High-throughput continuous powder atomic layer deposition equipment
By designing a high-throughput continuous powder atomic layer deposition equipment, the preheating functions of the first and second reaction chambers and buffer chambers are used to solve the problems of uniform coating of powder materials and precise control of atomic levels, and efficient powder film preparation and performance optimization are achieved.
Patent Information
- Application Number
- CN202510267081.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-07
- Publication Date
- 2025-06-17
- Estimated Expiration
- 2045-03-07
AI Technical Summary
Existing chemical vapor deposition, physical vapor deposition and spraying technologies are difficult to achieve uniform coating of powder materials and precise atomic control of thickness and components, limiting the performance optimization of catalyst and battery materials.
A high-throughput continuous powder atomic layer deposition equipment is designed, including a powder automatic feeding system, first and second reaction chambers, pumping systems, precursors and carrier gas delivery systems, heating systems and control systems. The device performs surface chemical reactions through the first and second reaction chambers respectively, and combines the preheating function of the buffer chamber to improve the preparation efficiency of the powder film.
The uniform coating and precise atomic control of powder materials are achieved, the preparation efficiency of macroscopic powder atomic layer deposition is improved, and the performance of catalyst and battery materials is optimized.
Smart Images

Figure CN119753640B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of thin film preparation, and in particular to a high-throughput continuous powder atomic layer deposition device. Background Art
[0002] The powder atomic layer deposition system is a process system for coating the surface of powder materials. Its principle is the atomic layer deposition technology, also known as atomic layer epitaxy technology, which is an ordered, surface self-limiting saturation, "bottom-up" chemical vapor thin film deposition technology. Two precursors alternately undergo molecular-level self-limiting reactions on the surface of an object, thereby realizing the uniform and controllable deposition of a thin film, and its thickness can be achieved by changing the number of ALD deposition cycles.
[0003] The uniform coating and surface modification of powder materials is an important technology in modern materials science, and is widely used in the fields of lithium batteries, energy catalysis, medicine, metallurgy, and military. These technologies enhance the performance of powder raw materials, improve chemical stability, conductivity, or catalytic activity, etc., by uniformly coating one or more layers of substances on the surface of powder particles or by changing the surface properties of the powder through chemical or physical methods.
[0004] However, for the uniform coating and surface modification of powder materials, existing chemical vapor deposition (CVD), physical vapor deposition (PVD), spraying technology, etc. are difficult to achieve uniform coating of powder materials and atomic-level precise control of their thickness and composition, which greatly limits the optimization of their performance such as catalyst and battery material modification. The atomic layer deposition (ALD) technology, based on the unique technical characteristics of self-limiting surface molecular reactions, provides a powder material modification solution that takes into account uniformity, conformality, and atomic precision, and provides a new technical approach for the best optimization of material performance. With the increasing demand for high-performance composite materials, the research and development of macro-scale powder ALD equipment and technology is particularly important.
[0005] To solve the above technical problems, a novel atomic layer deposition device is urgently needed. Summary of the Invention
[0006] To solve the problem of macro-scale powder coating, the present invention proposes a high-throughput continuous powder atomic layer deposition device.
[0007] The high-throughput continuous powder atomic layer deposition device of the present invention includes a powder automatic feeding system, a first reaction chamber, a second reaction chamber, a pumping system, a precursor and carrier gas delivery system, a heating system, and a control system. Among them,
[0008] The first reaction chamber is used for the surface chemical reaction between powder and the first precursor to generate a thin film.
[0009] The second reaction chamber is used to perform a surface chemical reaction between the powder after the reaction in the first reaction chamber and the second precursor to complete the growth of the required thin film;
[0010] The pumping system is used to evacuate the first reaction chamber and the second reaction chamber, or adjust the pressure in the first reaction chamber and the second reaction chamber by pumping air from the first reaction chamber and the second reaction chamber, or evacuate the unadsorbed or unreacted precursor and / or reaction by-products in the first reaction chamber and the second reaction chamber;
[0011] The precursor and carrier gas pipeline system is used to supply the first precursor and carrier gas to the first reaction chamber, and supply the second precursor and carrier gas to the second reaction chamber;
[0012] The control system is used to control the automation of the entire atomic layer deposition process; wherein, it further includes:
[0013] A first buffer chamber communicated with the first reaction chamber to preheat the powder falling into the first reaction chamber; and a second buffer chamber communicated with the first reaction chamber and the second reaction chamber respectively to preheat the powder falling into the second reaction chamber.
