A vacuum powder ALD apparatus

Abstract

The application is a vacuum powder ALD device, the structure of which is that a turbine air inlet is connected with a feeding pipe, an air outlet is connected with an air inlet pipe, the air inlet pipe is connected with a process pipe and a powder collecting pipe respectively, the air inlet pipe is connected with a vacuum ball valve and connected with a circulating pipe inlet, the feeding pipe is connected with a vacuum ball valve and connected with a circulating pipe outlet, the process pipe and the powder collecting pipe are connected with two-stage cyclone dust collectors after being gathered, a vacuum filter and a vacuum pump are connected with the two-stage cyclone dust collector outlet in sequence, and the two-stage cyclone dust collector is connected with the feeding pipe. The application has the advantages that: the powder is circulated in the pipe at high speed continuously by the turbine air fan to realize the vacuum powder ALD coating. The powder and the process reaction gas are circulated in the pipe continuously to fully coat the powder surface under the high vacuum environment by the turbine air fan. Meanwhile, the powder and the process gas flow at high speed in the pipe. The powder is circulated in the pipe to realize the process under the high vacuum environment.

Description

Technical Field

[0001] This invention relates to a vacuum powder ALD device, belonging to the field of ALD technology. Background Technology

[0002] In the context of vacuum powder coating, atomic layer deposition (ALD) technology is the core equipment for achieving high-end surface modification of powder materials, aiming to achieve atomic-level uniform ultrathin coating on the surface of each particle, with precise and controllable film thickness.

[0003] In existing technologies, the industry mainly uses vertical fluidized beds, horizontal rolling beds (drum type), and planar vibrating beds for powder coating. However, these existing coating methods have shortcomings: for example, horizontal rolling beds rely on the frictional tumbling of powder for coating, and the powder still suffers from local particle overlap and stacking during the tumbling process, making it difficult to achieve coating without dead corners and agglomeration; at the same time, the temperature of the powder and the partial pressure of the precursor are not completely consistent between the deep and shallow layers in existing equipment, resulting in local temperature and gas field deviations; in addition, the film thickness dispersion of drum equipment is high, the thickness fluctuation of a single cycle growth is large, and the atomic-level conformal coating consistency is poor, making it difficult to meet the coating requirements of high-end powder materials. Summary of the Invention

[0004] The present invention proposes a vacuum powder ALD device, which aims to overcome the above-mentioned shortcomings of the existing technology and realize the high-speed continuous coating of powder through a turbine fan in the pipeline.

[0005] The technical solution of this invention: A vacuum powder ALD equipment, the structure of which includes a turbine blower, the inlet of the turbine blower connected to one end of the feed pipe, the outlet of the turbine blower connected to one end of the air inlet pipe, the portion of the air inlet pipe near the turbine blower connected to one end of the process pipeline and one end of the powder collection pipeline respectively, the other end of the air inlet pipe connected in sequence to a transparent PC window and a first KF50 vacuum ball valve and connected to the inlet of the vacuum circulation pipeline, the other end of the feed pipe connected in sequence to another PC window and a second KF50 vacuum ball valve and connected to the outlet of the circulation pipeline, the other ends of the process pipeline and the other end of the powder collection pipeline converge and are connected in sequence to a primary cyclone dust collector and a secondary cyclone dust collector, the outlet of the secondary cyclone dust collector is connected in sequence to a vacuum filter and a vacuum pump, the bottom of the primary cyclone dust collector and the secondary cyclone dust collector are respectively connected to the feed pipe through pipelines, and a vortex flow meter is provided at the PC window of the feed pipe. The turbine fan provides circulating power, the feed pipe is used for material feeding and powder drop during the process, the air inlet pipe is used to introduce process gas to contact the powder for coating process, the PC window is used for powder circulation observation, the circulation pipe is used for powder process circulation, the primary cyclone dust collector and the secondary cyclone dust collector achieve efficient powder separation through bipolar filtration, and the vacuum filter is used to filter vacuum powder to prevent powder from entering the vacuum pump and causing pump contamination.

