CN103247752B - Ge-Pb-Te-Se composite thermoelectric material and preparation method thereof - Google Patents
Ge-Pb-Te-Se composite thermoelectric material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 7
- 229910005900 GeTe Inorganic materials 0.000 claims description 32
- 229910002665 PbTe Inorganic materials 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 13
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 8
- 239000000956 alloy Substances 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000003708 ampul Substances 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
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- 238000006243 chemical reaction Methods 0.000 claims description 4
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- 238000001330 spinodal decomposition reaction Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 description 10
- 230000005619 thermoelectricity Effects 0.000 description 8
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Abstract
The invention provides a Ge-Pb-Te-Se composite thermoelectric material and a preparation method thereof, which are suitable for the technical field of novel energy materials. The chemical formula of the thermoelectric material is Ge1-xPbxTe1-ySey, wherein x represents the quantity that Pb replaces Ge, the value of x is larger than or equal to 0.10 and is smaller than or equal to 0.90, y represents the quantity that Se replaces Te, and the value of y is larger than or equal to 0.10 and is smaller than or equal to 0.70. The composite thermoelectric material provided by the invention has lower thermal conductivity, higher non-dimensional figure of merit and good thermoelectric property, and the non-dimensional figure of merit ZT reaches 1.58 at the temperature of 40 DEG C. The invention further provides the preparation method of the composite thermoelectric material.
Description
Technical field
The present invention relates to novel energy field of material technology, especially relate to a kind of middle temperature composite thermoelectric material and its preparation
Method.
Background technology
Thermoelectric material is a kind of specific function material, using its have electric current by when produce thermograde and two ends are deposited
Produce electromotive force in the temperature difference or the pyroelectric effect of electric current can achieve temperature control, thermo-electric generation and energising refrigeration.These freeze and send out
Electric system has small volume, lightweight, no any mechanical rotation part, noiselessness in work, does not cause environmental pollution, using the longevity
Life long it is easy to the advantages of control is it is considered to be very competitive energy substitution material in the future, in the following environmental protection energy
Engineering and Refrigeration Engineering aspect have broad application prospects.
The conversion efficiency of thermoelectric device is to be determined by the performance of thermoelectric material, and the performance of thermoelectric material is then by immeasurable
Guiding principle figure of merit ZT=S2Weighing, wherein S is Seebeck to σ T/k（Seebeck）Coefficient, σ and k be respectively material electrical conductivity and
Thermal conductivity, T is absolute temperature.A kind of thermoelectric material of excellent performance must have high Seebeck coefficient, high conductivity and low grade fever
Conductance.
Group IV-VI semi-conductor thermoelectric material, is middle temperature semi-conductor thermoelectric material including PbTe, GeTe and PbSe, can be used for
The temperature difference electricity generation device that warm area (400-800K) works, especially applies and utilizes in the recovery of industrial waste heat and automobile engine residual heat
In field.Although the electrical conductivity of GeTe is higher compared with PbTe base thermoelectricity material, but its thermal conductivity is also higher, leads to its thermoelectricity
Figure of merit ZT is less.
The effective way reducing GeTe base composite thermoelectric material thermal conductivity is introduced into nano-second-phase, increases and phonon is dissipated
Penetrate, and on electrical conductivity impact less such that it is able to have high dimensionless figure of merit.
Content of the invention
The technical problem to be solved is to provide a kind of composite thermoelectric material and preparation method thereof, it is desirable to provide
A kind of nanometer phase comprising a small amount of PbTe cubic structure and the composite thermoelectric material of GeTe trigonal crystal structure matrix phase, have very low grade fever
Conductance and good thermoelectricity capability.
The present invention is achieved in that the mutually formation rule according to the counterfeit binary phase diagraml of GeTe-PbTe with spinodal decomposition transformation
The composition of rule design alloy and Technology for Heating Processing, are prepared for a kind of GeTe base composite thermoelectric material, the chemistry of described thermoelectric material
Formula is Ge1-xPbxTe1-ySey, wherein x is the amount of Pb replacement Ge, and x span is 0.10 x 0.90, and y replaces Te's for Se
Amount, y span is 0.10 y 0.70.
A kind of preparation method of described GeTe base composite thermoelectric material, including step：According to Ge1-xPbxTe1-ySeyMiddle x and y
Numerical value, with metal Ge, Pb, Te and Se simple substance as raw material, weigh raw material according to proportioning；The raw material weighing is made and obtains Ge1- xPbxTe1-ySeySingle-phase alloy；By Ge1-xPbxTe1-ySeyCarry out discharge plasma sintering after alloy grind into powder, comprised
The nanometer phase of PbTe cubic structure and the composite thermoelectric material of GeTe trigonal crystal structure matrix phase.
