Temperature-variable accessory for testing infrared temperature-variable reflectivity of thin film and testing method

Abstract

The invention belongs to the technical field of reflectivity spectral measurement, and discloses a variable temperature accessory for testing film infrared variable temperature reflectivity and a testing method.The variable temperature accessory comprises an insulating layer, a heating layer, a heat insulation layer and a metal clamp which are sequentially arranged in a laminated mode; wherein a power line is connected in the insulating layer; the heat insulation layer and the metal clamp are detachably mounted on the insulation layer, so that a to-be-tested film sample is mounted between the heating layer and the heat insulation layer; round holes are formed in the middle parts of the heat insulation layer and the metal clamp, so that part of the upper surface of the mounted thin film sample to be tested is exposed through the round holes to form a test area of the thin film sample to be tested. The variable-temperature accessory disclosed by the invention can be used for a Bruker VERTEX70 type microscopic infrared spectrometer, and can be combined with a specular reflection method to realize a micro-area test of variable-temperature infrared reflectivity of a thin film at 25-200 DEG C.

Description

Technical Field

[0001] The invention relates to the technical field of reflectivity spectrum measurement, and in particular to a variable temperature accessory and a testing method for testing infrared variable temperature reflectivity of a thin film. Background Art

[0002] Infrared optical materials are materials specially used to process or transmit infrared light. These materials have excellent optical and mechanical properties and are often used in infrared lasers, infrared sensors and other optical devices.

[0003] The infrared optical properties of infrared optical materials play an important role in promoting the application and development of infrared optical materials. Since Fourier transform infrared spectrometer (FTIR) can perform micro-area infrared analysis, failure analysis, and material infrared optical properties analysis, and has the advantages of easy operation, simple optical path, high resolution, fast scanning speed, high sensitivity, and the ability to measure reflection spectra, simple sample preparation, and non-destructive testing, it has become the main technical means for analyzing the infrared optical properties of infrared optical materials.

[0004] However, currently FTIR can usually only test the infrared reflectivity of thin films at room temperature, and the test area is usually large. Although there are variable temperature accessories for FTIR in the prior art, the variable temperature accessories in the current FTIR are mostly for ATR or other component analysis modes, and the reflectivity of the material cannot be characterized in these modes. However, the infrared reflection characteristics of existing infrared optical materials usually change with temperature, making it difficult to analyze the variable temperature infrared reflection characteristics through the variable temperature accessories in the prior art, and it is also unable to meet the micro-area reflectivity characterization requirements of some smaller optical devices. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a variable temperature accessory and a testing method for testing infrared variable temperature reflectivity of thin films. The present invention provides a variable temperature accessory that can be used with a Bruker VERTEX70 microscopic infrared spectrometer, and the variable temperature accessory of the present invention can be combined with a specular reflection method to achieve micro-area testing of the variable temperature infrared reflectivity of thin films at 25°C to 200°C.

[0006] The temperature-changing accessory and the testing method for testing the infrared temperature-changing reflectivity of a thin film of the present invention are realized by the following technical solutions:

[0007] The first object of the present invention is to provide a temperature-changing accessory for testing the infrared temperature-changing reflectivity of a thin film, comprising an insulating layer, a heating layer, a heat-insulating layer and a metal clamp.

[0008] It should be noted that, in the present invention, a power line is connected inside the insulating layer to facilitate the connection between the heating platinum wire and the control power supply.

[0009] In the present invention, the heating layer is arranged on the upper surface of the insulating layer to achieve the function of temperature control.

[0010] In the present invention, the heat insulating layer is arranged on the upper surface of the heating layer and can be detachably installed on the insulating layer, so that the film sample to be tested can be installed between the heating layer and the heat insulating layer.

[0011] In the present invention, the metal clamp is arranged on the upper surface of the thermal insulation layer and can be detachably mounted on the insulation layer, so as to facilitate the fixation of the thin film sample to be tested.

[0012] In the present invention, circular holes are provided in the middle of the heat insulating layer and the metal fixture, so that part of the upper surface of the installed film sample to be tested can be leaked out through the circular holes to form a test area of ​​the film sample to be tested.

