CN102944573B - Method for simultaneously measuring laser absorptivity and thermal conductivity of single micro-nano wire rod - Google Patents
Method for simultaneously measuring laser absorptivity and thermal conductivity of single micro-nano wire rod Download PDFInfo
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- CN102944573B CN102944573B CN201210436540.5A CN201210436540A CN102944573B CN 102944573 B CN102944573 B CN 102944573B CN 201210436540 A CN201210436540 A CN 201210436540A CN 102944573 B CN102944573 B CN 102944573B
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Abstract
The invention provides a method for simultaneously measuring the laser absorptivity and thermal conductivity of a single micro-nano wire rod, belonging to the technical field of characterization of property of nano-materials. The method disclosed herein is characterized by using contactless laser Raman measurement technology to position and carry out temperature calibration on the single micro-nano wire rod; then respectively using laser heating and electric heating methods in a vacuum environment to reach equal core temperature of samples to be measured and measure respective heating power; substituting the geometry size, core temperature and heating power of the micro-nano wire rod in a theoretical formula to simultaneously calculate the laser absorptivity and thermal conductivity of the samples to be measured. According to the invention, the method has the advantages of wide range of application, simple principle and convenient operation, is suitable for various micro-nano wire rods which have characteristic Raman spectrum and have different materials, diameters and lengths, fills the technical gap of measuring the laser absorptivity of the single micro-nano wire rod, and provides valuable basic physical property data for practical engineering application.
Description
Technical field
The present invention relates to the thermal characteristic technical field of measurement and test of micro-nano wire rod, be specifically related to a kind of method of simultaneously measuring single micro-nano wire laser absorptivity and thermal conductivity.
Background technology
Micro-nano wire rod comprises carbon fiber, silicon/Ge nanoline, carbon nano-tube etc., in heat dissipation from microelectronic devices, the exploitation of Novel hot electric material, Aerospace Engineering field, has engineering background widely.Wherein carbon nano-tube is described as the most promising nano material of 21 century especially, professor Iijima in Japanese NEC Corporation's fundamental research laboratory in 1991 finds carbon nano-tube first, it is the one-dimensional material being curled into by individual layer (or which floor) carbon atom, has high mechanical strength, thermal conductivity and excellent field emission characteristic.The diameter of carbon nano-tube is generally 2 ~ 10nm, and length is at micron to centimetre magnitude, and it is more difficult that little geometric scale like this makes the hot physical property sign of carbon nano-tube compare other micro-nano wire rods.How the local temperature of Measurement accuracy single-root carbon nano-tube and the heat that absorbs become the crucial difficult problem in thermal property experiment field, and patent retrieval is found domestic at present also not about the effective ways report of single-root carbon nano-tube thermophysical property measurement.
Conventional resistance thermometer, thermopair size, in millimeter magnitude, cannot directly be measured the temperature of micro-nano wire rod; Contact temperature-measuring method based on scan-probe (Scanning Thermal Microscopy) can be measured the local temperature (M.E.Pumarol of nano material, M.C.Rosamond, et al., Nano Lett., 2012,12:2906-2911), but introduce nano-probe, can change the local temperature field of measured material, thereby bring certain experimental error.Laser raman measuring technique is a kind of non-contact type temp measuring method of development in recent years; have the advantages that principle is simple, reproducible, temperature measurement accuracy is high; be particularly suitable for the measurement (I.K.Hsu of micro-nano wire rod local temperature; M.T.Pettes; etal., J.Appl.Phys., 2010; 108,084307; Y.Y.Zhang, L.M.Xie, et al., J.Phys.Chem.C, 2007,111:14031-14034).
