A device and method for preparing tantalum disulfide thin film based on atomic layer deposition

Abstract

The embodiment of the present invention discloses a tantalum disulfide thin film preparation device and method based on atomic layer deposition, which relates to the field of micro-nano manufacturing technology and can reduce the temperature of synthetic growth, so as to reduce energy consumption and component loss, thereby increasing the service life of components and reducing the cost of use. The present invention includes: source path I, multi-temperature zone coordinated solid source conveying device, source path II, reaction chamber device, and tail gas treatment device.

Description

Technical Field

[0001] The present invention relates to the field of micro-nano manufacturing technology, and in particular to a tantalum disulfide film preparation device and method based on atomic layer deposition. Background Art

[0002] Tantalum disulfide (TaS2) thin films have attracted widespread attention due to their excellent mechanical, electrical, optical and catalytic properties. They have important application value in the fields of hydrodesulfurization catalysis, photovoltaic cells, photocatalysis, nanofriction, lithium batteries and dry lubrication. Mechanical exfoliation is usually used to prepare layered tantalum disulfide films, and the tantalum disulfide prepared by this method has a perfect crystal structure. However, the tantalum disulfide film prepared by this method is small in size and very inefficient. Due to size and efficiency limitations, the method of preparing tantalum disulfide films by mechanical exfoliation cannot be used on a large scale in fields such as integrated circuit manufacturing. It is particularly urgent to artificially synthesize and grow large-area, high-quality tantalum disulfide films.

[0003] Based on the existing semiconductor industry technology, the most popular method for artificially synthesizing tantalum disulfide is chemical vapor deposition (CVD). This method is to heat the tantalum source (TaO3 or TaCl5) and the sulfur source (S powder) to produce the corresponding gas precursor, and then transport them to the vicinity of the substrate through an inert gas (Ar or N2) to generate the required tantalum disulfide film on the substrate. Although this method can obtain large-area, high-quality tantalum disulfide, it has its shortcomings: since the growth process is continuous, the thickness of the film is not easy to accurately control, especially for some high aspect ratio structures, such as holes and grooves, the CVD method cannot deposit a uniform film, and the material will be deposited at the open edge. At the same time, the temperature of the synthetic growth is relatively high, requiring 650℃-1000℃, which limits the application on substrates that are not resistant to high temperatures, and maintaining high temperatures for a long time will also increase energy waste and accelerate component loss. Summary of the invention

[0004] The embodiments of the present invention provide a tantalum disulfide thin film preparation device and method based on atomic layer deposition, which can reduce the temperature of synthetic growth, so as to reduce energy consumption and component loss, thereby increasing the service life of components and reducing the cost of use.

[0005] To achieve the above object, the embodiments of the present invention adopt the following technical solutions:

[0006] On the one hand, a tantalum disulfide thin film preparation device based on atomic layer deposition is provided, and the components of the tantalum disulfide thin film preparation device include: a source path I, a multi-temperature zone coordinated solid source conveying device, a source path II, a reaction chamber device and an exhaust gas treatment device;

[0007] The source path I is used to transport a Ta source (tantalum source) for atomic layer deposition of a tantalum disulfide film to the reaction chamber device, and comprises: a Ta source (18), a manual valve V1 (17), a pneumatic valve V11 (13), a first carrier gas flow meter (20) and a source path I pressure sensor P1 (21);

[0008] The multi-temperature zone coordinated solid source conveying device is installed along the pipeline in the source path I, and the multi-temperature zone coordinated solid source conveying device includes: a solid source heating device 1 (1), a solid source heating device 2 (15), a solid source heating device 3 (16) and a solid source heating device 4 (19);

[0009] The source path II is used to transport an S source (sulfur source) for atomic layer deposition of a tantalum disulfide film to a reaction chamber device, and comprises: an S source (12), a manual valve V2 (11), a pneumatic valve V22 (10), a source path II pressure sensor P2 (9) and a second carrier gas flow meter (14);

[0010] The reaction chamber device is used for atomic layer deposition reaction of tantalum disulfide thin film, and comprises: a chamber pressure sensor P0 (2), a reaction chamber (3) and a chamber heating device (4);

[0011] The exhaust gas treatment device is used to treat the exhaust gas of atomic layer deposition tantalum disulfide film to avoid polluting the environment, comprising: a vacuum pump (5), an anti-backflow device (6), an exhaust gas treatment device 1 (7) and an exhaust gas treatment device 2 (8), wherein a neutralizing solution is built in the exhaust gas treatment device 1 (7), and an indicating solution is built in the exhaust gas treatment device 2 (8).

