Testing device and testing system for temperature-induced phase change material

Abstract

The invention provides a testing device and a testing system for a temperature-induced phase change material. The testing device comprises a device main body, a heating assembly, a pair of conductive probe assemblies and an automatic control system. When the device is used, the device body is used for being connected with an XRD diffractometer, the heating assembly responds to a temperature regulation and control instruction of an automatic control system so that the temperature of the temperature-induced phase change material can be increased or decreased to multiple preset temperatures, and heat preservation is conducted for a preset duration when each preset temperature is reached. In the heating or cooling process of the temperature-induced phase change material, the automatic control system continuously collects the temperature and electric signals of the temperature-induced phase change material, XRD scanning is conducted on a sample through an XRD diffractometer in the heat preservation process, and XRD data are collected; and finally, outputting the temperature value of the temperature-induced phase change material in the heating process and the cooling process, and the corresponding relationship between the electric signal and the XRD data. According to the testing device for the temperature-induced phase change material, the effect of real-time coupling observation of electrical and structural characteristics of the temperature-induced phase change material in the temperature changing process can be achieved.

Description

Technical Field

[0001] The invention relates to the field of material science and application technology, and in particular to a testing device and a testing system for thermotropic phase change materials. Background Art

[0002] Temperature-dependent phase change materials occupy an important position in the field of modern materials science and applied technology. They can undergo significant crystal phase structure changes under temperature changes, accompanied by obvious changes in electrical properties. Based on these unique properties, temperature-dependent phase change materials are widely used in many high-tech fields. For example, vanadium dioxide (VO2) undergoes a phase change from semiconductor to metal at about 68°C, accompanied by a sharp change in infrared reflectivity and resistance. This property makes VO2 an ideal material for smart windows, which can be used to adjust infrared transmittance, thereby achieving energy saving and temperature control. Barium titanate (BaTiO3) undergoes a ferroelectric-paraelectric phase transition near the Curie temperature (about 120°C), and electrical properties such as dielectric constant and resistance will change dramatically. Therefore, BaTiO3 and its related materials are widely used in memory elements and non-volatile memory devices, using their temperature-responsive electrical properties to achieve information storage and conversion. Cobalt oxide (CoO) undergoes an antiferromagnetic-paramagnetic phase transition at 290K, accompanied by a significant change in magnetoelectric properties. It is widely used in smart coatings and temperature-sensitive devices to adjust electromagnetic properties in the form of coatings or films to achieve flexible temperature response. In-depth research on these temperature-induced phase change materials will not only help reveal the mechanism of change in their electrical properties during the phase change process, but also provide theoretical support for the design of new smart materials and devices. Therefore, studying the coordinated changes in the crystal structure and electrical properties of temperature-induced phase change materials during the temperature-dependent phase change process is of great significance for promoting the development of smart materials and a deep understanding of the phase change mechanism.

[0003] At present, several patents have disclosed special test devices for specific temperature-induced phase change materials. For example, patent CN209086181U proposes an X-ray diffraction in-situ variable temperature test sample table for vanadium dioxide phase change process for VO2 materials; patent CN106153582A focuses on infrared temperature control materials, and evaluates its temperature control characteristics by monitoring the changes in infrared irradiance and transmittance of the materials. However, the existing devices on the market are difficult to simultaneously collect and couple temperature, electrical, and XRD data for structure-activity relationship research. Summary of the invention

[0004] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides a testing device and a testing system for thermotropic phase change materials, aiming to solve the problem that the existing devices are difficult to simultaneously collect and couple temperature, electrical, and XRD data for structure-activity relationship research.

[0005] The present invention provides a testing device for a temperature-dependent phase change material, comprising: A device body, the device body being used for detachably connecting with an XRD diffractometer; A heating component is arranged on the device body, and a heating end of the heating component is used to contact the temperature-dependent phase change material to change the temperature of the temperature-dependent phase change material and detect the temperature value of the temperature-dependent phase change material; A pair of conductive probe assemblies, arranged on the device body, the contacts of each group of the conductive probe assemblies are used to contact the temperature-induced phase change material, and the contacts of the two groups of the conductive probe assemblies are spaced a certain distance apart; The automatic control system comprises a program temperature control module, a temperature acquisition module, an electric signal acquisition module, an XRD data acquisition module and a data processing module, wherein the program temperature control module and the temperature acquisition module are both connected to the heating component, the program temperature control module is used to control the heating temperature of the heating component to rise or fall, and is used to control the heating component to keep warm for a preset time at a preset temperature, the temperature acquisition module collects and records the temperature value of the temperature-induced phase change material in real time through the heating component, the electric signal acquisition module is connected to the conductive probe component, the electric signal acquisition module is used to collect and record the electric signal between two groups of the conductive probe components in real time, the XRD data acquisition module is used to connect to the XRD diffractometer, the XRD data acquisition module is used to collect and record XRD data when the program temperature control module executes a heat preservation instruction, the program temperature control module, the temperature acquisition module, the electric signal acquisition module and the XRD data acquisition module are all connected to the data processing module, and the data processing module outputs the corresponding relationship between the temperature value, the electric signal and the XRD data based on the temperature value, the electric signal and the XRD data.

