Atomic layer deposition reaction residue treatment device

Abstract

The embodiment of the utility model discloses a reaction residue treatment device for atomic layer deposition, which relates to the technical field of micro-nano manufacturing, and is characterized in that a metal source and a hydrogen sulfide source are connected with a reaction cavity, and a PT (potential transformer) pressure gauge is mounted on the reaction cavity; the output of the reaction cavity is processed through a multi-line system, and each processing line is connected with the reaction cavity through a gas conveying pipe. According to the scheme, green recovery treatment is carried out on reaction residues of atomic layer deposition through double treatment lines, environmental pollution is avoided, meanwhile, energy is recycled, the purpose of saving energy is achieved, the implementation mode of the treatment lines is relatively simple, and large-scale and industrial production application is also facilitated.

Description

Technical Field

[0001] The utility model relates to the technical field of micro-nano manufacturing, in particular to a device for processing reaction residues of atomic layer deposition. Background Art

[0002] In recent years, the application of atomic layer deposition of metal sulfides has received widespread attention and research. However, since the atomic layer deposition process is a process of continuous reaction, there will be residual reactants and residues after the reaction that need to be discharged. The reaction residues of atomic layer deposition of metal sulfides are composed of toxic hydrogen sulfide, hydrochloric acid that is easy to corrode pipelines, expensive metal halides, carrier gas and other components. If these substances are not treated and directly discharged into the atmosphere, on the one hand, it will seriously pollute the environment. On the other hand, since these reaction residues are expensive, direct discharge will cause a waste of resources. Therefore, the existing atomic layer deposition metal sulfide process technology is mainly suitable for laboratory preparation. In terms of large-scale, industrial production applications, the problem of tail gas residue treatment needs to be solved. Utility Model Content

[0003] The embodiment of the utility model provides a device for treating reaction residues of atomic layer deposition, which can solve the problem of treating tail gas residues.

[0004] In order to achieve the above-mentioned purpose, the embodiment of the utility model adopts the following technical scheme:

[0005] A device for processing reaction residues of atomic layer deposition, the components of the device comprising: a metal source (24) connected to a reaction chamber (2) via a pneumatic valve V1 (23), a hydrogen sulfide source (21) connected to the reaction chamber (2) via a pneumatic valve V2 (20), and a PT pressure gauge (1) installed on the reaction chamber (2);

[0006] The output of the reaction chamber (2) is processed through a dual-line system, wherein the gas transmission line of the dual-line system is composed of a processing line I and a processing line II, and the processing line I and the processing line II are each connected to the reaction chamber (2) through a gas transmission pipe;

[0007] The dual-line system includes at least two modes. In the first mode of the dual-line system, the series connection sequence of the devices in the processing line I is: condensation absorption device, dissolution absorption device, drying device and gas storage device; the series connection sequence of the devices in the processing line II is: dissolution absorption device, drying device and gas storage device;

[0008] In the second mode of the dual-circuit system, two condensation absorption devices are connected in series in treatment line I; the series connection order of the devices in treatment line II is: combustion chamber, oxidation absorption device and solution absorption device.

[0009] In the first mode, it also includes: pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4), pneumatic valve V8 (18), a first condensation absorption device (7), a dissolution absorption device I (10), a dissolution absorption device II (9), a heating device (8), a drying device I (11), a drying device II (12), a first vacuum pump (13), an air storage device I (15), an air storage device II (17), a pressure reducing valve V11 (3) and a pressure reducing valve V22 (19); wherein the pneumatic valve V3 (5), the first condensation absorption device (7), the dissolution absorption device I (10), the drying device I (11), the drying device II (12), the first vacuum pump (13), the air storage device I (15), the air storage device II (17), the pressure reducing valve V11 (3) and the pressure reducing valve V22 (19); The drying device I (11), the first vacuum pump (13), the pneumatic valve V5 (14), the gas storage device I (15), the pneumatic valve V7 (4), and the pressure reducing valve V11 (3) are connected in sequence through a gas pipeline to form a processing line I; the pneumatic valve V4 (6), the dissolving and absorbing device II (9), the drying device II (12), the first vacuum pump (13), the pneumatic valve V6 (16), the gas storage device II (17), the pneumatic valve V8 (18), and the pressure reducing valve V22 (19) are connected in sequence through a gas pipeline to form a processing line II; the pneumatic valve V3 (5) of the processing line I and the pneumatic valve V4 (6) of the processing line II are both connected to the reaction chamber (2) through a gas pipeline. Optionally, a flow controller 1 (22) can be optionally provided at the hydrogen sulfide source (21), and a flow controller 2 (25) can be optionally provided at the metal source (24). In the second mode, it also includes: a combustion chamber (26), a pneumatic valve V10 (27), a second condensation absorption device 1 (28), a third condensation absorption device 2 (29), a pneumatic valve V9 (30), a second vacuum pump (31), a pneumatic valve V13 (32), a solution absorption device III (33), an oxidation absorption device (34), a pneumatic valve V12 (35) and a pneumatic valve V11 (36);

