CN104034752A - Device and method for measuring longitudinal thermal conductivity of film - Google Patents
Device and method for measuring longitudinal thermal conductivity of film Download PDFInfo
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- CN104034752A CN104034752A CN201410267294.4A CN201410267294A CN104034752A CN 104034752 A CN104034752 A CN 104034752A CN 201410267294 A CN201410267294 A CN 201410267294A CN 104034752 A CN104034752 A CN 104034752A
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Abstract
The invention relates to a method for measuring the longitudinal thermal conductivity of a film. A device comprises a phase-locked amplifier, a current-source function generator, a differential amplifier, an adjustable resistor, a metal wire, a thermoelectric module and a direct-current voltage stabilizing source. The method can overcome the measurement error caused by length and width, is more accurate and adopts 3omega method to measure the longitudinal thermal conductivity of the film. The method has the advantages that a plurality of times of measurement of different widths and lengths are carried out by depositing the metal wires with different widths and lengths to overcome the measurement error caused by the length and the width, and simultaneously the film materials with different conducting performances can be tested; based on the principle of the differential 3omega method, the operation is convenient, the response is fast and the measurement accuracy is high.
Description
Technical field
The invention belongs to material properties test technical field, be specifically related to a kind of device and method of measuring the longitudinal thermal conductivity of film.
Background technology
At the end of the eighties in last century, Cahill proposes to utilize 3 ω methods to carry out the thermal conductivity coefficient of test material, and 3 ω methods are a kind of transient measurement methods, mainly can be used for testing the thermal conductivity coefficient of vertical thin-film direction.For other film thermal quantitative measurement methods, 3 ω methods are utilized the temperature fluctuation of METAL HEATING PROCESS line and the heat transfer theory model of finite width heating source to combine to determine the thermal conductivity coefficient of material, do not need to take a long time to keep the stable of hot-fluid, and can effectively reduce the impact of heat radiation on test result precision, thereby can improve speed and the precision of test.3 ω methods, through constantly development for many years, have become a kind of important means of film thermal conductivity coefficient test at present.Measuring principle: can produce the Joule heat that frequency is 2 ω while passing to frequency and be the alternating current of ω in metal wire, and cause the fluctuation of metal wire temperature.For simple metal, its resistance and temperature line relationship, therefore, be the concussion resistance of 2 ω by the frequency of occurrences in metal wire.This frequency is the concussion resistance of 2 ω and the alternating current acting in conjunction that frequency is ω, so just obtained frequency, is the voltage of 3 ω, by measuring 3 ω voltages, just can obtain the temperature fluctuation situation of metal wire.3 ω methods are directly applied to metallic film thermal conductance to be measured, can be because heating element is close with measured material thermal property, introduce larger measuring error, therefore 3 traditional ω methods cannot directly apply to metallic film material, and also most important for the selection of heated wire, because heated wire is longer, the upper frequency limit of measuring is higher, and lower limit is lower, but oversize, be difficult to guarantee that bar is wide evenly, thereby cause heat flux distribution inhomogeneous.Heated wire is narrower, and just higher for the lower-frequency limit of measuring, available scope is just narrower; Width is too large, can make again the thermoosmosis of he and film suitable, and relation can not linearization between the logarithm of heating frequency for Temperature Distribution, also can bring larger error to thermal conductivity measurement.
Summary of the invention
The defect existing for prior art, the object of this invention is to provide a kind of device and method of measuring the longitudinal thermal conductivity of film, if film to be measured is non-insulating material, can between film to be measured and heated wire, increase an insulation course, play the effect of insulation, can measure the film of conductor, semiconductor, insulating material simultaneously, by micro fabrication, deposit multiple different in width, length heated wire simultaneously, carrying out heated wire optionally measures, increase the accuracy of measuring, improve precision.