[0006] According to the testing device for temperature-dependent phase change materials provided by the present invention, the heating component includes a heater, a heating platform and a temperature detector, the heater is communicatively connected to the program temperature control module, the temperature detector is communicatively connected to the temperature acquisition module, the heater is used to control the temperature increase or decrease of the temperature of the temperature-dependent phase change material under the control of the program temperature control module, and control the heater to keep warm for the preset time when the temperature of the temperature-dependent phase change material reaches the preset temperature, the temperature detector is used to detect the temperature value of the temperature-dependent phase change material, and the heating platform is arranged at the heating end of the heater.

[0007] According to the testing device for thermotropic phase change materials provided by the present invention, the device body includes a thermal insulation support assembly, the heater is arranged in the thermal insulation support assembly, and the heating end of the heater extends upward to the outside of the thermal insulation support assembly.

[0008] According to the testing device for temperature-induced phase change materials provided by the present invention, the conductive probe assembly includes a probe and an adjustment bracket, the probe is connected to the device body through the adjustment bracket, the adjustment bracket is used to adjust and fix the position of the contact of the probe, and the probe is communicatively connected to the electrical signal acquisition module.

[0009] According to the testing device for thermotropic phase change materials provided by the present invention, the adjustment bracket includes a height adjustment mechanism and a horizontal position adjustment mechanism connected to each other, one of the height adjustment mechanism and the horizontal position adjustment mechanism is connected to the device body, and the other is connected to the probe.

[0010] According to the testing device for temperature-induced phase change materials provided by the present invention, the height adjustment mechanism includes a first rotating shaft and an eccentric rotating arm, the first rotating shaft is rotatably connected to the device body, and the rotation axis of the first rotating shaft is parallel to the heating platform, there is damping between the first rotating shaft and the device body, one end of the eccentric rotating arm is connected to the first rotating shaft to prevent rotation, and the other end of the eccentric rotating arm extends radially along the first rotating shaft and is connected to the probe through the horizontal position adjustment mechanism.

[0011] According to the testing device for temperature-induced phase change materials provided by the present invention, the horizontal position adjustment mechanism includes a second rotating shaft, the second rotating shaft is rotatably connected to the end of the eccentric rotating arm away from the first rotating shaft, the rotation axis is parallel to the rotation axis of the first rotating shaft, and there is damping between the second rotating shaft and the eccentric rotating arm, the probe is arranged at the end of the second rotating shaft away from the eccentric rotating arm, and the axis of the probe is perpendicular to the axis of the second rotating shaft.

[0012] According to the testing device for thermotropic phase change materials provided by the present invention, the probe is a gold-plated probe.

[0013] According to the testing device for temperature-induced phase change materials provided by the present invention, the probe includes a probe body and a probe head, the tail end of the probe is slidably inserted in the probe body, a spring is arranged between the probe body and the tail end of the probe, and the spring is used to provide a force to extend the probe to the outside of the probe body.

[0014] The present invention also provides a testing system for thermotropic phase change materials, comprising the testing device for thermotropic phase change materials and an XRD diffractometer as described above, wherein the device body comprises a docking fixture, and the docking fixture is used to be detachably connected to the XRD diffractometer.

[0015] The present invention adopts the above technical solution, which has the following advantages: The testing device for temperature-induced phase change material provided by the present invention comprises a device body, a heating component, a pair of conductive probe components and an automatic control system. The device body is used to be connected to an XRD diffractometer. The heating component is arranged on the device body, and its heating end is used to contact the temperature-induced phase change material to change the temperature of the temperature-induced phase change material and detect the temperature value of the temperature-induced phase change material. The conductive probe component is arranged on the device body, and the contacts of each group of conductive probe components are used to contact the temperature-induced phase change material, and the contacts of the two groups of conductive probe components are spaced a certain distance apart. The automatic control system comprises a program temperature control module, a temperature acquisition module, an electrical signal acquisition module, an XRD data acquisition module and a data processing module. The program temperature control module and the temperature acquisition module are both connected to the heating component, the electrical signal acquisition module is connected to the conductive probe component, the XRD data acquisition module is used to be connected to the XRD diffractometer, and the program temperature control module, the temperature acquisition module, the electrical signal acquisition module and the XRD data acquisition module are all connected to the data processing module. When in use, first the device body is connected to the XRD diffractometer, the temperature-induced phase change material is placed at the heating end of the heating component, and the contacts of the two sets of conductive probe components are in contact with the temperature-induced phase change material. The heating component responds to the heating instruction of the program temperature control module to heat the temperature-induced phase change material, so that the temperature of the temperature-induced phase change material gradually rises to multiple preset temperatures at a certain heating rate, and is kept warm for a preset time when each preset temperature is reached. Then the heating component responds to the cooling instruction of the program temperature control module to cool the temperature-induced phase change material, so that the temperature of the temperature-induced phase change material gradually drops to multiple preset temperatures at a certain cooling rate, and is kept warm for a preset time when each preset temperature is reached. During the heating and cooling process of the temperature-induced phase change material, the temperature acquisition module continuously collects and records the temperature value of the temperature-induced phase change material, and the electrical signal acquisition module collects and records the electrical signals between the two sets of conductive probe components in real time. When the heating component executes the insulation instruction, the operator performs an in-situ XRD scan of the temperature-induced phase change material through the XRD diffractometer, and the XRD data acquisition module collects and records the XRD data. The temperature values, electrical signals and XRD data collected are all transmitted to the data processing module, and the data processing module outputs the corresponding relationship between the temperature values, electrical signals and XRD data based on the data. The testing device for temperature-induced phase change materials provided by the present invention can be installed on an XRD diffractometer to detect the electrical properties of the temperature-induced phase change materials during the program temperature control process, and at the same time achieve the effect of in-situ XRD measurement of the temperature-induced phase change materials, automatically realize the synchronous collection of multiple data, and provide a complete data chain for the phase change mechanism and structure-activity relationship research of the temperature-induced phase change materials.

