CN103399044B - The apparatus and method of in-situ test conductive species transport property under High Temperature High Pressure - Google Patents
The apparatus and method of in-situ test conductive species transport property under High Temperature High Pressure Download PDFInfo
- Publication number
- CN103399044B CN103399044B CN201310323217.1A CN201310323217A CN103399044B CN 103399044 B CN103399044 B CN 103399044B CN 201310323217 A CN201310323217 A CN 201310323217A CN 103399044 B CN103399044 B CN 103399044B
- Authority
- CN
- China
- Prior art keywords
- pressure
- sample
- anvil
- high temperature
- thermopair
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
Under High Temperature High Pressure of the present invention, the apparatus and method of in-situ test conductive species transport property, belong to the field of high-pressure science technique and material science and technology.Device introduces the electrode of 4 copper wires (4) as measured resistivity, introduce two pairs of thermopairs (10) for measuring Seebeck coefficient, the pressure fixing that sample (5) produces by high temperature high pressure device with electrode, thermopair (10) pad.By recording relative resistance R
a, R
bwith the thickness d calculation sample resistivity after sample pressurization; By measuring the electric potential difference V of the positive interpolar of two pairs of thermopairs
efand the electric potential difference V between negative pole
hgcalculation sample Seebeck coefficient.The inventive method is simple, and easy to implement, success ratio is high, and experiment repetition rate is good; Solve the problem that wire and thermopair under high pressure easily rupture; Prevent the electric signal measured by the interference of heating current, guarantee the accuracy of result.
Description
Technical field
The invention belongs to the field of high-pressure science technique and material science and technology, particularly a kind of conductive species original position transport property at high temperature under high pressure---the technology of electronic transport (conductivity) and thermotransport (Seebeck coefficient) in-situ test.Object is the operation interval found high performance thermoelectric material and find out its thermoelectricity capability the best.
Background technology
Along with the increase of pressure, the electric conductivity of conductive species increases.Especially semiconductor material, its with gap reduces along with the increase of pressure, thus strengthens its electric conductivity.In addition, temperature effect has very important impact to the with gap of semiconductor material too.Generally speaking, the with gap of semiconductor material reduces along with the increase of temperature.In a semiconductor material, due to the electric potential difference that charge carrier occurs under thermograde, it is an important parameter of reaction material thermoelectricity capability.
Thermoelectric material is a kind of functional material heat energy and electric energy directly mutually transformed, and can realize utilizing electric energy directly to freeze or by the function of the heat energy direct generation of electricity.The thermo-electric device prepared by thermoelectric material have pollution-free, volume is little, lightweight, be convenient for carrying, the advantage such as long service life, it is applied, the cooling etc. of the cooling of such as portable refrigerator, generator, high speed lsi, high power laser and infrared eye in a lot of field.Although the advantage that thermo-electric device has conventional electrical devices incomparable, its transformation efficiency low so limit its application.Find high performance thermoelectric material is the direction that people make great efforts always.High performance thermoelectric material known is at present nearly all semiconductor material.
As previously mentioned, pressure and temperature all can modulate the energy gap width of material (especially semiconductor material), the electric conductivity of reinforcing material.But how in real time there is huge technical barrier in detected pressures and the change of temperature to material transfer character.Because the related experiment technology of carrying out in-situ test is at high temperature under high pressure very complicated.Be not only because need to arrange the loop that transport property is tested in High Temperature High Pressure cavity, also need to design in material to be measured in high-pressure chamber the thermograde produced needed for thermotransport property detection.Therefore, in current reported home position testing method, the conductivity test mainly under high pressure carried out, the device of employing is also mainly at diamond anvil cell.And utilizing large high-pressure chamber multiface upsetting machine, the resistivity of in site measurement material and Seebeck coefficient rarely have report at high temperature under high pressure.
The principle of thermoelectric effect: temperature difference produces electric potential difference, and Seebeck coefficient S definition is S=Δ V/ Δ T.The Seebeck coefficient that the temperature difference at sample two ends and electric potential difference can obtain sample is measured according to definition.The measurement of temperature difference adopts differential thermocouple method and the method with standard substance comparison usually, but this method measuring error is comparatively large, and sample, by the restriction of shape and size, should not under high pressure carry out.
