A measuring device for the phase transition temperature of a thin film material

Abstract

An embodiment of the present invention discloses a measuring device for the phase transition temperature of a thin film material, comprising: an optical component; a vacuum chamber, an incident light hole is formed at the top of the vacuum chamber, and the incident light hole is disposed opposite to the incident light of the optical component; a high-temperature furnace, the high-temperature furnace is disposed in the vacuum chamber, and resistance heating sheets are installed at the bottom and side of the high-temperature furnace, and the resistance heating sheets are connected to a power supply through wires; a sample chamber, the sample chamber is disposed in the high-temperature furnace, the sample chamber is thermally connected to the resistance heating sheet through a heat conduction structure, and a sample is placed in the sample chamber, a thermocouple is embedded in the sample chamber and is in contact with the sample through a probe. It improves the measurement accuracy of the phase transition temperature of the thin film material.

Description

Technical Field

[0001] The present invention relates to the technical field of methods for measuring the properties of thin film materials, and particularly to an apparatus for measuring the phase transition temperature of thin film materials. Background Art

[0002] The information provided in this section is only background information related to the present disclosure, and it is not necessarily prior art.

[0003] Since the properties of thin film materials are different from those of bulk materials and are affected by various factors such as size, stress, and film thickness, the accurate measurement of the phase transition temperature is of great significance for the preparation and development of thin film materials with excellent properties. The traditional methods for studying the phase transition temperature characteristics of thin films are, one is to theoretically calculate using thermodynamic equations, and the other is to experimentally obtain the phase transition temperature by measuring the changes in other properties such as optical and acoustic properties during the temperature change process of the thin film material.

[0004] Currently, the apparatus for measuring the phase transition temperature of thin film materials includes a high-temperature furnace cavity, an infrared heater, a support frame for placing samples, and a thermocouple. The support frame is connected to the cavity door of the high-temperature furnace cavity. During measurement, the sample is placed in the sealed high-temperature furnace cavity, the thermocouple is placed on the surface of the thin film material sample, and the thin film material is heated by the infrared heater while recording the reflected light power on the sample surface and plotting a curve. Since the reflected light power of the thin film material changes significantly during the phase transition, the inflection point on the curve is the phase transition point of the thin film material, and the corresponding temperature is the phase transition temperature.

[0005] However, in the existing measurement apparatus, the sample is placed on the support frame, and the support frame is connected to the cavity door of the high-temperature furnace cavity. Then, each time the sample is introduced, the position of the sample will move; during the heating process, due to the principle of thermal expansion and contraction, the support frame will also undergo a small deformation, resulting in a change in the position of the sample, thereby causing a change in the optical path due to the change in the sample position, which affects the measurement accuracy. And since the sample is sent in on the support frame, the position of the sample will change during each measurement, and the optical path needs to be manually adjusted, so the consistency of the measurement results cannot be guaranteed.

[0006] Moreover, currently, the heating method of the high-temperature furnace is usually infrared heating, which makes the temperature field in the high-temperature furnace linearly distributed. This will cause the actual temperature on the surface of the thin film to be inconsistent with the measured temperature of the thermocouple, and during repeated measurements, it will lead to inaccurate measurement of the phase transition temperature. And during infrared heating, the four infrared heating tubes are distributed in four directions of the sample. Since it is linear radiation heating, there will be a certain distribution difference among the four heating tubes, so it will cause uneven temperature distribution and affect the accuracy of the measurement results.

[0007] Meanwhile, during the measurement process, the thermocouple probe is only placed on the surface of the sample, and it is considered that the two are in contact during the measurement process. However, in the actual measurement process, there is no contact pressure between the probe of the thermocouple and the sample. Therefore, the temperature measured by this temperature measurement method is not the true temperature of the sample surface, which also greatly affects the accurate measurement of the phase transition temperature of the thin film material. Moreover, during the measurement, only one probe of the thermocouple is used to measure the temperature of a point on the surface of the sample, while the sample has a certain area, and the measured temperature cannot fully represent the actual temperature of the sample surface.

