CN102655204A - Sr-doping oxide BiCuSeO thermoelectric material and preparation method thereof - Google Patents
Sr-doping oxide BiCuSeO thermoelectric material and preparation method thereof Download PDFInfo
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- CN102655204A CN102655204A CN2012101324297A CN201210132429A CN102655204A CN 102655204 A CN102655204 A CN 102655204A CN 2012101324297 A CN2012101324297 A CN 2012101324297A CN 201210132429 A CN201210132429 A CN 201210132429A CN 102655204 A CN102655204 A CN 102655204A
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- 239000000463 material Substances 0.000 title claims abstract description 82
- 229910002903 BiCuSeO Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 46
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 18
- 230000014759 maintenance of location Effects 0.000 claims description 12
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Inorganic materials [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 11
- 238000012856 packing Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000003746 solid phase reaction Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- 238000007599 discharging Methods 0.000 abstract 2
- 230000005520 electrodynamics Effects 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 239000007790 solid phase Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000005619 thermoelectricity Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000003708 ampul Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010671 solid-state reaction Methods 0.000 description 2
- 229910016339 Bi—Sb—Te Inorganic materials 0.000 description 1
- 229910005900 GeTe Inorganic materials 0.000 description 1
- 229910018321 SbTe Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
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- 239000012071 phase Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a Sr-doping oxide BiCuSeO thermoelectric material and a preparation method of the Sr-doping oxide BiCuSeO thermoelectric material, belonging to the technical field of new energy source materials. The preparation method comprises the following steps of ball-milling material mixing, solid-phase sintering, ball-milling refining, and discharging plasma sintering, and specifically comprises the following steps of: mixing Bi2O3 with the purity of 99.99%, SrO with the purity of 99.99%, Cu with the purity of 99.99%, Se with the purity of 99.99% and Bi with the purity of 99.99% according to a stoichiometric ratio, uniformly mixing in a ball milling manner, carrying out cold-pressing, carrying out a solid-phase reaction, pulverizing in the ball milling manner, and then carrying out the discharging plasma sintering to prepare Bi1-xSrxCuSeOoxide block bodies (x=0-0.125). Compared with other oxide thermoelectric materials, the Sr-doping oxide BiCuSeO thermoelectric material disclosed by the invention has the advantages of high conductivity, high temperature-difference electrodynamic potential, low thermal conductivity and the like; and the preparation method has the advantages of simple and convenient process, short synthesis and formation times and the like.
Description
Technical field
The invention belongs to the new energy materials technical field, particularly relate to a kind of Sr doping oxide BiCuSeO thermoelectric material and preparation method, relate to ball milling, solid phase reaction and discharge plasma sintering process.
Background technology
Thermoelectric material be a kind of can be with electric energy and the heat energy direct energy and material of conversion each other.The remarkable advantage of thermoelectric material is a kind of eco-friendly green energy resource material of noiselessness, pollution-free, movement-less part.An important performance indexes weighing thermoelectric material is exactly a thermoelectric figure of merit.Thermoelectricity comprises thermoelectric cooling and two phenomenons of thermo-electric generation, and generated output and refrigerating efficiency and thermoelectric figure of merit are proportional.To a certain material, its thermoelectricity capability figure of merit is provided by following formula: ZT=α
2σ T/ κ, wherein α is the thermoelectric power (Seebeck coefficient) of material, and σ is a conductivity of electrolyte materials, and κ is a thermal conductivity, and T is absolute temperature [G.J.Snyder, and E.S.Toberer, Nature Mater.7,105 (2008)].The dimensionless thermoelectric figure of merit of present most of thermoelectric materials is about " 1 ", and conversion efficiency of thermoelectric is about 1/3 of diesel engine generator generating efficiency about 10%, if thermoelectric figure of merit can reach about " 3 ", thermoelectric power generation will replace diesel generation to dominate the market.But the good thermoelectric material of using at present of performance all contains heavy metal element, and costs an arm and a leg.Like the Bi-Sb-Te alloy [B.Poudel, et al.Science 320,634 (2008)] of nanostructure, ancient ore deposit, filling side [A.Harnwunggmoung, et al.Appl.Phys.Lett.96,202107 (2010)], AgPb
18+xSbTe
20System [K.F.Hsu, et al.Science 303,818 (2004)], (AgSbTe
2)
1-x(GeTe)
xAlloy [B.A.Cook, et al.J.Appl.Phys.101,053715 (2007)], In4Se
3Alloy [J.Rhyee, et al.Nature (London) 459,965 (2009)] etc.Compare with these materials, oxide pyroelectric material has high-temperature stability, and advantages such as low price receive much concern, yet oxide pyroelectric material ubiquity conductivity is bad, and thermal conductivity is high, causes the dimensionless thermoelectric figure of merit generally not high, like Zn
0.96Al
0.02Ga
0.02The ZT value of O oxide under the 1247K temperature is 0.65 [D.Berardan, et al.Solid State Comm.146,97 (2008)], In
1.8Ge
0.2O
3The ZT value of oxide under the 1273K temperature is 0.45 [M.Ohtaki, et al.J.Electron.Mater.38,1234 (2009)], yet these oxides can't be compared with traditional alloy phase on using.