[0014] In an optional embodiment, a powder vertical lifting device and a vibrating screen mesh coaxial with the cavity of the reaction chamber are respectively arranged in the first reaction chamber and the second reaction chamber. After the powder is lifted by the powder vertical lifting device, it undergoes a surface chemical reaction with the precursor, then vibrates and disperses and falls through the vibrating screen mesh, and is lifted again by the powder vertical lifting device, and the cycle repeats.
[0015] In an optional embodiment, a gas on-line analysis system is further included. The gas on-line analysis system is connected to the first reaction chamber and the second reaction chamber respectively, and is used to monitor the content of the reaction by-products in the reaction chamber in real time on-line and judge in real time whether the reaction has been completed.
[0016] In an optional embodiment, the first buffer chamber includes a material storage chamber. An inlet vacuum valve is arranged at the inlet of the material storage chamber. An outlet vacuum valve is arranged between the outlet of the material storage chamber and the inlet of the first reaction chamber. A vacuum pump and a pressure gauge are arranged on the material storage chamber to evacuate the material storage chamber of the first buffer chamber; wherein, when the vacuum degree of the first buffer chamber is close to the vacuum degree of the first reaction chamber, the outlet gate valve of the first buffer chamber is opened.
[0017] The second buffer chamber includes a material storage chamber, a feed port vacuum valve is provided at the feed port of the material storage chamber, and a discharge port vacuum valve is provided between the discharge port of the material storage chamber and the feed port of the second reaction chamber. A vacuum pump and a pressure gauge are provided on the material storage chamber for evacuating and monitoring the pressure of the material storage chamber of the second buffer chamber. Wherein, when the vacuum degree of the second buffer chamber is close to the vacuum degree of the second reaction chamber, the discharge port vacuum valve of the second buffer chamber is opened.
[0018] In an alternative embodiment, it further includes an exhaust gas heat treatment system respectively connected to the first reaction chamber and the second reaction chamber. The exhaust gas heat treatment system is arranged in front of the pumping system and is used for pyrolyzing the unreacted precursor and / or reaction by-product at a high temperature before they reach the pumping system, so as to decompose them into safe gases that can be directly recycled for exhaust gas.
[0019] In an alternative embodiment, the vibrating screen is provided with at least two layers.
[0020] In an alternative embodiment, the vibrating screen is elastically connected to the first reaction chamber and the second reaction chamber respectively.
[0021] In an alternative embodiment, the pumping system further includes a pneumatic valve for opening or blocking the vacuum pumping of the first reaction chamber and the second reaction chamber by the pumping system.
[0022] In an alternative embodiment, it further includes a first material lifting conveyor belt, wherein the first material lifting conveyor belt is used for feeding the powder from the powder automatic feeding system into the first buffer chamber.
[0023] In an alternative embodiment, it further includes a second material lifting conveyor belt, and the second material lifting conveyor belt is used for feeding the powder after reaction in the first reaction chamber into the second buffer chamber.
[0024] In an alternative embodiment, it further includes a vibrating material collector, and the vibrating material collector is arranged at the discharge port of the second reaction chamber for collecting the powder after the film growth is completed.
[0025] Compared with the prior art, the atomic layer deposition equipment of the present invention improves the preparation efficiency of macro-scale powder atomic layer deposition by providing a first reaction chamber and a second reaction chamber and buffer chambers respectively connected to the first reaction chamber and the second reaction chamber, preheating the powder in the pre-storage chamber in advance before entering the reaction chamber, and carrying out the reaction of the powder with different precursors in different reaction chambers.
