CN103399044A - Device and method for carrying out in-situ testing on transport properties of conductor materials at high temperature and high pressure - Google Patents
Device and method for carrying out in-situ testing on transport properties of conductor materials at high temperature and high pressure Download PDFInfo
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Abstract
The invention discloses a device and a method for carrying out in-situ testing on the transport properties of conductor materials at high temperature and high pressure, and belongs to the field of high-pressure science and technologies and material science technologies. In the device, four copper wires (4) are introduced to a side face of a high-temperature and high-pressure synthetic assembling block and used as electrodes for measuring the resistivity, two pairs of thermocouples (10) are introduced for measuring seebeck coefficients, and welding points of a sample (5) and the electrodes as well as the sample (5) and the thermocouples (10) are fixed by using a pressure generated by a high-temperature and high-pressure device. The resistivity of the sample is calculated through measuring relative resistance values RA and RB and the thickness d of the sample subjected to pressurization; the seebeck coefficient of the sample is calculated through measuring a potential difference Vef between positive poles of the two pairs of thermocouples and a potential difference Vhg between negative poles of the two pairs of thermocouples. The method disclosed by the invention is simple, easy to implement, high in success rate, and good in experimental repetition rate; a problem that wires and the thermocouples are easy to fracture at the high pressure is solved; a situation that measured electrical signals are interfered by heating current is prevented, thereby ensuring the accuracy of results.
Description
Technical field
The invention belongs to the field of high-pressure science technology and material science and technology, particularly a kind of conductor material original position transport property under High Temperature High Pressure---the technology of electronic transport (conductivity) and thermotransport (Seebeck coefficient) in-situ test.Purpose is the operation interval of finding high performance thermoelectric material and finding out its thermoelectricity capability the best.
Background technology
Along with the increase of pressure, the electric conductivity of conductor material increases.Especially semiconductor material, its Bands gap reduces along with the increase of pressure, thereby strengthens its electric conductivity.In addition, temperature effect has very important impact to the Bands gap of semiconductor material too.Generally speaking, the Bands gap of semiconductor material reduces along with the increase of temperature.In semiconductor material,, due to charge carrier occurs under thermograde electric potential difference, be an important parameter of reaction material thermoelectricity capability.
Thermoelectric material is a kind of functional material that heat energy and electric energy are directly transformed mutually, can realize utilizing directly refrigeration or with the function of the heat energy direct generation of electricity of electric energy.By the thermo-electric device of thermoelectric material preparation have pollution-free, volume is little, lightweight, be convenient for carrying, the advantage such as long service life, make it in a lot of fields, be applied, cooling etc. such as cooling, the high power laser of portable refrigerator, generator, high speed lsi and infrared eye.Although thermo-electric device has the incomparable advantage of conventional electrical equipment, its transformation efficiency low so limited its application.Find high performance thermoelectric material is the direction that people make great efforts always.Known high performance thermoelectric material is nearly all semiconductor material at present.
As previously mentioned, pressure and temperature all can be modulated the energy gap width of material (especially semiconductor material), the electric conductivity of reinforcing material.Yet how in real time there are huge technical barrier in detected pressures and temperature to the variation of material transport property.Because it is very complicated carrying out the related experiment technology of in-situ test under High Temperature High Pressure.Be not only because need to arrange the loop of transport property test in the High Temperature High Pressure cavity, also need to design the required thermograde of generation thermotransport property detection in material to be measured in high-pressure chamber.Therefore, in the present home position testing method of reporting, be mainly the conductivity test of under high pressure carrying out, the device of employing is mainly also at diamond anvil cell.And utilize large high-pressure chamber multiface upsetting machine, the resistivity of in site measurement material and Seebeck coefficient rarely have report under High Temperature High Pressure.
