CN102280570A - Trace Cu-doped Bi2S3-based thermoelectric material - Google Patents
Trace Cu-doped Bi2S3-based thermoelectric material Download PDFInfo
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- CN102280570A CN102280570A CN2011102181830A CN201110218183A CN102280570A CN 102280570 A CN102280570 A CN 102280570A CN 2011102181830 A CN2011102181830 A CN 2011102181830A CN 201110218183 A CN201110218183 A CN 201110218183A CN 102280570 A CN102280570 A CN 102280570A
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 239000000843 powder Substances 0.000 claims abstract description 41
- 239000000126 substance Substances 0.000 claims abstract description 15
- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 4
- WHBHBVVOGNECLV-OBQKJFGGSA-N 11-deoxycortisol Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 WHBHBVVOGNECLV-OBQKJFGGSA-N 0.000 claims abstract description 3
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 230000005619 thermoelectricity Effects 0.000 claims description 20
- 238000012360 testing method Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 238000005245 sintering Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005551 mechanical alloying Methods 0.000 abstract description 2
- 230000001427 coherent effect Effects 0.000 abstract 1
- 230000008021 deposition Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 51
- 238000001035 drying Methods 0.000 description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 7
- 238000004891 communication Methods 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 7
- 230000001681 protective effect Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000001238 wet grinding Methods 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 description 2
- 239000002800 charge carrier Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of energy materials and in particular relates to a trace Cu-doped Bi2S3-based thermoelectric material. In the thermoelectric material, metal simple substance Bi and Cu powder with the purity of 99.99 percent and simple substance S powder serve as raw materials, the thermoelectric material is prepared according to a chemical general formula of CuxBi2-xS3, wherein x is mole fraction of a Cu component and x is more than or equal to 0.001 and less than or equal to 0.05, and the thermoelectric material is prepared into a block material by combining a discharge plasma sintering technology and a mechanical alloying method. By the method, the trace Cu-doped Bi2S3-based block thermoelectric material can be easy and convenient to prepare, trace Cu is introduced into a Bi2S3 lattice, the carrier concentration of a sample is improved, a power factor is optimized, a Cu-S nano deposition coherent with a substrate structure is formed, and the thermal conductivity is greatly reduced; therefore, the thermoelectric performance of the Bi2S3-based block material can be greatly improved.
Description
Technical field
The invention belongs to the energy and material technical field, particularly a kind of micro Cu doping Bi
2S
3Base thermoelectricity material.
Background technology
Along with socioeconomic continuous development, environment and energy problem are more and more paid attention to by the mankind.Thermoelectric material can directly be realized the mutual conversion of heat energy and electric energy, and thermoelectric device is pollution-free, zero discharge and structure is light, volume is little, the life-span is long, is subjected to people's attention day by day.The electrothermal module that with the thermoelectric device is core parts has a wide range of applications at aspects such as semiconductor refrigerating, thermoelectric cells.With the competition of the refrigeration modes of routine and conventional power source in, thermoelectric device realizes that the key of extensive use is to improve the efficient of thermoelectric cooling and thermoelectric power generation.Thermoelectricity capability characterizes ZT=TS with dimensionless thermoelectric figure of merit ZT
2σ/κ, S are Seebeck coefficients, and σ is a conductivity, and κ is a thermal conductivity, and T is an absolute temperature; S
2σ is called power factor, is used for characterizing the electrical transmission performance of thermoelectric material, and thermal conductivity κ is charge carrier thermal conductivity κ
eWith lattice thermal conductivity κ
LSum.Well behaved thermoelectric material need have high power factor and low thermal conductivity.But above-mentioned each physical quantity is interrelated, all relevant with carrier concentration, high carrier concentration helps obtaining high power factor, but the charge carrier thermal conductivity is risen, therefore the thermoelectricity capability that improves material must be controlled suitable carrier concentration, and reduces lattice thermal conductivity.The method that improves the block materials thermoelectricity capability has doping, texture, Composition Control etc.These methods are when improving power factor, and thermal conductivity slightly increases; When perhaps power factor descended slightly, thermal conductivity declined to a great extent, the lifting of combined influence thermoelectric figure of merit.