[0013] In some preferred embodiments of the present invention, the overall height of the temperature variable attachment is 15 mm ± 0.2 mm, and the width is 40 mm ± 0.2 mm.

[0014] In some preferred embodiments of the present invention, the insulating layer is made of polytetrafluoroethylene.

[0015] In some preferred embodiments of the present invention, the thickness of the insulating layer is 10 mm±0.2 mm.

[0016] In some preferred embodiments of the present invention, the heating layer is made of nickel-chromium alloy.

[0017] In some preferred embodiments of the present invention, the thickness of the heating layer is 3 mm ± 0.2 mm.

[0018] In some preferred embodiments of the present invention, the thermal insulation layer is made of polytetrafluoroethylene and has a thickness of 1 mm±0.1 mm, so as to prevent the bottom heating radiation from affecting the infrared reflection test through the thermal insulation layer.

[0019] In some preferred embodiments of the present invention, the diameter of the circular hole is 8 mm±0.2 mm.

[0020] The second object of the present invention is to provide a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0021] Step 1: Install the film sample to be tested:

[0022] The film sample to be tested is placed on the heating layer in the above-mentioned variable temperature accessory, and then the thermal insulation layer and the metal clamp are coaxially placed on the upper surface of the film sample to be tested in sequence, so that part of the upper surface of the film sample to be tested is located below the circular hole to form a test area of ​​the film sample to be tested; the thermal insulation layer and the metal clamp are then fixed to the insulating layer by bolts to obtain a variable temperature accessory with the film sample to be tested installed.

[0023] Step 2: Use a gold mirror to collect background images:

[0024] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0025] Step 3, install the heating accessory on the stage and focus:

[0026] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus on the sample to be tested.

[0027] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0028] The test temperature was set and the platinum wire resistance heating mode was used for heating. After reaching the set temperature, the temperature was kept constant until thermal equilibrium was reached. Then, the sample reflected light intensity in the focal area was tested and analyzed with the reflected light intensity of the gold mirror back to obtain the infrared variable temperature reflectivity of the film compared with the gold mirror.

[0029] It should be noted that, compared with the gold mirror, the infrared temperature-dependent reflectivity of the thin film can be directly tested by Fourier transform infrared spectrometer, and the principle and method of thin film infrared reflectivity can be found in the prior art "Li Gang, Wang Nanlin. Principles and methods of infrared reflectivity spectroscopy [J]. Physics, 2006, (10): 873-878".

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] The variable temperature accessory of the present invention can be combined with the specular reflection method to realize micro-area testing of the variable temperature infrared reflectivity of the film at 25° C. to 200° C. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is a structural schematic diagram of the temperature-changing accessory of the present invention.

[0033] Figure 2 This is a real photo of the temperature-changing accessory of the present invention.

[0034] Figure 3These are the test results of the infrared reflectivity of the samarium nickelate films of Examples 3 to 12. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present invention are described clearly and completely below. It should be noted that in the following embodiments of the present invention, the Fourier transform infrared spectrometer used is a Bruker VERTEX70 microscopic infrared spectrometer. And the aluminum oxide substrate used is a (0001) oriented aluminum oxide substrate with a size of 10mm×10mm×5mm purchased from Hefei Kejing Materials Technology Co., Ltd.

[0036] Example 1

[0037] See also Figure 1 This embodiment provides a variable temperature accessory for testing the infrared variable temperature reflectivity of a thin film, including an insulating layer 1, a heating layer 2, a heat insulation layer 3 and a metal fixture 4.

[0038] The overall height of the temperature-changing accessory of this embodiment is 15 mm±0.2 mm, and the width is 40 mm±0.2 mm.

[0039] In the temperature-changing accessory of this embodiment, the insulating layer is made of polytetrafluoroethylene with a thickness of 10 mm±0.2 mm, and a power line 5 is connected inside the insulating layer 1 .

[0040] In the temperature-changing accessory of this embodiment, the heating layer 2 is arranged on the upper surface of the insulating layer 1 , and the material of the heating layer 2 is nickel-chromium alloy, and the thickness is 3 mm±0.2 mm.