The principle of thermoelectric effect: temperature difference produces electric potential difference, and Seebeck coefficient S definition is S=Δ V/ Δ T.Measure the temperature difference at sample two ends and the Seebeck coefficient that electric potential difference can be obtained sample according to definition.The method that the measurement of temperature difference is usually adopted the differential thermocouple method and with standard substance, compared, but this method measuring error is larger, and sample is subjected to 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 to adopt new method to measure resistivity and the Seebeck coefficient of conductive material under High Temperature High Pressure.The method is compared with additive method has characteristics simple to operate, that success ratio is high, error is little, main by using new experimental technique to change the layout of test circuit, wire and thermopair can accurately be located be not easy occurrence positions under High Pressure and move and rupture, thereby guaranteed 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 electronic transport character in-situ test is that resistivity and the Seebeck coefficient of conductive materials are tested.
Test experiments carries out under High Temperature High Pressure, so will make the environment of High Temperature High Pressure.Test experiments of the present invention is completed 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 to press anvil extruding pressure transmitting medium, forms the simulated hollow high pressure chest of sealing in pressure transmitting medium, produces thus high pressure.The generation principle of high temperature is: heating system, pressure anvil, steel cap, graphite flake, graphite-pipe form an electricity loop, heating system is from pressing the anvil input current, graphite flake and graphite-pipe have electric current to pass through and will generate heat, heat spreads to the high-pressure chamber center by insulation course, thereby produces high temperature in seal chamber.This type of type of heating is heater-type.During this experiment High Temperature High Pressure used was assembled, pressure transmitting medium was pyrophillite, and heating resistor is graphite-pipe, and insulating material is magnesia tube and oxidation magnesium sheet (seeing accompanying drawing 1 for details).
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 laminar, and fixing thickness is arranged, uniformly resistivity (not allowed cavity in sample).At first need sample is prepared as laminar, meet the test request of the method.Under High Temperature High Pressure, the resistivity measurement loop is divided into as inner looping (under high-temperature and high-pressure conditions) and external loop (condition of normal pressure).Inner looping is concrete connect as follows: four wires on cloth on surface of laminar sample, the pressure fixing that produces by high-tension unit that contacts of wire and sample.The contact point of wire and sample is positioned at the edge of sample and enough little.The wire of these four test loops passes the aperture in High Temperature High Pressure pressure transmission sealing medium, at the intersection of thermopair and graphite-pipe, with ceramic pipe, insulate, and is connected to finally on the pressure anvil in high temperature high pressure device, forms the build-in test loop.The pressure anvil of outer test loop line and high-tension unit is connected to form test loop.Press the electrode of anvil as the electric current input and output for wherein two, two other presses the electrode of anvil as measuring voltage.Select suitable steady current input, measure magnitude of voltage, according to formula, calculate resistivity.
The present invention adopts round-about way to need not to measure the temperature difference can obtain the Seebeck coefficient of sample equally.Under High Temperature High Pressure, the Seebeck coefficient test loop is similar to the resistivity measurement loop, also is divided into inner looping (under high-temperature and high-pressure conditions) and external loop (condition of normal pressure).The concrete connection of inner looping is as follows: a pair of 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 the pressure fixing that produces by high-tension unit with contacting of sample equally.These two pairs of thermopairs pass the aperture in High Temperature High Pressure pressure transmission sealing medium, at the intersection of thermopair and graphite-pipe,, equally with the ceramic pipe insulation, are connected to finally on the pressure anvil in high temperature high pressure device, form the build-in test loop.External loop is will press anvil and multimeter to be connected to form with wire.Measure respectively two pairs of thermopairs anodal and anodal, the electric potential difference between negative pole and negative pole, the substitution formula calculates Seebeck coefficient.
Under High Temperature High Pressure of the present invention, the concrete technical scheme of in-situ test conductor transport of substances character device is as described below.
