CN102655204B - Preparation method of sr-doping oxide BiCuSeO thermoelectric material - Google Patents
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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 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 by electric energy and the heat energy direct energy and material of conversion mutually.The remarkable advantage of thermoelectric material is noiselessness, the eco-friendly green energy resource material of one pollution-free, movement-less part.An important performance indexes weighing thermoelectric material is exactly 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 the conductivity of material, and κ is 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 most thermoelectric material is in " 1 " left and right, and conversion efficiency of thermoelectric, in 10% left and right, is about 1/3 of diesel engine generator generating efficiency, if thermoelectric figure of merit can reach " 3 " left and right, thermoelectric power generation will replace diesel generation to dominate the market.But the good thermoelectric material of performance of application all contains heavy metal element at present, and expensive.As the Bi-Sb-Te alloy of nanostructure [B.Poudel, et al.Science 320,634 (2008)], 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.Compared with these materials, oxide pyroelectric material has high-temperature stability, low price etc., and advantage receives much concern, but oxide pyroelectric material ubiquity conductivity is bad, and thermal conductivity is high, causes dimensionless thermoelectric figure of merit generally not high, as Zn
0.96al
0.02ga
0.02the ZT value of O oxide at 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 at 1273K temperature is 0.45[M.Ohtaki, et al.J.Electron.Mater.38,1234 (2009)], but these oxides cannot be compared with traditional alloy phase in application.
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, by after mixing, colds pressing, and adopts solid-state reaction, ball milling and discharge plasma sintering are prepared Sr doping BiCuSeO oxide pyroelectric material.
Concrete technology flow process is as follows:
(1), adopt Bi
2o
3, SrO, Cu, Se and Bi powder be as initial feed, by 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, 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, Ball-milling Time is 1～50h.
(3), by the powder mixing, cold pressing, pressure is 100～250MPa, is pressed into disk.
(4), by the disk after cold moudling, be placed in quartz ampoule and carry 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, is highly the Bi of 4～6mm
1-xsr
xcuSeO (x=0.025～0.125) block materials.
(5), again by 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, Ball-milling Time is 1～50h.
(6), pack (5) gained powder into graphite jig, put sintering in discharge plasma sintering stove into, sintering environment is 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.
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 large, thermal conductivity is low, dimensionless thermoelectric figure of merit is high;
(2) thermoelectric material preparation method simple process provided by the invention, the time synthetic and moulding is short.
Accompanying drawing explanation
Fig. 1 is BiCuSeO and Bi
0.925sr
0.075cuSeO x-ray diffractogram of powder;
Fig. 2 is BiCuSeO and Bi
0.925sr
0.075the conductivity variation with temperature relation of CuSeO block materials;
Fig. 3 is BiCuSeO and Bi
0.925sr
0.075the thermoelectromotive force variation with temperature relation of CuSeO block materials;
Fig. 4 is BiCuSeO and Bi
0.925sr
0.075the thermal conductivity variation with temperature relation of CuSeO block materials;
Fig. 5 is BiCuSeO and Bi
0.925sr
0.075the dimensionless thermoelectric figure of merit variation with temperature relation of CuSeO block materials.
Embodiment
Below in conjunction with drawings and Examples, Sr doping oxide BiCuSeO thermoelectric material provided by the invention and preparation method thereof is elaborated.
The invention provides a kind of Sr doping oxide BiCuSeO thermoelectric material and preparation method thereof, 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, thermoelectromotive force excursion is+100～+ 375 μ VK
-1, 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 by the 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 as initial feed, by 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.
(2) mixed material.Above-mentioned raw materials is put into ball mill ball milling 15min～96h under 100～500rpm rotating speed together.
(3), by the powder mixing, pack in the steel die that diameter is 10～20mm and be pressed into disk under 100～250MPa pressure.
(4) by the disk after cold moudling, be placed in quartz ampoule at 300～700 ℃ of temperature sintering 48～240 hours, programming rate be 40～180 ℃ per hour, obtaining diameter is 10～20mm, is highly 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 by 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) finally pack gained powder into graphite jig, put sintering in discharge plasma sintering stove into, sintering environment is 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:by method provided by the invention, prepare a kind of Sr doping oxide BiCuSeO thermoelectric material Bi0.975Sr0.025CuSeO, concrete preparation process is as follows:
(1) prepare 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 100rpm rotating speed together.
(3), by the powder mixing, pack in the steel die that diameter is 10～20mm and be pressed into disk under 150MPa pressure.
(4) by the disk after cold moudling, be placed in quartz ampoule at 300 ℃ of temperature sintering 240 hours, programming rate be 180 ℃ per hour, obtain identical with mould diameter, be highly the Sr doping oxide BiCuSeO block materials of 4mm.
(5) and then by 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) finally pack gained powder into graphite jig, put sintering in discharge plasma sintering stove into, sintering environment is 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 preparing is 0.45 at 873K.
embodiment 2:by method provided by the invention, prepare a kind of Sr doping oxide BiCuSeO thermoelectric material Bi0.925Sr0.075CuSeO, concrete preparation process is as follows:
(1) prepare 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 100rpm rotating speed together.
(3), by the powder mixing, pack in the steel die that diameter is 10～20mm and be pressed into disk under 250MPa pressure.
