Chemical vapor deposition reaction apparatus and x-ray diffraction in-situ detection apparatus

Abstract

The application discloses a chemical vapor deposition reaction device and an X-ray diffraction in-situ detection device. The opening of the lower cover is arranged upwards, a through hole is formed in the bottom of the lower cover, a cylinder is arranged in the lower cover, the upper end of the cylinder is arranged as a closed end, the lower end of the cylinder is communicated with the through hole, and the cavity surrounded by the cylinder and the lower cover is used for loading a precursor. A substrate sample pool used for loading a substrate is arranged on the upper end surface of the cylinder. A gasket is arranged on the upper end surface of the substrate sample pool. The lower end of the upper cover is connected with the lower cover, and a light transmission window is formed in the upper cover. A sealing window is sealingly arranged in the upper cover. After the precursor volatilizes under a high-temperature condition, the precursor can be attached to the substrate to form a deposition layer. Since the light transmission window is formed in the upper cover, the X-ray diffraction can be used to detect the changes of the phase, size, stress, orientation and structure of the generated product in the chemical vapor deposition process in the chemical vapor deposition reaction device, and the staff can help to establish the structure-activity relationship of a research system.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of material detection, in particular to a chemical vapor deposition reaction device and an X-ray diffraction in-situ detection device. BACKGROUND

[0002] X-ray diffraction technology is an important means in material science research, and is widely used in material phase, size, stress, orientation and structure characterization. Chemical vapor deposition is a process in which gaseous reactants or vapor of solid or liquid reactants are introduced into a reaction chamber to form a solid deposition layer at the gas-solid interface. In order to dynamically detect the changes of the generated phase, size, stress, orientation and structure during the deposition process, X-ray diffraction technology is needed during the chemical vapor deposition process.

[0003] However, the existing technology cannot directly use X-ray diffraction technology to detect the products of the deposition process of chemical vapor deposition, and therefore there is an urgent need for a chemical vapor deposition reaction device that can use X-ray diffraction technology for detection. SUMMARY

[0004] Therefore, the embodiments of the present application provide a chemical vapor deposition reaction device and an X-ray diffraction in-situ detection device to solve the problem that the existing technology cannot directly use X-ray diffraction technology to detect the products of the deposition process of chemical vapor deposition.

[0005] To achieve the above-mentioned purpose, the embodiments of the present application provide the following technical solutions:

[0006] The first aspect of the present application discloses a chemical vapor deposition reaction device, comprising: an upper cover, a sealing window, a gasket, a substrate sample pool and a lower cover;

[0007] The lower cover is open upward, and a through hole is formed in the bottom of the lower cover. A cylinder is arranged in the lower cover, the upper end of the cylinder is a closed end, the lower end of the cylinder communicates with the through hole, and the cavity surrounded by the cylinder and the lower cover is used for loading a precursor;

[0008] The substrate sample pool is arranged on the upper end surface of the cylinder, and the substrate sample pool is used for loading a substrate;

[0009] The gasket is arranged on the upper end surface of the substrate sample pool;

[0010] The lower end of the upper cover is connected with the lower cover, and the upper cover is provided with a light-transmitting window;

[0011] The sealing window is sealingly arranged in the upper cover.

[0012] Preferably, the lower part of the upper cover is provided with an internal thread;

[0013] The upper part of the lower cover is provided with an external thread matched with the internal thread.

[0014] Preferably, the sealing window is made of graphite sheet;

[0015] The upper end surface of the base sample pool is provided with a groove, and a plurality of protruding pieces are arranged along the circumference of the groove.

[0016] Preferably, the groove is of a circular structure.

[0017] Preferably, the plurality of protruding pieces are uniformly arranged along the circumference of the groove.

[0018] The second aspect of the present application discloses an X-ray diffraction in-situ detection device, comprising: a light source, a first light path assembly, a detector, a second light path assembly, a high-temperature measurement system and the chemical vapor deposition reaction device disclosed in the first aspect of the present application;

[0019] The first light path assembly is arranged between the light source and the high-temperature measurement system.

[0020] The second light path assembly is arranged between the high-temperature measurement system and the detector.

[0021] The chemical vapor deposition reaction device is arranged on the sample table of the high-temperature measurement system.