Summary of the invention
The object of the present invention is to provide a kind of Sr doping oxide BiCuSeO thermoelectric material and preparation method, the present invention is with Bi
2O
3, SrO, Cu, Se and Bi powder be as initial feed, colds pressing through after mixing, and adopts solid-state reaction, ball milling and discharge plasma sintering prepare Sr doping BiCuSeO oxide pyroelectric material.
Concrete technological process is following:
(1), adopts Bi
2O
3, SrO, Cu, Se and Bi powder be as initial feed, presses Bi
2O
3: SrO: Cu: Se: Bi=(1/3-x): x: 1: 1: [1-2* (1/3-x)] atomic ratio batching.Wherein x=0.025～0.125 is preferred, x=0.023～0.075.
(2), raw material put into ball grinder evenly mix, rotational speed of ball-mill is 100～500rpm, the time is 15min～96h.Preferably, the ball milling time is 1～50h.
(3), with the powder that mixes, cold pressing, pressure is 100～250MPa, is pressed into disk.
(4), with the disk after the cold moudling, be placed on and carry out sintering in the quartz ampoule, sintering temperature is 300～700 ℃, temperature retention time is 48～240 hours, programming rate be 40～180 ℃ per hour, obtaining diameter is 10～20mm, highly is the Bi of 4～6mm
1-xSr
xCuSeO (x=0.025～0.125) block materials.
(5), again with Bi
1-xSr
xCuSeO (x=0.025～0.125) block materials ball milling powdered, rotational speed of ball-mill is 100～500rpm, the time is 15min～96h.Preferably, the ball milling time is 1～50h.
(6), with (5) gained powder graphite jig of packing into, put sintering in the discharge plasma sintering stove into, the sintering environment is a vacuum, vacuum degree is 4～7Pa.Under certain temperature, pressure, temperature retention time, carry out sintering, obtain Sr doping oxide BiCuSeO thermoelectric material; Sintering temperature is 200～500 ℃, and temperature retention time is 2～8min, and sintering pressure is 20～60MPa, and programming rate is 40 ℃～180 ℃/min.
The invention has the advantages that:
(1) thermoelectric material provided by the invention is compared with other oxide pyroelectric materials, and conductivity is higher, and thermoelectromotive force is big, thermal conductivity is low, the dimensionless thermoelectric figure of merit high;
(2) thermoelectric material preparation method technology provided by the invention is easy, and the synthetic time with moulding is short.
Description of drawings
Fig. 1 is BiCuSeO and Bi
0.925Sr
0.075The CuSeO x-ray diffractogram of powder;
Fig. 2 is BiCuSeO and Bi
0.925Sr
0.075The conductivity of CuSeO block materials concerns with variation of temperature;
Fig. 3 is BiCuSeO and Bi
0.925Sr
0.075The thermoelectromotive force of CuSeO block materials concerns with variation of temperature;
Fig. 4 is BiCuSeO and Bi
0.925Sr
0.075The thermal conductivity of CuSeO block materials concerns with variation of temperature;
Fig. 5 is BiCuSeO and Bi
0.925Sr
0.075The dimensionless thermoelectric figure of merit of CuSeO block materials concerns with variation of temperature.