[0012] Specifically, the solid source heating device 1 (1) is installed close to the pipeline from the pneumatic valve V11 (13) to the reaction chamber device, and the heating range of the solid source heating device 1 (1) is the first temperature zone, and the heating range of the first temperature zone at least covers the pipeline from the pneumatic valve V11 (13) to the reaction chamber device; the solid source heating device 2 (15) is installed close to the pneumatic valve V11 (13), and the heating range of the solid source heating device 2 (15) is the second temperature zone, and the heating range of the second temperature zone at least covers the pneumatic valve V11 (13); the solid source heating device 3 (16) is installed close to the manual valve V1 (17), and the heating range of the solid source heating device 3 (16) is the third temperature zone, and the heating range of the third temperature zone at least covers the manual valve V1 (17); the solid source heating device 4 (19) is installed close to the Ta source (18), and the heating range of the solid source heating device 4 (19) is the fourth temperature zone, and the heating range of the fourth temperature zone at least covers the Ta source (18).

[0013] Among them, in the multi-temperature zone coordinated solid source conveying device, the solid source heating device 1 (1), the solid source heating device 2 (15), the solid source heating device 3 (16) and the solid source heating device 4 (19) are all connected to the solid-state relay, the solid-state relay is connected to the controller, and the controller is connected to the host computer; the controller is also connected to a sensor data acquisition device for acquiring the sensor data and converting it and transmitting it to the controller. The sensor data acquisition device receives the temperature signals returned by all temperature sensors, wherein at least one temperature sensor is installed in each temperature zone. The sensor data acquisition device also receives the pressure signal returned by the source path I pressure sensor P1 (21). The multi-temperature zone coordinated solid source conveying device is composed of a host computer, a controller, a solid source relay, a solid source heating device 1 (1), a solid source heating device 2 (15), a solid source heating device 3 (16), a solid source heating device 4 (19), a temperature sensor, and a sensor data acquisition device. It can realize the coordinated control of the four temperature zones of the Ta source (18), the manual valve V1 (17), the pneumatic valve V11 (13), and the pipeline to form a multi-temperature gradient Ta source conveying to improve the accuracy of the solid Ta source conveying amount, reduce the condensation phenomenon of the valve body and the pipeline, increase the service life of the components, and reduce the use cost. In practical applications, the host computer can be a computer, the controller can be a single-chip microcomputer, the solid state relay can be a PLC, and the heating device can be a heating wire.

[0014] Specifically, the neutralizing solution built into the tail gas treatment device 1 (7) is a sodium hydroxide solution or a potassium hydroxide solution; the indicating solution built into the tail gas treatment device 2 (8) is a copper sulfate solution. In the tail gas treatment device 1 (7), a solution capable of neutralizing hydrogen sulfide and hydrochloric acid is built in, and the specific composition is not required. Preferably, a sodium hydroxide solution with a concentration of 5g / L or a potassium hydroxide solution with a concentration of 5g / L is selected; in the tail gas treatment device 2 (8), a solution capable of indicating the content of hydrogen sulfide and hydrochloric acid is built in, and the specific composition is not required. Preferably, a copper sulfate solution with a concentration of 1g / L is selected.

