Extremely low temperature X-ray diffraction device

Abstract

The invention discloses an extremely low temperature X-ray diffraction device, and relates to the technical field of low temperature detection devices, the extremely low temperature X-ray diffraction device comprises a device main body, the device main body is divided into an X-ray diffraction zone and a low temperature control zone from top to bottom, and the extremely low temperature X-ray diffraction device also comprises: a sample chamber, which is located in the X-ray diffraction zone and is internally provided with a sample loading plate; the X-ray diffraction mechanism is located in the X-ray diffraction area, the X-ray diffraction mechanism comprises an X-ray generation unit and an X-ray receiving unit which are located on the two sides of the sample cavity, and an X-ray detector is integrated in the X-ray receiving unit; the temperature control mechanism comprises a low-temperature assembly and a high-temperature assembly, the low-temperature assembly is installed in the low-temperature control area, the conduction end of the low-temperature assembly is detachably connected with the bottom wall of the sample loading plate, and the high-temperature assembly is installed on the sample loading plate. And material crystal structure analysis at different temperatures from an extremely low temperature region to a high temperature region can be realized.

Description

Technical Field

[0001] The present invention relates to the technical field of low-temperature detection devices, and more particularly to an extremely low-temperature X-ray diffraction device. Background Art

[0002] As one of the important tools of modern scientific research, X-ray diffraction technology is widely used in many fields such as materials science, chemistry, physics and biology. Many materials show unique physical and chemical properties in extremely low temperature environments, which are difficult to observe at room temperature. The ultra-low temperature X-ray diffraction device can reveal the microstructure and lattice constant of materials in extremely low temperature environments, and is an important tool for studying the low-temperature properties of materials. By accurately measuring the lattice structure and atomic occupancy of polycrystalline, single crystal and thin film materials at low temperatures, we can gain a deep understanding of the physical and chemical properties of materials, thereby guiding the synthesis and application development of new materials.

[0003] At present, although low-temperature X-ray diffraction technology has made certain progress, the existing low-temperature X-ray diffraction devices still have some limitations; for example, the accuracy and measurement temperature range of the goniometer are limited, and cannot fully meet the needs of material research under extremely low temperature conditions; most of the existing low-temperature X-ray diffraction devices use liquid nitrogen refrigeration to achieve low-temperature X-ray diffraction analysis near the liquid nitrogen temperature. Although it has realized the characteristics of many materials in low-temperature environments to a certain extent, there are still certain limitations in the measurement temperature range. It can only perform low-temperature X-ray diffraction analysis within a specific low-temperature range, which cannot meet the needs of material research.

[0004] Therefore, how to provide an ultra-low temperature X-ray diffraction device that can be expanded to the ultra-low temperature region to achieve a wider temperature measurement range while improving control accuracy is an urgent problem that technicians in this field need to solve. Summary of the invention

[0005] In view of this, the present invention provides an ultra-low temperature X-ray diffraction device, aiming to solve the above technical problems.

[0006] In order to achieve the above object, the present invention adopts the following technical solution:

[0007] A very low temperature X-ray diffraction device, comprising a device body, wherein the device body is divided from top to bottom into an X-ray diffraction area and a low temperature control area, and further comprising:

[0008] A sample cavity, wherein the sample cavity is located in the X-ray diffraction area and a sample carrier is installed inside the sample cavity;

[0009] An X-ray diffraction mechanism, the X-ray diffraction mechanism is located in the X-ray diffraction area, the X-ray diffraction mechanism comprises an X-ray generating unit and an X-ray receiving unit located on both sides of the sample cavity, and an X-ray detector is integrated in the X-ray receiving unit;

[0010] The temperature control mechanism comprises a low-temperature component and a high-temperature component. The low-temperature component is installed in the low-temperature control area, and its conducting end is detachably connected to the bottom wall of the sample carrier. The high-temperature component is installed on the sample carrier.

[0011] Through the above technical scheme, the present invention provides an ultra-low temperature X-ray diffraction device, the main body of the device realizes the integration of X-ray diffraction experiment and ultra-low temperature control, the setting of the sample cavity allows the sample to be directly placed in the X-ray diffraction area for testing, and the installation of the sample carrier provides a support platform for the sample; through the cooperation of the low-temperature component and the high-temperature component, a wide temperature range measurement from the ultra-low temperature (4K) to the adjustable high temperature (1000K) zone can be achieved; combined with the X-ray diffraction mechanism, the crystal structure analysis of materials at different temperatures from the ultra-low temperature to the high temperature zone can be realized to meet the needs of material research.

