CN113203680A - Device and method for measuring thermal diffusivity of thin film element and bulk material based on surface thermal lens technology - Google Patents

Device and method for measuring thermal diffusivity of thin film element and bulk material based on surface thermal lens technology Download PDF

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CN113203680A
CN113203680A CN202110382141.4A CN202110382141A CN113203680A CN 113203680 A CN113203680 A CN 113203680A CN 202110382141 A CN202110382141 A CN 202110382141A CN 113203680 A CN113203680 A CN 113203680A
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李大伟
胡晨璐
刘晓凤
赵元安
连亚飞
邵建达
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Shanghai Institute of Optics and Fine Mechanics of CAS
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract

A device and a method for measuring the thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technology comprise a pump light laser, a pump light path power adjusting component, a chopper, a pump light path reflector, a pump light path lens, a lens two-dimensional displacement platform, a sample to be measured, a sample two-dimensional displacement platform, a detection light laser, a detection light path power adjusting component, a detection light path reflector, a detection light path lens, a diaphragm, a detector two-dimensional displacement platform, a computer and a phase-locked amplifier. The thermal diffusivity of the thin film material is calculated according to the relationship between the phase position of the photo-thermal signal and the detection distance and the relationship between the thermal diffusion length and the modulation frequency. The invention can effectively realize the measurement of the thermal diffusivity of the thin film element and the bulk material.

Description

Device and method for measuring thermal diffusivity of thin film element and bulk material based on surface thermal lens technology
Technical Field
The invention relates to measurement of thermal diffusivity of a thin film element and a bulk material, in particular to a device and a method for measuring the thermal diffusivity of the thin film element and the bulk material based on a surface thermal lens technology.
Background
Micro-electro-mechanical systems (MEMS), nanotechnology, micro devices, low-dimensional and nano materials are currently rapidly developing. Thermal effects become more and more important as the size of machinery decreases and its power handling specifications increase. Operation and failure of MEMS and like devices can be limited by heat transfer, and scaling of integrated circuits and increasing power density presents significant challenges to thermal management in the development of advanced microelectronic devices. The integration level of the device is higher and higher, the heat generated in the unit time of the device is quite large, the temperature rises quickly, the normal work of the device is influenced, and even the device is burnt. This presents thermal design and management problems for microelectronic devices, and it is necessary to study the generation and diffusion of heat in these devices, and to perform forced heat dissipation if necessary.
In general, for thermal management in microelectronics, thermal energy must be transported through different thin film materials, and the thermal diffusivity of these thin films plays a key role in assessing the transport efficiency and temperature of the device.
For the thin film element material, the heat transfer behavior is different from that of the bulk material, and the material shows obvious specific performance, and the traditional method and device for testing the thermophysical property of the bulk material have difficulty in testing the thin film. Due to the diversity of the submicron/nanometer film types, the thickness difference can reach several orders, the influence of the substrate and the film interface, and the like, the test needs to be carried out by methods with different characteristics correspondingly, the film thermophysical property test difficulty is very high, the test results of researchers often have larger difference, and a test method and a device with universal applicability do not exist so far.
Disclosure of Invention
In order to solve the problems, the invention provides a device and a method for measuring the thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technology, which can effectively realize the measurement of the thermal diffusivity of the thin film material. The invention uses the thermal lens effect, irradiates a film sample to be measured by a beam of pumping light, and forms a thermal pack on the surface of the film. Then, the detection light with the light spot radius larger than that of the pump light irradiates the heat pack area, and the surface heat pack change and the detection light spot change of the thin film sample to be detected have the same frequency as the pump light. Measuring phases corresponding to thermal signals at different positions of the reflected detection light spots, calculating temperature propagation time by using the phases, calculating temperature propagation speed according to the propagation distance, and further solving by using the relation between the temperature propagation speed and the thermal diffusivity.
The technical solution of the invention is as follows:
a device for measuring the thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technology is characterized by comprising a pump light laser, a pump light path power adjusting component, a chopper, a pump light path reflector, a pump light path lens, a sample to be measured, a detection light laser, a detection light path power adjusting component, a detection light path reflector, a detection light path lens, a diaphragm, a detector, a two-dimensional displacement platform and a phase-locked amplifier.
