CN110031504A - The test method of thermal contact resistance between a kind of circular cross-section one-dimensional nano structure - Google Patents
The test method of thermal contact resistance between a kind of circular cross-section one-dimensional nano structure Download PDFInfo
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- CN110031504A CN110031504A CN201910213215.4A CN201910213215A CN110031504A CN 110031504 A CN110031504 A CN 110031504A CN 201910213215 A CN201910213215 A CN 201910213215A CN 110031504 A CN110031504 A CN 110031504A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
Abstract
The invention discloses a kind of test methods of thermal contact resistance between circular cross-section one-dimensional nano structure, under optical microscopy or scanning electron microscope, a piece circular cross-section one-dimensional nano structure is broken into 2 sections using micromanipulator, be overlapped on respectively hanging micro element heat source, it is heat sink on, and make this two sections of samples heat source, it is heat sink between form parallel contact, the sample is tested using heat bridge method, obtains apparent thermal resistance Rtot1；Under optical microscopy or scanning electron microscope, this two sections of samples are become into cross-contact from parallel contact using micromanipulator, the sample is tested using heat bridge method, obtains apparent thermal resistance Rtot2；The thermal contact resistance of two sections of sample room unit areas can be approximated to be RCA=(Rtot2‑Rtot1)×Ac2, wherein Ac2The contact area of cross-contact between two sections of samples.The present invention improves successfully tested rate, reduces to sample quality coherence request, improves measuring accuracy.
Description
Technical field
The invention belongs to thermal physical property of solid material parameter testing technical fields, and in particular to a kind of circular cross-section 1-dimention nano
The test method of thermal contact resistance between structure.
Background technique
Thermal contact resistance between one-dimensional nano structure has microelectronic component design, thermal interfacial material design etc. important
Value.The testing scheme of thermal contact resistance can be divided into two classes between reported measurement one-dimensional nano structure: one kind can be referred to as multipoint method,
One kind can be referred to as single-point method.
In multipoint method, nanostructure heap is pressed into film, is there is in the film between a large amount of nanostructure in this way
Contact point counter can release the thermal contact resistance between nanostructure by the hot physical property of testing film sample, such as document Physical
Review Letters 102,105901(2009).However, needing to know that nanostructure is indirect in film sample in multipoint method
The density of contact, and water touching point density can not be measured accurately, cause the measurement error of multipoint method very big, or even have in magnitude
Deviation.
In single-point method, two nanostructures are overlapped, a single contact point is formed, directly or indirectly surveys
Thermal contact resistance between them out.Due to not needing the density of estimation contact point, the measuring accuracy of single-point method is significantly higher than multiple spot
Method.
Application No. is disclosing a kind of measurement method of one-dimensional material thermal contact resistance in the patent of CN201210426861.7,
This method determines the temperature on interface both sides based on the characteristic peak frequency displacement of Raman spectrum, and then determines the temperature difference on interface, obtains one
Tie up the thermal contact resistance of material.The process employs this non-contact temperature means of testing of Raman technology, simplify sample preparation
Process.But this method is only used in the material with significant Raman spectrum temperature frequency shift property, and for one-dimensional nano structure
For, since spot diameter is much larger than the characteristic size of sample, cause measuring signal weak, measurement error is big.
Application No. is disclosing a kind of thermoelectricity capability measuring system of nano material in the patent of CN201720450926.X,
The system is based on T-type law technology, can not only measure conductivity, thermal conductivity, Seebeck coefficient of one-dimensional nano structure etc., moreover it is possible to
Sample is measured with the thermal contact resistance between hot line.Since within the system, hot line is led as electrical-heating source it is necessary to have good
Electrical property, thus cannot be used for the thermal contact resistance between the one-dimensional nano structure of two kinds of electrical isolations of test.
Heat bridge method based on hanging micro element is a kind of steady state test technology, be widely used in one-dimensional nano structure conductivity,
The test of thermal conductivity and Seebeck coefficient.Inventor realizes the measurement of thermal contact resistance between carbon nanotube using heat bridge method
(Physical Review Letters 112,205901(2014)).In this scenario, measurement first is by two nanostructures
Then the entire thermal resistance for contacting sample measures the thermal resistance and its same heat source, heat sink contact heat of this two nanostructures respectively again
Resistance, to calculate the thermal contact resistance between this two nanostructures.The advantages of testing scheme is the conduction etc. to measured material
Performance has no requirement.The disadvantage is that: 1) successfully tested rate lower.In the testing scheme, need to carry out nanostructure
It is mobile on a large scale, it is easily damaged or is lost sample, reduces successfully tested rate；2) high to sample quality coherence request.Sample
It will be accumulated in the test error to thermal contact resistance in the fluctuation of length direction thermal coefficient.
