CN102931336A - Germanium telluride (GeTe) based composite thermoelectric material and preparation method thereof - Google Patents
Germanium telluride (GeTe) based composite thermoelectric material and preparation method thereof Download PDFInfo
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- CN102931336A CN102931336A CN2012104009576A CN201210400957A CN102931336A CN 102931336 A CN102931336 A CN 102931336A CN 2012104009576 A CN2012104009576 A CN 2012104009576A CN 201210400957 A CN201210400957 A CN 201210400957A CN 102931336 A CN102931336 A CN 102931336A
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- 239000000463 material Substances 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 title 1
- 229910005900 GeTe Inorganic materials 0.000 claims abstract description 62
- 239000000126 substance Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 14
- 229910045601 alloy Inorganic materials 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 11
- 239000003708 ampul Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005275 alloying Methods 0.000 claims description 8
- 239000008188 pellet Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000005476 soldering Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 230000005619 thermoelectricity Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 230000005496 eutectics Effects 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 229910002665 PbTe Inorganic materials 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
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Abstract
The invention provides a composite thermoelectric material. A chemical formula of the composite thermoelectric material is (GeTe)1-x(Ag8GeTe6)x, wherein x is between 0.02 and 0.20. The invention also provides a preparation method of the composite thermoelectric material. The composite thermoelectric material provided by the invention is leadless, low in thermal conductivity, high in dimensionless merit figure ZT and high in thermoelectric performance.
Description
Technical field
The present invention relates to novel energy material technology field, especially relate to a kind of unleaded middle temperature composite thermoelectric material and preparation method thereof.
Background technology
Thermoelectric material is a kind of specific function material, utilize its have electric current by the time produce temperature gradient and two ends produce the thermoelectric effect of electromotive force or electric current when having the temperature difference and can realize temperature control, thermo-electric generation and energising refrigeration.It is little, lightweight that these refrigeration and electricity generation system have a volume, without any mechanical rotation part, noiselessness in the work, do not cause environmental pollution, long service life, be easy to the advantages such as control, be considered in the future very competitive energy substitution material, having broad application prospects aspect following environmental protection energy project and the Refrigeration Engineering.
The conversion efficiency of thermoelectric device is to be determined by the performance of thermoelectric material, and the performance of thermoelectric material then is by dimensionless figure of merit ZT=S
2σ T/k weighs, and wherein S is Seebeck (Seebeck) coefficient, and σ and k are respectively conductivity and the thermal conductivities of material, and T is absolute temperature.A kind of thermoelectric material of excellent performance must have high Seebeck coefficient, high conductivity and lower thermal conductivity.
IV-VI family semi-conductor thermoelectric material comprises that PbTe, GeTe and PbSe are middle temperature semi-conductor thermoelectric material, can be used for the temperature difference electricity generation device of warm area (400-800K) work, especially is applied in the fields such as the recovery of industrial waste heat and automobile engine residual heat utilization.Compare with the PbTe base thermoelectricity material, the GeTe thermoelectric material does not contain Pb, although the conductivity of GeTe is higher, its thermal conductivity is also higher, causes its thermoelectric figure of merit ZT less.
Therefore, be necessary to provide a kind of composite thermoelectric material and preparation method thereof, not leaded, have lower thermal conductivity, thereby can have high dimensionless figure of merit.
Summary of the invention
The invention provides a kind of composite thermoelectric material and preparation method thereof.
A kind of composite thermoelectric material, the chemical formula of described composite thermoelectric material are (GeTe)
1-x(Ag
8GeTe
6)
x, wherein the span of x is 0.02＜=x＜=0.20.
Wherein, Ag
8GeTe
6Be distributed among the GeTe, x is determining to be distributed in the Ag among the GeTe
8GeTe
6The thermoelectricity capability of phase content and material.
A kind of preparation method of described composite thermoelectric material comprises step: according to (GeTe)
1-x(Ag
8GeTe
6)
xThe numerical value of middle x take metal Ge, Te and Ag simple substance as raw material, takes by weighing raw material according to proportioning; The raw material that takes by weighing is made formation GeTe base alloy; Described GeTe base alloying pellet is clayed into power, and the powder that described GeTe base alloying pellet is worn into carries out discharge plasma sintering, obtain described composite thermoelectric material.