[0015] The working process of the multi-temperature zone coordinated solid source conveying device includes: the host computer records the preset heating temperatures of the four solid source heating devices, namely, solid source heating device 1 (1), solid source heating device 2 (15), solid source heating device 3 (16) and solid source heating device 4 (19), according to the user's input operation; the host computer transmits the preset heating temperatures of the four solid source heating devices to the controller; the controller controls the four solid source heating devices to start heating through the solid-state relay until their respective temperatures reach the preset heating temperatures; the sensor data acquisition device collects the temperatures of the four temperature zones through the temperature sensors installed in the four temperature zones, and collects the pressure value returned by the source path I pressure sensor P1 (21), and then the sensor data acquisition device feeds back the collected temperatures and pressure values ​​of the four temperature zones to the controller to form a closed-loop control. In this embodiment, the host computer, controller, solid-state relay, solid source heating device 1 (1), solid source heating device 2 (15), solid source heating device 3 (16), solid source heating device 4 (19), temperature sensor, sensor data acquisition device are composed, which can realize the coordinated control of four temperature zones of Ta source (18), manual valve V1 (17), pneumatic valve V11 (13), and pipeline, and form multi-temperature gradient Ta source delivery, so as to improve the accuracy of solid Ta source delivery, reduce condensation phenomenon of valve body and pipeline, increase component service life, and reduce use cost.

[0016] This embodiment also provides a method for preparing a tantalum disulfide thin film based on atomic layer deposition, comprising:

[0017] Step S1, starting the chamber heating device (4), heating the reaction chamber (3) containing the sample to be deposited to a preset temperature of the reaction chamber, and maintaining the reaction chamber at the preset temperature for a first preset time;

[0018] The sample to be deposited refers to the substrate on which the tantalum disulfide film is to be deposited, specifically some conventional substrates, such as silicon wafers, silicon oxide wafers, conductive glass, etc., which are substrate materials that are often deposited by atomic layer deposition in the art.

[0019] Step S2, start the multi-temperature zone coordinated solid source conveying device to heat the source path I, wherein the heating areas of the solid source heating device 1 (1), the solid source heating device 2 (15), the solid source heating device 3 (16) and the solid source heating device 4 (19) are respectively used as the first temperature zone to the fourth temperature zone to heat the Ta source (18), the manual valve V1 (17), the pneumatic valve V11 (13) and the pipeline respectively;

[0020] Step S3, open the manual valve V1 (17) and introduce the carrier gas through the first carrier gas flowmeter (20) to form Ta source vapor and send it into the reaction chamber (3), the manual valve V1 (17) remains open until the third preset time is reached and then closed; after the manual valve V1 (17) is closed, the carrier gas continues to be introduced until the fourth preset time is reached; the time from the start of the introduction to the end of the introduction is maintained to the third preset time, so that the Ta source and the sample surface undergo self-limiting chemical adsorption, after the Ta source vapor is introduced, the carrier gas continues to be introduced and maintained until the fourth preset time, the reaction by-products and residual Ta source are rinsed clean, and sent to the exhaust gas treatment device for treatment and discharge.

[0021] Step S4, open the manual valve V2 (11) and introduce the carrier gas through the second carrier gas flow meter (14), form hydrogen sulfide and send it into the reaction chamber (3), the manual valve V2 (11) remains open until the fifth preset time is reached and then closed; after the manual valve V2 (11) is closed, continue to introduce the carrier gas until the sixth preset time is reached. The time from the start of introduction to the end of introduction is maintained to the fifth preset time, so that the S source (12) and the Ta source adsorbed on the sample surface in step S3 undergo a self-limiting chemical reaction, and a layer of tantalum disulfide film is generated on the substrate sample. After the S source (12) is blown in, continue to introduce the carrier gas and maintain it until the sixth preset time, so that the reaction byproducts and residual S source are washed away and sent to the tail gas treatment device for treatment and discharge.

[0022] In a preferred embodiment, in step S1: 200°C ≤ the preset temperature of the reaction chamber ≤ 500°C; 1 min ≤ the first preset time ≤ 120 min.