[0026] The above technical features can be combined in various technically feasible ways to produce new embodiments as long as the purpose of the present invention can be achieved. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The present invention will be described in more detail below based on only non-limiting embodiments and with reference to the accompanying drawings. Among them:
[0028] Figure 1 shows a schematic structural diagram of a high-throughput continuous powder atomic layer deposition device according to the present invention;
[0029] Figure 2 shows Figure 1 a schematic structural diagram of the buffer chamber of the deposition device in;
[0030] Figure 3 shows Figure 1 a schematic structural diagram of the first reaction chamber of the deposition device in;
[0031] Figure 4 shows a schematic structural diagram of a high-throughput continuous powder atomic layer deposition device according to another embodiment of the present invention.
[0032] In the figure, the same components are marked with the same reference numerals. The drawings are not drawn to actual scale.
[0033] Among them, the reference numerals are:
[0034] 1. Automatic powder feeding system; 2. First lifting conveyor belt; 3. First buffer chamber; 31. Inlet vacuum valve; 32. Stock chamber; 33. Outlet vacuum valve; 34. Pressure gauge; 35. Vacuum pump; 4. First reaction chamber; 41. Housing; 42. Reaction cavity; 43. Outlet vacuum valve; 45, 48. Vibrating screen; 46. Elastic connection; 47. Jet port; 49. Powder vertical lifting device; 410. Vacuum gauge; 411. Pneumatic valve; 5. Second lifting conveyor belt; 6. Second buffer chamber; 7. Second reaction chamber; 8. Vibrating material collector; 9. Control system; 10. Precursors and carrier gas pipeline system; 11. Pumping system; 12. Tail gas heat treatment system; 13. Gas on-line analysis system. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0035] The present invention will be further described in detail below with reference to the accompanying drawings of the specification and specific embodiments. It should be noted that as long as there is no conflict, the various embodiments in the present invention and the various features in each embodiment can be combined with each other, and the technical solutions formed are all within the protection scope of the present invention.
[0036] Those parts not described in the present invention can be implemented by adopting or referring to the existing technologies.
[0037] Such as Figure 1As shown in the figure, a high-throughput continuous powder atomic layer deposition device includes a powder automatic feeding system 1, a first reaction chamber 4, a second reaction chamber 7, a pumping system 11, and a heating system. Among them,
[0038] The first reaction chamber 4 is used for the surface chemical reaction between the powder and the first precursor to generate a thin film;
[0039] The second reaction chamber 7 is used for the surface chemical reaction between the powder after the reaction in the first reaction chamber 4 and the second precursor to complete the growth of the required thin film;
[0040] The pumping system 11 is used to evacuate the first reaction chamber 4 and the second reaction chamber 7, or adjust the pressure in the first reaction chamber and the second reaction chamber by pumping air from the first reaction chamber and the second reaction chamber, or evacuate the unadsorbed or unreacted precursors and / or reaction by-products in the first reaction chamber 4 and the second reaction chamber 7; Among them, it also includes
[0041] A first buffer chamber 3 communicated with the first reaction chamber 4 to preheat the powder falling into the first reaction chamber 4; and a second buffer chamber 6 communicated with the first reaction chamber 4 and the second reaction chamber 7 respectively to preheat the powder falling into the second reaction chamber 7.
[0042] The atomic layer deposition device of the present invention is provided with a first reaction chamber and a second reaction chamber, and the reactions of the powder with different precursors are carried out in different reaction chambers respectively, which improves the preparation efficiency of the powder thin film. At the same time, the device is provided with a buffer chamber, and the powder is preheated in the buffer chamber before entering the reaction chamber, which further improves the preparation efficiency of the powder thin film, and can realize macro-scale thin film preparation treatment.
[0043] In an optional embodiment, a powder vertical lifting device 49 and a vibrating screen 48 coaxial with the reaction chamber are respectively arranged in the first reaction chamber 4 and the second reaction chamber 7. Among them, after the powder is lifted by the powder vertical lifting device 49, it undergoes a surface chemical reaction with the precursor and then vibrates and disperses and falls through the vibrating screen 48, and is lifted again by the powder vertical lifting device 19, and circulates reciprocally.
