CN111060555A - Method and device for measuring thermal conductivity and thermal diffusivity of thin film material under strain - Google Patents
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Abstract
The invention discloses a method and a device for measuring the thermal conductivity and thermal diffusivity of a thin film material under strain, wherein a sample is tensioned by a tensioning mechanism, the sample, the tensioning mechanism and a driving mechanism are placed in a vacuum chamber, the sample is heated by laser, a temperature distribution diagram of the sample in the whole process from the beginning to the steady state under fixed strain is obtained by an infrared camera, the thin film is treated as two-dimensional heat transfer, an experimental picture is processed to obtain the temperature of each pixel point on the surface of the thin film, the thin film is divided into a plurality of infinitesimals according to the size of the pixel point, a steady state thermal equilibrium equation and a transient thermal equilibrium equation are established, the thermal conductivity and the thermal diffusivity of the thin film under different temperatures are solved, the driving mechanism drives the sample to generate different strains, and the condition that the thermal conductivity and the thermal diffusivity of the sample under different. The method is convenient to operate, has high measurement accuracy, and can obtain the condition that the thermal conductivity and the thermal diffusivity of the sample change along with the temperature under different strains.
Description
Technical Field
The invention belongs to the technical field of heat transfer, and particularly relates to a method and a device for measuring the thermal conductivity coefficient and the thermal diffusivity of a thin film material under strain.
Background
Not only is the film the most effective material for achieving miniaturization of devices and systems, but in the field of sensors, the film also serves as one of the elements for measuring various physical quantities. The operating temperature of the film is generally variable, and small strains are generated due to stresses of different degrees, such as transfer, vibration, and heat generation, during use. The reliability of the device or the system is to be verified after the thermal physical property of the film is changed, so that the relationship between the thermal conductivity coefficient and the thermal diffusion coefficient of the film under strain and the temperature is correctly measured, the reliability of the system is determined, and the method is of great significance for perfecting the design of electronic devices.
However, the current technical schemes for measuring the thermal conductivity and thermal diffusivity of the film material have some defects:
the infrared imaging technology is a method for obtaining the temperature of an object by receiving the surface radiant energy of the object, the temperature of each pixel point can be accurately obtained by calibrating the surface emissivity of the object, and the temperature resolution is high; in a patent (publication No. CN 109001250 a) "method for analyzing film thermal conductivity based on infrared imaging method", after obtaining temperature distribution based on infrared thermal imaging technology, inputting boundary conditions of a model, setting the film thermal conductivity to 70% -100% of a theoretical value for simulation, and obtaining the value of the film thermal conductivity when a simulated temperature distribution curve is fitted to a test result. The method has the problems that the theoretical value of the thermal conductivity of the material needs to be known in advance, and the method has limitation; secondly, on the basis, the value of the heat conductivity coefficient needs to be modified for many times to be matched with the test temperature distribution diagram, so that the workload is large and the error is also large.
In a patent (publication No. CN 106813718A) "an apparatus and method for measuring film strain and thermal conductivity", although the thermal conductivity of a conductive film material under different strains can be measured, the pretreatment of the material is complicated, the film needs to be plated on a substrate, four pads are sputtered according to a 3 ω method, and a micron-sized metal strip is simultaneously fabricated on the surface of the film, and the four pads are connected to the metal strip. In addition, the method also has requirements on the conductivity of the thin film material, and strain can be calculated only by knowing the Young modulus, so that the method has more limitations.
In a patent (publication No. CN 110487842 a) "apparatus and method for simultaneously measuring thermal conductivity and infrared emissivity in a thin film surface", a temperature distribution is formed on the thin film surface by using light heating, and the thermal conductivity is obtained by testing and fitting a curve of spatial distribution of infrared radiation. However, the thermal equation established in the method is one-dimensional heat transfer, and in fact, the film, as a common two-dimensional material, cannot ignore the heat transfer in the width direction even under the condition that the heating light field has an aspect ratio of more than 2, so that the thermal conductivity error obtained by the method through the one-dimensional thermal conductivity equation is large.
