Multifunctional cold wall type vapor deposition self-heating sample table and application method thereof

Abstract

The invention discloses a multifunctional cold wall type vapor deposition self-heating sample table and an application method thereof. The multifunctional cold wall type vapor deposition self-heating sample table comprises a screen, a plane / powder sample containing table, a sample heating table, a temperature control / temperature measurement thermocouple, a supporting rod, a vacuum sealing cover and a handheld rod. The multifunctional cold wall type vapor deposition self-heating sample table is inserted into the vapor deposition reaction cavity and is in vacuum connection with vapor deposition equipment through the vacuum sealing cover; the heating wire and the temperature control / temperature measurement thermocouple are sealed and insulated through a vacuum sealing cover, and are respectively connected with temperature control, temperature measurement and other related instruments and equipment in the application process. According to the invention, the cold wall type vapor deposition process can be realized, that is, the vapor deposition reaction cavity is not heated or is heated to a lower temperature, and a to-be-treated sample (plane or powder) is at a target temperature by heating the self-heating sample table, so that the device is particularly suitable for the high-temperature vapor deposition process; according to the invention, the energy consumption in the vapor deposition reaction process can be greatly reduced.

Description

Technical Field

[0001] This invention belongs to the field of device development and thin film material preparation, and relates to vapor phase thin film deposition technology including chemical vapor deposition and atomic layer deposition. Specifically, it relates to a multifunctional cold-wall vapor phase deposition self-heating sample stage and its application method. Background Technology

[0002] Chemical vapor deposition (CVD) is a technique that utilizes one or more gaseous or vaporous precursor substances to decompose or react at the gas phase or gas-solid interface to generate solid deposits. CVD is generally referred to as chemical vapor deposition (CVD) and atomic layer deposition (ALD). Both are essentially CVD processes, but they differ significantly in process control, process conditions, film deposition methods, and film growth characteristics. Regarding process conditions, the typical CVD process temperature is much higher than ALD, but some special ALD reaction temperatures are also relatively high, reaching up to 500℃ (ChemCatChem 2022, 14(19), e202200406). The higher process temperature not only places special requirements on the material of the ALD reaction chamber—for example, commonly used stainless steel is prone to intergranular corrosion under prolonged high-temperature use, leading to structural damage—but also presents a series of problems such as poor structural integrity, insufficient sealing, and low temperature tolerance of rubber seals during use if a high-temperature resistant quartz reaction chamber is used.

[0003] To effectively reduce the requirements of CVD and high-temperature ALD reaction processes on the vapor deposition reaction chamber, cold-wall vapor deposition (CVD) has emerged. However, most reported cold-wall CVD applications are relatively singular and cannot simultaneously meet the requirements for cold-wall CVD of planar materials and powder materials. Furthermore, existing cold-wall CVD designs are mostly single-wall CVD designs, failing to achieve bidirectional selection between cold-wall and hot-wall CVD. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention aims to provide a multifunctional cold-wall vapor deposition self-heating sample stage and its application method, solving the problem of the current single function in cold-wall vapor deposition processes, which cannot simultaneously meet the requirements of cold-wall vapor deposition for powder and planar samples. The modular design of this invention can retain the original hot-wall vapor deposition function, and cold-wall vapor deposition can be achieved by installing the functional component of this invention when cold-wall vapor deposition is required.

[0005] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0006] A multifunctional cold-walled vapor deposition self-heating sample stage includes a sieve, a sample holding stage, a sample heating stage, a vacuum sealing cover, a support rod, and a handheld rod.

[0007] The sieve, sample holding platform, and sample heating platform are stacked in sequence, and the sample holding platform and sample heating platform are connected by bolt holes or welding to achieve integration.

[0008] The screen is used in the vapor deposition process with powder particles as the substrate to ensure that the chemical atmosphere in the vapor reaction process penetrates into the sample holding stage, while preventing the airflow from carrying the powder particles out of the sample holding stage.

[0009] The sample holding platform includes: a sample tank and a temperature control thermocouple and a temperature measuring thermocouple installed at its bottom. The sample tank is used to hold planar or powder materials, and the temperature control thermocouple and the temperature measuring thermocouple need to be led out from one end of the sample tank.

[0010] The sample heating stage is equipped with uniformly arranged electric heating wires inside, and heating wire leads are extended from one end of the sample heating stage.

[0011] The support rod is suitable for fixing the sample holding stage and the sample heating stage to one side of the vacuum sealing cover, which is used to connect the interface of the vapor deposition equipment and achieve vacuum sealing.

[0012] A hand handle is provided on the outside of the vacuum-sealed cover.