The device of in-situ test conductor transport of substances character under a kind of High Temperature High Pressure, structure has the assembled block of the high temperature high pressure device put into, and assembled block is by pyrophillite 8 as pressure transmitting medium, and the interior order of pyrophyllite block 8 is equipped with cylindrical shape graphite-pipe 3 and magnesium oxide insulated pipe 6; The disc sample 5 of packing in magnesium oxide insulated pipe 6, sample 5 top and bottom are equipped with respectively oxidation magnesium sheet 7 and graphite flake 2 in turn, graphite flake 2 forms hollow cylinder as heating resistor with graphite-pipe 3, 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 1 shutoff of steel cap; It is characterized in that, in the side of assembled block, by aperture, introduce 4 copper wires 4 as the electrode of measuring sample 5 resistivity, introduce two pairs of thermopairs 10 as the Seebeck coefficient of measuring sample 5;
The contact point of described copper wire 4 one ends is separately positioned on the edge of sample quadrant position, the pressure fixing that produces by high temperature high pressure device, the other end is connected respectively to 4 sides in high temperature high pressure device and presses on anvil, in ceramic pipe 9 insulation of the intersection of copper wire 4 and graphite-pipe 3; Press anvil to be connected with direct supply, the voltage table of serial connection reometer respectively for 4 during detection;
Described thermopair 10, a pair of 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, intersection at thermopair 10 and graphite-pipe 3 insulate with ceramic pipe 9, and the termination of two pairs of thermopairs is connected respectively to 4 sides in high temperature high pressure device and presses on anvil; During detection 4 sides press anvil respectively with the Instrument connection of 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 conductor transport of substances character, described thermopair 10, can be the NiCr-NiAl thermopair under High Temperature High Pressure; The anodal 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 conductor transport of substances character under High Temperature High Pressure, the method for in-situ test conductor transport of substances character has the method for testing of conductor material resistivity and the method for testing of conductor material Seebeck coefficient.Concrete measuring technology scheme is as described below.
A kind of method of in-situ test conductor material resistivity under High Temperature High Pressure, utilize the device of in-situ test conductor transport of substances character under aforesaid High Temperature High Pressure to measure; At first assembled block is put into cubic hinge press, by 5 pressurizations of 8 pairs of samples of pyrophyllite block; Two of up and down press anvil to connect heating power supply by 3 pairs of sample heating of graphite flake 2 and graphite-pipe, reach detected pressures and the detected temperatures of sample; 4 sides pressure anvils are got in order first and are pressed anvil and second to press anvil to be connected in series direct supply and reometer, and the 3rd presses anvil and the 4th to press anvil connection voltage table, records I
1And V
1, then get second and press anvil and the 3rd to press anvil to be connected in series direct supply and reometer, first presses anvil and the 4th to press anvil to connect voltage table, records I
2And V
2According to formula
exp（-πR
Ad/ρ)+exp(-πR
Bd/ρ)=1
Calculate the electricalresistivityρ, wherein R
A=V
1/ I
1, R
B=V
2/ I
2, d, for the rear thickness of sample of pressurization, measures after being taken out from high-pressure chamber by sample.
A kind of method of in-situ test conductor material Seebeck coefficient under High Temperature High Pressure, utilize the device of in-situ test conductor transport of substances character under aforesaid High Temperature High Pressure to measure; At first assembled block is put into cubic hinge press, by 5 pressurizations of 8 pairs of samples of pyrophyllite block, two of up and down press anvil to connect heating power supply by graphite flake 2 and 5 heating of 3 pairs of samples of graphite-pipe, 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, the Seebeck coefficient S=S of sample 5
--[V
ef(S
--S
+)/(V
ef-V
hg)], S wherein
+, S
-Be respectively the Seebeck coefficient of thermopair positive pole, negative pole.
Experiment shows: the inventive method is simple, and is easy to implement, and success ratio is high, and the experiment repetition rate is good; Solved the problem that wire and thermopair under high pressure easily rupture; The insulation that has guaranteed wire and thermopair prevents that the electric signal of measuring is subject to the interference for heating current, guarantees the accuracy of result.Compare with the 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 the cavity type of heating to control temperature difference carries out the Seebeck coefficient test, adopts round-about way to need not to measure the temperature difference and can obtain equally the Seebeck coefficient etc. of sample.This method of testing is not only applicable to thermoelectric material, also is applicable to test resistivity and the Seebeck coefficient of other conductive materials.
Description of drawings
Fig. 1 is that the present invention tests the assembled block longitudinal diagram.
Fig. 2 is that the present invention tests the assembled block drawing in side sectional elevation.
Fig. 3 is that embodiment 4 maintenance pressure are that 3GPa is constant, β-Ag
2Te resistivity variation with temperature curve.