Disclosure of Invention
The invention aims to provide a method and a device for measuring the thermal conductivity and the thermal diffusivity of a thin film material under strain.
The technical scheme adopted by the invention is as follows:
a method of measuring thermal conductivity and thermal diffusivity of a thin film material under strain, comprising the steps of:
s1, spreading the sample, tensioning the sample by the tensioning mechanisms at two ends, placing the sample, the tensioning mechanism and the driving mechanism into a vacuum cavity, sealing and vacuumizing the vacuum cavity, and only considering heat conduction and heat radiation;
s2, heating the sample in the vacuum cavity by using continuous laser, and obtaining a temperature distribution diagram of the sample in the whole process from the beginning to the steady state under the fixed strain through an infrared camera;
s3, because the thickness of the film is far smaller than the side length, the film is regarded as two-dimensional heat transfer, the experimental picture is processed to obtain the temperature of each pixel point on the surface of the film, the film is divided into a plurality of micro-elements according to the size of the pixel point, and thus the temperature values of different micro-elements under fixed strain are obtained;
s4, establishing a steady-state and transient-state heat balance equation, and solving the heat conductivity coefficient and the heat diffusion coefficient of the film at different temperatures;
s5, the driving mechanism drives the tensioning mechanism, the sample is controlled to generate the micro displacement delta x, the sample generates different strains, and the conditions that the thermal conductivity and the thermal diffusivity of the sample change along with the temperature under different strains are obtained according to the steps S2 to S4.
Further, in step S4, a steady state process is established
Established transient process
Wherein,
where Δ x and Δ y represent the lengths of the infinitesimal elements in the x-and y-directions, respectively, and λ(m，n)RepresentsThermal conductivity of the element, d represents the thickness of the sample, T(m-1，n)And T(m+1，n)Respectively representing the temperatures, T, of two units in front and behind the infinitesimal in the x direction(m，n-1)And T(m，n+1)Respectively representing the temperature of the front unit and the rear unit of the infinitesimal in the y direction;
p Δ x Δ y represents the amount of heat that the laser heats to flow into the infinitesimal element, wherein P is the incident intensity of the laser;
Further, before measurement, the emissivity of the sample is determined, the thermocouple is used for measuring the surface temperature of the sample, and the emissivity of the infrared camera is adjusted at the same time until the surface temperature measured by the infrared camera is the same as the temperature measured by the thermocouple, wherein the emissivity is the real emissivity of the sample.
A device for measuring the heat conductivity coefficient and the thermal diffusion coefficient of a thin film material under strain comprises a vacuum cavity with a light transmission window, a laser probe hermetically extending into the vacuum cavity, a laser connected with the laser probe, an air suction pump used for vacuumizing the vacuum cavity, an infrared camera for shooting a sample in the vacuum cavity facing the light transmission window, a data processing module connected with the infrared camera, and a tensioning mechanism and a driving mechanism which are positioned in the vacuum cavity, wherein the tensioning mechanism is used for tensioning two ends of the sample, and the driving mechanism is used for driving the tensioning mechanism to control the sample to generate micro displacement.
Further, the light-transmitting window adopts a germanium window.
Further, the tensioning mechanism comprises two pairs of heat sinks which are flush and respectively located at two ends of the sample, and each pair of heat sinks clamps and fastens the ends of the sample from the upper side and the lower side through bolts.
Furthermore, the driving mechanism comprises a guide rail, a rack, a motor and a gear transmission system, one pair of heat sinks are fixed in position, the lower heat sinks of the other pair of heat sinks are in sliding fit with the guide rail, the upper heat sinks of the other pair of heat sinks are fixed with the rack, the motor is meshed with the rack through the gear transmission system, and a power line of the motor hermetically extends out of the vacuum cavity and is connected with a power supply.
Further, the gear transmission system comprises a motor output shaft, a pinion A arranged on the motor output shaft, a fixed shaft, and a bull gear B and a pinion C which are arranged on the fixed shaft, wherein the pinion A is meshed with the bull gear B, and the pinion C is meshed with the rack.
