[0024] In order to make the objectives, technical solutions, and advantages of the present invention clearer, the following further describes the present invention in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, but not to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
[0025] Such as figure 1 As shown, an embodiment of the present invention provides a continuous atomic layer deposition device for coating the surface of nanoparticles, including a feed bin 4, a first reaction chamber, a second reaction chamber, and a discharge bin 17, wherein the feed The bin 4 is used to control the nano-particles to enter the first reaction chamber. The nano-particles are dispersed by the ultrasonic vibrating net 9 inside the first reaction chamber and react with the first precursor reactant; the reacted nano-particles undergo the first rotation The feeding device 7 enters the first cleaning chamber 12, and cleans the reaction by-products by gas purging inside the first cleaning chamber 12; the nanoparticles cleaned by the first cleaning chamber are sent to the second reaction chamber and are The inside of the second reaction chamber is broken up by the ultrasonic vibrating net 9 and reacts with the second precursor reactant; the reacted nanoparticles enter the second cleaning chamber through the second rotating feeding device, and are inside the second cleaning chamber The reaction by-products are cleaned by gas purging, and finally sent to the output bin 17. Through the mutual cooperation of the above-mentioned components, the continuous and uniform deposition of nanoparticles is realized without agglomeration.
[0026] Each component will be described in more detail below.
[0027] Such as figure 1 As shown, the feed bunker 4 is used to control the entry of nanoparticles into the first reaction chamber, which includes a feed bunker body, a feed bunker vacuum valve 6 and a feed bunker suction port 5 arranged on the feed bunker body, wherein The silo vacuum valve is used to realize the selective isolation and communication between the feeding silo and the first reaction chamber and the external environment, and the inlet of the feeding silo is used to extract the gas in the feeding silo and maintain its vacuum degree. There are two vacuum valves. In actual operation, the vacuum valve of the feed bin close to the external environment is opened to allow the nanoparticles to enter the feed bin, and then the valve is closed and the feed bin body is evacuated through the inlet of the feed bin. When the vacuum in the feeding bin is the same or similar to the vacuum in the first reaction chamber, stop vacuuming the feeding bin, and open the vacuum valve connected to the feeding bin and the first reaction chamber to make the nanoparticles The feed bin enters the first reaction chamber.
[0028] Such as figure 1 As shown, the discharge bin 17 is used to control the removal of nanoparticles from the second cleaning chamber, which includes a discharge bin body, a discharge bin vacuum valve 19 and a discharge bin inflation port 18 arranged on the discharge bin body, wherein The silo vacuum valve is used to realize isolation and communication between the discharge silo and the second reaction chamber and the external environment, and the discharge silo inflation port is used to extract the gas in the discharge silo and maintain its vacuum. Specifically, there are two vacuum valves in the discharge bin. The discharge bin is connected to the second cleaning chamber and the external environment through a vacuum valve respectively to control the nanoparticles to leave the entire deposition equipment. When the nanoparticles leave the deposition equipment, the discharge bin is close to the first 2. The vacuum valve of the cleaning chamber is opened to allow the nanoparticles to enter the discharge bin, then the valve is closed and the discharge bin is filled with inert gas through the discharge bin inflation port. When the discharge bin pressure is the same or similar to the external environment pressure, Stop inflating the discharge bin and open the vacuum valve that connects the discharge bin with the external environment, so that the nanoparticles will enter the outside from the discharge bin to be collected.
[0029] Specific, such as figure 1 As shown, the ultrasonic vibrating mesh is a cone-shaped vibrating mesh, which uses ultrasonic vibration to break up the agglomeration between nanoparticles. The ultrasonic vibration frequency of the ultrasonic vibrating mesh is 30000Hz-40000Hz. At this vibration frequency, high-frequency vibration is generated. The force is greater than the agglomeration force between particles to effectively prevent particle agglomeration. At the same time, the introduction of ultrasonic vibration can effectively prevent the screen from clogging. The cone angle of the conical vibrating net is on the top, that is, it is arranged in an inverted V shape, and it is arranged with multiple layers.
[0030] Such as figure 1 As shown, the first reaction chamber includes a first reaction chamber 1, a first precursor reactant inlet 2 provided on the side of the first reaction chamber, and a first precursor reactant provided above the first reaction chamber The suction port 3, the first reaction chamber 1 is equipped with an ultrasonic vibration net. The nanoparticles are dispersed by the ultrasonic vibration net in the first reaction chamber and react with the first precursor reactant, which enters through the first precursor reactant. Air port 2 supplies the first precursor reactant to react with the surface of the nanoparticle and adsorb on the surface of the nanoparticle. The first precursor reactant suction port 3 is connected to a vacuum pump to remove by-products and non-participating reactions. The precursor reactant of the reaction, while maintaining the required vacuum during the reaction.
