High-flux continuous powder atomic layer deposition equipment

By designing a high-throughput continuous powder atomic layer deposition equipment, the first and second reaction chambers are used to perform surface chemical reactions with different precursors respectively, and the powder is preheated in the buffer chamber, the powder material coating and control problems are solved, and efficient film preparation is achieved.

CN119753640AActive Publication Date: 2025-04-04ACME (BEIJING) TECH CO LTD
View PDF 7 Cites 0 Cited by

Patent Information

Application Number
CN202510267081.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-07
Publication Date
2025-04-04
Estimated Expiration
2045-03-07

AI Technical Summary

Technical Problem

The existing chemical vapor deposition, physical vapor deposition and spraying technologies are difficult to achieve uniform coating of powder materials and precise atomic control of the thickness and components, limiting the performance optimization of catalyst and battery materials.

Method used

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 with different precursors through the first and second reaction chambers, and preheats the powder in the buffer chamber to improve the preparation efficiency.

Benefits of technology

The uniform coating of powder materials and the atomic precision control of films are achieved, the preparation efficiency of macro-level powder ALD equipment is improved, and high-throughput film preparation and treatment can be achieved.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119753640A_ABST
    Figure CN119753640A_ABST
Patent Text Reader

Abstract

The high-flux continuous powder atomic layer deposition equipment comprises an automatic powder feeding system, a first reaction cavity, a second reaction cavity, a pumping system, a precursor and carrier gas conveying system, a heating system and a control system, and further comprises a first buffer cavity communicated with the first reaction cavity and used for preheating powder falling into the first reaction cavity; the high-flux continuous powder atomic layer deposition equipment comprises a first reaction cavity, a second reaction cavity, a buffer cavity connected with the first reaction cavity and a buffer cavity communicated with the second reaction cavity, and a second buffer cavity communicated with the second reaction cavity and used for preheating powder falling into the second reaction cavity. The powder is preheated in the pre-storage cavity in advance before entering the reaction cavity, and the reaction of the powder and different precursors is carried out in different reaction cavities, so that the preparation efficiency of macro-magnitude powder atomic layer deposition is improved.
Need to check novelty before this filing date? Find Prior Art

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 used for surface coating of powder materials. Its principle is atomic layer deposition technology, also known as atomic layer epitaxy technology, which is a chemical vapor thin film deposition technology based on order, surface self-limiting saturation, and "bottom-up". The two precursors alternately undergo molecular-level self-limiting reactions on the surface of the object, thereby achieving uniform and controllable deposition of the film, and its thickness can be achieved by changing the number of ALD deposition cycles.

[0003] 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, electrical conductivity or catalytic activity, etc. by uniformly coating one or more layers of substances on the surface of powder particles or changing the surface properties of powders by chemical or physical methods.

[0004] However, for the uniform coating and surface modification of powder materials, the existing chemical vapor deposition (CVD), physical vapor deposition (PVD), spraying technology, etc. are difficult to achieve uniform coating of powder materials and precise atomic-level control of their thickness and composition, which greatly limits the optimization of their performance such as catalyst and battery material modification. Based on the unique technical characteristics of self-limiting surface molecular reactions, atomic layer deposition (ALD) technology provides a powder material modification solution that takes into account uniformity, conformality and atomic precision, providing a new technical approach for the optimal optimization of material properties. With the increasing demand for high-performance composite materials, the research and development of large-scale powder ALD equipment and technology is particularly important.

[0005] In order to solve the above technical problems, a new type of atomic layer deposition equipment is urgently needed. Summary of the invention

[0006] In order to solve the problem of large-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 comprises 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, 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; Control system for automation of the entire atomic layer deposition process; including: A first buffer chamber connected to the first reaction chamber is used 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 is used to preheat the powder falling into the second reaction chamber.

[0008] In an optional embodiment, 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 is vibrated and dispersed and falls through the vibrating screen, and is lifted again by the powder vertical lifting device, repeating a reciprocating cycle.

[0009] In an optional embodiment, a gas online analysis system is further included, 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.

[0010] In an optional embodiment, the first buffer chamber includes a material storage chamber, a material inlet vacuum valve is provided at the material inlet of the material storage chamber, a material outlet vacuum valve is provided 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 provided on the material storage chamber for vacuumizing 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 gate valve of the first buffer chamber is opened.

[0011] 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 vacuuming 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.

[0012] In an optional embodiment, 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, so as to decompose them into safe gases that can be directly used for exhaust gas recovery. In an optional embodiment, the vibrating screen is provided with at least two layers.