Composite thermoelectric material provided by the invention utilizes GeTe-Ag
8GeTe
6The Ag that disperse distributes is introduced in the eutectic transformation of phasor in the GeTe matrix
8GeTe
6Second-phase forms the composite thermoelectric material with eutectic structure, greatly reduces the thermal conductivity of material, thereby has improved its thermoelectricity capability.
Description of drawings
Fig. 1 is (GeTe)
1-x(Ag
8GeTe
6)
xThe X-ray diffractogram of (x=0.02,0.05 and 0.11) composite thermoelectric material.
Fig. 2 is (GeTe)
1-x(Ag
8GeTe
6)
x(x=0.11) microstructure picture of composite thermoelectric material.
Fig. 3 is (GeTe)
1-x(Ag
8GeTe
6)
x(x=0,0.02,0.05, the 0.08 and 0.11) resistivity of composite thermoelectric material and the variation relation schematic diagram of temperature.
Fig. 4 (GeTe)
1-x(Ag
8GeTe
6)
x(x=0,0.02,0.05, the 0.08 and 0.11) Seebeck coefficient of composite thermoelectric material and the variation relation schematic diagram of temperature.
Fig. 5 (GeTe)
1-x(Ag
8GeTe
6)
x(x=0,0.02,0.05, the 0.08 and 0.11) thermal conductivity of composite thermoelectric material and the variation relation schematic diagram of temperature.
Fig. 6 (GeTe)
1-x(Ag
8GeTe
6)
xThe dimensionless figure of merit (ZT) of (x=0,0.02,0.05,0.08 and 0.11) composite thermoelectric material and the variation relation schematic diagram of temperature.
Specific implementation method
A kind of composite thermoelectric material that the technical program is provided below in conjunction with accompanying drawing and preparation method thereof is elaborated.
A kind of composite thermoelectric material, the chemical formula of described composite thermoelectric material are (GeTe)
1-x(Ag
8GeTe
6)
x, wherein the span of x is 0.02＜=x＜=0.20, is preferably 0.02＜=x＜=0.15.
Wherein, Ag
8The GeTe6 second-phase is distributed in the GeTe matrix, and x is determining to be distributed in the Ag among the GeTe
8GeTe
6The thermoelectricity capability of phase content and material.
A kind of preparation method of described composite thermoelectric material comprises step:
The first step is according to (GeTe)
1-x(Ag
8GeTe
6)
xThe numerical value of middle x take metal Ge, Te and Ag simple substance as raw material, takes by weighing raw material according to proportioning;
Second step is made formation GeTe base alloy with the raw material that takes by weighing;
The 3rd step; Described GeTe base alloying pellet is clayed into power;
In the 4th step, the powder that described GeTe base alloying pellet is worn into carries out discharge plasma sintering, obtains described composite thermoelectric material.
Wherein, in the first step, can obtain according to the difference of x numerical value the proportioning of different metal Ge, Te and Ag.The span of X is 0.02＜=x＜=0.20.
In second step, described raw material was reacted 20 hours under 900 degrees celsius in quartz ampoule, thereby obtain GeTe base alloy.
In the 3rd step, can adopt planetary ball mill that GeTe base alloy is carried out ball milling.
In the 4th step, under vacuum environment, carry out plasma discharging (SPS) sintering, vacuum degree is 1 * 10
-2During Pa, pressure 30 ~ 50MPa, 600 ~ 650 ° of C of sintering temperature, temperature retention time 5 ~ 10 minutes can obtain described composite thermoelectric material.
The composite thermoelectric material that makes (GeTe)
1-x(Ag
8GeTe
6)
xAdopt X-ray diffractogram as shown in Figure 1 to characterize.Fig. 1 has showed that x is 0.02,0.05 and the X-ray diffractogram of 0.11 o'clock composite thermoelectric material, and Fig. 2 is the microstructure picture of described composite thermoelectric material (x=0.11), and Fig. 1 and Fig. 2 show that the thermoelectric material that the present invention makes has comprised GeTe matrix phase and Ag
8GeTe
6Second-phase.