[0022] Preferably, the first light path assembly comprises: a light path conversion module, a first Soller slit and an incident line divergence slit.

[0023] The light path conversion module, the first Soller slit and the incident line divergence slit are sequentially arranged between the light source and the high-temperature measurement system, wherein the light path conversion module is used for converting a focused light path into a parallel light path, the first Soller slit is used for adjusting the divergence of incident light, and the incident line divergence slit is used for adjusting the spot area.

[0024] Preferably, the second light path assembly comprises: a scattering slit, a second Soller slit and an acceptance slit.

[0025] The scattering slit, the second Soller slit and the acceptance slit are sequentially arranged between the high-temperature measurement system and the detector.

[0026] Preferably, it further comprises: a goniometer.

[0027] Preferably, the high-temperature measurement system is provided with a temperature sensor, a cooling water channel and a gas channel.

[0028] The cooling water channel is used for cooling the high-temperature measurement system.

[0029] The gas channel is used for introducing protective gas into the high-temperature measurement system.

[0030] The temperature sensor is used for real-time detection of the temperature of the chemical vapor deposition reaction device.

[0031] From the above, the application discloses a chemical vapor deposition reaction device and a chemical vapor deposition X-ray diffraction in-situ detection device. The opening of the lower cover is arranged upwards, a through hole is arranged at the bottom of the lower cover, a cylinder is arranged in the lower cover, the upper end of the cylinder is arranged as a closed end, the lower end of the cylinder is communicated with the through hole, the lower end of the cylinder is matched with the sample table of the high-temperature measurement system, and the cavity surrounded by the cylinder and the lower cover is used for loading the precursor. The substrate sample pool used for loading the substrate is arranged on the upper end surface of the cylinder. The gasket is arranged on the upper end surface of the substrate sample pool. The lower end of the upper cover is connected with the lower cover, the upper cover is provided with a light transmission window, and the sealing window is sealingly arranged in the upper cover. Through the above disclosed chemical vapor deposition reaction device, the precursor can be volatilized and attached on the substrate to form a deposition layer under the high-temperature condition. Since the light transmission window is arranged in the upper cover, the X-ray diffraction can be used to detect the changes of the phase, size, stress, orientation and structure of the generated product in the chemical vapor deposition process in the chemical vapor deposition reaction device, so as to help the staff to establish the structure-activity relationship of the research system. BRIEF DESCRIPTION OF DRAWINGS

[0032] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only the embodiments of the present application, and for those skilled in the art, other drawings can also be obtained without creative labor on the basis of the provided drawings.

[0033] Figure 1 An exploded view of a chemical vapor deposition reaction device provided by the embodiment of the present application;

[0034] Figure 2 A top view of the lower cover provided by the embodiment of the present application;

[0035] Figure 3 A side view of the lower cover provided by the embodiment of the present application;

[0036] Figure 4 A structure schematic view of an X-ray diffraction in-situ detection device provided by the embodiment of the present application;

[0037] Figure 5 A structure schematic view of a high-temperature measurement system provided by the embodiment of the present application;

[0038] Figure 6 A powder X-ray diffraction spectrum of a chemical vapor deposition layer material at different temperatures provided by the embodiment of the present application.

[0039] The upper cover 1, the light-transmitting window 1-1, the sealing window 2, the gasket 3, the base sample pool 4, the groove 41, the convex piece 42, the lower cover 5, the barrel 51, the cavity 52, the light source 6, the light path conversion module 7, the first Soller slit 8, the incident line divergence slit 9, the goniometer 10, the high-temperature measuring system 12, the temperature sensor 111, the cooling water channel 112, the gas channel 113, the sample table 11, the chemical vapor deposition reaction device 13, the scattering slit 14, and the second Soller slit 15. DETAILED DESCRIPTION

[0040] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by a person of ordinary skill in the art without creative work fall within the protection scope of the present application.

[0041] In the present application, the terms "comprising", "containing" or any other variants thereof are intended to cover the non-exclusive inclusion, so that the process, method, article or equipment including a series of elements not only includes those elements, but also includes other elements not explicitly listed or inherent to such process, method, article or equipment. Without more limitations, the element defined by the statement "including a" does not exclude the presence of another identical element in the process, method, article or equipment including the element.