for achieving the above object, technical scheme of the present invention is:
1. a device of measuring the longitudinal thermal conductivity of film, comprising: lock-in amplifier, current source function generator, differential amplifier, adjustable resistor, metal wire, temperature control platform electrothermal module and direct-flow voltage regulation source.It is characterized in that: described differential amplifier comprises the first differential amplifier and the second differential amplifier; Described metal wire is drawn four contact electrodes and is used for line, comprises the first, the second, three, the 44 contact electrode; Described current source function generator is connected with metal wire contact electrode, is used for producing the electric current of setting value to metal wire; The 3rd metal wire contact electrode is connected with differential amplifier, is used for amplification voltage signal; The second metal wire contact electrode is connected with adjustable resistor; Adjustable resistor is connected with the second differential amplifier, is used for amplification voltage signal; Through the first and second differential amplifiers, be connected with lock-in amplifier respectively with adjustable resistor with metal wire, be used for extracting voltage signal; Direct-flow voltage regulation source is connected with temperature control platform electrothermal module, is used to provide uniform heating.
2. according to the device of the longitudinal thermal conductivity of measurement film described in claims 1, it is characterized in that: described metal wire has different live widths and line length according to design.
3. according to the device of the longitudinal thermal conductivity of measurement film described in claims, it is characterized in that: described film to be measured is conductive film or non-conductive film, and shape is any.
4. measure a method for the longitudinal thermal conductivity of film, adopt said apparatus to measure, comprise that film sample to be measured prepares metal wire and thermal conductance testing procedure, it is characterized in that:
1) step of described film preparation metal wire to be measured is as follows:
(1) conductive film sample with magnetron sputtering, at film sample to be measured and reference sample front, plates insulation course respectively, if need to be taked this step;
(2) positive at film sample to be measured, make to carry out with photoresist the metal line pattern that photoetching forms multiple different in width, length, reference sample is done to identical processing simultaneously;
(3) pattern of described two samples is carried out to reactive ion etching or inductively coupled plasma etching;
(4) in described film sample to be measured, reference sample front, with magnetron sputtering, plate articulamentum Ti film and metal wire Ag film;
(5) plate metal wire film, carried out peeling off of photoresist;
2) described thermal conductance testing procedure is as follows:
(1) D.C. regulated power supply is connected to a temperature control platform electrothermal module, reference sample is positioned on temperature control platform electrothermal module, and thermocouple wire is fixed on reference sample with high temperature gummed tape;
(2) open the power supply of current source function generator, lock-in amplifier and differential amplifier, on current source, selecting electric current is effective value pattern;
(3) four probes are contacted respectively to us and plate out on the metal wire of reference sample, by four probe method, survey the resistance of metal wire;
(4) open the power supply of direct-flow voltage regulation source, give temperature control platform electrothermal module voltage, heat, by data collector, gather the relation between metal wire resistance and temperature, by linear fit, obtain slope, further obtain reference sample temperature-coefficient of electrical resistance;
(5) by current source, give the electric current of metal wire certain value, regulate the resistance value of variable resistance box, make the detection registration of lock-in amplifier for minimum;
(6) select 3 overtones bands of lock-in amplifier, and by changing the power frequency of the input of current source, with data collector, obtain the voltage of reference sample 3 overtones bands simultaneously;
(7) by the temperature-coefficient of electrical resistance of reference sample and the voltage substitution theoretical formula of 3 overtones bands that obtain before:
, obtain the undulating quantity of reference sample temperature, in formula, represent the temperature fluctuation of film to be measured (2b),
represent 3 overtones bands of metal wire,
the current value of representative input metal wire, represents temperature-coefficient of electrical resistance;
(8) with reference to sample, change film sample to be measured into, open the power supply of direct-flow voltage regulation source, give temperature control platform voltage, heat, by data collector, gather the relation between film metal line resistance to be measured and temperature, by linear fit, obtain slope, further obtain the temperature-coefficient of electrical resistance of film to be measured
(9) by knowing reference sample and film sample to be measured, and guarantee that reference sample and film sample to be measured have identical power input, determine the electric current of input film to be measured, and carry out the test of corresponding temperature-coefficient of electrical resistance and 3 overtones bands;
(10) by the temperature-coefficient of electrical resistance of film sample to be measured and the voltage substitution theoretical formula of 3 overtones bands that obtain:
, obtain the undulating quantity of film temperature;
(11) pass through formula
, obtain
, utilize formula
, obtain the thermal conductance value of film to be measured
, in formula
represent the temperature fluctuation that film sample to be measured and reference sample are total,
represent reference sample temperature fluctuation,
film sample temperature fluctuation to be measured,
represent the width of metal wire,
represent the length of metal wire,
represent film thickness;
(12) utilize the different length plating before us, the metal wire of width, can carry out repeatedly the thermal conductance test of film.