Furthermore, when the motor is a stepping motor, the sample stretching amount generated by single pulse
Wherein r isA、rBAnd rCRepresents radii of gear A, gear B and gear C, θ0Representing the pitch angle of the motor.
Further, the laser probe is obliquely incident on the sample.
The invention has the beneficial effects that:
the invention has no conductive requirement on the film material, does not need a pretreatment process, can measure only by fixing the two ends of the sample to be measured, and has convenient operation; the heating mode of the invention is non-contact, reduces the influence caused by contact thermal resistance, introduces a vacuum environment, avoids the influence of convection heat transfer, and improves the accuracy and convenience of calculation; the invention adopts the experiment picture of the infinitesimal treatment and combines the numerical calculation method, the principle is simple, and the heat conductivity coefficient and the heat diffusion coefficient under each temperature can be directly calculated; the invention can make the sample produce different strain through the driving mechanism, and can measure the thermophysical property parameter under different strain; according to the invention, through laser heating, the output power of laser is adjustable, and the heat conductivity coefficients and the heat diffusion coefficients of materials with different heat conductivity capacities and different sizes at different temperature levels can be researched.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus according to an embodiment of the present invention.
Fig. 2 is a schematic view showing the operation of the tension mechanism and the drive mechanism (the guide rail is omitted) in the embodiment of the present invention.
Fig. 3 is a thermal equilibrium analysis of steady state heat transfer in a laser spot in an embodiment of the invention.
Fig. 4 is a graph of thermal conductivity versus relative position for the center of the spot in an embodiment of the invention.
Fig. 5 is a graph of thermal diffusivity versus relative position for the center of a spot in an embodiment of the present invention.
Fig. 6 is a graph showing the sensitivity of temperature to thermal conductivity in the example of the present invention.
FIG. 7 is a graph comparing the inversion result of the thermal conductivity at different temperatures with the initial value in the embodiment of the present invention.
In the figure: 1-vacuum chamber; 2-heat sink; 3-a guide rail; 4-sample; 5-a gear train; 6, a motor; 7-a power supply; 8-an air pump; 9-a germanium window; 10-a computer; 11-an infrared camera; 12-a laser probe; 13-laser.
Detailed Description
The invention is explained in more detail below with reference to the drawings and examples.
As shown in figure 1, the device for measuring the thermal conductivity and the thermal diffusivity of the thin film material under strain comprises a vacuum cavity 1 with a light transmission window, a laser probe 12 which is hermetically extended into the vacuum cavity 1, a laser 13 which is connected with the laser probe 12, an air suction pump 8 which is used for vacuumizing the vacuum cavity 1, an infrared camera 11 which faces the light transmission window and shoots a sample in the vacuum cavity 1 (the infrared camera 11 is fixedly installed through a support frame), a data processing module (a computer 10) which is connected with the infrared camera 11, a tensioning mechanism and a driving mechanism which are positioned in the vacuum cavity 1, wherein the tensioning mechanism is used for tensioning two ends of the sample 4, and the driving mechanism is used for driving the tensioning mechanism to control the sample 4 to generate micro displacement.
Preferably, the light transmission window is a germanium window 9.
As shown in fig. 1, the laser probe 12 is preferably obliquely incident on the sample 4 to prevent interference with the imaging of the infrared camera 11. The incident power and the incident angle of the laser can be changed for samples with different sizes, so that the sample 4 can reach the required temperature rise.
As shown in fig. 1 and 2, the tension mechanism preferably includes two pairs of heat sinks 2 (the heat sinks 2 may be made of tungsten copper alloy) which are flush with each other and located at both ends of the sample, and each pair of heat sinks 2 clamps and bolts the ends of the sample 4 from the upper and lower sides.
As shown in fig. 1 and fig. 2, preferably, the driving mechanism includes a guide rail 3, a rack D, a motor 6 and a gear train 5, one pair of heat sinks 2 is fixed, the lower heat sink 2 of the other pair of heat sinks 2 is slidably fitted on the guide rail 3, the upper heat sink 2 is fixed with the rack D, the motor 6 is engaged with the rack D through the gear train 5, and a power line of the motor 6 is hermetically extended out of the vacuum chamber 1 and connected with a power supply 7.