[0042] The embodiments of the present application provide a chemical vapor deposition reaction device, referring to Figures 1 to 3 , Figure 1 The chemical vapor deposition reaction device includes an upper cover 1, a sealing window 2, a gasket 3, a base sample pool 4 and a lower cover 5.

[0043] The lower cover 5 is upwardly open, a through hole is formed in the bottom of the lower cover 5, a barrel 51 is arranged in the lower cover 5, the upper end of the barrel 51 is a closed end, the lower end of the barrel 51 communicates with the through hole, and the cavity 52 surrounded by the barrel 51 and the lower cover 5 is used for loading a precursor;

[0044] The base sample pool 4 is arranged on the upper end surface of the barrel 51, and the base sample pool 4 is used for loading a substrate;

[0045] The gasket 3 is arranged on the upper end surface of the base sample pool 4;

[0046] The lower end of the upper cover 1 is connected with the lower cover 5, and the upper cover 1 is provided with a light-transmitting window 1-1;

[0047] The sealing window 2 is sealingly arranged in the upper cover 1.

[0048] It should be noted that by setting the barrel 51 in the lower cover 5, setting the upper end of the barrel 51 as a closed end, and setting the lower end of the barrel 51 in communication with the through hole at the lower end of the barrel 51, loading the precursor into the cavity 52 surrounded by the barrel 51 and the lower cover 5, and setting the substrate sample pool 4 for loading the substrate on the upper end surface of the barrel 51, the precursor can be attached to the substrate to form a deposition layer under the action of high temperature after volatilization.

[0049] It should be further noted that the precursor can be iron acetylacetone, or other metal or non-metal compounds that can volatilize under high temperature conditions; the substrate can be sodium chloride, or other materials that will not volatilize or decompose under high temperature conditions, and a person skilled in the art can select according to requirements.

[0050] The embodiment of the present application sets the opening of the lower cover 5 upward, sets a through hole at the bottom of the lower cover 5, sets the barrel 51 in the lower cover 5, sets the upper end of the barrel 51 as a closed end, sets the lower end of the barrel 51 in communication with the through hole, and sets the cavity 52 surrounded by the barrel 51 and the lower cover 5 for loading the precursor; the substrate sample pool 4 for loading the substrate is set on the upper end surface of the barrel 51; the gasket 3 is set on the upper end surface of the substrate sample pool 4; the lower end of the upper cover 1 is connected with the lower cover 5, the upper cover 1 is provided with a light transmission window 1-1; and the sealing window 2 is sealingly arranged in the upper cover 1. Through the above-mentioned chemical vapor deposition reaction device, the precursor can be attached to the substrate to form a deposition layer under high temperature conditions after volatilization. Since the light transmission window 1-1 is provided in the upper cover 1, the product phase, size, stress, orientation and structure changes in the chemical vapor deposition process in the chemical vapor deposition reaction device can be detected by X-ray diffraction, helping the staff to establish the structure-activity relationship of the research system.

[0051] Specifically, the lower part of the upper cover 1 is provided with an internal thread;

[0052] The upper part of the lower cover 5 is provided with an external thread matched with the internal thread.

[0053] It should be noted that by setting the internal thread in the lower part of the upper cover 1 and setting the external thread matched with the internal thread on the upper part of the lower cover 5, the staff can conveniently separate the upper cover 1 from the lower cover 5, thereby facilitating the staff to place the precursor and the substrate.

[0054] It should be further noted that the upper cover 1 and the lower cover 5 can be sealed by thread cooperation or buckle cooperation, and a person skilled in the art can select according to requirements.

[0055] Further, the sealing window 2 is made of graphite sheet;

[0056] The upper end surface of the substrate sample pool 4 is provided with a groove 41, and a plurality of protruding pieces 42 are arranged along the circumference of the groove 41.

[0057] It should be noted that the graphite sheet is a material with corrosion resistance, high temperature resistance and high X-ray transmittance. The sealing window 2 can be made of graphite sheet or aluminum foil. Those skilled in the art can choose according to the needs.