[0041] In the temperature-variable accessory of this embodiment, the heat-insulating layer 3 is arranged on the upper surface of the heating layer 2, and the heat-insulating layer 3 is detachably mounted on the insulating layer 1, so that the film sample 6 to be tested can be mounted between the heating layer 2 and the heat-insulating layer 3. The heat-insulating layer 3 is made of polytetrafluoroethylene with a thickness of 1 mm ± 0.2 mm.

[0042] In the temperature-changing accessory of this embodiment, the metal clamp 4 is disposed on the upper surface of the heat-insulating layer 3 , and the metal clamp 4 can be detachably mounted on the insulating layer 1 .

[0043] In the temperature-variable accessory of this embodiment, circular holes 7 are provided in the middle of the heat-insulating layer 3 and the metal clamp 4, so that part of the upper surface of the installed film sample 6 to be tested can be leaked through the circular holes 7 to form a test area for the film sample 6 to be tested.

[0044] In a preferred embodiment of the present invention, the diameter of the circular hole is 8 mm±0.2 mm±0.2 mm.

[0045] Example 2

[0046] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0047] Step 1: Install the film sample to be tested:

[0048] The film sample to be tested is placed on the heating layer 2 in the variable temperature accessory of Example 1, and then the thermal insulation layer 3 and the metal clamp 4 are coaxially placed on the upper surface of the film sample to be tested 6 in sequence, so that part of the upper surface of the film sample to be tested 6 is located below the circular hole 7 to form a test area for the film sample to be tested 6; the thermal insulation layer 3 and the metal clamp 4 are then fixed to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample to be tested 6 installed.

[0049] Step 2: Use a gold mirror to collect background images:

[0050] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0051] Step 3, install the heating accessory on the stage and focus:

[0052] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0053] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0054] Set the test temperature, keep it warm for 1 minute to reach thermal equilibrium, then test the sample reflected light intensity in the focus area, analyze the sample reflected light intensity and the gold mirror back reflection light intensity, and obtain the film infrared temperature reflectivity R compared with the gold mirror. Relative .

[0055] Example 3

[0056] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0057] Step 1: Install the film sample to be tested:

[0058] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0059] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0060] Step 2: Use a gold mirror to collect background images:

[0061] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0062] Step 3, install the heating accessory on the stage and focus:

[0063] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample.

[0064] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0065] The test temperature range is set to 60℃. After reaching the set temperature, keep it warm for 1 minute to reach thermal equilibrium. Then test the sample reflected light intensity in the focus area. The sample reflected light intensity and the gold mirror back reflected light intensity are analyzed by the formula shown in formula 1 to obtain the infrared temperature reflectivity R of the film compared with the gold mirror. Relative , and in this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7μm-14μm band Relative It is 0.415.

[0066] Example 4

[0067] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0068] Step 1: Install the film sample to be tested:

[0069] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0070] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0071] Step 2: Use a gold mirror to collect background images:

[0072] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0073] Step 3, install the heating accessory on the stage and focus:

[0074] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0075] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0076] The test temperature range was set to 70°C. After reaching the set temperature, the temperature was kept for 1 minute to reach thermal equilibrium. Then the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-reflected light intensity to obtain the infrared temperature-dependent reflectivity R of the film compared with the gold mirror. Relative .

[0077] That is, the difference between this embodiment and embodiment 3 is only that:

[0078] The test temperature of this embodiment is 70°C.

[0079] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.420.

[0080] Example 5

[0081] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0082] Step 1: Install the film sample to be tested:

[0083] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0084] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0085] Step 2: Use a gold mirror to collect background images:

[0086] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0087] Step 3, install the heating accessory on the stage and focus:

[0088] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0089] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0090] The test temperature range was set to 80°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0091] That is, the difference between this embodiment and embodiment 3 is only that:

[0092] The test temperature of this embodiment is 80°C.

[0093] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.420.

[0094] Example 6

[0095] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0096] Step 1: Install the film sample to be tested:

[0097] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0098] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0099] Step 2: Use a gold mirror to collect background images:

[0100] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0101] Step 3, install the heating accessory on the stage and focus:

[0102] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0103] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0104] The test temperature range was set to 90°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0105] That is, the difference between this embodiment and embodiment 3 is only that:

[0106] The test temperature of this embodiment is 90°C.