the present invention compared with prior art, has following apparent outstanding substantive distinguishing features and technical progress:
The invention has the advantages that by the metal wire of deposition different in width, length, according to actual conditions, optionally selecting resistance wire tests, and carry out repeatedly different in width, linear measure longimetry, overcome the measuring error of bringing because of length, width, by sputter insulation course, can test the membraneous material of different electric conductivities simultaneously.
Accompanying drawing explanation
Fig. 1 is the heated wire that the present invention proposes different length, width
1a: long: 2mm, wide: 2 μ m; 1(b): long: 2mm, wide: 10 μ m;
1c: long: 2mm, wide: 20 μ m; 1(d): long: 2mm, wide: 30 μ m;
1e: long: 4mm, wide: 2 μ m; 1(f): long: 4mm, wide: 10 μ m;
1g: long: 4mm, wide: 20 μ m; 1(h): long: 4mm, wide: 30 μ m;
Fig. 2 is testing sample, the reference sample of the preparation that proposes of the present invention
2a: testing sample; 2b: reference sample; 2c: substrate; 2d: film to be measured;
2e: insulation course; 2f: metal wire;
Fig. 3 is a kind of structural representation of measuring the longitudinal thermal conductivity device of film that the present invention proposes.
Fig. 4 is the reference sample resistance that records in embodiment and the relation of temperature;
Fig. 5 is the voltage of reference sample 3 overtones bands that record in embodiment and the relation of frequency;
Fig. 6 is the film sample resistance to be measured that records in embodiment and the relation of temperature;
Fig. 7 is the voltage of film sample to be measured 3 overtones bands that record in embodiment and the relation of frequency;
Fig. 8 is the reference sample recording in embodiment, the voltage of film sample to be measured 3 overtones bands and the relation of frequency.
Embodiment
Details are as follows by reference to the accompanying drawings for the preferred embodiments of the present invention:
embodiment mono-:
Referring to figure tri-, the device of the longitudinal thermal conductivity of this measurement film, comprise: lock-in amplifier (3f), current source function generator (3c), differential amplifier (3e), adjustable resistor (3g), metal wire (3d), temperature control platform electrothermal module (3b) and direct-flow voltage regulation source (3a).It is characterized in that: described differential amplifier (3e) comprises the first differential amplifier (3e1) and the second differential amplifier (3e2); Described metal wire (3d) is drawn four contact electrodes and is used for line, comprises the first, the second, three, the 44 contact electrode (3d1,3d2,3d3,3d4); Described current source function generator (3c) is connected with metal wire contact electrode (3d1), is used for producing the electric current of setting value to metal wire (3d); The 3rd metal wire contact electrode (3d3) is connected with differential amplifier (3e1), is used for amplification voltage signal; The second metal wire contact electrode (3d2) is connected with adjustable resistor (3g); Adjustable resistor (3g) is connected with the second differential amplifier (3e2), is used for amplification voltage signal; Through the first and second differential amplifiers (3e1,3e2), be connected with lock-in amplifier (3f) respectively with metal wire (3d) and adjustable resistor (3g), be used for extracting voltage signal; Direct-flow voltage regulation source (3a) is connected with temperature control platform electrothermal module (3b), is used to provide uniform heating.