Embodiment
Below in conjunction with accompanying drawing and embodiment Sr doping oxide BiCuSeO thermoelectric material provided by the invention and preparation method thereof is elaborated.
The present invention provides a kind of Sr doping oxide BiCuSeO thermoelectric material and preparation method thereof, and the chemical formula of described Sr doping oxide BiCuSeO thermoelectric material is Bi
1-xSr
xCuSeO, x=0.025～0.125, preferred, x=0.025～0.075.The conductivity variations scope of described thermoelectric material is 470～48000Sm
-1, the thermoelectromotive force excursion is+100～+ 375 μ VK
-1, the thermal conductivity excursion is 0.45～1.05Wm
-1K
-1, maximum dimensionless thermoelectric figure of merit is 0.76 at 873K.
Above-mentioned Sr doping oxide BiCuSeO thermoelectric material prepares through following method:
(1) raw material is prepared: adopt Bi
2O
3(purity is 99.9%), SrO (purity is 99.99%), Cu (purity is 99.99%), Se (purity is 99.99%) and Bi (purity is 99.99) powder are pressed Bi as initial feed
2O
3: SrO: Cu: Se: Bi=(1/3-x): x: 1: 1: [1-2* (1/3-x)] atomic ratio batching, x=0.025～0.125.
(2) mixed material.Above-mentioned raw materials is put into ball mill ball milling 15min～96h under 100～500rpm rotating speed together.
(3) with the powder that mixes, the diameter of packing into is to press down at 100～250MPa pressure in the steel die of 10～20mm to process disk.
(4) with the disk after the cold moudling, be placed in the quartz ampoule 300～700 ℃ of sintering temperatures 48～240 hours, programming rate be 40～180 ℃ per hour, obtaining diameter is 10～20mm, highly is the Sr doping oxide BiCuSeO block materials of 4～6mm.Preferably, getting sintering temperature is 200-500 ℃, and sintering time is 2-8 minute.
(5) and then with Bi
1-xSr
xCuSeO (x=0.025～0.125) block materials ball milling powdered, rotational speed of ball-mill is 100～500rpm, the time is 15min～96h.
(6) at last with the gained powder graphite jig of packing into, put sintering in the discharge plasma sintering stove into, the sintering environment is a vacuum, and vacuum degree is 4～7Pa.Under certain temperature, pressure, temperature retention time, carry out sintering, obtain Sr doping oxide BiCuSeO thermoelectric material; Sintering temperature is 200～500 ℃, and temperature retention time is 2～8min, and sintering pressure is 20～60MPa, and programming rate is 40 ℃～180 ℃/min.
Embodiment 1:Prepare a kind of Sr doping oxide BiCuSeO thermoelectric material Bi0.975Sr0.025CuSeO through method provided by the invention, concrete preparation process is following:
(1) prepares raw material: according to Bi
2O
3: SrO: Cu: Se: Bi=(1/3-x): x: 1: 1: [1-2* (1/3-x)] atomic ratio batching, x=0.025.Bi
2O
3(purity is 99.9%), SrO (purity is 99.99%), Cu (purity is 99.99%), Se (purity is 99.99%) and Bi (purity is 99.99) are powder.
(2) mixed material.Above-mentioned raw materials is put into ball mill ball milling 1h under the 100rpm rotating speed together.
(3) with the powder that mixes, the diameter of packing into is to press down at 150MPa pressure in the steel die of 10～20mm to process disk.
(4) with the disk after the cold moudling, be placed in the quartz ampoule 300 ℃ of sintering temperatures 240 hours, programming rate be 180 ℃ per hour, obtain identical with mould diameter, highly be the Sr doping oxide BiCuSeO block materials of 4mm.
(5) and then with Bi
1-xSr
xCuSeO (x=0.025) block of material ball milling powdered, rotational speed of ball-mill is 100rpm, the time is 96h.
(6) at last with the gained powder graphite jig of packing into, put sintering in the discharge plasma sintering stove into, the sintering environment is a vacuum, and vacuum degree is 4～7Pa.Under certain temperature, pressure, temperature retention time, carry out sintering, obtain Sr doping oxide BiCuSeO thermoelectric material; Sintering temperature is 300 ℃, and temperature retention time is 3min, and sintering pressure is 60MPa, and programming rate is 180 ℃/min.The dimensionless thermoelectric figure of merit of the Sr doping oxide BiCuSeO thermoelectric material for preparing is 0.45 at 873K.