See also Fig. 3, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xResistivity increase along with the rising of temperature.Under uniform temp, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xResistivity high temperature under less than the conductance of GeTe.See also Fig. 4, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xSeebeck coefficient increase along with the rising of temperature, under uniform temp, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xSeebeck coefficient be slightly less than the Seebeck coefficient of GeTe.See also Fig. 5, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xThermal conductivity reduce along with the rising of temperature.And, under uniform temp, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xThermal conductivity all significantly be lower than the thermal conductivity of GeTe.And, under the uniform temp, along with the increase of x numerical value, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xThermal conductivity numerical value reduce.Can be drawn composite thermoelectric material (GeTe) by Fig. 5
1-x(Ag
8GeTe
6)
xThan GeTe, can reduce the thermal conductivity of thermoelectric material.See also Fig. 6, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xThe dimensionless figure of merit increase along with the rising of temperature.And, under uniform temp, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xThe dimensionless figure of merit all greater than the dimensionless figure of merit of GeTe.And, under the uniform temp, along with the increase of x numerical value, composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xDimensionless figure of merit numerical value increase.Can be drawn composite thermoelectric material (GeTe) by Fig. 6
1-x(Ag
8GeTe
6)
xThan GeTe, can increase the dimensionless figure of merit of thermoelectric material, thereby increase the thermoelectricity capability of material.
Below, specifically illustrate that with embodiment 1 to 3 present technique puts composite thermoelectric material that case provides and preparation method thereof.
Take Ge, Te and Ag as raw material, according to chemical molecular formula (GeTe)
0.89(Ag
8GeTe
6)
0.11Carry out in weighing proportioning and the quartz ampoule of packing into, vacuumize the good quartz ampoule of rear soldering and sealing and place Muffle furnace to react, reaction temperature is 900 ° of C, and the reaction time is 20 hours, obtains GeTe base alloy; Reaction is obtained GeTe base alloy grind into powder, put into ball grinder with abrading-ball, be filled with Ar gas after the forvacuum, adopt planetary ball mill under the protection of Ar gas, to make attritive powder, 200 rev/mins of drum'ss speed of rotation, ratio of grinding media to material 20:1, Ball-milling Time 8 hours; Powder behind the ball milling is carried out plasma discharging (SPS) sintering under vacuum environment, vacuum degree is 1 * 10
-2Pa, pressure 50MPa, 620 ° of C of sintering temperature, temperature retention time 5 minutes namely obtains Ag
8GeTe
6Be distributed in the unleaded composite thermoelectric material (GeTe) in the matrix GeTe matrix
0.89(Ag
8GeTe
6)
0.11
The composite thermoelectric material that the present embodiment makes (GeTe)
0.89(Ag
8GeTe
6)
0.11Phase, microstructure and thermoelectricity capability shown in Fig. 1-6, its thermal conductivity is 1.23W/m.K at 673K, is 38% of the synthermal lower 3.23W/m.K of pure GeTe; And its maximum figure of merit (ZT) is 1.15, exceeds 125% than 0.51 of pure GeTe.
Embodiment 2
Take Ge, Te and Ag as raw material, according to chemical molecular formula (GeTe)
0.95(Ag
8GeTe
6)
0.05Carry out in weighing proportioning and the quartz ampoule of packing into, vacuumize the good quartz ampoule of rear soldering and sealing and place Muffle furnace to react, reaction temperature is 900 ° of C, and the reaction time is 20 hours, obtains GeTe base alloy; Reaction is obtained GeTe base alloy grind into powder, put into ball grinder with abrading-ball, be filled with Ar gas after the forvacuum, adopt planetary ball mill under the protection of Ar gas, to make attritive powder, 200 rev/mins of drum'ss speed of rotation, ratio of grinding media to material 20:1, Ball-milling Time 8 hours; Powder behind the ball milling is carried out plasma discharging (SPS) sintering under vacuum environment, vacuum degree is 1 * 10
-2Pa, pressure 50MPa, 620 ° of C of sintering temperature, temperature retention time 5 minutes namely obtains Ag
8GeTe
6Be distributed in the unleaded composite thermoelectric material (GeTe) in the matrix GeTe matrix
0.95(Ag
8GeTe
6)
0.05
The composite thermoelectric material that the present embodiment makes (GeTe)
0.95(Ag
8GeTe
6)
0.05Phase and thermoelectricity capability shown in Fig. 1,3-6, its thermal conductivity is 1.98W/m.K at 673K, is 61% of the synthermal lower 3.23W/m.K of pure GeTe; And its maximum figure of merit (ZT) is 1.03, exceeds 102% than 0.51 of pure GeTe.
