CN104614557A - Device and method for measuring micro-zone electric conductance and thermoelectric properties of material and application thereof - Google Patents
Device and method for measuring micro-zone electric conductance and thermoelectric properties of material and application thereof Download PDFInfo
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- CN104614557A CN104614557A CN201510053658.3A CN201510053658A CN104614557A CN 104614557 A CN104614557 A CN 104614557A CN 201510053658 A CN201510053658 A CN 201510053658A CN 104614557 A CN104614557 A CN 104614557A
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- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims description 24
- 239000000523 sample Substances 0.000 claims abstract description 165
- 239000000758 substrate Substances 0.000 claims abstract description 59
- 238000012360 testing method Methods 0.000 claims abstract description 32
- 238000003384 imaging method Methods 0.000 claims abstract description 21
- 238000005259 measurement Methods 0.000 claims description 56
- 238000012876 topography Methods 0.000 claims description 20
- 239000010408 film Substances 0.000 claims description 19
- 239000002184 metal Substances 0.000 claims description 18
- 239000013078 crystal Substances 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 2
- 239000002120 nanofilm Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 238000001338 self-assembly Methods 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 claims description 2
- 230000001360 synchronised effect Effects 0.000 abstract description 10
- 239000013068 control sample Substances 0.000 abstract 2
- 230000010365 information processing Effects 0.000 abstract 2
- 238000005057 refrigeration Methods 0.000 abstract 2
- 238000004630 atomic force microscopy Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013480 data collection Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
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Abstract
The invention provides a device for measuring micro-zone electric conductance and thermoelectric properties of a material. The device comprises a testing system and a control and information processing system; the testing system comprises a conductive probe (1), a refrigeration storage (5), a conductive substrate (3) and a temperature control sample table (4); the conductive probe (1) is connected with the refrigeration storage (5); the conductive substrate (3) is adhered to the temperature control sample table (4); the control and information processing system comprises a first relay (6), a second relay (7), a front voltage amplifier (8), a program controlling current source table (9), a program control voltage meter (10), an atomic force microscope controller (11), a host computer (12) and an atomic force microscope host (13). With the adoption of the device, the micro-zone electric conductance of a sample, the seebeck coefficient measuring, the electric conductance and thermoelectric force alterative measuring, and synchronous imaging of thermoelectric force and sample appearance can be carried out.
Description
Technical field
The invention belongs to conductance and thermoelectric property fields of measurement, relate to the measurement mechanism of a kind of material domain conductance and thermoelectric property, measuring method and uses thereof, particularly relate to a kind of based on the material domain conductance of atomic force microscopy and the measurement mechanism, measuring method and uses thereof of thermoelectric property.
Background technology
Heat energy can be directly changed into electric energy or electric energy is directly changed into heat energy by thermoelectric effect, decreases the pilot process of energy conversion, and thermoelectric material has very large application prospect in solution energy problem and environmental problem.Seebeck coefficient represents the size of the thermoelectrical potential that thermoelectric material produces under the unit temperature difference, can characterize the ability of thermoelectric material in energy conversion.The thermoelectric property of material is measured mainly to the measurement of its Seebeck coefficient, traditional Seebeck coefficient measuring method is due to the restriction of size, the Seebeck coefficient of material can only be recorded in macro-scale (being greater than micron dimension), as patent CN103512914A discloses a kind of Seebeck coefficient measuring system, comprise test example platform, temperature difference warm table, hot junction heated beam, cold junction heated beam, hot junction sample mounting table, cold junction sample mounting table, signal acquisition and processing system and temperature control system, it achieves the measurement of Seebeck coefficient, but it only can be measured material in macro-scale, cannot measure the conductance of material domain and thermoelectrical potential.
Summary of the invention
For the problem cannot measured material domain conductance and thermoelectrical potential existed in prior art, the invention provides a kind of based on the material domain conductance of atomic force microscopy and the measurement mechanism, measuring method and uses thereof of thermoelectric property.Described device can realize the conductance measurement of sample in microcell, and thermoelectrical potential measures (i.e. Seebeck coefficient measure), and conductance-thermoelectrical potential is measurement alternately, and thermoelectrical potential and sample topography synchronous imaging.
For reaching this object, the present invention by the following technical solutions:
A kind of conductance of material domain and the measurement mechanism of thermoelectric property, described measurement mechanism comprises test macro and control and information handling system, described test macro comprises conducting probe, freezer, conductive substrates and temperature controlled sample platform, wherein conducting probe is connected with freezer, and conductive substrates attaches on temperature controlled sample platform.