Embodiment 2:Prepare a kind of Sr doping oxide BiCuSeO thermoelectric material Bi0.925Sr0.075CuSeO through method provided by the invention, concrete preparation process is following:
(1) prepares raw material: according to Bi
2O
3: SrO: Cu: Se: Bi=(1/3-x): x: 1: 1: [1-2* (1/3-x)] atomic ratio batching, x=0.075.Bi
2O
3(purity is 99.9%), SrO (purity is 99.99%), Cu (purity is 99.99%), Se (purity is 99.99%) and Bi (purity is 99.99) are powder.
(2) mixed material.Above-mentioned raw materials is put into ball mill ball milling 50h under the 100rpm rotating speed together.
(3) with the powder that mixes, the diameter of packing into is to press down at 250MPa pressure in the steel die of 10～20mm to process disk.
(4) with the disk after the cold moudling, be placed in the quartz ampoule 700 ℃ of sintering temperatures 48 hours, programming rate be 40 ℃ per hour, obtaining diameter is 10～20mm, highly is the Sr doping oxide BiCuSeO block materials of 6mm.
(5) and then with Bi
1-xSr
xCuSeO (x=0.075) bulk ball milling powdered, rotational speed of ball-mill is 500rpm, the time is 15min.
(6) at last with the gained powder graphite jig of packing into, put sintering in the discharge plasma sintering stove into, the sintering environment is a vacuum, and vacuum degree is 4～7Pa.Under certain temperature, pressure, temperature retention time, carry out sintering, sintering temperature is 500 ℃, and temperature retention time is 5min, and sintering pressure is 20MPa, and programming rate is 40 ℃/min.The dimensionless thermoelectric figure of merit that obtains Sr doping oxide BiCuSeO thermoelectric material is 0.62 at 873K.
Adopt to prepare BiCuSeO, prepare the technological parameter embodiment 0 as shown in table 1 of BiCuSeO, x=0, and the Bi for preparing with the present invention with embodiment 2 identical preparation methods
0.925Sr
0.075The CuSeO comparative analysis as a result that makes an experiment, sample that will be behind oversintering, carry out surface finish with sand paper after, carry out X-ray diffraction analysis and identify the thing phase composition.Fig. 1 is BiCuSeO and Bi
0.925Sr
0.075The x-ray diffractogram of powder of CuSeO.Can know that through analyzing main characteristic peak is the characteristic diffraction peak of BiCuSeO, successfully prepare Sr doping oxide BiCuSeO thermoelectric material.
After Sr doping oxide BiCuSeO block materials carried out surface finish cutting with sand paper, carry out the thermophysical property test, mainly comprise: thermoelectricity capability (conductivity, thermoelectromotive force, thermal conductivity) test.According to the above data that record, through the performance of thermal conductivity evaluating materials such as (thermal diffusion coefficient, specific heat and test density three's products).Fig. 2 is BiCuSeO and Bi
0.925Sr
0.075The conductivity of CuSeO block materials concerns that with variation of temperature Fig. 3 is BiCuSeO and Bi
0.925Sr
0.075The thermoelectromotive force of CuSeO block materials concerns that with variation of temperature Fig. 4 is BiCuSeO and Bi
0.925Sr
0.075The thermal conductivity of CuSeO block materials concerns that with variation of temperature Fig. 5 is BiCuSeO and Bi
0.925Sr
0.075The dimensionless thermoelectric figure of merit of CuSeO block materials concerns with variation of temperature.Gained dimensionless thermoelectric figure of merit is the peak of the oxide pyroelectric material of present report, shows that Sr doping oxide BiCuSeO block materials is a kind of thermoelectric material that development potentiality is arranged very much.
Find that in process of the test BiCuSeO has good thermoelectricity capability, the dimensionless thermoelectric figure of merit of 873K is 0.40, and after mixing through Sr, the conductivity variations scope is 470～48000Sm
-1, the thermoelectromotive force excursion is+100～+ 375 μ VK
-1, the thermal conductivity excursion is 0.45～1.05Wm
-1K
-1, the maximum dimensionless thermoelectric figure of merit that Sr optimizes the back acquisition of mixing is 0.76 at 873K.Above performance all is better than the oxide pyroelectric material of having reported in electrical transmission and heat transfer, can compare mutually with traditional alloy type figure of merit thermoelectric material.