1. The pump light laser outputs pump light, the light path of the pump light laser is called as a pump light path, a pump light path power adjusting component, a chopper, a pump light path reflector, a pump light path lens and a sample to be detected are sequentially arranged at the output end of the pump light laser along the light path, and finally the pump light vertically irradiates the sample to be detected. The detection light laser outputs detection light, a light path of the detection light laser is called as a detection light path, and a detection light path power adjusting component, a detection light path reflector, a detection light path lens and a sample to be detected are sequentially placed at an output end of the detection light laser along the light path, so that the detection light irradiates the sample to be detected at an angle close to the vertical direction. And a diaphragm and a two-dimensional displacement platform are sequentially arranged on a reflection detection light path passing through a sample to be detected, and a detector is arranged on the two-dimensional displacement platform. And connecting the output end of the detector with the input end of the test signal of the phase-locked amplifier. And connecting the output end of the chopper with the reference signal input end of the phase-locked amplifier.
A method for measuring thermal diffusivity of thin film elements and bulk materials based on a surface thermal lens technology comprises the following steps:
firstly, turning on a pump light laser power supply, selecting proper beam power according to the characteristics of a sample to be detected, sequentially turning on a detection light laser power supply, a chopper (setting modulation frequency f), a detector and a switch of a phase-locked amplifier, and preheating for more than half an hour to enable the detection light laser power supply, the chopper (setting modulation frequency f), the detector and the switch to reach a stable working state.
Adjusting the light path direction to make the pump light beam coincide with the center of the detection light beam.
And thirdly, aligning the center of the detector to the center of the reflected detection light spot. A small-caliber diaphragm is arranged in front of the light-sensitive surface of the detector and can measure the local light intensity of the detection light beam.
And fourthly, slowly adjusting the two-dimensional displacement platform to enable the two-dimensional displacement platform to move along the x (or y) single direction. And meanwhile, observing the amplitude window indication of the phase-locked amplifier, adjusting the measuring range according to the indication, and stopping moving the detector when the window indication is less than 10 μ V.
Fifthly, the knob of the two-dimensional displacement platform is rotated in the reverse direction for a short distance (the indication value of the amplitude window of the lock-in amplifier is kept below 10 muV), and when the indication value of the lock-in amplifier is stable, the phase at the moment is recorded
Figure BDA0003013414970000021
And detector position x1(or y)1)。
Sixthly, the knob of the two-dimensional displacement platform continues to rotate for a distance along the same direction of the rotation direction in the fifth step, and the phase position at the moment is recorded when the indication number of the phase-locked amplifier is stable
Figure BDA0003013414970000022
And detector position x2(or y)2)。
Seventhly, repeating the step (c), recording the position x of the detector at intervalsi(or y)i) And its corresponding phase
Figure BDA0003013414970000031
The measurement is stopped (i > 20) when the amplitude window reading to the lock-in amplifier is again below 10 μ v. At this point, a complete radial data set of reflected probe spots can be obtained.
And after the standard sample is measured, detaching the sample to be measured and replacing the sample to be measured with the standard sample, so that the pump light and the detection light irradiate the intact area of the standard sample.
And ninthly, blocking the pumping light and recording and detecting light spots by using a CCD camera.
The probe light is blocked at the red (R), the pump light irradiates the standard sample, the power of the pump light is properly increased to enable the pump light to damage the standard sample, and a damage point is formed on the standard sample by the pump light.
Figure BDA0003013414970000032
Blocking the pump light, irradiating the sample with the detection light, recording the detection light spot by a CCD camera, comparing the detection light spots before and after the damage of the standard sample, and recording the diameter D of the detection region affected by the damage point1
Figure BDA0003013414970000033
Measuring the diameter D of the damage point on the standard sample2
Figure BDA0003013414970000034
After all measurements are finished, the power supply of the phase-locked amplifier is turned off after the measuring range of the phase-locked amplifier is adjusted to the maximum. The power supply to the detector, chopper, pump laser and probe laser is then turned off.
Figure BDA0003013414970000035
Data processing
Calculating to obtain the magnification factor mAThe formula is as follows:
mA=D1/D2
then, the photo-thermal signal phase of the sample to be detected is made
Figure BDA0003013414970000036
Detecting position (x) along with surface heat pack of sample 6 to be detectedi/mA) And changing the curve to obtain the slope m. Calculating to obtain the thermal diffusivity alpha of the sample to be measured, wherein the formula is as follows:
α=πf/m2
in order to improve the measurement accuracy of the thermal diffusivity of the film material, the film material can be measured for multiple times under different modulation frequencies to obtain different modulation frequencies fiLower corresponding slope miMaking a slope miAnd a modulation frequency fiSquare root, the slope m' of the curve is obtained.