As shown in fig. 2, it is preferable that the gear train 5 includes a motor output shaft, a pinion gear a provided on the motor output shaft, a fixed shaft, and a large gear B and a pinion gear C provided on the fixed shaft, the pinion gear a being engaged with the large gear B, and the pinion gear C being engaged with the rack D.
Before measurement, the emissivity of the sample 4 is determined, the thermocouple is used for measuring the surface temperature of the sample, and the emissivity of the infrared camera is adjusted at the same time until the surface temperature measured by the infrared camera is the same as the temperature measured by the thermocouple, wherein the emissivity is the real emissivity of the sample 4.
When measuring the thermal conductivity and thermal diffusivity of a thin film material under strain, the method comprises the following steps:
s1, placing the sample 4, the tensioning mechanism and the driving mechanism into the vacuum cavity 1, fixing one pair of heat sinks 2 on the guide rail 3, matching the other pair of heat sinks 2 with the guide rail 3, spreading the sample 4 with the two pairs of heat sinks 2 at the same height, respectively clamping two ends of the sample 4 by the two pairs of heat sinks 2 to enable the sample 4 to be kept horizontal, and then fastening by using bolts to prevent the relative displacement with the heat sinks 2 in the stretching process.
S2, installing a gear transmission system 5 to enable a motor 6 to be meshed with a rack D through the gear transmission system 5, and when the motor is a stepping motor, the sample stretching amount generated by single pulse
Wherein r isA、rBAnd rCRepresents radii of gear A, gear B and gear C, θ0Representing the pitch angle of the motor 6.
The total amount of stretching being equal to the number of pulses multiplied by the amount of stretching produced by a single pulse, e.g. by using a two-phase stepping motor 6, the length of the film side Lx80mm, its step angle theta01.8 degrees, the gear radius is rA＝rC＝5mm，rBWhen the thickness is 50mm, the stretching amount Deltax of the film generated by corresponding single pulse is 15.7um and the strain is changed
By adjusting the radius of the gear, the strain value can be smaller and can be adjusted correspondingly according to the size of the film.
And S3, covering a top cover with a germanium window 9, and obliquely extending the laser probe 12 into the vacuum chamber 1.
And S4, after the infrared camera 11 is adjusted up and down to focus, the infrared camera is fixed and is in stable data connection with the data processing module (the computer 10).
S5, detecting the interface of the vacuum cavity 1 to ensure the interface is sealed and airtight, starting the air pump 8 to keep the air pressure in the vacuum cavity 1 at 1 x 10-4Pa。
And S6, turning on the laser, wherein the power and the incident angle of the laser can be adjusted, and a stable and uniform heat source is provided for the sample 4.
Meanwhile, the temperature inside the vacuum cavity 1 is photographed in real time through the infrared camera 11, and a temperature distribution diagram of the whole process from the beginning of heating to the temperature distribution reaching the temperature is obtained.
S7, regarding the sample 4 as two-dimensional heat transfer (by using data processing software such as MATLAB) to process the experimental picture to obtain the temperature of each pixel point on the surface of the sample 4, and dividing the sample 4 into a plurality of infinitesimals according to the size of the pixel point, thereby obtaining the temperature values of different infinitesimals under fixed strain.
And S8, establishing a steady-state and transient-state heat balance equation, and solving the thermal conductivity and thermal diffusivity of the sample 4 at different temperatures.