[0107] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.429.

[0108] Example 7

[0109] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0110] Step 1: Install the film sample to be tested:

[0111] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0112] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0113] Step 2: Use a gold mirror to collect background images:

[0114] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0115] Step 3, install the heating accessory on the stage and focus:

[0116] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0117] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0118] The test temperature range was set to 100°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0119] That is, the difference between this embodiment and embodiment 3 is only that:

[0120] The test temperature of this embodiment is 100°C.

[0121] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.446.

[0122] Example 8

[0123] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0124] Step 1: Install the film sample to be tested:

[0125] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0126] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0127] Step 2: Use a gold mirror to collect background images:

[0128] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0129] Step 3, install the heating accessory on the stage and focus:

[0130] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0131] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0132] The test temperature range was set to 110°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0133] That is, the difference between this embodiment and embodiment 3 is only that:

[0134] The test temperature of this embodiment is 110°C.

[0135] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.483.

[0136] Example 9

[0137] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0138] Step 1: Install the film sample to be tested:

[0139] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0140] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0141] Step 2: Use a gold mirror to collect background images:

[0142] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0143] Step 3, install the heating accessory on the stage and focus:

[0144] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0145] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0146] The test temperature range was set to 120°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0147] That is, the difference between this embodiment and embodiment 3 is only that:

[0148] The test temperature of this embodiment is 120°C.

[0149] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative is 0.535.

[0150] Example 10

[0151] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0152] Step 1: Install the film sample to be tested:

[0153] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0154] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0155] Step 2: Use a gold mirror to collect background images:

[0156] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0157] Step 3, install the heating accessory on the stage and focus:

[0158] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0159] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0160] The test temperature range was set to 130°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0161] That is, the difference between this embodiment and embodiment 3 is only that:

[0162] The test temperature of this embodiment is 130°C.

[0163] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.635.

[0164] Embodiment 11

[0165] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0166] Step 1: Install the film sample to be tested:

[0167] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0168] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0169] Step 2: Use a gold mirror to collect background images:

[0170] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0171] Step 3, install the heating accessory on the stage and focus:

[0172] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0173] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0174] The test temperature range was set to 140°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0175] That is, the difference between this embodiment and embodiment 3 is only that:

[0176] The test temperature of this embodiment is 140°C.

[0177] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.736.

[0178] Example 12

[0179] This embodiment provides a method for testing the infrared temperature-dependent reflectivity of a thin film, comprising the following steps:

[0180] Step 1: Install the film sample to be tested:

[0181] 1.1) In this embodiment, an aluminum oxide substrate is used as the substrate, and a 10 mm×10 mm×200 nm samarium nickelate film is formed on the surface of the substrate by spin coating. The formed samarium nickelate film is used as a film sample to be tested.

[0182] 1.2) Place the film sample 6 to be tested formed in 1.1) above on the heating layer 2 in the variable temperature accessory of Example 1, and then coaxially place the thermal insulation layer 3 and the metal clamp 4 on the upper surface of the film sample 6 to be tested in sequence, so that part of the upper surface of the film sample 6 to be tested is located below the circular hole 7, so as to form a test area for the film sample 6 to be tested; then fix the thermal insulation layer 3 and the metal clamp 4 to the insulating layer 1 by bolts to obtain a variable temperature accessory with the film sample 6 to be tested installed, heat it by a platinum wire resistor, and control the temperature by an external controller in the control range of room temperature to 200°C.

[0183] Step 2: Use a gold mirror to collect background images:

[0184] Use a standard gold mirror as a reference object and place it on the stage of the Fourier transform infrared spectrometer. Adjust the coarse focusing screw and fine focusing screw of the microscope in turn to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror.

[0185] Step 3, install the heating accessory on the stage and focus:

[0186] The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample 6 to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample to be tested.