Calculating to obtain the thermal diffusivity alpha' of the film material, wherein the formula is as follows:
Figure BDA0003013414970000037
compared with the prior art, the invention has the technical effects that:
1. simple structure and data processing, wide application range, low device adjustment requirement, simple and easy measurement method, and measurement accuracy up to 10-9m2/s。
2. Can change slightly on the absorptive device of surperficial thermal lens survey, realize that one set of device accomplishes two kinds of measurements: absorption and thermal diffusivity.
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FIG. 1 is a schematic structural diagram of an apparatus for measuring thermal diffusivity of thin film elements and bulk materials based on surface thermal lens technology according to the present invention.
In the figure, 1-pump light laser, 2-pump light path power adjusting component, 3-chopper, 4-pump light path reflector, 5-pump light path lens, 6-sample to be measured, 7-detecting light laser, 8-detecting light path power adjusting component, 9-detecting light path reflector, 10-detecting light path lens, 11-diaphragm, 12-detector, 13-two-dimensional displacement platform and 14-phase-locked amplifier.
Detailed Description
The invention is further illustrated with reference to the following examples and figures, without thereby limiting the scope of the invention.
Referring to fig. 1, fig. 1 is a schematic diagram of an apparatus for measuring thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technique. As shown in the figure, the device for measuring the thermal diffusivity of the thin film element and the bulk material based on the surface thermal lens technology comprises a pump light laser 1, a pump light path power adjusting component 2, a chopper 3, a pump light path reflector 4, a pump light path lens 5, a sample to be measured 6, a detection light laser 7, a detection light path power adjusting component 8, a detection light path reflector 9, a detection light path lens 10, a diaphragm 11, a detector 12, a two-dimensional displacement platform 13 and a lock-in amplifier 14; the output end of the detector 12 is connected with the test signal input end of the lock-in amplifier 14, and the synchronous signal output end of the chopper 3 is connected with the reference signal input end of the lock-in amplifier 14;
the laser output by the pump light laser 1 is pump light, and the pump light passes through the pump light path power adjusting component 2, the chopper 3, the pump light path reflector 4 and the pump light path lens 5 and then is incident on a sample 6 to be measured. The laser output by the detection light laser 7 is detection light, and the detection light passes through the detection light path power adjusting part 8, the detection light path reflector 9 and the detection light path lens 10 and then enters the sample 6 to be detected. The detection light is reflected on the surface of the sample 6 to be detected, passes through the diaphragm 11 and enters the detector 12. The detector 12 output signal is input to a lock-in amplifier 14. The chopper 3 modulates the frequency signal and inputs the frequency signal to the lock-in amplifier 14.
The detection light laser 7 outputs detection light, the light path of the detection light laser is called as a detection light path, the output end of the detection light path is sequentially provided with a detection light path power adjusting component 8, a detection light path reflector 9, a detection light path lens 10 and a sample 6 to be detected along the light path, so that the detection light irradiates the sample 6 to be detected at an angle close to the vertical direction, a diaphragm 11 and a two-dimensional displacement platform 13 are sequentially arranged on the reflection detection light path passing through the sample 6 to be detected, and a detector 12 is arranged on the two-dimensional displacement platform 13.
The output of the detector 12 is connected to the test signal input of the lock-in amplifier 14. The output terminal of the chopper 3 is connected to the reference signal input terminal of the lock-in amplifier 14.
A method for measuring thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technology comprises the following steps:
firstly, turning on a power supply of a pump laser 1, selecting proper beam power according to the characteristics of a sample to be detected, sequentially turning on switches of a power supply of a detection laser 10, a chopper 4 (setting a modulation frequency f), a detector 12 and a phase-locked amplifier 14, and preheating for more than half an hour to enable the power supply, the chopper 4, the detector 12 and the phase-locked amplifier to reach a stable working state.
Adjusting the light path direction to make the pump light beam coincide with the center of the detection light beam.
And thirdly, aligning the center of the detector 12 to the center of the reflected detection light spot. A small-caliber diaphragm is arranged in front of the light-sensitive surface of the detector and can measure the local light intensity of the detection light beam.