[0010] Among them, the pneumatic valve V3 (5), the second condensation absorption device 1 (28), the third condensation absorption device 2 (29) and the pneumatic valve V9 (30) are connected in sequence through a gas pipeline to form a processing line I; the pneumatic valve V10 (27), the combustion chamber (26), the pneumatic valve V12 (35), the oxidation absorption device (34), the solution absorption device (33) and the pneumatic valve V13 (32) are connected in sequence through a gas pipeline to form a processing line II, wherein a pneumatic valve V11 (36) is also installed at the air inlet of the combustion chamber (26); the pneumatic valve V9 (30) of the processing line I and the pneumatic valve V13 (32) of the processing line II are both connected to the second vacuum pump (31) through the gas pipeline, and the second vacuum pump (31) is used to discharge gas.

[0011] Specifically, a neutralization reaction solution is built into the dissolution absorption device I (10), and the neutralization reaction solution is used to react with hydrochloric acid HCl for neutralization; a desiccant is built into the drying device I (11), and the desiccant is used to remove water vapor introduced from the dissolution absorption device I (10); the reaction solution built into the dissolution absorption device I (10) is a sodium hydroxide NaOH solution or a potassium hydroxide KOH solution; the desiccant is soda lime or silica gel; the pressure reducing valve V11 (3) is used to reduce the pressure of the carrier gas of the gas storage device I (15) and pass it into the metal source path; the pressure reducing valve V22 (19) is used to reduce the pressure of the hydrogen sulfide and the carrier gas of the gas storage device II (17), and pass them into the hydrogen sulfide source path.

[0012] In the dissolution absorption device II (9), a neutralization reaction solution is built in, and the neutralization reaction solution is used to react with hydrochloric acid HCl for neutralization reaction; a heating device (8) is installed outside the dissolution absorption device II (9); and a desiccant is built in the drying device II (12). The reaction solution built in the dissolution absorption device II (9) is a sodium disulfide NaS2 solution or a sodium hydrosulfide NaHS solution.

[0013] Pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4) and pneumatic valve V8 (18) are all connected to electromagnetic reversing valves, and the electromagnetic reversing valves are connected to a programmable logic controller PLC. Pneumatic valve V11 (36), pneumatic valve V10 (27), pneumatic valve V9 (30), pneumatic valve V13 (32) and pneumatic valve V12 (35) are all connected to electromagnetic reversing valves, and the electromagnetic reversing valves are connected to a programmable logic controller PLC. The reaction solution built into the solution absorption device (33) uses dilute sulfuric acid; the oxidation absorption device (34) uses vanadium pentoxide V205.

[0014] The atomic layer deposition reaction residue processing device provided by the embodiment of the utility model is for the atomic layer deposition reaction residue, which is greenly recycled through processing lines I and II. On the one hand, it avoids environmental pollution and recycles energy to achieve energy saving. On the other hand, due to the repeated use of expensive niobium chloride sources, waste is avoided and the cost of atomic layer deposition metal sulfide is greatly reduced. The implementation method of the two sets of processing lines is relatively simple, which is also convenient for large-scale and industrial production applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0016] Figure 1 A schematic diagram of the overall structure of the device provided by the embodiment of the utility model;

[0017] Figure 2 A schematic diagram of a specific structure of a first possible implementation of the device provided in an embodiment of the utility model;

[0018] Figure 3 A detailed schematic diagram of a first possible implementation method provided for an embodiment of the utility model;

[0019] Figure 4 A schematic diagram of a specific structure of a second possible implementation of the device provided in an embodiment of the utility model;

[0020] Figure 5 A detailed schematic diagram of a second possible implementation method provided for an embodiment of the utility model;

[0021] The symbols in the above drawings respectively represent: 1. PT pressure gauge; 2. reaction chamber; 3. pressure reducing valve V11; 4. pneumatic valve V7; 5. pneumatic valve V3; 6. pneumatic valve V4; 7. first condensation absorption device; 8. heating device; 9. dissolution absorption device II; 10. dissolution absorption device I; 11. drying device I; 12. drying device II; 13. first vacuum pump; 14. pneumatic valve V5; 15. gas storage device I; 16. pneumatic valve V6; 17. gas storage device II; 18. pneumatic valve V8; 1 9. Pressure reducing valve V22; 20. Pneumatic valve V2; 21. Hydrogen sulfide source; 22. Flow control meter 1; 23. Pneumatic valve V1; 24. Metal source; 25. Flow control meter 2; 26. Combustion chamber; 27. Pneumatic valve V10; 28. Second condensation absorption device 1; 29. ​​Third condensation absorption device 2; 30. Pneumatic valve V9; 31. Second vacuum pump; 32. Pneumatic valve V13; 33. Solution absorption device; 34. Oxidation absorption device; 35. Pneumatic valve V12; 36. Pneumatic valve V11;

[0022] Figure 6 , 7 A detailed schematic diagram of an implementation method of integrating two possible solutions provided in an embodiment of the utility model;