[0012] Preferably, in the ultra-low temperature X-ray diffraction device provided above, an X-ray protection door is provided in the X-ray diffraction area to prevent X-rays from leaking to the external environment, thereby improving the safety of operation.

[0013] Preferably, in the extremely low temperature X-ray diffraction device provided above, the upper surface of the sample carrier is provided with an inwardly recessed sample slot, and the lower surface thereof is fixed with a slot, and the slot is detachably connected to the conductive end of the low temperature component. The sample slot is used to hold the powder sample to be tested, and the detachable connection between the slot and the conductive end of the low temperature component makes the connection more effective and convenient for replacement; at the same time, this structural arrangement enables the sample carrier to be heated at high temperature and cooled at extremely low temperature.

[0014] Preferably, in the ultra-low temperature X-ray diffraction device provided above, the low temperature control zone has a low temperature chamber, the low temperature chamber is located below the sample chamber, the low temperature assembly includes a compressor, a drive unit, a cold head transmission unit and a cold head conduction head; the compressor is located outside the device body, the drive unit is installed in the low temperature control zone, and is connected to the outlet of the compressor through a delivery pipeline, the cold head transmission unit is located in the low temperature chamber, and is transmission-connected to the drive unit, the cold head conduction head is installed at the end of the cold head transmission unit, and is plugged into the slot. Helium delivery and temperature control from the compressor to the cold head conduction head are realized, ensuring that the sample chamber can reach an ultra-low temperature state.

[0015] Preferably, in the ultra-low temperature X-ray diffraction device provided above, a reflux pipe is connected between the driving part and the inlet end of the compressor. By providing the reflux pipe, effective recovery and reuse of helium is achieved, the economy and environmental protection of the system are improved, and gas waste is reduced.

[0016] Preferably, in the ultra-low temperature X-ray diffraction device provided above, the X-ray diffraction mechanism further includes a power control unit and an X-ray tube, the power control unit is installed in the low temperature control area, and the X-ray tube is connected to the X-ray generating unit and electrically connected to the power control unit. The power control unit is a high-low voltage power supply unit, which provides the X-ray tube with the high voltage required to generate X-rays, so as to generate X-rays; through the setting of the power control unit and the X-ray tube, the precise control of the X-ray generating unit and the generation of X-rays are realized, and the stability and reliability of X-rays in the X-ray diffraction experiment are ensured.

[0017] Preferably, in the ultra-low temperature X-ray diffraction device provided above, the outer side of the sample carrier is provided with a protective cover, and a film window is provided on the protective cover, and the film window corresponds to the X-ray outgoing light path of the X-ray generating unit and the X-ray incident light path of the X-ray receiving unit. The design of the protective cover and the film window protects the sample from the influence of the external environment, while allowing the X-ray to pass smoothly. This design ensures the accuracy of the X-ray diffraction experiment and the safety of the sample.

[0018] Preferably, in the ultra-low temperature X-ray diffraction device provided above, a 2θ angle driving mechanism is further included, and the 2θ angle driving mechanism is used to adjust the angle of the X-ray generating unit and the X-ray receiving unit. The setting of the 2θ angle driving mechanism enables the angle of the X-ray generating unit and the receiving unit to be accurately adjusted, thereby realizing X-ray diffraction analysis of samples at different angles. This design improves the flexibility and accuracy of the experiment.

[0019] Preferably, in the ultra-low temperature X-ray diffraction device provided above, the high temperature component includes a mounting plate and a heating wire, the mounting plate is mounted inside the sample carrier, and the heating wire is arranged on the mounting plate. The sample carrier can achieve high temperature control, and the coordination with the low temperature component enables the device to adapt to X-ray diffraction experiments under wide temperature range conditions.

[0020] Preferably, in the ultra-low temperature X-ray diffraction device provided above, a thermocouple is installed on the sample carrier plate. The setting of the thermocouple enables the temperature of the sample carrier plate to be accurately monitored, thereby achieving accurate control of the sample temperature.

[0021] Preferably, in the above-mentioned ultra-low temperature X-ray diffraction device, a communication interface is provided on the sample chamber, and the communication interface is connected to a vacuum pump through a connecting pipe, so as to realize a vacuum environment of the sample chamber, which is very important for preventing the sample from being oxidized or frozen at an extremely low temperature, and also improves the accuracy of the X-ray diffraction experiment.

