of the first heat exchanger and an outlet of the first induced draft fan are communicated with the upper part of the fluidization chamber;
the lower circulation assembly comprises a second heat exchanger, a second dehydrogenation device and a second induced draft fan which are sequentially communicated, and an inlet of the second heat exchanger and an outlet of the second induced draft fan are communicated with the lower portion of the fluidization chamber.
The beneficial effect of adopting the further proposal is that the upper part and the lower part of the fluidization chamber are respectively provided with an upper circulation component and a lower circulation component, the upper part and the lower part of the fluidization chamber are respectively pumped out, and the hydrogen in the gas is removed and then sent to the reflow chamber for recycling.
Further, the silicon negative electrode CVD and carbon cladding equipment further comprises a high-temperature fan, an air distribution plate and a discharge pipe, wherein the air distribution chamber is arranged at the bottom of the fluidization chamber, an air inlet of the high-temperature fan is communicated with the lower part of the fluidization chamber, an air outlet of the high-temperature fan is communicated with the air distribution chamber, the air distribution plate is fixed at the top of the air distribution chamber, the discharge pipe is vertically arranged and penetrates through the air distribution plate and is fixedly connected with the air distribution plate, and the discharge pipe is provided with a discharge hole.
The technical proposal has the advantages that the high temperature fan blows air into the fluidization chamber from bottom to top through the air distribution plate, and agitates the air at the lower part of the fluidization chamber to make the carbon coating reaction uniform. The silicon negative electrode product is discharged from the discharge pipe.
Further, the silicon cathode CVD and carbon coating equipment further comprises a discharge auger, and the discharge auger is communicated with the discharge hole.
The silicon anode product is discharged by the discharging auger, and the auger is used for feeding, so that the silicon anode product and auger blades can be used for preventing external air from entering the fluidization chamber, isolating oxygen and guaranteeing the safety of the production process.
Further, the heater is provided with two groups, wherein one group of the heater is arranged in the middle of the fluidization chamber, the fluidization chamber is divided into an upper fluidization chamber positioned at the upper part of the fluidization chamber and a lower fluidization chamber positioned at the lower part of the fluidization chamber, and the other group of the heater is arranged at the bottom of the fluidization chamber.
The fluidization chamber is naturally divided into the upper chamber and the lower chamber which are mutually communicated by the heater, so that the fluidization chamber can be fully heated, the structure of the fluidization chamber is simplified, and structures such as a baffle plate and the like do not need to be additionally processed in the fluidization chamber.
Further, the heater is an electric heater, the heater is annular, and the heater is provided with an inverted conical guide hole.
The guide hole is funnel-shaped and is used for converging materials and gradually flowing into the lower fluidization chamber, so that the materials can stay in the upper fluidization chamber for a sufficient time and can slow down the speed of falling into the lower fluidization chamber, and the materials have sufficient reaction time in both the upper fluidization chamber and the lower fluidization chamber. The heater is an electric heater, adopts resistance wire heating, can insulate oxygen heating, avoids oxygen introduced by combustion heating or explosion risk introduced, and is beneficial to controlling the oxygen content in the fluidization chamber below 5 ppm.
Further, carbon skeleton feed arrangement includes front end feed cylinder, pushes away feed hydraulic cylinder and air outlet cylinder, front end feed cylinder is fixed to be set up, push away the feed hydraulic cylinder be fixed in the one end of front end feed cylinder, the middle part of front end feed cylinder has the front end feed inlet, the air outlet cylinder is fixed to be set up and overlap to be established the front end feed cylinder outside, the one end of reactor with the air outlet cylinder rotates to be connected, and with the other end of front end feed cylinder and the air outlet cylinder intercommunication, the air outlet cylinder is located the one end outside the reactor has the gas sucking hole.
The technical scheme has the advantages that the carbon frame is conveyed into the front-end feeding cylinder from the front-end feeding port, the pushing hydraulic cylinder conveys the carbon frame in the front-end feeding cylinder into the reactor, and the front-end feeding cylinder can be sealed by the carbon frame during feeding, so that air introduced during feeding is less. The gas in the reactor is led out through the gas outlet cylinder and returns to the fluidization chamber under the power action of the exhaust fan.