Summary of the invention
The technical problem to be solved in the present invention is the resistivity and the Seebeck coefficient that adopt new method to measure conductive material at high temperature under high pressure.The method has simple to operate, that success ratio is high, error is little feature compared with additive method, mainly through the layout using new experimental technique to change test circuit, wire and thermopair can accurately be located under High Pressure position is less likely to occur move and rupture, thus ensure that the accuracy of test, and the method is easy to implement.
Under High Temperature High Pressure of the present invention, the main task of conductive materials Electric transport properties in-situ test is tested the resistivity of conductive materials and Seebeck coefficient.
Test experiments carries out at high temperature under high pressure, so will manufacture the environment of High Temperature High Pressure.Test experiments of the present invention completes on domestic DS029B type cubic hinge press.Domestic cubic hinge press provides the principle of work of pressure to be: oil pump is to six working cylinder fuel feeding, and the piston in working cylinder promotes pressure anvil extruding pressure transmitting medium, forms the simulated hollow high pressure chest of sealing, produce high pressure thus in pressure transmitting medium.The generation principle of high temperature is: heating system, pressure anvil, steel cap, graphite flake, graphite-pipe form an electrical return, heating system is from pressure anvil input current, graphite flake and graphite-pipe have electric current to pass through to generate heat, heat is spread to high-pressure chamber center by insulation course, thus produces high temperature in seal chamber.This type of type of heating is heater-type.This is tested in High Temperature High Pressure assembling used, and pressure transmitting medium is pyrophillite, and heating resistor is graphite-pipe, and insulating material is magnesia tube and oxidation magnesium sheet (referring to accompanying drawing 1).
Carry out the measurement of resistivity under High Temperature High Pressure, what test loop adopted is four-point method, and theoretical foundation is vanderburg method principle.The sample of vanderburg method measuring resistance rate is flake, has fixing thickness, uniform resistivity (not allowed cavity in sample).First need sample to be prepared as flake, meet the test request of the method.Under High Temperature High Pressure, resistivity measurement loop is divided into inner looping (under high-temperature and high-pressure conditions) and external loop (condition of normal pressure).Inner looping specifically connects as follows: four wires on cloth on laminar sample surface, the pressure fixing that the contact of wire and sample is produced by high-tension unit.The contact point of wire and sample is positioned at the edge of sample and enough little.The wire of these four test loops, through the aperture in High Temperature High Pressure pressure transfer sealing medium, insulate at the intersection ceramic pipe of thermopair and graphite-pipe, is finally connected on the pressure anvil in high temperature high pressure device, forms build-in test loop.The pressure anvil of outer test loop line and high-tension unit is connected to form test loop.Two pressure anvils are wherein as the electrode of electric current input and output, and two other pressure anvil is as the electrode of measuring voltage.Select suitable steady current input, measure magnitude of voltage, go out resistivity according to formulae discovery.
The present invention adopts round-about way can obtain the Seebeck coefficient of sample equally without the need to measuring the temperature difference.Under High Temperature High Pressure, Seebeck coefficient test loop is similar to resistivity measurement loop, is also divided into inner looping (under high-temperature and high-pressure conditions) and external loop (condition of normal pressure).Inner looping specifically connects as follows: a pair thermopair is placed on the upper surface of sample, another is placed on the lower surface of sample to thermopair, the pad of two pairs of thermopairs all will be placed on the circle centre position of sample, and pad is same with the contact of sample is the pressure fixing produced by high-tension unit.These two pairs of thermopairs, through the aperture in High Temperature High Pressure pressure transfer sealing medium, insulate with ceramic pipe equally at the intersection of thermopair and graphite-pipe, are finally connected on the pressure anvil in high temperature high pressure device, form build-in test loop.External loop pressure anvil and multimeter is connected to form with wire.Measure two pairs of thermopair positive poles and positive pole respectively, the electric potential difference between negative pole and negative pole, substitute into formulae discovery and draw Seebeck coefficient.
Under High Temperature High Pressure of the present invention, the concrete technical scheme of in-situ test conductive species transport property device is as described below.