[0022] It can be seen from the above technical solutions that, compared with the prior art, the present invention discloses a very low temperature X-ray diffraction device, which has the following beneficial effects:

[0023] The present invention integrates an X-ray diffraction mechanism and a temperature control mechanism, and utilizes the scattering phenomenon caused by the interaction between X-rays and crystal materials to detect and record diffraction patterns at extremely low temperatures (such as liquid helium temperature) through a high-precision X-ray detector. These patterns carry information about the internal structure of the crystal, such as unit cell parameters, crystal symmetry, crystal defects, etc. Through the cooperation of the two, experiments can be carried out in a wide range from extremely low temperatures to high temperatures, and an extremely low-temperature low-temperature component can be combined with an X-ray diffraction mechanism to realize X-ray diffraction analysis of materials in an extremely low-temperature environment as low as 4K. In addition, with the assistance of a high-temperature component, variable-temperature X-ray diffraction analysis can be realized in a larger temperature range, providing flexibility for studying the properties of materials at different temperatures. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0025] Figure 1 The accompanying drawing is a schematic structural diagram of a very low temperature X-ray diffraction device provided by the present invention;

[0026] Figure 2 The accompanying drawing is a side view of the sample loading plate provided by the present invention;

[0027] Figure 3 The accompanying drawing is a top view of the sample loading plate provided by the present invention.

[0028] in:

[0029] 1-Device body;

[0030] 11-X-ray diffraction area; 12-low temperature control area; 13-low temperature chamber;

[0031] 2- Sample chamber;

[0032] 21-Connectivity interface;

[0033] 3- Sample loading board;

[0034] 31-sample slot; 32-slot; 33-protective cover; 34-thermocouple;

[0035] 4-X-ray diffraction mechanism;

[0036] 41-X-ray generating unit; 42-X-ray receiving unit; 43-X-ray detector; 44-power control unit; 45-X-ray tube;

[0037] 5- Low temperature components;

[0038] 51- compressor; 52- driving part; 53- cold head transmission part; 54- cold head conduction head; 55- delivery pipeline; 56- return pipeline;

[0039] 6-High temperature components;

[0040] 61-mounting plate; 62-heating wire;

[0041] 7-2θ angle drive mechanism;

[0042] 8-Control system. DETAILED DESCRIPTION

[0043] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0044] See attached Figure 1-3 The embodiment of the present invention discloses a very low temperature X-ray diffraction device, including a device body 1, the device body 1 is divided into an X-ray diffraction area 11 and a low temperature control area 12 from top to bottom, and also includes:

[0045] A sample chamber 2, the sample chamber 2 is located in the X-ray diffraction area 11, and a sample carrier plate 3 is installed inside the sample chamber 2;

[0046] An X-ray diffraction mechanism 4, the X-ray diffraction mechanism 4 is located in the X-ray diffraction area, the X-ray diffraction mechanism 4 comprises an X-ray generating unit 41 and an X-ray receiving unit 42 located on both sides of the sample cavity 2, and an X-ray detector 43 is integrated in the X-ray receiving unit 42;

[0047] The temperature control mechanism includes a low-temperature component 5 and a high-temperature component 6. The low-temperature component 5 is installed in the low-temperature control area 12, and its conducting end is detachably connected to the bottom wall of the sample carrier plate 3. The high-temperature component 6 is installed on the sample carrier plate 3.

[0048] In order to further optimize the above technical solution, an inwardly recessed sample groove 31 is provided on the upper surface of the sample carrier plate 3 , and a slot 32 is fixed on the lower surface thereof, and the slot 32 is detachably connected to the conducting end of the cryogenic component 5 .

[0049] In order to further optimize the above technical solution, the low-temperature control zone 12 has a low-temperature chamber 13, which is located below the sample chamber 2. The low-temperature component 5 includes a compressor 51, a driving unit 52, a cold head transmission unit 53 and a cold head conduction head 54; the compressor 51 is located on the outside of the device body, the driving unit 52 is installed in the low-temperature control zone 12, and is connected to the outlet of the compressor 51 through a conveying pipe 55, the cold head transmission unit 53 is located in the low-temperature chamber 13, and is transmission-connected to the driving unit 52, and the cold head conduction head 54 is installed at the end of the cold head transmission unit 53 and is plugged into the slot 32.