[0023] It should be noted that, in order to facilitate the distinction from the aforementioned reference numerals, Figure 7The relevant components and numerical labels are distinguished in the following ways: the attributive “second category” is added before the names of the relevant components in the “integrated solution”, such as “second category PT pressure gauge”, “second category reaction chamber”, “second category condensation absorption device III”, but the functions and models of these components can be the same as those in the aforementioned solutions, and they are only distinguished in terms of the names; the capital letter “A” is added before the numerical labels, such as “second category PT pressure gauge (A1)”, “second category reaction chamber (A2)”, “second category condensation absorption device III (A18)”;

[0024] Figure 7 The marks in the figure represent respectively: A1. Second type PT pressure gauge; A2. Second type reaction chamber; A3. Second type combustion chamber; A4. Second type pneumatic valve V13; A5. Second type pneumatic valve V12; A6. Second type oxidation absorption device; A7. Second type heating device Ⅰ; A8. Second type solution absorption device Ⅲ; A9. Second type pneumatic valve V11; A10. Second type pneumatic valve V9; A11. Second type pneumatic valve V3; A12. Second type pneumatic valve V6; A13. Second type condensation absorption device Ⅱ; A14. Second type condensation absorption device Ⅰ; A15. Second type heating device Ⅱ; A16. Second type solution absorption device Ⅱ; A17. Second type solution absorption device Ⅰ; A18. Second type condensation absorption device Ⅲ; A19. A20. A21. A2 ... DETAILED DESCRIPTION

[0025] In order to enable those skilled in the art to better understand the technical solution of the utility model, the utility model is further described in detail below in conjunction with the accompanying drawings and specific embodiments. The embodiments of the utility model will be described in detail below, and examples of the embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements with the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the utility model, and cannot be interpreted as limiting the utility model. It can be understood by those skilled in the art that, unless specifically stated, the singular forms "one", "one", "said" and "the" used here may also include plural forms. It should be further understood that the wording "including" used in the specification of the utility model refers to the presence of the features, integers, steps, operations, elements and / or components, but does not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or their groups. It should be understood that when we say that an element is "connected" or "coupled" to another element, it can be directly connected or coupled to other elements, or there may also be intermediate elements. In addition, the "connection" or "coupling" used here may include wireless connection or coupling. The wording "and / or" used herein includes any unit and all combinations of one or more associated listed items. It can be understood by those skilled in the art that, unless otherwise defined, all terms (including technical terms and scientific terms) used herein have the same meaning as the general understanding of ordinary technicians in the field to which the utility model belongs. It should also be understood that those terms such as those defined in general dictionaries should be understood to have a meaning consistent with the meaning in the context of the prior art, and will not be interpreted with an idealized or overly formal meaning unless defined as here.

[0026] The present invention provides an atomic layer deposition reaction residue processing device, the components of which include: a metal source (24) connected to a reaction chamber (2) via a pneumatic valve V1 (23), a hydrogen sulfide source (21) connected to the reaction chamber (2) via a pneumatic valve V2 (20), and a PT pressure gauge (1) installed on the reaction chamber (2);

[0027] The output of the reaction chamber (2) is processed through a dual-line system, wherein the gas transmission line of the dual-line system is composed of a processing line I and a processing line II, and the processing line I and the processing line II are each connected to the reaction chamber (2) through a gas transmission pipe;

[0028] The dual-line system includes at least two modes. In the first mode of the dual-line system, the series connection sequence of the devices in the processing line I is: condensation absorption device, dissolution absorption device, drying device and gas storage device; the series connection sequence of the devices in the processing line II is: dissolution absorption device, drying device and gas storage device;

[0029] In the second mode of the dual-circuit system, two condensation absorption devices are connected in series in treatment line I; the series connection order of the devices in treatment line II is: combustion chamber, oxidation absorption device and solution absorption device.

[0030] In the first mode, if Figure 1 , 2 As shown, it includes: pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4), pneumatic valve V8 (18), a first condensation absorption device (7), a dissolution absorption device I (10), a dissolution absorption device II (9), a heating device (8), a drying device I (11), a drying device II (12), a first vacuum pump (13), an air storage device I (15), an air storage device II (17), a pressure reducing valve V11 (3), and a pressure reducing valve V22 (19).

[0031] The pneumatic valve V3 (5), the first condensation absorption device (7), the dissolution absorption device I (10), the drying device I (11), the first vacuum pump (13), the pneumatic valve V5 (14), the gas storage device I (15), the pneumatic valve V7 (4), and the pressure reducing valve V11 (3) are connected in sequence to form a processing line I for recovering and treating the metal source reaction residues of atomic layer deposition metal sulfides, including metal halide, hydrochloric acid HCl, and carrier gas (inert gas such as nitrogen N2, argon Ar, etc.). The pneumatic valve V4 (6), the dissolution absorption device II (9), the drying device II (12), the first vacuum pump (13), the pneumatic valve V6 (16), the gas storage device II (17), the pneumatic valve V8 (18), and the pressure reducing valve V22 (19) are connected in sequence to form a processing line II for recovering and treating the hydrogen sulfide source reaction residues of atomic layer deposition metal sulfides, including hydrogen sulfide, hydrochloric acid, and carrier gas (inert gas such as nitrogen N2, argon Ar, etc.).