Fig. 4 is that embodiment 5 maintenance temperature are that 520K is constant, β-Ag
2Te resistivity is with the change curve of pressure.
Fig. 5 is that embodiment 6 maintenance pressure are that 3GPa is constant, β-Ag
2Te Seebeck coefficient variation with temperature curve.
Fig. 6 is that embodiment 7 maintenance temperature are that 520K is constant, β-Ag
2The Te Seebeck coefficient is with the change curve of pressure.
Embodiment
Following examples are all completed on domestic DS029B type cubic hinge press, and with Ag
2Te is specimen.
Under High Temperature High Pressure, the apparatus structure of in-situ test conductor transport of substances character is provided by Fig. 1 and Fig. 2.In Fig. 1 and Fig. 2,1 is the steel cap, and 2 is graphite flake, and 3 is graphite-pipe, 4 are copper wire (amount to 4 copper wires and count respectively a, b, c, d), 5 is sample, and 6 is the MgO insulation tube, and 7 is the MgO insulating trip, 8 is pyrophyllite block, 9 is ceramic pipe, and 10 are thermopair (two pairs of thermopairs can all be selected the NiCr-NiAl thermopair, and e, h are that positive pole and negative pole f, the g of a pair of thermopair is another positive pole to thermopair and negative pole).
Shown in Fig. 1,2, the assembled block synthetic with general High Temperature High Pressure is the same, the assembled block sidewall consists of pyrophyllite block 8, graphite-pipe 3, MgO insulation tube 6, the assembled block two ends are by MgO insulating trip 7, graphite flake 2 and 1 shutoff of steel cap, space in graphite-pipe 3 and up and down two graphite flakes 2 sample 5 of packing into, graphite-pipe 3 and graphite flake 2 press anvil to be electrically connected to as two of heating resistor and up and down, press anvil to connect power supply for two and are used to sample 5 heating.Be drilled with eight holes on four sides of pyrophyllite block 8, and the graphite-pipe 3 corresponding with hole site, MgO insulation tube 6 places hole respectively, that is, each hole penetrates pyrophyllite block 8, graphite-pipe 3 and MgO insulation tube 6.Respectively with a, b, c, d place in copper wire 4(Fig. 2) and NiCr-NiAl thermopair 10(Fig. 2 in e, f, g, h place) pass pyrophyllite block 8, graphite-pipe 3 and MgO insulation tube 6 by aperture respectively, with copper wire 4, the wire that connects thermopair 10 and graphite-pipe 3 insulation, ceramic pipe 9 can be Al with eight ceramic pipes 9
2O
3Material.The sample 5 of disc is put into height be pressed into piece, copper wire 4 is pressed close to sample 5(such as β-Ag
2Te) edge is placed; Center with a pair of NiCr-NiAl thermopair 10 by cavity is the upper surface (seeing Fig. 2 solid line eh) of sample, and another is placed on the lower surface (seeing Fig. 2 dotted line fg) of sample to NiCr-NiAl thermopair 10, and (ef is NiCr, the positive pole of thermopair; Gh is NiAl, the negative pole of thermopair), the pad of two pairs of thermopairs, all in the center of sample, is fixed wire and thermopair by the pressure that high-tension unit produces.
The assembled block that height is pressed into assembles by the structure (being the structure of assembled block shown in Fig. 1,2) of embodiment 1, puts into press.Pressing 4 sides anvils to be connected measurement instrument with direct supply with wire connects.Set pressure and temperature, bring into operation, start heating after press is raised to set pressure.Temperature constant (temperature constant after generally heating ten minutes) until the cavity center starts to carry out resistivity measurement.
Referring to Fig. 2, electric current I
abFlow into b from a and flow out, at d, c place, measure voltage drop V
dc, note relative resistance value R
A=V
dc/ I
abElectric current I
bcFlow into c from b and flow out, at a, d place, record voltage drop V
ad, note relative resistance value R
B=V
ad/ I
bcThe pass between sample resistivity ρ, thickness of sample d and relative resistance value is:
Exp (π R
AD/ ρ)+exp (π (
BD/ ρ)=1 calculates resistivity with the above-mentioned formula of measurement data substitution.
