In-situ temperature changing assembly based on X-ray diffractometer

Abstract

The utility model discloses an in-situ temperature changing assembly based on an X-ray diffractometer, and relates to the technical field of diffractometer accessories, the in-situ temperature changing assembly comprises a heating sleeve, a heating part, an X-ray transmission window and a diffraction grating, one end of the heating sleeve is closed, and the other end of the heating sleeve is open and is detachably connected with an angle measuring part of the X-ray diffractometer; the interior of the heating sleeve is hollow, the heating sleeve is in a cavity state and is in a negative pressure environment during working, heating parts are evenly distributed in the heating sleeve, an X-ray penetrating window is arranged on the cavity wall of the heating sleeve in a sealed mode, and the diffraction grating is arranged below the X-ray penetrating window. Incident rays and sample diffraction rays can penetrate through the X-ray penetrating window and the diffraction grating to irradiate a sample. The heating assembly can be detachably connected to the position of the diffractometer goniometer and the position of the sample frame in a direct buckling mode, samples are convenient to replace, heating parts are evenly distributed, and it is guaranteed that the samples are evenly heated.

Description

Technical Field

[0001] This utility model relates to the technical field of diffractometer accessories, and in particular to an in-situ temperature-changing component based on an X-ray diffractometer. Background Technology

[0002] Currently, some commercially available X-ray diffractometers, both domestically and internationally, are equipped with high-temperature accessories for determining the structure of materials under high-temperature conditions. Most solid materials possess stable crystal structures, with sizes typically ranging from one-tenth to one-hundredth of a nanometer, comparable to the wavelength of X-rays. Specific crystal structures enable diffraction of incident rays at suitable wavelengths; by recording these diffraction fringes, we can obtain rich information about the crystal structure. Existing X-ray diffractometers are based on this principle, automatically measuring crystal structure information. Temperature changes affect the microstructure of materials; therefore, recording the crystal structure information of materials under a set temperature environment is of great significance for research in materials science, chemistry, and physics.

[0003] To address this, X-ray diffractometer manufacturers have designed their own in-situ variable-temperature measurement accessories. Current high-temperature accessories are mostly box-shaped, but due to their large size and the exposed resistance wire in the center, the sample can only be placed on the heating element, with one side in contact with it for heating or cooling, resulting in uneven sample heating. Furthermore, the sample holder needs to be moved with the high-temperature accessory during use, but these accessories are bulky, lack flexibility, are difficult to install and disassemble, have complex operation procedures, and are prone to malfunction. Utility Model Content

[0004] The purpose of this invention is to provide an in-situ variable temperature component based on an X-ray diffractometer to solve the problems existing in the prior art, making sample heating operation of the X-ray diffractometer easy and uniform, and the component convenient to disassemble and move.

[0005] To achieve the above objectives, this utility model provides the following solution:

[0006] This invention provides an in-situ temperature-controlled component based on an X-ray diffractometer, comprising a heating sleeve, heating elements, an X-ray transmission window, and a diffraction grating. One end of the heating sleeve is closed, and the other end is open and detachably connected to the angle measuring part of the X-ray diffractometer. The interior of the heating sleeve is hollow and under negative pressure during use. Heating elements are evenly distributed inside the heating sleeve. The X-ray transmission window is sealed on the cavity wall of the heating sleeve. The diffraction grating is located below the X-ray transmission window. Both incident X-rays and sample diffracted X-rays can pass through the X-ray transmission window and the diffraction grating to irradiate the sample.

[0007] Preferably, the heating sleeve includes an outer sleeve and an inner sleeve, the inner sleeve is fitted inside the outer sleeve and its ends are flush, and the X-ray transmission window is provided at the same position on both the outer sleeve and the inner sleeve.

[0008] Preferably, the X-ray transmission window of the outer sleeve is a polyimide film, which is connected to the opening of the heating sleeve cavity wall by a pressure plate and bolts.

[0009] Preferably, the X-ray transmission window of the inner sleeve is sealed with transparent glass.

[0010] Preferably, the outer sleeve is made of metal.

[0011] Preferably, the inner sleeve is made of high-temperature resistant ceramic, and the outer wall of the inner sleeve is coated with a high-temperature resistant heat insulation coating.