Take Ge, Te and Ag as raw material, according to chemical molecular formula (GeTe)
0.92(Ag
8GeTe
6)
0.08Carry out in weighing proportioning and the quartz ampoule of packing into, vacuumize the good quartz ampoule of rear soldering and sealing and place Muffle furnace to react, reaction temperature is 900 ° of C, and the reaction time is 20 hours, obtains GeTe base alloy; Reaction is obtained GeTe base alloy grind into powder, put into ball grinder with abrading-ball, be filled with Ar gas after the forvacuum, adopt planetary ball mill under the protection of Ar gas, to make attritive powder, 200 rev/mins of drum'ss speed of rotation, ratio of grinding media to material 20:1, Ball-milling Time 8 hours; Powder behind the ball milling is carried out plasma discharging (SPS) sintering under vacuum environment, vacuum degree is 1 * 10
-2Pa, pressure 50MPa, 620 ° of C of sintering temperature, temperature retention time 5 minutes namely obtains Ag
8GeTe
6Be distributed in the unleaded composite thermoelectric material (GeTe) in the matrix GeTe matrix
0.92(Ag
8GeTe
6)
0.08
The composite thermoelectric material that this example makes (GeTe)
0.92(Ag
8GeTe
6)
0.08Phase and thermoelectricity capability shown in Fig. 1,3-6, its thermal conductivity is 1.62W/m.K at 673K, is 50% of the synthermal lower 3.23W/m.K of pure GeTe; And its maximum figure of merit (ZT) is 0.87, exceeds 71% than 0.51 of pure GeTe.
Composite thermoelectric material provided by the invention utilizes (GeTe)
1-x(Ag
8GeTe
6)
xEutectic transformation, in the GeTe matrix, introduce the Ag that disperse distributes
8GeTe
6Second-phase forms the composite thermoelectric material with eutectic structure, greatly reduces the thermal conductivity of material, thereby has improved its thermoelectricity capability.
Claims (6)
1. composite thermoelectric material, the chemical formula of described composite thermoelectric material is (GeTe)
1-x(Ag
8GeTe
6)
x, wherein the span of x is 0.02＜=x＜=0.20.
2. composite thermoelectric material as claimed in claim 1, the span of x is 0.02＜=x＜=0.15 in the described chemical formula.
3. the preparation method of a right 1 or 2 described composite thermoelectric materials comprises step:
According to (GeTe)
1-x(Ag
8GeTe
6)
xThe numerical value of middle x take metal Ge, Te and Ag simple substance as raw material, takes by weighing raw material according to proportioning;
The raw material that takes by weighing is made formation GeTe base alloy;
Described GeTe base alloying pellet is clayed into power; And
The powder that described GeTe base alloying pellet is worn into carries out discharge plasma sintering, obtains described composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
x
4. the preparation method of composite thermoelectric material as claimed in claim 3, it is characterized in that, the raw material that takes by weighing is made the method that forms GeTe base alloy is: take by weighing to such an extent that raw material is packed in the quartz ampoule with described, vacuumize the good quartz ampoule of rear soldering and sealing and place Muffle furnace to react, reaction temperature is 900 ° of C, reaction time is 20 hours, obtains GeTe base alloy.
