In-situ high-temperature XRD reaction device

Abstract

The utility model discloses an in-situ high-temperature XRD (X-Ray Diffraction) reaction device which comprises an end cover and a main body, the end cover and the main body are enclosed and fixed to form a reaction cavity, and one end, horizontally extending into the reaction cavity along the axial direction of the main body, of the end cover is fixedly connected with a sample support. According to the utility model, the sample support is arranged on the end cover at the position coaxial with the main body in the axial direction, so that the sample support can horizontally enter the center of the reaction cavity, namely the zero point position of the XRD, the problem of secondary zero point adjustment is avoided, personal errors in the operation process are reduced, and the experiment efficiency is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to material structure performance integration in situ characterization technical field more specifically relates to in situ high temperature XRD reaction device. BACKGROUND

[0002] In-situ X-ray diffraction (In-situ XRD) technology as a universal technology for material microstructure analysis in the field of material science research has been widely used in recent years. At present, under the background of striving for "carbon peak and carbon neutral", the field of energy research has become the focus of researchers, and many researchers have devoted themselves to the field of battery electrode materials, CO2 catalytic reduction and other fields to carry out energy storage and catalysis research. In this process, in-situ XRD technology has become an important tool for studying the crystal structure transformation of materials and obtaining real-time information on material structure changes.

[0003] For the research and development of in-situ XRD devices, most of them are currently focused on the field of electrochemistry, such as patent documents with patent publication numbers CN217133006U, CN217385281U and CN215678176U, which focus on realizing in-situ characterization of battery electrode materials and real-time changes of battery materials during charging and discharging. This type of in-situ device cannot meet the needs of gas-solid heterogeneous catalysis. For related in-situ devices that can be applied to high-temperature catalytic research, there is further research and development space. Patent document CN114965524A discloses a compact high-temperature atmosphere in-situ XRD reaction cell, which has a circular groove-shaped sample table on the main body of the reaction cell. The sample table is filled with catalysts to be characterized by in-situ atmosphere XRD. However, according to the patent information, the maximum test upper limit of the temperature is 300℃, which obviously cannot meet the experimental needs in various high-temperature environments.

[0004] Based on the research of existing patent devices, there is room for improvement in sample placement methods and temperature measurement methods. UTILITY MODEL CONTENT

[0005] The technical problem to be solved by the utility model is how to improve the experimental efficiency.

[0006] The utility model solves the above technical problems through the following technical means: an in-situ high-temperature XRD reaction device, comprising an end cover and a main body, the end cover and the main body are fixed and enclosed to form a reaction cavity, and a sample holder is fixedly connected to one end of the end cover extending horizontally into the reaction cavity along the axis of the main body.

[0007] As a preferred technical solution, the main body is provided with a window around the circumference, and the window angle is 5°-160°.

[0008] As a preferred technical scheme, the end cover and the main body are both provided with water cooling cavities, the end cover is provided with water cooling joints three and four which are in communication with the water cooling cavity in the end cover, and the main body is provided with water cooling joints one and two which are in communication with the water cooling cavity in the main body.

[0009] As a preferred technical scheme, the reaction cavity is fixedly connected with a heat insulation layer, and the heat insulation layer is fixedly connected with a heating furnace.

[0010] As a preferred technical scheme, the main body is fixedly connected with a window through a window cover in the circumferential direction, the window cover is connected and fastened with the main body through a window fixing screw, and the connecting end of the window and the main body is further provided with a window sealing ring.

[0011] As a preferred technical scheme, the water cooling joints two, one, four and three are sequentially communicated, and the water cooling joints two and three are connected with an external cooling circulation system.

[0012] As a preferred technical scheme, the heat insulation layer comprises two heat insulation layers one and two which are in the form of half cylinders and oppositely arranged, one end of the heat insulation layer one is fixedly connected with the end cover, the other end is fixedly connected with the heat insulation layer two, and a gap is left between the heat insulation layer one and the heat insulation layer two.

[0013] As a preferred technical scheme, the heat insulation layer is fixedly connected with a heating furnace support on the inner wall, the heating furnace support is fixedly connected with heating furnaces one and two on the heating furnace support, a gap is left between the heating furnaces one and two, and a through hole is formed in the heat insulation layer and the heating furnaces.