Summary of the invention
Successfully tested rate is low, be the one-dimensional nano structure based on heat bridge method between sample quality coherence request height contact heat
The problem of resistance test, the present invention is directed to circular cross-section one-dimensional nano structure, proposes a kind of circular cross-section 1-dimention nano
The test method of thermal contact resistance between structure, this method reduce the manipulation amplitudes of sample, improve successfully tested rate, reduce pair
Sample quality coherence request, improves measuring accuracy.
To solve prior art problem, the technical scheme adopted by the invention is as follows:
The test method of thermal contact resistance between a kind of circular cross-section one-dimensional nano structure, comprising the following steps:
Step 1, under optical microscopy or scanning electron microscope, using micromanipulator by a circular cross-section one-dimensional nano structure
2 sections are broken into, is denoted as sample A and B respectively；
Step 2, under optical microscopy or scanning electron microscope, sample A and B be overlapped on respectively using micromanipulator hanging micro-
The heat source of device, it is heat sink on, and make sample A, B heat source, it is heat sink between form parallel contact；
Step 3, the sample is tested using heat bridge method, obtains apparent thermal resistance Rtot1, and Rtot1For
Rtot1=Rmh1+Rmc1+Rs1 (1)
Wherein, Rmh1And Rmc1Respectively this test between sample A and heat source, sample B and it is heat sink between contact heat
Resistance, Rs1For heat source, it is heat sink between parallel contact sample intrinsic thermal resistance, Rs1For
Rs1=R1/L×(LCE+LEF/2+LDF)+f×RCA/Ac1 (2)
R1/LFor the intrinsic thermal resistance of sample A and B unit length, LCEThe length of sample A between CE, C are sample A with heat source side
The contact point of edge, E are the starting point of sample A and B parallel contact, LEFThe length of sample parallel contact between EF, F are flat for sample A and B
The terminal of row contact, LDFThe length of sample B between DF, D are contact point of the sample B with heat sink edge, RCABetween sample A, B
The thermal contact resistance of unit area, Ac1In the contact area of EF parallel contact section between sample A, B, it can obtain f's by thermal modeling
Expression formula
Wherein
The width of w contact surface when parallel contact between sample A, B；
Step 4, under optical microscopy or scanning electron microscope, sample A and B are become handing over from parallel contact using micromanipulator
Fork, to guarantee that the contact between sample A and heat source does not change in the process, sample B and it is heat sink between contact do not change
Become, sample A and B cross-contact point G will be between Fig. 1 parallel contact section EF, and to meet in sample testing length sync rapid 2
It is approximately equal, i.e.,
LCG+LDG≈LCE+LEF/2+LDF (4)
Step 5, the sample is tested using heat bridge method, obtains apparent thermal resistance Rtot2, and Rtot2For
Rtot2=Rmh2+Rmc2+Rs2 (5)
Wherein, Rmh2And Rmc2Respectively this test in sample A between heat source, sample B and it is heat sink between contact heat
Resistance, Rs2For heat source it is heat sink between cross-contact sample intrinsic thermal resistance, Rs2For
Rs2=R1/L×(LCG+LDG)+RCA/Ac2 (6)
Wherein, Ac2For the contact area in the sample between sample A, B；
Step 6, since in above-mentioned steps 4, the contact maintained between sample A and heat source does not change, sample B and heat
Contact between heavy does not change, thus has Rmh1=Rmh2, Rmc1=Rmc2, also maintain sample be tested length it is of substantially equal, i.e.,
Formula (4), therefore, by the thermal contact resistance of unit area between formula (1), formula (5) formula available sample A, B:
For circular cross-section one-dimensional nano structure, Ac1Much larger than fAc2, therefore formula (7) formula can be approximated to be
RCA=(Rtot2-Rtot1)×Ac2 (8)
I.e. by the measurement twice in step 3 and step 5, the total heat of parallel contact sample and cross-contact sample is obtained
Resistance, the thermal contact resistance of circular cross-section one-dimensional nano structure unit area is calculated by formula (8).
In order to guarantee in step 4, the contact between sample A and heat source does not change, sample B and it is heat sink between contact
Do not change, Pt can be deposited in the same heat source of sample A, B, heat sink contact position using e-beam induced deposition technology in step 2,
With preferably fixed sample.
It is that measurement is approximately equal in length in step 2 and step 4, difference between the two, i.e. formula (4) as improved
The actual difference of the right and left should be included in RCAIn test error, due to being approximation, so having error, so this difference should
It is included in the error of final result.
The utility model has the advantages that
Compared with prior art, the beneficial effects of the present invention are:
(1) successfully tested rate is high.