The invention also provides a continuous mass production method for the CVD and the carbon coating of the silicon cathode, which is realized by adopting the equipment for the CVD and the carbon coating of the silicon cathode, and comprises the following steps:
Feeding a porous carbon skeleton into the reactor through a carbon skeleton feeding device;
Meanwhile, the heater heats the fluidization chamber to 800-900 ℃, monosilane and nitrogen are introduced from an upper air inlet, monosilane is heated and cracked into silicon simple substance and hydrogen, and under the power action of an exhaust fan, the silicon simple substance enters the reactor from the fluidization hole and contacts with the carbon frame in a countercurrent way so as to be deposited in the porous structure of the carbon frame, thus obtaining a deposited product;
along with the rotation of the reactor, the deposition product flows into the fluidization chamber through the fluidization Kong Sa, and the deposition product is fully fluidized and falls into the lower part of the fluidization chamber under the action of self gravity; simultaneously, under the power action of an exhaust fan, the elemental silicon, nitrogen and hydrogen in the reactor return to a fluidization chamber, acetylene and nitrogen are introduced from a lower air inlet, the acetylene is heated and cracked into elemental carbon and hydrogen, and the elemental carbon is coated on the outer side of a deposition product to obtain a silicon anode product;
The silicon negative electrode product is discharged from the discharge hole.
The method has the advantages that the two processes of CVD and carbon coating of the silicon negative electrode are realized by utilizing the matched reactor and the fluidization chamber, the silicon negative electrode product can be produced continuously, the yield of the silicon negative electrode is improved, the production cost is reduced, and the silicon negative electrode can be produced and used on a large scale.
The continuous mass production method for the CVD and carbon coating of the silicon cathode further comprises the step that a high-temperature fan enables gas at the lower part of the fluidization chamber to flow from bottom to top through an air distribution plate, so that carbon simple substances are fully contacted with deposition products.
The technical proposal has the advantages that the high temperature fan blows air into the fluidization chamber from bottom to top through the air distribution plate, and agitates the air at the lower part of the fluidization chamber to make the carbon coating reaction uniform. The silicon negative electrode product is discharged from the discharge pipe.
Drawings
FIG. 1 is a schematic diagram of a silicon anode CVD and carbon cladding apparatus according to the present invention;
Fig. 2 is a schematic view of the material flow direction of the silicon anode CVD and carbon coating apparatus of the invention.
In the drawings, the list of components represented by the various numbers is as follows:
1. the device comprises a carbon frame feeding device, a 101, a feeding hopper, a 102, a pushing hydraulic cylinder, a 103 and an air outlet cylinder;
2. reactor, 201, fluidization hole, 202, extension cylinder, 203, end feeding cylinder;
3. a fluidization chamber; 301, upper inlet holes, 302, lower inlet holes, 303, upper fluidization chamber, 304, lower fluidization chamber;
4. the device comprises a heater, a high-temperature fan, a 6 air distribution plate, a 7 discharge auger, a 8 filter, a 9 exhaust fan;
10. The upper circulation assembly, 1001, a first heat exchanger, 1002, a first dehydrogenator, 1003, a first induced draft fan;
11. The lower circulation assembly, 1101, second heat exchanger, 1102, second dehydrogenator, 1103, second induced draft fan.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1-2, this embodiment provides a silicon negative electrode CVD and carbon coating apparatus, which comprises a carbon frame feeding device 1, a reactor 2, a fluidization chamber 3, a heater 4 and an exhaust fan 9, wherein one end of the reactor 2 is rotatably connected and communicated with the carbon frame feeding device 1, the other end of the reactor extends into the fluidization chamber 3 and is rotatably connected with the upper portion of the fluidization chamber 3, a plurality of fluidization holes 201 are formed in the side wall of the other end of the reactor 2, one end of the reactor 2 is further provided with an air suction hole, the air suction hole is communicated with the upper portion of the fluidization chamber 3 through the exhaust fan 9, an upper air inlet 301 is formed in the upper portion of the fluidization chamber 3, the upper air inlet 301 is used for introducing monosilane and nitrogen, a lower air inlet 302 is formed in the lower portion of the fluidization chamber 3, acetylene and nitrogen are introduced into the lower air inlet 302, a discharge hole is formed in the bottom of the fluidization chamber 3, and the heater 4 is fixedly connected with the inner wall of the fluidization chamber 3.