5. the preparation method of composite thermoelectric material as claimed in claim 4; it is characterized in that; the method that described GeTe base alloying pellet is clayed into power is: reaction is obtained GeTe base alloy grind into powder; put into ball grinder with abrading-ball; be filled with Ar gas after the forvacuum, adopt planetary ball mill under the protection of Ar gas, to make attritive powder, 200 ~ 400 rev/mins of drum'ss speed of rotation; ratio of grinding media to material 20:1, Ball-milling Time 0.5 ~ 14 hour.
6. the preparation method of composite thermoelectric material as claimed in claim 5 is characterized in that, the powder that described GeTe base alloying pellet is worn into carries out discharge plasma sintering, obtains described composite thermoelectric material (GeTe)
1-x(Ag
8GeTe
6)
xMethod be: powder behind the ball milling is carried out plasma discharging (SPS) sintering under vacuum environment, vacuum degree is 1 * 10
-2Pa, pressure 30 ~ 50MPa, 600 ~ 650 ° of C of sintering temperature, temperature retention time 5 ~ 10 minutes namely obtains Ag
8GeTe
6Be distributed in the unleaded composite thermoelectric material in the matrix GeTe matrix.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103552998A (en) * | 2013-10-17 | 2014-02-05 | 厦门大学 | Preparation method of GeTe microcrystal |
| CN104733610A (en) * | 2013-12-23 | 2015-06-24 | 杭州华为数字技术有限公司 | Metal-doped germanium tellurium base resistance change storage material, preparation method and resistance change unit device |
| CN106098923A (en) * | 2016-07-21 | 2016-11-09 | 同济大学 | A kind of argyrodite thermoelectric material and preparation method thereof |
| CN107799646A (en) * | 2017-09-14 | 2018-03-13 | 同济大学 | A kind of alloy thermoelectric semiconductor material and preparation method thereof |
| CN108735888A (en) * | 2018-04-27 | 2018-11-02 | 同济大学 | Novel Ge antimony tellurium compound thermoelectric material with high concentration vacancy and preparation method thereof |
| CN109950389A (en) * | 2019-03-18 | 2019-06-28 | 清华大学 | Middle warm area high performance thermoelectric material preparation method and middle warm area high performance thermoelectric material |
| CN110491988A (en) * | 2019-07-31 | 2019-11-22 | 深圳大学 | A kind of GeSe base thermoelectricity material and its preparation method and application of Ag doping |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103552998A (en) * | 2013-10-17 | 2014-02-05 | 厦门大学 | Preparation method of GeTe microcrystal |
| CN103552998B (en) * | 2013-10-17 | 2015-02-04 | 厦门大学 | Preparation method of GeTe microcrystal |
| CN104733610A (en) * | 2013-12-23 | 2015-06-24 | 杭州华为数字技术有限公司 | Metal-doped germanium tellurium base resistance change storage material, preparation method and resistance change unit device |
| CN104733610B (en) * | 2013-12-23 | 2017-12-15 | 杭州华为数字技术有限公司 | Metal-doped germanium telluro resistance-change memory material and preparation method and resistive element device |
| CN106098923A (en) * | 2016-07-21 | 2016-11-09 | 同济大学 | A kind of argyrodite thermoelectric material and preparation method thereof |
| CN107799646A (en) * | 2017-09-14 | 2018-03-13 | 同济大学 | A kind of alloy thermoelectric semiconductor material and preparation method thereof |
| CN107799646B (en) * | 2017-09-14 | 2020-04-28 | 同济大学 | Alloy thermoelectric semiconductor material and preparation method thereof |
| CN108735888A (en) * | 2018-04-27 | 2018-11-02 | 同济大学 | Novel Ge antimony tellurium compound thermoelectric material with high concentration vacancy and preparation method thereof |
| CN109950389A (en) * | 2019-03-18 | 2019-06-28 | 清华大学 | Middle warm area high performance thermoelectric material preparation method and middle warm area high performance thermoelectric material |
| CN110491988A (en) * | 2019-07-31 | 2019-11-22 | 深圳大学 | A kind of GeSe base thermoelectricity material and its preparation method and application of Ag doping |
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| Publication number | Publication date |
|---|---|
| CN102931336B (en) | 2016-08-03 |
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