A device for in-situ test conductive species transport property under High Temperature High Pressure, structure has the assembled block putting into high temperature high pressure device, and assembled block is by pyrophillite 8 as pressure transmitting medium, and in pyrophyllite block 8, order is equipped with cylindrical shape graphite-pipe 3 and magnesium oxide insulated pipe 6; Disc sample 5 is loaded in magnesium oxide insulated pipe 6, sample 5 top and bottom are equipped with oxidation magnesium sheet 7 and graphite flake 2 respectively in turn, graphite flake 2 and graphite-pipe 3 form hollow cylinder as heating resistor, heating wires connects respectively and presses down anvil and be connected with power supply, and the round hole at pyrophyllite block 8 two ends is by steel cap 1 shutoff; It is characterized in that, introduce 4 copper wires 4 as the electrode measuring sample 5 resistivity in the side of assembled block by aperture, introduce the Seebeck coefficient that two pairs of thermopairs 10 are used as to measure sample 5;
The contact point of described copper wire 4 one end is separately positioned on the edge of sample quadrant position, by the pressure fixing that high temperature high pressure device produces, the other end is connected respectively to 4 sides in high temperature high pressure device and presses on anvils, insulate at the intersection ceramic pipe 9 of copper wire 4 and graphite-pipe 3; During detection, 4 pressure anvils are connected with the serial connection direct supply of reometer, voltage table respectively;
Described thermopair 10, a pair thermopair is placed on the upper surface of sample 5, another is placed on the lower surface of sample 5 to thermopair, the pad of two pairs of thermopairs 10 is placed on the circle centre position of sample 5, insulate at the intersection ceramic pipe 9 of thermopair 10 and graphite-pipe 3, the termination of two pairs of thermopairs is connected respectively to 4 sides in high temperature high pressure device and presses on anvils; During detection 4 sides pressure anvil respectively with the Instrument connection measuring electric potential difference, the upper surface of sample 5 or lower surface are by the center of assembled block.
In the device of in-situ test conductive species transport property at high temperature under high pressure, described thermopair 10 can be NiCr-NiAl thermopair; The positive pole NiCr of two thermopairs is connected on two adjacent pressure anvils; The negative pole NiAl of two thermopairs is connected on another two adjacent pressure anvils.
Utilize the device of in-situ test conductive species transport property under High Temperature High Pressure, the method for in-situ test conductive species transport property has the method for testing of conductive species resistivity and the method for testing of conductive species Seebeck coefficient.Concrete measuring technology scheme is as described below.
A method for in-situ test conductive species resistivity under High Temperature High Pressure, utilizes the device of in-situ test conductive species transport property under aforesaid High Temperature High Pressure to measure; First assembled block is put into cubic hinge press, pressurizeed by pyrophyllite block 8 pairs of samples 5; Upper and lower two pressure anvils are connected heating power supply and are heated by graphite flake 2 and graphite-pipe 3 pairs of samples, reach detected pressures and the detected temperatures of sample; 4 side pressure anvils are got the first pressure anvil and second in order and are pressed anvil to be connected in series direct supply and reometer, and the 3rd pressure anvil is connected voltage table with the 4th pressure anvil, records I
1and V
1, then get the second pressure anvil and the 3rd and press anvil to be connected in series direct supply and reometer, the first pressure anvil and the 4th pressure anvil are connected voltage table, record I
2and V
2; According to formula
exp（-πR
Ad/ρ)+exp(-πR
Bd/ρ)=1
Calculate electricalresistivityρ, wherein R
a=V
1/ I
1, R
b=V
2/ I
2, d is thickness of sample after pressurization, measures obtain by sample from high-pressure chamber after being taken out.
A method for in-situ test conductive species Seebeck coefficient under High Temperature High Pressure, utilizes the device of in-situ test conductive species transport property under aforesaid High Temperature High Pressure to measure; First assembled block is put into cubic hinge press, pressurizeed by pyrophyllite block 8 pairs of samples 5, upper and lower two pressure anvils are connected heating power supply and are heated by graphite flake 2 and graphite-pipe 3 pairs of samples 5, reach detected pressures and the detected temperatures of sample; Measure the positive interpolar electric potential difference V of two pairs of thermopairs
efand electric potential difference V between negative pole
hg, then the Seebeck coefficient S=S of sample 5
--[V
ef(S
--S
+)/(V
ef-V
hg)], wherein S
+, S
-be respectively the Seebeck coefficient of thermopair positive pole, negative pole.