In this example, a porous carbon skeleton was fed into a reactor 2 through a carbon skeleton feeding device 1, and monosilane (SiH 4) and nitrogen gas (N 2) were introduced into a fluidization chamber 3 through an upper inlet hole 301 by a heater 4 to form a high-temperature environment, and the monosilane was thermally decomposed into elemental silicon (Si) and hydrogen gas (H 2). The suction fan 9 provides power to enable gas and silicon simple substance at the upper part of the fluidization chamber 3 to enter the reactor 2 through the fluidization holes 201, and then return to the fluidization chamber 3 through the suction holes. The silicon simple substance and the carbon frame are in countercurrent contact in the reactor 2, the contact is sufficient, the silicon simple substance is deposited in the pores of the carbon frame to obtain a deposition product, thereby realizing chemical vapor deposition, and the silicon simple substance, nitrogen and hydrogen in the reactor 2 return to the fluidization chamber 3 under the power action of the exhaust fan 9, so that the silicon simple substance is recycled, and the utilization rate of monosilane is improved. Subsequently, as the reactor 2 rotates, the deposition product is thrown from the fluidization holes 201 to the upper portion of the fluidization chamber 3, and is sufficiently fluidized. At this time, since the concentration of the silicon simple substance in the upper portion of the fluidization chamber 3 is higher than that in one end of the reactor 2, if there is a part of the carbon skeleton that does not finish depositing with the silicon simple substance, it is also possible to sufficiently contact and deposit with the silicon simple substance in the upper portion of the fluidization chamber 3. The deposited product directly enters the lower part of the fluidization chamber 3 under the action of gravity, acetylene (C 2H2) and nitrogen (N 2) are introduced from the lower air inlet hole 302, the acetylene is heated and cracked into carbon simple substance (C) and hydrogen (H 2), the carbon simple substance is coated on the outer side of the deposited product, a carbon coating process is realized, a silicon negative electrode product is obtained, and the silicon negative electrode product is discharged from the discharge hole.
The reactor 2 and the fluidization chamber 3 are in a high-temperature low-oxygen environment, the two devices complement each other, no external air or only a small amount of air is introduced in the production process, and the oxygen content in the reactor can be controlled below 5 ppm. By feeding the carbon skeleton feeding device 1, no oxygen or only a small amount of oxygen can be ensured to enter the carbon skeleton feeding device 1. Therefore, the silicon anode product can be continuously produced in the reactor 2 and the fluidization chamber 3 without stopping, the yield of the silicon anode is improved, the production cost is reduced, and the silicon anode can be produced and used in a large scale.
Specifically, the side wall of the reactor 2 outside the fluidization chamber 3 is wrapped with a heat-insulating layer, so that heat loss is reduced. The inner wall of the reactor 2 is fixed with a spiral material guiding plate, or a plurality of material guiding plates are arranged at intervals along the spiral direction, and along with the rotation of the reactor 2, the material guiding plates can push the carbon frame to the direction of the fluidization holes 201.
Specifically, in monosilane and nitrogen gas introduced into the upper gas inlet 301, the volume ratio of monosilane to all the gases introduced into the upper gas inlet 301 is less than or equal to 1%.
Alternatively, the reactor 2 may be cylindrical, or the reactor 2 may be tapered with one end having a larger diameter than the other end, i.e., the end near the carbon skeleton feeding device 1 may have a larger diameter.
Specifically, the outer wall of the reactor 2 is sleeved with an outer gear which is coaxially arranged, a motor is fixed on the frame, an output shaft of the motor is fixed with a driving gear, and the driving gear is meshed with the outer gear, so that the reactor 2 is driven to rotate around the axis of the reactor. And carrier rollers are arranged on two sides below the reactor 2, the axes of the carrier rollers are parallel to the axis of the reactor 2, the carrier rollers are rotatably arranged on the frame, and the carrier rollers are in butt joint with the outer wall of the reactor 2 to support the reactor 2. The carrier rollers are provided with a plurality of groups at intervals along the axial direction of the reactor 2.
On the basis of the technical scheme, the silicon anode CVD and carbon coating equipment further comprises a tail end feeding cylinder 203, one end of the tail end feeding cylinder 203 is fixedly arranged outside the fluidization chamber 3 and is provided with a tail end feeding port, and the other end of the reactor 2 is rotatably connected with the other end of the tail end feeding cylinder 203.
Monosilane and nitrogen gas can be introduced from the other end of the reactor 2 through the end feed cylinder 203, so that the introduction efficiency of monosilane is increased and the yield is improved.
Specifically, the terminal feed port is used for introducing monosilane and nitrogen. Preferably, the terminal feed port and the upper inlet port 301 are both in communication with a first gas supply conduit for delivering monosilane and nitrogen.
Further, the other end of the reactor 2 is also fixed with and communicated with an extension tube 202, the diameter of the extension tube 202 is smaller than that of the other end of the reactor 2, the extension tube 202 extends out of the fluidization chamber 3 and is rotationally connected with the other end of the terminal feeding tube 203, and the diameter of the terminal feeding tube 203 is smaller than that of the extension tube 202. This gradually decreasing diameter configuration reduces heat loss to some extent. Preferably, a pair of carrier rollers is provided below the portion of the extension tube 202 outside the fluidization chamber 3, supporting the extension tube 202.
