CN107765161A - A kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance - Google Patents
A kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance Download PDFInfo
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Abstract
The invention discloses a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance is provided, it includes：The making of step 1, adiabatic insulated compound pad；Step 2, the deposition in diamond anvil face progress W Ta film thermocouples；Step 3, Seebeck coefficient measurement is carried out to sample under high pressure；The conductivity measurement of sample under step 4, high pressure；Although solving in the prior art using DAC, people can observe the change of the structure and physical property of material under ultra-high voltage environment.And the energy reduction of band and the increase of electrical conductivity can all occur under high pressure for most of semi-conducting material, this just provides excellent laboratory facilities to improve the thermoelectricity capability of semi-conducting material.However, in existing experimental technique, without a set of ripe measuring method for measuring sample thermoelectric property in DAC, cause that conducting material thermoelectricity performance can not be carried out the technical problems such as simple and convenient test.
Description
Technical field：
The invention belongs in physical quantity in-situ technique field, more particularly to a kind of diamond anvil cell under condition of high voltage
The method of in site measurement conducting material thermoelectricity performance.
Background technology：
With the increasingly depleted of fossil energy, energy problem turns into countries in the world focus of attention.Scientists from all over the world exist
It is directed to seeking efficient, free of contamination new energy trans-utilization mode.Then, since the last century the nineties, the energy turns
The research of conversion materials (thermoelectric material) turns into a study hotspot of material science.Thermoelectric material, also known as thermoelectric material, it is
One kind has the new function material of fuel factor and the mutual transformation of electrical effect, can be by heat using this property of thermoelectric material
Directly can mutually it be converted between electric energy.Thermoelectric material is mainly used in thermo-electric generation field.Compared with conventional electric generators,
Semiconductor thermoelectric generator have it is simple in construction, when need not use transmission parts, work it is noiseless, without dumping thing, without environment
The advantages that pollution, dependable performance, long service life, it is a kind of functional material with wide application prospect.
Most basic effect involved by thermoelectric material is Seebeck effect (Seebeck effect)：It is in closed circuit,
If line one end is placed in condition of high temperature T2(hot junction), and the other end is in open circuit and is in low-temperature condition T1(cold end), then cold
It is directly proportional with the temperature difference Δ T at hot cold both ends that end can produce open-circuit voltage Δ V, Seebeck voltage Δ V, i.e.,：Δ V=S Δs T=S
(T1-T2), wherein S is Seebeck coefficient, is determined by material own electronic band structure.To weigh semi-conducting material thermoelectricity performance
Superior index, A Chike wishes proposed thermoelectric figure of merit formula in 1911：Z=S2σ/k.Wherein S, σ and k are respectively material
Seebeck coefficient, electrical conductivity and thermal conductivity.And three parameters are not separate, the size that they are worth depends on material
Electronic structure and carrier transport and scattered situation.Therefore, S the and σ values of material are improved as far as possible, while amplitude peak drops
The k values of low material are to improve the key of conducting material thermoelectricity performance；In the device of many change material electric properties, diamond is to top
Anvil (Diamond Anvil Cell, abbreviation DAC) is the currently the only science apparatus that can produce million atmospheric pressure static pressures,
It is high-pressure science and most important scientific instrument in technical field of research.Using DAC, people can observe thing under ultra-high voltage environment
The change of the structure and physical property of matter.And reduction and the electricity of energy band can all occur under high pressure for most of semi-conducting material
The increase of conductance, this just provides excellent laboratory facilities to improve the thermoelectricity capability of semi-conducting material.However, in existing reality
Test in technology, without a set of ripe measuring method that sample thermoelectric property is measured in DAC, causing can not be to conducting material thermoelectricity
Simple and convenient test can be carried out.