Wherein, temperature controlled sample platform is used for the temperature of regulation and control conductive substrates, thus controls the temperature of testing sample; Freezer is obtained by the material that temperature conductivity is high, and it is in room temperature in order to the temperature maintaining conducting probe.
Preferably, described control and information handling system comprise the first relay, second relay, voltage preamplifier, programmable current source table, program-controlled voltage table, atomic force microscope controller, main frame and atomic force microscope main frame, wherein the first stationary contact of the first relay is connected with programmable current source table with the first stationary contact of the second relay simultaneously, second stationary contact of the first relay is connected with voltage preamplifier with the second stationary contact of the second relay simultaneously, programmable current source table is connected with main frame, voltage preamplifier, program-controlled voltage table is connected successively with main frame, voltage preamplifier, atomic force microscope controller is connected successively with atomic force microscope main frame.
Wherein, host computer control relay carries out the measurement switching to realize conductance and thermoelectric property, and it carries out acquisition and processing to data simultaneously.
Preferably, described conducting probe is connected with the moving contact of the first relay after being connected with freezer.
Preferably, described conductive substrates is connected with the moving contact of the second relay.
Preferably, described conducting probe is simple metal probe or plating probe.
Preferably, described conductive substrates is conducting metal substrate.
Preferably, described voltage preamplifier is high input impedance direct supply prime amplifier, and the local thermoelectrical potential that sample upper and lower surface produces is amplified, to carry out subsequent treatment by it.
Wherein, described local thermoelectrical potential refers to: because sample is heated by sample stage, be in the temperature higher than room temperature, and conducting probe is in room temperature.When conducting probe contacts with sample surfaces, due to heat conducting effect, the region of sample near needle point will form local temperature gradient distribution, i.e. micro-area temperature gradient.Due to the existence of pyroelectric phenomena, this thermograde can cause sample to produce the thermoelectrical potential of local.
A measuring method for above-mentioned measurement mechanism, described measuring method comprises the measurement of conductance and/or the measurement of thermoelectric property, the measurement of such as conductance, and the measurement of thermoelectric property or conductance and thermoelectric property are measured simultaneously.
Preferably, the measurement of described conductance comprises the following steps: be placed in by testing sample in conductive substrates, by conducting probe contact measured sample surfaces, host computer control first relay and the first stationary contact of the second relay are in closure state makes conducting probe and conductive substrates all be connected with programmable current source table, host computer control programmable current source table output voltage is in conducting probe and conductive substrates, and measure the current value returned from conducting probe and conductive substrates, obtain conducting trace.
Wherein, conducting probe atomic force microscope control under with testing sample surface contact, form two electrodes with the conductive substrates below testing sample.When conducting probe contact measured sample surfaces, host computer control programmable current source table output voltage is in conducting probe and conductive substrates, between conducting probe and conductive substrates, add certain bias voltage, measure by the electric current between probe and substrate simultaneously, the microcell conductance of material can be obtained.
Preferably, the measurement of described thermoelectric property comprises the measurement of thermoelectrical potential and/or the imaging of sample topography, i.e. the measurement of thermoelectrical potential, the imaging of sample topography, and the synchronous imaging of thermoelectrical potential and sample topography.
Preferably, the measurement of described thermoelectrical potential comprises: be placed in by testing sample in conductive substrates, by temperature controlled sample platform, testing sample is heated to above the temperature of room temperature, by conducting probe contact measured sample surfaces, maintain conducting probe by freezer and be in room temperature, electric potential difference is formed between conductive substrates and conducting probe, host computer control first relay and the second stationary contact of the second relay are in closure state makes conducting probe be connected with voltage preamplifier with conductive substrates simultaneously, the electric potential difference formed is measured by program-controlled voltage table after voltage preamplifier amplifies, and processed by main frame, obtain thermoelectrical potential.
Wherein, testing sample is heated to above the temperature of room temperature by temperature controlled sample platform, and freezer maintains conducting probe and is in room temperature, makes conducting probe annex produce the thermograde of a microcell, this thermograde will form electric potential difference between conductive substrates and conducting probe, i.e. thermoelectrical potential.Thermoelectrical potential is amplified by voltage preamplifier, then is gathered by host computer control voltage table, or realizes the synchronous imaging of surface topography and thermoelectrical potential by the controller of atomic force microscope.By changing thermograde, and measuring this thermoelectrical potential, the linear relationship between thermoelectrical potential and temperature can be obtained, and then try to achieve the Seebeck coefficient of material.
Preferably, need before and after the measurement of described thermoelectrical potential to measure conductance respectively, measurement due to thermoelectrical potential must ensure that the upper surface of conducting probe and testing sample has good physical contact, and record electric conductivity value obtain size can as the amount judging probe and sample surfaces contact condition, therefore measure conductance all respectively, to ensure that measured thermoelectrical potential is all valid data in the front and back measuring thermoelectrical potential.