[0058] It should be further noted that since the sealing window 2 is made of graphite sheet, the sealing window 2 is easy to deform and adhere to the base sample pool 4, so that the precursor decomposition product cannot enter the base sample pool 4. By providing a plurality of protruding pieces 42 along the circumference of the groove 41, the protruding pieces 42 can support the sealing window 2, so that the sealing window 2 maintains a certain gap with the base sample pool 4. Thus, the precursor can adhere to the base through the gap between the sealing window 2 and the base sample pool 4 after volatilization.

[0059] Specifically, the groove 41 is a circular structure.

[0060] It should be noted that the groove 41 can be a circular structure or other types of structures. Those skilled in the art can choose according to the needs.

[0061] Further, the plurality of protruding pieces 42 are evenly arranged along the circumference of the groove 41.

[0062] It should be noted that the plurality of protruding pieces 42 are evenly arranged along the circumference of the groove 41, which can ensure that the sealing window 2 is uniformly stressed, and avoid local collapse of the sealing window 2 due to uneven stress.

[0063] Based on the above disclosed chemical vapor deposition reaction device, referring to Figure 4 and Figure 5 The embodiment of the present application also provides an X-ray diffraction in-situ detection device.

[0064] The X-ray diffraction in-situ detection device comprises a light source 6, a first light path assembly, a detector, a second light path assembly, a high temperature measurement system 12 and a chemical vapor deposition reaction device 13.

[0065] The first light path assembly is arranged between the light source 6 and the high temperature measurement system 12.

[0066] The second light path assembly is arranged between the high temperature measurement system 12 and the detector.

[0067] The chemical vapor deposition reaction device 13 is arranged on the sample table 11 of the high temperature measurement system 12.

[0068] The chemical vapor deposition reaction device 13 comprises an upper cover 1, a sealing window 2, a gasket 3, a base sample pool 4 and a lower cover 5.

[0069] The lower cover 5 is opened upward, a through hole is formed in the bottom of the lower cover 5, a cylinder 51 is arranged in the lower cover 5, the upper end of the cylinder 51 is a closed end, the lower end of the cylinder 51 is communicated with the through hole, and a cavity 52 surrounded by the cylinder 51 and the lower cover 5 is used for loading a precursor;

[0070] The base sample pool 4 is arranged on the upper end surface of the cylinder 51, and the base sample pool 4 is used for loading a base;

[0071] The gasket 3 is arranged on the upper end surface of the base sample pool 4;

[0072] The lower end of the upper cover 1 is connected with the lower cover 5, and the upper cover 1 is provided with a light transmission window 1-1;

[0073] The sealing window 2 is sealingly arranged in the upper cover 1.

[0074] It should be noted that the lower end of the cylinder 51 can cooperate with the sample table 11 of the high-temperature measurement system 12, so as to realize the fixation of the chemical vapor deposition reaction device 13.

[0075] In the embodiment of the application, the first light path assembly is arranged between the light source 6 and the high-temperature measurement system 12, the second light path assembly is arranged between the high-temperature measurement system 12 and the detector, and the chemical vapor deposition reaction device 13 is arranged on the sample table 11 of the high-temperature measurement system 12. Through the X-ray in-situ detection device disclosed above, the light source 6 can provide the required X-ray, the first light path assembly can adjust the X-ray emitted by the light source 6, and the adjusted X-ray can be shot into the high-temperature measurement system 12, and the detector can detect the changes of phase, size, orientation, stress and structure through the second light path assembly, so as to help the staff to establish the structure-activity relationship of the research system.

[0076] Specifically, the first light path assembly comprises a light path conversion module 7, a first Soller slit 8 and an incident line divergence slit 9.

[0077] The light path conversion module 7, the first Soller slit 8 and the incident line divergence slit 9 are sequentially arranged between the light source 6 and the high-temperature measurement system 12.

[0078] It should be noted that the light path conversion module 7 can convert the focused light path into a parallel light path, the first Soller slit 8 can adjust the incident light divergence of the parallel light path, and the incident line divergence slit 9 can adjust the spot area of the parallel light path. Through the light path conversion module 7, the first Soller slit 8 and the incident line divergence slit 9 disclosed above, the required light can be obtained.