[0012] Preferably, the heating element is a heating wire, which is spirally wound at equal intervals on the inner wall of the inner sleeve, and the heating wire is wound along the length of the heating sleeve. Both ends of the heating wire pass through the cavity wall of the heating sleeve, and the outer wall of the heating sleeve is provided with a power-connecting interface for connecting to a power source.

[0013] Preferably, the heating wire is made of nickel-chromium alloy, a temperature sensor is installed inside the inner sleeve, the heating wire is connected to a temperature controller, and the temperature sensor is communicatively connected to the temperature controller.

[0014] Preferably, the closed end of the heating sleeve is bolted to a transparent observation window. The observation window is circular and has air holes that can be connected to a pipe for vacuuming.

[0015] Preferably, the open end of the heating sleeve is sealed to the angle measuring part of the X-ray diffractometer via a flange and bolts.

[0016] The present invention achieves the following technical advantages over the prior art:

[0017] The heating component of this invention can be detachably connected to the diffractometer, goniometer, and sample holder via a direct snap-fit ​​method, which facilitates sample replacement. Furthermore, the evenly distributed heating components ensure uniform heating of the sample. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the internal structure of the in-situ temperature-changing component based on an X-ray diffractometer in an embodiment of this utility model;

[0020] Figure 2 This is a schematic diagram of the assembly structure of the in-situ temperature-changing component based on an X-ray diffractometer in an embodiment of this utility model.

[0021] Figure 3 This is a schematic diagram of the external structure of the in-situ temperature-changing component based on an X-ray diffractometer in an embodiment of this utility model. Figure 1 ;

[0022] Figure 4 This is a schematic diagram of the external structure of the in-situ temperature-changing component based on an X-ray diffractometer in an embodiment of this utility model. Figure 2 ;

[0023] Figure 5 This is a schematic diagram of the external structure of the in-situ temperature-changing component based on an X-ray diffractometer in an embodiment of this utility model. Figure 3 ;

[0024] In the figure: 1-X-ray transmission window, 2-inner sleeve, 3-thermal insulation coating, 4-observation window, 5-heating wire, 6-diffraction grating, 7-temperature sensor, 8-outer sleeve, 9-pore, 10-polyimide film, 11-X-ray diffractometer, 12-sample holder, 13-bolt, 14-glass, 15-power connector. Detailed Implementation

[0025] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0026] The purpose of this invention is to provide an in-situ variable temperature component based on an X-ray diffractometer to solve the problems existing in the prior art, making sample heating operation of the X-ray diffractometer easy and uniform, and the component convenient to disassemble and move.

[0027] To make the above-mentioned objectives, features and advantages of this utility model more apparent and understandable, the utility model will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0028] Example 1

[0029] like Figures 1 to 5As shown, this embodiment provides an in-situ variable temperature assembly based on an X-ray diffractometer, including a heating sleeve, heating components, an X-ray transmission window 1, and a diffraction grating 6. One end of the heating sleeve is closed, and the other end is open and detachably connected to the angle measuring part of the X-ray diffractometer 11. The interior of the heating sleeve is hollow and under negative pressure during use. Heating components are evenly distributed inside the heating sleeve. The X-ray transmission window 1 is sealed on the cavity wall of the heating sleeve. The diffraction grating 6 is located below the X-ray transmission window 1, allowing both incident X-rays and sample diffracted X-rays to pass through the X-ray transmission window 1 and the diffraction grating 6 to irradiate the sample. The sample holder 12 of the X-ray diffractometer 11 extends into the middle of the heating sleeve. The sample holder 12 is independent of the heating sleeve, thus eliminating the cumbersome operation when changing samples.

[0030] As an optional solution, in this embodiment, the heating sleeve includes an outer sleeve 8 and an inner sleeve 2. The inner sleeve 2 is fitted inside the outer sleeve 8 and its ends are flush. An X-ray transmission window 1 is provided at the same position on both the outer sleeve 8 and the inner sleeve 2.

[0031] As an optional solution, in this embodiment, the X-ray transmission window 1 of the outer sleeve 8 is a polyimide film 10 (Kapton film), and the polyimide film 10 is connected to the opening in the cavity wall of the heating sleeve by a pressure plate and bolts 13. In this embodiment, the opening on the heating sleeve, the polyimide film 10, and the pressure plate are all arc-shaped and connected by bolts 13, which allows for easy replacement of the polyimide film 10.

