Low-temperature temperature control device for liquid large-angle X-ray scattering

Abstract

The utility model provides a low-temperature temperature control device for liquid large-angle X-ray scattering, the low-temperature temperature control device comprises a heat preservation cavity, a semiconductor chilling plate, a sample carrying table and a radiator, the heat preservation cavity is provided with an X-ray transmission window, the semiconductor chilling plate is located in the heat preservation cavity, and the sample carrying table is located in the heat preservation cavity. The sample carrying table is located in the heat preservation cavity and arranged at the top end of the semiconductor chilling plate, the sample carrying table is aligned with the X-ray transmission window, and the radiator is arranged at the bottom end of the semiconductor chilling plate. The low-temperature temperature control device is simple in overall equipment structure and convenient to move and carry.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of temperature control equipment, and in particular relates to a low-temperature temperature control device for liquid wide-angle X-ray scattering. BACKGROUND

[0002] The long-range ordered periodic structure of crystals has been studied for a hundred years, and both theory and experiment have been mature. However, the mother liquor structure of the crystals has been neglected for a long time and has become a blind spot in modern science. The mother liquor structure is often inherited by the offspring crystals and determines the purity, size and morphology of the precipitated crystals, thereby further affecting the purity and particle size of the product. Some discoveries of the mother liquor structure may directly lead to the invention of high technology in some chemical processes. Many developed countries abroad have listed the solution structure research as a key research field in the 21st century, which is a frontier subject with great knowledge innovation value and broad application prospect. The X-ray scattering method of liquid structure is an important experimental method for directly obtaining structural information. It can not only measure the bond length, coordination number, bond angle and spatial configuration of the first coordination layer, but also obtain the structural information outside the first coordination layer. At present, the main experimental methods of wide-angle X-ray scattering include flat sample cell reflection method and capillary transmission method. Among them, the flat sample cell reflection scattering data correction is simple, and the corresponding device is developed by the skilled in the art to realize the structure test of high-temperature molten salt, but the experimental data of the flat sample cell reflection method is easily affected by the liquid surface, and the data reproducibility is poor. In recent years, more research work has been carried out around the flat sample cell scattering. At present, most of the experimental researches on solutions are carried out at room temperature. The range from negative tens of degrees to positive tens of degrees is closely related to the solution and the electrolyte of the battery and the actual chemical process. Due to the imperfect temperature control condition, there are few experimental research reports on this temperature range which is most concerned about the solution structure research. Although some synchrotron radiation centers have extreme low temperature (liquid nitrogen, liquid helium refrigeration) and extreme high temperature (up to 2000K) temperature control environment, these temperature control environments are mainly for the temperature control of solid samples, but the structure of these temperature control equipment is complex and difficult to carry, and it cannot adapt to the change of experimental site. CONTENT OF THE UTILITY MODEL

[0003] The technical problem solved by the present application is how to provide a low-temperature temperature control device for liquid wide-angle X-ray scattering which has a simpler structure and is convenient to carry.

[0004] The present application provides a low-temperature temperature control device for liquid wide-angle X-ray scattering, which comprises:

[0005] A heat preservation cavity is provided with an X-ray transmission window;

[0006] A semiconductor refrigeration piece is located in the heat preservation cavity.

[0007] a sample stage, located inside the insulation cavity and arranged at the top end of the semiconductor refrigeration sheet, and aligned with the X-ray transmission window;

[0008] a heat sink, arranged at the bottom end of the semiconductor refrigeration sheet.

[0009] Optionally, the low-temperature temperature control device further comprises:

[0010] a bracket, the insulation cavity is mounted on the bracket, and the bracket is used for mounting to a fixed platform.

[0011] Optionally, the bottom of the insulation cavity is open, and the bottom of the insulation cavity is connected with the bracket to enclose a sealed space.

[0012] Optionally, the heat sink is mounted on the bracket and located in the sealed space, and the heat sink is a circulating cooler, and the water inlet end and the water outlet end of the circulating cooler extend out of the sealed space.