[0044] Optionally, the powder vertical lifting device 49 can be a feeding screw or the like.
[0045] Such as Figure 1 and Figure 3As shown in the figure, taking the first reaction chamber 4 as an example, the first reaction chamber 4 includes a housing 41. Inside the first reaction chamber 4, there are a powder vertical lifting device 49, vibrating sieve meshes 45 and 48 that are coaxially arranged with the reaction cavity 42. When the powder is preheated in the first buffer chamber 3 and then falls into the first reaction chamber 4, it is lifted by the powder vertical lifting device 49. After being lifted, the powder undergoes a surface chemical reaction with the first precursor in the first reaction chamber and then falls. When the powder falls onto the vibrating sieve meshes 45 and 48, the vibrating sieve meshes 45 and 48 vibrate to disperse the powder as it falls. The falling powder is lifted again by the powder vertical lifting device 49 to continue the surface chemical reaction with the first precursor. This cycle is repeated, so that all the powders are in full contact with the first precursor. During each deposition process, a large amount of powders are uniformly coated, effectively improving the powder coating rate and deposition uniformity.
[0046] The vibrating sieve meshes 45 and 48 disperse the powder falling on them through vibration to prevent powder agglomeration.
[0047] The structure of the second reaction chamber 7 is the same as that of the first reaction chamber 4. The reaction steps of the powder with the second precursor after falling into the second reaction chamber 7 are the same as those of the powder with the first precursor after falling into the first reaction chamber 4, and will not be elaborated here.
[0048] After the surface chemical reaction of the powder with the first precursor in the first reaction chamber 4 is completed, the powder falls into the second reaction chamber 7 and continues to undergo a surface chemical reaction with the second precursor to complete the growth of the thin film.
[0049] Furthermore, the first precursor and the second precursor can be respectively fed into the first reaction chamber 4 and the second reaction chamber 7 through the precursor and carrier gas gas path system 10.
[0050] In an optional embodiment, the deposition device of the present invention further includes a gas online analysis system 13, and the gas online analysis system 13 is respectively connected to the first reaction chamber 4 and the second reaction chamber 7.
[0051] Optionally, the gas online analysis system 13 can be composed of a residual gas analyzer and a vacuum differential chamber, and the vacuum degree range of the gas online analysis system 13 is 5E - 6 mbar.
[0052] By setting the gas online analysis system 13, the content of reaction by-products in the reaction chamber can be monitored online in real time, and it can be judged in real time whether the reaction has been completed.
[0053] Optionally, the gas online analysis system 13 is arranged between the pumping system 11 and the first reaction chamber 4 / second reaction chamber 7.
[0054] In an alternative embodiment, the first buffer chamber 3 includes a material storage chamber 32. A feed port vacuum valve 31 is provided at the feed port of the material storage chamber 32. A discharge port vacuum valve 33 is provided between the discharge port of the material storage chamber 32 and the feed port of the first reaction chamber 4. A vacuum pump 35 and a pressure gauge 34 are provided on the material storage chamber 32 for performing a vacuum pumping operation on the material storage chamber 32 of the first buffer chamber 3. Among them, the first buffer chamber 3 is disposed above the first reaction chamber 4. When the vacuum degree of the first buffer chamber 3 is the same as that of the first reaction chamber 4, the discharge port vacuum valve 33 of the first buffer chamber 3 is opened.
[0055] After all the powder materials enter the material storage chamber 32 of the first buffer chamber 3, the feed port vacuum valve 31 and the discharge port vacuum valve 33 of the first buffer chamber 3 are in a closed state. At this time, the powder materials entering the first buffer chamber 3 are preheated. Meanwhile, the vacuum pump 35 is used to perform a vacuum pumping operation on the material storage chamber 32. When the vacuum degree of the material storage chamber 32 is the same as or substantially the same as that of the first reaction chamber 4, the discharge port vacuum valve 33 is opened, and the powder materials enter the first reaction chamber 4 under the action of gravity. At this time, the discharge port vacuum valve 33 is closed again.