[0187] Step 4: Characterization of the infrared reflectivity of the film at variable temperature:

[0188] The test temperature range was set to 150°C. After reaching the set temperature, it was kept warm for 1 minute to reach thermal equilibrium. Then, the sample reflected light intensity in the focus area was tested. The sample reflected light intensity was analyzed with the gold mirror back-end reflected light intensity to obtain the infrared temperature-dependent reflectivity of the film compared with the gold mirror.

[0189] That is, the difference between this embodiment and embodiment 3 is only that:

[0190] The test temperature of this embodiment is 150°C.

[0191] In this embodiment, compared with the average infrared temperature-dependent reflectivity R of the gold mirror film in the 7 μm to 14 μm band, Relative It is 0.754.

[0192] The present invention organizes the test results of the infrared reflectivity of the samarium nickelate films of the above-mentioned embodiments 3 to 12 as follows: Figure 3 As shown by Figure 3 It can be seen from the test results that the samarium nickelate film, as a film with metal-insulator transition, has an infrared reflectivity that shows obvious temperature dependence in the process of temperature changes. This indicates that the variable temperature accessory of the present invention can be combined with the mirror reflection method to realize micro-area testing of the variable temperature infrared reflectivity of the samarium nickelate film at 30°C to 150°C.

[0193] Obviously, the above embodiments are only some embodiments of the present invention, not all 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.

Claims

1. A variable temperature accessory for testing infrared variable temperature reflectivity of thin films, characterized in that: Including insulation layer, heating layer, thermal insulation layer and metal clamps; A power line is connected inside the insulating layer; The heating layer is arranged on the upper surface of the insulating layer; The heat-insulating layer is arranged on the upper surface of the heating layer, and can be detachably mounted on the insulating layer, so as to facilitate the installation of the film sample to be tested between the heating layer and the heat-insulating layer; The metal fixture is arranged on the upper surface of the thermal insulation layer and can be detachably mounted on the insulation layer to fix the film sample to be tested; The heat insulating layer and the middle of the metal fixture are both provided with circular holes, so that a part of the upper surface of the installed film sample to be tested can be leaked out through the circular holes to form a test area of ​​the film sample to be tested.

2. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The overall height of the temperature-changing accessory is 15 mm ± 0.2 mm, and the width is 40 mm ± 0.2 mm.

3. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The insulating layer is made of polytetrafluoroethylene.

4. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The thickness of the insulating layer is 10 mm±0.2 mm.

5. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The material of the heating layer is nickel-chromium alloy.

6. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The thickness of the heating layer is 3 mm ± 0.2 mm.

7. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The material of the heat insulation layer is polytetrafluoroethylene.

8. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The thickness of the heat insulation layer is 1 mm±0.1 mm.

9. The temperature-variable accessory for testing infrared temperature-variable reflectivity of thin films as claimed in claim 1, characterized in that: The diameter of the circular hole is 8 mm±0.2 mm.

10. A method for testing infrared temperature-dependent reflectivity of a thin film, characterized in that: The following steps are involved: Placing the film sample to be tested on the heating layer in the temperature-variable attachment according to any one of claims 1 to 9, and then coaxially placing the thermal insulation layer and the metal clamp on the upper surface of the film sample to be tested in sequence, so that a portion of the upper surface of the film sample to be tested is located below the circular hole, so as to form a test area of ​​the film sample to be tested; Then, the heat insulation layer and the metal clamp are fixed to the insulating layer by bolts to obtain a temperature-variable accessory on which the film sample to be tested is installed; Use a standard gold mirror as a reference object, place it on the stage of the Fourier transform infrared spectrometer, adjust the coarse focusing screw and fine focusing screw of the microscope in sequence to focus the gold mirror, and then test the intensity of the reflected light from the back of the gold mirror; The standard gold mirror is replaced by the variable temperature accessory on which the thin film sample to be tested is installed, and the coarse focusing screw and the fine focusing screw of the microscope are adjusted in sequence to focus the thin film sample; Set the test temperature, keep it warm until thermal equilibrium is reached after reaching the set temperature, then test the sample reflected light intensity in the focus area, analyze the sample reflected light intensity with the gold mirror back-end reflected light intensity, and obtain the infrared temperature-dependent reflectivity of the film compared to the gold mirror.

Images