[0013] Optionally, the sample stage is provided with a sample through hole and a transmission through hole penetrating each other, the sample through hole is used for placing a sample to be tested, and the transmission through hole is opposite to the X-ray transmission window.

[0014] Optionally, the low-temperature temperature control device further comprises a sample carrying tube, the sample carrying tube is placed in the sample through hole, and the sample carrying tube is used for loading a liquid sample to be tested.

[0015] Optionally, the top end of the semiconductor refrigeration sheet is a cold end, and the cold end is connected with the sample stage through a heat conduction layer.

[0016] Optionally, the bottom end of the semiconductor refrigeration sheet is a hot end, and the hot end is connected with the heat sink through a heat conduction layer.

[0017] Optionally, the material of the sample stage and the heat sink is red copper.

[0018] Optionally, the insulation cavity further has a quick connector, and the quick connector is used for connecting a vacuumizing equipment.

[0019] The low-temperature temperature control device for liquid wide-angle X-ray scattering provided in the application has the following technical effects:

[0020] The overall equipment structure of the low-temperature temperature control device is simple, and the low-temperature temperature control device is convenient to move and carry. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 is a schematic view of a low-temperature temperature control device for liquid wide-angle X-ray scattering according to one or more embodiments;

[0022] Figure 2 Structure exploded schematic diagram of a low-temperature temperature control device for liquid wide-angle X-ray scattering according to one or more embodiments;

[0023] Figure 3 Use state schematic diagram of a low-temperature temperature control device for liquid wide-angle X-ray scattering according to one or more embodiments;

[0024] Figure 4 Schematic diagram of a sample stage and a sample carrying tube according to one or more embodiments.

[0025] The correspondence between the reference signs and the component names is as follows:

[0026] Thermal insulation cavity-10, X-ray transmission window-11, quick connector-12, semiconductor refrigeration sheet-20, sample stage-30, sample through hole-31, transmission through hole-32, heat sink-40, water inlet end-41, water outlet end-42, bracket-50, base-52, support plate-51, connecting piece-53, sample carrying tube-60, temperature sensor-70, DC power supply-80, fixed platform-100, vacuum pumping device-200, water circulating device-300. DETAILED DESCRIPTION

[0027] In order to make the purposes, technical solutions and advantages of the present application clearer, further detailed description will be made below in combination with the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not to limit the present application.

[0028] Before describing various embodiments of the present application in detail, first briefly describe the technical concept of the present application: the low-temperature temperature control equipment currently applied to wide-angle X-ray scattering experiments has problems such as complex equipment, inconvenient to carry, etc. Therefore, the present application provides a low-temperature temperature control device for liquid wide-angle X-ray scattering, which is provided with a semiconductor refrigeration sheet and a sample stage in a thermal insulation cavity. The semiconductor refrigeration sheet is used for refrigeration, and the heat generated during the refrigeration process is discharged by a heat sink, so that the sample to be tested on the sample stage is in a low-temperature environment. The overall equipment structure of the low-temperature temperature control device is simple, and it is convenient to move and carry. The specific principles of the low-temperature temperature control device for liquid wide-angle X-ray scattering of the present application will be described below in combination with more embodiments.

[0029] Specifically, as Figure 1 and Figure 2As shown, the low-temperature temperature control device for liquid large-angle X-ray scattering in the embodiment comprises a heat preservation cavity 10, a semiconductor refrigeration sheet 20, a sample stage 30, and a heat sink 40. The heat preservation cavity 10 is provided with an X-ray transmission window 11. The semiconductor refrigeration sheet 20 is located in the heat preservation cavity 10. The sample stage 30 is located in the heat preservation cavity 10 and is arranged at the top end of the semiconductor refrigeration sheet 20, and the sample stage 30 is aligned with the X-ray transmission window 11. The heat sink 40 is arranged at the bottom end of the semiconductor refrigeration sheet 20. The sample stage 30 is used to load the sample to be measured. The semiconductor refrigeration technology is a new type of refrigeration method using a P-N junction of special semiconductor materials to form a thermocouple pair to produce a Peltier effect through direct current refrigeration. The refrigeration technology has fast refrigeration response and small volume. The reverse connection wire can also realize the switching of refrigeration and heating. The semiconductor refrigeration sheet 20 can adopt a single-layer refrigeration sheet structure or a multi-layer refrigeration sheet stack structure. The semiconductor refrigeration sheet 20 will have a temperature difference on both sides after being connected to the power supply, one side refrigerates and the other side heats. If the semiconductor refrigeration sheet 20 is powered for a long time without a heat sink, it is easy to burn out. The cooling of the semiconductor refrigeration sheet is the key to ensuring the stable refrigeration / heating, so the heat sink 40 is used for heat dissipation.