[0032] The first condensation absorption device (7) has a settable condensation temperature and is used to condense and recover precious metal halides, which can be reused in subsequent atomic layer deposition processes, thereby saving costs.

[0033] The dissolving and absorbing device I (10) is equipped with a solution capable of neutralizing and absorbing hydrochloric acid HCl. The specific composition of the solution is not required, as long as it can react with the hydrochloric acid HCl to neutralize and absorb the alkaline solution of the hydrochloric acid HCl. Preferably, NaOH or KOH solution is used.

[0034] The drying device I (11) is used to dry the carrier gas in the metal source reaction residue and remove the water vapor introduced in the dissolution absorption device I (10). The drying device I (11) is equipped with a desiccant. The specific composition of the desiccant is not required, as long as it can dry and remove the water vapor in the carrier gas. Preferably, soda lime and silica gel are used.

[0035] The first vacuum pump (13) is used to maintain the vacuum degree in the system and ensure the flow of carrier gas and source material.

[0036] The gas storage device I (15) is used to store the dried carrier gas, saving costs and can be reused in subsequent atomic layer deposition processes.

[0037] The pressure reducing valve V11 (3) reduces the pressure of the carrier gas in the gas storage device I (15) according to the pressure of the metal source path during the atomic layer deposition process, and passes the carrier gas into the metal source path for repeated use.

[0038] The dissolving and absorbing device II (9) is equipped with a solution capable of neutralizing and absorbing hydrochloric acid HCl, and is used to filter and absorb the hydrochloric acid HCl in the hydrogen sulfide source reaction residue. The specific composition of the solution is not required, and it is mainly capable of absorbing the hydrochloric acid HCl and ensuring that hydrogen sulfide passes smoothly. Preferably, NaS2 and NaHS solutions are used. The dissolving and absorbing device II (9) is equipped with an external heating device (8), and the heating temperature can be set to ensure that the NaS2 and NaHS solutions react with the hydrochloric acid HCl to generate hydrogen sulfide.

[0039] The drying device II (12) has a built-in desiccant for drying hydrogen sulfide and carrier gas in the hydrogen sulfide source reaction residue. The specific composition of the desiccant is not required, as long as it can dry and remove water vapor in hydrogen sulfide and carrier gas. Preferably, phosphorus pentoxide P2O5 is used.

[0040] The gas storage device II (17) is used to store the dried hydrogen sulfide and carrier gas, which saves costs and can be reused in the subsequent atomic layer deposition process.

[0041] The pressure reducing valve V22 (19) reduces the pressure of the hydrogen sulfide and carrier gas in the gas storage device II (17) according to the pressure of the hydrogen sulfide source path during the atomic layer deposition process, and passes them into the hydrogen sulfide source path for repeated use.

[0042] Among them, Figure 3 As shown, the pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4), and pneumatic valve V8 (18) are controlled by a computer, a PLC, and an electromagnetic reversing valve, and are opened and closed according to the process sequence in the atomic layer deposition process to ensure that the metal source reaction residues of the atomic layer deposition metal sulfide can enter the processing line I for recovery treatment, and the hydrogen sulfide source reaction residues can enter the processing line II for recovery treatment.

[0043] Optionally, in the second mode, it also includes: a combustion chamber (26), a pneumatic valve V10 (27), a second condensation absorption device 1 (28), a third condensation absorption device 2 (29), a pneumatic valve V9 (30), a second vacuum pump (31), a pneumatic valve V13 (32), a solution absorption device (33), an oxidation absorption device (34), a pneumatic valve V12 (35) and a pneumatic valve V11 (36);

[0044] Among them, the pneumatic valve V3 (5), the second condensation absorption device 1 (28), the third condensation absorption device 2 (29) and the pneumatic valve V9 (30) are connected in sequence through the gas transmission pipe to form a processing line I;

[0045] The pneumatic valve V10 (27), the combustion chamber (26), the pneumatic valve V12 (35), the oxidation absorption device (34), the solution absorption device (33) and the pneumatic valve V13 (32) are connected in sequence through a gas pipeline to form a processing line II, wherein a pneumatic valve V11 (36) is also installed at the air inlet of the combustion chamber (26);

[0046] The pneumatic valve V9 (30) of the processing line I and the pneumatic valve V13 (32) of the processing line II are both connected to the second vacuum pump (31) through the gas transmission pipe, and the second vacuum pump (31) is used to exhaust gas.

[0047] The second mode can be used for green treatment of the reaction residues of atomic layer deposition metal sulfide NbS2. The carrier gas is nitrogen, the metal source is niobium chloride, and the sulfur source is hydrogen sulfide. The reaction residues are niobium chloride, hydrochloric acid HCL, hydrogen sulfide, and nitrogen. Figure 4 The operation process can be seen:

[0048] During the atomic layer deposition of NbS2, the pneumatic valve V1 (23) is opened, the pneumatic valve V2 (20) is closed, and the metal source (24) is fed into the reaction chamber (2) using niobium chloride for reaction. After the reaction is completed, under the control of the computer, PLC and electromagnetic reversing valve, the pneumatic valves V3 (5) and V9 (30) are opened, and the pneumatic valves V10 (27), V11 (36), V12 (35) and V13 (32) are closed. The niobium chloride reaction residues, niobium chloride, hydrochloric acid HCl and nitrogen carrier gas, enter the processing line I for recycling.