Experiment shows: the inventive method is simple, and easy to implement, success ratio is high, and experiment repetition rate is good; Solve the problem that wire and thermopair under high pressure easily rupture; Ensure that the interference that the insulation of wire and thermopair prevents the electric signal measured and is subject to for heating current, guarantee the accuracy of result.Compared with diamond anvil cell in-situ testing technique, the present invention has plurality of advantages: operating cost is low, control system is simple accurately, sample size is large, be convenient to lead-in wire, experimental error is little, utilize cavity type of heating control temperature difference to carry out Seebeck coefficient test, adopts round-about way can obtain the Seebeck coefficient etc. of sample equally without the need to measuring the temperature difference.This method of testing is not only applicable to thermoelectric material, is also applicable to resistivity and the Seebeck coefficient of testing other conductive materials.
Accompanying drawing explanation
Fig. 1 is that the present invention tests assembled block longitudinal diagram.
Fig. 2 is that the present invention tests assembled block drawing in side sectional elevation.
Fig. 3 is that embodiment 4 keeps pressure to be that 3GPa is constant, β-Ag
2te resistivity variation with temperature curve.
Fig. 4 is that embodiment 5 keeps temperature to be that 520K is constant, β-Ag
2te resistivity is with the change curve of pressure.
Fig. 5 is that embodiment 6 keeps pressure to be that 3GPa is constant, β-Ag
2te Seebeck coefficient variation with temperature curve.
Fig. 6 is that embodiment 7 keeps temperature to be that 520K is constant, β-Ag
2te Seebeck coefficient is with the change curve of pressure.
Embodiment
Following examples all complete on domestic DS029B type cubic hinge press, and with Ag
2te is test sample.
Embodiment 1
Under High Temperature High Pressure, the apparatus structure of in-situ test conductive species transport property is provided by Fig. 1 and Fig. 2.In fig. 1 and 2,1 is steel cap, and 2 is graphite flake, and 3 is graphite-pipe, 4 (amount to 4 copper wires and count a, b, c, d) respectively for copper wire, 5 is sample, and 6 is MgO insulation tube, and 7 is MgO insulating trip, 8 is pyrophyllite block, 9 is ceramic pipe, and 10 is thermopair (two pairs of thermopairs all can select NiCr-NiAl thermopair, and e, h are the positive pole of a pair thermopair and negative pole f, g is that another is to the positive pole of thermopair and negative pole).
Shown in Fig. 1,2, the same with the assembled block of general HP-HT synthesize, assembled block sidewall is made up of pyrophyllite block 8, graphite-pipe 3, MgO insulation tube 6, assembled block two ends are by MgO insulating trip 7, graphite flake 2 and steel cap 1 shutoff, space in graphite-pipe 3 and upper and lower two graphite flakes 2 loads sample 5, graphite-pipe 3 and graphite flake 2 press anvil to be electrically connected as heating resistor with upper and lower two, and two pressure anvils connect power supply and are used for heating for sample 5.Four sides of pyrophyllite block 8 are drilled with eight holes, and the graphite-pipe 3 corresponding with hole site, MgO insulation tube 6 place hole respectively, that is, each hole penetrates pyrophyllite block 8, graphite-pipe 3 and MgO insulation tube 6.Respectively by a, b, c, d place in copper wire 4(Fig. 2) and NiCr-NiAl thermopair 10(Fig. 2 in e, f, g, h place) respectively by aperture through pyrophyllite block 8, graphite-pipe 3 and MgO insulation tube 6, copper wire 4, the wire connecting thermopair 10 and graphite-pipe 3 are insulated with eight ceramic pipes 9, ceramic pipe 9 can be Al
2o
3material.The sample 5 of disc is put into high-pressure synthesis block, and copper wire 4 presses close to sample 5(as β-Ag
2te) edge is placed; By a pair NiCr-NiAl thermopair 10 by the center of cavity and the upper surface (see Fig. 2 solid line eh) of sample, another is placed on the lower surface (see Fig. 2 dotted line fg) of sample to NiCr-NiAl thermopair 10, and (ef is the positive pole of NiCr, thermopair; Gh is the negative pole of NiAl, thermopair), the pad of two pairs of thermopairs is all in the center of sample, and wire and thermopair are fixed by the pressure produced by high-tension unit.
