CN110823945A - Optical thin film thermal expansion coefficient measuring device based on ellipsometer and measuring method thereof - Google Patents
Optical thin film thermal expansion coefficient measuring device based on ellipsometer and measuring method thereof Download PDFInfo
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- CN110823945A CN110823945A CN201911113246.9A CN201911113246A CN110823945A CN 110823945 A CN110823945 A CN 110823945A CN 201911113246 A CN201911113246 A CN 201911113246A CN 110823945 A CN110823945 A CN 110823945A
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/16—Investigating or analyzing materials by the use of thermal means by investigating thermal coefficient of expansion
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Abstract
The invention discloses an ellipsometer-based optical thin film thermal expansion coefficient measuring device and a measuring method thereof. The device for measuring the thermal expansion coefficient of the optical thin film utilizes the ellipsometer to accurately measure the thickness of the optical thin film and measure the nanometer-scale change of the heated optical thin film, so that the measurement of the thermal expansion coefficient of a micron-scale optical thin film sample is realized. The invention designs an experimental device for measuring micro displacement by using an ellipsometer, aiming at the defect that the traditional method for measuring the thermal expansion coefficient of the material cannot measure nano-scale displacement. The method is simple to operate and convenient to adjust, and can measure the thermal expansion coefficient of a micron-sized sample, so that the requirement of the optical film on the test of the micro size is met.
Description
Technical Field
The invention belongs to the technical field of material performance measurement, and particularly relates to an ellipsometer-based optical thin film thermal expansion coefficient measuring device and a measuring method thereof.
Background
The thermal expansion coefficient of the bulk material has been used in the past to characterize the thermal expansion coefficient of the thin film, however, as the knowledge further deepens, it is gradually understood that the deposition mode of the thin film determines the difference between the structure and the bulk material. There is a large error in the correlation calculation of the thin film using the material parameters of the bulk material. Even if the thermal expansion coefficient of the bulk material is used, the thermal expansion performance of the film cannot be correctly characterized, and even the thermal expansion coefficients of films made of the same material and prepared by different deposition modes are different. Therefore, we need to propose a measurement method for the thermal expansion coefficient of the thin film.
In the aspect of thermal expansion coefficient testing, the existing measuring methods mainly comprise a push rod indirect method, a telescope direct reading method and a laser measuring method, and a common sample is a solid material with variation above micron level and is only suitable for measuring the sample with the dimension above millimeter. However, it is difficult to prepare a millimeter-sized optical thin film test piece, and therefore, an apparatus capable of precisely measuring the thermal expansion coefficient of an optical thin film is urgently needed.
Disclosure of Invention
In order to overcome the defect that the thermal expansion coefficient of the optical thin film cannot be measured due to the influence of the size and the measurement precision of a sample in the prior art, the invention provides a measurement device and a measurement method for the thermal expansion coefficient of the optical thin film.
The technical scheme adopted by the invention for solving the technical problems is as follows: an ellipsometer-based optical thin film coefficient of thermal expansion measurement device, the measurement device comprising: the ellipsometer comprises an ellipsometer, a sample clamp assembly, a thermocouple, an infrared heating lamp and a computer, wherein the sample clamp assembly can fix a sample to be measured on a carrying surface of the ellipsometer, a temperature measuring hole is formed in the center of the sample clamp assembly where the sample to be measured is placed, the thermocouple is arranged at the temperature measuring hole, a thermocouple probe is fixed on the back surface of the sample to be measured through the sample clamp assembly, the infrared heating lamp is arranged opposite to the sample to be measured and irradiates the sample perpendicularly to a plane, the ellipsometer and the thermocouple collect ellipsometric data and temperature data before and after heating to the computer, the computer fits the thickness information of the sample to be measured by utilizing the ellipsometric data, and the coefficient of thermal expansion of the sample to be measured can be calculated by combining the temperature.