After the completion of parallel contact test, it is only necessary to carry out micro- manipulation by a small margin to sample, it is become cross-contact
?；Due to not needing to be moved on a large scale to sample, the loss late of sample is reduced, to improve successfully tested rate；
(2) requirement to sample quality consistency is reduced.
Technical solution disclosed in this invention only requires sample quality with higher one in parallel contact section
Cause property, sample in defect of other positions etc. on test result without influence, improve measurement accuracy.
Detailed description of the invention
Fig. 1 is heat bridge method test philosophy and parallel contact schematic diagram, wherein 1- heat source, the first miniature coils of 2-, 3- first
Hanging arm, 4- substrate, the hanging arm of 5- second, the second miniature coils of 6-, 7- is heat sink；
Fig. 2 is cross-contact schematic diagram.
Specific embodiment
The testing scheme of thermal contact resistance, used measuring technology between circular cross-section one-dimensional nano structure disclosed by the invention
For heat bridge method.The present invention is described in further details with embodiment with reference to the accompanying drawing.
Fig. 1 gives the heat bridge method test hot physical property schematic diagram of one-dimensional nano structure.This method passes through MEMS work using one
The hanging micro element of skill preparation, including hanging heat source 1 and more heat sink 7, to support heat source first hanging arms 3, support is heat sink
More second hanging arms 5 and substrate 4.It is miniature the first miniature coils 2 and second have been made respectively on heat source 1 and heat sink 7
Coil 6, wherein the first miniature coils 2 come heat source and detection heat source temperature as heater and temperature sensor simultaneously, the
Two miniature coils 6 detect heat sink 7 temperature as temperature sensor.Tested sample is overlapped on heat source 1, among heat sink 7.
Test carries out in vacuum constant temperature chamber, therefore the influence of heat convection can be ignored.By using layer 2-3 heat radiation
Radiation effect can be reduced to negligible level by shielding case.Alterating and direct current I is passed through in the first miniature coils of heat source side 2
+iac, wherein I is DC current, for generating the Joule heat of heat source, iacFor detection alternating current.Heat source is detected respectively
Hold the AC voltage drop v on the first miniature coils 2 and heat sink the second miniature coils of 7 end 6ac, it is based on the available line of Ohm's law
The resistance of circle.Based on steady state method heat conduction model, it can be deduced that the apparent thermal resistance of tested sample are as follows:
Wherein, Δ ThWith Δ TsThe respectively temperature rise of heat source 1 and heat sink 7, and the first miniature coils 2 of measurement and the can be passed through
The resistance variations of two miniature coils 6 obtain, QhAnd QLRespectively heated current I is hanging in the first miniature coils of heat source side 2 and one
The Joule heat generated in arm 3.RtotIt include thermal contact resistance between thermal resistance, sample and the heat source of sample itself, sample and heat sink
Thermal contact resistance between 7.
By taking diameter contacts thermo-resistance measurement between the carbon nanotube of 68nm as an example, specific test process includes following main
Step: (1) under an optical microscope, the carbon nanotube that using micromanipulator by length be about 30 μm, diameter is 68nm exists
2 sections are broken into close to middle position, is denoted as sample A and B respectively；
(2) as Fig. 1 signal, under an optical microscope, sample A and B are overlapped on vacantly respectively using micromanipulator
The heat source of micro element, it is heat sink on, and make sample A, B heat source, it is heat sink between form parallel contact.Quilt is measured under scanning electron microscope
Each segment length of sample, result LCE=4.5 μm, LDF=4.8 μm, contact length LEF=2.1 μm.In order to guarantee that sample A, B are same
Heat source, it is heat sink have firm contact, using e-beam induced deposition technology the same heat source of sample A, B, heat sink contact position deposit gold
Belong to Pt, in addition, arrow pointed location EF is the parallel contact formed between sample A, B in Fig. 1；
(3) sample is tested using heat bridge method, obtains apparent thermal resistance Rtot1=2.13 × 107K/W；
(4) as Fig. 2 signal, under an optical microscope, sample A and B are become from parallel contact using micromanipulator
Cross-contact.Since induction and deposition in step 2 Pt metal, the contact between sample A and heat source do not change, sample
B and it is heat sink between contact do not change.It is measured under scanning electron microscope, LCG+LDG=10.48 μm, same to LCE+LEF/2+LDFDifference
0.13 μm, meet the requirement of formula 4 in technical solution, the angle of the crossing is 88.6 °.Sample A and B can be calculated by contact mechanics and be connect
Contacting surface product is Ac2=51.68nm2。
(5) sample is tested using heat bridge method, obtains apparent thermal resistance Rtot2=3.60 × 107K/W；
(6) R that will be obtainedtot1、Rtot2And Ac2Bring formula 8 in technical solution, available R intoCA=7.6 × 10-10m2K/
W。
In order to be reduced to error brought by formula (8) from formula (7) in estimation technique scheme, to institute's carbon determination nanotube
Intrinsic thermal conductivity coefficient is measured, and is obtained its intrinsic thermal conductivity coefficient k=199.8W/m-K, is brought into formula (3) and obtain f=
5.76.It is finally 7% by the error that formula (7), formula (8) can be simplified introducing.In view of contacting heat between nanostructure
The difficulty of test is hindered, which can receive completely.