[0013] The present invention also includes the following technical features:

[0014] Specifically, the electric heating wire has a surface with high-temperature resistant insulation.

[0015] Specifically, the temperature control thermocouple, temperature measurement thermocouple, and heating wire all extend from one side of the vacuum seal cover through an insulated and sealed manner.

[0016] Specifically, the vacuum sealing cover is selected from one of the following: vacuum CF flange sealing cover, KF flange sealing cover, and ISO flange sealing cover.

[0017] Specifically, the mesh size of the sieve is adjusted according to the size of the powder particles.

[0018] Specifically, the self-heating sample stage is a multi-functional cold-wall type self-heating sample stage for vapor deposition. The cold wall refers to the fact that the vapor deposition reaction chamber is not heated or the heating temperature is lower than the vapor deposition temperature.

[0019] Specifically, the vapor deposition temperature is the actual temperature value of the heated sample stage.

[0020] Specifically, vapor deposition is a type of chemical vapor deposition or atomic layer deposition.

[0021] The application method of the aforementioned multifunctional cold-wall vapor deposition self-heating sample stage includes the following steps:

[0022] Select the vacuum sealing cap specifications according to the vapor deposition equipment;

[0023] Place the sample on the sample holding platform and determine whether to install a sieve according to the sample type. If the sample is a silicon wafer, no sieve is needed. If the sample is a SiO2 powder material, install a sieve on the sample holding platform.

[0024] Insert the multi-functional cold-wall vapor deposition self-heating sample stage into the vapor deposition equipment, and use clamps or bolts and nuts to vacuum seal the vacuum sealing cover with the vapor deposition equipment.

[0025] The sample heating stage uses an internal electric heating wire for self-heating, and the reaction temperature is set to perform vapor deposition.

[0026] Compared with the prior art, the present invention has the following technical effects:

[0027] 1. The present invention adopts a modular design scheme, which can be added independently as an existing hot-wall vapor deposition module. It can retain the original hot-wall vapor deposition function and at the same time carry out cold-wall vapor deposition.

[0028] 2. This invention can be applied to a wider range of sample surface vapor deposition processes, including planar samples and powder samples.

[0029] 3. The present invention has a clear structure and is easy to use. Users can adjust the relevant parameters according to actual application needs to achieve the cold wall vapor deposition required for different samples. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the overall structure of the device of the present invention.

[0031] Figure 2 XPS curves of TiO2 thin films prepared by ALD with cold and hot walls.

[0032] Figure 3 These are XPS curves of Al2O3 surface-modified layers prepared by cold-wall and hot-wall ALD.

[0033] The meanings of the various markings in the diagram are as follows:

[0034] 1. Sieve, 2. Sample holding platform, 3. Sample heating platform, 4. Vacuum sealing cover, 5. Support rod, 6. Hand handle, 7. Sample tank, 8. Temperature control thermocouple, 9. Temperature measurement thermocouple, 10. Electric heating wire, 11. Heating wire lead wire, 12. Flat sample. Detailed Implementation

[0035] This invention provides a multifunctional cold-wall vapor deposition self-heating sample stage and its application method. The heating wire inside the heating stage needs to be insulated and heat-resistant. The heating wire, temperature control thermocouple, and temperature measuring thermocouple pass through the vacuum sealing cover in an insulated and sealed manner. A suitable vacuum sealing cover is selected and processed to connect the device of this invention with existing thermal vapor deposition equipment and achieve the vacuum sealing function.

[0036] Specifically, such as Figure 1 As shown, the multifunctional cold-wall vapor deposition self-heating sample stage of the present invention includes a sieve 1, a sample holding stage 2, a sample heating stage 3, a vacuum sealing cover 4, a support rod 5, and a handheld rod 6.

[0037] The sieve 1, sample holding platform 2 and sample heating platform 3 are stacked in sequence. The sample holding platform 2 and sample heating platform 3 are connected by bolt holes or welding to achieve integration.

[0038] The sieve 1 is used in the vapor deposition process with powder particles as the substrate. It can ensure that the chemical atmosphere in the vapor reaction process can easily penetrate into the sample holding stage 2, and at the same time, it can prevent the airflow from carrying the powder particles out of the sample holding stage 2.

[0039] The sample holding platform 2 includes a sample tank 7 and a temperature control thermocouple 8 and a temperature measuring thermocouple 9 installed at its bottom. The sample tank 7 is used to hold flat or powder materials. The temperature control thermocouple 8 and the temperature measuring thermocouple 9 need to be led out from one end of the sample tank 7.