[0031] Such as figure 1 As shown, the second reaction chamber includes a second reaction chamber 14, a second precursor reactant inlet 16 provided on the side of the second reaction chamber, and a second precursor reactant provided above the second reaction chamber At the suction port 15, the second reaction chamber 14 is equipped with an ultrasonic vibration net. The nanoparticles are dispersed by the ultrasonic vibration net in the second reaction chamber and react with the second precursor reactant, which enters through the second precursor reactant. The gas port 16 supplies the second precursor reactant to react with the first precursor reactant adsorbed on the surface of the nanoparticle to form a thin film. The second precursor reactant suction port 15 is connected to a vacuum pump for pumping In addition to reaction by-products and precursor reactants not participating in the reaction, while maintaining the required vacuum during the reaction. Specifically, both the first reaction chamber and the second reaction chamber are provided with heating and heat preservation devices 10.
[0032] Specifically, the first cleaning chamber and the second cleaning chamber are fluidized and cleaned in the cleaning chamber by continuously introducing inert gas, and the structure of the two is the same, such as figure 1 As shown, both the first cleaning chamber and the second cleaning chamber include a cleaning chamber cavity and an inert gas inlet 11 and a cleaning chamber suction port 8 provided on the cleaning chamber cavity, wherein the inert gas inlet is provided in the cleaning chamber The bottom and sides of the cavity are used to pass inert gas into the cleaning chamber cavity to clean the excess precursor reactants and reaction by-products on the surface of the nanoparticles. During cleaning, the inert gas is continuously introduced into the cleaning chamber cavity through the air inlet At the same time, the suction port is always connected with the vacuum pump, and the unreacted precursor and reaction by-products are sucked away from the suction port by the vacuum pump to realize the cleaning of particles. The cleaning chamber air extraction port is located above the cleaning chamber cavity, which is connected with a vacuum pump, and is used to extract the gas in the cleaning chamber cavity to maintain the vacuum state inside the cleaning chamber. During the cleaning process of nanoparticles, the cleaning chamber air extraction port is always Connect the vacuum pump for vacuuming. After cleaning, turn off the vacuum pump to make the nanoparticles fall and enter the next cavity through the rotating feeding device. Specifically, the cleaning chamber cavity of the first cleaning chamber is connected to the first reaction chamber 1 of the first reaction chamber through the first rotary feeding device, and the cleaning chamber cavity of the second cleaning chamber is connected to the first reaction chamber 1 of the first reaction chamber through the second rotary feeding device. It is connected to the second reaction chamber 14 of the second reaction chamber.
[0033] Specifically, the nanoparticles cleaned in the first cleaning chamber are sent into the second reaction chamber through the conveyor belt 13. A third rotary feeding device is provided between the conveyor belt and the first cleaning chamber, and the third rotary feeding device is used for The first cleaning chamber is connected to the conveyor belt to supply the materials cleaned in the first cleaning chamber to the conveyor belt, and then the cleaned materials are sent to the second reaction chamber through the conveyor belt.
[0034] Further, a fourth rotary feeding device is provided between the second cleaning chamber and the discharging bin, and the fourth rotary feeding device is used to connect the second cleaning chamber and the discharging bin to connect the second cleaning chamber The cleaned materials are sent to the discharge bin.
[0035] Specifically, the structures of the first rotary feeding device to the fourth rotary feeding device are the same, such as figure 2 As shown, they all include a feeding cavity, a rotor 20 and an isolation assembly arranged inside the feeding cavity. The upper part of the feeding cavity is provided with a feeding port, and the lower part is provided with a discharging port for connecting the reaction chamber with The cleaning chamber of the cleaning chamber is connected, or the cleaning chamber of the cleaning chamber is connected with the conveyor belt, or the cleaning chamber of the cleaning chamber is connected with the discharge bin, the isolation component is used to isolate the feeding chamber into multiple parts. A sub-cavity. Such as figure 2 As shown, the isolation assembly includes a sliding piece 22 and a spring 21 arranged on one end of the sliding piece. The rotor 20 is provided with a groove, and the end of the sliding piece 22 where the spring is installed is inserted into the groove of the rotor, such as figure 2 As shown, the spring is in a compressed state, and the sliding plate is always in contact with the inner wall of the feeding cavity under the action of the elastic force of the spring during operation to divide the feeding cavity into multiple sub-cavities. At the same time, with use, the sliding piece The end gradually wears out, and at this time, the elastic force of the spring can still ensure that the end of the slide is always in contact with the inner wall of the feeding cavity. The rotary feeding device drives the spring and the sliding plate to rotate intermittently through the intermittent rotation of the rotor, thereby realizing quantitative feeding in the reaction process, that is, the intermittent rotation of the rotary feeding device controls the nano particles in the first reaction chamber and the first reaction chamber. Transfer between the cleaning chambers, between the first cleaning chamber and the conveyor belt, between the second reaction chamber and the second cleaning chamber, and between the second cleaning chamber and the discharge bin. Such as figure 2 As shown, a total of three sets of isolation components are provided to divide the feeding cavity into three sub-cavities.