[0008] In addition, in the prior art, a quartz glass tube is used as the vacuum chamber. On the one hand, using a quartz tube will result in a low vacuum degree in the chamber, which will cause the sample to oxidize during the heating process, and its oxides will contaminate the tube wall, resulting in a decrease in the light transmittance. On the other hand, the circular structure of the glass tube requires the laser to be perpendicularly incident at the center point of the quartz tube, making it difficult to adjust the optical path. Moreover, the vacuum degree in the high-temperature furnace is low, and no inert protective gas is filled, so the sample will oxidize during the heating process, resulting in inaccurate measurement results, and the uniformity and stability of the temperature field distribution have an impact on the accuracy of the measurement results. Summary of the Invention

[0009] Therefore, an embodiment of the present invention provides a device for measuring the phase transition temperature of a thin film material to solve the technical problem of poor accuracy of the measurement result of the phase transition temperature of the thin film material in the prior art.

[0010] In order to achieve the above object, the embodiment of the present invention provides the following technical solutions:

[0011] A device for measuring the phase transition temperature of a thin film material, comprising:

[0012] An optical component;

[0013] A vacuum chamber, an incident light hole is opened at the top of the vacuum chamber, and the incident light hole is arranged opposite to the incident light of the optical component;

[0014] A high-temperature furnace, the high-temperature furnace is arranged in the vacuum chamber, resistance heating sheets are installed at the bottom and side of the high-temperature furnace, and the resistance heating sheets are connected to a power supply through wires;

[0015] A sample chamber, the sample chamber is arranged in the high-temperature furnace, the sample chamber is thermally connected to the resistance heating sheet through a heat conduction structure, and a sample is placed in the sample chamber, a thermocouple is embedded in the sample chamber, and is in contact with the sample through a probe.

[0016] Further, the optical component includes:

[0017] A support frame;

[0018] A laser generator, which is installed on the top of the support frame;

[0019] A beam splitter. The light emitted by the laser generator is split by the beam splitter to form the incident light and the reflected light. The incident light is incident on the sample in the sample chamber through the light incident hole;

[0020] A photodetector, which receives the reflected light to obtain the reflectivity through the photodetector.

[0021] Further, the optical component further includes:

[0022] An optical path automatic calibration module, which images the laser spot and automatically adjusts the angle of the laser through calculation and analysis of the image to achieve automatic calibration of the optical path.

[0023] Further, the optical path automatic calibration module includes:

[0024] An image sensor, which is arranged on one side of the beam splitter and is used to image the laser spot;

[0025] A three-dimensional adjuster, which is connected to the laser generator and automatically adjusts the angle of the laser through calculation and analysis of the image to achieve automatic calibration of the optical path.

[0026] Further, the vacuum chamber has a high-temperature resistant metal outer wall.

[0027] Further, air holes are provided on the metal outer wall of the vacuum chamber, and the air holes are connected to the pumping device or the gas filling device through pipelines.

[0028] Further, water cooling holes are provided on the metal outer wall of the vacuum chamber, and the water cooling holes are connected to the water cooler through pipelines.

[0029] Further, an accessory box is further included, and the power supply, the driving module of the optical component, and the control module of the optical component are all installed in the accessory box.

[0030] Further, the driving module of the optical component includes a photoelectric driving module and a laser driving module;

[0031] The control module of the optical component includes a control panel, a master control module, a digital acquisition module, and a PID control module.

[0032] Further, a heat dissipation module is also installed in the accessory box.

[0033] In one or more embodiments, the measuring device for the phase change temperature of the thin film material provided by the present invention has the following technical effects: through the improvement of the high-temperature furnace structure, the temperature distribution uniformity in the high-temperature furnace is improved; and by setting a directly contacting sample chamber in the high-temperature furnace and embedding the thermocouple into the sample chamber, the thermocouple is in true contact with the sample, ensuring that the high-temperature furnace, the sample chamber and the sample are heated synchronously, improving the heating uniformity and ensuring the accuracy of the detection results. At the same time, since the sample is loaded into the sample chamber, the measurement position of the sample is fixed, and the sample position remains unchanged during repeated measurements, ensuring the consistency of the sample position during multiple measurements, thereby improving the measurement accuracy.

