CN101354388B - Method and system for measuring quasi one-dimensional nano-material Seebeck coefficient - Google Patents
Method and system for measuring quasi one-dimensional nano-material Seebeck coefficient Download PDFInfo
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Abstract
The invention discloses a method and a system that are used for measuring the Seebeck coefficient of a quasi-one-dimensional nano material; two line transition electrodes with micrometer-scaled cross sections are respectively contacted with two centimeter-scaled block metal electrodes, a nano probe system is utilized for leading a single rod of the quasi-one-dimensional nano material to be detected to be connected with the two transition electrodes, temperature difference between the two block metal electrodes is altered, and the temperature difference and corresponding potential difference between the two electrodes are simultaneously measured, thus obtaining the Seebeck coefficient of the quasi-one-dimensional nano material. The corresponding testing system comprises three parts of an experimental platform, a temperature altering device and a data collecting and processing device. The method and the system solve the problem of the contact transition between the centimeter-scaled electrodes and the nano sample to be detected through the micrometer-scaled transition electrodes, utilize the nano probe system for installing the nano material, and lead the nano material not to be randomly dispersed at two sides of the electrodes, thus improving experimental success rate, controllability and reliability; and the provided measuring system has the advantages of simple structure, low cost and easy popularization and the like.
Description
Technical field
The present invention relates to the field of measuring technique of thermoelectric material Seebeck coefficient, particularly measure for example method and system of the Seebeck coefficient of the quasi-one-dimensional nanometer material of nanotube, nano wire and nano belt etc.
Background technology
Thermoelectric material has the advantages that standard machinery freezes or the thermo-electric generation means are difficult to match in excellence or beauty such as size is little, light weight, nothing machinery part, noiseless.The sign of thermoelectric material is dimensionless figure of merit ZT=S
2σ/κ, wherein, S is Seebeck coefficient (a Seebeck coefficient), and σ is a conductivity, and κ is a thermal conductivity.It intuitively meaning be the ratio that refrigeration absorbs energy and power consumption, but the ZT coefficient of common block materials is less than 1, and the ZT coefficient of people's such as recent B.Poudeld block materials can reach 1.4-1.6[B.Poudel, Q.Hao, Y.Ma, Y.Lan, A.Minnich, B.Yu, X.Yan, D.Wang, A.Muto, D.Vashaee, X.Chen, J.Liu, M.S.Dresselhaus, G.Chen, and Z.F.Ren, " High-ThermoelectricPerformance of Nanostructured Bismuth Antimony Telluride Bulk Alloys ", Science320 (5876): 634-638,2008.].And the ZT coefficient of thermoelectric material arrival 3 just can match in excellence or beauty with present refrigerant compression engine efficiency.Theoretical Calculation shows that the ZT coefficient of low-dimensional materials can be compared the big 3-10 of block materials doubly.The R.Venkatasubramanian of U.S. RTI research institute etc. has reported that the thickness cycle is that the ZT coefficient of super crystal lattice material when 300K of 5nm can arrive 2.4[R.Venkatasubramanian.et al., " Thin-film thermoelectric devices with highroom-temperature figures of merit ", Nature413 (2001) 597.], comparing present block materials has had qualitative leap.
The ZT coefficient of theoretical prediction quasi-one-dimensional nanometer material can arrive more than 6, but because the singularity of quasi-one-dimensional nanometer material, difficult aspect the measurement of thermoelectric parameter, common report is a thermoelectricity capability of measuring nano-wire array, the thermoelectricity capability of the nanotube bundle (bundle) that perhaps a large amount of nanotubes are formed.But the test result of these methods is coarse, does not have repeatability, can not obtain the character of single nano-wire.In the single nano-wire thermoelectricity capability experiment report few in number, what mainly continue to use is the example platform of ten microns sizes of thin film photolithography technology preparation, utilize multilayer technique on platform, to plate out resistive platinum wire, as thermometric and temperature control dual purpose, sample then is [the P.Kim that is sprinkled upon at random on the sample stage, L.Shi, A.Majumdar, and P.L.McEuen. ＂ Thermal Transport Measurements of Individual Multiwalled Nanotubes ＂ .Phys.Rev.Lett., 87 (21): 215502, Oct2001.], this method is promoted ability owing to the application that platform prepares complex technology causes the high of cost.And this method temperature measurement accuracy is limited.Add the method for spilling at random of sample and cause success ratio low and to the restriction of measuring samples, problem is mainly reflected in two aspects: first method of spilling sample at random is difficult to obtain single sample wire, and the experiment consumes resources is many; The second, the use of multilayer film platform technology and MEMS technology makes cost improve greatly, and it is unfavorable that platform is promoted.