[0016] Further, in the test system for the temperature-induced phase change material provided by the present invention, an XRD diffractometer and the test device for the temperature-induced phase change material as described above are provided, and the device body of the test device includes a docking fixture, and the docking fixture is used to be detachably connected to the XRD diffractometer. Since the test device for the temperature-induced phase change material as described above is provided, the same advantages as described above are provided. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions in the present invention or 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 some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 is a schematic structural diagram of a testing device for a thermotropic phase change material provided by an embodiment of the present invention; Figure 2 is a cross-sectional view of a testing device for a thermotropic phase change material provided by an embodiment of the present invention; Figure 3 is a graph showing the relationship between time and temperature and between temperature and resistance value provided by an embodiment of the present invention; Figure 4 is a temperature-resistance curve of VO2 provided by an embodiment of the present invention; Figure 5 This is an in-situ variable temperature XRD spectrum of VO2 provided in one embodiment of the present invention.

[0019] Reference numerals: 110: base; 120: support column; 130: first thermal insulation support plate; 140: second thermal insulation support plate; 150: conductive column; 160: probe fixing frame; 170: ceramic connecting block; 210: heater; 220: heating platform; 310: probe body; 320: probe head; 400: docking fixture; 510: electrical signal circuit board; 520: external circuit board; 610: first rotating shaft; 620: eccentric rotating arm; 710: second rotating shaft. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the drawings of the present invention. Obviously, the described embodiments are 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.

[0021] In the description of the present invention, it is to be understood that the terms “center”, “longitudinal”, “lateral”, “length”, “width”, “thickness”, “up”, “down”, “front”, “back”, “left”, “right”, “vertical”, “horizontal”, “top”, “bottom”, “inside”, “outside”, “clockwise”, “counterclockwise”, “axial”, “radial”, “circumferential”, etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0022] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is more than two, unless otherwise clearly and specifically defined.

[0023] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0024] In the present invention, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediate medium. Moreover, a first feature being "above", "above" or "above" a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is higher in level than the second feature. A first feature being "below", "below" or "below" a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is lower in level than the second feature.

[0025] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, without contradiction.

[0026] The testing device for temperature-induced phase change material provided by the present invention comprises a device body, a heating component, a pair of conductive probe components and an automatic control system. The device body is used to be connected to an XRD diffractometer. The heating component is arranged on the device body, and its heating end is used to contact the temperature-induced phase change material to change the temperature of the temperature-induced phase change material and detect the temperature value of the temperature-induced phase change material. The conductive probe component is arranged on the device body, and the contacts of each group of conductive probe components are used to contact the temperature-induced phase change material, and the contacts of the two groups of conductive probe components are spaced a certain distance apart. The automatic control system comprises a program temperature control module, a temperature acquisition module, an electrical signal acquisition module, an XRD data acquisition module and a data processing module. The program temperature control module and the temperature acquisition module are both connected to the heating component, the electrical signal acquisition module is connected to the conductive probe component, the XRD data acquisition module is used to be connected to the XRD diffractometer, and the program temperature control module, the temperature acquisition module, the electrical signal acquisition module and the XRD data acquisition module are all connected to the data processing module. When in use, first the device body is connected to the XRD diffractometer, the temperature-induced phase change material is placed at the heating end of the heating component, and the contacts of the two sets of conductive probe components are in contact with the temperature-induced phase change material. The heating component responds to the heating instruction of the program temperature control module to heat the temperature-induced phase change material, so that the temperature of the temperature-induced phase change material gradually rises to multiple preset temperatures at a certain heating rate, and is kept warm for a preset time when each preset temperature is reached. Then the heating component responds to the cooling instruction of the program temperature control module to cool the temperature-induced phase change material, so that the temperature of the temperature-induced phase change material gradually drops to multiple preset temperatures at a certain cooling rate, and is kept warm for a preset time when each preset temperature is reached. During the heating and cooling process of the temperature-induced phase change material, the temperature acquisition module continuously collects and records the temperature value of the temperature-induced phase change material, and the electrical signal acquisition module collects and records the electrical signals between the two sets of conductive probe components in real time. When the heating component executes the insulation instruction, the operator performs an in-situ XRD scan of the temperature-induced phase change material through the XRD diffractometer, and the XRD data acquisition module collects and records the XRD data. The temperature values, electrical signals and XRD data collected are all transmitted to the data processing module, and the data processing module outputs the corresponding relationship between the temperature values, electrical signals and XRD data based on the data. The testing device for temperature-induced phase change materials provided by the present invention can be installed on an XRD diffractometer to detect the electrical properties of the temperature-induced phase change materials during the program temperature control process, and at the same time achieve the effect of in-situ XRD measurement of the temperature-induced phase change materials, automatically realize the synchronous collection of multiple data, and provide a complete data chain for the phase change mechanism and structure-activity relationship research of the temperature-induced phase change materials.