[0049] Niobium chloride passes through the second condensation absorption device 1 (28) to condense gaseous niobium chloride into solid niobium chloride for recovery and reuse in the subsequent atomic layer deposition process. The condensation temperature is set to 110 degrees Celsius according to the physical properties. Hydrochloric acid HCl passes through the third condensation absorption device 2 (29) to condense hydrochloric acid HCl gas into liquid for recovery and reuse. The condensation temperature is set to 20 degrees Celsius according to the physical properties.

[0050] The filtered nitrogen carrier gas is discharged through the second vacuum pump (31).

[0051] During the atomic layer deposition of NbS2, under the control of the computer, PLC and electromagnetic reversing valve, the pneumatic valves V3 (5), V9 (30), V10 (27), V12 (35) and V13 (32) are closed, and the pneumatic valve V11 (36) is opened. After the air enters the combustion chamber (26), the pneumatic valve V11 (36) is closed to prepare for the treatment of the hydrogen sulfide source reaction residues. The pneumatic valve V1 (23) is closed, the pneumatic valve V2 (20) is opened, and the hydrogen sulfide source (21) is sent into the reaction chamber (2) for reaction. After the reaction is completed, the pneumatic valve V10 (27) is opened, and the hydrogen sulfide source reaction residues, hydrogen sulfide and nitrogen carrier gas, enter the treatment line II for recovery treatment.

[0052] The reaction residue hydrogen sulfide is burned in the combustion chamber (26) to preheat the precursor source of the reaction chamber (2), thereby realizing the recycling of hydrogen sulfide and achieving the purpose of energy saving. After the hydrogen sulfide is fully burned, the pneumatic valve V12 (35) and the pneumatic valve V13 (32) are opened, and the sulfur dioxide SO2 generated by the combustion is oxidized to sulfur trioxide SO3 by vanadium pentoxide V2O5 in the oxidation absorption device (34), and then the sulfur dioxide is adsorbed and recycled by dilute sulfuric acid in the solution absorption device (33), and the remaining harmless gases such as nitrogen are discharged through the second vacuum pump (31).

[0053] Further, such as Figure 5 As shown, the pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4), pneumatic valve V8 (18), pneumatic valve V9 (9), pneumatic valve V10 (6), pneumatic valve V11 (3), pneumatic valve V12 (14), and pneumatic valve V13 (11) are controlled by a computer, a PLC, and an electromagnetic reversing valve, and are opened and closed according to the process sequence in the atomic layer deposition process to ensure that the metal source reaction residues of the atomic layer deposition metal sulfide can enter the processing line I for recovery treatment, and the hydrogen sulfide source reaction residues can enter the processing line II for recovery treatment.

[0054] It should be noted that the computer and PLC used in this embodiment can both be purchased from products currently available on the market, and the control method based on controlling the switch of the electromagnetic reversing valve based on the pressure in the source path is also the most basic reversing valve control method in this field. Therefore, the entire "computer-PLC-electromagnetic reversing valve" control method is a technology that already exists in the prior art and is widely used. The specific control method of the electromagnetic reversing valve will not be repeated in this embodiment.

[0055] Optionally, this embodiment also provides an implementation method that integrates the above two possible solutions. The specific structure is as follows: Figure 6 , 7 As shown, there are two usage modes in actual application, mode 1: running line I and line II; mode 2: running line III and line IV.

[0056] The second type of pneumatic valve V3 (A11), the second type of condensation absorption device Ⅰ (A14), the second type of dissolution absorption device Ⅰ (A17), the second type of drying device Ⅰ (A20), the second type of vacuum pump Ⅱ (A21), the second type of pneumatic valve V4 (A24), the second type of gas storage device Ⅰ (A27), the second type of pneumatic valve V5 (A30), and the second type of pressure reducing valve V11 (A32) are connected in sequence through a gas transmission pipe to form a processing line Ⅰ;

[0057] The second type of pneumatic valve V6 (A12), the second type of dissolving and absorbing device Ⅱ (A15), the second type of drying device Ⅱ (A19), the second type of vacuum pump Ⅱ (A21), the second type of pneumatic valve V7 (A25), the second type of gas storage device Ⅱ (A28), the second type of pneumatic valve V8 (A29), and the second type of pressure reducing valve V22 (A31) are connected in sequence through a gas pipeline to form a processing line Ⅱ; the second type of pneumatic valve V3 (A11) of the processing line Ⅰ and the second type of pneumatic valve V6 (A12) of the processing line Ⅱ are both connected to the reaction chamber (A2) through a gas pipeline.

