Optical integrated thin film material phase transition temperature measuring device and optical integrated thin film material phase transition temperature measuring method

Through the optically integrated phase change temperature measurement device of thin film material, the problems of cumbersome operation of optical devices and large errors in measurement results in traditional methods are solved, and the accuracy and diversity of phase change temperature measurement is achieved, and the film material can be accurately analyzed. Chemical composition and molecular structure.

CN119147580AInactive Publication Date: 2024-12-17NATIONAL INSTITUTE OF METROLOGY CHINA +1
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Patent Information

Application Number
CN202411323925.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-23
Publication Date
2024-12-17
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The traditional thin film material phase change temperature measurement method has problems such as cumbersome operation of optical devices, large errors in measurement results and single measurement performance, and it is impossible to accurately determine the crystal state of the material.

Method used

The phase change temperature measurement device of thin film material with integrated optical arrangement includes an optical component fixing frame and a vacuum cavity. The optical component is fixed by a flange, and a photodetector, spectroscopy component, focusing mirror, CCD sensor and laser are provided to achieve laser accuracy. Accurate detection of direct incident and reflected light signals.

Benefits of technology

The phase change temperature measurement process of phase change film materials is simplified, the measurement accuracy and versatility are improved, and chemical composition and molecular structure can be accurately analyzed.

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Abstract

The invention discloses an optically integrated thin film material phase transition temperature measuring device and method, and belongs to the technical field of thin film thermal performance detection.The optically integrated thin film material phase transition temperature measuring device comprises an optical assembly fixing frame and a vacuum cavity, and the vacuum cavity is connected to the lower portion of the optical assembly fixing frame through a flange; a photoelectric detector, a first light splitting assembly, a second light splitting assembly, a first focus lens, a CCD sensor, a reflective mirror, a second focus lens and a laser are arranged on the optical assembly fixing frame; the second light splitting assembly is arranged at the transmitting end of the laser, the first focus lens is arranged below the second light splitting assembly, the first light splitting assembly and the photoelectric detector are sequentially arranged above the second light splitting assembly, and the second focus lens and the reflective mirror are sequentially arranged on the right side of the first light splitting assembly. The process of measuring the phase-change temperature of the phase-change film material is simplified, and meanwhile, the accuracy and diversity of measuring the phase-change temperature of the phase-change film material are improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of thin film thermal performance detection, and in particular relates to a thin film material phase change temperature measurement device and method with an optically integrated arrangement. Background Art

[0002] At present, the traditional thin film material phase change temperature measurement method is usually based on technologies such as thermocouples or infrared sensors, but these methods have some problems. For example, the optical reflection power receiving module of the existing phase change thin film material thermal performance test is separated from the furnace cavity in the lower part of the instrument. Due to the looseness of the sample position or the shaking of the optical path part relative to the furnace cavity part, the optical path will not be fixed in each experiment, resulting in the optical path not being collimated on the sample. Therefore, it takes time to debug the instrument every time an experiment is performed, which will also lead to poor accuracy of the test results. However, after testing, it was found that only when the light is vertically irradiated on the sample in the heating furnace can the optical power be minimized and the change of optical power be fed back in time. Therefore, the optical part and the heating part of the instrument must have an exact position and be fixed, so this is a challenge faced in the thermal performance test of phase change thin film materials; in addition, Raman spectroscopy analysis will be considered. Raman spectroscopy analysis is a modern spectral analysis method. The Raman characteristic peaks corresponding to different crystal phases of the same substance are different. Therefore, the thin film sample is heated, its Raman peak is measured at different temperatures, and then the crystal state is judged according to the Raman characteristic peak. For the same material, its Raman characteristic peak at a certain temperature may be significantly different from the Raman characteristic peak measured after annealing it to room temperature. Therefore, the traditional Raman spectrometer can only measure the Raman signal at room temperature. The optical power module can only measure the phase change temperature of the thin film material, but cannot accurately determine the crystal state of the material. Therefore, the current instrument is only used to detect the light reflection power and then output the light signal, and the test task is single. Therefore, there is an urgent need for a thin film material phase change temperature measurement device and method with an optical integrated setting to simplify the process of measuring the phase change temperature of the phase change thin film material and improve the accuracy of the phase change temperature measurement. Summary of the invention

[0003] The purpose of the present invention is to provide an optically integrated thin film material phase change temperature measurement device and method to solve the problems of the above-mentioned technology that the optical device of the existing instrument is cumbersome to operate, the measurement result has large errors and the measurement performance is single.

[0004] To achieve the above-mentioned purpose, the present invention provides a thin film material phase change temperature measuring device with an optical integrated setting, comprising an optical component fixing frame and a vacuum chamber, wherein the vacuum chamber is connected to the bottom of the optical component fixing frame through a flange; a photodetector, a first spectroscopic component, a second spectroscopic component, a first focusing mirror, a CCD sensor, a reflector, a second focusing mirror and a laser are arranged on the optical component fixing frame; the second spectroscopic component is arranged at the emitting end of the laser, the first focusing mirror is arranged below the second spectroscopic component, the first spectroscopic component and the photodetector are arranged above the second spectroscopic component in sequence, and the second focusing mirror and the reflector are arranged on the right side of the first spectroscopic component in sequence.