[0023] The preset heating temperatures of the first temperature zone to the fourth temperature zone are T1 to T4, respectively, T1∈[50°C, 250°C], T2∈[50°C, 250°C], T3∈[50°C, 250°C], T4∈[50°C, 250°C], and T1<T2<T3<T4; after each temperature zone reaches its own preset heating temperature, the temperature is maintained until the second preset time, wherein 1min≤second preset time≤120min. Specifically, the heating temperature of the first temperature zone to the heating temperature of the fourth temperature zone increases successively, so that they form a temperature gradient that gradually decreases from the reaction chamber (3) to the Ta source (18), and the sensor data acquisition device collects the temperature of the Ta source (18), the manual valve V1 (17), the pneumatic valve V11 (13) and the pipeline and the pressure in the pipeline through the temperature sensor and the pressure sensor P1 (21), and feeds it back to the controller for correction.

[0024] In the preferred embodiment, the Ta source (18) needs to have a self-limiting chemical reaction capability, and has a built-in tantalum organic metal or tantalum halide; in the step S3, 0.1s≤the third preset time≤10s, 1s≤the fourth preset time≤50s. The S source (12) needs to have a self-limiting chemical reaction capability, and has a built-in hydrogen sulfide, a thiol-containing organic matter, and a plasma containing a thiol-containing organic matter, wherein the plasma in this embodiment is a plasma containing a thiol-containing organic matter, for example: the S source (12) can be selected from a plasma of hydrogen sulfide, a plasma organic matter containing a thiol group, or a plasma containing a thiol-containing organic matter (select one of these three, not all three of them are built-in at the same time); in the step S4, 0.1s≤the fifth preset time≤10s, 1s≤the sixth preset time≤50s.

[0025] In a preferred embodiment, the carrier gas is an inert gas such as nitrogen or argon, and the carrier gas flow rate is 10 to 500 mL / min.

[0026] In this embodiment, steps S3 and S4 include two self-limiting chemical reactions, which constitute a complete cycle, namely, the atomic layer deposition tantalum disulfide film cycle. By controlling the number of cycles, the thickness of the atomic layer deposited TaS2 film can be accurately controlled to obtain a TaS2 film with uniform quality and a smooth surface.

[0027] The tantalum disulfide thin film preparation device and method based on atomic layer deposition provided by the embodiment of the present invention can improve the accuracy of the solid Ta source delivery amount and reduce the condensation phenomenon of the valve body and pipeline; and the temperature of the synthetic growth is low, which reduces energy consumption and component loss, thereby increasing the service life of the components and reducing the cost of use. In actual tests, the film grown by the process of this embodiment has uniform quality, a smooth surface, good repeatability, and can be grown on substrates with complex structures. It is suitable for large-scale preparation and production of tantalum disulfide thin films. At the same time, there is no harmful exhaust gas emission, achieving the purpose of green manufacturing. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] 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 paying creative work.

[0029] Figure 1 A schematic diagram of the structure of a device provided in an embodiment of the present invention.

[0030] Figure 2 A schematic diagram of a control method for a multi-temperature zone coordinated solid source conveying device provided in an embodiment of the present invention.

[0031] Figure 3This is a SEM picture of a tantalum disulfide film prepared by the method of the present invention. It can be seen from the picture that the surface of the grown tantalum disulfide film is flat and uniform.

[0032] Figure 4 The Raman spectrum of the tantalum disulfide film prepared by the method of the present invention is shown in the figure. It can be clearly seen that the characteristic peak of the tantalum disulfide film is 83cm -1 .

[0033] Figure 5 This is an XPS graph of a tantalum disulfide film prepared by the method of the present invention, wherein Ta peak and S peak signals are obvious.