[0034] Furthermore, since heating sheets are provided on both the side and the bottom of the high-temperature furnace, multi-point measurement is realized, solving the problems that single-point temperature measurement cannot truly represent the surface temperature of the sample and the non-uniform temperature distribution caused by the sample heating method; during the measurement process, the vacuum chamber environment is stable, making the measurement environment (vacuum degree, protective gas) stable and avoiding the problem that the measurement environment affects the measurement accuracy; the setting of the optical component makes it possible to automatically adjust the optical path and avoid the problem of inaccurate measurement caused by manual calibration of the optical path. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only exemplary, and for those of ordinary skill in the art, without creative efforts, other implementation drawings can be obtained according to the provided drawings.

[0036] The structures, ratios, sizes, etc. shown in this specification are only used to cooperate with the content disclosed in the specification for those who are familiar with this technology to understand and read, and are not used to limit the limiting conditions for the implementation of the present invention. Therefore, they do not have technical essence. Any modification of the structure, change of the proportional relationship or adjustment of the size, without affecting the effects that the present invention can produce and the purposes that can be achieved, should still fall within the scope covered by the technical content disclosed by the present invention.

[0037] Figure 1 It is a schematic structural diagram of the measuring device for the phase change temperature of the thin film material provided by the present invention;

[0038] Figure 2 is Figure 1 The structural schematic diagram of other accessories shown in the measuring device.

[0039] Description of the reference numerals:

[0040] 1 - Control panel 2 - Master control module 3 - PID control module 4 - Heat dissipation module 5 - Power supply

[0041] 6 - Digital acquisition module 7 - Photoelectric drive module 8 - Thermocouple 9 - Vacuum chamber 10 - Air hole

[0042] 11 - Photoelectric detector 12 - Three - dimensional regulator 13 - Laser generator 14 - Beam splitter

[0043] 15 - Support frame 16 - Light inlet hole 17 - High - temperature furnace 18 - Sample chamber 19 - Water - cooling hole 20 - Vacuum gauge

[0044] 21 - Laser driver module Specific implementation mode

[0045] The following specific embodiments illustrate the implementation manners of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0046] The measuring device for the phase transition temperature of the thin - film material provided by the present invention is provided with a sample chamber 18, so as to truly measure the temperature of the sample in contact, making the measured temperature closer to the true temperature of the sample surface. And through solutions such as the vacuum chamber 9, heating method, sample injection method, optical path adjustment method, vacuum degree, multi - point temperature measurement, etc., the condition consistency during repeated measurements can be ensured, making the measurement results more stable.

[0047] In a specific implementation manner, as Figure 1 shown, the measuring device for the phase transition temperature of the thin - film material provided by the present invention includes an optical component, a vacuum chamber 9, a high - temperature furnace 17 and a sample chamber 18. Among them, a light inlet hole 16 is opened at the top of the vacuum chamber 9, and the light inlet hole 16 is arranged opposite to the incident light of the optical component; the vacuum chamber 9 has a heat - resistant metal outer wall, and the vacuum chamber 9 is enclosed by the metal outer wall to form a sealed vacuum chamber 9. An air hole 10 is opened on the metal outer wall of the vacuum chamber 9, and the air hole 10 is connected to the pipeline of the air extraction device or the gas filling device to realize air extraction and inflation. A water - cooling hole 19 is also opened on the metal outer wall of the vacuum chamber 9, and the water - cooling hole 19 is connected to the pipeline of the water cooler to facilitate the introduction of cooling water.

[0048] The high - temperature furnace 17 is arranged inside the vacuum chamber 9. Resistance heating sheets are installed at the bottom and side of the high - temperature furnace 17. The resistance heating sheets are connected to the power supply through wires. After the resistance heating sheets are powered on, they can generate heat, and appropriate range of uniform heating can be realized by selecting the specifications of the resistance heating sheets.

[0049] A sample chamber 18 is newly added to the measuring device. The sample chamber 18 is arranged inside the high-temperature furnace 17. The sample chamber 18 is thermally connected to the resistance heating sheet through a heat conduction structure. A sample is placed inside the sample chamber 18. The thermocouple 8 is embedded in the sample chamber 18 and is in contact with the sample through a probe.