[0005] Preferably, a heating cavity is provided in the vacuum cavity, a sample stage is provided in the heating cavity, and a sample stage receiving frame is provided above the vacuum cavity and between the sample stage.

[0006] Preferably, the photoelectric detector detects the laser reflected by the sample to be tested through the first focusing mirror, the second beam splitter component and the first beam splitter component, and converts the optical signal into an electrical signal for output.

[0007] Preferably, the CCD sensor receives the laser reflected by the sample to be tested through the first focusing mirror, the second beam splitting component, the first beam splitting component, the second focusing mirror, and the reflector, and finally outputs a Raman signal.

[0008] Preferably, the first beam splitter component and the second beam splitter component have exactly the same structure, and both include a beam splitter frame and a beam splitter.

[0009] The present invention also provides a method for measuring the phase transition temperature of a thin film material with an optically integrated arrangement, comprising the following steps:

[0010] Step 1: The laser emits a laser beam to the left through the second beam splitter component. The second beam splitter component splits the incident laser into two parts. One part directly passes through the second beam splitter component horizontally to the left, and the other part passes through the first focusing mirror horizontally downward under the action of the second beam splitter component and is incident on the surface of the sample stage. The optical path is adjusted so that the first beam splitter component and the sample are on the same axis. In this way, the laser can be collimated and incident on the sample, thereby ensuring that the reflected laser and the incident laser coincide, which is convenient for subsequent experiments.

[0011] Step 2: The sample stage surface reflects the incident laser upward into the first focusing mirror, the second spectrometer, and the first spectrometer; then the reflected laser from the first spectrometer is divided into two paths, one path goes horizontally upward to the photodetector to detect the reflected light power change signal, and the other path of reflected light signal goes horizontally to the right through the second focusing mirror and the reflector and then reaches the CCD sensor to detect its Raman signal.

[0012] Therefore, the present invention adopts the above-mentioned thin film material phase change temperature measurement device and method with an optically integrated setting, which has the following beneficial effects:

[0013] (1) Fix the optical component holder and the vacuum chamber through flanges to avoid errors caused by optical path deviation due to shaking, reduce the impact of the dry pump and other instruments on the optical device during the phase change temperature measurement of the phase change film material, and improve the accuracy of the phase change temperature measurement;

[0014] (2) The integrated design of optical components and the fixed optical path eliminate the need for frequent optical path adjustment, thus simplifying the process of measuring the phase change temperature of phase change thin film materials;

[0015] (3) The Raman signal of the thin film material is detected by the CCD sensor to analyze the chemical composition and molecular structure, thereby improving the versatility of the test device and increasing the diversity of overall applications.

[0016] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 This is a schematic diagram of the overall structure of an optically integrated thin film material phase change temperature measurement device of the present invention;

[0018] Figure 2 A schematic diagram of the internal structure of an optically integrated thin film material phase change temperature measurement device of the present invention;

[0019] Figure 3 It is a structural schematic diagram of the optical component fixing frame of the present invention;

[0020] Figure 4 is a schematic structural diagram of the first light splitting component of the present invention;

[0021] Figure 5 A schematic diagram of a method for measuring phase transition temperature of a thin film material with an optically integrated arrangement according to the present invention;

[0022] Among them; 1. optical component fixing frame; 2. flange; 3. vacuum chamber; 4. sample stage receiving frame; 5. heating chamber; 6. photoelectric detector; 7. first spectroscopic component; 71. spectroscope; 72. spectroscope frame; 8. second spectroscopic component; 9. first focusing mirror; 10. CCD sensor; 11. second focusing mirror; 12. reflector; 13. laser; 14. adjustment rod. DETAILED DESCRIPTION

[0023] The following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents selected embodiments of the present invention. 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.

[0024] See also Figure 1-4 , an optically integrated thin film material phase change temperature measuring device, comprising an optical component fixing frame 1 and a vacuum chamber 3, the vacuum chamber 3 is connected to the bottom of the optical component fixing frame 1 through a flange 2; a photodetector 6, a first light splitting component 7, a second light splitting component 8, a first focusing mirror 9, a CCD sensor 10, a reflector 12, a second focusing mirror 11 and a laser 13 are arranged on the optical component fixing frame 1; the second light splitting component 8 is arranged at the emission end of the laser 13, the first focusing mirror 9 is arranged below the second light splitting component 8, the first light splitting component 7 and the photodetector 6 are arranged above the second light splitting component 8 in sequence, and the second focusing mirror 11 and the reflector 12 are arranged on the right side of the first light splitting component 7 in sequence. A heating cavity 5 is arranged in the vacuum chamber 3, a sample stage is arranged in the heating cavity 5, and a sample stage receiving frame 4 is arranged between the top of the vacuum chamber 3 and the sample stage. The photodetector 6 detects the laser reflected by the sample to be measured through the first focusing mirror 9, the second light splitting component 8 and the first light splitting component 7, and converts the optical signal into an electrical signal for output. The CCD sensor 10 receives the laser reflected by the sample to be tested through the first focusing mirror 9, the second beam splitter assembly 8, the first beam splitter assembly 7, the second focusing mirror 11, and the reflector 12, and finally outputs a Raman signal. The first focusing mirror 9 and the second focusing mirror 11 are both used to improve the ability of the edge light beam to be incident on a point; using the same detector area can expand the field of view, increase the incident flux, and make the non-uniform illumination on the photosensitive surface of the detector uniform; the first beam splitter assembly 7 and the second beam splitter assembly 8 have the same structure, both including a beam splitter frame 72 and a beam splitter 71, and an adjustment rod 14 is arranged above the beam splitter frame 72, which can make slight adjustments to the angle of the beam splitter 71.