[0030] The X-ray transmission window 11 is designed according to the diffraction light path of the transmission method. The X-ray transmission window 11 is sealed by an X-ray special Compton film or a beryllium sheet which has small X-ray absorption. The material of the heat preservation cavity 10 can be aluminum alloy, 3D printed plastic, etc.

[0031] In one or more embodiments, as shown, Figure 3 The low-temperature temperature control device further comprises a support 50. The heat preservation cavity 10 is installed on the support 50. The support 50 is used to be installed on a fixed platform 100. The low-temperature temperature control device is installed on different positions through the support 50, which is convenient for testing experiments in different environments. The bottom of the heat preservation cavity 10 is open. The bottom of the heat preservation cavity 10 is connected with the support 50 to form a sealed space. The whole sample stage 30 is sealed in the cavity, which can effectively avoid the condensation of water vapor on the sample. The whole cavity is in a room temperature state, which is safe and reliable.

[0032] Specifically, the support 50 comprises a base 52 and a support plate 51. The bottom surface of the support plate 51 is installed on the base 52. The top surface of the support plate 51 is protruded at the edge. The bottom of the heat preservation cavity 10 is attached to the top surface of the support plate 51 and is located within the edge to form a sealed space. The top surface of the support plate 51 is provided with a mounting hole. The side wall of the heat preservation cavity 10 and the mounting hole are connected through a connecting piece 53 to fix the heat preservation cavity 10 on the support 50. The connecting piece 53 is detachably connected with the side wall of the heat preservation cavity 10 and the mounting hole, which is convenient for moving and carrying the low-temperature temperature control device.

[0033] In one or more embodiments, the heat sink 40 is mounted on the bracket 50 and located in the sealed space, the heat sink 40 is a circulating cooler, and the water inlet end 41 and the water outlet end 42 of the circulating cooler extend out of the sealed space. Exemplarily, the support plate 51 of the bracket 50 is provided with two through holes, the heat sink 40 is mounted on the top surface of the support plate 51, the water inlet end 41 and the water outlet end 42 extend out of the two through holes respectively, and the water inlet end 41 and the water outlet end 42 are connected with the water circulating device 300. The circulating water is used to continuously discharge the heat generated by the semiconductor refrigeration sheet 20 in the refrigeration process out of the heat preservation cavity, so as to ensure the normal refrigeration process. In other embodiments, the heat sink 40 can be a fan refrigeration type heat sink. Preferably, the circulating cooler has good heat dissipation effect, small size and no obvious noise.

[0034] In one or more embodiments, the top end of the semiconductor refrigeration sheet 20 is a cold end, and the cold end is connected with the sample stage 30 through a heat conduction layer. The bottom end of the semiconductor refrigeration sheet 20 is a hot end, and the hot end is connected with the heat sink 40 through a heat conduction layer. The heat transfer efficiency between the semiconductor refrigeration sheet 20 and the sample stage 30 and the heat sink 40. Exemplarily, the heat conduction layer can be at least one of double-sided adhesive copper foil, heat-conducting double-sided adhesive, and curable heat-conducting silicone grease. The material of the sample stage 30 and the heat sink 40 is red copper, which has high thermal conductivity and excellent heat conductivity, and is conducive to realizing sample constant temperature. In other embodiments, the material of the sample stage 30 and the heat sink 40 can also use materials with high thermal conductivity such as aluminum alloy and stainless steel.