[0058] The second type of pneumatic valve V9 (A10), the second type of condensation absorption device II (A13), the second type of condensation absorption device III (A18) and the second type of pneumatic valve V10 (A22) are connected in sequence through a gas transmission pipe to form a processing line III;

[0059] The second type of pneumatic valve V11 (A9), the second type of combustion chamber (A3), the second type of pneumatic valve V13 (A4), the second type of oxidation absorption device (A6), the second type of solution absorption device III (A8) and the second type of pneumatic valve V14 (A26) are connected in sequence through a gas pipeline to form a processing line IV, wherein a second type of pneumatic valve V12 (A5) is also installed at the air inlet of the second type of combustion chamber (A3);

[0060] The second type of pneumatic valve V10 (A22) of the processing line III and the second type of pneumatic valve V14 (A26) of the processing line IV are both connected to the second type of vacuum pump I (A23) through the gas pipeline, and the second type of vacuum pump I (A23) is used to exhaust gas.

[0061] Mode 1 Line Ⅰ, Line Ⅱ

[0062] During the atomic layer deposition of NbS2, when the second pneumatic valve V1 (A36) is opened and the second metal source niobium chloride (A37) is fed into the second reaction chamber (A2) for reaction, under the control of the computer, PLC and electromagnetic reversing valve, the second pneumatic valve V3 (A11) and the second pneumatic valve V4 (A24) are opened, and the second pneumatic valve V6 (A12), the second pneumatic valve V7 (A25), the second pneumatic valve V5 (A30), the second pneumatic valve V8 (A29), the second pneumatic valve V9 (A10), the second pneumatic valve V10 (A22), the second pneumatic valve V11 (A9), the second pneumatic valve V12 (A5), the second pneumatic valve V13 (A4) and the second pneumatic valve V14 (A26) are closed, and the niobium chloride reaction residues, niobium chloride, hydrochloric acid HCl and carrier gas, enter the processing line I for recovery treatment.

[0063] Niobium chloride is condensed into solid niobium chloride through the second type condensation absorption device I (A14) to recover the gaseous niobium chloride. It can be reused in the subsequent atomic layer deposition process. The hydrochloric acid HCl is neutralized and absorbed by the NaOH solution in the second type dissolution absorption device I (A17). The remaining carrier gas is dried and filtered by the soda lime in the second type drying device I (A20). The second type condensation absorption device I

[0064] (A14), to ensure that niobium chloride is condensed and hydrochloric acid HCl passes smoothly, according to their physical properties, the condensation temperature is set to 110 degrees Celsius. The carrier gas after drying and filtration passes through the second type vacuum pump II (A21) and is stored in the second type gas storage device I (A27) for recycling.

[0065] During the atomic layer deposition process of NbS2, when the second type of pneumatic valve V1 (A36) is closed, the second type of pneumatic valve V2 (A33) is opened, and the second type of hydrogen sulfide source (A34) is sent into the reaction chamber (A2) for reaction, under the control of the computer, PLC and electromagnetic reversing valve, the second type of pneumatic valve V3 (A11) and the second type of pneumatic valve V4 (A24) are closed, and the second type of pneumatic valve V6 (A12) and the second type of pneumatic valve V7 (A25) are opened, and the second type of hydrogen sulfide source reaction residues, hydrogen sulfide, hydrochloric acid HCl, and carrier gas enter the processing line II for recovery treatment.

[0066] In the second-type hydrogen sulfide source reaction residue, hydrochloric acid HCl reacts with NaS2 and NaHS solutions in the second-type dissolving and absorbing device Ⅱ (A16) under heating in the second-type heating device Ⅱ (A15) (heating temperature is 65 degrees Celsius) to generate hydrogen sulfide, which is filtered and absorbed. The remaining hydrogen sulfide and carrier gas are dried and filtered through phosphorus pentoxide P2O5 in the second-type drying device Ⅱ (A19).

[0067] The dried and filtered hydrogen sulfide and carrier gas are stored in the second type gas storage device II (A28) through the second type vacuum pump II (A21) and can be reused in the subsequent atomic layer deposition process.

[0068] When it is necessary to use the carrier gas in the second-class gas storage device I (A27), open the second-class pneumatic valve V5 (A30), set the output pressure of the second-class pressure reducing valve V11 (A32) according to the pressure of the niobium chloride source during the atomic layer deposition process, and transport the carrier gas in the second-class gas storage device I (A27) to the niobium chloride source for repeated use; when it is necessary to use the hydrogen sulfide and carrier gas in the second-class gas storage device II (A28), set the output pressure of the second-class pressure reducing valve V22 (A31) according to the pressure of the second-class hydrogen sulfide source during the atomic layer deposition process, and transport the hydrogen sulfide and carrier gas in the second-class gas storage device II (A28) to the second-class hydrogen sulfide source for repeated use.

[0069] After the above steps, the reaction residues of the niobium chloride source and the second type of hydrogen sulfide source of atomic layer deposition of NbS2 are respectively recycled through processing lines I and II for green treatment. On the one hand, environmental pollution is avoided. On the other hand, due to the reuse of the expensive niobium chloride source and the second type of hydrogen sulfide source, waste is avoided, which greatly reduces the cost of atomic layer deposition of metal sulfides and can be used for large-scale industrial production and application.

