CN113203680B - 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 PDFInfo
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- CN113203680B CN113203680B CN202110382141.4A CN202110382141A CN113203680B CN 113203680 B CN113203680 B CN 113203680B CN 202110382141 A CN202110382141 A CN 202110382141A CN 113203680 B CN113203680 B CN 113203680B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/8422—Investigating thin films, e.g. matrix isolation method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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 invention calculates the thermal diffusivity of the thin film material through the relationship between the phase 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
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 heat generation and dissipation 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. Because the diversity and thickness difference of the submicron/nanometer film category can reach several orders, the influence of the substrate and the film interface can reach several orders, the test needs to be carried out by methods with different characteristics correspondingly, the film thermophysical property test difficulty is very large, the test results of researchers often have great difference, and no test method and device with universal applicability 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 thermal diffusivity of thin film elements and bulk materials 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 probe light laser, a probe light path power adjusting component, a probe light path reflector, a probe 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 angle. 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 test signal input end 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:
(1) and (3) turning on a pump light laser power supply, selecting proper beam power according to the characteristics of the 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 phase-locked amplifier to reach a stable working state.
(2) And adjusting the direction of the optical path to enable the centers of the pump beam and the detection beam to coincide.
(3) And 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.
(4) And slowly adjusting 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.
(5) The knob of the two-dimensional displacement platform is rotated in the reverse direction for a short distance (the indication number of the amplitude window of the phase-locked amplifier is kept below 10 mu V), and when the indication number of the phase-locked amplifier is stable, the phase at the moment is recorded
And detector position x 1 (or y) 1 )。
(6) Continuously rotating the knob of the two-dimensional displacement platform for a certain distance along the same direction of the rotating direction in the step (5), and recording the phase at the moment when the reading of the phase-locked amplifier is stable
And detector position x 2 (or y) 2 )。
(7) And (5) repeating the step, and recording the position x of the detector at intervals i (or y) i ) And its corresponding phase
The measurement is stopped (i > 20) when the amplitude window indication 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.
(8) After the standard sample is measured, the sample to be measured is disassembled and replaced by the standard sample, so that the pump light and the detection light irradiate on the intact area of the standard sample.
(9) And blocking the pump light, and recording the detection 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.
Calculating to obtain the magnification factor m A The formula is as follows:
m A ＝D 1 /D 2
then, the photo-thermal signal phase of the sample to be detected is made
Position (x) detected by surface heat pack of sample 6 to be detected i /m A ) 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/m 2
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 f i Lower corresponding slope m i Making a slope m i And a modulation frequency f i Square 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:
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 -9 m 2 /s。
2. The device for measuring the absorption of the surface thermal lens can be slightly changed, and one set of device can complete two kinds of measurement: absorption and thermal diffusivity.
Drawings
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-a pump light laser, 2-a pump light path power adjusting component, 3-a chopper, 4-a pump light path reflector, 5-a pump light path lens, 6-a sample to be measured, 7-a detection light laser, 8-a detection light path power adjusting component, 9-a detection light path reflector, 10-a detection light path lens, 11-a diaphragm, 12-a detector, 13-a two-dimensional displacement platform and 14-a 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 device and a bulk material based on a surface thermal lens technology. 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 part 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 is incident on 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 it 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:
(1) the power supply of the pump light laser 1 is turned on, proper beam power is selected according to the characteristics of a sample to be detected, the power supply of the detection light laser 10, the chopper 4 (with the set modulation frequency f), the detector 12 and the switch of the phase-locked amplifier 14 are turned on in sequence, and the preheating is carried out for more than half an hour, so that the laser and the phase-locked amplifier reach stable working states.
(2) And adjusting the direction of the optical path to enable the centers of the pump beam and the detection beam to coincide.
(3) The center of the detector 12 is aligned with the center of the reflected detection 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.
(4) The two-dimensional displacement platform 13 is slowly adjusted to move in a single direction 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.