[0050] In this way, first, the vacuum chamber 9 and the heating method are transformed. The original quartz glass tube is transformed into a high-temperature-resistant metal outer wall, thereby improving the airtightness of the entire cavity and increasing the vacuum degree. The infrared heating is transformed into resistance heating. Resistance heating sheets are provided at both the bottom and the side of the high-temperature furnace 17. There is a fixed sample chamber 18 inside the cavity to ensure that the position is consistent each time a sample is placed. And, a flat optical incident window (i.e., the light incident hole 16) is provided above the vacuum chamber 9, which is conducive to the adjustment of the optical path. Fourth, due to the good airtightness and high vacuum degree, the sample is not easily oxidized after filling with the protective gas, and the optical window is not easily polluted. Fifth, the three-sided overall heating makes the temperature distribution inside the cavity more uniform. Sixth, since the sample is placed at the bottom of the vacuum furnace during the heating process, its thermal deformation is relatively very small, which can greatly reduce the influence on the optical path during the measurement process.

[0051] The above-mentioned sample chamber 18 for placing the sample is welded to the heating plate through a heat-conducting material, which belongs to contact heat conduction. The sample is placed in the sample chamber 18. Through the structural design, the sample is in full contact with the sample chamber 18. The thermocouple 8 is embedded in the sample chamber 18, so it is also in contact. In this way, the sample, the thermocouple 8, and the heating resistor are integrated through the connection of the sample chamber 18, and the measured temperature remains consistent. The temperature measured by the thermocouple 8 is closer to the true temperature of the sample surface. Since the sample chamber 18 itself is a small airtight environment, the temperature inside it is more uniform, and the temperature measurement accuracy can be guaranteed in the high-temperature region. Since a sample chamber 18 is added, multiple thermocouples 8 can be distributed inside the high-temperature heating furnace, so that the temperature inside the furnace can be characterized more comprehensively and accurately.

[0052] Specifically, the above-mentioned optical component includes a support frame 15, a laser generator 13, a beam splitter 14, and a photodetector 11. Among them, the laser generator 13 is installed on the top of the support frame 15. The light emitted by the laser generator 13 is split by the beam splitter 14 to form the incident light and the reflected light. The incident light is incident on the sample in the sample chamber 18 through the light incident hole 16, and the photodetector 11 receives the reflected light to obtain the reflectivity through the photodetector 11.

[0053] During the working process, the laser emitted by the laser 13 serves as the incident light and is incident on the sample in the sample chamber 18 of the high-temperature furnace 17 through the beam splitter 14. Its reflected light passes through the beam splitter 14, and the reflectance is detected by the photoelectric detection module 11. The high-temperature furnace 17 heats the sample as required. When heated to a certain temperature, the crystal phase of the thin film material changes, and its optical reflectance also changes accordingly. By recording the temperature at the moment when the reflectance changes, the phase transition temperature of the thin film material is obtained.

[0054] The optical component further includes an optical path automatic calibration module. The optical path automatic calibration module images the laser spot and automatically adjusts the angle of the laser through the calculation and analysis of the image to achieve automatic calibration of the optical path. Specifically, the optical path automatic calibration module includes an image sensor and a three-dimensional adjuster 12. The image sensor is disposed on one side of the beam splitter 14 and is used to image the laser spot. The three-dimensional adjuster 12 is connected to the laser generator 13 and automatically adjusts the angle of the laser through the calculation and analysis of the image to achieve automatic calibration of the optical path.

[0055] That is to say, a three-dimensional adjuster 12 is added at the laser, and a CCD is added at the other end of the beam splitter 14 to image the laser spot. The angle of the laser is automatically adjusted through the calculation and analysis of the image to achieve automatic calibration of the optical path. In this way, the optical path can be adjusted in a quantitative manner to ensure the consistency of repeated measurements.

[0056] It should be understood that in order to achieve its basic functions, the optical component needs to be provided with a power supply 5 (this power supply can also be used as the power supply for the resistance heating sheet), a drive module, and a control module. For the convenience of installation and setting, as Figure 2 shown, the above-mentioned power supply 5, the drive module of the optical component, and the control module of the optical component are all installed in the accessory box. In addition, a heat dissipation module 4 and a vacuum gauge 20 are also installed in the accessory box.

[0057] Specifically, the drive module of the optical component includes a photoelectric drive module 7 and a laser drive module 21, and the control module of the optical component includes a control panel 1, a master control module 2, a digital acquisition module 6, and a PID control module 3.