[0034] Figure 1 The relevant labeled names are as follows: 1. Solid source heating device 1; 2. Cavity pressure sensor P0; 3. Reaction chamber; 4. Cavity heating device; 5. Vacuum pump; 6. Anti-backflow device; 7. Exhaust treatment device 1; 8. Exhaust treatment device 2; 9. Source path II pressure sensor P2; 10. Pneumatic valve V22; 11. Manual valve V2; 12. S source; 13. Pneumatic valve V11; 14. Flow meter 2; 15. Solid source heating device 2; 16. Solid source heating device 3; 17. Manual valve V1; 18. Ta source; 19. Solid source heating device 4; 20. Flow meter 1; 21. Source path I pressure sensor P1. DETAILED DESCRIPTION

[0035] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. The embodiments of the present invention 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 present invention, and cannot be interpreted as limiting the present invention. It can be understood by those skilled in the art that, unless specifically stated, the singular forms "one", "one", "said" and "the" used herein may also include plural forms. It should be further understood that the term "including" used in the specification of the present invention 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 term "and / or" used herein includes any unit and all combinations of one or more associated listed items. It will 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 generally understood by those of ordinary skill in the art to which the present invention belongs. It should also be understood that terms such as those defined in general dictionaries should be understood to have meanings consistent with the meanings in the context of the prior art, and will not be interpreted with idealized or overly formal meanings unless defined as herein.

[0036] The atomic layer deposition process (ALD) relies on the self-limiting chemical reaction of the precursor on the surface of the substrate sample to deposit a thin film. By alternately introducing precursor pulses, atomic layer deposition can uniformly deposit thin films on structures with high aspect ratios, and the thickness of the film can be precisely controlled by controlling the number of cycles. However, due to the difficulties such as the transportation of solid sources that easily cause pipeline blockage and the treatment of sulfide tail gas, the preparation scheme of atomic layer deposition tantalum disulfide film still has defects. This embodiment is improved on the basis of the atomic layer deposition process (ALD). On the one hand, it solves the problem that the transportation of solid sources easily causes pipeline blockage; on the other hand, it also solves the problem of treating sulfide tail gas, thereby realizing the green and pollution-free preparation of atomic layer deposition tantalum disulfide film.

[0037] Specifically, an embodiment of the present invention provides a device for atomic layer deposition of tantalum disulfide thin film, such as Figure 1 As shown, the device includes: source path I, a multi-temperature zone coordinated solid source conveying device, source path II, a reaction chamber device, and an exhaust gas treatment device.

[0038] The source path I is composed of a Ta source (18), a manual valve V1 (17), a pneumatic valve V11 (13), a flow meter 1 (20), and a source path I pressure sensor P1 (21), and is used to transport the Ta source for atomic layer deposition of tantalum disulfide film to the reaction chamber device.

[0039] like Figure 1 and Figure 2 As shown, the multi-temperature zone coordinated solid source conveying device is composed of a host computer, a controller, a solid-state relay, a solid source heating device 1 (1), a solid source heating device 2 (15), a solid source heating device 3 (16), a solid source heating device 4 (19), a temperature sensor, and a sensor data acquisition device. The multi-temperature zone coordinated solid source conveying device can realize the coordinated control of four temperature zones of the Ta source (18), the manual valve V1 (17), the pneumatic valve V11 (13), and the pipeline, forming a Ta source conveying with multiple temperature gradients, so as to improve the accuracy of the solid Ta source conveying amount, reduce the condensation phenomenon of the valve body and the pipeline, increase the service life of the components, and reduce the use cost. The working process is as follows: according to the requirements of the atomic layer deposition process, the heating temperatures of the four solid source heating devices are preset on the host computer, and then the host computer transmits the heating temperature parameters to the controller. The controller controls the four solid source heating devices to heat according to the preset temperature through the solid-state relay. The sensor data acquisition device feeds back the temperatures (T1, T2, T3, T4) and pipeline pressure (P1) of the four solid source heating devices to the controller through the temperature sensor and the source path I pressure sensor P1 (21), thus forming a closed-loop control.

[0040] The source path II is composed of an S source (12), a manual valve V2 (11), a pneumatic valve V22 (10), a source path II pressure sensor P2 (9), and a flow meter 2 (14), and is used to transport the S source for atomic layer deposition of tantalum disulfide thin film to a reaction chamber device.