[0006] Preferably, the process pipeline is equipped with a first ferrule ball valve, the powder collection pipeline is equipped with a second ferrule ball valve, a material box is provided on the pipeline between the bottom of the primary cyclone dust collector and the feed pipe, a third and a fourth ferrule ball valve are provided on the pipeline between the primary cyclone dust collector and the material box, a fifth and a sixth ferrule ball valve are provided on the pipeline between the material box and the feed pipe, and a seventh ferrule ball valve is provided on the pipeline between the bottom of the secondary cyclone dust collector and the feed pipe.

[0007] Preferably, during operation, the first ferrule ball valve, the second ferrule ball valve, the third ferrule ball valve, the fourth ferrule ball valve, the fifth ferrule ball valve, the sixth ferrule ball valve, the first KF50 vacuum ball valve, and the second KF50 vacuum ball valve are closed, while the seventh ferrule ball valve is opened, and material is loaded first; Turn on the chiller for water cooling, and open the first KF50 vacuum ball valve and the second KF50 vacuum ball valve; Then turn on the vacuum pump to evacuate the vacuum until the vacuum level, magnetofluid temperature, and vacuum pipe temperature meet the requirements. Start the turbine fan, open the first ferrule ball valve, the third ferrule ball valve, and the fourth ferrule ball valve, and then open the fifth ferrule ball valve and the sixth ferrule ball valve to proceed with the process; The sixth and seventh ferrule ball valves are used to return powder to the circulating pipeline to continue the process. During the process cycle, the powder flow rate is measured in real time by a vortex flow meter. After the process is completed, first close the third ferrule ball valve, then close the fourth ferrule ball valve; Then close the first ferrule ball valve, open the second ferrule ball valve, close the sixth and fifth ferrule ball valves, and collect dust until the process is complete. After completion, close the second ferrule ball valve, then close the third and fourth ferrule ball valves; Finally, shut down the turbine fan.

[0008] Advantages of this invention: The structure is rationally designed. Throughout the pipeline, powder undergoes high-speed continuous circulation and coating via a vacuum powder ALD turbine fan. The turbine fan enables continuous circulation and reaction of the powder and process reaction gases within the pipeline under high vacuum, fully coating the powder surface. Simultaneously, it allows for high-speed flow of the powder and process gases within the pipeline; the continuous circulation and reaction of the powder within the pipeline enables the process to be carried out under high vacuum. Attached Figure Description

[0009] Figure 1 This is a schematic diagram of the structure of the vacuum powder ALD device of the present invention.

[0010] In the diagram, 1 is the turbine fan, 2 is the air inlet pipe, 3 is the PC window, 41 is the first KF50 vacuum ball valve, 42 is the second KF50 vacuum ball valve, 5 is the circulation pipe, 6 is the feed pipe, 7 is the process pipe, 8 is the powder collection pipe, 9 is the first compression sleeve ball valve, 10 is the second compression sleeve ball valve, 11 is the material box, 12 is the fourth compression sleeve ball valve, 13 is the third compression sleeve ball valve, 141 is the primary cyclone dust collector, 142 is the secondary cyclone dust collector, 15 is the vacuum filter, 16 is the fifth compression sleeve ball valve, 17 is the sixth compression sleeve ball valve, 18 is the seventh compression sleeve ball valve, and 19 is the vortex flow meter. Detailed Implementation

[0011] The present invention will be further described in detail below with reference to embodiments and specific implementation methods.

[0012] like Figure 1 As shown, a vacuum powder ALD (Alternating Current Distribution) device includes a turbine blower 1. The inlet of the turbine blower 1 is connected to one end of a feed pipe 6, and the outlet of the turbine blower 1 is connected to one end of an air inlet pipe 2. The portion of the air inlet pipe 2 near the turbine blower 1 is connected to one end of a process pipe 7 and one end of a powder collection pipe 8. The other end of the air inlet pipe 2 is sequentially connected to a transparent PC window 3 and a first KF50 vacuum ball valve 41, and is connected to the inlet of a vacuum circulation pipe 5. The other end of the feed pipe 6 is sequentially connected to another PC window 3. The second KF50 vacuum ball valve 42 is connected to the outlet of the circulation pipeline 5. The other end of the process pipeline 7 and the other end of the powder collection pipeline 8 are connected to the first-stage cyclone dust collector 141 and the second-stage cyclone dust collector 142 in sequence. The outlet of the second-stage cyclone dust collector 142 is connected to the vacuum filter 15 and the vacuum pump (not shown) in sequence. The bottom of the first-stage cyclone dust collector 141 and the second-stage cyclone dust collector 142 are respectively connected to the feed pipe 6 through pipelines. A vortex flow meter 19 is installed at the PC window 3 of the feed pipe 6.