[0027] Combine the following Figures 1 to 5 The present invention describes a testing device and a testing system for a thermotropic phase change material.

[0028] An embodiment of the present invention provides a testing device for a temperature-induced phase change material, comprising a device body, a heating component, a pair of conductive probe components and an automatic control system.

[0029] The device body provides a mounting carrier for the heating component and the conductive probe component, and the device body is used to be detachably connected to the XRD diffractometer.

[0030] The heating component is arranged on the device body. When in use, the temperature-sensitive phase change material is placed on the heating end of the heating component. The heating component can change the temperature of the temperature-sensitive phase change material by heat conduction, and the heating component can also detect the temperature value of the temperature-sensitive phase change material.

[0031] The conductive probe assembly includes two groups, which are arranged in pairs and are both arranged on the device body. The contacts of each group of conductive probe assemblies are used to contact the temperature-induced phase change material, and the contacts of the two groups of conductive probe assemblies are separated by a certain distance when contacting the temperature-induced phase change material.

[0032] The automatic control system includes a computer and a special test software embedded in the computer. The computer is equipped with a program temperature control module, a temperature acquisition module, an electrical signal acquisition module, an XRD data acquisition module and a data processing module. The program temperature control module and the temperature acquisition module are both connected to the heating component. The program temperature control module is used to control the heating temperature of the heating component, so that the heating temperature of the heating component increases or decreases at a certain rate, and can control the heating component to keep warm for a preset time when the temperature rises or drops to a preset temperature. The temperature acquisition module is used to collect and record the temperature value of the temperature-induced phase change material.

[0033] The electrical signal acquisition module is electrically connected to the conductive probe assembly and is used for real-time acquisition and recording of electrical signals between the two groups of conductive probe assemblies.

[0034] The XRD data acquisition module is used to connect with the XRD diffractometer. When the program temperature control module executes the insulation instruction, the experimenter can operate the XRD diffractometer to perform in-situ XRD scanning on the temperature-induced phase change material. At this time, the XRD data acquisition module is used to collect and record XRD data.

[0035] The testing device for thermotropic phase change materials provided by the present invention is used for detachably connecting to an XRD diffractometer, and the specific testing process is as follows: Firstly, the test device is installed on the XRD diffractometer through the device body, and then the temperature-induced phase change material is placed on the heating end of the heating component, and the contacts of the two sets of conductive probe components are brought into contact with the temperature-induced phase change material.

[0036] Then, the dedicated test software built into the computer is opened. Under the control of the dedicated test software instructions, the heating component responds to the heating instructions of the program temperature control module to heat the temperature-induced phase change material, so that the temperature of the temperature-induced phase change material gradually rises to multiple preset temperatures at a certain heating rate, and is kept warm for a preset time when each preset temperature is reached. Then, the heating component responds to the cooling instructions of the program temperature control module to cool the temperature of the temperature-induced phase change material, so that the temperature of the temperature-induced phase change material gradually drops to multiple preset temperatures at a certain cooling rate, and is kept warm for a preset time when each preset temperature is reached.

[0037] During the process of heating and cooling of the temperature-induced phase change material, the temperature acquisition module continuously acquires and records the temperature value of the temperature-induced phase change material, and the electrical signal acquisition module acquires and records the electrical signal between the two sets of conductive probe assemblies in real time.

[0038] When the heating component executes the insulation instruction, the operator performs an in-situ XRD scan on the temperature-induced phase change material through the XRD diffractometer, and the XRD data acquisition module collects and records the XRD data.

[0039] The temperature values, electrical signals and XRD data collected above are all transmitted to the data processing module, and the data processing module outputs the corresponding relationship between the temperature values, electrical signals and XRD data based on the above data.

[0040] The testing device for temperature-induced phase change materials provided by the present invention can be installed on an XRD diffractometer to detect the electrical properties of the temperature-induced phase change materials during programmed temperature control, while achieving the effect of in-situ XRD measurement of the temperature-induced phase change materials, automatically realizing the synchronous collection of multiple data, and providing a complete data chain for the phase change mechanism and structure-activity relationship research of the temperature-induced phase change materials.