[0035] It should be noted that the working process of the semiconductor refrigeration sheet 20 is controlled by the direct current power supply 80. The temperature regulation can be realized by changing the size of the input current and voltage of the direct current power supply. Meanwhile, the change of the input direction of the direct current can also realize the conversion between constant temperature refrigeration and heating. At this time, the top end of the semiconductor refrigeration sheet 20 is a hot end, and the bottom end of the semiconductor refrigeration sheet 20 is a cold end.

[0036] In one or more embodiments, as shown in Figure 4 The sample stage 30 is provided with a sample through hole 31 and a transmission through hole 32 which are mutually through. The sample through hole 31 is used for placing a sample to be measured, and the transmission through hole 32 is opposite to the X-ray transmission window 11. Exemplarily, the extension direction of the sample through hole 31 and the extension direction of the transmission through hole 32 are perpendicular to each other. Further, the low-temperature temperature control device further comprises a sample carrying tube 60, the sample carrying tube 60 is placed in the sample through hole 31, and the sample carrying tube 60 is used for loading a liquid sample to be measured. By arranging the sample carrying tube 60, the X-ray scattering experiment of the liquid sample in the low-temperature environment can be realized. Exemplarily, the sample carrying tube 60 can be a glass capillary tube.

[0037] In one or more embodiments, the heat preservation cavity 10 also has a quick connector 12 for connecting a vacuumizing device 200, such as a vacuum pump. The vacuumizing device is used to prevent water vapor in the air from condensing on the sample-bearing tube 60 and to achieve air pressure monitoring.

[0038] In one or more embodiments, the low-temperature temperature control device also includes a temperature sensor 70 installed on the sample stage 30 to monitor the temperature of the sample. Exemplarily, the temperature sensor 70 uses a sheet-shaped thermocouple that is attached to the sample stage 30 and is connected to a digital thermometer to achieve real-time monitoring of the sample temperature.

[0039] To verify the performance of the low-temperature temperature control device for liquid large-angle X-ray scattering in this embodiment, a static temperature control performance test was conducted:

[0040] (1) Empty constant temperature test. Turn on the circulating water of the heat sink 40 and turn on the vacuum pump. After the vacuum degree reaches -0.8 kPa, turn off the vacuum pump. Set the voltage of the direct current power supply to 8.46 V and the current to 1.56 A. The sample is stabilized to -40℃ in 5 minutes from room temperature 25.8℃, and the temperature fluctuation is ±0.1℃ within 5 minutes after stabilization. Then, reduce the voltage of the direct current power supply to 4.26 V and the current to 0.86 A. The temperature rises to -10℃ in about 4 minutes, and the temperature fluctuation is ±0.1℃ within 5 minutes after stabilization. Further, reduce the voltage of the direct current power supply to 2.26 V and the current to 0.84 V. The temperature rises to 0℃ in about 3 minutes, and the temperature fluctuation is ±0.1℃ within 5 minutes after stabilization. Reverse the positive and negative electrodes, set the voltage to 1.26 V and the current to 0.16 A. The temperature rises to 30℃ in about 10 minutes, and the temperature fluctuation is ±0.1℃ within 5 minutes after stabilization. Further, reverse the positive and negative electrodes, set the voltage to 1.56 V and the current to 0.16 A. The temperature rises to 50℃ in about 6 minutes, and the temperature fluctuation is ±0.1℃ within 5 minutes after stabilization. Further, reverse the positive and negative electrodes, set the voltage to 4.56 V and the current to 0.86 A. The temperature rises to 70℃ in about 6 minutes, and the temperature fluctuation is ±0.2℃ within 5 minutes after stabilization.