[0036] Preferably, such as image 3 As shown, a guide post 23 is arranged in the groove of the rotor, and the spring 21 is sleeved on the guide post 23. The guide post plays a role of protecting the spring and preventing the spring from collapsing sideways during installation and rotation. Further, the rotation speed of the rotary feeding device is 5-30r/min, and the intermittent time is related to the speed of the powder falling during the reaction, and the general intermittent time is 5s-30s.
[0037] The working process of the continuous atomic layer deposition apparatus of the present invention will be described below.
[0038] The continuous atomic layer deposition equipment for nanoparticle coating coats the nanoparticles entering the reaction chamber through chemical adsorption and reaction. The temperature of the first reaction chamber and the second reaction chamber can be maintained so that no precursor reactants are produced Within the decomposition temperature range, the reaction chamber of each reaction chamber is fed with only one precursor reactant. The nanoparticles first react with one precursor reactant, and then enter another reaction chamber to react with another precursor. The thing reacts.
[0039] First, open the vacuum valve of the feed bin close to the external environment to allow the nanoparticles to enter the feed bin, then close the valve, and vacuum the feed bin through the feed bin exhaust port 5, and wait for the vacuum of the feed bin to react with the first reaction When the vacuum of the cavity is the same or similar, stop pumping the feed bin, open the valve of the feed bin close to the first reaction chamber to allow the nanoparticles to enter the first reaction chamber, and then close the valve. Repeating the above steps can continuously transport the nanoparticles into the reaction chamber with a certain degree of vacuum.
[0040] After the nanoparticles enter the first reaction chamber 1, under the action of the conical ultrasonic vibrating mesh, the agglomeration between the nanoparticles is continuously destroyed, and the dispersed nanoparticles are formed from the filter mesh under the action of gravity and vibration. Pass to the next layer of filter screen. Because the filter screen used by ultrasonic vibration is in a positive cone shape, the number of nanoparticles falling from the edge of the filter screen is more than the number of nanoparticles falling from the center of the filter screen. The precursor reactant is introduced into the reaction chamber from the first precursor reactant inlet 2 and the first precursor reactant inlet is provided on the side wall of the reaction chamber. Therefore, from the side wall to the reaction chamber The concentration of the precursor reactant at the center of the nanoparticle gradually decreases, so that more precursor reactants (that is, higher concentration) pass into the place with a large number of nanoparticles, which is beneficial to improve the utilization of the precursor.
[0041] After passing through the ultrasonic vibration filter, the nanoparticles enter the first cleaning chamber through the rotary feeding device. Then, the entire cleaning chamber is filled with inert gas while the cleaning chamber is evacuated by a vacuum pump, so that the cleaning process is always in a vacuum state. And make the nano-particles are constantly blown up and down in the cleaning chamber under the action of the airflow. After a period of cleaning, stop filling the inert gas and stop vacuuming the cleaning chamber, and the nanoparticles fall to the The bottom of the cleaning chamber is dropped on the conveyor belt through the rotating feeding device, and the flow of inert gas is 10-500sccm.
[0042] Nanoparticles enter the second reaction chamber 14 under the conveying operation of the conveyor belt. The second precursor reactant enters the second reaction chamber through the second precursor reactant inlet 16 and interacts with the chemical groups on the surface of the nanoparticle. The reaction forms a thin film, and the nano particles that have completed the reaction enter the second cleaning chamber through the rotating feeding device to clean the nano particles.
[0043] The cleaned nanoparticles leave the reaction system from the discharge bin 17. When the nanoparticles leave the reaction system, first open the vacuum valve on the side of the discharge bin close to the second cleaning chamber to make the nanoparticles enter the discharge bin from the cleaning chamber, and then Close the valve and at the same time fill the discharge bin with inert gas through the discharge bin air inlet 18. When the pressure in the discharge bin is the same or similar to the outside pressure, stop charging and open the discharge bin near the outside environment. The vacuum valve allows the nanoparticles to enter the external environment to be collected.
[0044] Nanoparticles enter the reaction chamber from the feed bin to leave the cleaning chamber from the discharge bin to complete an atomic layer deposition reaction cycle. When you need to deposit multiple layers of films or thicker films on the surface of nanoparticles, you only need to connect the outlet of the discharge bin with the inlet of the inlet, and allow the nanoparticles to pass through the two reaction chambers multiple times. Finish the coating of a thicker film.
[0045] The continuous atomic layer deposition device for coating nanoparticles of the present invention overcomes the agglomeration between nanoparticles by means of ultrasonic vibration, and increases the probability of contact between nanoparticles and precursor reactants through the vibration of the cone screen , Improve the utilization rate of the precursor, realize the uniform deposition of the film on the particle surface, and realize the continuous deposition of the film on the surface of the nano particle by setting an independent continuous reaction chamber and a cleaning chamber.