Use the laser absorption rate that the thermal conductivity of the micro-nano wire rod of laser raman commercial measurement must first known micro Nano material, according to existing literature search, find to only have the seminar of American South University of California report the laser absorption rate (I.K.Hsu of the method measurement carbon nano-tube bundle (diameter 7 ~ 10nm) that utilizes microelectrode resistance temperature measurement, M.T.Pettes, et al., Nano Lett., 2009,9 (2): 590-594.), in addition yet there are no the effective ways of measuring micro-nano wire laser absorptivity.Yet the method utilizes microelectrode can only measure the end points temperature of micro-nano wire rod as temperature sensor (characteristic length ~ 10 μ m), can not obtain along the Temperature Distribution of micro-nano length of wires direction; Between microelectrode and testing sample, can there is contact resistance and thermal contact resistance unavoidably in addition, increase thermometric uncertainty.
Summary of the invention
For solving above-mentioned problems of the prior art, the object of the present invention is to provide a kind of method of simultaneously measuring micro-nano wire laser absorptivity and thermal conductivity.The method is applicable to the micro-nano wire rod of various different materials, diameter, length, as long as testing sample has typical feature Raman spectrum.There is feature applied widely, that principle is simple, measuring accuracy is high, reproducible.
For achieving the above object, the technical solution adopted in the present invention is:
A method of simultaneously measuring single micro-nano wire laser absorptivity and thermal conductivity, comprises the steps:
Step 1: the suprabasil unsettled micro-nano wire rod sample of preparation silica/silicon, its two ends deposit metal electrodes is for energising;
Step 2: utilize respectively scanning electron microscope and atomic force microscope to measure length l and the diameter D of micro-nano wire rod sample;
Step 3: utilize the method for laser raman location to determine the position of micro-nano wire rod sample under optical microscope;
Step 4: utilize cold and hot temperature that changes testing sample substrate, the feature raman frequency variation with temperature of micro-nano wire rod sample and being offset, measures the temperature variant skew slope of feature raman frequency;
Step 5: utilize two kinds of methods of LASER HEATING and electrical heating that micro-nano wire rod sample central point temperature is raise, the side-play amount of measuring micro-nano wire rod sample characteristic raman frequency obtains central point temperature rise Δ T
m, under the equal condition of central point temperature, measure laser power S
lwith electric power S
e;
Step 6: by the length l of micro-nano wire rod sample and diameter D, central point temperature rise Δ T
m, the laser power S under identical temperature condition
lwith electric power S
esubstitution formula 1) and formula 2), calculate to obtain laser absorption rate α and the thermal conductivity λ of micro-nano wire rod sample.
The preparation method of the micro-nano wire rod sample described in step 1 is specially: on the square silicon wafer of 1cm * 1cm * 500 μ m, utilize the method for chemical etching to obtain rectangle cutting, its width can be selected according to user's request, generally at 2 μ m between 200 μ m, conduit etching depth is at tens microns; Silicon base is carried out to surface oxidation and form silicon dioxide electric insulation layer; On conduit both sides, utilize metal electrode that the method for physical vapour deposition (PVD) prepares 10 μ m * 10 μ m for energising, the metal lead wire of 2 μ m live widths is for measuring voltage, prepares the central channel that needs protection in the process of metal electrode and avoids being covered by metallic particles; In silica/silicon substrate, prepare micro-nano wire rod and make it unsettled being overlapped between metal electrode, guarantee that testing sample can not contact conduit bottom.
The method of utilizing laser raman location described in step 3 determines that the concrete grammar of micro-nano wire rod position is: utilize Raman spectrometer at the feature Raman signal of the micro-nano wire rod sample of objective plane region interscan, the position that occurs feature Raman signal is exactly the position of micro-nano wire rod sample, and the Raman signal of all the other positions is zero; Near measured raman frequency is chosen in to the characteristic frequency that signal is the strongest, (carbon nano-tube is 1580cm
-1), to existing the region of sample to carry out flat scanning, the moving step length of automatically controlled platform is chosen as 1 μ m.
The concrete grammar of measuring the temperature variant skew slope of feature raman frequency described in step 4 is: utilize cold and hot base reservoir temperature that changes micro-nano wire rod sample, reach to set and wait for 30 minutes after temperature and keep temperature stabilization, measure the feature raman frequency of micro-nano wire rod sample, complete after all design temperatures are measured and obtain the temperature variant skew slope of feature raman frequency, by measuring micro-nano wire rod sample characteristic raman frequency side-play amount and then obtaining its local temperature, in experiment, need to guarantee that each LASER HEATING power of measuring is identical with the time shutter.