embodiment bis-:
Referring to Fig. 3, the device of the longitudinal thermal conductivity of this measurement film, comprise: lock-in amplifier (3f), current source function generator (3c), differential amplifier (3e), adjustable resistor (3g), metal wire (3d), electrothermal module (3b), direct-flow voltage regulation source (3a).Current source function generator (3c) is connected with metal wire, be used for producing certain value to metal wire (3d) and obtain electric current, that function generator adopts is AC/DC current source Keithley 2182A, and it can provide amplitude range is that 2 pA-100 mA frequency ranges are the ac current signal of 1 mHz-100 kHz; Metal wire (3d) is connected with differential amplifier (3e), is used for amplification voltage signal, and differential amplifier model is AD524AD, and the model of adjustable resistor is ZX25P, and precision is 0.01 Ω; Metal wire (3d) is connected with adjustable resistor (3g); Adjustable resistor (3g) is connected with differential amplifier (3e), is used for amplification voltage signal; The differential amplifier (3e) being connected respectively with adjustable resistor (3g) with metal wire (3d) be connected, be used for extracting voltage signal, lock-in amplifier is U.S. Stanford Research Systems product, model is SR830, and it can extract the feeble signal in test 1 mHz-102.4 kHz frequency range; Direct-flow voltage regulation source (3a) is connected with temperature control platform electrothermal module (3b), be used to provide uniform heating, temperature control platform is the electrothermal module of 50 mm * 50 mm, and model is TEC1-12726, and the heating that its surface can provide or cryogenic temperature scope are-10 ℃-100 ℃.
embodiment tri-:
The method of the longitudinal thermal conductivity of this testing film, adopts said apparatus measurement to comprise film sample preparation to be measured and two parts of thermal conductance testing procedure:
1. the concrete embodiment of sample preparation is as follows:
(1) by N-type, crystalline phase, be (100), the monocrystalline silicon piece of hydrofluorite removal thermal oxide generation monox is soaked as substrate in surface, and preparing one has film to be measured and do not have film sample to be measured (reference sample);
(2) with magnetron sputtering, in film sample to be measured and reference sample film front, plate respectively the Si of 150～250nm
3n
4film, as insulation course, if conductive film must plate insulation course;
(3) to being coated with Si
3n
4film to be measured and the reference sample of film insulation course, used different length, width resistance wire layer mask plate, and even painting negative photoresist carries out photoetching, forms resistive layer pattern, as shown in Figure 1;
(4) to be measured film and the reference sample complete to even glue photoetching, carries out reactive ion etching, is mainly that the shape of the metal wire that guarantee to form is more smooth, stable;
(5) complete to even glue photoetching and be coated with Si
3n
4film to be measured and the reference sample of film insulation course, used magnetron sputtering first to plate lower floor's articulamentum of Ti (10～30 nm) conduct, then continues with magnetron sputtering Ag(150～250nm) metal wire, Si after peeling off
3n
4film forms the pattern identical with metal wire, as shown in Figure 1;
2. it is as follows that thermal conductance is tested concrete embodiment
(1) D.C. regulated power supply 3a is connected to a temperature control platform 3b, and the temperature control platform 3b that we adopt is electrothermal module, reference sample 2b is positioned on electrothermal module, and thermocouple wire is fixed on reference sample with high temperature gummed tape;
(2) open the power supply of current source function generator 3c, data collector, lock-in amplifier 3f and differential amplifier 3e, on current source, selecting electric current is effective value pattern;
(3) four probes are contacted respectively to us and plate out the metal wire 3d of reference sample upper, by four probe method, survey the resistance of metal wire
(4) open the power supply of direct-flow voltage regulation source, give temperature control platform (electrothermal module) voltage, heat, by data collector, gather the relation between metal wire resistance and temperature, by linear fit, obtain slope, further obtain reference sample temperature-coefficient of electrical resistance;
(5) by current source, give the electric current of metal wire set-point (getting 50mA here), regulate the resistance value of variable resistance box 3g, make the detection registration of lock-in amplifier for minimum;
(6) select 3 overtones bands of lock-in amplifier, and by changing the power frequency of the input of current source, frequency values is got: 101,112,126 here, 141,158,178,199,224,251,282,316,355,398,447,501,562,631,708,794,891,999, unit: hertz, with data collector, obtain the voltage of reference sample 3 overtones bands simultaneously;
(7) by the temperature-coefficient of electrical resistance of reference sample (comprising substrate, insulation course) and the voltage substitution theoretical formula of 3 overtones bands that obtain before:
, obtain the undulating quantity of reference sample temperature, as Fig. 5, in formula
represent the temperature fluctuation of film to be measured (2b),
represent 3 overtones bands of metal wire,
the current value of representative input metal wire,
represent temperature-coefficient of electrical resistance;
(8) with reference to sample, change film sample to be measured into, open the power supply of direct-flow voltage regulation source, give temperature control platform (electrothermal module) voltage, heat, by data collector, gather the relation between film metal line resistance to be measured and temperature, by linear fit, obtain slope, further obtain temperature-coefficient of electrical resistance
(9) by knowing reference sample and film sample to be measured, and guarantee that reference sample and film sample to be measured have identical power input, determine the electric current (49.35mA) of input film to be measured, and carry out the test of corresponding temperature-coefficient of electrical resistance and 3 overtones bands.