[0079] Specifically, the second light path assembly comprises a scattering slit 14, a second Soller slit 15 and an acceptance slit.

[0080] The scattering slit 14, the second Soller slit 15 and the acceptance slit are sequentially arranged between the high-temperature measurement system 12 and the detector.

[0081] It should be noted that by providing the scattering slit 14, the second Solar slit 15 and the receiving slit, errors caused by radiation broadening and divergence can be reduced, and controlling the appropriate slit degree can improve the diffraction peak intensity, resolution and line shape.

[0082] Furthermore, the X-ray diffraction in-situ detection device further includes: a goniometer 10 for measuring the diffraction angle.

[0083] Specifically, the high temperature measurement system 12 is provided with a temperature sensor 111, a cooling water channel 112 and a gas channel 113;

[0084] The cooling water channel 112 is used to cool the high-temperature measurement system 12;

[0085] The gas channel 113 is used to supply protective gas to the high-temperature measurement system 12;

[0086] The temperature sensor 111 is used to detect the temperature of the chemical vapor deposition reaction device in real time.

[0087] It should be noted that by arranging a temperature sensor 111, a cooling water channel 112 and a gas channel 113 in the high-temperature measurement system 12, the high-temperature measurement system 12 can be cooled through the cooling water channel 112, and a protective gas can be introduced into the high-temperature measurement system 12 through the gas channel 113, and the temperature of the chemical vapor deposition reaction device can be detected in real time through the temperature sensor 111. When the temperature sensor 111 detects that the temperature in the high-temperature measurement system 12 is too high, the high-temperature measurement system 12 is cooled through the cooling water channel 112 so that the temperature in the high-temperature measurement system 12 is within the required temperature range, and the protective gas is introduced into the high-temperature measurement system 12 through the gas channel 113, which can prevent oxygen from entering the chemical vapor deposition reaction device and reacting with the deposition layer.

[0088] Based on the chemical vapor deposition X-ray diffraction in-situ detection device disclosed above, an embodiment of the present invention further provides a chemical vapor deposition X-ray diffraction in-situ detection method.

[0089] The chemical vapor deposition X-ray diffraction in-situ detection method includes the following steps:

[0090] 1. The matrix sample pool 4 is loaded with the matrix sample, and the precursor sample pool is loaded with the precursor sample.

[0091] 2. Place the matrix sample pool 4 on the protruding cylinder in the middle of the lower cover 5, put on the gasket 3, put on the sealing window 2, and cover the upper cover 1.

[0092] 3. Adjust the lower cover 5 so that the upper surface of the base is close to the upper surface of the upper cover 1.

[0093] 4. Put the in-situ detection device 13 loaded with samples on the sample stage 11 of the powder X-ray diffraction high temperature measurement system 12. Insert the sample stage 11 into the cylinder of the lower cover 5 of the chemical vapor deposition reaction device 13. Adjust the height of the sample stage 11 system to make the detection device in the appropriate position. The detection device can be freely moved and is very convenient to install on the existing powder X-ray diffractometer.

[0094] 5. By repeatedly adjusting the two degrees of freedom of Z axis and omega, the surface of the window is found and made parallel to the light path, and the chemical vapor deposition reaction device 13 can basically obtain an accurate test position.

[0095] 6. The X-ray diffraction light tube is raised to full power. Set the scanning parameters of the powder X-ray diffractometer, the 2theta range is 10-80 degrees, the scanning mode is set to theta-2theta, the step is 0.02 degrees, the scanning speed is 10 degrees per minute, and the X-ray diffraction data is collected through the one-dimensional detector zero-dimensional mode to obtain the diffraction spectrum of the sample.

[0096] 7. The X-ray diffractometer optimizes the diffraction intensity and position of the substrate and scans to find the diffraction peak of the substrate.

[0097] 8. Set the test temperature point, heating rate, and temperature retention time parameters, heat the chemical vapor deposition reaction device 13 to the set temperature through the diffraction instrument high temperature measurement system 12, collect in-situ X-ray diffraction data, and analyze the test data.