On the basis of the technical scheme, the silicon anode CVD and carbon cladding equipment further comprises a filter 8, and the air suction holes, the filter 8, the exhaust fan 9 and the upper part of the fluidization chamber 3 are sequentially communicated through pipelines.
A filter 8 is provided at the inlet of the suction fan 9 to prevent carbon skeleton or sediment products from entering the suction fan 9 so that they can only be discharged from the fluidization holes 201.
Specifically, the mesh diameter of the filter 8 is smaller than the diameter of the carbon skeleton and larger than the particle diameter of the elemental silicon generated in the fluidization chamber 3.
On the basis of the technical scheme, the silicon anode CVD and carbon coating equipment further comprises an upper circulation assembly 10 and a lower circulation assembly 11, wherein the upper circulation assembly 10 comprises a first heat exchanger 1001, a first dehydrogenator 1002 and a first induced draft fan 1003 which are sequentially communicated, and an inlet of the first heat exchanger 1001 and an outlet of the first induced draft fan 1003 are both communicated with the upper part of the fluidization chamber 3;
The lower circulation assembly 11 comprises a second heat exchanger 1101, a second dehydrogenator 1102 and a second induced draft fan 1103 which are sequentially communicated, and an inlet of the second heat exchanger 1101 and an outlet of the second induced draft fan 1103 are both communicated with the lower part of the fluidization chamber 3.
An upper circulation assembly 10 and a lower circulation assembly 11 are respectively arranged at the upper part and the lower part of the fluidization chamber 3, the upper gas and the lower gas of the fluidization chamber 3 are respectively pumped out, and the hydrogen in the gas is removed and then returned to the fluidization chamber 3 for recycling.
Specifically, silane and acetylene can be cracked as long as they enter the fluidization chamber 3, H 2 remains after the reaction in the upper and lower parts of the fluidization chamber 3, the gas flow in the upper part of the fluidization chamber 3 (upper fluidization chamber 303) includes elemental silicon (solids that can flow with gas), hydrogen and nitrogen, and the gas flow in the lower part of the fluidization chamber 3 (lower fluidization chamber 304) includes elemental carbon, hydrogen and nitrogen, so that the gas flows in the upper and lower fluidization chambers 303 and 304 can be reused after the hydrogen is removed.
The first heat exchanger 1001 of the upper circulation assembly 10 is used for cooling the air flow pumped by the upper fluidization chamber 303, and the second dehydrogenator 1102 removes the hydrogen in the air flow of the upper fluidization chamber 303 and returns the hydrogen to the upper fluidization chamber 303 by the first induced draft fan 1003.
The second heat exchanger 1101 of the lower circulation assembly 11 is configured to cool the air flow extracted from the lower fluidization chamber 304, and the second dehydrogenation unit 1102 removes the hydrogen in the air flow of the lower fluidization chamber 304 and sends the hydrogen back to the lower fluidization chamber 304 by the second induced draft fan 1103.
Wherein the first dehydrogenator 1002 and the second dehydrogenator 1102 may employ a low-temperature catalytic oxidation reactor, the inside of which is filled with a catalyst (e.g., pd/Al 2O3) by which hydrogen is oxidized into water.
On the basis of the technical scheme, the silicon negative electrode CVD and carbon coating equipment further comprises a high-temperature fan 5, an air distribution plate 6 and a discharge pipe, wherein the air distribution chamber is arranged at the bottom of the fluidization chamber 3, an air inlet of the high-temperature fan 5 is communicated with the lower part of the fluidization chamber 3, an air outlet of the high-temperature fan 5 is communicated with the air distribution chamber, the air distribution plate 6 is fixed at the top of the air distribution chamber, the discharge pipe is vertically arranged and penetrates through the air distribution plate 6 and is fixedly connected with the air distribution plate 6, and the discharge pipe is provided with a discharge hole.
The high-temperature fan 5 blows air into the fluidization chamber 3 from bottom to top through the air distribution plate 6, and agitates the air at the lower part of the fluidization chamber 3, so that the carbon coating reaction is uniform. The silicon negative electrode product is discharged from the discharge pipe.
Alternatively, the discharge tube may be provided with one or more.
Specifically, the air distribution plate 6 is an air distribution plate with a hood, the air distribution plate 6 is plate-shaped and is provided with a plurality of through holes, each through hole is provided with a hood, the hood is provided with a plurality of air holes with different angles, and if a silicon negative electrode product falls on the air distribution plate 6, the silicon negative electrode product can be blown up again for fluidization until the silicon negative electrode product falls into a discharge pipe and can not be discharged.
On the basis of the technical scheme, the silicon cathode CVD and carbon coating equipment further comprises a discharging auger 7, and the discharging auger 7 is communicated with the discharging hole.