[0050] In order to further optimize the above technical solution, the cold head transmission part 53 is divided into a cold head primary piston 531 and a cold head secondary piston 532. Both the primary piston 531 and the cold head secondary piston 532 are round structures. The diameters of the cylinder and piston of the cold head primary piston 531 are relatively large, which can compress more helium and generate less pressure; while the diameters of the cylinder and piston of the cold head secondary piston 532 are small, and under the same motor output power, a greater pressure can be generated to further compress the helium; the driving part 52 drives the pistons of the cold head primary piston 531 and the cold head secondary piston 532 to reciprocate through a connecting rod to realize the reciprocating process of compressing and releasing helium; the structural settings and working principles of the cold head primary piston 531 and the cold head secondary piston 532 are all existing technologies, and reference can be made to patent number CN 117948731 A, and the patent name is ultra-low temperature refrigerator and operation method of ultra-low temperature refrigerator, which will not be repeated here.

[0051] In order to further optimize the above technical solution, a return pipe 56 is connected between the driving part 52 and the inlet end of the compressor 51 .

[0052] In order to further optimize the above technical solution, the X-ray diffraction mechanism 4 also includes a power control unit 44 and an X-ray tube 45. The power control unit 44 is installed in the low temperature control area. The X-ray tube 45 is connected to the X-ray generating unit 41 and is electrically connected to the power control unit 44.

[0053] In order to further optimize the above technical solution, a protective cover 33 is provided on the outer side of the sample carrier 3 , and a film window is opened on the protective cover 33 , which corresponds to the X-ray output light path 411 of the X-ray generating unit 41 and the X-ray incident light path 421 of the X-ray receiving unit 42 .

[0054] In order to further optimize the above technical solution, a 2θ angle driving mechanism 7 is also included. The 2θ angle driving mechanism 7 is used to adjust the angles of the X-ray generating unit 41 and the X-ray receiving unit 42.

[0055] In order to further optimize the above technical solution, a precision stepper motor and necessary control modules are integrated inside the 2θ angle driving mechanism 7. The stepper motor can drive the X-ray generating unit 41 to rotate clockwise and the X-ray receiving unit 42 to rotate counterclockwise synchronously through the instructions given by the control module; a θ angle scan can be achieved at one end, and a 2θ angle scan can be achieved synchronously at both ends, which can achieve high-precision angle control and improve the accuracy of the measurement results.

[0056] In order to further optimize the above technical solution, the high temperature component 6 includes a mounting plate 61 and a heating wire 62 . The mounting plate 61 is installed inside the sample carrier plate 3 , and the heating wire 62 is arranged on the mounting plate 61 .

[0057] In order to further optimize the above technical solution, a thermocouple 34 is installed on the sample carrier 3.

[0058] In order to further optimize the above technical solution, a communication interface 21 is provided on the sample chamber 2, and the communication interface 21 is connected to the vacuum pump through a connecting pipe.

[0059] In order to further optimize the above technical solution, a control system 8 is also included. The control system 8 is used to control the operation of the above components and to coordinate and control them to ensure the accuracy and synchronization of the generation, diffraction and detection processes of X-rays, while achieving coordinated control of high and low temperatures; and can adjust the operating speed, temperature and other parameters of each component in real time according to information such as the monitoring results of the components.

[0060] The working process of the present invention is:

[0061] Temperature control link:

[0062] The powder sample to be tested is spread flat on the sample slot 31 of the sample carrier 3 according to the general requirements of material X-ray diffraction analysis; the sample can be heated to above 1000K by the resistive heating of the heating wire 62 according to the design requirements; the slot 32 at the bottom of the sample carrier 3 is plugged into the cold head conductive head 54, where the lowest temperature can reach 4K; the compressor 51 compresses the helium and transports it to the drive unit 52 through the delivery pipe 55. Under the drive of the drive unit 52, the first-stage piston 531 of the cold head is driven to further compress the helium, and the helium passes through the second-stage piston 532 of the cold head. After further compressing the helium, the liquid helium temperature of 4K can be achieved at the end of the cold head secondary piston (15), and the extremely low temperature can be transmitted to the sample carrier 3 through the cold head conduction head 54; according to the experimental needs, the control system 8 can detect the experimental temperature information through the thermocouple 34, and then coordinately control the heating wire 62 and the compressor 51 to achieve the target temperature; in this process, the sample chamber 2 can be evacuated to a vacuum state through the connecting structure 21 by a vacuum pump to prevent the sample from being oxidized at high temperature or to prevent the sample chamber 2 from freezing in an extremely low temperature environment.