[0013] In an optional embodiment, the vibrating screen is elastically connected to the first reaction chamber and the second reaction chamber respectively.

[0014] In an optional embodiment, 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.

[0015] In an optional embodiment, it further 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.

[0016] In an optional embodiment, a second material lifting conveyor belt is further included, and the second material lifting conveyor belt is used to load the powder after the reaction in the first reaction chamber into the second buffer chamber.

[0017] In an optional embodiment, it further comprises 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 thin film growth.

[0018] Compared with the prior art, the atomic layer deposition equipment of the present invention provides a first reaction chamber and a second reaction chamber and a buffer chamber respectively connected to the first reaction chamber and the second reaction chamber, so that the powder is preheated in the pre-storage chamber before entering the reaction chamber, and the powder reacts with different precursors in different reaction chambers, thereby improving the preparation efficiency of macro-scale powder atomic layer deposition. The above-mentioned 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

[0019] The invention will be described in more detail below based on non-limiting examples and with reference to the accompanying drawings, in which: Figure 1 A schematic structural diagram of a high-throughput continuous powder atomic layer deposition device according to the present invention is shown; Figure 2 Shows Figure 1 A schematic diagram of the structure of the buffer chamber of the deposition device; Figure 3 Shows Figure 1 A schematic structural diagram of a first reaction chamber of a deposition device; Figure 4 A schematic structural diagram of a high-throughput continuous powder atomic layer deposition device according to another embodiment of the present invention is shown.

[0020] In the figures, the same components are indicated by the same reference numerals. The figures are not drawn to scale.

[0021] Wherein, the accompanying drawings are marked as follows: 1. Automatic powder feeding system; 2. First material lifting conveyor belt; 3. First buffer chamber; 31. Feed inlet vacuum valve; 32. Storage chamber; 33. Discharge outlet vacuum valve; 34. Pressure gauge; 35. Vacuum pump; 4. First reaction chamber; 41. Shell; 42. Reaction chamber; 43. Discharge vacuum valve; 45, 48. Vibrating screen; 46. Elastic connection; 47. Jet nozzle; 49. Powder vertical lifting device; 410. Vacuum gauge; 411. Pneumatic valve; 5. Second material lifting conveyor belt; 6. Second buffer chamber; 7. Second reaction chamber; 8. Vibrating receiver; 9. Control system; 10. Precursor and carrier gas system; 11. Pumping system; 12. Exhaust gas heat treatment system; 13. Gas online analysis system. DETAILED DESCRIPTION

[0022] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments. It should be noted that, as long as there is no conflict, the various embodiments of the present invention and the various features in the embodiments can be combined with each other, and the technical solutions formed are all within the protection scope of the present invention.

[0023] Parts not described in the present invention can be implemented by adopting or drawing on existing technologies.

[0024] like Figure 1 As shown, 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, wherein: The first reaction chamber 4 is used for the powder to react with the first precursor to produce a thin film; The second reaction chamber 7 is used for the powder reacted in the first reaction chamber 4 to undergo a surface chemical reaction with the second precursor to complete the growth of the desired thin film; The pumping system 11 is used to evacuate the first reaction chamber 4 and the second reaction chamber 7, or to adjust the pressure in the first reaction chamber 4 and the second reaction chamber 7 by evacuating the first reaction chamber 4 and the second reaction chamber 7, or to extract the unabsorbed or unreacted precursors and / or reaction by-products in the first reaction chamber 4 and the second reaction chamber 7; wherein, it also includes The first buffer chamber 3 is connected to the first reaction chamber 4 to preheat the powder falling into the first reaction chamber 4; and the second buffer chamber 6 is connected to the first reaction chamber 4 and the second reaction chamber 7 respectively to preheat the powder falling into the second reaction chamber 7.

[0025] The atomic layer deposition equipment of the present invention is provided with a first reaction chamber and a second reaction chamber. The reactions of powder and different precursors are respectively carried out in different reaction chambers, thereby improving the preparation efficiency of powder films. Meanwhile, the equipment is provided with a buffer chamber, and the powder is preheated in the buffer chamber before entering the reaction chamber, thereby further improving the preparation efficiency of powder films and realizing macro-scale film preparation processing.

[0026] In an optional embodiment, a powder vertical lifting device 49 and a vibrating screen 48 coaxially arranged with the reaction chambers are respectively provided in the first reaction chamber 4 and the second reaction chamber 7, wherein the powder is lifted by the powder vertical lifting device 49, undergoes 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, repeating the cycle.

[0027] Optionally, the powder vertical lifting device 49 can be a lifting screw or the like.