The present invention shows, can prepare a kind of Sr doping oxide BiCuSeO thermoelectric material through simple method, and test result shows that it is a kind of potential thermoelectric block body material, and the thermoelectricity capability of this oxide does not appear in the newspapers at present as yet.
Adopt preparation method provided by the invention,, prepared various Bi as shown in table 1 below respectively through changing technological parameter
1-xSr
xThe CuSeO thermoelectric material:
Table 1: use preparation method provided by the invention and prepare Bi
1-xSr
xThe embodiment of CuSeO
In sum, the present invention has prepared a kind of Sr doping oxide BiCuSeO thermoelectric material that development potentiality is arranged very much through solid-state reaction, ball milling and discharge plasma sintering method.Described Sr doping oxide BiCuSeO thermoelectric material at the dimensionless thermoelectric figure of merit of 873K greater than 0.28; Maximum reaches 0.76; And have suitable conductivity, thermoelectromotive force and thermal conductivity, a kind of temperature difference energy source conversion material that can thermoelectricity directly be converted into electric energy that warm area is used in being suitable for.Have great application prospect at used heat utilization, energy development and field of environment protection.
Claims (6)
1. Sr doping oxide BiCuSeO thermoelectric material, it is characterized in that: the chemical formula of described thermoelectric material is Bi
1-xSr
xCuSeO, x=0.025～0.125.
2. a kind of Sr doping oxide BiCuSeO thermoelectric material according to claim 1, it is characterized in that: the chemical formula of described thermoelectric material is Bi
1-xSr
xCuSeO, x=0.025～0.075.
3. a kind of Sr doping oxide BiCuSeO thermoelectric material according to claim 1, it is characterized in that: the conductivity variations scope of described thermoelectric material is 470～48000Sm
-1, the thermoelectromotive force excursion is+100～+ 375 μ VK
-1, the thermal conductivity excursion is 0.45～1.05Wm
-1K
-1, maximum dimensionless thermoelectric figure of merit is 0.76 at 873K.
4. the preparation method of the described Sr doping oxide of claim 1 a BiCuSeO thermoelectric material is characterized in that comprising the steps:
The first step adopts Bi
2O
3, SrO, Cu, Se and Bi powder be as initial feed, presses Bi
2O
3: SrO: Cu: Se: Bi=(1/3-x): x: 1: 1: [1-2* (1/3-x)] atomic ratio batching, x=0.025～0.125;
Second step, raw material to be put into ball grinder evenly mix, rotational speed of ball-mill is 100～500rpm, the time is 15min～96h;
The 3rd step, the powder that mixes to be colded pressing, pressure is 100～250MPa, is pressed into disk;
The 4th the step, the disk after the cold moudling is carried out sintering, sintering temperature is 300～700 ℃, temperature retention time is 48～240 hours, programming rate be 40～180 ℃ per hour, obtaining diameter is 10～20mm, highly is the Bi of 4～6mm
1-xSr
xCuSeO block materials, wherein x=0.025～0.125;
The 5th step is again with Bi
1-xSr
xCuSeO block materials ball milling powdered, rotational speed of ball-mill is 100～500rpm, the ball milling time is 15min～96h;
In the 6th step,, put sintering in the discharge plasma sintering stove into the 5th step gained powder graphite jig of packing into; The sintering environment is a vacuum, and vacuum degree is 4～7Pa, carries out sintering; Sintering temperature is 200～500 ℃, and temperature retention time is 2～8min, and sintering pressure is 20～60MPa; Programming rate is 40 ℃～180 ℃/min, obtains Sr doping oxide BiCuSeO thermoelectric material.
5. the preparation method of Sr doping oxide BiCuSeO thermoelectric material according to claim 4 is characterized in that: the temperature of discharge plasma sintering is 300～500 ℃ among the described preparation method, and temperature retention time is 3～8min.
6. the preparation method of Sr doping oxide BiCuSeO thermoelectric material according to claim 4 is characterized in that: the ball milling time is 1～50h in said second step.
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