In the above apparatus for measuring coefficient of thermal expansion of optical thin film, the sample holder assembly comprises a main copper frame; two fixing screws are respectively arranged on two sides of the main copper frame; an asbestos heat insulation pad is arranged behind the main copper frame; two sample clamping grooves are formed in the front face of the main body copper frame; the middle of the sample clamping groove is provided with a temperature measuring hole, and the temperature measuring hole is provided with a polytetrafluoroethylene gasket with a groove and a spring and used for fixing the thermocouple probe to enable the thermocouple probe to be tightly attached to the back of the sample without influencing the flatness of the sample to be measured, so that the calibration of the ellipsometer is facilitated.
According to the optical film thermal expansion coefficient measuring device, the condensing lampshade is arranged on the infrared heating lamp, so that infrared light can be condensed on the surface of a sample to be measured without radiating other parts, and measuring errors caused by creep deformation of the clamp are avoided.
The device for measuring the thermal expansion coefficient of the optical thin film has the advantages that the device for measuring the thermal expansion coefficient of the optical thin film accurately measures the thickness of the optical thin film by using the ellipsometer, and measures the nanometer-scale change of the optical thin film after being heated, so that the measurement of the thermal expansion coefficient of a micron-scale optical thin film sample is realized. The sample clamp assembly is provided with the asbestos heat insulation pad, so that the ellipsometer component is not influenced by heating conditions. The thermocouple measures the temperature on the back of the sample through the temperature measuring hole, and the temperature measurement is not affected by the direct irradiation of the infrared lamp. The polytetrafluoroethylene gasket with the groove and the spring ensure that the thermocouple probe can be tightly attached to a sample to be measured and ensure the smoothness of the surface to be measured so as to calibrate the ellipsometer.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic diagram of the construction of the sample holder assembly of FIG. 1;
FIG. 3 is a side view of the internal structure of the orifice of the sample holder assembly of FIG. 2.
In the figure: 1 ellipsometer, 2 sample clamp assemblies, 3 thermocouples, 4 infrared heating lamps, 5 computers, 6 samples to be measured, 7 ellipsometer object carrying surfaces, 8 temperature measuring holes, 9 thermocouple probes, 10 main body copper frames, 11 fixing screws, 12 asbestos heat insulation pads, 13 sample clamping grooves, 14 polytetrafluoroethylene gaskets, 15 springs, 16 condenser lamp covers, 17 ellipsometer object carrying table adjusting knobs, 18 monochromators, 19 incident lights, 20 reflected lights and 21 analyzers.
Detailed Description
The invention is further illustrated with reference to the figures and examples.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention.
An optical film thermal expansion coefficient measuring apparatus comprising: the ellipsometer comprises an ellipsometer 1, a sample clamp component 2, a thermocouple 3, an infrared heating lamp 4 and a computer 5, wherein the sample clamp component 2 can fix a sample 6 to be measured on a loading surface 7 of the ellipsometer, a temperature measuring hole 8 is formed in the center of the sample clamp component 2 where the sample 6 to be measured is placed, a thermocouple probe 9 is arranged at the temperature measuring hole 8, the thermocouple probe 9 is fixed on the back surface of the sample 6 to be measured by the sample clamp component 2, the infrared heating lamp 4 is arranged right opposite to the sample 6 to be measured, the infrared heating lamp 4 irradiates the plane of the sample 6 to be measured perpendicularly, the ellipsometer 1 and the thermocouple 3 collect ellipsometric data and temperature data before and after heating to the computer 5, the computer 5 utilizes the ellipsometric data to fit thickness information of a sample film to be measured, and combines the temperature data to calculate the thermal expansion coefficient of the.