The imaging of described sample topography comprises the following steps: be placed in by testing sample in conductive substrates, by temperature controlled sample platform, testing sample is heated to above the temperature of room temperature, by conducting probe contact measured sample surfaces, maintain conducting probe by freezer and be in room temperature, electric potential difference is formed between conductive substrates and conducting probe, host computer control first relay and the second stationary contact of the second relay are in closure state makes conducting probe be connected with voltage preamplifier with conductive substrates simultaneously, the electric potential difference formed sends into atomic force microscope controller after voltage preamplifier amplifies, again by atomic force microscope host process, obtain the imaging of sample topography.
Preferably, need to measure conductance respectively before and after the imaging of described sample topography.
Preferably, the imaging of described sample topography synchronously can complete with the measurement of thermoelectrical potential.Thermoelectrical potential is amplified by voltage preamplifier, control voltage table by computing machine again to gather, or by the controller of atomic force microscope by the thermoelectrical potential signal feedback that exports in atomic force microscope, the synchronous imaging of thermoelectrical potential and sample topography can be obtained.
Preferably, described testing sample is crystal or non-crystal thin film sample.
Preferably, described testing sample be in organic semiconductor crystal thin film, organic self assembly Small molecular film or inorganic two-dimensional film material any one.
Preferably, described testing sample is placed in conductive substrates is adopt the mode of deposition to be placed in conductive substrates.
Preferably, described measurement mechanism be applied to film sample perpendicular to the microcell conductance in film surface direction and the measurement of thermoelectric property.
Compared with prior art, the present invention has following beneficial effect:
Based on the microprobe technology of atomic force microscopy in the property representation of material domain as each side such as mechanics, electricity and magnetics have unique advantage.The present invention, in conjunction with microprobe technology, (nanometer scale) can measure the thermoelectrical potential (Seebeck coefficient) of material, the thermoelectric property of exosyndrome material in microcell.Measurement mechanism provided by the present invention can realize the conductance measurement of sample in microcell, and Seebeck coefficient is measured, and conductance-thermoelectrical potential is alternately measured, and thermoelectrical potential and sample topography synchronous imaging.
Accompanying drawing explanation
Fig. 1 is the measurement mechanism schematic diagram of material domain of the present invention conductance and microcell thermoelectric property;
Fig. 2 is the voltage-current curve graph that measurement mechanism of the present invention measurement conductivity of material obtains;
Fig. 3 is the thermoelectrical potential curve map that measurement mechanism of the present invention measurement thermoelectrical potential obtains;
Fig. 4 is the synchronous imaging figure of the thermoelectrical potential that records of measurement mechanism of the present invention and sample topography;
Wherein, 1-conducting probe, 2-testing sample, 3-conductive substrates, 4-temperature controlled sample platform, 5-freezer, 6-first relay, 7-second relay, 8-voltage preamplifier, 9-programmable current source table, 10-program-controlled voltage table, 11-atomic force microscope controller, 12-main frame, 13-atomic force microscope main frame.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
Specific embodiments of the invention adopt measurement mechanism as shown in Figure 1 film sample to be carried out to the test of microcell conductance and microcell thermoelectric property.Those skilled in the art should understand, the present invention is not limited to sample cited in embodiment, according to measurement mechanism provided by the invention, measuring method and uses thereof, those skilled in the art can measure the microcell conductance of crystal or non-crystal thin film sample and thermoelectric property.
Embodiment 1: the conductance of film sample is measured
As described in Figure 1, film sample 2 is deposited in conducting metal substrate 3, conducting metal substrate 3 is attached to temperature controlled sample platform 4, conducting probe 1 atomic force microscope controller 11 control under with film sample 2 surface contact, two electrodes are formed with the conducting metal substrate 3 below film sample 2, main frame 12 controls the first relay 6 and is in closure state with the first stationary contact of the second relay 7 conducting probe 1 is all connected with programmable current source table 9 with conducting metal substrate 3, main frame 12 controls programmable current source table 9 and exports series of voltage on conducting probe 1 and conducting metal substrate 3, and measure the current value returned from conducting probe 1 and conducting metal substrate 3, obtain conducting trace, record result as shown in Figure 2.