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.Industry technology
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (3)
1. contacting thermo-resistance measurement method between a kind of circular cross-section one-dimensional nano structure, which comprises the following steps:
Step 1, under optical microscopy or scanning electron microscope, a piece circular cross-section one-dimensional nano structure is broken into using micromanipulator
2 sections, it is denoted as sample A and B respectively；
Step 2, under optical microscopy or scanning electron microscope, sample A and B are overlapped on hanging micro element respectively using micromanipulator
Heat source, it is heat sink on, and make sample A, B heat source, it is heat sink between form parallel contact；
Step 3, the sample is tested using heat bridge method, obtains apparent thermal resistance Rtot1, and Rtot1For
Rtot1=Rmh1+Rmc1+Rs1 (1)
Wherein, Rmh1And Rmc1Respectively this test between sample A and heat source, sample B and it is heat sink between thermal contact resistance, Rs1
For heat source, it is heat sink between parallel contact sample intrinsic thermal resistance, Rs1For
Rs1=R1/L×(LCE+LEF/2+LDF)+f×RCA/Ac1 (2)
R1/LFor the intrinsic thermal resistance of sample A and B unit length, LCEThe length of sample A between CE, C are sample A with heat source edge
Contact point, E are the starting point of sample A and B parallel contact, LEFThe length of sample parallel contact between EF, F, which is that sample A is parallel with B, to be connect
The terminal of touching, LDFThe length of sample B between DF, D are contact point of the sample B with heat sink edge, RCAThe unit between sample A, B
The thermal contact resistance of area, Ac1In the contact area of EF parallel contact section between sample A, B, the expression of f can be obtained by thermal modeling
Formula
Wherein
Wherein, the width of w contact surface when parallel contact between sample A, B；Step 4, under optical microscopy or scanning electron microscope,
Sample A and B is become into cross-contact from parallel contact using micromanipulator, to be guaranteed between sample A and heat source in the process
Contact do not change, sample B and it is heat sink between contact do not change, sample A and B cross-contact point G will be located at parallel connect
Touch section EF between, and to meet it is approximately equal in sample testing length sync rapid 2, i.e.,
LCG+LDG≈LCE+LEF/2+LDF(4)；
Step 5, the sample is tested using heat bridge method, obtains apparent thermal resistance Rtot2, and Rtot2For
Rtot2=Rmh2+Rmc2+Rs2 (5)
Wherein, Rmh2And Rmc2Respectively this test in sample A between heat source, sample B and it is heat sink between thermal contact resistance, Rs2
For heat source it is heat sink between cross-contact sample intrinsic thermal resistance, Rs2For
Rs2=R1/L×(LCG+LDG)+RCA/Ac2 (6)
Wherein, Ac2For the contact area in the sample between sample A, B；
Step 6, since in above-mentioned steps 4, the contact maintained between sample A and heat source does not change, sample B and it is heat sink it
Between contact do not change, thus have Rmh1=Rmh2, Rmc1=Rmc2, also maintain sample of substantially equal, the i.e. formula that is tested length
(4), therefore, by the thermal contact resistance of unit area between formula (1), formula (5) formula available sample A, B
For circular cross-section one-dimensional nano structure, Ac1Much larger than fAc2, therefore formula (7) can be approximated to be
RCA=(Rtot2-Rtot1)×Ac2 (8)
I.e. by the measurement twice in step 3 and step 5, the entire thermal resistance of parallel contact sample and cross-contact sample is obtained, by
The thermal contact resistance of circular cross-section one-dimensional nano structure unit area is calculated in formula (8).
2. contacting thermo-resistance measurement method between circular cross-section one-dimensional nano structure according to claim 1, which is characterized in that be
Guarantee that the contact between sample A and heat source does not change in step 4, sample B and it is heat sink between contact do not change,
Pt can be deposited in the same heat source of sample A, B, heat sink contact position using e-beam induced deposition technology in step 2, with preferably
Fixed sample.
3. contacting thermo-resistance measurement method between circular cross-section one-dimensional nano structure according to claim 1, which is characterized in that step
Rapid 2 and step 4 in measure and be approximately equal in length, the actual difference of difference between the two, i.e. formula (4) the right and left is accrued
Enter RCAIn test error.
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