[0014] As a preferred technical scheme, the end cover is further fixedly connected with a thermocouple at one end of the end cover which horizontally extends into the reaction cavity along the axial direction of the main body, and the thermocouple is located outside the sample holder.

[0015] As a preferred technical scheme, the end cover is further provided with an electrode interface, and the electrode interface is electrically connected with the heating furnace.

[0016] The utility model discloses the beneficial effect lies in:

[0017] (1) in the utility model, by setting the sample holder on the end cover and the main body axial coaxial position, make the sample holder can horizontally enter the center of the reaction cavity, namely XRD zero point position, avoid the problem of secondary adjustment zero point, reduce the human error in the operation process, improve the experimental efficiency.

[0018] (2) The utility model discloses, through the window angle is set to 5-160 DEG, make the device can realize 160 DEG big opening angle test, compared with traditional XRD equipment, this design has remarkable advantage in data acquisition and material analysis, big opening angle test can not only cover wider diffraction angle range, can also capture the microstructure information of sample under big angle, thereby provide more abundant crystallography data, for the research complex material, film and nanometer material etc. Field is especially important, can help researcher to understand material's phase change, crystal structure and phase composition.

[0019] (3) The utility model discloses, through being set in the center of reaction cavity in proper order heating furnace, heat -proof layer, forms annular heating field, can improve the uniformity of temperature heating. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 It is the front view structural schematic diagram provided for the utility model embodiment;

[0021] Figure 2 It is the side view structural schematic diagram provided for the utility model embodiment;

[0022] Figure 3 It is the cross section structural schematic diagram provided for the utility model embodiment;

[0023] Figure number: 1, main body;2, gas inlet;3, guide column;4, guide rod;5, electrode connector;6, water cooling connector one;7, water cooling connector two;8, gas outlet;9, base;10, window fixing screw;11, window;12, window cover;13, thermocouple;14, water cooling connector three;15, water cooling connector four;16, sample holder fixing screw;17, end cover;18, heat insulation layer one;19, end cover sealing ring;20, heating furnace one;21, sample support;22, heating furnace support;23, heating furnace two;24, sample area;25, heat insulation layer two;26, window sealing ring;27, sample holder. DETAILED DESCRIPTION

[0024] In order to make the purpose, technical scheme and advantage of the utility model embodiment more clear, the technical scheme in the utility model embodiment will be described clearly and completely below, obviously, the described embodiment is a part of the embodiment of the utility model, not all the embodiment. Based on the embodiment in the utility model, all other embodiments obtained by the ordinary skill in the art without making creative labor belong to the range of the utility model protection.

[0025] Reference Figure 1 , Figure 3, the in-situ high temperature XRD reaction device, including an end cover 17, a main body 1, a base 9, the end cover 17 and the main body 1 are fixedly enclosed at one end and form a sealed reaction cavity, the connecting end of the end cover 17 and the main body 1 is provided with an end cover sealing ring 19, the other end of the main body 1 is fixedly connected with the base 9, the end cover 17 is fixedly connected with a heat insulation layer one 18 at one end in the reaction cavity, the heat insulation layer one 18 is fixedly connected with a heat insulation layer two 25 through a screw, the thickness of the heat insulation layer one 18 and the heat insulation layer two 25 is greater than or equal to 30mm, the material can be selected from various porous materials or a barrel-shaped multilayer heat insulation layer structure designed by a metal thin layer, the heat insulation layer one 18 and the heat insulation layer two 25 are also fixedly connected with a heating furnace support 22, the heating furnace support 22 is fixedly connected with a heating furnace one 20 and a heating furnace two 23, the heating furnace one 20 and the heating furnace two 23 can be electric heating, the material can be selected from one or more combinations of heating resistance wire, Pt wire, W wire and other heating materials;