[0028] like Figure 1 and Figure 3 As shown, taking the first reaction chamber 4 as an example, the first reaction chamber 4 includes a shell 41, and a powder vertical lifting device 49 and a vibrating screen 45, 48 coaxially arranged with the reaction chamber body 42 are provided in the first reaction chamber 4. When the powder is preheated by the first buffer chamber 3, it falls into the first reaction chamber 4 and 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 falls. When the powder falls to the vibrating screens 45, 48, the vibrating screens 45, 48 vibrate to disperse the powder and let it fall. The fallen powder is lifted again by the powder vertical lifting device 49 to continue to undergo a surface chemical reaction with the first precursor, and the cycle continues, so that all powders are in full contact with the first precursor. In each deposition process, a large amount of powder is evenly coated, effectively improving the powder coating rate and deposition uniformity.

[0029] The vibrating screens 45 and 48 disperse the powders falling thereon by vibration, thereby preventing the powders from agglomerating.

[0030] 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 material with the second precursor after falling into the second reaction chamber 7 are the same as the reaction steps of the powder material with the first precursor after falling into the first reaction chamber 4 , which will not be repeated here.

[0031] After the powder has finished the surface chemical reaction with the first precursor in the first reaction chamber 4, it falls into the second reaction chamber 7 and continues to have the surface chemical reaction with the second precursor to complete the growth of the film.

[0032] Furthermore, the first precursor and the second precursor may be fed into the first reaction chamber 4 and the second reaction chamber 7 respectively through the precursor and carrier gas system 10 .

[0033] In an optional embodiment, the deposition apparatus of the present invention further includes a gas online analysis system 13 , and the gas online analysis system 13 is connected to the first reaction chamber 4 and the second reaction chamber 7 , respectively.

[0034] Optionally, the gas online analysis system 13 may be composed of a residual gas analyzer and a vacuum differential chamber, and the vacuum degree of the gas online analysis system 13 is in the range of 5E-6 mbar.

[0035] By setting up the gas online analysis system 13, the content of the reaction by-products in the reaction chamber can be monitored online in real time, and whether the reaction has been completed can be determined in real time.

[0036] Optionally, the gas online analysis system 13 is disposed between the pumping system 11 and the first reaction chamber 4 / the second reaction chamber 7 .

[0037] In an optional embodiment, the first buffer chamber 3 includes a material storage chamber 32, a material inlet vacuum valve 31 is arranged at the material inlet of the material storage chamber 32, a material outlet vacuum valve 33 is arranged between the material outlet of the material storage chamber 32 and the material inlet of the first reaction chamber 4, and a vacuum pump 35 and a pressure gauge 34 are arranged on the material storage chamber 32, which are used to perform a vacuum operation on the material storage chamber 32 of the first buffer chamber 3; wherein, the first buffer chamber 3 is arranged above the first reaction chamber 4, and when the vacuum degree of the first buffer chamber 3 is the same as the vacuum degree of the first reaction chamber 4, the material outlet vacuum valve 33 of the first buffer chamber 3 is opened.

[0038] When all the powder materials enter the 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. At the same time, the storage chamber 32 is evacuated by a vacuum pump 35. When the vacuum degree of the storage chamber 32 is the same or substantially the same as the vacuum degree 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.

[0039] Preferably, the first cache cavity 3 has a self-heating function, the heating temperature is 180-200°C, and the maximum heating temperature can be 200°C.

[0040] The structure of the second buffer chamber 6 is the same as that of the first buffer chamber 3, and it also includes a material storage chamber. A feed inlet vacuum valve is arranged at the feed inlet of the material storage chamber, and a discharge port vacuum valve is arranged between the discharge port of the material storage chamber and the feed inlet of the second reaction chamber. A vacuum pump and a pressure gauge are arranged on the material storage chamber to vacuum the material storage chamber of the second buffer chamber. When the vacuum degree of the second buffer chamber is the same as the vacuum degree of the second reaction chamber, the discharge port vacuum valve of the second buffer chamber is opened.

[0041] Similarly, the second buffer chamber also has a self-heating function, with a heating temperature of 180-200°C, and a maximum heating temperature of 200°C. The self-heating of the second buffer chamber starts at the beginning of the equipment and keeps warm until the reaction is completed.

[0042] Furthermore, the self-heating functions of the first cache cavity 3 and the second cache cavity 6 are controlled by the control system 9 .

[0043] In an optional embodiment, the apparatus of the present invention further includes an exhaust gas heat treatment system 12 connected to the first reaction chamber 4 and the second reaction chamber 7, respectively. The exhaust gas heat treatment system 12 is disposed in front of the pumping system 11, and is used for performing 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 11.