(10) by the temperature-coefficient of electrical resistance of film sample to be measured and the voltage substitution theoretical formula of 3 overtones bands that obtain:
, obtain the undulating quantity of film sample to be measured (comprising substrate, film, insulation course) temperature, as Fig. 7;
(11) pass through formula
, obtain
, as Fig. 8, utilize formula
, obtain
, in formula
represent the temperature fluctuation (2b) that film sample to be measured (2a) and reference sample are total,
represent reference sample (2b) temperature fluctuation,
film sample to be measured (2a) temperature fluctuation,
represent the width of metal wire (3b),
represent the length of metal wire (3b),
represent film thickness;
(12) utilize the different length plating before us, the metal wire of width, can carry out repeatedly the thermal conductance test of film.
Claims (4)
1. a device of measuring the longitudinal thermal conductivity of film, comprise: lock-in amplifier (3f), current source function generator (3c), differential amplifier (3e), adjustable resistor (3g), metal wire (3d), temperature control platform electrothermal module (3b) and direct-flow voltage regulation source (3a); It is characterized in that: described differential amplifier (3e) comprises the first differential amplifier (3e1) and the second differential amplifier (3e2); Described metal wire (3d) is drawn four contact electrodes and is used for line, comprises the first, the second, three, the 44 contact electrode (3d1,3d2,3d3,3d4); Described current source function generator (3c) is connected with metal wire contact electrode (3d1), is used for producing the electric current of setting value to metal wire (3d); The 3rd metal wire contact electrode (3d3) is connected with differential amplifier (3e1), is used for amplification voltage signal; The second metal wire contact electrode (3d2) is connected with adjustable resistor (3g); Adjustable resistor (3g) is connected with the second differential amplifier (3e2), is used for amplification voltage signal; Through the first and second differential amplifiers (3e1,3e2), be connected with lock-in amplifier (3f) respectively with metal wire (3d) and adjustable resistor (3g), be used for extracting voltage signal; Direct-flow voltage regulation source (3a) is connected with temperature control platform electrothermal module (3b), is used to provide uniform heating.
2. according to the device of the longitudinal thermal conductivity of measurement film described in claims 1, it is characterized in that: described metal wire (3d) has different live widths and line length according to design.
3. according to the device of the longitudinal thermal conductivity of measurement film described in claims, it is characterized in that: described film to be measured is conductive film or non-conductive film, and shape is any.