Embodiment 2: the thermoelectrical potential of film sample is measured
Film sample 2 is deposited in conducting metal substrate 3, conducting metal substrate 3 is attached to temperature controlled sample platform 4, by temperature controlled sample platform 4, testing sample 2 is heated to above the known temperature of room temperature, conducting probe 1 atomic force microscope controller 11 control under with film sample 2 surface contact, two electrodes are formed with the conducting metal substrate 3 below film sample 2, maintain conducting probe 1 by the freezer 5 that temperature conductivity is high and be in room temperature, by the thermograde of a generation microcell near conducting probe 1, this thermograde forms electric potential difference between conducting metal substrate 3 and conducting probe 1, main frame 12 controls the first relay 6 and the second stationary contact of the second relay 7 and is in closure state conducting probe 1 and conductive substrates 3 are connected with high input impedance DC voltage prime amplifier 8 simultaneously, the electric potential difference formed is measured by program-controlled voltage table 10 after high input impedance DC voltage prime amplifier 8 amplifies, and carry out Data Collection and process by main frame 12, obtain the thermoelectrical potential curve map at same position different heating temperature, as shown in Figure 3.
Embodiment 3: the thermoelectrical potential of film sample and the synchronous imaging of sample topography
Film sample 2 is deposited in conducting metal substrate 3, conducting metal substrate 3 is attached to temperature controlled sample platform 4, by temperature controlled sample platform 4, testing sample 2 is heated to above the known temperature of room temperature, conducting probe 1 atomic force microscope controller 11 control under with film sample 2 surface contact, two electrodes are formed with the conducting metal substrate 3 below film sample 2, maintain conducting probe 1 by the freezer 5 that temperature conductivity is high and be in room temperature, by the thermograde of a generation microcell near conducting probe 1, this thermograde forms electric potential difference between conducting metal substrate 3 and conducting probe 1, main frame 12 controls the first relay 6 and the second stationary contact of the second relay 7 and is in closure state conducting probe 1 and conductive substrates 3 are connected with high input impedance DC voltage prime amplifier 8 simultaneously, the electric potential difference formed is measured by program-controlled voltage table 10 after high input impedance DC voltage prime amplifier 8 amplifies, and carry out Data Collection and process by main frame 12, meanwhile, the electric potential difference formed sends into atomic force microscope controller 11 after high input impedance DC voltage prime amplifier 8 amplifies, carried out collection and the process of data again by atomic force microscope main frame 13, realize the synchronous imaging of sample topography and thermoelectrical potential, as shown in Figure 4.
Comprehensive above-described embodiment can be found out, the present invention, in conjunction with microprobe technology, (nanometer scale) can measure the thermoelectrical potential (Seebeck coefficient) of material, the thermoelectric property of exosyndrome material in microcell.Measurement mechanism provided by the present invention can realize the conductance measurement of sample in microcell, and Seebeck coefficient is measured, and conductance-thermoelectrical potential is alternately measured, and thermoelectrical potential and sample topography synchronous imaging.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. the conductance of a material domain and the measurement mechanism of thermoelectric property, it is characterized in that, described measurement mechanism comprises test macro and control and information handling system, described test macro comprises conducting probe (1), freezer (5), conductive substrates (3) and temperature controlled sample platform (4), wherein conducting probe (1) is connected with freezer (5), and conductive substrates (3) attaches on temperature controlled sample platform (4).
2. measurement mechanism according to claim 1, it is characterized in that, described control and information handling system comprise the first relay (6), second relay (7), voltage preamplifier (8), programmable current source table (9), program-controlled voltage table (10), atomic force microscope controller (11), main frame (12) and atomic force microscope main frame (13), wherein the first stationary contact of the first relay (6) is connected with programmable current source table (9) with the first stationary contact of the second relay (7) simultaneously, second stationary contact of the first relay (6) is connected with voltage preamplifier (8) with the second stationary contact of the second relay (7) simultaneously, programmable current source table (9) is connected with main frame (12), voltage preamplifier (8), program-controlled voltage table (10) is connected successively with main frame (12), voltage preamplifier (8), atomic force microscope controller (11) is connected successively with atomic force microscope main frame (13).
3. measurement mechanism according to claim 1 and 2, is characterized in that, is connected after described conducting probe (1) is connected with freezer (5) with the moving contact of the first relay (6);
Preferably, described conductive substrates (3) is connected with the moving contact of the second relay (7).
4. the measurement mechanism according to any one of claim 1-3, is characterized in that, described conducting probe (1) is simple metal probe or plating probe;
Preferably, described conductive substrates (3) is conducting metal substrate;
Preferably, described voltage preamplifier (8) is high input impedance direct supply prime amplifier.
5. utilize the measuring method of the measurement mechanism described in any one of claim 1-4, it is characterized in that, described measuring method comprises the measurement of conductance and/or the measurement of thermoelectric property.