[0044] The incompletely reacted precursor and / or reaction by-products are subjected to high-temperature decomposition by the tail gas heat treatment system 12, and the tail gas is recovered by the tail gas recovery system after reaching the tail gas recovery standard to prevent environmental pollution. In an optional embodiment, the vibrating screen is provided with at least two layers. Figure 3 As shown, the vibrating screen includes a vibrating screen 45 located at the upper layer and a vibrating screen 48 located at the lower layer. The powder is dispersed by the vibration of the two vibrating screens to prevent the powder from agglomerating.

[0045] Furthermore, the vibrating screens 45 and 48 are elastically connected to the first reaction chamber 4 and the second reaction chamber 7 respectively.

[0046] Taking the first reaction chamber 4 as an example, the first reaction chamber 4 is a vacuum sealed chamber, and therefore, the stability of the installation needs to be maintained. The first reaction chamber 4 and the second reaction chamber 7 are provided with a chamber branch pipe flange, and the oscillator is installed on the chamber branch pipe flange through an elastic structure. The vibration screens 45 and 48 are connected to the oscillator in the first reaction chamber 4 through an elastic connection 46. When the vibration screens 45 and 48 break up 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 vibration screen, thereby ensuring the stability of the first reaction chamber 4 and thus ensuring the vacuum sealing of the first reaction chamber 4.

[0047] Similarly, the vibration screen in the second reaction chamber 7 is connected to the oscillator in the second reaction chamber 7 through an elastic connection, so as to prevent the second reaction chamber 7 from vibrating due to the vibration of the vibration screen, thereby ensuring the vacuum sealing of the second reaction chamber 7.

[0048] Furthermore, an air jet 47 is installed on the side wall of the cavity branch pipe near the elastic connection 46 to prevent powder from entering the vibrator fixed together with the elastic connection 46 .

[0049] In one embodiment, the pumping system further includes a pneumatic valve 411 for opening or blocking the vacuum pumping of the first reaction chamber 4 and the second reaction chamber 7 by the pumping system 11 .

[0050] In one embodiment, the device of the present invention also includes a first material lifting conveyor belt 2, wherein the first material lifting conveyor belt 2 is connected to the discharge port of the automatic powder feeding system 1 and the feed port of the first buffer chamber 3, and is used to feed the powder from the automatic powder feeding system 1 to the first buffer chamber 3.

[0051] Optionally, the device of the present invention may further include a second material lifting conveyor belt 5, which connects the discharge port of the first reaction chamber 4 and the feed port of the second buffer chamber 6, and is used to load the powder after reaction in the first reaction chamber 4 into the second buffer chamber 6.

[0052] Alternative, such as Figure 4 As 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 material lifting conveyor belt 5.

[0053] When the powder enters the second buffer chamber 6, the second batch of powder can continue to pass through the automatic powder feeding system 1, enter the first buffer chamber 3 through the first material lifting conveyor belt 2, and start a new round of film growth, thereby realizing a high-throughput powder continuous film growth process.

[0054] In one embodiment, the device of the present invention further comprises a vibrating material receiver 8, which is disposed below the second reaction chamber 7 and is used to collect powder materials that have completed thin film growth.

[0055] Furthermore, a discharge vacuum valve 43 is provided 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 feeding conveyor belt 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 collector 8 to collect the powder that has completed the film growth.

[0056] 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 the control of the material lifting motor of the device, the opening and closing control of all pneumatic valves, the control of all heating points of the device, the control of the vibration screen, the flow control of the precursor and gas, the extraction and reading of the vacuum degree of each cavity, and the interlocking control of the vacuum degree and the process flow, the automatic reading and data analysis of the gas online analysis system, and the control of the tail gas heat treatment system. The entire process of the device of the present invention is fully automated, without the need for manual intervention, saving manpower and material resources, and improving the deposition efficiency of the atomic layer, so that the powder film preparation processing volume can be achieved.

[0057] Below is a Figure 1 Taking the device shown in the figure as an example, the working process of the atomic layer deposition device of the present invention is described: The bagged powder is manually placed into the automatic powder feeding system 1, and the powder flows into the first material 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 through the first material 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 feed port vacuum valve 31 is closed, and the discharge port vacuum valve 33 is always 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 nearly consistent with the vacuum degree of the first reaction chamber 4, the control system 9 controls the opening of the discharge port vacuum valve 33. After the powder enters the first reaction chamber 4 under the action of gravity, the discharge port vacuum valve 33 is closed.