[0056] Preferably, the first buffer chamber 3 has a self-heating function, and the heating temperature is 180 - 200 °C, and the maximum heating temperature can be 200 °C.
[0057] The structure of the second buffer chamber 6 is the same as that of the first buffer chamber 3, and also includes a material storage chamber. A feed port vacuum valve is provided at the feed port of the material storage chamber. A discharge port vacuum valve is provided between the discharge port of the material storage chamber and the feed port of the second reaction chamber. A vacuum pump and a pressure gauge are provided on the material storage chamber for performing a vacuum pumping operation on the material storage chamber of the second buffer chamber. When the vacuum degree of the second buffer chamber is the same as that of the second reaction chamber, the discharge port vacuum valve of the second buffer chamber is opened.
[0058] Similarly, the second buffer chamber also has a self-heating function, and the heating temperature is 180 - 200 °C, and the maximum heating temperature can be 200 °C. Among them, the self-heating of the second buffer chamber starts heating at the initial stage when the equipment starts to work and keeps warm until the reaction ends.
[0059] Furthermore, the self-heating functions of the first buffer chamber 3 and the second buffer chamber 6 are controlled by a control system 9.
[0060] In an alternative embodiment, the equipment of the present invention further includes a tail gas heat treatment system 12 respectively connected to the first reaction chamber 4 and the second reaction chamber 7. The tail gas heat treatment system 12 is disposed in front of the pumping system 11 for performing high-temperature decomposition on the incompletely reacted precursor and / or reaction by-products before they reach the pumping system 11.
[0061] The unreacted precursors and / or reaction by-products are pyrolyzed by the tail gas heat treatment system 12, and after meeting the tail gas recovery standard, the tail gas is recovered by the tail gas recovery system to prevent environmental pollution.
[0062] In an optional embodiment, the vibrating screen is provided with at least two layers. As Figure 3 shown, the vibrating screen includes an upper vibrating screen 45 and a lower vibrating screen 48. Through the vibration dispersion of the two vibrating screens, the agglomeration of the powder is prevented.
[0063] Furthermore, the vibrating screens 45 and 48 are respectively elastically connected to the first reaction chamber 4 and the second reaction chamber 7.
[0064] Taking the first reaction chamber 4 as an example, the first reaction chamber 4 is a vacuum-sealed cavity. Therefore, the stability of the installation needs to be maintained. Chamber branch flanges are provided on the cavities of the first reaction chamber 4 and the second reaction chamber 7. The vibrator is installed on the chamber branch flange through an elastic structure. The vibrating screens 45 and 48 are connected to the vibrator in the first reaction chamber 4 through an elastic connection 46. When the vibrating screens 45 and 48 disperse the powder agglomeration through vibration, the vibration force generated by the vibration is absorbed by the elastic connection 46, preventing the first reaction chamber 4 from vibrating due to the vibration of the vibrating screen, ensuring the stability of the first reaction chamber 4, and thus ensuring the vacuum tightness of the first reaction chamber 4.
[0065] Similarly, the vibrating screen in the second reaction chamber 7 is connected to the vibrator in the second reaction chamber 7 through an elastic connection, preventing the second reaction chamber 7 from vibrating due to the vibration of the vibrating screen and ensuring the vacuum tightness of the second reaction chamber 7.
[0066] Furthermore, an air jet port 47 is installed on the side wall of the chamber branch near the elastic connection 46 to prevent the powder from entering the vibrator fixed together with the elastic connection 46.
[0067] In an embodiment, the pumping system further includes pneumatic valves 411, which are respectively used to open or block the vacuum pumping of the pumping system 11 to the first reaction chamber 4 and the second reaction chamber 7.
[0068] In an embodiment, the device of the present invention further includes a first lifting conveyor belt 2. Among them, the first lifting conveyor belt 2 connects the discharge port of the powder automatic feeding system 1 and the feed port of the first buffer chamber 3, and is used to feed the powder from the powder automatic feeding system 1 into the first buffer chamber 3.