The discharging auger 7 discharges the silicon negative electrode product, and the auger feeding is adopted, so that the silicon negative electrode product and auger blades can be utilized to prevent external air from entering the fluidization chamber 3, thereby isolating oxygen and guaranteeing the safety of the production process.
Specifically, the lower end of the discharge pipe penetrates out of the air distribution chamber and is communicated with a feed inlet of the discharge auger 7.
On the basis of the above technical solution, the heaters 4 are provided with two groups, wherein one group of the heaters 4 is arranged in the middle of the fluidization chamber 3, and divides the fluidization chamber 3 into an upper fluidization chamber 303 positioned at the upper part thereof and a lower fluidization chamber 304 positioned at the lower part thereof, and the other group of the heaters 4 is arranged at the bottom of the fluidization chamber 3.
The fluidization chamber 3 is naturally divided into an upper chamber and a lower chamber which are communicated with each other by the heater 4, so that the fluidization chamber 3 can be fully heated, the structure of the fluidization chamber 3 is simplified, and structures such as a partition plate and the like do not need to be additionally processed in the fluidization chamber 3.
Specifically, the other end of the reactor 2, the upper inlet orifice 301 and the upper circulation assembly 10 are all located in an upper fluidization chamber 303, and the lower inlet orifice 302 is located in a lower fluidization chamber 304.
On the basis of the technical scheme, the heater 4 is an electric heater, the heater 4 is annular, and the heater 4 is provided with an inverted conical guide hole.
The pilot holes are funnel-shaped and are used for converging and gradually flowing into the lower fluidization chamber 304, so that the materials can fully stay in the upper fluidization chamber 303 and can slow down the speed of falling into the lower fluidization chamber 304, and the materials can fully react in the upper fluidization chamber 303 and the lower fluidization chamber 304. The heater 4 is an electric heater, adopts resistance wire heating, can insulate oxygen heating, avoids oxygen introduced by combustion heating or explosion risk introduced, and is beneficial to controlling the oxygen content in the fluidization chamber 3 below 5 ppm.
In one specific example, as shown in fig. 1, the heater 4 has a ring shape whose longitudinal section is a right triangle. Alternatively, in another example, the heater 4 is ring-shaped with a right trapezoid in longitudinal section.
Preferably, the outer surface of the heater 4 is covered with an insulating layer to avoid explosion risk caused by static electricity or electric spark.
On the basis of the technical scheme, the carbon skeleton feeding device 1 comprises a front-end feeding cylinder, a pushing hydraulic cylinder 102 and an air outlet cylinder 103, wherein the front-end feeding cylinder is fixedly arranged, the pushing hydraulic cylinder 102 is fixed in one end of the front-end feeding cylinder, a front-end feeding port is formed in the middle of the front-end feeding cylinder, the air outlet cylinder 103 is fixedly arranged and sleeved outside the front-end feeding cylinder, one end of the reactor 2 is rotationally connected with the air outlet cylinder 103, the air outlet cylinder 103 is communicated with the other end of the front-end feeding cylinder, and one end of the air outlet cylinder 103, which is positioned outside the reactor 2, is provided with the air pumping hole.
The carbon skeleton is sent into the front-end feeding cylinder from the front-end feeding port, the pushing hydraulic cylinder 102 sends the carbon skeleton in the front-end feeding cylinder into the reactor 2, and the front-end feeding cylinder can be sealed by the carbon skeleton while feeding, so that the air introduced during feeding is less. The gas in the reactor 2 is led out through the gas outlet cylinder 103 and returns to the fluidization chamber 3 under the power of the exhaust fan 9.
Specifically, a feed hopper 101 is fixed on the front-end feed inlet, and materials are fed into the front-end feed cylinder through the feed hopper 101.
Alternatively, the carbon skeleton feeding device 1 is a feeding auger, and external air can be prevented from entering the reactor 2 by using the auger feeding.
On the basis of the above technical scheme, the side wall of the lower part (lower fluidization chamber 304) of the fluidization chamber 3 is also provided with an exhaust gas discharge hole, the silicon anode CVD and the carbon cladding equipment are cleaned by nitrogen before being used, after cleaning, redundant nitrogen in the fluidization chamber 3 can be discharged outside through the exhaust gas discharge hole, and a proper gas purifying device can be arranged outside the exhaust gas discharge hole according to requirements. The exhaust gas exhaust hole is provided with an exhaust valve for opening and closing.