[0098] The present application has the following advantages:

[0099] 1. The present application combines the configuration of the existing target switching X-ray diffraction equipment (with high intensity light source 6, high speed detector, high temperature measurement system 11 HTK1200N temperature coverage range: room temperature ~ 1200℃) and does not need to modify the high temperature measurement system 12. By adding the chemical vapor deposition reaction device 13, an in-situ detection environment for chemical vapor deposition is constructed, and a new in-situ chemical vapor deposition reaction test system and method are developed.

[0100] 2. The in-situ environment of chemical vapor deposition of the present system can use the basic functions of high-power X-ray diffraction equipment to detect the deposition in-situ evolution process, dynamically detect the changes of product phase, size, orientation, stress and structure, etc., and plays a pioneering role.

[0101] 3. The present application introduces the X-ray diffraction parallel light measurement mode, reduces the influence of the height error of the measured sample position on the diffraction data, and is suitable for in-situ detection of deposited thin films.

[0102] 4. The chemical vapor deposition reaction device is directly inserted into the sample table 11 socket of the high temperature measurement system 12 through modular design, and can be conveniently calibrated by combining the functions of the X-ray diffractometer. In the parallel light mode of the X-ray diffractometer, the phase, size, orientation, stress and structure change of the research object are detected in real time, and the difficulty of the test is significantly reduced.

[0103] Specifically, the application also provides a method for in-situ real-time detection of chemical vapor deposition material structure by powder X-ray diffraction.

[0104] The method for in-situ real-time detection of chemical vapor deposition material structure by powder X-ray diffraction comprises the following steps:

[0105] 1. Turn on the diffractometer and increase the voltage and current to 45 kV and 200 mA respectively. Before X-ray diffraction, the light path needs to be adjusted in the horizontal and vertical directions, which is the same as the general diffractometer light adjustment and will not be described here.

[0106] 2. Adjust the light path to parallel light mode, and the detector uses zero-dimensional mode. Turn on the cooling water of the high temperature measurement system 12.

[0107] 3. Prepare the sample. Fill the precursor (acetylacetone iron) into the lower cover 5 precursor cavity, and put the substrate (sodium chloride) into the substrate sample pool 4. For example, the substrate is a block-shaped substrate with a size and thickness suitable for the design of the sample pool.

[0108] 4. Equip the chemical vapor deposition reaction device. Place the sample pool on the lower cover 5 cylinder, put the gasket 3, sealing window 2 (graphite), and screw into the upper cover 1, and then adjust the lower cover 5 so that the sample pool limiting protrusion tightly abuts the gasket 3.

[0109] 5. Take out the sample table 11 of the high temperature measurement system 12, and insert the chemical vapor deposition reaction device 13 into the sample table 11 without fixing. Put the sample table 11 back into the high temperature measurement system 12.

[0110] 6. Adjust the zero point height of the sample, lift the sample from bottom to top, perform Z scanning of the X-ray diffractometer, so that the count intensity of the X-ray is half of the original, and then adjust the inclination angle of the sample in the parallel X-ray direction to make the count intensity reach the maximum.

[0111] 7. Considering the X-ray diffraction intensity and resolution, determine the scanning step, speed, and divergence slit, scattering slit 14, and acceptance slit. Set appropriate test parameters on the X-ray diffraction operation software interface, set the scanning mode to theta-2theta, the step to 0.02 degrees, and the scanning speed to 10 degrees per minute. Set the test temperature point, temperature rising rate, temperature retention time and other parameters. The test parameters can be adjusted according to the actual data effect and requirements during the test process.

[0112] 8. Combined with the high temperature measurement system 12, the chemical vapor deposition reaction device 13 is heated. When the chemical vapor deposition layer material changes with the applied temperature, it is scanned at each temperature point to collect the diffraction data of the research material. The phase, lattice constant, orientation, stress and microstructure are analyzed based on the peak position, peak shape and peak intensity of the diffraction data. Figure 6 , Figure 6 The figure shows the powder X-ray diffraction spectra of chemical vapor deposition layer materials at different temperatures. The horizontal axis of the figure on the right is the 2Theta angle, and the vertical axis is the diffraction intensity. Real-time detection reveals changes in the material's microstructure.