[0026] The end cover 17 is fixedly connected with a sample holder 27 through a sample holder fixing screw 16, the sample holder 27 is fixedly connected with a guide column 3, the guide column 3 is a hollow column structure, the end cover 17 is threadedly connected with a guide rod 4, the guide rod 4 can pass through the center through hole of the guide column 3, the sample holder 27 is fixedly connected with an air inlet 2, the air inlet 2 is located in the middle of the end cover 17, the main body 1 is also provided with an air outlet 8 located at the tail of the main body 1, so that the gas can fully pass through the sample and ensure the smoothness of the entire gas path, the end cover 17 is fixedly connected with a thermocouple 13, a sample holder 21 is fixedly connected with the sample holder 27, one end of the sample holder 21 extending into the heating furnace one 20 and the heating furnace two 23 is provided with a sample area 24, the sample area 24 is used for smearing or placing a sample, in the embodiment, the sample holder 21 horizontally enters the center of the reaction cavity along the axis direction of the reaction cavity, and is located in the central region of the heating furnace one 20 and the heating furnace two 23, so that the uniformity of temperature heating is improved, at the same time, after the end cover 17 and the main body 1 are connected and fastened, the sample holder 21 is just located at the horizontal position of the center of the reaction cavity, that is, the zero position of the XRD, so that the problem of secondary adjustment of the zero point is avoided, the thermocouple 13 is located below the sample area 24 of the reaction cavity, so that the accuracy of temperature measurement is improved, the sample can be quickly and accurately taken and placed, the human error in the operation process is reduced, at the same time, the problem of zero point calibration is effectively solved, the consistency and reliability of the test data are ensured every time, the experimental efficiency is improved, and the working strength of the researchers in the operation process is greatly reduced.

[0027] Referring to Figure 2 , Figure 3The circumference of the main body 1 is also fixedly connected with the window 11 through the window cover 12, the window cover 12 is fixedly connected with the main body 1 through the window fixing screw 10, so as to press the window 11 on the main body 1, the connecting end of the window 11 and the main body 1 is also provided with a window sealing ring 26, so that the reaction cavity can withstand a gas pressure condition of not higher than 2 atmospheres and a low vacuum environment, the window 11 can be selected from various materials with X-ray transmittance, including various polymer film materials such as kapton film, PEEK film, various light metals such as beryllium and carbon materials, etc., the angle of the window 11 is 5<2θ<160°, so that the device can realize a large opening angle test of 160°, compared with the traditional XRD equipment, this design has significant advantages in data acquisition and material analysis, the large opening angle test can not only cover a wider diffraction angle range, but also can capture the microstructure information of the sample at a large angle, so as to provide more abundant crystallographic data, which is particularly important for the research of complex materials, thin films and nanomaterials, etc., and can help researchers to deeply understand the phase transition, crystal structure and phase composition of the material.

[0028] Referring to Figure 2 , Figure 3 The main body 1 and the end cover 17 are both provided with a water cooling cavity, the water cooling cavity is connected with an external cooling water circulation system through a plurality of water cooling connectors, wherein the plurality of water cooling connectors are water cooling connector one 6, water cooling connector two 7, water cooling connector three 14 and water cooling connector four 15 in sequence, the water cooling connector four 15 and the water cooling connector three 14 are fixedly connected on the end cover 17, the water cooling connector two 7 and the water cooling connector one 6 are fixedly connected on the main body, the water cooling connector two 7, the water cooling connector one 6, the water cooling connector four 15 and the water cooling connector three 14 are communicated in sequence, wherein the water cooling connector two 7 and the water cooling connector three 14 form an input end and an output end respectively, the input end and the output end are connected with the external cooling water circulation system, and the external cooling water circulation system can be composed of an existing water pipe, a water pump and a valve, so as to cool the whole reaction cavity and avoid high temperature from causing harm to human body.

[0029] It should be noted that the window cover 12 is made of stainless steel, and the main body 1, the end cover 17, the air inlet 2, the air outlet 8, the water cooling connector one 6, the water cooling connector two 7, the water cooling connector three 14 and the water cooling connector four 15 are all made of stainless steel.

[0030] Referring to Figure 3The heating furnace in the embodiment adopts an environmental field heating arrangement, that is, the first heat insulation layer 18 and the second heat insulation layer 25 are in a semi-ring structure, and a gap is left between them. The heating furnace support 22 at the gap is in a cylinder structure. The first heat insulation layer 18 and the heating furnace 20 are provided with through holes for the thermocouple 13 and the sample holder 21 to extend into. The heating furnace 20 and the heating furnace 23 in the heating furnace support 22 are in a ring structure, which surrounds the sample holder 21. The device can realize a high temperature environment of up to 1400 degrees, and adopts an environmental field heating mode to ensure the uniformity of the temperature. This feature exhibits more excellent temperature control performance compared with the heating mode of the traditional XRD high temperature test equipment. The uniform temperature distribution not only avoids the physical change or chemical reaction of the sample due to local overheating, but also ensures the accuracy and repeatability of the test results. In addition, the test capability under the high temperature environment greatly expands the research range of materials, especially in the fields of metal materials, ceramic materials and high temperature superconducting materials, which can deeply study the phase behavior and structure evolution process of materials under high temperature conditions, promote the development and application of related materials, and improve the test efficiency and accuracy.