The composite thermoelectric material that the present invention provides, carries out alloying component by the one-tenth phase rule of related system and technique sets
Meter, is obtained single solid solution, is obtained by discharge plasma sintering preparation technology and comprise a small amount of PbTe using melting, heat treatment
The nanometer phase of cubic structure and the composite Ge of GeTe trigonal crystal structure matrix phase1-xPbxTe1-ySey, described thermoelectric material has
Very low thermal conductivity simultaneously has higher thermoelectricity capability, and dimensionless figure of merit ZT reaches 1.58 when 400 °C.
Brief description
Fig. 1 is Ge1-xPbxTe0.5Se0.5（X=0,0.1,0.2,0.25,0.3,0.4 and 0.5）The X of composite thermoelectric material penetrates
Ray diffraction diagram.
Fig. 2 is Ge0.75Pb0.25Te0.5Se0.5The high resolution electron microscopy photo of composite thermoelectric material.
Fig. 3 is Ge1-xPbxTe0.5Se0.5（X=0,0.1,0.2,0.25,0.3,0.4 and 0.5）Composite thermoelectric material and GeTe
The resistivity of compound and the variation relation figure of temperature.
Fig. 4 is Ge1-xPbxTe0.5Se0.5（X=0,0.1,0.2,0.25,0.3,0.4 and 0.5）Composite thermoelectric material and GeTe
The Seebeck coefficient of compound and the variation relation figure of temperature.
Fig. 5 is Ge1-xPbxTe0.5Se0.5（X=0,0.1,0.2,0.25,0.3,0.4 and 0.5）Composite thermoelectric material and GeTe
The thermal conductivity of compound and the variation relation figure of temperature.
Fig. 6 is Ge1-xPbxTe0.5Se0.5（X=0,0.1,0.2,0.25,0.3,0.4 and 0.5）Composite thermoelectric material and GeTe
The dimensionless figure of merit of compound（ZT）Variation relation figure with temperature.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, and
It is not used in the restriction present invention.
A kind of GeTe base composite thermoelectric material, the chemical formula of described thermoelectric material is Ge1-xPbxTe1-ySey, wherein x is Pb
Replace the amount of Ge, span is 0.10 x 0.90, y replaces the amount of Te for Se, span is 0.10 y 0.70.
Wherein, a small amount of PbTe cubic structure is scattered in nanometer phase GeTe trigonal crystal structure matrix phase, and x decides and is distributed in
PbTe phase content in GeTe and the thermoelectricity capability of material.
Preferably, the span for 0.5, x for the value of y is 0.10 x 0.50.
A kind of preparation method of described GeTe base composite thermoelectric material, including step：
The first step, according to described Ge1-xPbxTe1-ySeyThe numerical value of middle x and y, is former with metal Ge, Pb, Te and Se simple substance
Material, weighs raw material according to proportioning；；
Second step, the raw material weighing is made and obtains Ge1-xPbxTe1-ySeySingle-phase alloy；
3rd step, by Ge1-xPbxTe1-ySeyCarry out discharge plasma sintering after alloy grind into powder, obtain comprising PbTe
The nanometer phase of cubic structure and the composite thermoelectric material of GeTe trigonal crystal structure matrix phase.
Wherein, the proportioning of different metal Ge, Pb, Te and Se in the first step, can be obtained according to the difference of x and y numerical value.x
Span is 0.10 x 0.90, and y span is 0.10 y 0.70.
In second step, the raw material weighing is loaded in quartz ampoule, is extracted into 6 × 10-3After Pa vacuum, the good quartz ampoule of soldering and sealing is simultaneously
It is placed in Muffle furnace and carries out smelting, reaction temperature is 1000 DEG C, the response time is 20 hours, then, slow cooling to 600
DEG C, quench after 600 DEG C of insulations carry out solid solution treatment in 4 hours, obtain Ge1-xPbxTe1-ySeySingle-phase alloy
In the third step, by Ge1-xPbxTe1-ySeyCarry out discharge plasma sintering, vacuum is after alloy grind into powder
1×10-2Pa, pressure 30～50MPa, 450～500 DEG C of sintering temperature, temperature retention time 5～10 minutes, can obtain described compound
Thermoelectric material.