4. measure a method for the longitudinal thermal conductivity of film, comprise that film sample to be measured prepares metal wire and thermal conductance testing procedure, it is characterized in that:
The step of described film preparation metal wire to be measured is as follows:
Conductive film sample with magnetron sputtering, at film sample to be measured (2a) and reference sample (2b) front, plates insulation course respectively, if need to be taked this step;
Positive at film sample to be measured, make to carry out with photoresist the metal line pattern that photoetching forms multiple different in width, length, reference sample is done to identical processing simultaneously;
The pattern of described two samples is carried out to reactive ion etching or inductively coupled plasma etching;
In described film sample to be measured (2a), reference sample (2b) front, with magnetron sputtering, plate articulamentum Ti film and metal wire Ag film;
Plate metal wire (3d) film, carried out peeling off of photoresist;
Described thermal conductance testing procedure is as follows:
D.C. regulated power supply (3a) is connected to a temperature control platform electrothermal module (3b), reference sample (2b) is positioned over to temperature control platform electrothermal module (3b) upper, and thermocouple wire is fixed on reference sample (2b) with high temperature gummed tape;
Open the power supply of current source function generator (3c), lock-in amplifier (3f) and differential amplifier (3e), on current source, selecting electric current is effective value pattern;
Four probes are contacted respectively to us and plate out the metal wire (3d) of reference sample (2b) upper, by four probe method, survey the resistance of metal wire;
Open the power supply of direct-flow voltage regulation source (3a), give temperature control platform electrothermal module (3b) voltage, heat, by data collector, gather the relation between metal wire resistance and temperature, by linear fit, obtain slope, further obtain reference sample (2b) temperature-coefficient of electrical resistance;
By current source, give the electric current of metal wire (3d) certain value, regulate the resistance value of variable resistance box (3g), make the detection registration of lock-in amplifier (3f) for minimum;
Select 3 overtones bands of lock-in amplifier (3f), and by changing the power frequency of the input of current source, with data collector, obtain the voltage of reference sample 3 overtones bands simultaneously;
Voltage substitution theoretical formula with temperature-coefficient of electrical resistance and 3 overtones bands of the reference sample obtaining before (2b):, obtain the undulating quantity of reference sample temperature, in formula
represent the temperature fluctuation of film to be measured (2b), represent 3 overtones bands of metal wire,
the current value of representative input metal wire,
represent temperature-coefficient of electrical resistance;
With reference to sample (2b), change film sample to be measured (2a) into, open the power supply of direct-flow voltage regulation source (3a), give temperature control platform (3b) voltage, heat, by data collector, gather the relation between film metal line (3b) resistance to be measured and temperature, by linear fit, obtain slope, further obtain the temperature-coefficient of electrical resistance of film to be measured (3a)
By knowing reference sample (2b) and film to be measured (2a) sample, and guarantee that reference sample (2b) and film sample to be measured (2a) product have identical power input, determine the electric current of input film to be measured (2a), and carry out the test of corresponding temperature-coefficient of electrical resistance and 3 overtones bands;
Voltage substitution theoretical formula with temperature-coefficient of electrical resistance and 3 overtones bands of the film sample to be measured (2a) obtaining:
, obtain the undulating quantity of film temperature;
Pass through formula
, obtain
, utilize formula
, obtain the thermal conductance value of film to be measured
, in formula
represent the temperature fluctuation (2b) that film sample to be measured (2a) and reference sample are total,
represent reference sample (2b) temperature fluctuation,
film sample to be measured (2a) temperature fluctuation,
represent the width of metal wire (3b),
represent the length of metal wire (3b),
represent film thickness;
Utilize the different length plating before us, the metal wire of width, can carry out repeatedly the thermal conductance test of film.
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| CN105241918A (en) * | 2015-09-30 | 2016-01-13 | 北京大学 | Low temperature thermal conductivity measurement method |
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| US11275041B2 (en) | 2018-01-24 | 2022-03-15 | Wuhan Joule Yacht Science & Technology Co., Ltd. | Method and device for testing thermal conductivity of nanoscale material |
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| CN108398456A (en) * | 2018-01-24 | 2018-08-14 | 武汉嘉仪通科技有限公司 | The test method and device of nanometer sized materials thermal conductivity |
| CN111458369A (en) * | 2020-05-20 | 2020-07-28 | 国家纳米科学中心 | Device and method for measuring in-plane thermal conductivity of thin film |
| CN111458369B (en) * | 2020-05-20 | 2023-03-31 | 国家纳米科学中心 | Device and method for measuring heat conductivity in thin film surface |
| CN111537561A (en) * | 2020-06-17 | 2020-08-14 | 清华大学 | Method and system for measuring interface thermal resistance |
| CN111537561B (en) * | 2020-06-17 | 2021-11-23 | 清华大学 | Method and system for measuring interface thermal resistance |
| CN113820355A (en) * | 2021-08-31 | 2021-12-21 | 东南大学 | 3 omega test bed and test method thereof |
| CN114509469A (en) * | 2022-01-14 | 2022-05-17 | 清华大学 | Method for measuring thermal conductivity and interface thermal resistance of heterojunction sample thin film and substrate |
| CN114509469B (en) * | 2022-01-14 | 2023-11-14 | 清华大学 | Method for measuring thermal conductivity and interface thermal resistance of heterojunction sample film and substrate |
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Application publication date: 20140910 |