Embodiment 2
The structure (i.e. the structure of Fig. 1,2 shown in assembled block) of the assembled block of high-pressure synthesis by embodiment 1 is assembled, puts into press.With wire, 4 side pressure anvils are connected with direct supply, measurement instrument.Set pressure and temperature, bring into operation, after press is raised to set pressure, starts heating.Temperature constant (generally heating after ten minutes temperature constant) until chamber central starts to carry out resistivity measurement.
See Fig. 2, electric current I
abflow into b from a to flow out, measure voltage drop V at d, c place
dc, note relative resistance R
a=V
dc/ I
ab; Electric current I
bcflow into c from b to flow out, record voltage drop V at a, d place
ad, note relative resistance R
b=V
ad/ I
bc.Then sample resistivity ρ, pass between thickness of sample d and relative resistance are:
Exp (-π R
ad/ ρ)+exp (-π (
bd/ ρ)=1 measurement data is substituted into above-mentioned formulae discovery go out resistivity.
Embodiment 3
The structure (i.e. the structure of Fig. 1,2 shown in assembled block) of the assembled block of high-pressure synthesis by embodiment 1 assembled, put into press, wherein the upper surface of sample 5 or lower surface are by the center of assembled block.With wire 4 side pressure anvils and the Instrument connection measuring electric potential difference.Set pressure and temperature, bring into operation, after press is raised to set pressure, starts heating, heats the temperature constant treating chamber central after ten minutes, start to carry out Seebeck coefficient measurement.
See Fig. 2, measure the electric potential difference V of the positive interpolar of two pairs of thermopairs respectively
efand the electric potential difference V between negative pole
hg; According to formula V
ef=(S
niCr-S) Δ T, V
hg=(S
niAl-S) Δ T, simultaneous obtains: S=S
niAl-[V
ef (s
niAl-S
niCr)/(V
ef-V
hg)].Wherein S
niCr, S
niAlbe respectively the Seebeck coefficient of thermopair both positive and negative polarity, its value is known.Above data are substituted into formulae discovery and goes out Seebeck coefficient.
Embodiment 4
Adopt the device of embodiment 1, i.e. the assembled block of the HP-HT synthesize shown in Fig. 1,2, selects β-Ag
2sample 5 made by Te material, and assembled block puts into hexahedron top press high-pressure cavity.In cavity, pressure is raised to 3Gpa, carries out pressurize.Ascending adjustment heating power, rises to each design temperature point successively, and allows cavity inner temperature reach stable respectively.By electrically connected method and the test process measurement resistance value R at each temperature of embodiment 2
aand R
b, then press exp (-π R
ad/ ρ)+exp (-π R
bd/ ρ)=1 calculating resistivity (d is the thickness of sample after pressurization, requires that use vernier caliper or milscale etc. are direct measure according to measuring accuracy).Concrete β-Ag
2te resistivity variation with temperature relation is shown in Fig. 3.
Embodiment 5
Adopt the device of embodiment 1, i.e. the assembled block of the HP-HT synthesize shown in Fig. 1,2, selects β-Ag
2sample 5 made by Te material, and assembled block puts into hexahedron top press high-pressure cavity.In cavity, temperature rises to 520K, is incubated.Ascending adjustment pressure, rises to each set pressure point successively, and pressurize allows cavity internal pressure stablize for ten minutes.The resistance value R under each pressure is measured by the electrically connected method of embodiment 2 and test process
aand R
b, then press exp (-π R
ad/ ρ)+exp (-π R
bd/ ρ)=1 calculating resistivity (d is the thickness of sample after pressurization).Concrete β-Ag
2te resistivity is shown in Fig. 4 with the variation relation of pressure.
