CN105241918A - Low temperature thermal conductivity measurement method - Google Patents
Low temperature thermal conductivity measurement method Download PDFInfo
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- CN105241918A CN105241918A CN201510642265.6A CN201510642265A CN105241918A CN 105241918 A CN105241918 A CN 105241918A CN 201510642265 A CN201510642265 A CN 201510642265A CN 105241918 A CN105241918 A CN 105241918A
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Abstract
The invention relates to a low temperature thermal conductivity measurement method. The method can be used for measuring the thermal conductivity of a solid substrate or a film at normal temperature or a low temperature. The method is a 3omega method based on solid material thermal conductivity measurement, and is improved from the following aspects: the thickness of a film on a substrate is changed, measurement is carried out multiple times, and the vertical thermal conductivity of the film is obtained through a difference technology, so the measured value deviation caused by boundary thermal resistance on a film and substrate interface is effectively avoided; a preamplifier with extremely low linear deflection is arranged in front a lock-in amplifier for measurement, and amplifies a signal 10 times, so the measurement precision is effectively improved; the amplification factor of the preamplifier is adjusted through a one-chip microcomputer control digital potentiometer, so fully-automatic measurement is realized; and a measurement warm area is expanded to extremely low temperature by adopting magnetic material permalloy.
Description
Technical field
The present invention is a kind of measuring method of solid material thermal conductivity, especially a kind of method measuring solid substrate or film thermal conductivity under normal temperature or low temperature.
Background technology
3 ω methods are a kind of methods measuring solid substrate or thermal conductivity of thin film.(Thermalconductivitymeasurementfrom30to750K:the3 ω method, Cahill, DavidG., ReviewofScientificInstruments, 61,802-808 (1990)) low-temperature thermal conductivity measuring method involved in the present invention is based on 3 ω methods.
The measuring principle of 3 ω methods is: put a thin conductor silk on solid dielectric material surface, applies sinusoidal alternating current, and measure the voltage signal at conductor silk two ends by external circuit to conductor silk.Because exchange current produces heating power with the double frequency of source signal on conductor silk, the temperature change in oscillation thereupon of conductor silk, and then resistance value is with the double frequency change in oscillation of source signal, thus the voltage signal at conductor silk two ends comprises an overtones band and treble frequency two compositions of source signal, its ratio reflects the amplitude of conductor silk temperature oscillation.Concrete quantitative relationship is:
Source signal same-phase component amplitude=(2/ conductor silk temperature-coefficient of electrical resistance) × (the treble frequency signal amplitude/mono-overtones band signal amplitude) of temperature oscillation.
The source signal same-phase component amplitude of temperature oscillation and the logarithm of source signal frequency linear, change source signal frequency repetitive measurement temperature amplitude, temperature amplitude-frequency logarithm figure line done to linear fit, can draw material thermal conductivity by slope.Concrete quantitative relationship is:
Temperature amplitude-frequency natural logarithm slope=﹣ conductor silk heating power/(2 π × conductor filament length degree × substrate thermal conductivity).
Membraneous material to be measured being grown on substrate, and on film, putting thin conductor silk, by measuring the measurement graphical comparisons of the temperature amplitude-frequency logarithm figure line obtained and the backing material not putting film, the thermal conductivity of film can be drawn from its difference.Concrete quantitative relationship is:
Difference=heating power × film thickness/(the conductor silk width × conductor filament length degree × thermal conductivity of thin film) of temperature amplitude.