[0069] Optionally, the device of the present invention may further include a second lifting conveyor belt 5. The second lifting conveyor belt 5 connects the discharge port of the first reaction chamber 4 and the feed port of the second buffer chamber 6, and is used to feed the powder after reaction in the first reaction chamber 4 into the second buffer chamber 6.
[0070] Alternatively, as Figure 4 shown, the feed port of the second buffer chamber 6 can also be directly connected to the discharge port of the first reaction chamber 4, thereby omitting the second lifting conveyor 5.
[0071] When the powder enters the second buffer chamber 6, the second batch of powder can continue to pass through the powder automatic feeding system 1, enter the first buffer chamber 3 through the first lifting conveyor 2, and start a new round of film growth, thereby realizing the process of continuous film growth of high-throughput powder.
[0072] In one embodiment, the device of the present invention further includes a vibrating material collector 8, which is arranged below the second reaction chamber 7 and is used to collect the powder after the film growth is completed.
[0073] Further, a discharge vacuum valve 43 is arranged below the discharge port of the first reaction chamber 4 / below the discharge port of the second reaction chamber 7. When the gas online analysis system 13 detects that the surface chemical reaction in the first reaction chamber 4 is completed, the discharge vacuum valve 43 below the discharge port of the first reaction chamber 4 is opened, and the powder is fed to the second buffer chamber 6 by the second lifting conveyor 5; when the gas online analysis system 13 detects that the surface chemical reaction in the second reaction chamber 7 is completed, the discharge vacuum valve below the discharge port of the second reaction chamber 7 is opened, and the powder enters the vibrating material collector 8 to collect the powder after the film growth is completed.
[0074] In one embodiment, the control system of the device of the present invention is used to control the automated operation of the entire atomic layer deposition process, including controlling the lifting motor of the device, the opening and closing of all pneumatic valves, all heating points of the device, vibrating screen control, the flow control of precursors and gases, the extraction, reading of the vacuum degree of each chamber and the interlock control of the vacuum degree and the process flow, the automatic reading and data analysis of the gas online analysis system, the control of the tail gas heat treatment system, etc. The entire process of the device of the present invention has realized automated control, without manual intervention in the middle, saving manpower and material resources, improving the deposition efficiency of the atomic layer, and thus can realize the powder film preparation throughput.
[0075] Next, taking a Figure 1 shown device as an example, the working process of the atomic layer deposition device of the present invention will be described:
[0076] The bagged powder is manually placed into the automatic powder feeding system 1. The powder flows into the first lifting conveyor belt 2 through the automatic bag cutter inside the automatic powder feeding system 1, and the powder is transported to the first buffer chamber 3 via the first lifting conveyor belt 2. The first buffer chamber 3 preheats the powder. When all the powder enters the storage chamber 32 of the first buffer chamber 3, the vacuum valve 31 at the feed port is closed, and at this time, the vacuum valve 33 at the discharge port has been in a closed state. The vacuum pump 35 is used to evacuate the storage chamber 32 of the first buffer chamber 3. When the vacuum degree of the storage chamber 32 is pumped to be close to the vacuum degree of the first reaction chamber 4, the control system 9 controls the opening of the vacuum valve 33 at the discharge port. After the powder enters the first reaction chamber 4 under the action of gravity, the vacuum valve 33 at the discharge port is closed.
[0077] At this time, the first reaction chamber 4 has been preheated by the control system 9, and the maximum temperature can be heated to 350 °C. Moreover, the required vacuum degree has been achieved by the pumping system 11. The vacuum degree is measured by the vacuum gauge 410, and the control system 9 reads the vacuum degree in real time and interlocks the action with the vacuum valve 33 at the discharge port of the first buffer chamber 3.
[0078] The powder undergoes a surface chemical reaction with the first precursor in the first reaction chamber 4 (after the control system 9 gives an instruction, the first precursor enters the first reaction chamber 4 through the precursor and carrier gas pipeline system 10). The powder falls onto the vibrating screen meshes 45 and 48, and the vibrating screen meshes vibrate and disperse the powder. After the powder falls through the double-layer vibrating screen meshes 45 and 48, it is lifted again through the powder vertical lifting device 49, and this cycle repeats. At the same time, the gas online analysis system 13 monitors the content of reaction by-products in real time online, and can judge in real time whether the reaction has been completed.