Embodiment 6
Adopt the device of embodiment 1, i.e. the assembled block of the HP-HT synthesize shown in Fig. 1,2, selects β-Ag
2sample 5 made by Te material, and the upper surface of sample 5 is by the center of assembled block, and assembled block puts into hexahedron top press high-pressure cavity.In cavity, pressure is raised to 3Gpa, carries out pressurize.Ascending adjustment heating power, rises to each design temperature point successively, heats and within ten minutes, allows cavity inner temperature reach stable.The electric potential difference V of the positive interpolar of two pairs of thermopairs is at each temperature measured by the electrically connected method of embodiment 3 and test process
efand the electric potential difference V between negative pole
hg; According to formula S=S
niAl-[V
ef(S
niAl-S
niCr)/(V
ef-V
hg)] calculate Seebeck coefficient, concrete β-Ag
2te Seebeck coefficient variation with temperature relation is shown in Fig. 5.
Embodiment 7
Adopt the device of embodiment 1, i.e. the assembled block of the HP-HT synthesize shown in Fig. 1,2, selects β-Ag
2sample 5 made by Te material, and the upper surface of sample 5 is by the center of assembled block, and assembled block puts into hexahedron top press high-pressure cavity.In cavity, temperature rises to 520K, is incubated.Ascending adjustment pressure, rises to each set pressure point successively, and pressurize allows cavity internal pressure stablize for ten minutes.The electric potential difference V of the positive interpolar of two pairs of thermopairs under each pressure is measured by the electrically connected method of embodiment 3 and test process
efand the electric potential difference V between negative pole
hg; According to formula S=S
niAl-[V
ef(S
niAl-S
niCr)/(V
ef-V
hg)] calculate Seebeck coefficient.Concrete β-Ag
2te Seebeck coefficient is shown in Fig. 6 with the variation relation of pressure.
Claims (3)
1. the device of in-situ test conductive species transport property under a High Temperature High Pressure, structure has the assembled block putting into high temperature high pressure device, assembled block is by pyrophyllite block (8) as pressure transmitting medium, and in pyrophyllite block (8), order is equipped with cylindrical shape graphite-pipe (3) and magnesium oxide insulated pipe (6); Disc sample (5) is loaded in magnesium oxide insulated pipe (6), sample (5) top and bottom are equipped with oxidation magnesium sheet (7) and graphite flake (2) respectively in turn, graphite flake (2) and graphite-pipe (3) form hollow cylinder as heating resistor, heating wires connects respectively and presses down anvil and be connected with power supply, and the round hole at pyrophyllite block (8) two ends is by steel cap (1) shutoff; It is characterized in that, introduce 4 copper wires (4) as the electrode measuring sample (5) resistance in the side of assembled block by aperture, introduce the Seebeck coefficient that two pairs of thermopairs (10) being used as measures sample (5);
The contact point of described copper wire (4) one end is separately positioned on the edge of sample quadrant position, by the pressure fixing that high temperature high pressure device produces, the other end is connected respectively to 4 sides in high temperature high pressure device and presses on anvils, insulate with ceramic pipe (9) at the intersection of copper wire (4) and graphite-pipe (3); 4 side pressure anvils are got the first pressure anvil and second in order and are pressed anvil to be connected in series direct supply and reometer, and the 3rd pressure anvil is connected voltage table with the 4th pressure anvil;
Described thermopair (10), a pair thermopair is placed on the upper surface of sample (5), another is placed on the lower surface of sample (5) to thermopair, the pad of two pairs of thermopairs (10) is placed on the circle centre position of sample (5), insulate with ceramic pipe (9) at the intersection of thermopair (10) and graphite-pipe (3), thermopair (10) adopts NiCr-NiAl thermopair, the positive pole NiCr of two thermopairs to be connected in high temperature high pressure device on two adjacent side pressure anvils, the negative pole NiAl of two thermopairs to be connected in high temperature high pressure device on another two adjacent side pressure anvils, during detection 4 sides pressure anvil respectively with the Instrument connection measuring electric potential difference, the upper surface of sample (5) or lower surface are by the center of assembled block.