Example two
The embodiment also provides a continuous mass production method for silicon anode CVD and carbon coating, which is realized by adopting the silicon anode CVD and carbon coating equipment and comprises the following steps:
feeding porous carbon frames into the reactor 2 through a carbon frame feeding device 1;
Meanwhile, the heater 4 heats the inside of the fluidization chamber 3 to 800-900 ℃, monosilane and nitrogen are introduced from the upper air inlet 301, monosilane is heated and cracked into silicon simple substance and hydrogen, and under the power action of the exhaust fan 9, the silicon simple substance enters the reactor 2 from the fluidization hole 201 and contacts with the carbon frame in a countercurrent way so as to be deposited in the porous structure of the carbon frame, thus obtaining a deposition product;
Along with the rotation of the reactor 2, the deposition product is scattered into the fluidization chamber 3 through the fluidization holes 201, the deposition product is fully fluidized and falls into the lower part of the fluidization chamber 3 under the action of self gravity, and simultaneously, the silicon simple substance, nitrogen and hydrogen in the reactor 2 return into the fluidization chamber 3 under the action of the power of the exhaust fan 9;
The silicon negative electrode product is discharged from the discharge hole.
The method has the advantages that the two processes of CVD and carbon coating of the silicon negative electrode are realized by utilizing the reactor 2 and the fluidization chamber 3 which are matched with each other, the silicon negative electrode product can be produced continuously and continuously, the yield of the silicon negative electrode is improved, the production cost is reduced, and the silicon negative electrode can be produced and used in a large scale.
Specifically, before the silicon anode CVD and carbon coating equipment is used, nitrogen is introduced through the upper air inlet hole 301 and/or the lower air inlet hole 302, the high-temperature fan 5, the exhaust fan 9, the first induced fan 1003 and the second induced fan 1103 are started, and the interior of the silicon anode CVD and carbon coating equipment is cleaned by utilizing the nitrogen, so that the nitrogen fills the reactor 2, the fluidization chamber 3 and all pipelines, and the oxygen content is ensured to be lower than 5ppm. The remaining gas in the fluidized chamber 3 is removed, and the excessive gas can be discharged from the exhaust gas outlet hole at the bottom of the fluidized chamber.
On the basis of the technical scheme, the continuous mass production method for the silicon cathode CVD and the carbon cladding further comprises the step that the high-temperature fan 5 enables gas at the lower part of the fluidization chamber 3 to flow from bottom to top through the air distribution plate 6, so that carbon simple substances are fully contacted with deposition products.
The high-temperature fan 5 blows air into the fluidization chamber 3 from bottom to top through the air distribution plate 6, and agitates the air at the lower part of the fluidization chamber 3, so that the carbon coating reaction is uniform. The silicon negative electrode product is discharged from the discharge pipe.
In the description of the present invention, it should be noted that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
In the description of the present invention, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected, directly connected, or indirectly connected through an intermediary, or may be in communication with the interior of two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (10)