[0013] A first ferrule ball valve 9 is provided on the process pipeline 7, a second ferrule ball valve 10 is provided on the powder collection pipeline 8, a material box 11 is provided on the pipeline between the bottom of the primary cyclone dust collector 141 and the feed pipe 6, a third ferrule ball valve 13 and a fourth ferrule ball valve 12 are provided on the pipeline between the primary cyclone dust collector 141 and the material box 11, a fifth ferrule ball valve 16 and a sixth ferrule ball valve 17 are provided on the pipeline between the material box 11 and the feed pipe 6, and a seventh ferrule ball valve 18 is provided on the pipeline between the bottom of the secondary cyclone dust collector 142 and the feed pipe 6.

[0014] In the above structure, the turbine fan 1 provides circulating power, the feed pipe 6 is used for feeding and powder dropping during the process, the air inlet pipe 2 is used to introduce process gas to contact the powder for coating process, the PC window 3 is used for powder circulation observation, the circulation pipe 5 is used for powder process circulation, the primary cyclone dust collector 141 and the secondary cyclone dust collector 142 achieve efficient powder separation through bipolar filtration, and the vacuum filter 15 is used to filter vacuum powder to prevent powder from entering the vacuum pump and causing contamination to the pump.

[0015] During the process, the first ferrule ball valve 9, the second ferrule ball valve 10, the third ferrule ball valve 13, the fourth ferrule ball valve 12, the fifth ferrule ball valve 16, the sixth ferrule ball valve 17, the first KF50 vacuum ball valve 41, and the second KF50 vacuum ball valve 42 are closed, and the seventh ferrule ball valve 18 is opened for loading. Turn on the chiller for water cooling and open the first KF50 vacuum ball valve 41 and the second KF50 vacuum ball valve 42; Then turn on the vacuum pump to evacuate the vacuum until the vacuum level, magnetofluid temperature, and vacuum pipe temperature meet the requirements. Start the turbine fan 1, open the first ferrule ball valve 9, the third ferrule ball valve 13, and the fourth ferrule ball valve 12, and then open the fifth ferrule ball valve 16 and the sixth ferrule ball valve 17 to proceed with the process; The sixth ferrule ball valve 17 and the seventh ferrule ball valve 18 are used for powder return, which enters the circulation pipeline 5 to continue the process. During the process circulation, the powder flow rate is measured in real time by the vortex flow meter 19. After the process is completed, first close the third ferrule ball valve 13, and then close the fourth ferrule ball valve 12; Then close the first ferrule ball valve 9, open the second ferrule ball valve 10, and close the sixth ferrule ball valve 17 and the fifth ferrule ball valve 16 to collect dust until it is complete. After completion, close the second ferrule ball valve 10, then close the third ferrule ball valve 13 and the fourth ferrule ball valve 12; Finally, shut down turbine fan 1.

[0016] Experiments showed that, under vacuum conditions, powder is circulated and vulcanized using a turbine fan at a process temperature of 100℃-150℃. By fluidizing the powder with the turbine fan, atomically uniform, ultra-thin coatings are achieved on the surface of each particle, with a precisely controllable film thickness of 0.1–100 nm. This coating process eliminates dead zones and agglomeration, enabling surface modification of powder materials. Specific production results are as follows: 1. The entire particle is dynamically suspended, with no dead corners or agglomeration. The bottom turbine fan continuously circulates the powder, which is completely fluidized and in a flowing state. Each particle runs continuously at high speed in 360° and is fully dispersed, with no problem of powder stacking or obscuring. Nano-ultrafine powder and high specific surface area lithium battery powder can also ensure that the precursor is evenly in contact with the surface of all particles.

[0017] 2. High uniformity of atomic-level conformal coating: single-cycle growth thickness fluctuation <3%, and minimal difference in film thickness across the entire batch of powder; in roller equipment, powder friction and tumbling still result in local particle overlap, and film thickness dispersion can reach 8%~15%.