[0040] The sample heating stage 3 is equipped with uniformly arranged electric heating wires 10 inside, and heating wires 11 are led out from one end of the sample heating stage 3.

[0041] The support rod 5 is used to fix the sample holding stage 2 and the sample heating stage 3 to one side of the vacuum sealing cover 4. The vacuum sealing cover 4 is used to connect the interface of the vapor deposition equipment and achieve vacuum sealing. The length of the support rod 5 is determined according to the distance between the vacuum sealing cover 4 and the vapor deposition reaction chamber. The strength of the support rod 5 is set according to the total mass of the sample holding stage 2 and the sample heating stage 3 and the length of the support rod 5.

[0042] The vacuum sealing cover 4 is equipped with a hand handle 6 on the outside. The hand handle 6 is a hand grip during operation, which is convenient for installation and disassembly. The length and thickness can be set according to usage habits.

[0043] The electric heating wire 10 has a surface with high-temperature resistant insulation.

[0044] The temperature control thermocouple 8, the temperature measuring thermocouple 9, and the heating wire 11 all extend from one side of the vacuum seal cover 4 through an insulated seal.

[0045] The vacuum sealing cover 4 is selected from one of the following: vacuum CF flange sealing cover, KF flange sealing cover, and ISO flange sealing cover, based on the actual structure design and temperature setting of the vapor deposition equipment.

[0046] The mesh size (mesh count) of screen 1 can be adjusted according to the size of the powder particles.

[0047] This self-heating sample stage is a multi-functional cold-wall type self-heating sample stage for vapor deposition. The cold wall refers to the fact that the vapor deposition reaction chamber is not heated or the heating temperature is lower than the vapor deposition temperature.

[0048] The vapor deposition temperature is the actual temperature of the heated sample stage.

[0049] Vapor deposition is a type of chemical vapor deposition or atomic layer deposition.

[0050] The application method of a multifunctional cold-wall vapor deposition self-heating sample stage includes the following steps:

[0051] Select vacuum sealing cap specification 4 based on the vapor deposition equipment;

[0052] Place the sample on the sample holding platform 2, and determine whether to install a sieve 1 according to the sample type. If the selected sample is a planar sample such as a silicon wafer, there is no need to install a sieve 1. If the selected sample is a powder material such as SiO2 powder material, then install a sieve 1 on the sample holding platform 2.

[0053] Insert the multifunctional cold-wall vapor deposition self-heating sample stage into the reaction chamber of the vapor deposition equipment, and connect the vacuum sealing cover 4 to the vapor deposition equipment and vacuum seal it using clamps or bolts and nuts.

[0054] The sample heating stage 3 is self-heated by the internal electric heating wire 10, and the reaction temperature is set to perform vapor deposition.

[0055] The following are specific embodiments of the present invention. It should be noted that the present invention is not limited to the following specific embodiments. All equivalent modifications made based on the technical solutions of this application fall within the protection scope of the present invention.

[0056] Example 1:

[0057] This embodiment provides a multifunctional cold-wall vapor deposition self-heating sample stage and its application method. The docking equipment is the FH-2 hot-wall ALD equipment produced by Xi'an Modern Chemistry Research Institute, and the deposited material is alumina (TiO2).

[0058] The FH-2 hot-wall ALD apparatus is a typical tubular ALD device, with standard ISO 63 sealing flanges for the sample inlet and outlet. The vacuum sealing cap used in this embodiment also conforms to ISO 63 specifications, and vacuum sealing of the sample inlet and outlet can be achieved using calipers or bolts and nuts. The sample used in this embodiment is a silicon wafer, and no sieve is required at the top of the sample stage. In this embodiment, the planar sample cold-wall vapor deposition self-heating sample stage is inserted into the FH-2 ALD reactor and sealed.

[0059] In this embodiment, two heating methods are selected to prepare the ALD film on the sample stage surface of the present invention: one is self-heating of the sample stage, i.e., cold-wall ALD process; the other is overall heating of the ALD reactor, i.e., hot-wall ALD process. The ALD reaction temperature is set at 150℃ for both heating processes. Figure 2 XPS curves of TiO2 thin films prepared by cold-wall and hot-wall ALD are shown. The results indicate that cold-wall ALD can achieve the same thin film deposition effect as hot-wall ALD.

[0060] Example 2:

[0061] This embodiment provides a multifunctional cold-wall vapor deposition self-heating sample stage and its application method. The docking equipment is the FH-2 hot-wall ALD equipment produced by Xi'an Modern Chemistry Research Institute, and the deposited material is alumina (Al2O3).