[0079] The unreacted precursor and reaction by-products in the first reaction chamber 4 are pumped to the tail gas heat treatment system 12 by the pumping system 11 for high-temperature decomposition to meet the standard of tail gas recovery, and then pumped to the tail gas recovery device.
[0080] After the powder completes the chemical reaction with the first precursor in the first reaction chamber 4, the control system 9 controls the opening of the discharge vacuum valve 43 below the first reaction chamber 4. The powder enters the second buffer chamber 6 via the second lifting conveyor belt 5. The vacuum valves at the feed port and the discharge port of the second buffer chamber 6 are closed, and vacuum pumping is carried out in the storage chamber of the second buffer chamber 6 through the vacuum pump. The unreacted precursor and by-products carried out in the first reaction chamber 4 in the powder are pumped to the tail gas heat treatment system 12 for high-temperature decomposition, decomposed into safe gases that can be directly recycled for tail gas, and discharged to the tail gas recovery equipment.
[0081] The powder continues to enter the second reaction chamber 7 from the second buffer chamber 6, repeating the same steps as in the first reaction chamber 4, reacting with the second precursor, and completing the growth of the required thin film. After that, the control system 9 controls the opening of the discharge vacuum valve below the second reaction chamber 7, and the powder enters the vibrating material collector 8 to complete the entire process flow.
[0082] When the powder enters the second buffer chamber 6, the second batch of powder can continue to pass through the powder automatic feeding system 1, enter the first buffer chamber 3 through the first lifting conveyor belt 2, and start a new round of thin film growth, realizing the process of continuous thin film growth with high-throughput powder.
[0083] If the reaction process is not limited to the first precursor and the second precursor, and if more precursor cycles need to participate in the reaction, additional reaction chambers can be added to implement this process flow.
[0084] Unless otherwise defined, the technical terms or scientific terms used in the present invention shall have the ordinary meanings understood by those of ordinary skill in the field to which the present invention pertains. The terms "first", "second" and similar terms used in the present invention do not denote any order, quantity or importance, but are only used to distinguish different components. The terms such as "comprising" or "including" mean that the elements or objects appearing before the term cover the elements or objects listed after the term and their equivalents, without excluding other elements or objects. The terms such as "connected" or "coupled" are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. In the description of the present invention, the orientation or positional relationship indicated by terms such as "vertical" is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly. Therefore, it should not be construed as a limitation to the present invention.
[0085] At this point, those skilled in the art should recognize that although the present invention has been described with reference to the preferred embodiments, various improvements can be made to it and components therein can be replaced with equivalents without departing from the scope of the present invention. In particular, as long as there is no structural conflict, the technical features mentioned in each embodiment can be combined in any way. The present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.
Claims
1. A high-throughput continuous powder atomic layer deposition device, characterized in that: It includes a powder automatic feeding system, a first reaction chamber, a second reaction chamber, a pumping system, a precursor and carrier gas system, a heating system and a control system, wherein: The first reaction chamber is used for the powder to react with the first precursor to produce a thin film through a surface chemical reaction; The second reaction chamber is used for the powder after the reaction in the first reaction chamber to undergo a surface chemical reaction with the second precursor to complete the growth of the desired thin film; The pumping system is used to evacuate the first reaction chamber and the second reaction chamber, or to adjust the pressure in the first reaction chamber and the second reaction chamber by evacuating the first reaction chamber and the second reaction chamber, or to extract the unabsorbed or unreacted precursors and / or reaction byproducts in the first reaction chamber and the second reaction chamber; The precursor and carrier gas system is used to provide a first precursor and a carrier gas to the first reaction chamber, and to provide a second precursor and a carrier gas to the second reaction chamber; A control system for controlling the automated operation of the entire atomic layer deposition process; which also includes: a first buffer chamber connected to the first reaction chamber to preheat the powder falling into the first reaction chamber; and a second buffer chamber connected to the first reaction chamber and the second reaction chamber respectively to preheat the powder falling into the second reaction chamber; The first reaction chamber and the second reaction chamber are respectively provided with a powder vertical lifting device and a vibrating screen coaxially arranged with the cavity body of the reaction chamber, wherein the powder is lifted by the powder vertical lifting device, undergoes surface chemical reaction with the precursor, and then falls through the vibrating screen for vibration dispersion, and is lifted again by the powder vertical lifting device, repeating a reciprocating cycle.