2. the method for in-situ test conductive species resistivity under High Temperature High Pressure, is characterized in that, utilizes the device of in-situ test conductive species transport property under the High Temperature High Pressure of claim 1 to measure; First assembled block is put into cubic hinge press, by pyrophyllite block (8), sample (5) is pressurizeed; Upper and lower two pressure anvils are connected heating power supply and are heated sample by graphite flake (2) and graphite-pipe (3), reach detected pressures and the detected temperatures of sample; 4 side pressure anvils are got the first pressure anvil and second in order and are pressed anvil to be connected in series direct supply and reometer, and the 3rd pressure anvil is connected voltage table with the 4th pressure anvil, records I
1and V
1, then get the second pressure anvil and the 3rd and press anvil to be connected in series direct supply and reometer, the first pressure anvil and the 4th pressure anvil are connected voltage table, record I
2and V
2; According to formula
exp(-πR
Ad/ρ)+exp(-πR
Bd/ρ)＝1
Calculate electricalresistivityρ, wherein R
a=V
1/ I
1, R
b=V
2/ I
2, d is thickness of sample after pressurization.
3. the method for in-situ test conductive species Seebeck coefficient under High Temperature High Pressure, is characterized in that, utilizes the device of in-situ test conductive species transport property under the High Temperature High Pressure of claim 1 to measure; First assembled block is put into cubic hinge press, by pyrophyllite block (8), sample (5) is pressurizeed, upper and lower two pressure anvils are connected heating power supply and are heated sample (5) by graphite flake (2) and graphite-pipe (3), reach detected pressures and the detected temperatures of sample; Measure the electric potential difference V of the positive interpolar of two pairs of thermopairs
efand the electric potential difference V between negative pole
hg, then the Seebeck coefficient S=S of sample (5)
--[V
ef(S
--S
+)/(V
ef-V
hg)], wherein S
+, S
-be respectively the Seebeck coefficient of thermopair positive pole, negative pole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310323217.1A CN103399044B (en) | 2013-07-29 | 2013-07-29 | The apparatus and method of in-situ test conductive species transport property under High Temperature High Pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310323217.1A CN103399044B (en) | 2013-07-29 | 2013-07-29 | The apparatus and method of in-situ test conductive species transport property under High Temperature High Pressure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103399044A CN103399044A (en) | 2013-11-20 |
| CN103399044B true CN103399044B (en) | 2015-11-18 |
Family
ID=49562708
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310323217.1A Expired - Fee Related CN103399044B (en) | 2013-07-29 | 2013-07-29 | The apparatus and method of in-situ test conductive species transport property under High Temperature High Pressure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103399044B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104777193B (en) * | 2015-04-13 | 2017-07-18 | 清华大学 | Transport property measurement apparatus in situ |
| CN106908309B (en) * | 2017-01-25 | 2020-01-10 | 吉林炭素有限公司 | Nondestructive testing method for flexural strength of graphite electrode and joint thereof |
| DE102017105317B3 (en) | 2017-03-14 | 2018-05-09 | Helmholtz-Zentrum Dresden - Rossendorf E.V. | Device for characterizing the electrical resistance of a test object |
| CN107290221B (en) * | 2017-06-02 | 2023-08-04 | 中国工程物理研究院核物理与化学研究所 | High-temperature high-pressure loading device for in-situ neutron diffraction |
| CN107765161A (en) * | 2017-10-13 | 2018-03-06 | 中国科学院地球化学研究所 | A kind of method of diamond anvil cell situ measurement conducting material thermoelectricity performance |
| CN108267237B (en) * | 2017-12-04 | 2021-10-08 | 郑州中南杰特超硬材料有限公司 | Method for measuring synthesis temperature of superhard material |
| CN108761172B (en) * | 2018-07-30 | 2020-05-01 | 珠海市运泰利自动化设备有限公司 | High-precision measurement method for Seebeck coefficient of thermoelectric material |
| CN110596564A (en) * | 2019-10-21 | 2019-12-20 | 山东大学 | Multipurpose photoelectric performance combined in-situ test pool and application thereof |
| CN112147414B (en) * | 2020-09-27 | 2021-10-01 | 中国科学院地球化学研究所 | Method for measuring resistivity of metallic iron under ultrahigh pressure |