The described base reservoir temperature of cold and hot the micro-nano wire rod sample of change of utilizing be take 30K as interval.
The concrete grammar that utilizes LASER HEATING described in step 5 is: under vacuum condition, Laser Focusing is heated in the center of micro-nano wire rod sample, measure the side-play amount of the rear feature raman frequency of heating, and then utilize the temperature variant slope of characteristic frequency to obtain central point temperature rise Δ T
m, the laser power of measuring now focusing objective len outlet is S
l, more by force but can not burn sample, the concrete numerical value of power is relevant with kind, the physical dimension of testing sample for the LASER HEATING power of selection.
To diameter, be 3.2nm, length is that the carbon nano-tube heating power of 24.8 μ m is 274.8 μ W.
The electrically heated concrete grammar that utilizes described in step 5 is: under vacuum condition, micro-nano wire rod sample is carried out to direct current energising heating, measure the side-play amount of feature raman frequency and utilize the temperature variant slope of characteristic frequency to obtain central point temperature rise, in experiment, increase electric power gradually until the temperature of micro-nano wire rod sample central point equates with the temperature of described LASER HEATING central point, record electric power S now
e.
Formula 1) and 2) calculating derivation as follows:
Under vacuum condition, direct current energising adds thermogenetic testing sample Temperature Distribution and is:
Wherein λ is the thermal conductivity of testing sample, T
0be environment temperature, the temperature rise of central point is:
The Temperature Distribution that testing sample central point is subject to LASER HEATING generation is:
The temperature rise of respective center point is:
Make Δ T
m2=Δ T
m1just can obtain formula 1) in laser absorption rate α and formula 2) in the expression formula of thermal conductivity λ.
Method provided by the invention has broken through a gordian technique difficult problem for single micro-nano wire temperature and heat Experimental Characterization, fill up the technological gap of measuring single-root carbon nano-tube laser absorption rate, for furtheing investigate nano material energy transport character and optical absorption characteristic, provide effective experimental technique.The method has following technical characterstic:
(1) realize the Raman location of single micro Nano material (as carbon nano-tube).Be not subject to the restriction of sample size, can under optical microscope, accurately determine the locus of single wall, multi-walled carbon nano-tubes.
(2) realize the non-contact type thermometric of single micro-nano wire rod.Utilize the local temperature that testing sample feature raman frequency can Measurement accuracy sample to the dependence of temperature, in measuring process, do not need contact measured sample, avoided the impact in thermoprobe local area temperature field in conventional method, improved temperature measurement accuracy.
(3) applied widely, principle is simple, reliability is high.The method is applicable to have arbitrarily the micro-nano wire rod of feature Raman spectrum, as carbon fiber, silicon/Ge nanoline, carbon nano-tube etc., physical dimension, electrical heating power, laser power and the central temperature of only measuring sample just can obtain laser absorption rate and the thermal conductivity of testing sample simultaneously, contact resistance and the thermal contact resistance of having avoided microelectrode temp measuring method to introduce, improved measuring accuracy.
Accompanying drawing explanation
Fig. 1 is the carbon nano-tube stereoscan photograph of preparation.
Fig. 2 is the Raman verification film of carbon nano-tube.
Fig. 3 is the skew of carbon nano-tube G peak frequency under condition of different temperatures.
Fig. 4 is the schematic diagram of LASER HEATING carbon nano-tube.
Fig. 5 is that carbon nano-tube G peak frequency is with the skew of LASER HEATING power.
Fig. 6 is the schematic diagram of electrical heating carbon nano-tube.