The Seebeck coefficient of measuring single quasi-one-dimensional nanometer material can provide measurement index and feedback information for the nano material of developing high thermoelectricity capability, for Theoretical Calculation provides experimental data, can also provide reference for the development of thermoelectric nano-device.As mentioned above, also there are not a kind of simple effective method and platform to realize the measurement of single quasi one-dimensional nano-material Seebeck coefficient at present.
Summary of the invention
The object of the present invention is to provide the measuring method and the system of low, the easy popularization of a kind of cost, easy to operate single quasi one-dimensional nano-material Seebeck coefficient.
Technical scheme of the present invention is as follows:
A kind of method of measuring quasi one-dimensional nano-material Seebeck coefficient may further comprise the steps:
(1) making two cross-sectional dimension is that micron-sized wire transition electrode is centimetre-sized with two sizes respectively the reguline metal electrode contacts;
(2) utilize the nano-probe system to make single quasi-one-dimensional nanometer material to be measured connect two transition electrodes;
(3) temperature difference between two reguline metal electrodes of change is measured the temperature difference of this two electrode and the electric potential difference of correspondence simultaneously, calculates the Seebeck coefficient of quasi-one-dimensional nanometer material by the relation between electric potential difference and the temperature difference.
In the said method, centimetre-sized reguline metal electrode need be selected all comparatively good and bigger material of thermal capacitance of electric conductivity and thermal conductivity for use, for example listed three kinds of metal red coppers, gold, silver all are good electrode materials in the table 1, but consideration for cost control, under the little situation of parameter difference, preferred red copper also can be selected metal materials such as stainless steel, brass, aluminium for use as the material of electrode.
Several outstanding electricity of table 1. are led, the metal of thermal conductance and specific heat
| Metal species | Conductivity/Sm -1 | Thermal conductivity/Wm -1·K -1 | Specific heat capacity/Jmol -1·K -1 |
| Red copper | 59.6×10 6 | 401 | 24.47 |
| Gold | 45.2×10 6 | 318 | 25.42 |
| Silver | 63.01×10 6 | 429 | 24.9 |
Material as for transition electrode, not only good heat-conductivity conducting to be arranged, also need its chemical property stable, be difficult for oxidized, and three kinds of materials have appearred because the introducing of transition electrode makes in the sample measurement loop, so transition electrode is preferably selected various aspects of performance (especially Seebeck coefficient) and the much the same material of centimetre-sized metal electrode for use, first-selection is a gold, also can be platinum.Transition electrode be shaped as wire, the square section dimension is preferably at 10 μ m-50 μ m, the general requirement of minimum spacing between two transition electrodes is lower than 100 μ m, so that the installation of testing sample (quasi-one-dimensional nanometer material), generally about 50 μ m.
The nano-probe system that above-mentioned steps (2) is used can be mounted in the nano-probe system in the scanning electron microscope (SEM), also can be that other can be for the system of nano collimation and manipulation, to handle quasi-one-dimensional nanometer material to be measured.
In the above-mentioned steps (3), the method that changes temperature difference between two block type electrodes normally keeps the temperature-resistant of an electrode, and changes the temperature of another electrode.Heating electrode can utilize infrared heating device or DC heating device, and refrigeration then can be utilized liquid nitrogen contact refrigeration (promptly by hot good conductor connection electrode and liquid nitrogen).The mensuration of two electrode temperature differences can realize by implant temperature sensor near the place of transition electrode in the electrode of centimetre-sized reguline metal.
The present invention also provides a measuring system that realizes said method, comprises experiment porch, changing device and data acquisition and treating apparatus three parts, wherein:
Experiment porch comprises that again the reguline metal electrode of two centimetre-sized, two cross-sectional dimension are a micron-sized wire transition electrode and a base, two reguline metal electrodes are installed on the base by heat insulating mattress, two transition electrodes closely contact with two reguline metal electrodes respectively, the minimum spacing of two transition electrodes is lower than 100 μ m, is used to install quasi-one-dimensional nanometer material to be measured;
Changing device is the device that the reguline metal electrode is heated and/or freezes;
Data acquisition and treating apparatus comprise two temperature sensors, voltage tester and a computing unit, the place of the implanted centimetre-sized of temperature sensor reguline metal electrode interior, next-door neighbour's transition electrode, and its signal wire is connected to computing unit; Voltage tester both end voltage lead-in wire connects two reguline metal electrodes respectively, and its electric potential difference that records is passed to computing unit; Computing unit receives and treatment temperature and voltage data, obtains the Seebeck coefficient of quasi-one-dimensional nanometer material.