[0058] In one or more of the above embodiments, the measuring device for the phase change temperature of the thin film material provided by the present invention has the following technical effects: By improving the structure of the high-temperature furnace 17, the temperature distribution uniformity in the high-temperature furnace 17 is improved; and, by providing a directly contacting sample chamber 18 in the high-temperature furnace 17 and embedding the thermocouple 8 into the sample chamber 18, the thermocouple 8 is in real contact with the sample, ensuring that the high-temperature furnace 17, the sample chamber 18 and the sample are heated synchronously, improving the heating uniformity and ensuring the accuracy of the detection results. At the same time, since the sample is loaded into the sample chamber 18, the measurement position of the sample is fixed, and the sample position remains unchanged during repeated measurements, ensuring the consistency of the sample position during multiple measurements, thereby improving the measurement accuracy.

[0059] Since heating sheets are provided on both the side and the bottom of the high-temperature furnace 17, multi-point measurement is achieved, solving the problems that single-point temperature measurement cannot truly represent the surface temperature of the sample and that the temperature distribution is uneven due to the sample heating method; during the measurement process, the environment in the vacuum chamber 9 is stable, making the measurement environment (vacuum degree, protective gas) stable and avoiding the problem that the measurement environment affects the measurement accuracy; the setting of the optical component makes it possible to automatically adjust the optical path, avoiding the problem of inaccurate measurement caused by manual calibration of the optical path.

[0060] The above specific embodiments have further elaborated on the purpose, technical solution and beneficial effects of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not used to limit the protection scope of the present invention. Any modifications, equivalent replacements, improvements, etc. made on the basis of the technical solution of the present invention shall be included in the protection scope of the present invention.

Claims

1. A measuring device for the phase transition temperature of a thin film material, characterized in that, it includes: an optical component; a vacuum chamber, an incident light hole is opened at the top of the vacuum chamber, and the incident light hole is arranged opposite to the incident light of the optical component; a high-temperature furnace, the high-temperature furnace is arranged in the vacuum chamber, resistance heating sheets are installed at the bottom and on the side of the high-temperature furnace, and the resistance heating sheets are connected to a power supply through wires; a sample chamber, the sample chamber is arranged in the high-temperature furnace, the sample chamber is thermally connected to the resistance heating sheet through a heat conduction structure, and a sample is placed in the sample chamber, a thermocouple is embedded in the sample chamber and is in contact with the sample through a probe; the sample chamber is a sealed chamber arranged in the high-temperature furnace.

2. The measuring device according to claim 1, characterized in that, the optical component includes: a support frame; a laser generator, the laser generator is installed on the top of the support frame; a beam splitter, the light emitted by the laser generator is split by the beam splitter to form the incident light and the reflected light, and the incident light is incident on the sample in the sample chamber through the incident light hole; a photodetector, the photodetector receives the reflected light to obtain the reflectivity through the photodetector.

3. The measuring device according to claim 2, characterized in that, the optical component further includes: an optical path automatic calibration module, the optical path automatic calibration module images the laser spot, and automatically adjusts the angle of the laser through calculation and analysis of the image to achieve automatic calibration of the optical path.

4. The measuring device according to claim 3, characterized in that, the optical path automatic calibration module includes: an image sensor, the image sensor is arranged on one side of the beam splitter and is used for imaging the laser spot; a three-dimensional adjuster, the three-dimensional adjuster is connected to the laser generator and automatically adjusts the angle of the laser through calculation and analysis of the image to achieve automatic calibration of the optical path.

5. The measuring device according to claim 1, characterized in that, the vacuum chamber has a high-temperature resistant metal outer wall.

6. The measuring device according to claim 5, characterized in that, air holes are opened on the metal outer wall of the vacuum chamber, and the air holes are connected to the pipeline of a pumping device or an inflation device.

7. The measuring device according to claim 5, characterized in that, water cooling holes are opened on the metal outer wall of the vacuum chamber, and the water cooling holes are connected to the pipeline of a water cooler.

8. The measuring device according to any one of claims 1-7, characterized in that, it further includes an accessory box, and the power supply, the drive module of the optical component, and the control module of the optical component are all installed in the accessory box.

9. The measuring device according to claim 8, characterized in that, the drive module of the optical component includes a photoelectric drive module and a laser drive module; the control module of the optical component includes a control panel, a master control module, a digital acquisition module, and a PID control module.

10. The measuring device according to claim 8, characterized in that, a heat dissipation module is further installed in the accessory box.

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