[0041] In some embodiments, the heating component may include a heater 210, a heating platform 220 and a temperature detector. The heater 210 and the temperature detector are both communicatively connected to a program temperature control module. The program temperature control module can respond to instructions from a dedicated test software to perform program temperature control, so that the temperature of the heater 210 is increased or decreased at a certain rate. The heater 210 can also be controlled to keep the temperature for a preset period of time when the temperature of the thermotropic phase change material reaches a preset temperature value.

[0042] The temperature acquisition module is connected to the temperature detector and is used to collect the temperature value of the temperature-induced phase change material collected by the temperature detector. The heating platform 220 is arranged at the heating end of the heater 210. In this embodiment, the heating end of the heater 210 is located at the top of the heater 210, the bottom surface of the heating platform 220 is connected to the top of the heater 210, and the top surface of the heating platform 220 is a plane, which is used to support the temperature-induced phase change material and perform heat exchange with the temperature-induced phase change material in a heat conduction manner to change the temperature value of the temperature-induced phase change material.

[0043] In some embodiments, the device body includes a thermal insulation support assembly, the heater 210 is disposed in the thermal insulation support assembly, and the heating end of the heater 210 extends upward to the outside of the thermal insulation support assembly.

[0044] Specifically, the device body includes a base 110, and the heat insulation support assembly includes four support columns 120, a first heat insulation support plate 130 and a second heat insulation support plate 140. A mounting groove is provided on the top of the first heat insulation support plate 130, and the bottom of the heater 210 is used to be fixed in the mounting groove. A mounting hole is provided in the middle of the second heat insulation support plate 140, and the mounting hole passes through the second heat insulation support plate 140. When installed, the second heat insulation support plate 140 is connected to the top of the first heat insulation support plate 130, and the heating end at the top of the heater 210 passes through the mounting hole to the top of the second heat insulation support plate 140.

[0045] In this way, the heater 210 is wrapped in the first heat insulation support plate 130 and the second heat insulation support plate 140, which can slow down the heat exchange between the heater 210 and the external environment, and play a role in heat preservation and energy consumption reduction.

[0046] The bottom of the first heat-insulating support plate 130 is connected to the top of the base 110 through four support columns 120, and the four support columns 120 can support the first heat-insulating support plate 130 from the base 110 to raise the height of the heating assembly. In this way, when the testing device is installed on the XRD diffractometer, the irradiation light can be irradiated to the sample of the temperature-induced phase change material on the top of the heating assembly.

[0047] Specifically, the first heat insulation support plate 130 and the second heat insulation support plate 140 may both be made of high temperature resistant insulating materials such as alumina.

[0048] In some embodiments, the conductive probe assembly includes a probe and an adjustment bracket, the probe is connected to the device body through the adjustment bracket, and the adjustment bracket is used to adjust and fix the position of the contact point of the probe.

[0049] Specifically, an electrical signal circuit board 510 is also provided at the bottom of the first thermal insulation support plate 130, and an external circuit board 520 is also provided at the bottom of the base 110. The electrical signal circuit board 510 is communicatively connected with the external circuit board 520, and the computer is connected to the data connector on the external circuit board 520 via a signal line. The above-mentioned electrical signal circuit board 510 and external circuit board 520 are both part of the automation control system.

[0050] The device body is also provided with conductive posts 150 and probe holders 160 . Two conductive posts 150 and two probe holders 160 are provided. Each set of conductive posts 150 and probe holders 160 is correspondingly installed with a set of conductive probe components.

[0051] The bottom end of the conductive pillar 150 is conductively connected to the electric signal circuit board 510, and the top end of the conductive pillar 150 passes through the first thermal insulation support plate 130 and the second thermal insulation support plate 140 and continues to extend upward. The probe holder 160 is connected to the top end of the conductive pillar 150, and the probe holder 160 is made of conductive material, and the probe holder 160 is conductively connected to the conductive pillar 150.

[0052] In order to prevent the conductive column 150 from conducting electricity with the first thermal insulation support plate 130 and the second thermal insulation support plate 140, the first thermal insulation support plate 130 and the second thermal insulation support plate 140 can use insulating materials, or an insulating layer can be set on the outside of the conductive column 150, or a gap can be set between the conductive column 150 and the first thermal insulation support plate 130 and the second thermal insulation support plate 140.

[0053] Each probe holder 160 is connected to an adjustment bracket, and each adjustment bracket is connected to a probe. The probe is electrically connected to the electrical signal circuit board 510 through the adjustment bracket, the probe holder 160 and the conductive column 150, and is used to collect the electrical signal of the temperature-induced phase change material, and transmit the electrical signal to the computer through the external circuit board 520 for processing by the test software.

[0054] The adjusting bracket is used to adjust the position of the contact point of the probe so that the contact point of the probe can contact or separate from the temperature-induced phase change material on the heating platform 220 placed on the top of the heater 210.