The implementation method of 3 ω methods is generally: rectangular tab detected materials cutting being made into surfacing, its length of side is about 0.5-1cm, thickness is about 400-600um, and surface metal mask plate or photoetching method define conductor filament shape thereon, physical vaporous deposition is used to make the metallic conductor silk that a layer thickness is about 20-100nm, its width is about 5-40um, the metal that the optional temperature-coefficient of electrical resistance of material is larger, as Au/Pt.The two ends of conductor silk are respectively provided with voltage end, current terminal two electrodes, and are connected with metering circuit.Metering circuit is generally: the sinusoidal signal being produced certain frequency by lock-in amplifier, connect with the conductor silk on fixed value resistance, sample, respectively the voltage at fixed value resistance and sample conductor silk two ends is amplified by two prime amplifiers, and regulate the enlargement ratio of prime amplifier on fixed value resistance, make an overtones band component of two paths of signals equal, finally this two paths of signals is inputted lock-in amplifier and difference measurement frequency tripling signal.Sample is placed in the environment (as refrigeration machine) of target temperature, is measured by metering circuit, obtain temperature oscillation-frequency logarithm figure line, do the thermal conductivity that linear fit can obtain sample.Heating power on conductor silk is generally 0.5-2mW, and the frequency range of source signal is about 1-3000Hz, and sample is generally placed under 5Pa vacuum environment to reduce cross-ventilated impact.
The advantages such as 3 ω methods have fast for the thermal conductivity measuring solid substrate or film, sample easily obtains, vacuum level requirements is lower.But existing 3 ω methods have following deficiency: when measuring the thermal conductivity of film, the thermal boundary resistance in film and substrate interface cannot be deducted, make the measured value of thermal conductivity of thin film inaccurate; Metallic conductor silk temperature-coefficient of electrical resistance under the low temperature of pole is less, and treble frequency voltage signal is excessively weak, and system effectively cannot be measured under pole low temperature (<20K).
Summary of the invention
The present invention solves the deficiency of the 3 ω methods that above-mentioned solid material thermal conductivity is measured from the following aspect, and improves it:
1. effectively prevent the measured value deviation that the thermal boundary resistance in film and substrate interface causes;
2. effectively improve measuring accuracy;
3. achieve all automatic measurement;
4. measurement warm area is expanded extremely low temperature (<20K).
Specifically, the present invention is a kind of low-temperature thermal conductivity measuring method based on 3 ω methods, is solved the above-mentioned deficiency of existing measuring method, and improve it by following technological means:
1., by changing the thickness repetitive measurement of film on substrate, obtaining longitudinal thermal conductivity of film with difference method, effectively prevent the measured value deviation that the thermal boundary resistance in film and substrate interface causes.Specifically, the similar sample that preparation two film on substrate thickness is different, measures their temperature amplitude-frequency logarithm figure line respectively, is contrasted by two figure lines, can draw the thermal conductivity of film from its difference.Concrete quantitative relationship is:
Difference=heating power × the film thickness of temperature amplitude is poor/and (conductor silk width × conductor filament length degree × thermal conductivity of thin film).
Because the film-substrate thermal boundary resistance of two samples is identical, only have thickness different, when therefore doing difference to two temperature amplitude-frequency logarithm figure line, the contribution of thermal boundary resistance is eliminated, and only remains the temperature amplitude difference that thickness difference causes, thus records longitudinal thermal conductivity of film.
2. by increasing the prime amplifier of an extremely low linear deviation before measurement lock-in amplifier, and signal being amplified 10 times, effectively improve measuring accuracy.Specifically, frequency tripling composition to be measured in measuring-signal is very faint, is even less than the amplitude of various noise and undesired signal, is difficult to direct lock-in amplifier and accurately measures.The present invention proposes the solution first using prime amplifier to amplify signal.This amplification process requires the linear deviation minimum (being less than-90dB) of amplifier, therefore enlargement ratio can not arrange too high, and the present invention adopts the best multiplying power 10 in experiment test.Achieved the amplification of this multiplying power by the prime amplifier of homemade extremely low linear deviation, drastically increase measuring accuracy and validity.