The content of the invention：
The technical problem to be solved in the present invention：A kind of side of diamond anvil cell situ measurement conducting material thermoelectricity performance is provided
Method, although to solve in the prior art using DAC, people can observe the structure of material and physical property under ultra-high voltage environment
Change.And the energy reduction of band and the increase of electrical conductivity can all occur under high pressure for most of semi-conducting material, this is just to carry
The thermoelectricity capability of high semi-conducting material provides excellent laboratory facilities.However, in existing experimental technique, without it is a set of into
The ripe measuring method for measuring sample thermoelectric property in DAC, cause that conducting material thermoelectricity performance can not be carried out simple and convenient survey
The technical problems such as examination.
Technical solution of the present invention：
A kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance is provided, it includes：
The making of step 1, adiabatic insulated compound pad；
Step 2, the deposition in diamond anvil face progress W-Ta film thermocouples；
Step 3, Seebeck coefficient measurement is carried out to sample under high pressure；
The conductivity measurement of sample under step 4, high pressure.
The preparation method of adiabatic insulated compound pad is described in step 1：
(a), select T301 steel discs or rhenium piece to make gasket material, precompressed is carried out with diamond anvil cell, on gasket material
Diamond anvil anvil face impression, diamond anvil chamfering impression and diamond anvil incline impression are outwards extruded by center, is utilized
Laser-beam drilling machine punches at diamond anvil anvil face impression concentric；
(b), being fixed on the concentric circle holes center of gasket material and apply pressure adiabatic mica sheet film makes adiabatic mica
Piece film is fixed, and uses laser boring；
(c) it is 4 in mass ratio by bortz powder, cubic boron nitride powder or alumina powder and epoxy resin:1 ratio is mixed
Close, inserted after grinding uniformly in adiabatic mica film perforation and in all impressions, then pressurizeed with diamond anvil cell concentric；
(d) sample cavity, the diameter of sample cavity are used as by the use of burrowing at laser DAC anvil face impression concentrics in the third step
Less than the internal diameter of adiabatic mica ring.
The method that the deposition of W-Ta film thermocouples is carried out in diamond anvil face described in step 2 includes：
Step 2.1, in clean diamond surface one layer of aluminum oxide film is sputtered, as heat insulation layer；
Step 2.2, W film is sputtered on heat insulation layer of aluminum oxide, thickness is
Step 2.3 and then the sputtering aluminium oxide thin film again on W film, film is covered as photoetching W film；
Step 2.4, by the aluminum oxide film photolithography patterning above W film, it would be desirable to the W film partial denudation removed goes out
Come；
Step 2.5, it will integrally be put into W corrosive liquids and corroded, W film is graphical；
Step 2.6, remove anvil face center as the aluminum oxide photoetching above the W film at thermal cross, to ensure
Only two kinds of metallic films are contacts here during sputtering Ta, in this, as temperature probe；
Ta films are sputtered in step 2.7, the film after step 2.6 processing；
Step 2.8, using with etching W film identical methods processing is patterned to Ta, obtain W-Ta film thermocouples
Deposition.
The sputtering time of the sputtering aluminium oxide thin film of step 2.1 is 9-10 hour；It is adiabatic in aluminum oxide in step 2.2
The time that layer sputters W film above is 4 minutes；In step 2.3 on W film again the time of sputtering aluminium oxide thin film be 4
Hour；Etching time is the 4-6 seconds in step 2.5；The time that Ta films are sputtered in step 2.7 is 4 minutes.In height described in step 3
Depress includes to the method for sample progress Seebeck coefficient measurement：
Step 3.1, semiconductor samples are put into the adiabatic insulated compound pad prepared；
Step 3.2, two that the adiabatic insulated compound pad with semiconductor samples is placed on to diamond anvil cell face
Between W-Ta film thermocouples；
Step 3.3, resistance wire is wound to heating around the bottom diamond of diamond anvil cell, make Buddha's warrior attendant up and down
Stone anvil face has temperature difference；
Step 3.4, the demarcation for entering trip temperature using upper and lower two W-Ta thin film thermoelectric couple samples both ends respectively；
Step 3.5, keeping temperature difference are constant, the thermo-electromotive force at measurement sample both ends；
The Seebeck coefficient of step 3.6 and then calculating sample at various pressures.