2. The high-throughput continuous powder atomic layer deposition device according to claim 1, characterized in that: It also includes a gas online analysis system, which is connected to the first reaction chamber and the second reaction chamber respectively, and is used for real-time online monitoring of the content of reaction by-products in the reaction chamber, and real-time judgment of whether the reaction has been completed.
3. The high-throughput continuous powder atomic layer deposition device according to claim 2, characterized in that: The first buffer chamber comprises a material storage chamber, a material inlet vacuum valve is arranged at the material inlet of the material storage chamber, a material outlet vacuum valve is arranged between the material outlet of the material storage chamber and the material inlet of the first reaction chamber, and a vacuum pump and a pressure gauge are arranged on the material storage chamber to perform vacuum operation and pressure monitoring on the material storage chamber of the first buffer chamber; wherein, when the vacuum degree of the first buffer chamber is close to the vacuum degree of the first reaction chamber, the material outlet vacuum valve of the first buffer chamber is opened; The second buffer chamber includes a material storage chamber, a material inlet vacuum valve is arranged at the material inlet of the material storage chamber, a material outlet vacuum valve is arranged between the material outlet of the material storage chamber and the material inlet of the second reaction chamber, and a vacuum pump and a pressure gauge are arranged on the material storage chamber for vacuumizing and pressure monitoring the material storage chamber of the second buffer chamber, wherein when the vacuum degree of the second buffer chamber is close to the vacuum degree of the second reaction chamber, the material outlet vacuum valve of the second buffer chamber is opened.
4. The high-throughput continuous powder atomic layer deposition device according to claim 3, characterized in that: It also includes an exhaust gas heat treatment system connected to the first reaction chamber and the second reaction chamber respectively. The exhaust gas heat treatment system is arranged in front of the pumping system and is used for high-temperature decomposition of the incompletely reacted precursor and / or reaction by-products before the incompletely reacted precursor and / or reaction by-products reach the pumping system.
5. The high-throughput continuous powder atomic layer deposition device according to claim 1, characterized in that: The vibrating screen is provided with at least two layers.
6. The high-throughput continuous powder atomic layer deposition device according to claim 5, characterized in that: The vibration screen is elastically connected to the first reaction chamber and the second reaction chamber respectively.
7. The high-throughput continuous powder atomic layer deposition device according to claim 1, characterized in that: The pumping system further comprises a pneumatic valve for opening or blocking the vacuum pumping of the first reaction chamber and the second reaction chamber by the pumping system.
8. The high-throughput continuous powder atomic layer deposition device according to claim 4, characterized in that: It also includes a first material lifting conveyor belt, wherein the first material lifting conveyor belt is used to load the powder from the automatic powder loading system into the first buffer chamber.
9. The high-throughput continuous powder atomic layer deposition device according to claim 8, characterized in that: It also includes a second material lifting conveyor belt, which is used to load the powder material after reaction in the first reaction chamber to the second buffer chamber.
10. The high-throughput continuous powder atomic layer deposition device according to claim 8 or 9, characterized in that: It also includes a vibrating material receiver, which is arranged at the discharge port of the second reaction chamber and is used to collect the powder material that has completed the film growth.
Citation Information
Patent Citations
Continuous atomic layer deposition equipment used for nano-particle surface wrapping
CN108220917A
Buffer tank, supply block comprising same, and gas supply device
CN117716065A
Buffer tank, supply block including buffer tank, and gas supply device
US20240316581A1