(4) by the disk after cold moudling, be placed in quartz ampoule at 700 ℃ of temperature sintering 48 hours, programming rate be 40 ℃ per hour, obtaining diameter is 10～20mm, is highly the Sr doping oxide BiCuSeO block materials of 6mm.
(5) and then by Bi
1-xsr
xcuSeO (x=0.075) bulk ball milling powdered, rotational speed of ball-mill is 500rpm, the time is 15min.
(6) finally pack gained powder into graphite jig, put sintering in discharge plasma sintering stove into, sintering environment is 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 the preparation method identical with embodiment 2 to prepare BiCuSeO, prepare the technological parameter embodiment 0 as shown in table 1 of BiCuSeO, x=0, and the Bi preparing with the present invention
0.925sr
0.075cuSeO carries out comparison of test results analysis, by the sample after oversintering, carries out after surface finish with sand paper, carries out X-ray diffraction analysis and identifies thing phase composition.Fig. 1 is BiCuSeO and Bi
0.925sr
0.075the x-ray diffractogram of powder of CuSeO.Known main characteristic peak is the characteristic diffraction peak of BiCuSeO by analysis, has successfully prepared Sr doping oxide BiCuSeO thermoelectric material.
Sr doping oxide BiCuSeO block materials is carried out, after surface finish cutting, carrying out thermophysical property test with sand paper, mainly comprise: thermoelectricity capability (conductivity, thermoelectromotive force, thermal conductivity) test.According to above data measured, by the performance of the evaluating materials such as thermal conductivity (thermal diffusion coefficient, specific heat and test density three's product).Fig. 2 is BiCuSeO and Bi
0.925sr
0.075the conductivity variation with temperature relation of CuSeO block materials, Fig. 3 is BiCuSeO and Bi
0.925sr
0.075the thermoelectromotive force variation with temperature relation of CuSeO block materials, Fig. 4 is BiCuSeO and Bi
0.925sr
0.075the thermal conductivity variation with temperature relation of CuSeO block materials, Fig. 5 is BiCuSeO and Bi
0.925sr
0.075the dimensionless thermoelectric figure of merit variation with temperature relation of CuSeO block materials.Gained dimensionless thermoelectric figure of merit is the peak of the oxide pyroelectric material of current report, shows that Sr doping oxide BiCuSeO block materials is a kind of thermoelectric material that has very much development potentiality.
In process of the test, find, BiCuSeO has good thermoelectricity capability, and the dimensionless thermoelectric figure of merit of 873K is 0.40, and after Sr doping, conductivity variations scope is 470～48000Sm
-1, thermoelectromotive force excursion is+100～+ 375 μ VK
-1, thermal conductivity excursion is 0.45～1.05Wm
-1k
-1, it is 0.76 at 873K that Sr optimizes the maximum dimensionless thermoelectric figure of merit obtaining after doping.Above performance is all better than the oxide pyroelectric material of having reported in electrical transmission and heat transmission, can be comparable with traditional alloy type figure of merit thermoelectric material.
The present invention shows, can prepare a kind of Sr doping oxide BiCuSeO thermoelectric material by simple method, and test result shows that it is a kind of potential thermoelectric block body material, and the thermoelectricity capability of this oxide has not yet to see report.
Adopt preparation method provided by the invention, by changing technological parameter, prepared respectively various Bi as shown in table 1 below
1-xsr
xcuSeO thermoelectric material:
Table 1: apply preparation method provided by the invention and prepare Bi
1-xsr
xthe embodiment of CuSeO
In sum, the present invention by solid-state reaction, ball milling and discharge plasma sintering legal system standby a kind of Sr doping oxide BiCuSeO thermoelectric material that has very much development potentiality.Described Sr doping oxide BiCuSeO thermoelectric material is greater than 0.28 at the dimensionless thermoelectric figure of merit of 873K, maximum reaches 0.76, and there is applicable conductivity, thermoelectromotive force and thermal conductivity, be suitable for a kind of temperature difference transducing source material that thermoelectricity directly can be converted to electric energy of middle warm area application.At used heat utilization, energy development and field of environment protection, have great application prospect.
Claims (3)
1. a preparation method for Sr doping oxide 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, by 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, puts into ball grinder by raw material and evenly mixes, and rotational speed of ball-mill is 100～500rpm, and the time is 15min～96h;
The 3rd step, colds pressing the powder mixing, and pressure is 100～250MPa, is pressed into disk;
The 4th step, carries out sintering by the disk after cold moudling, and sintering temperature is 300～700 ℃, and temperature retention time is 48～240 hours, programming rate be 40～180 ℃ per hour, obtaining diameter is 10～20mm, is highly the Bi of 4～6mm
1-xsr
xcuSeO block materials, wherein x=0.025～0.125;
The 5th step, then by Bi
1-xsr
xcuSeO block materials ball milling powdered, rotational speed of ball-mill is 100～500rpm, Ball-milling Time is 15min～96h;
The 6th step, pack the 5th step gained powder into graphite jig, put sintering in discharge plasma sintering stove into, sintering environment is vacuum, and vacuum degree is 4～7Pa, carry 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.
2. the preparation method of Sr doping oxide BiCuSeO thermoelectric material according to claim 1, is characterized in that: in described preparation method, the temperature of discharge plasma sintering is 300～500 ℃, temperature retention time is 3～8min.
3. the preparation method of Sr doping oxide BiCuSeO thermoelectric material according to claim 1, is characterized in that: in described second step, Ball-milling Time is 1～50h.
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