Fig. 7 is that carbon nano-tube G peak frequency is with the skew of electrical heating power.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Utilize method involved in the present invention to measure laser absorption rate and the thermal conductivity of single-root carbon nano-tube, specific embodiment is as follows:
(1) in silica/silicon substrate, utilize the method for chemical vapor deposition to prepare many carbon nano-tube, the center section of carbon nano-tube sample unsettled on the cutting of substrate for Raman Measurement.As shown in Figure 1, wherein circles mark is single-root carbon nano-tube measured in embodiment to the electromicroscopic photograph of carbon nano-tube sample, and the carbon nano-tube of all the other hamper measurements can focus on and blow with light laser.
(2) because the diameter of carbon nano-tube in the magnitude of several nanometers, optical microscope cannot observe directly carbon nano-tube sample.The three grades of grating Raman spectrometers of T64000 type that use HORIBA company in our experiment, at the feature Raman signal of objective plane region interscan carbon nano-tube, the position that occurs signal is exactly the position of carbon nano-tube.Raman localization method is not subject to the restriction of sample size size, is applicable to the carbon nano-tube of any caliber.Fig. 2 is shown as the optical photograph behind single-root carbon nano-tube Raman location.
(3) utilize cold and hot of the low temperature of LINKAM company, in the temperature range of-90 ℃ to 90 ℃, the Raman spectrum of carbon nano-tube sample is measured to (adjacent temperature interval 30.0K), sample G peak frequency variation with temperature relation as shown in Figure 3.The every rising 30.0K of measurement result displays temperature, wave number (cm of G peak frequency shift (FS)
-1).Known G peak frequency just can be determined by measuring frequency offset that different LASER HEATING power or electrical heating power cause the local temperature of carbon nano-tube sample after with the skew slope of temperature.T64000 spectrometer Jiao who uses in experiment reaches 1.8m, and spectral resolution is 0.15cm
-1, be one of spectrometer that resolution is the highest in the world at present, the resolution of corresponding measurement temperature is 4.5K.
(4) utilize scanning electron microscope and optical microscope photograph can determine that the length of carbon nano-tube sample to be measured is 24.8 μ m, utilizing atomic force microscope to measure carbon nano-tube diameter is 3.2nm.
(5) use the LASER HEATING carbon nano-tube of Stabilite 2018 type argons-krypton ion laser generation 514nm wavelength of SPECTRA PHYSICS company, as shown in Figure 4.In experiment by Laser Focusing the center in carbon nano-tube, change the temperature rise of LASER HEATING power measurement carbon nano-tube.Fig. 5 is shown as the G peak frequency that different LASER HEATING power is corresponding, and along with LASER HEATING increased power, carbon nano-tube central point temperature raises, and G peak frequency moves to lower wave number direction gradually.When LASER HEATING power is 274.8 μ W, central point temperature rise is 142K.
(6) the R6243 type precision DC stabilizer that uses ADVANTEST company is to the heating of switching on of carbon nano-tube sample, as shown in Figure 6.Utilize the voltage U that 2002 type eight and half high-accuracy voltage tables of KEITHLEY company can Measurement accuracy carbon nano-tube two ends, YOKOGAWA company 100 Ω measuring resistances are connected with carbon nano-tube, the voltage at measurement standard resistance two ends obtain electric current I divided by 100 Ω resistance more simultaneously.The electrical heating power S of carbon nano-tube
e=UI.In experiment, use a branch of temperature of weak laser measurement carbon nano-tube central point, Fig. 7 is shown as the G peak frequency shift (FS) that different electrical heating powers are corresponding.When electrical heating power is 0.96 μ W, the temperature rise of carbon nano-tube central point is 142K, and LASER HEATING temperature rise equates.
(7) formula 1 of analyzing according to measurement result in summary of the invention) and 2) laser absorption rate that can calculate carbon nano-tube is 0.17%, thermal conductivity is 2536Wm
-1k
-1.