The better also bigger material of thermal capacitance of the preferred electric conductivity of centimetre-sized reguline metal electrode of above-mentioned experiment porch and thermal conductivity is made, for example red copper, gold, silver, stainless steel, brass, aluminium etc.In order to reduce by two energy conversion that heat radiation and convection current brought between the electrode, the opposite face of two reguline metal electrodes can be made intilted from top to bottom ramped shaped.
The base of above-mentioned experiment porch requires to select thermal conductivity less (being generally less than 2W/mK), non electrically conductive material for use, plays the effect of support, can select glass for use, also can select the high polymerization electrically non-conductive material of Te Fulong or other hard for use.For the heat conduction between impeded electrode and the base, electrode links to each other with base by heat insulating mattress, and heat insulating mattress can be selected the hollow cap object of plastic material for use, and available multi-purpose adhesive is fixedly connected with the three.
In the above-mentioned experiment porch, transition electrode is being born the task of being connected transition by the centimetre-sized electrode between the nanoscale testing sample, its introducing need be avoided causing loose contact problem between testing sample line and the electrode because of oxidation, so need select good heat-conductivity conducting, chemical property for use stablizes, is difficult for oxidized, and various aspects of performance (especially Seebeck coefficient) and the much the same material of centimetre-sized metal electrode, first-selection is gold or platinum.Transition electrode be shaped as wire, the square section dimension is preferably at 10 μ m-50 μ m, about the preferred 50 μ m of minimum spacing between two transition electrodes.Can transition electrode be pressed on the surface of reguline metal electrode by compressing tablet.
Above-mentioned changing device is used for changing temperature difference between two reguline metal electrodes, generally keeps the temperature-resistant of an electrode, and the temperature variation of another electrode.Changing device is divided into heating and two kinds of refrigerating plants.Heating arrangement can be infrared heating device or DC heating device, for example by an infrared heater and the device that condenser is formed, the optional powerful infrared waves radiation bulb of infrared heater (super bath type), condenser is the cone-shaped body of an Aluminium Foil Package, the big muzzle of cone-shaped body is on infrared heater, an osculum is opened in the tip position, aims at a reguline metal electrode, can accomplish to make the purpose of its intensification.Refrigeration then can be utilized liquid nitrogen contact refrigeration, and it consists of a heat-preserving container and a copper litz wire, and it is interior and the other end contacts with a reguline metal electrode that dress liquid nitrogen in the heat-preserving container, braided wire one end plug advance heat-preserving container, can reach the purpose that makes it to lower the temperature.
The installation of the temperature sensor in above-mentioned data acquisition and the treating apparatus can be to cut a mouth at the reguline metal electrode near the position of transition electrode, form a cavity, implant temperature sensor then, fix, and the signal wire of temperature sensor is connected to computing unit with multi-purpose adhesive.The selection of temperature sensor can be adopted T or K type thermocouple or Pt100 or 1000 thermal resistances with different between measurement zone and different in the high-temperature region, can adopt Pt100 or 1000 thermal resistances or SiD sensor at low-temperature space.
Compared with prior art, beneficial technical effects of the present invention is:
1, can provide the concrete Seebeck coefficient of single accurate 1-dimention nano sample, thereby obtain the true attribute of sample, rather than to the statistics effect of a large amount of samples, repeatable high;
2, compare existing single accurate 1-dimention nano sample measurement method, with low cost, make simply, be easy to promote;
3, utilize the nano-probe system that nano material is installed, rather than be sprinkling upon the electrode both sides at random, improved success ratio, controllability and the reliability of experiment.
Description of drawings
Fig. 1 is the structural representation of the experiment porch of embodiment of the invention design.
Fig. 2 is testing sample is installed by the nano-probe system under SEM a photo.
Fig. 3 is the Seebeck effect synoptic diagram that the embodiment of the invention is measured the loop.
Fig. 4 is the temperature variant situation map of Seebeck coefficient that the embodiment of the invention records.
Among the figure:
1---centimetre-sized reguline metal electrode 2---transition electrode 3---quasi-one-dimensional nanometer material to be measured
4---compressing tablet 5---temperature sensor 6---bases
7---heat insulating mattress 8---nano-probe
Embodiment
Below in conjunction with accompanying drawing, further describe the present invention by embodiment, but the scope that does not limit the present invention in any way.