[0041] The reaction chamber device is composed of a chamber pressure sensor P0 (2), a reaction chamber (3), and a chamber heating device (4), and is used for atomic layer deposition reaction of tantalum disulfide thin film.

[0042] The tail gas treatment device is composed of a vacuum pump (5), an anti-backflow device (6), a tail gas treatment device 1 (7), and a tail gas treatment device 2 (8), and is used to treat the tail gas of the atomic layer deposition tantalum disulfide film to avoid polluting the environment. The tail gas treatment device 1 (7) is equipped with a solution that can neutralize hydrogen sulfide and hydrochloric acid, and the specific composition is not required. Preferably, sodium hydroxide and potassium hydroxide solutions are selected; the tail gas treatment device 2 (8) is equipped with a solution that can indicate the content of hydrogen sulfide and hydrochloric acid, and the specific composition is not required. Preferably, copper sulfate solution is selected.

[0043] The embodiment of the present invention also provides a method for preparing the above-mentioned atomic layer deposition tantalum disulfide film preparation device, combined with Figure 1 and Figure 2 , the method comprises the following steps:

[0044] Step S1, heating a reaction chamber (3) containing a sample to be deposited to a preset temperature by means of a chamber heating device (4), and maintaining the temperature for a first preset time.

[0045] The preset temperature range is 200-500°C.

[0046] The first preset time range is 1 to 120 minutes.

[0047] Step S2, using a multi-temperature zone coordinated solid source conveying device to heat the source path I. Specifically, the heating temperature is preset on the host computer, and the Ta source (18), manual valve V1 (17), pneumatic valve V11 (13) and pipeline are heated respectively through the controller, solid-state relay, solid source heating device 1 (1), solid source heating device 2 (15), solid source heating device 3 (16), and solid source heating device 4 (19), so that they form a gradually decreasing temperature gradient from the reaction chamber (3) to the Ta source (18). The sensor data acquisition device collects the temperature of the Ta source (18), manual valve V1 (17), pneumatic valve V11 (13) and pipeline and the pressure in the pipeline through the temperature sensor and pressure sensor P1 (21), and feeds it back to the controller for correction.

[0048] The preset heating temperature range of the solid source heating device 1 (1), the solid source heating device 2 (15), the solid source heating device 3 (16), and the solid source heating device 4 (19) is 50 to 250°C. After reaching the preset heating temperature, the second preset time is maintained.

[0049] The second preset time range is 1 to 120 minutes.

[0050] Step S3, open the manual valve V1 (17), use the carrier gas to deliver the Ta source (18) into the reaction chamber (3) through the pneumatic valve V11 (13) and the pipeline, and keep the time from the start of delivery to the end of delivery at the third preset time, so that the Ta source and the sample surface undergo self-limiting chemical adsorption. After the Ta source vapor is delivered, continue to introduce the carrier gas and keep it until the fourth preset time, rinse the reaction by-products and residual Ta source, and deliver them to the exhaust gas treatment device for treatment and discharge.

[0051] The Ta source needs to have a self-limiting chemical reaction capability, and is selected from tantalum organic metal or tantalum halide.

[0052] The third preset time is 0.1-10s.

[0053] The fourth preset time is 1 to 50 seconds.

[0054] Step S4, open the manual valve V2 (11), use the carrier gas to send the S source (12), hydrogen sulfide into the reaction chamber (3) through the pneumatic valve V22 (10) and the pipeline, and keep the time from the start of the feeding to the end of the feeding at the fifth preset time, so that the S source (12) and the Ta source adsorbed on the sample surface in step S3 undergo a self-limiting chemical reaction, and a layer of tantalum disulfide film is generated on the base sample. After the blowing of the S source (12) is completed, continue to introduce the carrier gas and keep it until the sixth preset time, rinse off the reaction by-products and residual S source, and send it to the exhaust gas treatment device for treatment and discharge.

[0055] The S source needs to have a self-limiting chemical reaction capability, and hydrogen sulfide, organic matter containing mercapto groups and plasma thereof are selected.

[0056] The fifth preset time is 0.1-10s.