3. regulated the method for prime amplifier enlargement factor by Single-chip Controlling digital regulation resistance, achieve all automatic measurement.Specifically, its resistance value is regulated by Single-chip Controlling digital regulation resistance, and then regulate the enlargement factor of prime amplifier, make each measure a frequency-doubled signal that front two prime amplifiers export accurately equal so that in the end in a prime amplifier difference disappear mutually, measurement is carried out.Other measuring system parts can utilize prior art program controlled automatic to run as refrigeration system, electronic instrument, make whole system can realize program control automatic and measure.
4., by adopting magnetic material permalloy, achieve the measurement of thermal conductivity under the low temperature of pole.Specifically, utilize dilute magnetic alloy under the low temperature of pole because Kondo effect causes the principle of resistance anomalous enhancement, make heater silk can detect sample surfaces because sine adds thermogenetic temperature oscillation, and then measure its thermal conductivity.The measurement range of this thermal conductivity measurement system is made to extend extremely low temperature.
The present invention is by taking above technological means, and carried out many-sided improvement to existing measuring method, the measuring system after improvement can arrive following effect:
1. when measuring the thermal conductivity of film, the measured deviation that the thermal boundary resistance eliminating film and substrate causes.
2. effectively improve measuring accuracy (± 5%).
3. achieve program control automatic to measure.
4. measurement range expands extremely low temperature (4K-320K).
Accompanying drawing explanation
Fig. 1 is samples devices one-piece construction schematic diagram
Fig. 2 is photo mask board design drawing
Fig. 3 is data measurement circuit structural drawing
Fig. 4 is temperature amplitude-frequency logarithm figure line exemplary plot
Embodiment
Specific embodiment of the invention method is as follows.Mainly be divided into element manufacturing and DATA REASONING two parts.It is below the implementation step of a typical practical measuring examples.
1. element manufacturing
1) sample obtains: by specimen material preparation or the rectangular tab cutting into 5mm × 7mm size, thickness is about 0.4-0.6mm.
2) surface clean: sample is put into and analyzed pure triclene ultrasonic cleaning 5min, analyzes ultrasonic cleaning 5min in pure acetone, analyzes ultrasonic cleaning 5min in pure isopropyl alcohol, dry up with high pure nitrogen.
3) dry: sample is placed on 100-200 DEG C of hot plate and toasts 10-30min.
4) whirl coating 1: sample is placed on whirl coating platform, surface drips MicroChemPMGISF6 photoresist 1-2 and drips, with 4000r/min rotating speed whirl coating 60s.
5) 1 is toasted: be placed on 170 DEG C of hot plates and toast 5min.
6) whirl coating 2: be placed on whirl coating platform, surface is continued to drip AZ1500 photoresist 1-2 and is dripped, with 5000r/min rotating speed whirl coating 60s.
7) 2 are toasted: be placed on 100 DEG C of hot plates and toast 60s.
8) photoresist trimming: with analyzing the edge corner angle of pure acetone wipe samples photomask surface glue to dissolve the tilting part of photoresist.
9) expose: use Lithographic template as shown in Figure 2 as light-blocking matter, with the mercury lamp of 300W power to sample exposure 11s.
10) dry afterwards: sample is placed on 140 DEG C of hot plates and toasts 120s.
11) develop: sample is put into AZ300MIF developer solution and to be developed 120s, puts into the fixing 60s of deionized water, put into MicroChemDeveloper101 developer solution and to develop 90s, put into the fixing 60s of deionized water, dry up with high pure nitrogen.
12) evaporation: under 20-30mTorr vacuum tightness, oxonium ion cleaning 5min is carried out to sample surfaces, then carry out physical vapour deposition (PVD) under 2E-6mbar vacuum tightness.First deposit 3nmTi, then deposit 20nmAu.
13) photoresist is removed: MicroChemRemoverPG put into by sample, at 60-150 DEG C, soak 10-30min, until photomask surface glue comes off.With high pure nitrogen, sample is dried up.