Prepared composite thermoelectric material Ge1-xPbxTe1-ySeyCharacterized using X-ray diffractogram as shown in Figure 1.Fig. 1
Illustrate the X-ray diffractogram that x is composite thermoelectric material when 0.5 for 0,0.1,0.2,0.25,0.3,0.4 and 0.5, y, Fig. 2 is
Described composite thermoelectric material Ge0.75Pb0.25Te0.5Se0.5（X is 0.25, y is 0.5）High resolution electron microscopy photo, Fig. 1 and Fig. 2 table
The described composite thermoelectric material that the bright present invention is obtained comprises nanometer phase and the GeTe trigonal crystal structure matrix of a small amount of PbTe cubic structure
Phase.
Refer to Fig. 3, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Resistivity become with the rising of temperature
Change.At the same temperature, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Resistivity be more than the conductivity of GeTe, and, compound
Thermoelectric material Ge1-xPbxTe0.5Se0.5Resistivity with x value increase and increase.
Refer to Fig. 4, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Seebeck coefficient become with the rising of temperature
Change.At the same temperature, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Seebeck coefficient be more than GeTe Seebeck coefficient,
And, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Seebeck coefficient with x value increase and increase.
Refer to Fig. 5, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Thermal conductivity reduce with the rising of temperature.And
And, at the same temperature, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Thermal conductivity all significantly be less than GeTe thermal conductivity.
And, at identical temperature, with the increase of x numerical value, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Thermal conductivity rate score reduce.
Can be drawn by Fig. 5, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Compared to GeTe, the thermal conductivity of thermoelectric material can be reduced.
Refer to Fig. 6, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Dimensionless figure of merit with temperature rising and
Increase.And, at the same temperature, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Dimensionless figure of merit be all higher than GeTe
Thermal conductivity.And, at identical temperature, with the increase of x numerical value, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Dimensionless
Figure of merit numerical value substantially increases.Can be drawn by Fig. 6, composite thermoelectric material Ge1-xPbxTe0.5Se0.5Compared to GeTe, permissible
Increase the dimensionless figure of merit of thermoelectric material, increase the thermoelectricity capability of material.
In the technical program, with regard to the figure of merit of pure GeTe compound in Fig. 3 to Fig. 6, reported according to Gelbstein et al.
The figure of merit of the pure GeTe compound in road, specifically refers to Y.Gelbstein, B.Dado, O.B.Yehuda, Y.Sadia,
Z.Dashevsky and M.P.Dariel,Chem.Mater.,2010,22,1054–1058.
Below, specifically illustrate that this technology puts composite thermoelectric material of case offer and preparation method thereof with embodiment.
With metal Ge, Pb, Te and Se simple substance as raw material, according to Ge0.75Pb0.25Te0.5Se0.5Numerical value, weigh according to proportioning
Raw material；The raw material weighing is loaded in quartz ampoule, is extracted into 6 × 10-3After Pa vacuum, the good quartz ampoule of soldering and sealing is placed in entering in Muffle furnace
Row smelting, reaction temperature is 1000 DEG C, and the response time is 20 hours, and then slow cooling, to 600 DEG C, is incubated 4 at 600 DEG C
Hour quenches after carrying out solid solution treatment, obtains Ge0.75Pb0.25Te0.5Se0.5Single-phase alloy.By Ge0.75Pb0.25Te0.5Se0.5Close
Carry out discharge plasma sintering, vacuum is 1 × 10 after golden grind into powder-2Pa, pressure 30～50MPa, sintering temperature 450～
500 DEG C, temperature retention time 5～10 minutes, that is, obtain nanometer phase and the GeTe trigonal crystal structure matrix comprising a small amount of PbTe cubic structure
The composite thermoelectric material Ge of phase0.75Pb0.25Te0.5Se0.5.
The composite thermoelectric material Ge that the present embodiment is obtained0.75Pb0.25Te0.5Se0.5Thing phase, microstructure and thermoelectricity capability
As shown in figures 1 to 6, its thermal conductivity is 0.66W/m.K in 673K, is the 20% of the synthermal lower 3.23W/m.K of pure GeTe；And it is maximum
Figure of merit（ZT）For 1.58,0.51 than pure GeTe exceeds 209%.
The compound thermal of difference x and y value it is understood that above-mentioned same or like method can be adopted, is obtained
Electric material Ge1-xPbxTe1-ySey..Wherein, when x is 0.5 for 0,0.1,0.2,0.25,0.3,0.4 and 0.5, y, prepared is compound
Thermoelectric material Ge1-xPbxTe1-ySeyPerformance can be found in Fig. 3-6.