And fourthly, slowly adjusting the two-dimensional displacement platform 13 to enable the two-dimensional displacement platform to move along the single direction of x (or y). Meanwhile, the amplitude window indication of the lock-in amplifier 14 is observed, the measuring range is adjusted according to the size of the indication, and when the window indication is smaller than 10 μ V, the detector 12 stops moving.
Fifthly, the knob of the two-dimensional displacement platform 13 is rotated in the reverse direction for a short distance (the indication value of the amplitude window of the lock-in amplifier 14 is kept below 10 muV), and when the indication value of the lock-in amplifier 14 is stable, the phase position at the moment is recorded
Figure BDA0003013414970000051
And detector position x1(or y)1)。
Sixthly, the knob of the two-dimensional displacement platform 13 is continuously rotated for a certain distance along the same direction of the rotation direction in the fifth step, and the phase at the moment is recorded when the reading of the lock-in amplifier 14 is stable
Figure BDA0003013414970000052
And detector position x2(or y)2)。
Seventhly, repeating the step (c), recording the position x of the detector 12 at intervalsi(or y)i) And its corresponding phase
Figure BDA0003013414970000053
The measurement is stopped (i > 20) when the amplitude window reading to the lock-in amplifier 14 is again below 10 μ v. At this point, a complete radial data set of reflected probe spots can be obtained.
After the standard sample is measured, the sample 6 to be measured is dismounted and replaced by the standard sample, and the pump light and the detection light are irradiated on the intact area of the standard sample.
And ninthly, blocking the pumping light and recording and detecting light spots by using a CCD camera.
The probe light is blocked at the red (R), the pump light irradiates the standard sample, the power of the pump light is properly increased to enable the pump light to damage the standard sample, and a damage point is formed on the standard sample by the pump light.
Figure BDA0003013414970000054
Blocking the pump light, irradiating the sample with the detection light, recording the detection light spot by a CCD camera, comparing the detection light spots before and after the damage of the standard sample, and recording the diameter D of the detection region affected by the damage point1
Figure BDA0003013414970000055
Measuring the diameter D of the damage point on the standard sample2
Figure BDA0003013414970000056
After all measurements are made, the lock-in amplifier 14 is first powered down after the range is maximized. The power supply of the detector 12, the chopper 3, the pump light laser 1 and the probe light laser 7 is then switched off.
Figure BDA0003013414970000057
Data processing
Calculating to obtain the magnification factor mAThe formula is as follows:
mA=D1/D2
then, 6 photo-thermal signal phases of the sample to be detected are made
Figure BDA0003013414970000061
Detecting position (x) along with surface heat pack of sample 6 to be detectedi/mA) And changing the curve to obtain the slope m. Calculating to obtain the thermal diffusivity alpha of the sample 6 to be measured, wherein the formula is as follows:
α=πf/m2
in order to improve the measurement accuracy of the thermal diffusivity of the film material, the film material can be measured for multiple times under different modulation frequencies to obtain different modulation frequencies fiLower corresponding slope miMaking a slope miAnd a modulation frequency fiSquare root, the slope m' of the curve is obtained. Calculating to obtain the thermal diffusivity alpha' of the film material, wherein the formula is as follows:
Figure BDA0003013414970000062
the present invention is not limited to the embodiments described herein, and those skilled in the art, having the benefit of the teachings of the present invention, may effect modifications and variations thereto without departing from the scope of the present invention.

Claims (3)

1. A device for measuring thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technology is characterized by comprising a pump light laser (1), a pump light path power adjusting component (2), a chopper (3), a pump light path reflector (4), a pump light path lens (5), a detection light laser (7), a detection light path power adjusting component (8), a detection light path reflector (9), a detection light path lens (10), a diaphragm (11), a detector (12), a two-dimensional displacement platform (13) for placing the detector (12) and a lock-in amplifier (14);
the pump laser (1) outputs pump light, and the pump light vertically irradiates a sample to be measured (6) after sequentially passing through the pump light path power adjusting component (2), the chopper (3), the pump light path reflector (4) and the pump light path lens (5);
the detection light laser (7) outputs detection light, the detection light irradiates a sample to be detected (6) at an inclined angle after sequentially passing through the detection light path power adjusting part (8), the detection light path reflector (9) and the detection light path lens (10), and the detection light is reflected by the sample to be detected (6) and then enters a detector (12) through the diaphragm (11);
the output end of the detector (12) is connected with the test signal input end of the phase-locked amplifier (14), and the output end of the chopper (3) is connected with the reference signal input end of the phase-locked amplifier (14).