The conductivity measuring method of sample is under high pressure described in step 4：Existed using film vanderburg four-probe measurement sample
Electrical conductivity under different pressures.
It is also included step 5, the thermoelectricity capability of sample under different pressures is assessed using thermoelectric figure of merit formula Z=S2 σ/k.
Beneficial effect of the present invention：
Magnetron sputtering technique, film micro-processing technology and diamond anvil cell technology are combined by the present invention, use metal
The electrode of thin film thermoelectric even summation film vanderburg four, construct a kind of experiment of the sample thermoelectricity capability of in site measurement under elevated pressure conditions
Device and experimental method；The integrated metallic film thermocouple of diamond anvil face not only accurately measures the temperature difference at sample both ends, together
When can function as the measurement that electrode pair sample enters thermo-electromotive force under horizontal high voltage.This invention overcomes under HTHP completely
The less shortcoming of DAC cavitys, compensate in DAC devices can not accurate thermometric blank.It is of the invention simple portable, it is safe and efficient,
Advantage is created for the improvement under HTHP to semi-conducting material thermoelectricity performance；Utilized in the prior art although solving
DAC, people can observe the change of the structure and physical property of material under ultra-high voltage environment.And most of semi-conducting material
The energy reduction of band and the increase of electrical conductivity can all occur under high pressure, this is just provided to improve the thermoelectricity capability of semi-conducting material
Excellent laboratory facilities.However, in existing experimental technique, without a set of ripe measurement sample thermoelectric property in DAC
Measuring method, cause that the technical problems such as simple and convenient test can not be carried out to conducting material thermoelectricity performance.
Brief description of the drawings：
Fig. 1 is structural representation in adiabatic insulated compound pad manufacturing process；
Fig. 2 is the W-Ta thermocouple structure schematic diagrames made using magnetron sputtering and micro-processing technology；
Fig. 3 is the apparatus structure schematic diagram that sample Bei Saike coefficients are measured under high pressure；
Fig. 4 is the electrode schematic diagram of film vanderburg four and conductivity measurement made using magnetron sputtering and micro-processing technology
Schematic device；
Fig. 5 is CoSb3The variation relation curve of the thermo-electromotive force measured under 1.03GPa and sample both ends temperature difference is illustrated
Figure；
Fig. 6 is CoSb3Seebeck coefficient schematic diagram at various pressures；
Fig. 7 is CoSb3Conductivity value schematic diagram at various pressures；
Fig. 8 is CoSb3Thermoelectric figure of merit schematic diagram at various pressures.
Embodiment：
A kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance is provided, it includes：
The making of step 1, adiabatic insulated compound pad；
Step 2, the deposition in diamond anvil face progress W-Ta film thermocouples；
Step 3, Seebeck coefficient measurement is carried out to sample under high pressure；
The conductivity measurement of sample under step 4, high pressure.
During high pressure diamond anvil calorifics and electrical measurement, the problem of sample is adiabatic and insulation is very important.
It is the metallic gaskets such as T301 steel, rhenium piece, leaf used in traditional diamond anvil, between pad, sample and metal electrode
The adiabatic problem of insulation and sample both sides is always the difficult point in high pressure electrical measurement.