[0070] Mode 2 Line III, Line IV

[0071] During the atomic layer deposition of NbS2, the second pneumatic valve V1 (A36) is opened, the second pneumatic valve V2 (A33) is closed, and the second metal source (A37) (using niobium chloride) is sent into the second reaction chamber (A2) for reaction. After the reaction is completed, under the control of the computer, PLC and electromagnetic reversing valve, the second pneumatic valve V9 (A10) and the second pneumatic valve V10 (A22) are opened, and the second pneumatic valve V3 (A11) and the second pneumatic valve V4 ( The second pneumatic valve V10 (A11), the second pneumatic valve V12 (A12), the second pneumatic valve V13 (A4), and the second pneumatic valve V14 (A26) are closed, and the niobium chloride reaction residues, niobium chloride, hydrochloric acid HCl, and nitrogen carrier gas, enter the processing line III for recovery treatment.

[0072] Niobium chloride is passed through the second type condensation absorption device II (A13) to condense gaseous niobium chloride into solid niobium chloride for recycling. It can be reused in the subsequent atomic layer deposition process. According to the properties of the object, the condensation temperature is set to 110 degrees Celsius. Hydrochloric acid HCl is passed through the second type condensation absorption device III (A18) to condense hydrochloric acid HCl gas into liquid for recycling. According to the physical properties, the condensation temperature is set to 20 degrees Celsius.

[0073] The filtered nitrogen carrier gas is discharged through the second type vacuum pump Ⅰ (A23).

[0074] During the atomic layer deposition of NbS2, under the control of the computer, PLC and electromagnetic reversing valve, the second pneumatic valve V9 (A10), the second pneumatic valve V10 (A22), the second pneumatic valve V11 (A9), the second pneumatic valve V13 (A4), and the second pneumatic valve V14 (A26) are closed, and the second pneumatic valve V12 (A5) is opened. After the air enters the second combustion chamber (A3), the second pneumatic valve V12 (A5) is closed to prepare for the treatment of the second hydrogen sulfide source reaction residue. The second pneumatic valve V1 (A36) is closed, the second pneumatic valve V2 (A33) is opened, and the second hydrogen sulfide source (A34) is sent to the second reaction chamber (A2) for reaction. After the reaction is completed, the second pneumatic valve V11 (A9) is opened, and the second hydrogen sulfide source reaction residues, hydrogen sulfide and nitrogen carrier gas, enter the treatment line IV for recovery treatment.

[0075] The reaction residue hydrogen sulfide is burned in the second combustion chamber (A3) to preheat the precursor source of the second reaction chamber (A2), thereby realizing the recycling of hydrogen sulfide and achieving the purpose of energy saving.

[0076] After the hydrogen sulfide is fully burned, the second type pneumatic valve V13 (A4) and the second type pneumatic valve V14 (A26) are opened, and the sulfur dioxide SO2 generated by the combustion is oxidized to sulfur trioxide SO3 by the vanadium pentoxide V205 in the second type oxidation absorption device (A6), and then the sulfur dioxide is adsorbed and recycled by the dilute sulfuric acid in the second type solution absorption device III (A8), and the remaining nitrogen and other harmless gases are discharged through the second type vacuum pump I (A23).

[0077] After the above steps, the reaction residues of atomic layer deposition of NbS2 are processed through processing lines III and IV for green recycling. On the one hand, environmental pollution is avoided, and energy is recycled to achieve energy saving. On the other hand, due to the repeated use of expensive niobium chloride sources, waste is avoided, the cost of atomic layer deposition of metal sulfides is greatly reduced, and large-scale, industrialized production and application are possible.

[0078] Each embodiment in this specification is described in a progressive manner, and the same or similar parts between the embodiments can be referred to each other, and each embodiment focuses on the differences from other embodiments. The above is only a specific implementation method of the utility model, but the protection scope of the utility model is not limited to this. Any changes or replacements that can be easily thought of by any technician familiar with the technical field within the technical scope disclosed by the utility model should be included in the protection scope of the utility model. Therefore, the protection scope of the utility model should be based on the protection scope of the claims.

Claims

1. A device for treating reaction residues of atomic layer deposition, characterized in that: The components of the device include: a metal source (24) connected to a reaction chamber (2) via a pneumatic valve V1 (23), a hydrogen sulfide source (21) connected to the reaction chamber (2) via a pneumatic valve V2 (20), and a PT pressure gauge (1) installed on the reaction chamber (2); The output of the reaction chamber (2) is processed through a dual-line system, wherein the gas transmission line of the dual-line system is composed of a processing line I and a processing line II, and the processing line I and the processing line II are each connected to the reaction chamber (2) through a gas transmission pipe; The dual-line system includes at least two modes. In the first mode of the dual-line system, the series connection sequence of the devices in the processing line I is: condensation absorption device, dissolution absorption device, drying device and gas storage device; the series connection sequence of the devices in the processing line II is: dissolution absorption device, drying device and gas storage device; In the second mode of the dual-circuit system, two condensation absorption devices are connected in series in treatment line I; the series connection order of the devices in treatment line II is: combustion chamber, oxidation absorption device and solution absorption device.