2. A method for measuring thermal diffusivity of thin film elements and bulk materials based on a surface thermal lens technology is characterized by comprising the following steps:
firstly, turning on a power supply of a pump light laser (1), selecting proper beam power according to the characteristics of a sample to be detected, sequentially turning on a power supply of a detection light laser (10), a chopper (3) (setting a modulation frequency f), a detector (12) and a switch of a phase-locked amplifier (14), and preheating for more than half an hour to enable the power supply, the chopper (3), the detector (12) and the switch to reach a stable working state;
adjusting the direction of the light path to ensure that the center of the pump light beam and the center of the detection light beam are superposed on the surface of the sample (6) to be detected;
aligning the center of the detector (12) to the center of the light spot of the detection light reflected by the sample to be detected (6), and assembling a small-caliber diaphragm in front of the light sensing surface of the detector for measuring the local light intensity of the detection light beam;
adjusting the two-dimensional displacement platform (13) to move along the x (or y) single direction, observing the amplitude window readings of the lock-in amplifier (14), adjusting the measuring range according to the magnitude of the readings, and stopping moving when the window readings are less than 10 mu V;
fifthly, the knob of the two-dimensional displacement platform (13) is rotated in the reverse direction for a short distance (the indication value of the amplitude window of the lock-in amplifier (14) is kept below 10 mu V), and when the indication value of the lock-in amplifier (14) is stable, the phase position at the moment is recorded
Figure FDA0003013414960000011
And detector position x1(or y)1);
Sixthly, the knob of the two-dimensional displacement platform (13) continues to rotate for a distance along the same direction of the rotation direction in the fifth step, and the phase at the moment is recorded when the reading of the phase-locked amplifier (14) is stable
Figure FDA0003013414960000027
And detector position x2(or y)2)。
Seventhly, repeating the step five, recording downward detection at intervalsThe position x of the detector (12)i(or y)i) And its corresponding phase
Figure FDA0003013414960000028
When the amplitude window reading of the phase-locked amplifier (14) is below 10 mu v again, stopping measurement (i is more than 20), and obtaining a complete radial data set of the reflection detection light spot;
after the sample (6) to be measured is measured, detaching the sample (6) to be measured and replacing the sample with a standard sample, and irradiating pump light and detection light on the intact area of the standard sample;
ninthly, blocking the pumping light, and recording the detection light spot by using a CCD camera;
blocking the detection light at the red (R), irradiating the standard sample with the pumping light, properly increasing the power of the pumping light to enable the standard sample to be damaged, and punching a damage point on the standard sample by using the pumping light;
Figure FDA0003013414960000021
blocking the pump light, irradiating the sample with the detection light, recording the detection light spot by a CCD camera, comparing the detection light spots before and after the damage of the standard sample, and recording the diameter D of the detection region affected by the damage point1
Figure FDA0003013414960000022
Measuring the diameter D of the damage point on the standard sample2
Figure FDA0003013414960000023
After the measurement is finished, firstly, the power supply of the phase-locked amplifier (14) is turned off after the measuring range is adjusted to the maximum, and then the power supplies of the detector (12), the chopper (3), the pump laser (1) and the detection laser (7) are turned off;
Figure FDA0003013414960000024
data processing
First, the magnification m is calculatedAThe formula is as follows:
mA=D1/D2
then, the photo-thermal signal phase of the sample (6) to be measured is made
Figure FDA0003013414960000025
Detecting position (x) along with surface heat pack of sample (6) to be detectedi/mA) Changing the curve to obtain a slope m;
finally, calculating the thermal diffusivity alpha of the sample to be measured (6), wherein the formula is as follows:
α=πf/m2
3. the method for measuring thermal diffusivity of thin film elements and bulk materials based on surface thermal lens technology of claim 2 further comprising performing multiple measurements at different modulation frequencies to obtain different modulation frequencies fiLower corresponding slope miMaking a slope miAnd a modulation frequency fiObtaining a curve slope m' by a relation curve of square root;
calculating to obtain the thermal diffusivity alpha' of the film material, wherein the formula is as follows:
Figure FDA0003013414960000026
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