[0058] At this time, the first reaction chamber 4 has been heated in advance by the control system 9, and the highest temperature can be heated to 350°C, and the required vacuum degree has been reached 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 with the vacuum valve 33 of the discharge port of the first cache chamber 3.

[0059] The powder undergoes a surface chemical reaction with the first precursor in the first reaction chamber 4 (the first precursor enters the first reaction chamber 4 through the precursor and carrier gas path system 10 after the control system 9 gives an instruction). The powder falls to the vibrating screens 45 and 48, and the vibrating screens vibrate and disperse the powder. After the powder falls through the double-layer vibrating screens 45 and 48, it is lifted again by the powder vertical lifting device 49, and the cycle continues. At the same time, the gas online analysis system 13 monitors the content of the reaction by-products in real time online, and can determine in real time whether the reaction has been completed.

[0060] The unreacted precursor and reaction by-products in the first reaction chamber 4 are pumped by the pumping system 11 to the tail gas heat treatment system 12 for high temperature decomposition to meet the tail gas recovery standard, and then pumped to the tail gas recovery device.

[0061] After the powder material completes the chemical reaction with the first precursor in the first reaction chamber 4, the control system 9 controls the discharge vacuum valve 43 below the first reaction chamber 4 to open, and enters the second buffer chamber 6 via the second material lifting conveyor belt 5, closes the feed inlet vacuum valve and the discharge outlet vacuum valve of the second buffer chamber 6, and performs vacuum pumping in the storage chamber of the second buffer chamber 6 through a vacuum pump. The unreacted precursor and side reaction products in the powder material brought out in the first reaction chamber 4 are pumped into the tail gas heat treatment system 12 for high temperature decomposition, decomposed into safe gas that can be directly used for tail gas recovery, and discharged to the tail gas recovery equipment.

[0062] The powder continues to enter the second reaction chamber 7 from the second buffer chamber 6, repeats the same steps as the first reaction chamber 4, reacts with the second precursor, and completes the growth of the desired film. Then the control system 9 controls the discharge vacuum valve below the second reaction chamber 7 to open, and the powder enters the vibrating receiver 8 to complete the entire process.

[0063] When the powder enters the second buffer chamber 6, the second batch of powder can continue to pass through the automatic powder feeding system 1, enter the first buffer chamber 3 through the first material lifting conveyor belt 2, and start a new round of film growth, realizing a high-throughput powder continuous film growth process.

[0064] 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, further reaction chambers may be added to implement this process flow.

[0065] Unless otherwise defined, the technical terms or scientific terms used in the present invention shall have the usual meanings understood by persons with ordinary skills in the field to which the present invention belongs. The terms "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words 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 position relationship indicated by the term "vertical" and the like is based on the orientation or position relationship shown in the accompanying drawings, which 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 described object changes, the relative position relationship may also change accordingly, so it cannot be understood as a limitation of the present invention.

[0066] At this point, it should be appreciated by those skilled in the art that, although the present invention has been described with reference to preferred embodiments, various modifications may be made thereto and parts thereof may be replaced with equivalents without departing from the scope of the present invention. In particular, the various technical features mentioned in the various embodiments may be combined in any manner as long as there is no structural conflict. 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 is used 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 is used to preheat the powder falling into the second reaction chamber.

2. The high-throughput continuous powder atomic layer deposition device according to claim 1, characterized in that: 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.

3. The high-throughput continuous powder atomic layer deposition device according to claim 2, 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.

4. The high-throughput continuous powder atomic layer deposition device according to claim 3, 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.

5. The high-throughput continuous powder atomic layer deposition device according to claim 4, 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.

6. The high-throughput continuous powder atomic layer deposition device according to claim 2, characterized in that: The vibrating screen is provided with at least two layers.

7. The high-throughput continuous powder atomic layer deposition device according to claim 6, characterized in that: The vibration screen is elastically connected to the first reaction chamber and the second reaction chamber respectively.

8. 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.

9. The high-throughput continuous powder atomic layer deposition device according to claim 5, 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.

10. The high-throughput continuous powder atomic layer deposition device according to claim 9, 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.

11. The high-throughput continuous powder atomic layer deposition device according to claim 9 or 10, 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

  • Atomic layer deposition method and atomic layer deposition device for coating ultrafine powder

    CN103451623A

  • Nano particle continuous-coating device and method based on spatial atomic layer deposition

    CN107254675A

  • Continuous atomic layer deposition equipment used for nano-particle surface wrapping

    CN108220917A

  • Thin film deposition method and device

    CN111286721A

  • Thin film deposition method and equipment

    CN117144339A