1.硅负极CVD和碳包覆设备,其特征在于,包括碳架进料装置(1)、反应器(2)、流化室(3)、加热器(4)和抽风机(9),所述反应器(2)的一端与所述碳架进料装置(1)转动连接并连通,其另一端伸入所述流化室(3)内,并与所述流化室(3)的上部转动连接,所述反应器(2)另一端侧壁具有多个流化孔(201),所述反应器(2)的一端还设有抽气孔,所述抽气孔通过所述抽风机(9)与所述流化室(3)的上部连通,所述流化室(3)的上部具有上进气孔(301),所述上进气孔(301)用于通入甲硅烷和氮气,所述流化室(3)的下部具有下进气孔(302),所述下进气孔(302)用于通入乙炔和氮气,所述流化室(3)的底部具有排料孔,所述加热器(4)与所述流化室(3)内壁固定连接。1. A silicon negative electrode CVD and carbon coating device, characterized in that it comprises a carbon rack feeding device (1), a reactor (2), a fluidizing chamber (3), a heater (4) and an exhaust fan (9), wherein one end of the reactor (2) is rotatably connected to and communicates with the carbon rack feeding device (1), and the other end thereof extends into the fluidizing chamber (3) and is rotatably connected to the upper part of the fluidizing chamber (3), the side wall of the other end of the reactor (2) has a plurality of fluidizing holes (201), and one end of the reactor (2) is also provided with There is an air extraction hole, which is connected to the upper part of the fluidizing chamber (3) through the exhaust fan (9), the upper part of the fluidizing chamber (3) has an upper air inlet (301), and the upper air inlet (301) is used to introduce monosilane and nitrogen. The lower part of the fluidizing chamber (3) has a lower air inlet (302), and the lower air inlet (302) is used to introduce acetylene and nitrogen. The bottom of the fluidizing chamber (3) has a discharge hole, and the heater (4) is fixedly connected to the inner wall of the fluidizing chamber (3). 2.根据权利要求1所述的硅负极CVD和碳包覆设备,其特征在于,还包括末端进料筒(203),所述末端进料筒(203)一端固定设置于所述流化室(3)外部,并具有末端进料口,所述反应器(2)另一端端部与所述末端进料筒(203)另一端转动连接。2. The silicon negative electrode CVD and carbon coating equipment according to claim 1 is characterized in that it also includes an end feed cylinder (203), one end of which is fixedly arranged outside the fluidizing chamber (3) and has an end feed port, and the other end of the reactor (2) is rotatably connected to the other end of the end feed cylinder (203). 3.根据权利要求1所述的硅负极CVD和碳包覆设备,其特征在于,还包括过滤器(8),所述抽气孔、所述过滤器(8)、所述抽风机(9)以及所述流化室(3)的上部依次通过管道连通。3. The silicon negative electrode CVD and carbon coating equipment according to claim 1, characterized in that it also includes a filter (8), and the exhaust hole, the filter (8), the exhaust fan (9) and the upper part of the fluidizing chamber (3) are connected in sequence through a pipeline. 4.根据权利要求1所述的硅负极CVD和碳包覆设备,其特征在于,还包括上循环组件(10)和下循环组件(11),所述上循环组件(10)包括依次连通的第一热交换器(1001)、第一脱氢器(1002)和第一引风机(1003),所述第一热交换器(1001)的进口和所述第一引风机(1003)的出口均与所述流化室(3)的上部连通;4. The silicon negative electrode CVD and carbon coating equipment according to claim 1, characterized in that it further comprises an upper circulation component (10) and a lower circulation component (11), wherein the upper circulation component (10) comprises a first heat exchanger (1001), a first dehydrogenator (1002) and a first induced draft fan (1003) which are connected in sequence, and an inlet of the first heat exchanger (1001) and an outlet of the first induced draft fan (1003) are both connected to the upper part of the fluidizing chamber (3); 所述下循环组件(11)包括依次连通的第二热交换器(1101)、第二脱氢器(1102)和第二引风机(1103),所述第二热交换器(1101)的进口和所述第二引风机(1103)的出口均与所述流化室(3)的下部连通。The lower circulation component (11) comprises a second heat exchanger (1101), a second dehydrogenator (1102) and a second induced draft fan (1103) which are connected in sequence, and an inlet of the second heat exchanger (1101) and an outlet of the second induced draft fan (1103) are both connected to the lower part of the fluidizing chamber (3). 5.根据权利要求1所述的硅负极CVD和碳包覆设备,其特征在于,还包括高温风机(5)、布风板(6)和排料管,所述流化室(3)的底部具有布风室,所述高温风机(5)的进气口与所述流化室(3)下部连通,所述高温风机(5)的出气口与所述布风室连通,所述布风室的顶部固定有所述布风板(6),所述排料管竖直设置,其穿过所述布风板(6)并与所述布风板(6)固定连接,所述排料管具有所述排料孔。5. The silicon negative electrode CVD and carbon coating equipment according to claim 1 is characterized in that it also includes a high-temperature fan (5), an air distribution plate (6) and a discharge pipe, the bottom of the fluidizing chamber (3) has an air distribution chamber, the air inlet of the high-temperature fan (5) is connected to the lower part of the fluidizing chamber (3), the air outlet of the high-temperature fan (5) is connected to the air distribution chamber, the top of the air distribution chamber is fixed with the air distribution plate (6), the discharge pipe is vertically arranged, passes through the air distribution plate (6) and is fixedly connected to the air distribution plate (6), and the discharge pipe has the discharge hole. 6.根据权利要求1所述的硅负极CVD和碳包覆设备,其特征在于,还包括出料搅龙(7),所述出料搅龙(7)与所述排料孔连通。6. The silicon negative electrode CVD and carbon coating equipment according to claim 1, characterized in that it also includes a discharge agitator (7), and the discharge agitator (7) is connected to the discharge hole. 7.根据权利要求1-6任一项所述的硅负极CVD和碳包覆设备,其特征在于,所述加热器(4)设有两组,其中一组所述加热器(4)设置于所述流化室(3)中部,并将所述流化室(3)分为位于其上部的上流化室(303)和位于其下部的下流化室(304),另一组所述加热器(4)设置于所述流化室(3)的底部;所述加热器(4)为电加热器,所述加热器(4)为环形,所述加热器(4)具有倒锥形的导向孔。