For the analysis of the infinitesimal heat balance in the laser spot in the steady-state two-dimensional heat transfer process, the heat balance is shown in FIG. 3
Wherein,
where Δ x and Δ y represent the lengths of the infinitesimal elements in the x-and y-directions, respectively, and λ(m，n)Represents the thermal conductivity of the infinitesimal element, d represents the thickness of the sample, T(m-1，n)And T(m+1，n)Respectively representing the temperatures, T, of two units in front and behind the infinitesimal in the x direction(m，n-1)And T(m，n+1)Respectively represent infinitesimal elements inThe temperature of the front and rear two units in the y direction;
p Δ x Δ y represents the amount of heat incident to the laser flowing into the micro-element;
Similarly, the heat balance equation outside the two-dimensional steady-state heat transfer light spot is written as
By combining the above equation and the temperature values of the points, λ at different positions can be obtained(m，n)And then the temperature T of the position corresponding to the temperature(m，n)The heat conductivity coefficient lambda of the film material at different temperatures can be obtainedT。
Similarly, writing out the heat balance equations inside and outside the two-dimensional transient heat transfer light spot, which are respectively
In the light spot
Outside the light spot
Wherein,
representing the change of internal energy of the infinitesimal due to temperature rise within the time delta tau, a represents the thermal diffusivity of the film material,
and
respectively representing the temperature value of the infinitesimal at the next moment and the moment. Combining the above equation, and adding the thermal conductivity lambda obtained in the previous stage, the thermal diffusion coefficient a at different temperatures can be obtained by numerical calculationT。
S9, driving the tensioning mechanism by the driving mechanism, controlling the sample 4 to generate a tiny displacement delta x (micrometer scale), generating different strains on the sample 4, and calculating the condition that the thermal conductivity and thermal diffusivity of the sample 4 change with temperature under different strains according to the steps S2-S4. The thermal conductivity coefficient lambda under different strains can be obtained by changing the film strainTAnd coefficient of thermal diffusion aT。
The heat transfer of the silica film was numerically solved using simulation software to obtain fig. 4 to 7. As can be seen from FIG. 6, when the error range of the temperature is + -1K, the influence on the thermal conductivity is only + -2%; when the thermal conductivity fluctuates within a range of ± 10%, the temperature changes by about 10K. The temperature is very sensitive to the change of the heat conductivity coefficient in the calculation mode, and the error of the temperature is smaller to the error of the required heat conductivity, so that the accurate result can be obtained.
The invention has no conductive requirement on the film material, does not need a pretreatment process, can measure only by fixing the two ends of the sample to be measured, and has convenient operation; the heating mode of the invention is non-contact, reduces the influence caused by contact thermal resistance, introduces a vacuum environment, avoids the influence of convection heat transfer, and improves the accuracy and convenience of calculation; the invention adopts the experiment picture of the infinitesimal treatment and combines the numerical calculation method, the principle is simple, and the heat conductivity coefficient and the heat diffusion coefficient under each temperature can be directly calculated; the invention can make the sample produce different strain through the driving mechanism, and can measure the thermophysical property parameter under different strain; according to the invention, through laser heating, the output power of laser is adjustable, and the heat conductivity coefficients and the heat diffusion coefficients of materials with different heat conductivity capacities and different sizes at different temperature levels can be researched.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (10)
1. A method for measuring the thermal conductivity and thermal diffusivity of a thin film material under strain is characterized in that: comprises the steps of (a) carrying out,
s1, spreading the sample, tensioning the sample by the tensioning mechanisms at two ends, placing the sample, the tensioning mechanism and the driving mechanism into a vacuum cavity, sealing and vacuumizing the vacuum cavity, and only considering heat conduction and heat radiation;
s2, heating the sample in the vacuum cavity by using continuous laser, and obtaining a temperature distribution diagram of the sample in the whole process from the beginning to the steady state under the fixed strain through an infrared camera;
s3, because the thickness of the film is far smaller than the side length, the film is regarded as two-dimensional heat transfer, the experimental picture is processed to obtain the temperature of each pixel point on the surface of the film, the film is divided into a plurality of micro-elements according to the size of the pixel point, and thus the temperature values of different micro-elements under fixed strain are obtained;
s4, establishing a steady-state and transient-state heat balance equation, and solving the heat conductivity coefficient and the heat diffusion coefficient of the film at different temperatures;
s5, the driving mechanism drives the tensioning mechanism, the sample is controlled to generate the micro displacement delta x, the sample generates different strains, and the conditions that the thermal conductivity and the thermal diffusivity of the sample change along with the temperature under different strains are obtained according to the steps S2 to S4.