14) dotted line: sample is pasted onto on copper specimen holder, is connected with the pin of specimen holder with the electrode of aluminium matter ligament by sample conductor silk.The one-piece construction of samples devices as shown in Figure 1.
2. DATA REASONING
1) install: specimen holder is arranged in refrigeration machine, connect and measure lead-in wire.5E-2mbar is evacuated to refrigeration cavity.
2) connecting circuit: connect metering circuit according to shown in Fig. 3, sample connect prime amplifier enlargement ratio be set to 1, fixed value resistance to connect the enlargement ratio of prime amplifier variable, lock-in amplifier connect prime amplifier enlargement ratio be set to 10.The signal frequency range that lock-in amplifier exports is 1.7Hz-3kHz, and makes the heating power on sample conductor silk be 0.5mW/mm.
3) programmable data collection: refrigeration machine is cooled to treats testing temperature, data acquisition program controls the sinusoidal ac of different frequency within the scope of output 1.7Hz-3kHz to sample conductor silk.Utilize the frequency-doubled signal on lock-in amplifier measurement sample conductor silk, rear program regulates the enlargement factor of fixed value resistance two ends prime amplifier automatically, until the frequency-doubled signal that lock-in amplifier measurement obtains is minimum, and utilize the size of treble frequency signal on lock-in amplifier collected specimens conductor silk.To each frequency, in 20s, measure 200 data points and calculating mean value and variance.Calculate the temperature amplitude under different frequency, and make temperature amplitude-frequency logarithm figure line as shown in Figure 4.
4) thermal conductivity matching: slope fit is done to the linear segment in temperature amplitude-frequency logarithm figure line, calculates specimen material thermal conductivity at such a temperature.
To film sample, the basic step that its thermal conductivity is measured is same as described above, that is: 2 samples that growing film thickness is different, carry out element manufacturing according to above-mentioned steps 1, and by step 2 1)-3) carry out DATA REASONING.Record two groups of temperature amplitude are subtracted each other, and makes the figure line of its difference about frequency.One section more flat in figure line is averaged, the thermal conductivity of film can be calculated.
For needing the sample measuring thermal conductivity under the low temperature of pole, magnetic material permalloy can be selected as conductor wire material, and measure according to step described above.Due to magnetic material resistance anomalous enhancement under the low temperature of pole, so the thermal conductivity of material under successfully can measuring pole low temperature.
Claims (4)
1. the low-temperature thermal conductivity measuring method based on 3 ω methods, thermal conductivity under normal temperature or low temperature can measure solid substrate or film, it is characterized in that: by changing the thickness repetitive measurement of film on substrate, obtain longitudinal thermal conductivity of film with difference method, effectively prevent the measured value deviation that the thermal boundary resistance in film and substrate interface causes.
2. low-temperature thermal conductivity measuring system according to claim 1, is characterized in that: being amplified by signal by increasing a prime amplifier before measurement lock-in amplifier, effectively improve measuring accuracy.
3. low-temperature thermal conductivity measuring system according to claim 1, is characterized in that: the method being regulated prime amplifier enlargement factor by Single-chip Controlling digital regulation resistance, achieves all automatic measurement.
4. low-temperature thermal conductivity measuring system according to claim 1, is characterized in that: by adopting magnetic material permalloy, measurement warm area is expanded extremely low temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110057862A (en) * | 2019-04-24 | 2019-07-26 | 苏州浪潮智能科技有限公司 | A kind of method and system using unary linear regression equation test thermal contact resistance |
| CN110521104A (en) * | 2017-04-21 | 2019-11-29 | 株式会社日立制作所 | Power inverter, its diagnostic system, diagnostic method and the motor control system using it |
| CN113820355A (en) * | 2021-08-31 | 2021-12-21 | 东南大学 | 3 omega test bed and test method thereof |
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| CN113820355A (en) * | 2021-08-31 | 2021-12-21 | 东南大学 | 3 omega test bed and test method thereof |
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