The composite thermoelectric material that the present invention provides, carries out alloying component by the one-tenth phase rule of related system and technique sets
Meter, is obtained single solid solution, is obtained by discharge plasma sintering preparation technology and comprise a small amount of PbTe using melting, heat treatment
The nanometer phase of cubic structure and the composite Ge of GeTe trigonal crystal structure matrix phase1-xPbxTe1-ySey, described thermoelectric material has
Very low thermal conductivity simultaneously has higher thermoelectricity capability, and dimensionless figure of merit ZT reaches 1.58 when 400 DEG C.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (3)
1. a kind of preparation method of composite thermoelectric material, the chemical formula of described thermoelectric material is Ge1-xPbxTe1-ySey, wherein x is
Pb replaces the amount of Ge, and x span is 0.10 x 0.40, and y replaces the amount of Te for Se, and y span is 0.10 y
0.70；Wherein PbTe cubic structure nanometer is mutually scattered in GeTe trigonal crystal structure matrix phase；
Described preparation method includes step：
According to Ge1-xPbxTe1-ySeyThe numerical value of middle x and y, with metal Ge, Pb, Te and Se simple substance as raw material, weighs former according to proportioning
Material；
The raw material weighing is made and obtains Ge1-xPbxTe1-ySeySingle-phase alloy；And
By Ge1-xPbxTe1-ySeyCarry out discharge plasma sintering after alloy grind into powder, obtain comprising PbTe cubic structure
The nanometer mutually composite thermoelectric material with GeTe trigonal crystal structure matrix phase；
The raw material weighing is made and forms Ge1-xPbxTe1-ySeyMethod be：The raw material weighing is loaded in quartz ampoule, is extracted into 6
×10-3After Pa vacuum, the good quartz ampoule of soldering and sealing is placed in Muffle furnace carrying out smelting, and reaction temperature is 1000 DEG C, the response time
For 20 hours, then, slow cooling, to 600 DEG C, quenches after 600 DEG C of insulations carry out solid solution treatment in 4 hours, obtains Ge1- xPbxTe1-ySeySingle-phase alloy.
2. the preparation method of composite thermoelectric material as claimed in claim 1 is it is characterised in that y is 0.5.
3. the preparation method of composite thermoelectric material as claimed in claim 1 is it is characterised in that by described Ge1-xPbxTe1-ySey
Carry out discharge plasma sintering, the method obtaining composite thermoelectric material is after alloy grind into powder:By Ge1-xPbxTe1-ySeyClose
Carry out discharge plasma sintering, vacuum is 1 × 10 after golden grind into powder-2Pa, pressure 30～50MPa, sintering temperature 450～
500 DEG C, temperature retention time 5～10 minutes, the spinodal decomposition using GeTe-PbTe system changes, and obtains described composite thermoelectric material.
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| CN105648258B (en) * | 2016-01-18 | 2017-07-07 | 浙江师范大学 | The method for lead telluride alloy thermoelectric material with reference to sensing hot pressing is got rid of in melt rotation |
| CN107799646B (en) * | 2017-09-14 | 2020-04-28 | 同济大学 | Alloy thermoelectric semiconductor material and preparation method thereof |
| CN108735887B (en) * | 2018-04-18 | 2020-10-02 | 同济大学 | Antimony-doped high-performance GeTe-PbTe solid solution thermoelectric material and preparation method thereof |
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| CN101217178A (en) * | 2007-12-26 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | A preparation method for antimonide molybdenum base thermoelectric material |
| CN101397612A (en) * | 2008-10-21 | 2009-04-01 | 同济大学 | Method for preparing skutterudite base thermoelectric block body material |
| CN101965312A (en) * | 2008-01-14 | 2011-02-02 | 俄亥俄州立大学研究基金会 | Improve by the thermoelectric figure of merit that improves density of electronic states |
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| CN101217178A (en) * | 2007-12-26 | 2008-07-09 | 中国科学院上海硅酸盐研究所 | A preparation method for antimonide molybdenum base thermoelectric material |
| CN101965312A (en) * | 2008-01-14 | 2011-02-02 | 俄亥俄州立大学研究基金会 | Improve by the thermoelectric figure of merit that improves density of electronic states |
| CN101397612A (en) * | 2008-10-21 | 2009-04-01 | 同济大学 | Method for preparing skutterudite base thermoelectric block body material |
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