Cu is a kind of good conductor, has and appraises at the current rate, though be a kind of doped chemical commonly used, yet there are no relevant Cu doping Bi
2S
3The relevant report of base thermoelectricity material.Cu is different from other doped chemicals simultaneously, and Cu and S very easily form available general formula Cu
2-xS(0≤x≤1) Biao Shi a series of compounds.If therefore at Bi
2S
3In carry out Cu when mixing experiment, can the part degree optimize carrier concentration though Cu mixes, this and other element doping effect is similar, helps improving its power factor.But when the Cu doping big or control not at that time, Cu and S be formation second impurity mutually easily, will cause the resistivity of system significantly to increase, and compares pure Bi under the room temperature
2S
3Resistivity increase severely 3 more than the order of magnitude, be unfavorable for the lifting of thermoelectricity capability.The application's patent utilizes Cu and S very easily to form Cu exactly
2-xS(0≤x≤1) characteristic of series compound, with the second phase Control of Impurities at nanoscale, make it in matrix, form the Cu-S nanometer precipitate of a large amount of and matrix phase structure coherence, when optimizing its power factor, significantly reduce its lattice thermal conductivity, reach the purpose that promotes thermoelectricity capability.
Summary of the invention
The objective of the invention is in order simply, conveniently, accurately to prepare the Bi that micro Cu is mixed
2S
3Matrix body material solves in the pyroelectric material performance optimizing process, and the problem that is difficult to improve power factor simultaneously and reduces thermal conductivity significantly improves Bi
2S
3The thermoelectricity capability of matrix body material.
Technical scheme of the present invention is: a kind of micro Cu doping Bi
2S
3Base thermoelectricity material, this thermoelectric material are that 99.99% metal simple-substance Bi, Cu powder and simple substance S powder are raw material with purity, according to chemical general formula Cu
x Bi
2-
x S
3(wherein
xBe the molar fraction of Cu component,
xSpan is 0.001≤
x≤ 0.05) configuration mixes, and adopts mechanical alloying method to be prepared into block materials in conjunction with discharge plasma sintering technique.
Principle of the present invention is: cross the addition of controlling various raw materials, accurately control the stoichiometric proportion of each element, make that the Cu of trace enters Bi in ma process and discharge plasma sintering process
2S
3In the lattice, regulate carrier concentration, improve the Cu-S nanometer precipitate of power factor and formation and matrix phase structure coherence, under the situation that does not influence conductivity, significantly reduce its lattice thermal conductivity.
The invention has the beneficial effects as follows: this method can simply, conveniently, accurately be prepared the Bi that micro Cu is mixed
2S
3Matrix body heat electric material is by the thermal conductivity that not only improves the power factor of sample but also significantly reduce sample of mixing of micro Cu.
Description of drawings
Fig. 1: the fracture stereoscan photograph of a kind of micro Cu doping of the present invention bismuth sulfide base thermoelectricity material block.
Fig. 2: the TEM photo of a kind of micro Cu doping of the present invention bismuth sulfide base thermoelectricity material.
Embodiment
Example 1
Press Cu:Bi: S mol ratio 0.001:1.999:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 400 rpm ball milling 10h after finishing take out ball grinder, inject 100 ml absolute ethyl alcohols in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 250 rpm wet-millings 30 minutes.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 2 h.Dried powder becomes block with discharge plasma sintering, and mould diameter is 20 mm, and programming rate is 100 ℃/min, 300 ℃ of temperature, and pressure 20Pa, temperature retention time is 5 min.Obtain the Cu that trace copper mixes at last
0.001Bi
1.999S
3Thermoelectric material, its power factor is 200 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.6 Wm
-1K
-1
Example 2
Press Cu:Bi: S mol ratio 0.002:1.998:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 450 rpm ball millings, 15 h after finishing take out ball grinder, inject the 100ml absolute ethyl alcohol in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 300 rpm wet-millings, 1 h.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 12 h.The powder of drying is become block with discharge plasma sintering, and mould diameter is 10 mm, and programming rate is 100 ℃/min, 550 ℃ of temperature, and pressure 60 Pa temperature retention times are 5 min.Obtain the Cu that trace copper mixes at last