[0055] Since the probe holder 160 is made of conductive material and is connected to the electrical signal circuit board 510 only through one conductive column 150 , a ceramic connecting block 170 may be provided between the two probe holders 160 to prevent conduction between the two probe holders 160 and to prevent the probe holders 160 from rotating about the axis of the conductive column 150 .

[0056] In some embodiments, the adjustment bracket includes a height adjustment mechanism and a horizontal position adjustment mechanism connected to each other, one of the height adjustment mechanism and the horizontal position adjustment mechanism is connected to the device body, and the other is connected to the probe.

[0057] Specifically, the height adjustment mechanism can be connected to the device body, more specifically, connected to the probe fixing frame 160, the horizontal position adjustment mechanism is connected to the moving end of the height adjustment mechanism, and moves synchronously with the height adjustment mechanism, and the probe is set on the horizontal position adjustment mechanism and moves synchronously with the horizontal position adjustment mechanism. The probe is conductively connected to the probe fixing frame 160 through the horizontal position adjustment mechanism and the height adjustment mechanism.

[0058] In some embodiments, the height adjustment mechanism includes a first rotating shaft 610 and an eccentric rotating arm 620. The first rotating shaft 610 is rotatably connected to the device body, and the rotation axis of the first rotating shaft 610 is parallel to the heating platform 220. There is damping between the first rotating shaft 610 and the device body. One end of the eccentric rotating arm 620 is connected to the first rotating shaft 610 to prevent rotation, and the other end of the eccentric rotating arm 620 extends radially along the first rotating shaft 610 and is connected to the probe through a horizontal position adjustment mechanism.

[0059] Specifically, a first axial hole is provided on the probe fixing frame 160 and passes through the probe fixing frame 160 in the front-to-back direction. The first rotating shaft 610 is inserted into the first axial hole, and a rubber gasket can be provided between the outer side of the first rotating shaft 610 and the inner side of the first axial hole to provide damping when the first rotating shaft 610 rotates, so that the first rotating shaft 610 can overcome the damping rotation under the action of external force, and the first rotating shaft 610 is prevented from rotating after the external force is removed.

[0060] One end of the eccentric rotating arm 620 is provided with a second axial hole passing through the eccentric rotating arm 620, and the end of the first rotating shaft 610 away from the probe fixing frame 160 is inserted into the second axial hole, and the eccentric rotating arm 620 can be key-connected with the first rotating shaft 610 to achieve a non-rotating connection between the eccentric rotating arm 620 and the first rotating shaft 610.

[0061] When in use, the outwardly extending end of the eccentric rotating arm 620 can be moved to rotate the first rotating shaft 610, thereby changing the height of the outwardly extending end of the eccentric rotating arm 620 to achieve height adjustment.

[0062] In some embodiments, the horizontal position adjustment mechanism includes a second rotating shaft 710, which is rotatably connected to an end of the eccentric rotating arm 620 away from the first rotating shaft 610, the rotation axis is parallel to the rotation axis of the first rotating shaft 610, and there is damping between the second rotating shaft 710 and the eccentric rotating arm 620, and the probe is disposed at an end of the second rotating shaft 710 away from the eccentric rotating arm 620, and the axis of the probe is perpendicular to the axis of the second rotating shaft 710.

[0063] Specifically, a third shaft hole penetrating the eccentric rotating arm 620 is provided at the extended end of the eccentric rotating arm 620, and the axes of the first shaft hole, the second shaft hole and the third shaft hole are parallel. One end of the second rotating shaft 710 is passed through the third shaft hole, and a rubber gasket is provided between the outer side of the second rotating shaft 710 and the inner side of the third shaft hole to provide damping when the second rotating shaft 710 rotates, so that the second rotating shaft 710 can overcome the damping and rotate under the action of an external force, and the second rotating shaft 710 is prevented from rotating after the external force is removed.

[0064] The probe is disposed at one end of the second shaft 710 away from the eccentric rotating arm 620, and the axis of the probe is perpendicular to the axis of the second shaft 710. When the probe is turned, the probe drives the second shaft 710 to rotate, so that the contact point of the probe swings in the left and right directions, thereby adjusting the horizontal position of the probe in the left and right directions.

[0065] In some embodiments, the probe may be a gold-plated probe. Plating the outer surface of the probe with gold can greatly improve the conductivity of the probe, reduce the resistance value, and reduce signal loss. In addition, the chemical properties of gold are very stable and it is not easy to react chemically with other substances. Therefore, gold plating can effectively prevent oxidation of the probe and extend its service life.

[0066] In some embodiments, the probe includes a probe body 310 and a probe head 320 , the tail end of the probe 320 can be slidably inserted into the probe body 310 , and a spring is arranged between the probe body 310 and the tail end of the probe 320 , and the spring is used to provide a force to extend the probe 320 to the outside of the probe body 310 .