[0032] As an optional solution, in this embodiment, a transparent glass 14 is sealed to the X-ray transmission window 1 of the inner sleeve 2, which ensures the airtightness of the inner sleeve 2 while allowing X-rays to pass through.

[0033] As an optional solution, in this embodiment, the outer sleeve 8 is made of metal, preferably stainless steel, which has excellent corrosion resistance and mechanical strength, and can remain stable in high temperature and vacuum environments, ensuring the overall reliability and durability of the system; the properties of stainless steel enable it to effectively resist the influence of external temperature changes on the internal environment of the component cavity, ensuring the accuracy of the measurement.

[0034] As an optional solution, in this embodiment, the inner sleeve 2 is made of high-temperature resistant ceramic, and the outer wall of the inner sleeve 2 is coated with a high-temperature resistant heat-insulating coating 3. By selecting the method of applying a high-temperature resistant heat-insulating coating to form a ceramic heat-insulating coating, heat loss and heat conduction are effectively prevented, thereby maintaining a stable internal temperature and preventing heat from the vacuum cavity from being transferred to the outside of the cavity, thus affecting the internal ambient temperature of the diffractometer.

[0035] As an optional solution, in this embodiment, the heating component is a heating wire 5. The heating wire 5 is spirally wound at equal intervals around the inner wall of the inner sleeve 2, and the heating wire 5 is wound along the length of the heating sleeve, thus maximizing the length of the heating wire 5 and ensuring sufficient and uniform heating. Both ends of the heating wire 5 pass through the cavity wall of the heating sleeve, and a power-connecting interface 15 is provided on the outer wall of the heating sleeve for connection to a power source. The heating wire 5 is a resistance wire, connected to the inner wall of the heating sleeve by bolts 13 using quenched screws, tightly fitting against the inner wall of the heating sleeve to effectively transfer heat to the sample inside the cavity. The heating sleeve is non-conductive, but the threaded connection of the heating wire 5 can effectively transfer current, ensuring its normal heating function. This connection method not only ensures the stability of the heating wire 5 but also ensures safety and effectiveness in a vacuum environment.

[0036] As an optional solution, the heating wire 5 in this embodiment is made of nickel-chromium alloy. Nickel-chromium alloy has a high melting point, good oxidation resistance, and excellent corrosion resistance. The nickel-chromium alloy heating wire 5 is suitable for high-temperature heating and can be used for a long time. A temperature sensor 7 is installed inside the inner sleeve 2, and the heating wire 5 is connected to a temperature controller. The temperature sensor 7 and the temperature controller are communicatively connected. In this embodiment, the heating temperature is uniform and continuously controllable. The communication connection between the temperature sensor 7 and the temperature controller ensures that the heating temperature is uniform and continuously controllable. The temperature sensor 7 is preferably located near the sample area near the heating wire 5 to monitor the sample surface temperature in real time and to achieve precise control through the temperature controller. The coil of the heating element is in contact with the inner wall of the heating sleeve, and the heating wire 5 is located near the sample stage, which can greatly save space and make the sample more evenly heated.

[0037] As an alternative, in this embodiment, the legs of the diffraction grating 6 are connected to the cavity wall of the inner sleeve 2 by bolts 13.

[0038] As an optional solution, in this embodiment, the closed end of the heating sleeve is connected to a transparent observation window 4 via bolt 13. The observation window 4 is circular and has an air vent 9 and a temperature sensor 7. The air vent 9 can be connected to a vacuum pump via a pipeline. In this embodiment, the observation window 4 can be made of high-strength and high-temperature resistant glass to ensure pressure and heat resistance in a vacuum environment, maintaining good visibility while withstanding a certain amount of external pressure. To ensure the sealing of the heating sleeve, a dedicated sealing gasket is placed between the observation window 4 and the cavity, typically made of silicone or polytetrafluoroethylene (PTFE). These materials have excellent sealing performance and high-temperature resistance, effectively preventing vacuum leakage. Furthermore, the bolt 13 connection design provides stable clamping force, further enhancing the sealing effect, thereby ensuring the normal operation of the heating sleeve and the accuracy of experimental data.