| CN113267683B (en) * | 2021-05-07 | 2023-05-12 | 武汉理工大学 | In-situ measurement method for metal resistivity at high temperature and high pressure |
| CN115877089A (en) * | 2021-08-24 | 2023-03-31 | 中国科学院地球化学研究所 | Impedance spectrum in-situ measurement method for dielectric constant of solid material under high-temperature and high-pressure conditions |
| CN115041096B (en) * | 2022-06-07 | 2023-08-15 | 中国工程物理研究院核物理与化学研究所 | High-temperature high-pressure device of two-sided press |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101007251A (en) * | 2006-01-23 | 2007-08-01 | 郑州人造金刚石及制品工程技术研究中心 | Outer indirect heating diamond synthesis block |
| RU2356615C1 (en) * | 2008-01-29 | 2009-05-27 | Альберт Павлович Новиков | Multiple-punch high-pressure apparatus for making diamonds |
| US7540075B2 (en) * | 2004-01-13 | 2009-06-02 | Chien-Min Sung | Method of applying high pressures to a high pressure assembly |
-
2013
- 2013-07-29 CN CN201310323217.1A patent/CN103399044B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7540075B2 (en) * | 2004-01-13 | 2009-06-02 | Chien-Min Sung | Method of applying high pressures to a high pressure assembly |
| CN101007251A (en) * | 2006-01-23 | 2007-08-01 | 郑州人造金刚石及制品工程技术研究中心 | Outer indirect heating diamond synthesis block |
| RU2356615C1 (en) * | 2008-01-29 | 2009-05-27 | Альберт Павлович Новиков | Multiple-punch high-pressure apparatus for making diamonds |
Non-Patent Citations (3)
| Title |
|---|
| 二硼化钛的高温高压制备及其物性;黎军军等;《物理学报》;20121211;第62卷(第2期);全文 * |
| 利用范德堡法在金刚石对顶砧中精确测量样品电阻率;吴宝嘉等;《吉林大学学报(理学版)》;20080930;第46卷(第5期);第957页第1-4段、图1 * |
| 高性能热电材料的高温高压合成;宿太超;《中国博士学位论文 基础科技辑》;20090815(第8期);第35、37、38、44和45页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103399044A (en) | 2013-11-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103399044B (en) | The apparatus and method of in-situ test conductive species transport property under High Temperature High Pressure | |
| Shi et al. | A novel self-powered wireless temperature sensor based on thermoelectric generators | |
| CN107607849B (en) | Thermoelectric device power generation performance testing device and method | |
| CN105203940B (en) | A kind of thermoelectric element reliability evaluation system and method | |
| CN201903526U (en) | Conductivity and Seebeck coefficient test device for semiconductor film materials at low temperatures | |
| CN105425026A (en) | Novel sealed constant-temperature double-load waveguide calorimeter | |
| CN103323780A (en) | Thermoelectric material thermoelectric conversion performance testing system and method | |
| CN105548857A (en) | Thermoelectricity module group generation performance test platform | |
| KR20150007686A (en) | Thermoelectric property measurement system | |
| CN107565011A (en) | The method that PbTe thermoelectricity capabilities are effectively improved based on Ga element dopings | |
| CN202853845U (en) | Pressure sensor temperature characteristic test device | |
| CN107037264A (en) | Pyroelectric material performance parameter measuring apparatus and measuring method | |
| CN206038785U (en) | Testing arrangement of thermoelectric module thermoelectric conversion efficiency | |
| Luo et al. | Realizing ultrahigh ZT value and efficiency of the Bi2Te3 thermoelectric module by periodic heating | |
| CN102865969B (en) | Pressure sensor temperature characteristic testing device | |
| CN103323284A (en) | Thermoelectric refrigeration performance measuring device and method | |
| CN103472318A (en) | Direct-current cable space charge measuring system | |
| CN107727951A (en) | A kind of thermo-electric generation monomer module thermoelectricity capability test table | |
| CN102891248B (en) | Flexible thermoelectric conversion system and manufacturing method thereof | |
| CN110530927A (en) | A kind of thermoelectric material Seebeck coefficient test device and method | |
| CN103336024B (en) | The thermoelectricity capability test system of thermoelectric material | |
| CN104359574A (en) | Fuel cell internal temperature-heat flux synchronous measurement sensor | |
| CN209878636U (en) | Thermoelectric parameter testing device | |
| CN102735891B (en) | A kind of temperature difference micro battery being applied to the electric device measuring of superconduction | |
| CN102759665A (en) | Device for detecting alternating-current resistance of high-pressure cable split conductor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151118 Termination date: 20160729 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |