CN103436724A - New method for quickly preparing high-performance PbS(1-x)Sex based thermoelectric material - Google Patents
New method for quickly preparing high-performance PbS(1-x)Sex based thermoelectric material Download PDFInfo
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Abstract
The invention relates to a new method for quickly preparing a high-performance PbS(1-x)Sex based thermoelectric material. The new method comprises the following steps of: 1) weighing Pb powder, S powder and Se powder as raw materials according to the stoichiometric ratio of all the atoms in PbS(1-x+y)Se(x+z), wherein x is greater than or equal to 0 and less than 1.0, y is equal to 0.02 and z is equal to 0; and when x is equal to 1.0, y is equal to 0 and z is equal to 0.02; next, grinding the powdery raw materials and mixing evenly, and then pressing into blocks; 2) arousing the self-propagating reaction of the blocks obtained in the step 1), naturally cooling after the reaction is completed, thereby obtaining a single-phase PbS(1-x)Sex solid solution; 3) grinding the PbS(1-x)Sex solid solution into powder, performing discharge plasma activated sintering to obtain the high-performance PbS(1-x)Sex based thermoelectric material. The new method provided by the invention has the advantages of high reaction speed, simple process, high efficiency and energy conservation, good repeatability and the like; the whole preparation process can be completed in 0.5 hour.
Description
Technical field
The invention belongs to the new energy materials preparing technical field, be specifically related to a kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material.
Background technology
The efficient energy conversion material of development of new and technology, can alleviate the destruction day by day of physical environment and the day by day exhaustion of fossil energy.At present, a lot of scientific workers in the whole world are concentrating on its attention and are finding and the exploitation thermoelectric generation technology---on reproducible new forms of energy switch technology.
Thermoelectric generation technology can realize the direct mutual conversion between electric energy and heat energy by Seebeck effect and the Peltier effect of thermoelectric material, it is as a kind of environmentally friendly Energy conversion technology at industrial exhaust heat and used heat, and there is important application prospect the recycling aspects such as automobile exhaust gas.Simultaneously it also has the advantages such as, noiselessness little without drive disk assembly, volume, good reliability.The efficiency of conversion of thermoelectric material is mainly by thermoelectric figure of merit
zTdetermine,
zT=
a 2 s T/
k, wherein
afor the Seebeck coefficient,
sfor specific conductivity,
kfor thermal conductivity,
tfor absolute temperature.
PbS
1-xse
xthe thermoelectric material of matrix system, have electrical property and lower thermal conductivity preferably, thereby have higher
zTvalue.Simultaneously, it has raw material and contains the advantages such as abundant and cheap.
At present, preparation PbS
1-xse
xthe method of base thermoelectricity material mainly adopts scorification.Yet, scorification temperature required higher (1100 ℃ of ﹥), and the fusing point of element own is very low, Pb(327 ℃), S(115 ℃) and Se(221 ℃), may cause like this loss of element evaporation, simultaneously the required reaction times is longer, therefore, aspect energy-efficient, certain deficiency is arranged.Therefore, a kind of simple and fast, less energy consumption, reproducible synthetic method are for preparation PbS
1-xse
xbase thermoelectricity material, seem extremely important.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of quick preparation high-performance PbS for the deficiency of above-mentioned prior art existence
1-xse
xthe method of base thermoelectricity material, speed of response is fast, technique is simple, reproducible, the PbS prepared
1-xse
xbase compact block thermoelectric material thermoelectricity capability is good.
The technical scheme that the problem that the present invention is the above-mentioned proposition of solution adopts is:
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press PbS
1-x+yse
x+zthe stoichiometric ratio of each atom takes Pb powder, S powder, Se powder as raw material, wherein is more than or equal to 0 while being less than 1.0 (0≤x ﹤ 1.0), y=0.02, z=0 as x; When x=1.0, y=0, z=0.02, then that the raw material powder ground and mixed is even, then that their ground and mixed is even, the powder mixed is pressed into to block;
2) step 1) gained block is caused to self-propagating reaction (SHS, Self-propagating High-temperature Synthesis) and reacted rear naturally cooling, can obtain single-phase PbS
1-xse
xcompound;
3) by above-mentioned products therefrom grind into powder, carry out discharge plasma activated sintering (PAS, Plasma Activated Sintering), obtain high-performance PbS
1-xse
xbase thermoelectricity material.
In such scheme, in described step 1), the quality purity of Pb powder, S powder and Se powder all is not less than 99.9%.
In such scheme, described step 2) in, self-propagating reaction is heated to initiation reaction to the block end.
In such scheme, described step 2) use air atmosphere or vacuum atmosphere or inert gas atmosphere in self-propagating reaction.
In such scheme, the process that described step 3) powder carries out discharge plasma activated sintering is: by the powder compacting in the graphite jig that diameter is 15mm of packing into, then be less than 10Pa and sintering pressure is to carry out sintering under the 35MPa condition in vacuum, temperature rise rate with 100 ℃/min is warmed up to 550 ℃, sintering densification time 7min.
Above-mentioned preparation method has obtained high-performance PbS
1-xse
xbase compact block thermoelectric material, at the x=0 place, the thermoelectricity capability figure of merit
zTreach 0.5 at 875K.
Take foregoing as basis, under the prerequisite that does not break away from basic fundamental thought of the present invention, ordinary skill knowledge and means according to this area, self-propagating reaction atmosphere modification, replacement or the change of various ways can also be arranged, as can be changed to other rare gas element do not reacted with Pb powder, S powder and Se powder etc. to its content.
The present invention need to provide necessary energy to bring out thermal chemical reaction to raw material, forms combustion wave, and reaction is after this just proceeded under the support of reacting before institute's release of heat, and reaction forms required PbS after spreading and finishing
1-xse
xthe base thermoelectricity material powder.
With existing PbS
1-xse
xthe preparation method compares, and advantage of the present invention is:
The first, the present invention adopts the self propagating high temperature synthetic technology to prepare PbS first
1-xse
xbase thermoelectricity material, have that speed of response is fast, equipment is simple, an advantage such as reproducible, energy-efficient and temperature rate is fast;
The second, the present invention can prepare PbS in 0.5h
1-xse
xbase compact block thermoelectric material, and material cost is cheap.
The accompanying drawing explanation
Fig. 1 is the XRD figure of block spectrum after powder and PAS after SHS in embodiment 1.
Fig. 2 is powder X-ray RD collection of illustrative plates after SHS in embodiment 2.
Fig. 3 is the XRD figure of block spectrum after powder and PAS after SHS in embodiment 3.
Fig. 4 is powder X-ray RD collection of illustrative plates after SHS in embodiment 4.
Fig. 5 is powder X-ray RD collection of illustrative plates after SHS in embodiment 5.
Fig. 6 (a) is the XRD figure of block spectrum after powder and PAS after SHS; Fig. 6 (b) is step 2) in the SEM figure (from left to right amplify respectively 5.00 k doubly and 10.00 k doubly) of powder after SHS; Fig. 6 (c) is sintering block zero dimension thermoelectric figure of merit
zTthe highest thermoelectric figure of merit of the material prepared with scorification
zTtemperature variant graph of a relation.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, further illustrate content of the present invention, but content of the present invention not only is confined to the following examples.
In following embodiment, the quality purity of Pb powder, S powder and Se powder all is not less than 99.9%.Self-propagating reaction in Figure of description (SHS) is " SHS " mark for products therefrom, and discharge plasma activated sintering (PAS) is " PAS " mark for products therefrom.
embodiment 1
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press chemical formula PbSe
(1+0.02)(be PbS
1-x+yse
x+zmiddle x=1.0, y=0, z=0.02) in, the stoichiometric ratio of each atom takes the Pb powder, (annotate: Se excessive 2% as raw material for the Se powder, it is the value of z, in order to compensate the volatilization loss of Se in reaction), total mass 4.5g, then that their ground and mixed is even, the powder mixed is pressed into to the cylindrical block block that diameter is 10mm (pressing process is: prior to 5MPa pressurize 5min, then in 8MPa pressurize 10min);
2) step 1) gained block is carried out in air atmosphere to lit-end initiation self-propagating reaction (SHS) and reacted rear naturally cooling;
3) by above-mentioned products therefrom grind into powder, by the powder compacting in the graphite jig of 15mm of packing into, then be less than 10Pa and sintering pressure is to carry out discharge plasma activated sintering (PAS) under the 35MPa condition in vacuum, temperature rise rate with 100 ℃/min is warmed up to 550 ℃, the sintering densification time is 7min, obtains PbSe compact block thermoelectric material.
As can be seen from Figure 1, after self-propagating reaction (SHS), after discharge plasma activated sintering (PAS), products therefrom is single-phase PbSe compound.
embodiment 2
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press PbS
(0.2+0.02)se
0.8(be PbS
1-x+yse
x+zmiddle x=0.8, y=0.02, z=0) in, the stoichiometric ratio of each atom takes Pb powder, S powder, (annotate: S excessive 2% as raw material for the Se powder, it is the value of y, in order to compensate the volatilization loss of S in reaction), total mass 4.5g, then that their ground and mixed is even, the powder mixed is pressed into to the cylindrical block block that diameter is 10mm (pressing process is: prior to 5MPa pressurize 5min, then in 8MPa pressurize 10min);
2) step 1) gained block is carried out in air atmosphere to lit-end initiation self-propagating reaction (SHS) and reacted rear naturally cooling;
3) above-mentioned products therefrom grind into powder is carried out to the XRD test.
As can be seen from Figure 2, after self-propagating reaction (SHS), products therefrom is single-phase PbS
0.2se
0.8sosoloid.
embodiment 3
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press PbS
(0.4+0.02)se
0.6(be PbS
1-x+yse
x+zmiddle x=0.6, y=0.02, z=0) in, the stoichiometric ratio of each atom takes Pb powder, S powder, (annotate: S excessive 2% as raw material for the Se powder, in order to compensate the volatilization loss of S in reaction), total mass 4.5g, then their ground and mixed is even, the powder mixed is pressed into to the cylindrical block block that diameter is 10mm (pressing process is: prior to 5MPa pressurize 5min, then in 8MPa pressurize 10min);
2) step 1) gained block is carried out in air atmosphere to lit-end initiation self-propagating reaction (SHS) and reacted rear naturally cooling;
3) by above-mentioned products therefrom grind into powder, by the powder compacting in the graphite jig of 15mm of packing into, then be less than 10Pa and sintering pressure is to carry out discharge plasma activated sintering (PAS) under the 35MPa condition in vacuum, temperature rise rate with 100 ℃/min is warmed up to 550 ℃, the sintering densification time is 7min, obtains PbSe compact block thermoelectric material.
As can be seen from Figure 3, after self-propagating reaction (SHS), after discharge plasma activated sintering (PAS), products therefrom is single-phase PbS
0.4se
0.6sosoloid.
embodiment 4
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press PbS
(0.6+0.02)se
0.4(be PbS
1-x+yse
x+zmiddle x=0.4, y=0.02, z=0) in, the stoichiometric ratio of each atom takes Pb powder, S powder, (annotate: S excessive 2% as raw material for the Se powder, in order to compensate the volatilization loss of S in reaction), total mass 4.5g, then their ground and mixed is even, the powder mixed is pressed into to the cylindrical block block that diameter is 10mm (pressing process is: prior to 5MPa pressurize 5min, then in 8MPa pressurize 10min);
2) step 1) gained block is carried out in air atmosphere to lit-end initiation self-propagating reaction (SHS) and reacted rear naturally cooling;
3) above-mentioned products therefrom grind into powder is carried out to the XRD test.
As can be seen from Figure 4, after self-propagating reaction (SHS), products therefrom is single-phase PbS
0.6se
0.4sosoloid.
embodiment 5
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press PbS
(0.8+0.02)se
0.2(be PbS
1-x+yse
x+zmiddle x=0.2, y=0.02, z=0) in, the stoichiometric ratio of each atom takes Pb powder, S powder, Se powder as raw material, total mass 4.5g, then their ground and mixed is even, the powder mixed is pressed into to the cylindrical block block that diameter is 10mm (pressing process is: prior to 5MPa pressurize 5min, then in 8MPa pressurize 10min);
2) step 1) gained block is carried out in air atmosphere to lit-end initiation self-propagating reaction (SHS) and reacted rear naturally cooling;
3) above-mentioned products therefrom grind into powder is carried out to the XRD test.
As can be seen from Figure 2, after self-propagating reaction (SHS), products therefrom is single-phase PbS
0.8se
0.2sosoloid.
embodiment 6
A kind of quick preparation high-performance PbS
1-xse
xthe novel method of base thermoelectricity material, it comprises the following steps:
1) press PbS
(1+0.02)(be PbS
1-x+yse
x+zmiddle x=1, y=0, z=0.02) in, the stoichiometric ratio of each atom takes Pb powder, S powder as raw material, total mass 4.5g, then their ground and mixed is even, the powder mixed is pressed into to the cylindrical block block that diameter is 10mm (pressing process is: prior to 5MPa pressurize 5min, then in 8MPa pressurize 10min);
2) step 1) gained block is carried out in air atmosphere to lit-end initiation self-propagating reaction (SHS) and reacted rear naturally cooling;
3) by above-mentioned products therefrom grind into powder, by the powder compacting in the graphite jig of 15mm of packing into, then be less than 10Pa and sintering pressure is to carry out discharge plasma activated sintering (PAS) under the 35MPa condition in vacuum, temperature rise rate with 100 ℃/min is warmed up to 550 ℃, the sintering densification time is 7min, obtains PbS compact block thermoelectric material.