The assembled block that height is pressed into assembles by the structure (being the structure of assembled block shown in Fig. 1,2) of embodiment 1, puts into press, and wherein the upper surface of sample 5 or lower surface are by the center of assembled block.With wire, 4 sides are pressed the Instrument connection of anvil and measurement electric potential difference.Set pressure and temperature, bring into operation, start heating after press is raised to set pressure, heat after ten minutes and treat the temperature constant at cavity center, start to carry out Seebeck coefficient and measure.
, referring to Fig. 2, measure respectively the electric potential difference V of the positive interpolar of two pairs of thermopairs
efAnd the electric potential difference V between negative pole
hgAccording 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)].S wherein
NiCr, S
NiAlBe respectively the Seebeck coefficient of thermopair both positive and negative polarity, its value is known.Above data substitution formula is calculated Seebeck coefficient.
Embodiment 4
Adopt the device of embodiment 1, namely the synthetic assembled block of the High Temperature High Pressure shown in Fig. 1,2, select β-Ag
2The Te material is made sample 5, and assembled block is put into the hexahedron top press high-pressure cavity.In cavity, pressure is raised to 3Gpa, carries out pressurize.Ascending adjusting heating power, rise to each design temperature point successively, and allow respectively the interior temperature of cavity reach stable.Press 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 calculated resistance rate (d is the thickness of sample after pressurization, according to measuring accuracy, requires to use vernier caliper or milscale etc. directly to measure).Concrete β-Ag
2Te resistivity variation with temperature relation is seen Fig. 3.
Adopt the device of embodiment 1, namely the synthetic assembled block of the High Temperature High Pressure shown in Fig. 1,2, select β-Ag
2The Te material is made sample 5, and assembled block is put into the hexahedron top press high-pressure cavity.In cavity, temperature rises to 520K, is incubated.Ascending adjusting pressure, rise to each set pressure point successively, and pressurize allowed cavity internal pressure stable in ten minutes.Measure resistance value R under each pressure 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 calculated resistance rate (d for pressurization after the thickness of sample).Concrete β-Ag
2Te resistivity is seen Fig. 4 with the variation relation of pressure.
Adopt the device of embodiment 1, namely the synthetic assembled block of the High Temperature High Pressure shown in Fig. 1,2, select β-Ag
2The Te material is made sample 5, and the upper surface of sample 5 is by the center of assembled block, and assembled block is put into the hexahedron top press high-pressure cavity.In cavity, pressure is raised to 3Gpa, carries out pressurize.Ascending adjusting heating power, rise to each design temperature point successively, heats and allowed the interior temperature of cavity reach stable in ten minutes.Press the electrically connected method of embodiment 3 and the electric potential difference V that test process is measured the positive interpolar of two pairs of thermopairs at each temperature
efAnd the electric potential difference V between negative pole
hgAccording 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 seen Fig. 5.
Adopt the device of embodiment 1, namely the synthetic assembled block of the High Temperature High Pressure shown in Fig. 1,2, select β-Ag
2The Te material is made sample 5, and the upper surface of sample 5 is by the center of assembled block, and assembled block is put into the hexahedron top press high-pressure cavity.In cavity, temperature rises to 520K, is incubated.Ascending adjusting pressure, rise to each set pressure point successively, and pressurize allowed cavity internal pressure stable in ten minutes.The electric potential difference V that measures the positive interpolar of two pairs of thermopairs under each pressure by electrically connected method and the test process of embodiment 3
efAnd the electric potential difference V between negative pole
hgAccording to formula S=S
NiAl-[V
ef(S
NiAl-S
NiCr)/(V
ef-V
hg)] calculate Seebeck coefficient.Concrete β-Ag
2The Te Seebeck coefficient is seen Fig. 6 with the variation relation of pressure.