The sample clamp assembly 2 comprises a main copper frame 10, two fixing screws 11 are respectively arranged on two sides of the main copper frame 10, the sample clamp assembly 2 is fixed on the ellipsometer object carrying surface 7 through the fixing screws 11, and an asbestos heat insulation pad 12 is arranged behind the main copper frame 10; the front surface of the main copper frame 10 is provided with two sample clamping grooves 13; the middle of the sample clamping groove 13 is provided with a temperature measuring hole 8, the temperature measuring hole 8 is provided with a polytetrafluoroethylene gasket 14 with a groove and a spring 15 for fixing the thermocouple probe 9, so that the thermocouple probe is tightly attached to the back of the sample without influencing the flatness of the sample, and the calibration of the ellipsometer 1 is facilitated.
The infrared heating lamp 4 is provided with the condensing lamp cover 16, infrared light can be condensed on the surface of the sample 6 to be measured without radiating other parts, and measurement errors caused by creep deformation of the sample clamp assembly 2 are avoided.
The working process of the device for measuring the thermal expansion coefficient of the optical film by using the ellipsometer comprises the following steps: firstly, switching on a power supply, starting the ellipsometer 1 and the computer 5, initializing the ellipsometer 1, and calibrating the ellipsometer by adjusting an adjusting knob 17 of an ellipsometer object stage; installing the sample clamp assembly 2 on the object carrying surface 7 of the ellipsometer by using a fixing screw 11, installing the sample 6 to be measured on a sample clamping groove 13, wherein the sample 6 to be measured is a micron-sized film deposited on an optical substrate, penetrating a thermocouple probe 9 out from between a main body copper frame 10 and an asbestos heat insulation pad 12 through a temperature measuring hole 8, fixing the thermocouple probe on the back surface of the sample 6 to be measured by using a polytetrafluoroethylene gasket 14 with a groove and a spring 15, and calibrating a plane to be measured by adjusting an adjusting knob 17 of an object carrying table of the ellipsometer;
the thermocouple 3 is connected with the computer 5, monitors the temperature of the sample 6 to be measured in real time, records the temperature T of the sample 6 to be measured before heating when the temperature is constant0Measuring ellipsometric parameters at room temperature with an ellipsometer 1;
after the measurement of the film ellipsometry parameters at room temperature is finished, the power supply of the infrared heating lamp 4 is turned on, the opening 16 of the condensing lamp shade of the infrared heating lamp is opposite to the surface of the sample 6 to be measured, the sample 6 to be measured is heated until the temperature is constant, and the temperature T after the stabilization is recorded1(ii) a Heating was continued while keeping the same power, while measuring the temperature T1The ellipsometric parameter of the sample 6 to be measured;
fitting the collected ellipsometry data with the ellipsometer 1 with the analysis software on the computer 5, and calculating the T before heating0Film thickness d at temperature1And heating to T1Film thickness d of2Calculating the displacement amount d ═ d2-d1Calculating the temperature difference between the constant temperature and the room temperature: Δ T ═ T1-T0Calculating the thermal expansion coefficient of the sample
The jig and the heating method according to the present embodiment are not limited to these, and may be replaced with other suitable methods.
Claims (4)
1. An ellipsometer-based optical thin film thermal expansion coefficient measuring device, comprising: ellipsometer (1), sample anchor clamps subassembly (2), thermocouple (3), infrared heating lamp (4), computer (5), characterized by: the sample clamp assembly (2) can fix a sample (6) to be measured on a loading surface (7) of the ellipsometer, a temperature measuring hole (8) is formed in the center, where the sample to be measured is placed, of the sample clamp assembly (2), a thermocouple probe (9) is arranged at the temperature measuring hole (8), the thermocouple probe (9) is fixed on the back surface of the sample (6) to be measured through the sample clamp assembly (2), an infrared heating lamp (4) is arranged on the right opposite surface of the sample (6) to be measured, the infrared heating lamp (4) irradiates the plane of the sample (6) to be measured perpendicularly, ellipsometry instruments (1) and thermocouples (3) collect ellipsometry data and temperature data of the sample (6) to be measured before and after the sample (6) to be measured is heated to a computer (5), the computer (5) utilizes the ellipsometry data to fit film thickness information of the sample (6), and combines the temperature data to calculate the thermal.