[0025] like Figure 5 , a method for measuring the phase transition temperature of a thin film material with an optically integrated arrangement, comprising the following steps:

[0026] Step 1, the laser 13 emits a laser beam to the left through the second beam splitter component 8, and the second beam splitter component 8 splits the incident laser into two parts, one part directly passes through the second beam splitter component 8 horizontally to the left, and the other part is horizontally downward through the first focusing mirror 9 under the action of the second beam splitter component 8 and enters the surface of the sample stage. The optical path is adjusted so that the second beam splitter component 8 and the sample are on the same axis, so that the laser can be collimated and incident on the sample, thereby ensuring that the reflected laser and the incident laser coincide, which is convenient for subsequent experiments;

[0027] Step 2, the sample stage surface reflects the incident laser upward into the first focusing mirror 9, the second spectroscopic component 8, and the first spectroscopic component 7; then the reflected laser from the first spectroscopic component 7 is divided into two paths, one path reaches the photodetector 6 horizontally upward to detect the reflected light power change signal, and the other path of reflected light signal horizontally to the right passes through the second focusing mirror 11 and the reflector 12 and then reaches the CCD sensor 10 to detect its Raman signal.

[0028] Therefore, the present invention adopts the above-mentioned optically integrated thin film material phase change temperature measurement device and method, which simplifies the process of phase change temperature measurement of phase change thin film materials, while improving the accuracy and diversity of phase change temperature measurement of phase change thin film materials, and solves the problems of cumbersome optical device operation, large measurement result errors and single measurement performance of existing instruments.

[0029] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solution of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solution to deviate from the spirit and scope of the technical solution of the present invention.

Claims

1. An optically integrated thin film material phase change temperature measurement device, characterized in that: It comprises an optical component fixing frame and a vacuum chamber, wherein the vacuum chamber is connected to the bottom of the optical component fixing frame through a flange; a photodetector, a first spectroscopic component, a second spectroscopic component, a first focusing mirror, a CCD sensor, a reflector, a second focusing mirror and a laser are arranged on the optical component fixing frame; the second spectroscopic component is arranged at the transmitting end of the laser, the first focusing mirror is arranged below the second spectroscopic component, the first spectroscopic component and the photodetector are arranged above the second spectroscopic component in sequence, and the second focusing mirror and the reflector are arranged on the right side of the first spectroscopic component in sequence.

2. The optically integrated thin film material phase transition temperature measuring device according to claim 1, characterized in that: A heating cavity is arranged in the vacuum cavity, a sample stage is arranged in the heating cavity, and a sample stage receiving frame is arranged between the upper part of the vacuum cavity and the sample stage.

3. The optically integrated thin film material phase transition temperature measuring device according to claim 1, characterized in that: The photoelectric detector detects the laser reflected by the sample to be tested through the first focusing mirror, the second light splitting component and the first light splitting component, and converts the optical signal into an electrical signal for output.

4. The optically integrated thin film material phase transition temperature measuring device according to claim 1, characterized in that: The CCD sensor receives the laser reflected by the sample to be tested through the first focusing mirror, the second light splitting component, the first light splitting component, the second focusing mirror, and the reflector, and finally outputs a Raman signal.

5. The optically integrated thin film material phase transition temperature measuring device according to claim 1, characterized in that: The first beam splitter component and the second beam splitter component have the same structure, and both include a beam splitter frame and a beam splitter.

6. A method for measuring the phase transition temperature of a thin film material with an optically integrated arrangement, characterized in that: The following steps are involved: Step 1: The laser emits a laser beam to the left through the second beam splitter assembly, and the second beam splitter assembly splits the incident laser into two parts, one part directly passes through the second beam splitter assembly horizontally to the left, and the other part, under the action of the second beam splitter assembly, passes through the first focusing mirror horizontally downward and is incident on the surface of the sample stage; Step 2: The sample stage surface reflects the incident laser upward into the first focusing mirror, the second spectrometer, and the first spectrometer; then the reflected laser from the first spectrometer is divided into two paths, one path goes horizontally upward to the photodetector to detect the reflected light power change signal, and the other path of reflected light signal goes horizontally to the right through the second focusing mirror and the reflector and then reaches the CCD sensor to detect its Raman signal.

Citation Information

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