2. The method of measuring thermal conductivity and thermal diffusivity of a thin film material under strain of claim 1 wherein:
in step S4, a steady state process is established
Established transient process
Wherein,
where Δ x and Δ y represent the lengths of the infinitesimal elements in the x-and y-directions, respectively, and λ(m，n)Represents the thermal conductivity of the micro-element, d represents the thickness of the sample, T(m-1，n)And T(m+1，n)Respectively representing the temperatures, T, of two units in front and behind the infinitesimal in the x direction(m，n-1)And T(m，n+1)Respectively representing the temperature of the front unit and the rear unit of the infinitesimal in the y direction;
p Δ x Δ y represents the amount of heat that the laser heats to flow into the infinitesimal element, wherein P is the incident intensity of the laser;
3. The method of measuring thermal conductivity and thermal diffusivity of a thin film material under strain of claim 1 wherein: before measurement, the emissivity of the sample is determined, the surface temperature of the sample is measured by using the thermocouple, and the emissivity of the infrared camera is adjusted at the same time until the surface temperature measured by the infrared camera is the same as the temperature measured by the thermocouple, wherein the emissivity is the real emissivity of the sample.
4. A device for measuring the thermal conductivity and thermal diffusivity of a thin film material under strain is characterized in that: the device comprises a vacuum cavity with a light transmission window, a laser probe hermetically extending into the vacuum cavity, a laser connected with the laser probe, an air pump used for vacuumizing the vacuum cavity, an infrared camera for shooting a sample in the vacuum cavity facing the light transmission window, a data processing module connected with the infrared camera, a tensioning mechanism and a driving mechanism, wherein the tensioning mechanism is used for tensioning two ends of the sample, and the driving mechanism is used for driving the tensioning mechanism to control the sample to generate micro displacement.
5. The apparatus for measuring thermal conductivity and thermal diffusivity of thin film materials under strain of claim 4 wherein: the light-transmitting window adopts a germanium window.
6. The apparatus for measuring thermal conductivity and thermal diffusivity of thin film materials under strain of claim 4 wherein: the tensioning mechanism comprises two pairs of heat sinks which are flush and respectively positioned at two ends of the sample, and each pair of heat sinks clamps the end part of the sample from the upper side and the lower side and is fastened through a bolt.
7. The apparatus for measuring thermal conductivity and thermal diffusivity of thin film materials under strain of claim 6 wherein: the driving mechanism comprises a guide rail, a rack, a motor and a gear transmission system, wherein one pair of heat sinks are fixed in position, the lower heat sink of the other pair of heat sinks is in sliding fit with the guide rail, the upper heat sink of the other pair of heat sinks is fixed with the rack, the motor is meshed with the rack through the gear transmission system, and a power line of the motor hermetically extends out of the vacuum cavity and is connected with a power supply.
8. The apparatus for measuring thermal conductivity and thermal diffusivity of thin film materials under strain of claim 7 wherein: the gear transmission system comprises a motor output shaft, a pinion A arranged on the motor output shaft, a fixed shaft, and a bull gear B and a pinion C arranged on the fixed shaft, wherein the pinion A is meshed with the bull gear B, and the pinion C is meshed with a rack.
9. The apparatus for measuring thermal conductivity and thermal diffusivity of thin film materials under strain of claim 8 wherein: sample stretching amount generated by single pulse when the motor is a stepping motor
Wherein r isA、rBAnd rCRepresents radii of gear A, gear B and gear C, θ0Representing the pitch angle of the motor.
10. The apparatus for measuring thermal conductivity and thermal diffusivity of thin film materials under strain of claim 4 wherein: the laser probe is obliquely incident on the sample.
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| CN112577992A (en) * | 2020-11-04 | 2021-03-30 | 亚士漆(上海)有限公司 | Thermal radiation testing device and method |
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| CN114113207A (en) * | 2021-11-12 | 2022-03-01 | 中国科学院上海光学精密机械研究所 | Method for measuring thermal diffusion coefficient of optical material |
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