[0062] In this embodiment, the sample used is SiO2 powder material, and a sieve is installed at the top of the sample stage. In this embodiment, the planar sample cold-wall vapor deposition self-heating sample stage is inserted into the FH-2 type ALD equipment reactor and sealed.

[0063] In this embodiment, two heating methods are selected to prepare the ALD thin film on the SiO2 powder surface of the sample stage: one is self-heating of the sample stage, i.e., cold-wall ALD process; the other is overall heating of the ALD reactor, i.e., hot-wall ALD process. The ALD reaction temperature is set at 120℃ for both heating processes. Figure 3 The XPS curves of Al2O3 surface-modified layers prepared by cold-wall and hot-wall ALD are shown. The results indicate that cold-wall ALD can achieve the same thin film deposition effect as hot-wall ALD.

[0064] The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings. However, the present invention is not limited to the specific details of the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0065] It should also be noted that the various specific technical features described in the above embodiments can be combined in any suitable manner without contradiction. To avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

[0066] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. A multi-functional cold-wall vapor deposition self-heating sample stage, characterized by, It comprises a screen (1), a sample holding platform (2), a sample heating platform (3), a vacuum sealing cover (4), a supporting rod (5), and a hand-held rod (6). The screen (1), the sample holding platform (2), and the sample heating platform (3) are stacked in sequence, and the sample holding platform (2) and the sample heating platform (3) are connected by bolt punching or welding to realize integration. The screen (1) is used for the vapor deposition process of powder particles as a substrate, ensures that the chemical atmosphere in the vapor reaction process penetrates into the sample holding platform (2), and prevents the airflow from carrying the powder particles out of the sample holding platform (2). The sample holding platform (2) comprises a sample groove (7), a temperature control thermocouple (8) and a temperature measuring thermocouple (9) installed at the bottom of the sample groove (7), and the temperature control thermocouple (8) and the temperature measuring thermocouple (9) are led out from one end of the sample groove (7). The sample heating platform (3) is internally provided with uniformly arranged and distributed electric heating wires (10) and a heating wire lead (11) led out from one end of the sample heating platform (3). The supporting rod (5) is suitable for fixing the sample holding platform (2) and the sample heating platform (3) to one side of the vacuum sealing cover (4), and the vacuum sealing cover (4) is used for connecting the interface of the vapor deposition equipment and realizing vacuum sealing. The vacuum sealing cover (4) is externally provided with the hand-held rod (6).

2. The multi-functional cold-wall vapor deposition self-heating sample table of claim 1, wherein, The electric heating wires (10) are surface high-temperature resistant and insulated.

3. The multi-functional cold-wall vapor deposition self-heating sample table of claim 1, wherein, The temperature control thermocouple (8), the temperature measuring thermocouple (9), and the heating wire lead (11) are all led out from one side of the vacuum sealing cover (4) in an insulated and sealed manner.

4. The multi-functional cold-wall vapor deposition self-heating sample table of claim 1, wherein, The vacuum sealing cover (4) is selected from one of a vacuum CF flange sealing cover, a KF flange sealing cover, and an ISO flange sealing cover.

5. The multi-functional cold-wall vapor deposition self-heating sample table of claim 1, wherein, The screen (1) is adjusted in size according to the size of the powder particles.

6. The multi-functional cold-wall vapor deposition self-heating sample table of claim 1, wherein, The self-heating sample platform is a multifunctional cold-wall vapor deposition self-heating sample platform, and the cold wall refers to that the vapor deposition reaction cavity is not heated or the heating temperature is lower than the vapor deposition temperature.

7. The multi-functional cold-wall vapor deposition self-heating sample table of claim 6, wherein, The vapor deposition temperature is the actual temperature value of the heating sample platform.

8. The multi-functional cold-wall vapor deposition self-heating sample table of claim 1, wherein, The vapor deposition is one of chemical vapor deposition or atomic layer deposition.

9. A method of using a multi-functional cold-wall vapor deposition self-heating sample table according to any one of claims 1 to 8, characterized in that, The method comprises the following steps: Selecting the vacuum sealing cover specification according to the vapor deposition equipment; Placing the sample on the sample holding platform, and determining whether to install the screen according to the sample category, if the sample is a planar sample, the screen is not needed to be installed, and if the sample is a powder material, the screen is installed on the sample holding platform; Inserting the multifunctional cold-wall vapor deposition self-heating sample platform into the reaction cavity of the vapor deposition equipment, and connecting the vacuum sealing cover with the vapor deposition equipment by a clamp or a bolt nut and vacuum sealing; The electric heating wires in the sample heating platform are self-heated, and the reaction temperature is set for vapor deposition.

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