[0057] The sixth preset time is 1 to 50 seconds.

[0058] The carrier gas is an inert gas such as nitrogen or argon, and the carrier gas flow rate is 10 to 500 mL / min.

[0059] Steps S3 and S4 include two self-limiting chemical reactions, which constitute a complete cycle, namely, the atomic layer deposition of tantalum disulfide film cycle. By controlling the number of cycles, the thickness of the atomic layer deposited TaS2 film can be accurately controlled to obtain a TaS2 film with uniform quality and smooth surface.

[0060] Further, in the preferred embodiment of the present invention, the Ta source and the S source are respectively tantalum pentafluoride TaF5 and hydrogen sulfide H2S, and the green atomic layer deposition of tantalum disulfide film is carried out. Figure 1 and Figure 2 , the above preparation method can be further optimized as follows:

[0061] Step S1, heating the reaction chamber (3) containing the sample to be deposited to 450° C. by means of a chamber heating device (4), and maintaining the temperature for 30 minutes.

[0062] Step S2, using a multi-temperature zone coordinated solid source conveying device to heat the source path I. Specifically, the heating temperature is preset on the host computer, and the Ta source (18), manual valve V1 (17), pneumatic valve V11 (13) and pipeline are heated respectively through the controller, solid-state relay, solid source heating device 1 (1), solid source heating device 2 (15), solid source heating device 3 (16), and solid source heating device 4 (19), so that they form a gradually decreasing temperature gradient from the reaction chamber (3) to the Ta source (18). The sensor data acquisition device collects the temperature of the Ta source (18), manual valve V1 (17), pneumatic valve V11 (13) and pipeline and the pressure in the pipeline through the temperature sensor and pressure sensor P1 (21), and feeds it back to the controller for correction.

[0063] The preset heating temperature ranges of the solid source heating device 1 (1), the solid source heating device 2 (15), the solid source heating device 3 (16), and the solid source heating device 4 (19) are 200°C, 180°C, 150°C, and 100°C, respectively. After reaching the preset heating temperature, maintain it for 30 minutes.

[0064] Step S3, open the manual valve V1 (17), use the carrier gas N2 to feed the Ta source TaF5 into the reaction chamber (3) through the pneumatic valve V11 (13) and the pipeline, and keep the time from the beginning of feeding to the end of feeding at 0.5s, so that TaF5 and the hydroxyl groups on the surface of the sample undergo self-limiting chemical adsorption. After the TaF5 vapor is fed, continue to feed the carrier gas and keep it for 20s to rinse the reaction by-products and residual TaF5, and feed it into the exhaust gas treatment device for treatment and discharge. The exhaust gas treatment device 1 (7) is equipped with a sodium hydroxide solution, and the exhaust gas treatment device 2 (8) is equipped with a copper sulfate solution.

[0065] Step S4, open the manual valve V2 (11), use the carrier gas N2 to send the S source H2S through the pneumatic valve V22 (10) and the pipeline into the reaction chamber (3), and keep the time from the beginning of the feeding to the end of the feeding at 0.5s, so that the H2S and the TaF5 adsorbed on the sample surface in step S3 undergo a self-limiting chemical reaction to form a tantalum disulfide film on the base sample. After the H2S blowing is completed, continue to introduce the carrier gas and keep it for 20s to rinse away the reaction by-products and residual H2S, and send it to the exhaust gas treatment device for treatment and discharge.

[0066] Steps S3 and S4 include two self-limiting chemical reactions, which constitute a complete cycle, namely, an atomic layer deposition cycle of tantalum disulfide film. By controlling the number of cycles, the thickness of the atomic layer deposition TaS2 film can be accurately controlled. After 100 cycles of deposition, a TaS2 film with uniform quality and smooth surface is obtained.