Therefore the present invention carries out the making of adiabatic insulated compound pad using following methods
The preparation method of adiabatic insulated compound pad is described in step 1：
(a), select T301 steel discs or rhenium piece to make gasket material, precompressed is carried out with diamond anvil cell, on gasket material
Diamond anvil anvil face impression, diamond anvil chamfering impression and diamond anvil incline impression are outwards extruded by center, is utilized
Laser-beam drilling machine punches at diamond anvil anvil face impression concentric；
(b), being fixed on the concentric circle holes center of gasket material and apply pressure adiabatic mica sheet film makes adiabatic mica
Piece film is fixed, and uses laser boring；
(c) it is 4 in mass ratio by bortz powder, cubic boron nitride powder or alumina powder and epoxy resin:1 ratio is mixed
Close, inserted after grinding uniformly in adiabatic mica film perforation and in all impressions, then pressurizeed with diamond anvil cell concentric；
(d) sample cavity, the diameter of sample cavity are used as by the use of burrowing at laser DAC anvil face impression concentrics in the third step
Less than the internal diameter of adiabatic mica sheet.
In Fig. 1：1 is laser ablated holes, and 2 be pad diamond chamfering impression, and 3 be diamond incline impression, and 4 be buffering
Ring, 5 be insulating powder, and 6 be the laser ablated holes on insulating powder.
For outer heating temperature calibration, the small-sized thermocouple wire of domestic and international generally use presses close to diamond anvil cell
Anvil face carries out thermometric.For many defects of the temperature measurement technology, (thermograde is larger, calibrated error is larger, not in sample
Directly contact etc.), the present invention utilizes thin film deposition and micro-processing technology, is looked unfamiliar in diamond anvil and grows W-Ta metallic film thermoelectricity
Couple sample carries out Accurate Calibration.
The method that the deposition of W-Ta film thermocouples is carried out in diamond anvil face described in step 2 includes：
Step 2.1, in clean diamond surface one layer of aluminum oxide film is sputtered, as heat insulation layer；
Step 2.2, W film is sputtered on heat insulation layer of aluminum oxide, thickness is
Step 2.3 and then the sputtering aluminium oxide thin film again on W film, film is covered as photoetching W film；
Step 2.4, by the aluminum oxide film photolithography patterning above W film, it would be desirable to the W film partial denudation removed goes out
Come；
Step 2.5, it will integrally be put into W corrosive liquids and corroded, W film is graphical；
Step 2.6, remove anvil face center as the aluminum oxide photoetching above the W film at thermal cross, to ensure
Only two kinds of metallic films are contacts here during sputtering Ta, in this, as temperature probe；
Ta films are sputtered in step 2.7, the film after step 2.6 processing；
Step 2.8, using with etching W film identical methods processing is patterned to Ta, obtain W-Ta film thermocouples
Deposition.
The sputtering time of the sputtering aluminium oxide thin film of step 2.1 is 9-10 hour；It is adiabatic in aluminum oxide in step 2.2
The time that layer sputters W film above is 4 minutes；In step 2.3 on W film again the time of sputtering aluminium oxide thin film be 4
Hour；Etching time is the 4-6 seconds in step 2.5；The time that Ta films are sputtered in step 2.7 is 4 minutes.In height described in step 3
Depress includes to the method for sample progress Seebeck coefficient measurement：
Step 3.1, semiconductor samples are put into the adiabatic insulated compound pad prepared；
Step 3.2, two that the adiabatic insulated compound pad with semiconductor samples is placed on to diamond anvil cell face
Between W-Ta film thermocouples；
Step 3.3, resistance wire is wound to heating around the bottom diamond of diamond anvil cell, make Buddha's warrior attendant up and down
Stone anvil face has temperature difference；
Step 3.4, the measurement for entering trip temperature using upper and lower two W-Ta thin film thermoelectric couple samples both ends respectively, obtain temperature
Poor Δ T.W-Ta film thermocouples are using the preceding calibration for entering trip temperature using K-type thermocouple；
Step 3.5, keeping temperature difference are constant, the thermo-electromotive force Δ V at measurement sample both ends；
The Seebeck coefficient of step 3.6 and then calculating sample at various pressures, calculation formula is Δ V/ Δs T.