The XRD figure spectrum that Fig. 6 (a) is block product after self-propagating reaction (SHS) after product powder and discharge plasma activated sintering (PAS); Fig. 6 (b) is step 2) in the SEM figure (from left to right amplify respectively 5.00 k doubly and 10.00 k doubly) of powder after SHS; Fig. 6 (c) is block zero dimension thermoelectric figure of merit after PAS
zTthe highest thermoelectric figure of merit of the material prepared with the Comparative Examples scorification
zTtemperature variant graph of a relation.
As can be seen from Figure 6, after SHS, products therefrom is single-phase PbS compound, and its powder grain size range is distributed more widely; After PAS, the gained block is single-phase PbS compound, this kind of thermoelectric material prepared by method, and in the temperature range more than 600K, the ratio of comparing has higher average
zTvalue, when temperature is 875K, can reach simultaneously
zT~ 0.57, with Comparative Examples, to compare, increase rate approaches 100%.
comparative Examples
Scorification technique: Pb powder, S powder are as raw material, according to mol ratio 1:1, mix, at the uniform velocity be raised to 1100 ℃ (time of at the uniform velocity heating up is 12h) from room temperature, and locate to be incubated 6h at 1100 ℃, then carry out the PAS sintering, PAS technique is: vacuum is less than 10Pa, and sintering pressure is 35MPa, temperature rise rate with 100 ℃/min is warmed up to 550 ℃, and the sintering densification time is 7min.
Claims (7)
1. one kind prepares high-performance PbS fast
1-xse
xthe novel method of base thermoelectricity material is characterized in that it comprises the following steps:
1) press PbS
1-x+yse
x+zthe stoichiometric ratio of each atom takes Pb powder, S powder and Se powder as raw material, wherein when 0≤x ﹤ 1.0, and y=0.02, z=0; When x=1.0, y=0, z=0.02, then be pressed into block by the powder stock ground and mixed after evenly;
2) step 1) gained block is caused to self-propagating reaction, reacted rear naturally cooling, obtain single-phase PbS
1-xse
xsosoloid;
3) by above-mentioned gained PbS
1-xse
xthe sosoloid grind into powder, carry out discharge plasma activated sintering, obtains high-performance PbS
1-xse
xbase thermoelectricity material.
2. a kind of quick preparation high-performance PbS according to claim 1
1-xse
xthe novel method of base thermoelectricity material, is characterized in that the quality purity of Pb powder in described step 1), S powder and Se powder all is not less than 99.9%.
3. a kind of quick preparation high-performance PbS according to claim 1
1-xse
xthe novel method of base thermoelectricity material, is characterized in that described step 1) pressing process is: the first step, pressurize 5min under 5MPa; Second step, pressurize 10min under 8MPa.
4. a kind of quick preparation high-performance PbS according to claim 1
1-xse
xthe novel method of base thermoelectricity material, is characterized in that described step 2) in self-propagating reaction the block end is heated to initiation reaction.
5. a kind of quick preparation high-performance PbS according to claim 1
1-xse
xthe method of base thermoelectricity material, is characterized in that described step 2) in use air atmosphere or vacuum atmosphere or inert gas atmosphere in self-propagating reaction.
6. a kind of quick preparation high-performance PbS according to claim 1
1-xse
xthe novel method of base thermoelectricity material, it is characterized in that the process that powder in described step 3) carries out discharge plasma activated sintering is: by the powder compacting in the graphite jig that diameter is 15mm of packing into, then be less than 10Pa and sintering pressure is to carry out sintering under the 35MPa condition in vacuum, temperature rise rate with 100 ℃/min is warmed up to 550 ℃, sintering densification time 7min.
7. the described preparation method of claim 1 obtains high-performance PbS
1-xse
xbase compact block thermoelectric material.
Priority Applications (12)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310430713.7A CN103436724B (en) | 2013-09-22 | 2013-09-22 | Method for quickly preparing high-performance PbS(1-x)Sex based thermoelectric material |
| US14/441,446 US10500642B2 (en) | 2013-03-19 | 2014-03-17 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| JP2015540043A JP6219399B2 (en) | 2013-03-19 | 2014-03-17 | Determination method of self-propagating combustion synthesis and preparation method of thermoelectric compounds based on the new criteria |
| EP14767900.5A EP2977129B1 (en) | 2013-03-19 | 2014-03-17 | Thermoelectric compound preparation based on self-propagating combustion synthesis new criterion |
| PCT/CN2014/000287 WO2014146485A1 (en) | 2013-03-19 | 2014-03-17 | Thermoelectric compound preparation based on self-propagating combustion synthesis new criterion |
| US16/667,143 US10913117B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US16/667,158 US10913118B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US16/667,173 US10913119B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US16/667,110 US10913115B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US16/667,128 US10913116B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US16/667,180 US11433456B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US16/667,081 US10913114B2 (en) | 2013-03-19 | 2019-10-29 | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
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| CN103934459A (en) * | 2014-01-20 | 2014-07-23 | 武汉理工大学 | Method for preparing high-performance Half-Heusler block thermoelectric materials at ultrahigh speed and low cost |
| WO2014146485A1 (en) * | 2013-03-19 | 2014-09-25 | 武汉理工大学 | Thermoelectric compound preparation based on self-propagating combustion synthesis new criterion |
| CN104946918A (en) * | 2015-05-25 | 2015-09-30 | 武汉理工大学 | New method for quickly preparing AgInSe2 based thermoelectric material |
| CN105152143A (en) * | 2015-07-22 | 2015-12-16 | 武汉理工大学 | Combustion synthesis method of Bi2SeO2-based thermoelectric material and combustion improver for Bi2SeO2-based thermoelectric material |
| CN106711317A (en) * | 2016-11-22 | 2017-05-24 | 同济大学 | Sulfur-group lead-compound thermoelectric material and preparation method thereof |
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| CN102633239A (en) * | 2012-05-11 | 2012-08-15 | 兰州大学 | Preparation method of PbSxSe1-x ternary nanocrystal |
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| CN102633239A (en) * | 2012-05-11 | 2012-08-15 | 兰州大学 | Preparation method of PbSxSe1-x ternary nanocrystal |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10913118B2 (en) | 2013-03-19 | 2021-02-09 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US10913117B2 (en) | 2013-03-19 | 2021-02-09 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US11433456B2 (en) | 2013-03-19 | 2022-09-06 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US10913114B2 (en) | 2013-03-19 | 2021-02-09 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US10500642B2 (en) | 2013-03-19 | 2019-12-10 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US10913116B2 (en) | 2013-03-19 | 2021-02-09 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| WO2014146485A1 (en) * | 2013-03-19 | 2014-09-25 | 武汉理工大学 | Thermoelectric compound preparation based on self-propagating combustion synthesis new criterion |
| US10913115B2 (en) | 2013-03-19 | 2021-02-09 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| US10913119B2 (en) | 2013-03-19 | 2021-02-09 | Wuhan University Of Technology | Thermoelectric materials synthesized by self-propagating high temperature synthesis process and methods thereof |
| CN103934459B (en) * | 2014-01-20 | 2016-05-11 | 武汉理工大学 | A kind of supper-fast low cost is prepared the method for high-performance Half-Heusler block thermoelectric material |
| CN103934459A (en) * | 2014-01-20 | 2014-07-23 | 武汉理工大学 | Method for preparing high-performance Half-Heusler block thermoelectric materials at ultrahigh speed and low cost |
| CN104946918A (en) * | 2015-05-25 | 2015-09-30 | 武汉理工大学 | New method for quickly preparing AgInSe2 based thermoelectric material |
| CN105152143B (en) * | 2015-07-22 | 2018-08-07 | 武汉理工大学 | A kind of Bi2SeO2The burning synthesis method and its combustion adjuvant of base thermoelectricity material |
| CN105152143A (en) * | 2015-07-22 | 2015-12-16 | 武汉理工大学 | Combustion synthesis method of Bi2SeO2-based thermoelectric material and combustion improver for Bi2SeO2-based thermoelectric material |
| CN106711317B (en) * | 2016-11-22 | 2019-06-11 | 同济大学 | A kind of sulfur family leaded object thermoelectric material and preparation method thereof |
| CN106711317A (en) * | 2016-11-22 | 2017-05-24 | 同济大学 | Sulfur-group lead-compound thermoelectric material and preparation method thereof |
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