[0067] The obtained TaS2 film was tested by scanning electron microscopy (SEM), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS). Figure 3 , Figure 4 , Figure 5 As shown. From the scanning electron microscope data, it can be seen that the quality of the prepared TaS2 film is uniform and the surface is flat. From the Raman spectrum data, it can be seen that the characteristic peak of the prepared tantalum disulfide film is located at 83cm -1 , which is a 2H structure. From the X-ray photoelectron spectroscopy data, it can be seen that the Ta peak and S peak signals are obvious, and the prepared film is indeed a tantalum disulfide film.

[0068] 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. In particular, for the device embodiment, since it is basically similar to the method embodiment, the description is relatively simple, and the relevant parts can be referred to the partial description of the method embodiment. The above is only a specific implementation method of the present invention, but the protection scope of the present invention is not limited thereto. 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 present invention should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A method for preparing a tantalum disulfide thin film based on atomic layer deposition, characterized in that: include: Step S1, starting the chamber heating device (4), heating the reaction chamber (3) containing the sample to be deposited to a preset temperature of the reaction chamber, and maintaining the reaction chamber at the preset temperature for a first preset time; Step S2, starting the multi-temperature zone coordinated solid source conveying device to heat the source path I, wherein the heating areas of the solid source heating device 1 (1), the solid source heating device 2 (15), the solid source heating device 3 (16) and the solid source heating device 4 (19) are respectively used as the first temperature zone to the fourth temperature zone to heat the Ta source (18), the manual valve V1 (17), the pneumatic valve V11 (13) and the pipeline respectively; Step S3, opening the manual valve V1 (17) and introducing carrier gas through the first carrier gas flow meter (20) to form Ta source vapor and send it into the reaction chamber (3), the manual valve V1 (17) remains open until a third preset time is reached and then closes; after the manual valve V1 (17) is closed, the carrier gas continues to be introduced until a fourth preset time is reached; Step S4, opening the manual valve V2 (11) and introducing a carrier gas through the second carrier gas flow meter (14) to form hydrogen sulfide and send it into the reaction chamber (3), the manual valve V2 (11) remains open until the fifth preset time is reached and then closes; after the manual valve V2 (11) is closed, the carrier gas continues to be introduced until the sixth preset time is reached; The solid source heating device 1 (1) is installed close to the pipeline from the pneumatic valve V11 (13) to the reaction chamber device, and the heating range of the solid source heating device 1 (1) is used as a first temperature zone, and the heating range of the first temperature zone at least covers the pipeline from the pneumatic valve V11 (13) to the reaction chamber device; The solid source heating device 2 (15) is installed close to the pneumatic valve V11 (13), and the heating range of the solid source heating device 2 (15) serves as a second temperature zone, and the heating range of the second temperature zone at least covers the pneumatic valve V11 (13); The solid source heating device 3 (16) is installed close to the manual valve V1 (17), and the heating range of the solid source heating device 3 (16) serves as a third temperature zone, and the heating range of the third temperature zone at least covers the manual valve V1 (17); The solid source heating device 4 (19) is installed close to the Ta source (18), and the heating range of the solid source heating device 4 (19) serves as a fourth temperature zone, and the heating range of the fourth temperature zone at least covers the Ta source (18); The preset heating temperatures of the first temperature zone to the fourth temperature zone are T1 to T4, T1∈[50°C, 250°C], T2∈[50°C, 250°C], T3∈[50°C, 250°C], T4∈[50°C, 250°C], and T1<T2<T3<T4; After each temperature zone reaches its own preset heating temperature, the temperature is maintained until a second preset time, wherein 1 min ≤ second preset time ≤ 120 min.

2. The method according to claim 1, characterized in that In step S1: 200℃≤preset temperature of reaction chamber≤500℃; 1 min≤first preset time≤120 min.

3. The method according to claim 1, characterized in that The Ta source (18) contains tantalum organometallic or tantalum halide; In the step S3, 0.1s≤the third preset time≤10s, 1s≤the fourth preset time≤50s; The S source (12) contains hydrogen sulfide, organic matter containing mercapto groups, and plasma containing organic matter containing mercapto groups; In the step S4, 0.1s≤fifth preset time≤10s, 1s≤sixth preset time≤50s.

Images