2. The ellipsometer-based optical film coefficient of thermal expansion measuring device of claim 1, wherein: the sample clamp assembly (2) comprises a main copper frame (10), two fixing screws (11) are respectively arranged on two sides of the main copper frame (10), the sample clamp assembly (2) is fixed on an ellipsometer object carrying surface (7) through the fixing screws (11), and an asbestos heat insulation pad (12) is arranged behind the main copper frame (10); two sample clamping grooves (13) are formed in the front face of the main copper frame (10); a temperature measuring hole (8) is formed in the middle of the sample clamping groove (13), a polytetrafluoroethylene gasket (14) with a groove and a spring (15) are arranged at the temperature measuring hole (8) and used for fixing the thermocouple probe (9), so that the thermocouple probe is tightly attached to the back of the sample (6) to be measured, the flatness of the sample is not affected, and the calibration of the ellipsometer (1) is facilitated.
3. The ellipsometer-based optical film coefficient of thermal expansion measuring device of claim 1, wherein: be provided with spotlight cover (16) on infrared heating lamp (4), can gather infrared light to the sample (6) surface that awaits measuring and do not radiate other parts, avoid the measuring error that sample anchor clamps subassembly (2) creep introduced.
4. An ellipsometer-based optical thin film thermal expansion coefficient measuring method is characterized in that: the method comprises the following steps:
firstly, a power supply is switched on, an ellipsometer (1) and a computer (5) are started, the ellipsometer (1) is initialized, and the ellipsometer is calibrated by adjusting an adjusting knob (17) of an objective table of the ellipsometer; installing a sample clamp assembly (2) on an object carrying surface (7) of an ellipsometer by using a fixing screw (11), installing a sample (6) to be measured on a sample clamping groove (13), wherein the sample (6) to be measured is a micron-sized film deposited on an optical substrate, penetrating a thermocouple probe (9) out of a position between a main body copper frame (10) and an asbestos heat insulation pad (12) through a temperature measuring hole (8), fixing the thermocouple probe on the back surface of the sample (6) to be measured by using a polytetrafluoroethylene gasket (14) with a groove and a spring (15), and calibrating a plane to be measured by adjusting an adjusting knob (17) of an ellipsometer object carrying table;
step two, the thermocouple (3) is connected with the computer (5), the temperature of the sample (6) to be measured is monitored in real time, and the temperature T of the sample (6) to be measured before heating is recorded when the temperature is constant0Measuring ellipsometric parameters at room temperature by using an ellipsometer (1);
step three, after the measurement of the film ellipsometry parameters at room temperature is finished, turning on the power supply of the infrared heating lamp (4), enabling the opening of the condensing lamp cover (16) to be opposite to the surface of the sample to be measured (6), heating the sample to be measured (6) until the temperature is constant, and recording the stable temperature T1(ii) a Heating was continued while keeping the same power, while measuring the temperature T1The ellipsometric parameter of the sample (6) to be measured;
step four, fitting the acquired ellipsometry data on a computer (5) by using an ellipsometer (1) with self-contained analysis software, and calculating the T before heating0Film thickness d at temperature1And heating to T1Film thickness d of2Calculating the displacement amount d ═ d2-d1Calculating the temperature difference between the constant temperature and the room temperature: Δ T ═ T1-T0Calculating the thermal expansion coefficient of the sample
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| JPH05259082A (en) * | 1992-03-10 | 1993-10-08 | Komatsu Denshi Kinzoku Kk | Epitaxial growth device and method |
| JP2000256848A (en) * | 1999-03-10 | 2000-09-19 | Canon Inc | Formation of film and device therefor |
| US6406637B1 (en) * | 1999-05-07 | 2002-06-18 | Tokyo Institute Of Technology | Thin film-planar structure and method for producing the same |
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Application publication date: 20200221 |