6. measuring method according to claim 5, it is characterized in that, the measurement of described conductance comprises the following steps: be placed in by testing sample (2) in conductive substrates (3), by conducting probe (1) contact measured sample (2) surface, main frame (12) controls the first relay (6) and is in closure state with the first stationary contact of the second relay (7) conducting probe (1) is all connected with programmable current source table (9) with conductive substrates (3), main frame (12) controls programmable current source table (9) output voltage in conducting probe (1) and conductive substrates (3), and measure the current value returned from conducting probe (1) and conductive substrates (3), obtain conducting trace.
7. the measuring method according to claim 5 or 6, is characterized in that, the measurement of described thermoelectric property comprises the measurement of thermoelectrical potential and/or the imaging of sample topography;
Preferably, the measurement of described thermoelectrical potential comprises: be placed in by testing sample (2) in conductive substrates (3), by temperature controlled sample platform (4), testing sample (2) is heated to above the temperature of room temperature, by conducting probe (1) contact measured sample (2) surface, maintain conducting probe (1) by freezer (5) and be in room temperature, electric potential difference is formed between conductive substrates (3) and conducting probe (1), main frame (12) controls the first relay (6) and the second stationary contact of the second relay (7) and is in closure state conducting probe (1) and conductive substrates (3) are connected with voltage preamplifier (8) simultaneously, the electric potential difference formed is measured by program-controlled voltage table (10) after voltage preamplifier (8) amplifies, and processed by main frame (12), obtain thermoelectrical potential,
Preferably, all need before and after the measurement of described thermoelectrical potential to measure conductance.
8. the measuring method according to any one of claim 5-7, it is characterized in that, the imaging of described sample topography comprises the following steps: be placed in by testing sample (2) in conductive substrates (3), by temperature controlled sample platform (4), testing sample (2) is heated to above the temperature of room temperature, by conducting probe (1) contact measured sample (2) surface, maintain conducting probe (1) by freezer (5) and be in room temperature, electric potential difference is formed between conductive substrates (3) and conducting probe (1), main frame (12) controls the first relay (6) and the second stationary contact of the second relay (7) and is in closure state conducting probe (1) and conductive substrates (3) are connected with voltage preamplifier (8) simultaneously, the electric potential difference formed sends into atomic force microscope controller (11) after voltage preamplifier (8) amplifies, again by atomic force microscope main frame (13) process, obtain the imaging of sample topography,
Preferably, all need before and after the imaging of described sample topography to measure microcell conductance;
Preferably, the imaging of described sample topography synchronously can complete with the measurement of thermoelectrical potential.
9. the measuring method according to any one of claim 5-8, is characterized in that, described testing sample is crystal or non-crystal thin film sample;
Preferably, described testing sample be in organic semiconductor crystal thin film, organic self assembly Small molecular film or inorganic two-dimensional film material any one;
Preferably, described testing sample is placed in conductive substrates (3) is adopt the mode of deposition to be placed in conductive substrates (3).
10. the purposes of the measurement mechanism according to any one of claim 1-4, is characterized in that, described measurement mechanism be applied to film sample perpendicular to the microcell conductance in film surface direction and the measurement of thermoelectric property.
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Cited By (7)
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| CN105137216A (en) * | 2015-07-09 | 2015-12-09 | 西安理工大学 | Zirconia film resistance conversion characteristic detection device and detection method thereof |
| CN105203825A (en) * | 2015-08-31 | 2015-12-30 | 国家纳米科学中心 | Manufacturing method of micro measuring electrode, measuring method of thermoelectrical potential and related device |
| CN109581060A (en) * | 2018-12-20 | 2019-04-05 | 云南大学 | A method of in uneven temperature test material conductivity off field |
| CN109738481A (en) * | 2018-11-27 | 2019-05-10 | 武汉嘉仪通科技有限公司 | A kind of the Seebeck coefficient measuring device and method of thin-film material |
| CN111122912A (en) * | 2019-12-24 | 2020-05-08 | 苏州大学 | Method for optimizing combination of conductive atomic force microscope and digital source meter |
| CN111289559A (en) * | 2020-02-24 | 2020-06-16 | 厦门大学 | Single-molecule junction thermal potential measuring method and equipment based on STM-BJ |
| CN112067851A (en) * | 2020-09-09 | 2020-12-11 | 四川大学 | Method for quantitatively measuring electric field force applied to organic polymer chain under action of electric field |
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| CN112067851A (en) * | 2020-09-09 | 2020-12-11 | 四川大学 | Method for quantitatively measuring electric field force applied to organic polymer chain under action of electric field |
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| CN104614557B (en) | 2017-07-18 |
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