7. The silicon negative electrode CVD and carbon coating equipment according to any one of claims 1 to 6, characterized in that the heater (4) is provided with two groups, wherein one group of the heaters (4) is arranged in the middle of the fluidizing chamber (3) and divides the fluidizing chamber (3) into an upper fluidizing chamber (303) located at the upper part thereof and a lower fluidizing chamber (304) located at the lower part thereof, and the other group of the heaters (4) is arranged at the bottom of the fluidizing chamber (3); the heater (4) is an electric heater, the heater (4) is annular, and the heater (4) has an inverted conical guide hole. 8.根据权利要求1-6任一项所述的硅负极CVD和碳包覆设备,其特征在于,所述碳架进料装置(1)包括前端进料筒、推料液压缸(102)和出气筒(103),所述前端进料筒固定设置,所述推料液压缸(102)固定于所述前端进料筒的一端内,所述前端进料筒的中部具有前端进料口,所述出气筒(103)固定设置并套设在所述前端进料筒外侧,所述反应器(2)的一端与所述出气筒(103)转动连接,并与所述前端进料筒的另一端以及所述出气筒(103)连通,所述出气筒(103)位于所述反应器(2)外的一端具有所述抽气孔。8. The silicon negative electrode CVD and carbon coating equipment according to any one of claims 1 to 6 is characterized in that the carbon frame feeding device (1) includes a front feed barrel, a pushing hydraulic cylinder (102) and an air outlet barrel (103), the front feed barrel is fixedly arranged, the pushing hydraulic cylinder (102) is fixed in one end of the front feed barrel, the middle part of the front feed barrel has a front feed port, the air outlet barrel (103) is fixedly arranged and sleeved on the outside of the front feed barrel, one end of the reactor (2) is rotatably connected to the air outlet barrel (103), and is communicated with the other end of the front feed barrel and the air outlet barrel (103), and the end of the air outlet barrel (103) located outside the reactor (2) has the exhaust hole. 9.硅负极CVD和碳包覆连续量产方法,其特征在于,采用如权利要求1-8任一项所述的硅负极CVD和碳包覆设备实现,包括以下步骤:9. A method for continuous mass production of silicon anode CVD and carbon coating, characterized by being implemented using the silicon anode CVD and carbon coating equipment according to any one of claims 1 to 8, comprising the following steps: 通过碳架进料装置(1)向反应器(2)内送入多孔的碳架;A porous carbon frame is fed into the reactor (2) through a carbon frame feeding device (1); 同时加热器(4)将流化室(3)内加热至800-900摄氏度,从上进气孔(301)通入甲硅烷和氮气,甲硅烷受热裂解为硅单质和氢气,在抽风机(9)的动力作用下,硅单质从流化孔(201)进入反应器(2)内,并与碳架逆流接触从而沉积在碳架的多孔结构内,得到沉积产品;At the same time, the heater (4) heats the fluidization chamber (3) to 800-900 degrees Celsius, and monosilane and nitrogen are introduced from the upper air inlet (301). The monosilane is thermally cracked into silicon and hydrogen. Under the power of the exhaust fan (9), the silicon enters the reactor (2) from the fluidization hole (201) and contacts the carbon frame in countercurrent flow, thereby being deposited in the porous structure of the carbon frame to obtain a deposited product. 随着反应器(2)的转动,所述沉积产品通过所述流化孔(201)撒入流化室(3)内,沉积产品充分流化,并在自身重力作用下落入流化室(3)下部;同时,在抽风机(9)的动力作用下反应器(2)内的硅单质、氮气和氢气回到流化室(3)内;从下进气孔(302)通入乙炔和氮气,乙炔受热裂解为碳单质和氢气,碳单质包覆在沉积产品外侧,得到硅负极产品;As the reactor (2) rotates, the deposited product is scattered into the fluidizing chamber (3) through the fluidizing hole (201), the deposited product is fully fluidized, and falls into the lower part of the fluidizing chamber (3) under the action of its own gravity; at the same time, the silicon element, nitrogen and hydrogen in the reactor (2) return to the fluidizing chamber (3) under the power of the exhaust fan (9); acetylene and nitrogen are introduced from the lower air inlet (302), and the acetylene is thermally cracked into carbon element and hydrogen, and the carbon element is coated on the outside of the deposited product to obtain a silicon negative electrode product; 所述硅负极产品从排料孔排出。The silicon negative electrode product is discharged from the discharge hole. 10.根据权利要求9所述的硅负极CVD和碳包覆连续量产方法,其特征在于,还包括:高温风机(5)通过布风板(6)使流化室(3)下部的气体由下至上流动,使碳单质与沉积产品充分接触。10. The method for continuous mass production of silicon negative electrode CVD and carbon coating according to claim 9 is characterized in that it also includes: a high-temperature fan (5) causes the gas in the lower part of the fluidizing chamber (3) to flow from bottom to top through the air distribution plate (6), so that the carbon element is fully in contact with the deposited product.
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