[0039] As an optional solution, in this embodiment, the open end of the heating sleeve is sealed to the angle measuring part of the X-ray diffractometer 11 via a flange and bolts 13. This embodiment is designed as an independent accessory, which can be detachably connected to the X-ray diffractometer 11, making it very easy to disassemble and assemble without removing the sample holder 12 of the X-ray diffractometer 11.

[0040] Example 2

[0041] This embodiment provides a method for using an in-situ temperature-changing component based on an X-ray diffractometer, the specific operation of which is as follows:

[0042] As an optional approach, the sample to be tested is placed on the sample stage inside the heating sleeve, ensuring the sample is securely fixed. Then, a vacuum pump is connected to the air inlet of the heating sleeve, and the pump is started to evacuate the sample, aiming for a vacuum level of 10. -3 Up to 10 -5 To ensure a low-pressure environment and avoid gas interference with the measurement results, a heating element 5 is properly connected to the power supply, and the target heating temperature is set according to experimental requirements, typically within the range of room temperature to 400°C. During heating, the temperature sensor 7 monitors the surface temperature of the sample (or vicinity) in real time and transmits the data to the temperature controller to ensure uniform heating of the sample. At the required temperature, X-ray diffractometer 11 is used to acquire data and record the diffraction pattern of the sample. The experimental time depends on the sample properties and measurement requirements. After the experiment, the heating element is turned off, and the heating sleeve is gradually cooled to room temperature. After ensuring that the pressure inside the chamber returns to normal, the vacuum pump is turned off. Once the pressure returns to atmospheric pressure, the observation window 4 is opened to remove the sample for subsequent analysis. These steps ensure the safety and accuracy of the experiment, providing a reliable data basis for studying the crystal structure changes of the sample at different temperatures.

[0043] This utility model uses specific examples to illustrate its principles and implementation methods. The above description of the embodiments is only for the purpose of helping to understand the method and core idea of ​​this utility model. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the idea of ​​this utility model. In summary, the content of this specification should not be construed as a limitation of this utility model.

Claims

1. An in-situ variable temperature component based on an X-ray diffractometer, characterized in that: The device includes a heating sleeve, heating elements, an X-ray transmission window, and a diffraction grating. One end of the heating sleeve is closed, and the other end is open and detachably connected to the angle measuring part of the X-ray diffractometer. The interior of the heating sleeve is hollow and under negative pressure during use. Heating elements are evenly distributed inside the heating sleeve. The X-ray transmission window is sealed on the cavity wall of the heating sleeve. The diffraction grating is located below the X-ray transmission window. Both incident X-rays and sample diffracted X-rays can pass through the X-ray transmission window and the diffraction grating to irradiate the sample.

2. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 1, characterized in that: The heating sleeve includes an outer sleeve and an inner sleeve. The inner sleeve is fitted inside the outer sleeve and its ends are flush. The X-ray transmission window is provided at the same position on both the outer sleeve and the inner sleeve.

3. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 2, characterized in that: The X-ray transmission window of the outer sleeve is a polyimide film, which is connected to the opening of the heating sleeve cavity wall by a pressure plate and bolts.

4. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 2, characterized in that: The inner sleeve's X-ray transmission window is sealed with transparent glass.

5. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 2, characterized in that: The outer sleeve is made of metal.

6. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 2, characterized in that: The inner sleeve is made of high-temperature resistant ceramic, and the outer wall of the inner sleeve is coated with a high-temperature resistant heat insulation coating.

7. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 6, characterized in that: The heating element is a heating wire, which is spirally wound at equal intervals on the inner wall of the inner sleeve and wound along the length of the heating sleeve. Both ends of the heating wire pass through the cavity wall of the heating sleeve, and a power-connecting interface for connecting to a power source is provided on the outer wall of the heating sleeve.

8. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 7, characterized in that: The heating wire is made of nickel-chromium alloy. A temperature sensor is installed inside the inner sleeve. The heating wire is connected to a temperature controller. The temperature sensor and the temperature controller are in communication connection.

9. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 1, characterized in that: The closed end of the heating sleeve is connected by bolts to a transparent observation window. The observation window is circular and has air holes that can be connected to a pipe for vacuuming.

10. The in-situ variable temperature assembly based on an X-ray diffractometer according to claim 1, characterized in that: The open end of the heating sleeve is sealed to the angle measuring part of the X-ray diffractometer via a flange and bolts.

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