Claims (4)
1. the device of in-situ test conductor transport of substances character under a High Temperature High Pressure, structure has the assembled block of the high temperature high pressure device put into, 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); The disc sample (5) of packing in magnesium oxide insulated pipe (6), sample (5) top and bottom are equipped with respectively oxidation magnesium sheet (7) and graphite flake (2) in turn, graphite flake (2) forms hollow cylinder as heating resistor with graphite-pipe (3), 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, in the side of assembled block, by aperture, introduce 4 copper wires (4) as the electrode of measuring sample (5) resistance, introduce two pairs of thermopairs (10) as the Seebeck coefficient of measuring sample (5);
The contact point of described copper wire (4) one ends is separately positioned on the edge of sample quadrant position, the pressure fixing that produces by high temperature high pressure device, the other end is connected respectively to 4 sides in high temperature high pressure device and presses on anvil, in ceramic pipe (9) insulation of the intersection of copper wire (4) and graphite-pipe (3); Press anvil to be connected with direct supply, the voltage table of serial connection reometer respectively for 4 during detection;
Described thermopair (10), a pair of 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), intersection at thermopair (10) and graphite-pipe (3) insulate with ceramic pipe (9), and the termination of two pairs of thermopairs is connected respectively to 4 sides in high temperature high pressure device and presses on anvil; During detection 4 sides press anvil respectively with the Instrument connection of measuring electric potential difference, the upper surface of sample (5) or lower surface are by the center of assembled block.
2. the device of in-situ test conductor transport of substances character under High Temperature High Pressure according to claim 1, is characterized in that described thermopair (10) is the NiCr-NiAl thermopair; The anodal 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.
3. the method for in-situ test conductor material resistivity under a High Temperature High Pressure, is characterized in that, utilizes the device of in-situ test conductor transport of substances character under the High Temperature High Pressure of claim 1 to measure; At first assembled block is put into cubic hinge press, by pyrophyllite block (8), sample (5) is pressurizeed; Press anvil connection heating power supply by graphite flake (2) and graphite-pipe (3), sample to be heated for two up and down, reach detected pressures and the detected temperatures of sample; 4 sides pressure anvils are got in order first and are pressed anvil and second to press anvil to be connected in series direct supply and reometer, and the 3rd presses anvil and the 4th to press anvil connection voltage table, records I
1And V
1, then get second and press anvil and the 3rd to press anvil to be connected in series direct supply and reometer, first presses anvil and the 4th to press anvil to connect voltage table, records I
2And V
2According to formula
exp(-πR
Ad/ρ)+exp(-πR
Bd/ρ)=1
Calculate the electricalresistivityρ, wherein R
A=V
1/ I
1, R
B=V
2/ I
2, d is the rear thickness of sample of pressurization.
4. the method for in-situ test conductor material Seebeck coefficient under a High Temperature High Pressure, is characterized in that, utilizes the device of in-situ test conductor transport of substances character under the High Temperature High Pressure of claim 1 to measure; At first assembled block is put into cubic hinge press, by pyrophyllite block (8), sample (5) is pressurizeed, press anvil connection heating power supply by graphite flake (2) and graphite-pipe (3), sample (5) to be heated for two up and down, 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, the Seebeck coefficient S=S of sample 5
--[V
ef(S
--S
+)/(V
ef-V
hg)], S wherein
+, S
-Be respectively the Seebeck coefficient of thermopair positive pole, negative pole.
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| CN113640586A (en) * | 2021-08-24 | 2021-11-12 | 中国科学院地球化学研究所 | Impedance spectrum in-situ measurement device and method for dielectric constant of solid material under high-temperature and high-pressure conditions |
| CN115041096A (en) * | 2022-06-07 | 2022-09-13 | 中国工程物理研究院核物理与化学研究所 | High-temperature and high-pressure device of double-sided jacking machine |
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 |
|---|
| 吴宝嘉等: "利用范德堡法在金刚石对顶砧中精确测量样品电阻率", 《吉林大学学报(理学版)》, vol. 46, no. 5, 30 September 2008 (2008-09-30), pages 956 - 958 * |
| 宿太超: "高性能热电材料的高温高压合成", 《中国博士学位论文 基础科技辑》, no. 8, 15 August 2009 (2009-08-15) * |
| 黎军军等: "二硼化钛的高温高压制备及其物性", 《物理学报》, vol. 62, no. 2, 11 December 2012 (2012-12-11) * |
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