(5) The knob of the two-dimensional displacement platform 13 is rotated in the reverse direction for a short distance (the amplitude window reading of the lock-in amplifier 14 is kept below 10 μ V), and when the reading of the lock-in amplifier 14 is stable, the phase at the moment is recorded
And detector position x 1 (or y) 1 )。
(6) 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 step (5), and when the reading of the phase-locked amplifier 14 is stable, the phase at the moment is recorded
And detector position x 2 (or y) 2 )。
(7) Repeating the step (5), and recording the position x of the detector 12 at intervals i (or y) i ) And its corresponding phase
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.
(8) 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.
(9) And blocking the pump light, and recording the detection 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.
Calculating to obtain the magnification factor m A The formula is as follows:
m A ＝D 1 /D 2
then, 6 photo-thermal signal phases of the sample to be detected are made
Position (x) detected by surface heat pack of sample 6 to be detected i /m A ) 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/m 2
in order to improve the measurement accuracy of the thermal diffusivity of the film material, the measurement can be carried out for multiple times under different modulation frequencies to obtain different modulation frequencies f i Lower corresponding slope m i Making a slope m i And a modulation frequency f i The square root is plotted to obtain the slope m'. Calculating to obtain the thermal diffusivity alpha' of the film material, wherein the formula is as follows:
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 (2)
1. A method for measuring by using a device for measuring thermal diffusivity of a thin film element and a bulk material based on a surface thermal lens technology comprises a pump 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 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 phase-locked 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 is incident to the 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); the method is characterized by comprising the following steps:
(1) 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 a power supply of a detection laser (10), a chopper (3), a modulation frequency f of the chopper, 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 and the chopper to reach a stable working state;
(2) adjusting the direction of the light path to ensure that the center of the pump beam and the center of the detection beam are superposed on the surface of the sample (6) to be detected;
(3) aligning the center of the detector (12) to the center of a detection light spot reflected by the sample to be detected (6), and assembling a small-aperture diaphragm in front of a light sensing surface of the detector for measuring the local light intensity of the detection light beam;
(4) adjusting a two-dimensional displacement platform (13) to move along the x or y single direction, observing the indication number of an amplitude window of a phase-locked amplifier (14), adjusting the measuring range according to the indication number, and stopping moving when the indication number of the window is less than 10 mu V;
(5) will twoThe knob of the dimensional displacement platform (13) rotates a short distance in the opposite direction, namely the indication number of the amplitude window of the phase-locked amplifier (14) is kept below 10 mu V, and when the indication number of the phase-locked amplifier (14) is stable, the phase at the moment is recorded
And detector position x 1 Or y 1 ；
(6) The knob of the two-dimensional displacement platform (13) is continuously rotated for a distance along the same direction of the rotation direction in the step (5), and when the indication number of the phase-locked amplifier (14) is stable, the phase at the moment is recorded
And detector position x 2 Or y 2 ；
(7) Repeating the step (5), and recording the position x of the detector (12) at intervals i Or y i And its corresponding phase
When the amplitude window reading of the phase-locked amplifier (14) is below 10 mu v again, stopping measurement when i is greater than 20, and obtaining a complete radial data set of the reflection detection light spot;
(8) after the sample (6) to be measured is measured, the sample (6) to be measured is dismounted and replaced by a standard sample, and the pump light and the detection light are irradiated on the intact area of the standard sample;
(9) blocking the pump light, and recording the detection light spots by using a CCD camera;
blocking the probe light at the r part, irradiating the standard sample by the pump light, properly increasing the power of the pump light to damage the standard sample, and punching a damage point on the standard sample by the pump light;
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 point 1 ；
Measuring the diameter D of the damage point on the standard sample 2 ；
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;
data processing
First, the magnification m is calculated A The formula is as follows:
m A ＝D 1 /D 2
then, the photo-thermal signal phase of the sample (6) to be measured is made
Detecting position x along with surface hot pack of sample (6) to be detected i /m A Changing a 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/m 2 。
2. the measurement method of claim 1, further comprising performing multiple measurements at different modulation frequencies to obtain different modulation frequencies f i Lower corresponding slope m i Making a slope m i And a modulation frequency f i Obtaining 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:
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