[0113] Each embodiment in this specification is described in a progressive manner. The same or similar parts between the embodiments can be referred to each other. Each embodiment focuses on the differences from other embodiments. In particular, for system or system embodiments, since they are basically similar to method embodiments, the description is relatively simple. For relevant parts, refer to the partial description of the method embodiment. The system and system embodiments described above are merely schematic, wherein the units described as separate components may or may not be physically separated, and the components displayed as units may or may not be physical units, that is, they may be located in one place, or they may be distributed on multiple network units. Some or all of the modules can be selected according to actual needs to achieve the purpose of the solution of this embodiment. A person of ordinary skill in the art can understand and implement it without expending creative work.

[0114] Professionals may further appreciate that the units and algorithm steps of each example described in conjunction with the embodiments disclosed herein can be implemented in electronic hardware, computer software, or a combination of the two. In order to clearly illustrate the interchangeability of hardware and software, the above description has generally described the components and steps of each example according to their functions. Whether these functions are performed in hardware or software depends on the specific application and design constraints of the technical solution. Professionals and technicians may use different methods to implement the described functions for each specific application, but such implementation should not be considered beyond the scope of the present invention.

[0115] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A chemical vapor deposition reaction device, characterized in that: include: Upper cover, sealing window, gasket, matrix sample cell and lower cover; The lower cover is opened upward, a through hole is provided at the bottom of the lower cover, a cylinder is provided inside the lower cover, the upper end of the cylinder is a closed end, the lower end of the cylinder is connected to the through hole, and the cavity enclosed by the cylinder and the lower cover is used for loading the precursor; The matrix sample pool is arranged on the upper end surface of the cylinder, and the matrix sample pool is used to load the matrix; The gasket is arranged on the upper end surface of the matrix sample pool; The lower end of the upper cover is connected to the lower cover, and the upper cover is provided with a light-transmitting window, and the light-transmitting window is used to detect products produced during the chemical vapor deposition process using X-ray diffraction; The sealing window is sealed in the upper cover; The sealing window is made of graphite flakes; A groove is provided on the upper end surface of the matrix sample pool, and a plurality of protrusions are provided along the circumference of the groove.

2. The chemical vapor deposition reaction device according to claim 1, characterized in that: The lower part of the upper cover is provided with an internal thread; The upper portion of the lower cover is provided with an external thread that matches the internal thread.

3. The chemical vapor deposition reaction device according to claim 1, characterized in that: The groove is a circular structure.

4. The chemical vapor deposition reaction device according to claim 3, characterized in that: The plurality of protrusions are evenly arranged along the circumference of the groove.

5. An X-ray diffraction in-situ detection device, characterized in that: include: A light source, a first optical path component, a detector, a second optical path component, a high temperature measurement system, and a chemical vapor deposition reaction device according to any one of claims 1 to 4; The first optical path component is arranged between the light source and the high temperature measurement system; The second optical path component is arranged between the high temperature measurement system and the detector; The chemical vapor deposition reaction device is arranged on the sample stage of the high temperature measurement system.

6. The X-ray diffraction in-situ detection device according to claim 5, characterized in that: The first optical path component includes: an optical path conversion module, a first Soller slit and an incident ray divergence slit; The optical path conversion module, the first Soller slit, and the incident ray divergence slit are sequentially arranged between the light source and the high-temperature measurement system, wherein the optical path conversion module is used to convert the focused light path into a parallel light path, the first Soller slit is used to adjust the divergence of the incident light, and the incident ray divergence slit is used to adjust the spot area.

7. The X-ray diffraction in-situ detection device according to claim 5, characterized in that: The second optical path component includes: a scattering slit, a second Solar slit and a receiving slit; The scattering slit, the second Solar slit and the receiving slit are sequentially arranged between the high temperature measurement system and the detector.

8. The X-ray diffraction in-situ detection device according to claim 5, characterized in that: Also includes: Goniometer.

9. The X-ray diffraction in-situ detection device according to claim 5, characterized in that: The high temperature measurement system is provided with a temperature sensor, a cooling water channel and a gas channel; The cooling water channel is used to cool the high-temperature measurement system; The gas channel is used to introduce protective gas into the high-temperature measurement system; The temperature sensor is used to detect the temperature of the chemical vapor deposition reaction device in real time.

Images