[0067] Specifically, the probe includes a probe body 310 and a probe head 320. The tail end of the probe body 310 is used to connect with the second rotating shaft 710. The head end of the probe body 310 is provided with a blind hole extending toward the tail end. The tail end of the probe head 320 is used to be slidably inserted into the blind hole. A spring is provided in the blind hole. The spring is compressed between the tail end of the probe head 320 and one end of the blind hole close to the tail end of the probe body 310. A limiter is also provided in the blind hole to prevent the tail end of the probe head 320 from sliding out of the blind hole.

[0068] The spring is in a compressed state and can always provide the probe 320 with a force to move outside the blind hole. When the contact of the probe 320 contacts the temperature-induced phase change material, the spring can press the contact of the probe 320 against the surface of the temperature-induced phase change material to prevent it from detaching.

[0069] An embodiment of the present invention also provides a testing system for thermotropic phase change materials, including a testing device for thermotropic phase change materials and an XRD diffractometer as described above, wherein the device body of the testing device includes a docking clamp 400, and the testing device can be detachably connected to the XRD diffractometer through the docking clamp 400.

[0070] In a specific embodiment, the present invention is further described by taking the temperature-dependent phase change material VO2 as an experimental material.

[0071] VO2 is a classic temperature-induced phase change material, which transforms from a low-temperature monoclinic phase (M phase) to a high-temperature rutile tetragonal phase (R phase) at around 68°C. At the same time, the resistivity, magnetic susceptibility, light transmittance and reflectivity also undergo mutations, showing a reversible change from insulator to metal.

[0072] Experimental steps: Step 1: The test device provided by the present invention is installed and fixed on an XRD diffractometer through a docking fixture 400. The model of the XRD diffractometer may be Malvern PANalytical Empyrean.

[0073] Step 2: Place the VO2 thin film sample (2wt% doped in alumina) at the heating end of the heating assembly, then adjust the position of the contacts of a pair of conductive probe assemblies so that the contacts of the conductive probe assemblies contact the upper surface of the VO2 thin film sample, and start the test software to begin recording the real-time resistance value of the sample VO2 thin film sample.

[0074] Step 3: The test software in the automated control system controls the temperature of the heating component. The temperature control program is as follows: heat up from room temperature to the target temperature of 40°C (heating rate 10°C per minute), and keep warm after reaching the target temperature for 8 minutes. Then, repeat the above operation to set the target temperature to 50°C, 60°C, 65°C, 70°C, 75°C, and 80°C. After reaching 80°C and keeping warm, control the heating component to cool down, and the target temperature is set to 75°C, 70°C, 65°C, 60°C, 50°C, and 40°C.

[0075] Step 4. During each heat preservation process in step 3, operate the XRD diffractometer to perform XRD scanning (2θ scanning: 24° to 30°, using Cu Kα radiation (λ=1.5405Å)) on the VO2 thin film sample and record the changes in the VO2 crystal phase peak position.

[0076] Experimental results: From Figure 4 From the temperature-resistance curve of VO2, we can see that during the heating process, in the range of 40℃-60℃, as the temperature rises, the resistance value of the sample slowly decreases, and when the temperature rises to the range of 60℃-80℃, it can be observed that the resistance value drops sharply, from hundreds of kilo-ohms to thousands of kilo-ohms, and the resistance value drops by two orders of magnitude, which is the transition from insulator to metal. The cooling process also shows the opposite change in resistance value, and the resistance value rises sharply in the range of 80℃-60℃, which is the transition from metal to insulator, showing the reversible temperature-induced resistance change phenomenon of VO2.

[0077] from Figure 5 The in-situ variable temperature XRD spectrum of VO2 shows that the diffraction peak near 2θ=27.6° has shifted and changed in intensity. At low temperatures (less than 60°C), the position of this diffraction peak corresponds to the (011) crystal plane of the low-temperature insulating phase (M phase), and when the temperature rises above 65°C, the position of this diffraction peak shifts to the (110) crystal plane of the metallic phase (R phase), showing the phase change process of VO2.

[0078] This experiment verifies the application value of the test system for temperature-induced phase change materials provided by the present invention in the research of temperature-induced phase change materials, and successfully captures the electrical and structural change characteristics of VO2 materials caused by phase change during temperature change. The lattice transformation caused by temperature change is observed, which further confirms the synergistic relationship between electrical property change and structural change.

[0079] The testing system for temperature-induced phase change materials provided by the present invention realizes in-situ XRD testing in conjunction with an XRD diffractometer on the basis of synchronous measurement of temperature control and electrical properties, thereby overcoming the defect of the prior art that the key property of electrical properties cannot be synchronously tested in-situ, and provides reliable structure-activity relationship data support for studying the changes in the crystal phase structure and electrical properties of temperature-induced phase change materials.

[0080] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them; although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application, and they should all be included in the scope of the claims and specification of the present application. In particular, as long as there is no structural conflict, the various technical features mentioned in the various embodiments can be combined in any way. The present application is not limited to the specific embodiments disclosed herein, but includes all technical solutions that fall within the scope of the claims.