0.002Bi
1.998S
3Thermoelectric material, its power factor is 240 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.54 Wm
-1K
-1
Example 3
Press Cu:Bi: S mol ratio 0.007:1.995:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 300 rpm ball millings, 20 h after finishing take out ball grinder, inject 100 ml absolute ethyl alcohols in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 425 rpm wet-millings, 3 h.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 8 h.The powder of drying is become block with discharge plasma sintering, and mould diameter is 25 mm, and programming rate is 100 ℃/min, 400 ℃ of temperature, and pressure 40 Pa, temperature retention time is 5 min.Obtain the Cu that trace copper mixes at last
0.007Bi
1.993S
3Thermoelectric material, its power factor is 303 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.3 Wm
-1K
-1
Example 4
Press Cu:Bi: S mol ratio 0.01:1.993:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 450 rpm ball millings, 15 h after finishing take out ball grinder, inject 100 ml absolute ethyl alcohols in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 200 rpm wet-millings, 3 h.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 2 h.The powder of drying is carried out discharge plasma sintering become block, mould diameter is 15 mm, and programming rate is 100 ℃/min, 580 ℃ of temperature, and pressure 40 Pa, temperature retention time is 5 min.Obtain the Cu that trace copper mixes at last
0.01Bi
1.99S
3Thermoelectric material, its power factor is 175 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.65 Wm
-1K
-1
Example 5
Press Cu:Bi: S mol ratio 0.05:1.99:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 600 rpm ball millings, 20 h after finishing take out ball grinder, inject the 100ml absolute ethyl alcohol in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 350 rpm wet-millings, 5 h.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 2 h.The powder of drying is become block with discharge plasma sintering, and mould diameter is 30 mm, and programming rate is 100 ℃/min, 600 ℃ of temperature, and pressure 60 Pa, temperature retention time is 5 min.Obtain the Cu that trace copper mixes at last
0.05Bi
1.95S
3Thermoelectric material, its power factor is 198 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.66 Wm
-1K
-1
Example 6
Press Cu:Bi: S mol ratio 0.025:1.975:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 425 rpm ball millings, 20 h after finishing take out ball grinder, inject the 50ml absolute ethyl alcohol in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 350 rpm wet-millings, 5 h.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 2 h.The powder of drying is become block with discharge plasma sintering, and mould diameter is 20 mm, and programming rate is 100 ℃/min, 600 ℃ of temperature, and pressure 60 Pa, temperature retention time is 5 min.Obtain the Cu that trace copper mixes at last
0.05Bi
1.95S
3Thermoelectric material, its power factor is 220 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.69 Wm
-1K
-1
Example 7
Press Cu:Bi: S mol ratio 0.045:1.955:3 is high-purity (99.99%) Cu powder, Bi powder and the S powder of weighing respectively, mixes, and puts into ball grinder, charges into Ar gas after vacuumizing, and circulates three times, makes Ar gas be full of ball grinder, and ball grinder is airtight.Then ball grinder is put into ball mill, 450 rpm ball millings, 20 h after finishing take out ball grinder, inject the 80ml absolute ethyl alcohol in ball grinder, in this process, keep the Ar air communication, in order to avoid destroy inert protective atmosphere, 350 rpm wet-millings, 5 h.Powder is taken out, put into the drying box drying, temperature is 80 ℃, and the time is 2 h.The powder of drying is become block with discharge plasma sintering, and mould diameter is 20 mm, and programming rate is 100 ℃/min, 600 ℃ of temperature, and pressure 60 Pa, temperature retention time is 5 min.Obtain the Cu that trace copper mixes at last
0.05Bi
1.95S
3Thermoelectric material, its power factor is 201 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.68 Wm
-1K
-1
Claims (8)
1. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: the composition of this material is that 99.99% metal simple-substance Bi, Cu powder and simple substance S powder are raw material with purity, and chemical general formula is Cu
x Bi
2-
x S
3, wherein
xBe the molar fraction of Cu component,
xSpan is 0.001≤
x≤ 0.05.
2. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: X=0.001, chemical formula are Cu
0.001Bi
1.999S
3Thermoelectric material, its power factor is 200 μ Wm when crossing test, calculating 573 K
-1K
-2, thermal conductivity is 0.6 Wm
-1K
-1
3. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: work as X=0.002, chemical formula is Cu
0.002Bi
1.998S
3Thermoelectric material, its power factor is 240 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.54 Wm
-1K
-1
4. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: work as X=0.007, chemical formula is Cu
0.007Bi
1.993S
3Thermoelectric material, its power factor is 303 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.3 Wm
-1K
-1
5. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: work as X=0.01, chemical formula is Cu
0.01Bi
1.99S
3Thermoelectric material, its power factor is 175 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.65 Wm
-1K
-1
6. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: work as X=0.05, chemical formula is Cu
0.05Bi
1.95S
3Thermoelectric material, its power factor is 198 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.66 Wm
-1K
-1
7. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: work as X=0.025, chemical formula is Cu
0.01Bi
1.975S
3Thermoelectric material, its power factor is 220 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.69 Wm
-1K
-1
8. micro Cu doping Bi
2S
3Base thermoelectricity material is characterized in that: work as X=0.045, chemical formula is Cu
0.045Bi
1.955S
3Thermoelectric material, its power factor is 201 μ Wm during through test, calculating 573 K
-1K
-2, thermal conductivity is 0.68 Wm
-1K
-1
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591103A (en) * | 2014-12-30 | 2015-05-06 | 华中科技大学 | Bi2Te3-xSx thermoelectric material and preparation method thereof |
| CN104692448A (en) * | 2015-03-18 | 2015-06-10 | 武汉理工大学 | Synthesis method of dynamic load of Ag2S (Silver Sulfide)-based compound and reactive assistant thereof |
| CN106418749A (en) * | 2016-10-11 | 2017-02-22 | 广东俏丹娜科技发展有限公司 | Detachable breathable massage bra |
| CN106587135A (en) * | 2016-12-28 | 2017-04-26 | 中国科学院上海高等研究院 | I-doped Cu-S-based thermoelectric material and preparation methods thereof |
| CN109659425A (en) * | 2018-12-29 | 2019-04-19 | 昆明理工大学 | A kind of bismuthino thermoelectric material and preparation method thereof promoting doping effect using barrier layer |
| CN111304492A (en) * | 2020-03-12 | 2020-06-19 | 中南大学 | Low-temperature n-type thermoelectric material and preparation method thereof |
| CN112299482A (en) * | 2020-09-22 | 2021-02-02 | 南京理工大学 | Method for reducing thermal conductivity of bismuth sulfide thermoelectric material |
| CN113511897A (en) * | 2021-04-25 | 2021-10-19 | 郑州大学 | Bi2S3Block thermoelectric material and high-voltage preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591103A (en) * | 2014-12-30 | 2015-05-06 | 华中科技大学 | Bi2Te3-xSx thermoelectric material and preparation method thereof |
| CN104692448A (en) * | 2015-03-18 | 2015-06-10 | 武汉理工大学 | Synthesis method of dynamic load of Ag2S (Silver Sulfide)-based compound and reactive assistant thereof |
| CN106418749A (en) * | 2016-10-11 | 2017-02-22 | 广东俏丹娜科技发展有限公司 | Detachable breathable massage bra |
| CN106418749B (en) * | 2016-10-11 | 2018-02-16 | 广东俏丹娜科技发展有限公司 | A kind of detachable type ventilating massage brassiere |
| CN106587135A (en) * | 2016-12-28 | 2017-04-26 | 中国科学院上海高等研究院 | I-doped Cu-S-based thermoelectric material and preparation methods thereof |
| CN106587135B (en) * | 2016-12-28 | 2017-12-29 | 中国科学院上海高等研究院 | Cu S base thermoelectricity materials of I doping and preparation method thereof |
| CN109659425A (en) * | 2018-12-29 | 2019-04-19 | 昆明理工大学 | A kind of bismuthino thermoelectric material and preparation method thereof promoting doping effect using barrier layer |
| CN109659425B (en) * | 2018-12-29 | 2020-07-10 | 昆明理工大学 | Bismuth-based thermoelectric material with doping effect improved by using barrier layer and preparation method thereof |
| CN111304492A (en) * | 2020-03-12 | 2020-06-19 | 中南大学 | Low-temperature n-type thermoelectric material and preparation method thereof |
| CN111304492B (en) * | 2020-03-12 | 2021-07-06 | 中南大学 | Low-temperature n-type thermoelectric material and preparation method thereof |
| CN112299482A (en) * | 2020-09-22 | 2021-02-02 | 南京理工大学 | Method for reducing thermal conductivity of bismuth sulfide thermoelectric material |
| CN112299482B (en) * | 2020-09-22 | 2022-09-27 | 南京理工大学 | Method for reducing thermal conductivity of bismuth sulfide thermoelectric material |
| CN113511897A (en) * | 2021-04-25 | 2021-10-19 | 郑州大学 | Bi2S3Block thermoelectric material and high-voltage preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN102280570B (en) | 2013-01-02 |
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