2. The device according to claim 1, characterized in that In the first mode, it also includes: pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4), pneumatic valve V8 (18), a first condensation absorption device (7), a dissolution absorption device I (10), a dissolution absorption device II (9), a heating device (8), a drying device I (11), a drying device II (12), a first vacuum pump (13), an air storage device I (15), an air storage device II (17), a pressure reducing valve V11 (3) and a pressure reducing valve V22 (19); Among them, the pneumatic valve V3 (5), the first condensation absorption device (7), the dissolution absorption device I (10), the drying device I (11), the first vacuum pump (13), the pneumatic valve V5 (14), the gas storage device I (15), the pneumatic valve V7 (4), and the pressure reducing valve V11 (3) are connected in sequence through the gas transmission pipe to form a processing line I; The pneumatic valve V4 (6), the dissolving and absorbing device II (9), the drying device II (12), the first vacuum pump (13), the pneumatic valve V6 (16), the gas storage device II (17), the pneumatic valve V8 (18), and the pressure reducing valve V22 (19) are connected in sequence through a gas transmission pipe to form a processing line II; The pneumatic valve V3 (5) of the processing line I and the pneumatic valve V4 (6) of the processing line II are both connected to the reaction chamber (2) through a gas pipeline.

3. The device according to claim 2, characterized in that In the dissolution absorption device I (10), a neutralization reaction solution is built in, and the neutralization reaction solution is used to react with hydrochloric acid HCl for neutralization; A desiccant is built into the drying device I (11), and the desiccant is used to remove water vapor introduced from the dissolution absorption device I (10); The reaction solution built into the dissolution absorption device I (10) is a sodium hydroxide NaOH solution or a potassium hydroxide KOH solution; the desiccant is soda lime or silica gel; The pressure reducing valve V11 (3) is used to reduce the pressure of the carrier gas in the gas storage device I (15) and pass it into the metal source path; The pressure reducing valve V22 (19) is used to reduce the pressure of hydrogen sulfide and carrier gas in the gas storage device II (17) and introduce them into the hydrogen sulfide source path.

4. The device according to claim 2, characterized in that In the dissolution absorption device II (9), a neutralization reaction solution is built in, and the neutralization reaction solution is used to react with the hydrochloric acid HCl for neutralization; A heating device (8) is installed outside the dissolution absorption device II (9); The drying device II (12) contains a desiccant.

5. The device according to claim 4, characterized in that The reaction solution built into the dissolution absorption device II (9) is a sodium disulfide NaS2 solution or a sodium hydrosulfide NaHS solution.

6. The device according to claim 5, characterized in that The desiccant in the drying device II (12) is phosphorus pentoxide P2O5.

7. The device according to claim 2, characterized in that Pneumatic valve V3 (5), pneumatic valve V4 (6), pneumatic valve V5 (14), pneumatic valve V6 (16), pneumatic valve V7 (4) and pneumatic valve V8 (18) are all connected to the electromagnetic reversing valve, and the electromagnetic reversing valve is connected to the programmable logic controller PLC.

8. The device according to claim 1, characterized in that In the second mode, it also includes: a combustion chamber (26), a pneumatic valve V10 (27), a second condensation absorption device 1 (28), a third condensation absorption device 2 (29), a pneumatic valve V9 (30), a second vacuum pump (31), a pneumatic valve V13 (32), a solution absorption device (33), an oxidation absorption device (34), a pneumatic valve V12 (35) and a pneumatic valve V11 (36); Among them, the pneumatic valve V3 (5), the second condensation absorption device 1 (28), the third condensation absorption device 2 (29) and the pneumatic valve V9 (30) are connected in sequence through the gas transmission pipe to form a processing line I; The pneumatic valve V10 (27), the combustion chamber (26), the pneumatic valve V12 (35), the oxidation absorption device (34), the solution absorption device III (33) and the pneumatic valve V13 (32) are connected in sequence through a gas pipeline to form a processing line II, wherein a pneumatic valve V11 (36) is also installed at the air inlet of the combustion chamber (26); The pneumatic valve V9 (30) of the processing line I and the pneumatic valve V13 (32) of the processing line II are both connected to the second vacuum pump (31) through the gas transmission pipe, and the second vacuum pump (31) is used to exhaust gas.

9. The device according to claim 8, characterized in that The pneumatic valve V11 (36), the pneumatic valve V10 (27), the pneumatic valve V9 (30), the pneumatic valve V13 (32) and the pneumatic valve V12 (35) are all connected to the electromagnetic reversing valve, and the electromagnetic reversing valve is connected to the programmable logic controller PLC.

10. The device according to claim 8, characterized in that The reaction solution built into the solution absorption device (33) is diluted sulfuric acid; Vanadium pentoxide V205 is used in the oxidation absorption device (34).

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