Claims (6)
1. a method of simultaneously measuring single micro-nano wire laser absorptivity and thermal conductivity, is characterized in that: comprise the steps:
Step 1: the suprabasil unsettled micro-nano wire rod sample of preparation silica/silicon, its two ends deposit metal electrodes is for energising;
Step 2: utilize respectively scanning electron microscope and atomic force microscope to measure length l and the diameter D of micro-nano wire rod sample;
Step 3: utilize the method for laser raman location to determine the position of micro-nano wire rod sample under optical microscope;
Step 4: utilize cold and hot temperature that changes testing sample substrate, the feature raman frequency variation with temperature of micro-nano wire rod sample and being offset, measures the temperature variant skew slope of feature raman frequency;
Step 5: utilize two kinds of methods of LASER HEATING and electrical heating that micro-nano wire rod sample central point temperature is raise, the side-play amount of measuring micro-nano wire rod sample characteristic raman frequency obtains central point temperature rise Δ T
m, under the equal condition of central point temperature, measure laser power S
lwith electric power S
e;
Step 6: by the length l of micro-nano wire rod sample and diameter D, central point temperature rise Δ T
m, the laser power S under identical temperature condition
lwith electric power S
esubstitution formula 1) and formula 2),
Calculate the laser absorption rate α and the thermal conductivity λ that obtain micro-nano wire rod sample.
2. a kind of method of simultaneously measuring single micro-nano wire laser absorptivity and thermal conductivity according to claim 1, it is characterized in that: the method for utilizing laser raman location described in step 3 determines that the concrete grammar of the position of micro-nano wire rod sample is: utilize Raman spectrometer at the feature Raman signal of the micro-nano wire rod sample of objective plane region interscan, the position that occurs feature Raman signal is exactly the position of micro-nano wire rod sample, and the Raman signal of all the other positions is zero; Measured raman frequency is chosen near the characteristic frequency that signal is the strongest, and to existing the region of sample to carry out flat scanning, the moving step length of automatically controlled platform is chosen as 1 μ m.
3. a kind of method of simultaneously measuring single micro-nano wire laser absorptivity and thermal conductivity according to claim 1, it is characterized in that: the concrete grammar of measuring the temperature variant skew slope of feature raman frequency described in step 4 is: utilize cold and hot base reservoir temperature that changes micro-nano wire rod sample, reach to set and wait for 30 minutes after temperature and keep temperature stabilization, measure the feature raman frequency of micro-nano wire rod sample, complete after all design temperatures are measured and obtain the temperature variant skew slope of feature raman frequency, by measuring micro-nano wire rod sample characteristic raman frequency side-play amount and then obtaining its local temperature, in experiment, need to guarantee that each LASER HEATING power of measuring is identical with the time shutter.
4. a kind of method of simultaneously measuring single micro-nano wire laser absorptivity and thermal conductivity according to claim 3, is characterized in that: the described base reservoir temperature of cold and hot the micro-nano wire rod sample of change of utilizing be take 30K as interval.
5. by a kind of method of measuring single micro-nano wire laser absorptivity and thermal conductivity claimed in claim 3 simultaneously, it is characterized in that: the concrete grammar that utilizes LASER HEATING described in step 5 is: under vacuum condition, Laser Focusing is heated in the center of micro-nano wire rod sample, measure the side-play amount of the rear feature raman frequency of heating, and then utilize the temperature variant slope of feature raman frequency to obtain central point temperature rise Δ T
m, the laser power of measuring now focusing objective len outlet is S
l, more by force but can not burn sample, the concrete numerical value of power is relevant with kind, the physical dimension of sample for the LASER HEATING power of selection.
6. by a kind of method of measuring single micro-nano wire laser absorptivity and thermal conductivity claimed in claim 5 simultaneously, it is characterized in that: the electrically heated concrete grammar that utilizes described in step 5 is: under vacuum condition, micro-nano wire rod sample is carried out to direct current energising heating, measure the side-play amount of feature raman frequency and utilize the temperature variant slope of feature raman frequency to obtain central point temperature rise, in experiment, increase electric power gradually until the temperature of micro-nano wire rod sample central point equates with the temperature of described LASER HEATING central point, record electric power S now
e.
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