[0018] 3. The temperature and precursor partial pressure of the powder in the deep and shallow layers are completely consistent, and there is no local temperature field or gas field deviation.

[0019] All of the components described above are existing technologies, and those skilled in the art can use any model and existing design that can achieve their corresponding functions.

[0020] The above description is only a preferred embodiment of the present invention. It should be noted that those skilled in the art can make several modifications and improvements without departing from the inventive concept of the present invention, and these all fall within the protection scope of the present invention.

Claims

1. A vacuum powder ALD device, characterized in that, Includes a turbine blower (1), the inlet of which is connected to one end of the feed pipe (6), and the outlet of which is connected to one end of the air inlet pipe (2). The part of the air inlet pipe (2) near the turbine blower (1) is connected to one end of the process pipe (7) and one end of the powder collection pipe (8). The other end of the air inlet pipe (2) is connected in sequence to a transparent PC window (3) and a first KF50 vacuum ball valve (41) and is connected to the inlet of the vacuum circulation pipe (5). The other end of the feed pipe (6) is connected in sequence to another PC window (3) and a second KF50 vacuum ball valve (41). A 50 vacuum ball valve (42) is connected to the outlet of the circulation pipeline (5). The other end of the process pipeline (7) and the other end of the powder collection pipeline (8) are connected to the first-stage cyclone dust collector (141) and the second-stage cyclone dust collector (142) in sequence. The outlet of the second-stage cyclone dust collector (142) is connected to the vacuum filter (15) and the vacuum pump in sequence. The bottom of the first-stage cyclone dust collector (141) and the second-stage cyclone dust collector (142) are connected to the feed pipe (6) through pipelines. A vortex flow meter (19) is provided at the PC window (3) of the feed pipe (6).

2. The vacuum powder ALD equipment as described in claim 1, characterized in that, The process pipeline (7) is equipped with a first ferrule ball valve (9), the powder collection pipeline (8) is equipped with a second ferrule ball valve (10), the pipeline between the bottom of the first-stage cyclone dust collector (141) and the feed pipe (6) is equipped with a material box (11), the pipeline between the first-stage cyclone dust collector (141) and the material box (11) is equipped with a third ferrule ball valve (13) and a fourth ferrule ball valve (12), the pipeline between the material box (11) and the feed pipe (6) is equipped with a fifth ferrule ball valve (16) and a sixth ferrule ball valve (17), and the pipeline between the bottom of the second-stage cyclone dust collector (142) and the feed pipe (6) is equipped with a seventh ferrule ball valve (18).

3. The vacuum powder ALD equipment as described in claim 1, characterized in that, During operation, the first ferrule ball valve (9), the second ferrule ball valve (10), the third ferrule ball valve (13), the fourth ferrule ball valve (12), the fifth ferrule ball valve (16), the sixth ferrule ball valve (17), the first KF50 vacuum ball valve (41), and the second KF50 vacuum ball valve (42) are closed, and the seventh ferrule ball valve (18) is opened to load materials. Turn on the chiller to cool down the water, and open the first KF50 vacuum ball valve (41) and the second KF50 vacuum ball valve (42). Then turn on the vacuum pump to evacuate the vacuum until the vacuum level, magnetofluid temperature, and vacuum pipe temperature meet the requirements. Start the turbine fan (1), open the first ferrule ball valve (9), the third ferrule ball valve (13), and the fourth ferrule ball valve (12), and then open the fifth ferrule ball valve (16) and the sixth ferrule ball valve (17) to carry out the process; The sixth ferrule ball valve (17) and the seventh ferrule ball valve (18) are used to return powder to the circulating pipeline (5) to continue the process. During the process cycle, the powder flow rate is measured in real time by the vortex flow meter (19). After the process is completed, first close the third ferrule ball valve (13), then close the fourth ferrule ball valve (12). Then close the first ferrule ball valve (9), open the second ferrule ball valve (10), close the sixth ferrule ball valve (17) and the fifth ferrule ball valve (16), and collect dust until it is complete; After completion, close the second ferrule ball valve (10), then close the third ferrule ball valve (13) and the fourth ferrule ball valve (12). Finally, shut down the turbine fan (1).

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