[0041] (2) Loading liquid sample constant temperature test. Open the circulating water of the heat sink 40, open the vacuum pump, and close the vacuum pump after the vacuum degree reaches-0.8 kPa. Set the voltage of the direct current power supply to 8.56V, the current to 1.56A, and the sample from room temperature 25.8℃ to-40℃ in 5 minutes. After stabilization, the temperature fluctuation is ±0.1℃ within 5 minutes. Then, reduce the voltage of the direct current power supply to 4.46V, the current to 0.86A, and the temperature to-10℃ in about 4 minutes. After stabilization, the temperature fluctuation is ±0.1℃ within 5 minutes. Further, reduce the voltage of the direct current power supply to 2.86V, the current to 0.84V, and the temperature to 0℃ in about 3 minutes. After stabilization, the temperature fluctuation is ±0.1℃ within 5 minutes. Reverse the positive and negative electrodes, set the voltage to 1.46V, the current to 0.19A, and the temperature to 30℃ in about 10 minutes. After stabilization, the temperature fluctuation is ±0.1℃ within 5 minutes. Further, reverse the positive and negative electrodes, set the voltage to 1.86V, the current to 0.36A, and the temperature to 50℃ in about 6 minutes. After stabilization, the temperature fluctuation is ±0.1℃ within 5 minutes. Further, reverse the positive and negative electrodes, set the voltage to 6.56V, the current to 1.36A, and the temperature to 70℃ in about 6 minutes. After stabilization, the temperature fluctuation is ±0.2℃ within 5 minutes.

[0042] According to the test results described above, the low-temperature control device for liquid large-angle X-ray scattering provided in the embodiment has high temperature control precision, and the temperature rising and falling processes are relatively fast.

[0043] The specific embodiments of the application are described in detail above, although some embodiments have been shown and described, those skilled in the art should understand that modifications and improvements can be made to these embodiments without departing from the principles and spirits of the application defined by the claims and their equivalents, and these modifications and improvements should also be within the protection scope of the application.

Claims

1. A low temperature control device for liquid large angle X-ray scattering, characterized by, The low-temperature temperature control device comprises: a heat preservation cavity, which is provided with an X-ray transmission window; a semiconductor refrigeration sheet, which is located in the heat preservation cavity; a sample stage, which is located in the heat preservation cavity and arranged on the top end of the semiconductor refrigeration sheet, and is aligned with the X-ray transmission window; a heat sink, which is arranged on the bottom end of the semiconductor refrigeration sheet.

2. The low temperature cell for liquid large angle X-ray scattering according to claim 1, characterized in that, The low-temperature temperature control device further comprises: a bracket, wherein the heat preservation cavity is mounted on the bracket, and the bracket is used for mounting on a fixed platform.

3. The low temperature cell for liquid large angle X-ray scattering according to claim 2, characterized in that, The bottom of the heat preservation cavity is open, and the bottom of the heat preservation cavity is connected with the bracket to form a sealed space.

4. The low temperature cell for liquid large angle X-ray scattering according to claim 3, characterized in that, The heat sink is mounted on the bracket and located in the sealed space, and the heat sink is a circulating cooler, wherein the water inlet end and the water outlet end of the circulating cooler extend out of the sealed space.

5. The low temperature cell for liquid large angle X-ray scattering according to claim 1, characterized in that, The sample stage is provided with a sample through hole and a transmission through hole which are mutually through, the sample through hole is used for placing a sample to be measured, and the transmission through hole is opposite to the X-ray transmission window.

6. The low-temperature temperature control device for liquid large-angle X-ray scattering according to claim 5, further comprising a sample bearing tube, wherein the sample bearing tube is placed in the sample through hole, and the sample bearing tube is used for loading a liquid sample to be measured.

7. The low temperature cell for liquid large angle X-ray scattering according to claim 3, characterized in that, The top end of the semiconductor refrigeration sheet is a cold end, and the cold end is connected with the sample stage through a heat conduction layer.

8. The low temperature cell for liquid large angle X-ray scattering according to claim 3, characterized in that, The bottom end of the semiconductor refrigeration sheet is a hot end, and the hot end is connected with the heat sink through a heat conduction layer.

9. The low temperature cell for liquid large angle X-ray scattering according to claim 1, wherein The sample stage and the heat sink are made of red copper.

10. The low temperature cell for liquid large angle X-ray scattering according to claim 1, characterized in that, The heat preservation cavity is further provided with a quick connector, which is used for connecting a vacuumizing device.

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