[0031] Referring to Figure 3 The end cover 17 is fixedly connected with the electrode connector 5. One end of the electrode connector 5 is connected with the heating furnace 20 and the heating furnace 23, and the other end is electrically connected with an external temperature control system for controlling the temperature and the heating rate and other parameters in the reaction chamber. The temperature control system is prior art and is not involved in improvement.

[0032] Method for use:

[0033] S1, install the device on the corresponding X-ray diffractometer to ensure that the center of the reaction chamber coincides with the zero position of the diffractometer;

[0034] S2. Move horizontally, pull out the sample holder 21, take out the sample holder 21, smear or place the sample on the sample area 24, and then insert the sample holder 21 back to the original position;

[0035] S3. If atmosphere protection or pressure application is performed, the valve at the gas inlet 2 needs to be closed first, then vacuum is performed through the gas outlet 8. When the vacuum value reaches the use requirement, the valve at the gas outlet 8 is closed, the valve at the gas inlet 2 is opened, and the pressure reaches the target value, then the valve at the gas inlet 2 is closed.

[0036] S4. If temperature parameters are applied, the cooling water circulation system can be opened first, and then the temperature control system is opened. At this time, the device starts to heat. At the same time, the spectrum acquisition function of the X-ray diffractometer can be started to synchronously acquire the XRD spectrum data of the sample under different temperature conditions.

[0037] The above examples are only used to illustrate the technical solutions of the present application, and are not intended to limit them; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that the technical solutions recorded in the foregoing examples can still be modified, or some technical features therein can be replaced by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. An in-situ high temperature XRD reaction apparatus characterized by, The utility model relates to a sample holder of reaction chamber, including end cover, main part, the end cover, main part enclose fixed and form a reaction cavity, the end cover is fixedly connected with sample holder along the horizontal extension of main part axial direction one end of reaction cavity, sample holder can enter the center of reaction cavity along the axial direction of reaction cavity, and the center of reaction cavity coincides with the zero position of diffractometer, and the main part is equipped with window circumference, and the angle of window is 5-160 DEG, and the fixed connection of heating furnace is set up in the reaction cavity of heat insulation layer, and the fixed connection of heating furnace is set up in the heat insulation layer, and the heat insulation layer includes two and is opposite and sets up heat insulation layer no.

2. The in-situ high temperature XRD reaction apparatus according to claim 1, characterized in that, The end cover, the main part are equipped with water cooling cavity, the end cover is equipped with water cooling joint three and water cooling joint four with the water cooling cavity in the end cover communication, the main part is equipped with water cooling joint one and water cooling joint two with the water cooling cavity in the main part communication.

3. The in-situ high temperature XRD reaction apparatus according to claim 1, characterized in that, The main part is fixedly connected with window circumference through window cover, and the window cover is connected with the main part fastening through window fixed screw, and the connecting end of window and main part is further equipped with window sealing ring.

4. The in-situ high-temperature XRD reaction apparatus according to claim 2, characterized by, Water cooling joint two, water cooling joint one, water cooling joint four, water cooling joint three are communicated in proper order, and water cooling joint two, water cooling joint three are connected with external cooling circulation system respectively.

5. The in-situ high-temperature XRD reaction apparatus according to claim 1, characterized in that, The gap is left between heating furnace one and heating furnace two, and the through -hole is set up on heat insulation layer and heating furnace.

6. The in-situ high-temperature XRD reaction apparatus according to claim 1, characterized in that, The end cover is further fixedly connected with thermocouple along the horizontal extension of main part axial direction one end of reaction cavity, and the thermocouple is located outside sample holder.

7. The in-situ high-temperature XRD reaction apparatus according to claim 1, characterized in that, The end cover is further equipped with electrode interface, and the electrode interface is electrically connected with heating furnace.

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