As shown in Figure 1, the centimetre-sized reguline metal electrode 1 of used experiment porch links to each other with base 6 by heat insulating mattress 7, two compressing tablets 4 that have same material to make are arranged on each reguline metal electrode 1, four altogether, one group of compressing tablet is used for pressing transition electrode 2 wherein, the one group of compressing tablet in outside is pushed down the voltage measurement line, and quasi-one-dimensional nanometer material 3 to be measured just places on two transition electrodes 2.
The size of reguline metal electrode 1 is about 10mm * 10mm * 40mm, and its material requirements thermal conductivity is greater than 100W/mK, and conductivity is greater than 15000000S/m, and preferred material is a red copper.In order to reduce the thermal convection between two electrodes, the face that electrode is relative is done aslope.Base 6 need play double action heat insulation and that support, so should select the lower material that certain degree of hardness is arranged of thermal conductance for use, generally require thermal conductivity less than 2W/mK, non-conductive, preferred material is a glass, also can select the high polymerization electrically non-conductive material of Te Fulong or other hard for use, can use the Bioexperiment microslide that is of a size of about 30mm * 100mm * 2mm.Heat insulating mattress 7 is the hollow cap of plastic material, and electrode 1 only accounts for the 10%-50% that it looks down sectional area with the contact area of base 6, reduces the heat conduction between electrode 1 and the base 6 as far as possible.Be connected by multi-purpose adhesive between metal electrode 1, heat insulating mattress 7 and base 6 threes.
For guaranteeing that transition electrode 2 contacts well with reguline metal electrode 1, require the surface of contact between compressing tablet 4 and the reguline metal electrode 1 very smooth.Transition electrode 2 is preferably used spun gold, about the spacing 50 μ m between two spun golds (referring to Fig. 2).
Cut a mouth at reguline metal electrode 1 near the position of transition electrode 2, make it to form a cavity, then can implant temperature sensor 5 therein, the signal wire with temperature sensor after guaranteeing to be connected with multi-purpose adhesive picks out to signal processing unit.The kind of temperature sensor is with different between measurement zone and different, can adopt T or K type thermocouple or Pt100 or 1000 thermal resistances in the high-temperature region, can adopt Pt100 or 1000 thermal resistances or SiD sensor at low-temperature space, size restrictions is advisable with interior at 5mm * 5mm * 5mm, and measuring error is less than 1K.
The assembling sequence of experiment porch is earlier temperature sensor 5 to be implanted in the reguline metal electrode 1, distinguish adhesion heat insulating mattress 7 and base 6 more in order, heat insulating mattress 7 and reguline metal electrode 1, then transition electrode 2 is connected on the reguline metal electrode 1, press with compressing tablet 4, notice that the distance between two transition electrodes 2 need be less than 100 microns, otherwise probably cause spacing to cause installing failure greater than the length of testing sample.Subsequently one group of compressing tablet in outside 4 is pressed voltage lead, entering SEM nano-probe system again carries out the installation of testing sample line [method is seen Q.Chen, S.Wang, and L.M.Peng, ＂ Establishing Ohmic contacts in situ current-voltage characteristic measurements on acarbon nanotube inside the scanning electron microscope, ＂ Nanotechnol., vol.17, no.4, pp.1087-1098, Jan.2006] (see figure 2).
After the experiment porch assembling is finished, control the temperature-resistant of a reguline metal electrode, and change the temperature of another reguline metal electrode, measure two ends temperature and voltage simultaneously.
Seebeck coefficient is defined by following formula:
Wherein E is an electric field intensity, and electromotive force is defined as:
Thermograde is pointed to the higher place of temperature, and electromotive force points to the lower direction of voltage, and relatively equation (1) and (2) can obtain:
(for example the reguline metal electrode is the red copper electrode when the Seebeck coefficient of materials such as each electrode of experiment porch of the present invention and voltage measurement lead is similar, transition electrode is a gold thread, lead is a copper cash), the Seebeck effect synoptic diagram in whole measurement loop can be as shown in Figure 3, wherein A is a testing sample, B is the voltage measurement circuit that electrode and lead etc. are formed, and has in total loop:
Wherein 1 is two points that are connected to voltage table with 4,1 and 4 isothermals, then
S in the formula (5)
AAbsolute Seebeck coefficient for testing sample; S
BFor measuring the absolute Seebeck coefficient (Absolute Seebeck Coefficient or Thermopower) of return path materials; Δ V is the electric potential difference that records, and Δ T is the temperature difference that records.