[0063] X-ray diffraction process:

[0064] The power control unit 44 can provide the X-ray tube 45 with the high voltage required to generate X-rays, so as to generate X-rays. After the X-ray output light path 411 of the X-ray generating unit enters through the film window, passes through the protective cover 33 and is shot to the powder sample to be tested, X-ray diffraction occurs. After the diffracted X-ray passes through the film window, it enters the X-ray receiving unit through the X-ray incident light path and is finally received by the X-ray detector. The X-ray detector is used to detect and measure the intensity of the diffracted X-rays, analyze the sample diffraction spectrum, and determine the crystal structure and other information; the control system 8 controls the 2θ angle driving mechanism 7 to realize the synchronous rotation of the X-ray generating unit 41 and the X-ray receiving unit 42, and finally realizes the collection of the sample diffraction X-ray intensity and 2θ angle information.

[0065] The control system 8 integrates the above temperature information and the X-ray diffraction information of the sample at the corresponding temperature, and can realize the X-ray diffraction of materials at different temperatures, especially the X-ray diffraction of materials at extremely low temperatures (4K).

[0066] The device combines extremely low-temperature components with X-ray diffraction mechanisms, enabling X-ray diffraction analysis of materials in extremely low-temperature environments as low as 4K. Assisted by high-temperature components, variable-temperature X-ray diffraction analysis can be achieved in a larger temperature range.

[0067] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0068] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be 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 will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A cryogenic X-ray diffraction device, comprising a device body (1), wherein the device body (1) is divided from top to bottom into an X-ray diffraction area (11) and a cryogenic control area (12), characterized in that: Also includes: A sample chamber (2), the sample chamber (2) being located in the X-ray diffraction area (11) and having a sample carrier plate (3) installed therein; An X-ray diffraction mechanism (4), the X-ray diffraction mechanism (4) being located in the X-ray diffraction area, the X-ray diffraction mechanism (4) comprising an X-ray generating unit (41) and an X-ray receiving unit (42) located on both sides of the sample cavity (2), and an X-ray detector (43) being integrated inside the X-ray receiving unit (42); A temperature control mechanism, the temperature control mechanism comprising a low-temperature component (5) and a high-temperature component (6), the low-temperature component (5) being installed in the low-temperature control area (12), and its conducting end being detachably connected to the bottom wall of the sample carrier (3), and the high-temperature component (6) being installed on the sample carrier (3).

2. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: The upper surface of the sample carrier plate (3) is provided with an inwardly recessed sample groove (31), and the lower surface thereof is fixed with a slot (32), and the slot (32) is detachably connected to the conduction end of the low-temperature component (5).

3. The ultra-low temperature X-ray diffraction device according to claim 2, characterized in that: The low temperature control zone (12) has a low temperature chamber (13), and the low temperature chamber (13) is located below the sample chamber (2). The low temperature component (5) includes a compressor (51), a driving unit (52), a cold head transmission unit (53) and a cold head conduction head (54); the compressor (51) is located outside the device body, the driving unit (52) is installed in the low temperature control zone (12), and is connected to the outlet of the compressor (51) through a delivery pipeline (55), the cold head transmission unit (53) is located in the low temperature chamber (13), and is transmission-connected to the driving unit (52), and the cold head conduction head (54) is installed at the end of the cold head transmission unit (53) and is plugged into the slot (32).

4. The ultra-low temperature X-ray diffraction device according to claim 3, characterized in that: A return pipe (56) is connected between the driving unit (52) and the inlet end of the compressor (51).

5. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: The X-ray diffraction mechanism (4) further comprises a power control unit (44) and an X-ray tube (45), wherein the power control unit (44) is installed in the low temperature control area, and the X-ray tube (45) is communicated with the X-ray generating unit (41) and is electrically connected to the power control unit (44).

6. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: The outer side of the sample carrier (3) is provided with a protective cover (33), and a film window is opened on the protective cover (33), and the film window corresponds to the X-ray output light path (411) of the X-ray generating unit (41) and the X-ray incident light path (421) of the X-ray receiving unit (42).

7. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: It also comprises a 2θ angle driving mechanism (7), wherein the 2θ angle driving mechanism (7) is used to adjust the angles of the X-ray generating unit (41) and the X-ray receiving unit (42).

8. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: The high-temperature component (6) comprises a mounting plate (61) and a heating wire (62); the mounting plate (61) is mounted inside the sample carrier plate (3); and the heating wire (62) is arranged on the mounting plate (61).

9. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: A thermocouple (34) is installed on the sample carrier (3).

10. The ultra-low temperature X-ray diffraction device according to claim 1, characterized in that: The sample chamber (2) is provided with a communication interface (21), and the communication interface (21) is connected to a vacuum pump via a connecting pipe.

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