Measurement structure is as shown in Figure 3.Wherein 7 be W metallic films, and 8 be Ta metallic films, and 9 be alumina insulation powder, and 10 are
Voltmeter, 11 be measured sample.T represents the temperature measured by sample both ends, at the same time the temperature difference caused by sample both ends
Electromotive force is measured by voltmeter 10.
The conductivity measuring method of sample is under high pressure described in step 4：Existed using film vanderburg four-probe measurement sample
Electrical conductivity under different pressures.Electrode configuration and dress sample are as shown in Figure 4.Wherein 12-15 is contact conductor, and 16 be metal Mo electricity
Pole, 17 be alumina insulation powder.Conductivity values that can be with effectively measuring sample at various pressures by the device.
It also includes step 5, utilizes thermoelectric figure of merit formula Z=S2σ/k assesses the thermoelectricity capability of sample under different pressures；S、
σ and k is respectively Seebeck coefficient, electrical conductivity and the thermal conductivity of material.
Illustrate application of the experimental technique in CoSb3 thermoelectricity parameters under measuring high pressure with reference to Fig. 5-8.
CoSb3 be it is a kind of than the thermoelectric material that has wide application prospects, its have at ambient pressure larger carrier mobility,
Larger electrical conductivity and moderate Seebeck coefficients.This example measures CoSb3 thermoelectricity capabilities with pressure by the invention device
Variation tendency.Fig. 5 is the variation relation of thermo-electromotive force and sample both ends temperature difference that CoSb3 is measured under 1.03GPa.Sample
Thermo-electromotive force V and temperature difference T before be the linear relation of a comparison.CoSb3 is obtained under 1.03GPa by linear fit
Seebeck coefficient be 72.1 μ V/K.Fig. 6 is the Seebeck coefficients of CoSb3 at various pressures, and the Seebeck coefficient of sample exists
~10GPa or so reaches maximum.Fig. 7 is CoSb3 conductivity values at various pressures, and the electrical conductivity of sample is with pressure on constantly
The trend of liter.Fig. 8 is the thermoelectric figure of merit of CoSb3 at various pressures.The thermoelectric figure of merit of sample reaches 15.8 μ W/ in 10GPa or so
Cm K2, it is the maximum of whole pressure range.By Fig. 8 it can also be seen that thermoelectricity capability of the sample in 10GPa is compared to normal
Pressure situation improves 8 times or so, is the strong evidence that high pressure improves conducting material thermoelectricity performance.
Claims (7)
1. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance, it includes：
The making of step 1, adiabatic insulated compound pad；
Step 2, the deposition in diamond anvil face progress W-Ta film thermocouples；
Step 3, Seebeck coefficient measurement is carried out to sample under high pressure；
The conductivity measurement of sample under step 4, high pressure.
2. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance according to claim 1, its feature
It is：
The preparation method of adiabatic insulated compound pad is described in step 1：
(a), select T301 steel discs or rhenium piece to make gasket material, precompressed is carried out with diamond anvil cell, on gasket material in
The heart outwards extrudes diamond anvil anvil face impression, diamond anvil chamfering impression and diamond anvil incline impression, utilizes laser
Puncher punches at diamond anvil anvil face impression concentric；
(b) adiabatic mica sheet film, is fixed on the concentric circle holes center of gasket material and applying pressure makes adiabatic mica sheet thin
Film is fixed, and uses laser boring；
(c) it is 4 in mass ratio by bortz powder, cubic boron nitride powder or alumina powder and epoxy resin:1 ratio mixing, grinds
Insert in adiabatic mica film perforation and in all impressions after mill is uniform, then pressurizeed with diamond anvil cell concentric；
(d) it is less than by the use of burrowing at laser DAC anvil face impression concentrics in the third step as sample cavity, the diameter of sample cavity
The internal diameter of adiabatic mica ring.
3. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance according to claim 1, its feature
It is：
The method that the deposition of W-Ta film thermocouples is carried out in diamond anvil face described in step 2 includes：
Step 2.1, in clean diamond surface one layer of aluminum oxide film is sputtered, as heat insulation layer；
Step 2.2, W film is sputtered on heat insulation layer of aluminum oxide, thickness is
Step 2.3 and then the sputtering aluminium oxide thin film again on W film, film is covered as photoetching W film；
Step 2.4, by the aluminum oxide film photolithography patterning above W film, it would be desirable to the W film partial denudation removed comes out；
Step 2.5, it will integrally be put into W corrosive liquids and corroded, W film is graphical；
Step 2.6, remove anvil face center as the aluminum oxide photoetching above the W film at thermal cross, to ensure to sputter
Only two kinds of metallic films are contacts here during Ta, in this, as temperature probe；
Ta films are sputtered in step 2.7, the film after step 2.6 processing；
Step 2.8, using with etching W film identical methods processing is patterned to Ta, obtain W-Ta film thermocouples sink
Product.
4. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance according to claim 3, its feature
It is：The sputtering time of the sputtering aluminium oxide thin film of step 2.1 is 9-10 hour；In step 2.2 in heat insulation layer of aluminum oxide
The time for sputtering W film above is 4 minutes；In step 2.3 the time of sputtering aluminium oxide thin film is 4 small again on W film
When；Etching time is the 4-6 seconds in step 2.5；The time that Ta films are sputtered in step 2.7 is 4 minutes.
5. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance according to claim 1, its feature
It is：Carrying out the method for Seebeck coefficient measurement described in step 3 to sample under high pressure includes：
Step 3.1, semiconductor samples are put into the adiabatic insulated compound pad prepared；
Step 3.2, two W-Ta that the adiabatic insulated compound pad with semiconductor samples is placed on to diamond anvil cell face
Between film thermocouple；
Step 3.3, resistance wire is wound to heating around the bottom diamond of diamond anvil cell, make diamond anvil up and down
Face has temperature difference；
Step 3.4, the demarcation for entering trip temperature using upper and lower two W-Ta thin film thermoelectric couple samples both ends respectively；
Step 3.5, keeping temperature difference are constant, the thermo-electromotive force at measurement sample both ends；
The Seebeck coefficient of step 3.6 and then calculating sample at various pressures.
6. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance according to claim 1, its feature
It is：The conductivity measuring method of sample is under high pressure described in step 4：Using film vanderburg four-probe measurement sample in difference
Electrical conductivity under pressure.
7. a kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance according to claim 1, its feature
It is：It also includes step 5, utilizes thermoelectric figure of merit formula Z=S2σ/k assesses the thermoelectricity capability of sample under different pressures.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110095505A (en) * | 2019-03-13 | 2019-08-06 | 东北电力大学 | A kind of method of Transition-metal dichalcogenide energy gap regulation |
| CN111175119A (en) * | 2020-01-15 | 2020-05-19 | 吉林大学 | Insulation method for metal gasket in diamond anvil cell |
| CN112062153A (en) * | 2020-09-15 | 2020-12-11 | 吉林大学 | Improve BaZrO3Method of electrical conductivity |
| CN112415055A (en) * | 2020-10-10 | 2021-02-26 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110095505A (en) * | 2019-03-13 | 2019-08-06 | 东北电力大学 | A kind of method of Transition-metal dichalcogenide energy gap regulation |
| CN111175119A (en) * | 2020-01-15 | 2020-05-19 | 吉林大学 | Insulation method for metal gasket in diamond anvil cell |
| CN112062153A (en) * | 2020-09-15 | 2020-12-11 | 吉林大学 | Improve BaZrO3Method of electrical conductivity |
| CN112415055A (en) * | 2020-10-10 | 2021-02-26 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
| CN112415055B (en) * | 2020-10-10 | 2023-06-13 | 牡丹江师范学院 | Comprehensive in-situ electric transport measurement method based on diamond anvil cell |
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