Claims

1. A testing device for thermotropic phase change materials, characterized in that: include: A device body, the device body being used for detachably connecting with an XRD diffractometer; A heating component is arranged on the device body, and a heating end of the heating component is used to contact the temperature-dependent phase change material to change the temperature of the temperature-dependent phase change material and detect the temperature value of the temperature-dependent phase change material; A pair of conductive probe assemblies, arranged on the device body, the contacts of each group of the conductive probe assemblies are used to contact the temperature-induced phase change material, and the contacts of the two groups of the conductive probe assemblies are spaced a certain distance apart; The automatic control system comprises a program temperature control module, a temperature acquisition module, an electric signal acquisition module, an XRD data acquisition module and a data processing module, wherein the program temperature control module and the temperature acquisition module are both connected to the heating component, the program temperature control module is used to control the heating temperature of the heating component to rise or fall, and is used to control the heating component to keep warm for a preset time at a preset temperature, the temperature acquisition module collects and records the temperature value of the temperature-induced phase change material in real time through the heating component, the electric signal acquisition module is connected to the conductive probe component, the electric signal acquisition module is used to collect and record the electric signal between two groups of the conductive probe components in real time, the XRD data acquisition module is used to connect to the XRD diffractometer, the XRD data acquisition module is used to collect and record XRD data when the program temperature control module executes a heat preservation instruction, the program temperature control module, the temperature acquisition module, the electric signal acquisition module and the XRD data acquisition module are all connected to the data processing module, and the data processing module outputs the corresponding relationship between the temperature value, the electric signal and the XRD data based on the temperature value, the electric signal and the XRD data.

2. The testing device for thermotropic phase change material according to claim 1, characterized in that: The heating component comprises a heater (210), a heating platform (220) and a temperature detector; the heater (210) is communicatively connected to the program temperature control module; the temperature detector is communicatively connected to the temperature acquisition module; the heater (210) is used to control the temperature of the temperature-dependent phase change material to rise or fall under the control of the program temperature control module, and to control the heater (210) to keep the temperature for a preset time period when the temperature of the temperature-dependent phase change material reaches a preset temperature; the temperature detector is used to detect the temperature value of the temperature-dependent phase change material; and the heating platform (220) is arranged at the heating end of the heater (210).

3. The testing device for thermotropic phase change material according to claim 2, characterized in that: The device body comprises a heat-insulating support assembly, the heater (210) is arranged in the heat-insulating support assembly, and the heating end of the heater (210) extends upward to the outside of the heat-insulating support assembly.

4. The testing device for thermotropic phase change material according to claim 3, characterized in that: The conductive probe assembly includes a probe and an adjustment bracket, the probe is connected to the device body through the adjustment bracket, the adjustment bracket is used to adjust and fix the position of the contact of the probe, and the probe is communicatively connected to the electrical signal acquisition module.

5. The testing device for thermotropic phase change material according to claim 4, characterized in that: The adjustment bracket includes a height adjustment mechanism and a horizontal position adjustment mechanism which are connected to each other. One of the height adjustment mechanism and the horizontal position adjustment mechanism is connected to the device body, and the other is connected to the probe.

6. The testing device for thermotropic phase change material according to claim 5, characterized in that: The height adjustment mechanism comprises a first rotating shaft (610) and an eccentric rotating arm (620); the first rotating shaft (610) is rotatably connected to the device body, and the rotation axis of the first rotating shaft (610) is parallel to the heating platform (220); there is damping between the first rotating shaft (610) and the device body; one end of the eccentric rotating arm (620) is non-rotatably connected to the first rotating shaft (610); the other end of the eccentric rotating arm (620) extends radially along the first rotating shaft (610) and is connected to the probe via the horizontal position adjustment mechanism.

7. The testing device for thermotropic phase change material according to claim 6, characterized in that: The horizontal position adjustment mechanism comprises a second rotating shaft (710), the second rotating shaft (710) being rotatably connected to one end of the eccentric rotating arm (620) away from the first rotating shaft (610), the rotating axis being parallel to the rotating axis of the first rotating shaft (610), and there being damping between the second rotating shaft (710) and the eccentric rotating arm (620), the probe being inserted through one end of the second rotating shaft (710) away from the eccentric rotating arm (620), and the axis of the probe being perpendicular to the axis of the second rotating shaft (710).

8. The testing device for thermotropic phase change material according to claim 4, characterized in that: The probe is a gold-plated probe.

9. The testing device for thermotropic phase change material according to claim 4, characterized in that: The probe comprises a probe body (310) and a probe head (320); the tail end of the probe head (320) is slidably inserted into the probe body (310); a spring is provided between the probe body (310) and the tail end of the probe head (320); the spring is used to provide a force for the probe head (320) to extend outward from the probe body (310).

10. A testing system for a thermotropic phase change material, characterized in that: It comprises a testing device for thermotropic phase change materials and an XRD diffractometer as claimed in any one of claims 1 to 9, wherein the device body of the testing device comprises a docking clamp (400), and the docking clamp (400) is used to be detachably connected to the XRD diffractometer.

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