At this Seebeck coefficient of measuring multi-walled carbon nano-tubes, the system voltage measurement has utilized Keithley2182ANanovoltmeter to measure minimum calibration 1nV, can satisfy the measurement demand.Can select the alternating temperature method is that liquid nitrogen refrigerating is (for the Seebeck coefficient of measuring the following temperature province of normal temperature, can be implemented to 180K at present) or Infrared Heating (can be implemented to 360K at present for measuring the above zone of normal temperature), can measure after connecting lead by Fig. 1, obtain the data (the cooling warm area has about 5000 groups in the data of 180K to 270K) of a series of electric potential differences and temperature difference, be that the slope of linear fit as the relative Δ T of Δ V of this interval temperature mid point made in the interval with every 10K then, d Δ V/d Δ T with the variation of temperature situation as shown in Figure 4.Utilize formula (5) S again
A=S
B-d Δ V/d Δ T, can find the Seebeck coefficient of material under different temperatures such as copper by existing documents and materials (be S
BKnown), then can obtain the absolute Seebeck coefficient S of the testing sample under the different temperatures
A
Claims (10)
1. method of measuring quasi one-dimensional nano-material Seebeck coefficient may further comprise the steps:
1) making two cross-sectional dimension is that micron-sized wire transition electrode is centimetre-sized with two sizes respectively the reguline metal electrode contacts;
2) utilize the nano-probe system to make single quasi-one-dimensional nanometer material to be measured connect two transition electrodes;
3) temperature difference between two reguline metal electrodes of change is measured the temperature difference of this two electrode and the electric potential difference of correspondence simultaneously, calculates the Seebeck coefficient of quasi-one-dimensional nanometer material.
2. the method for claim 1 is characterized in that: described reguline metal electrode uses red copper, gold, silver, stainless steel, brass or aluminium to make.
3. the method for claim 1, it is characterized in that: described transition electrode is spun gold or platinum filament, and its square section dimension is 10 μ m-50 μ m, and the minimum spacing between two transition electrodes is lower than 100 μ m.
4. the method for claim 1, it is characterized in that: in the described step 3), keep the temperature-resistant of a reguline metal electrode, and change the temperature of another reguline metal electrode, utilize the heating of infrared heating device or DC heating device, and utilize the mode of liquid nitrogen contact to freeze.
5. the method for claim 1 is characterized in that: the mensuration of temperature difference realizes by implant temperature sensor near the place of transition electrode in the electrode of reguline metal in the described step 3).
6. a system of measuring quasi one-dimensional nano-material Seebeck coefficient comprises experiment porch, changing device and data acquisition and treating apparatus three parts, wherein:
Experiment porch comprises that again the reguline metal electrode of two centimetre-sized, two cross-sectional dimension are a micron-sized wire transition electrode and a base, two reguline metal electrodes are installed on the base by heat insulating mattress, two transition electrodes closely contact with two reguline metal electrodes respectively, the minimum spacing of two transition electrodes is lower than 100 μ m, is used to install quasi-one-dimensional nanometer material to be measured;
Changing device is the device that the reguline metal electrode is heated and/or freezes;
Data acquisition and treating apparatus comprise two temperature sensors, voltage tester and a computing unit, the place of the implanted centimetre-sized of temperature sensor reguline metal electrode interior, next-door neighbour's transition electrode, and its signal wire is connected to computing unit; Voltage tester both end voltage lead-in wire connects two reguline metal electrodes respectively, and its electric potential difference that records is passed to computing unit; Computing unit receives and treatment temperature and voltage data, obtains the Seebeck coefficient of quasi-one-dimensional nanometer material.
7. system as claimed in claim 6 is characterized in that: described reguline metal electrode is made with red copper, gold, silver, stainless steel, brass or aluminium, and the opposite face of two reguline metal electrodes is intilted from top to bottom ramped shaped.
8. system as claimed in claim 6 is characterized in that: described transition electrode is spun gold or platinum filament, and its square section dimension is 10 μ m-50 μ m, is pressed on the reguline metal electrode top by compressing tablet.
9. system as claimed in claim 6, it is characterized in that: heating is made up of an infrared heater and a condenser with changing device, and condenser is the cone-shaped body of an Aluminium Foil Package, and the big muzzle of cone-shaped body is on infrared heater, an osculum is opened in the tip position, aims at a reguline metal electrode; Cooling changing device is made up of a heat-preserving container and a copper litz wire, and dress liquid nitrogen in the heat-preserving container, copper litz wire one end plug advance in the heat-preserving container and the other end contacts with a reguline metal electrode.
10. system as claimed in claim 6 is characterized in that: the temperature sensor that is used for measuring the high-temperature region adopts T or K type thermocouple, or the Pt100 thermal resistance; Be used for the temperature sensor employing Pt100 thermal resistance that low-temperature space is measured.
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