CN102088058A - Preparation method for high-performance n-type bismuth telluride base thermoelectricity power generation material - Google Patents
Preparation method for high-performance n-type bismuth telluride base thermoelectricity power generation material Download PDFInfo
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- CN102088058A CN102088058A CN201010565758.1A CN201010565758A CN102088058A CN 102088058 A CN102088058 A CN 102088058A CN 201010565758 A CN201010565758 A CN 201010565758A CN 102088058 A CN102088058 A CN 102088058A
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- 239000000463 material Substances 0.000 title claims abstract description 59
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 36
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 32
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000010248 power generation Methods 0.000 title abstract description 9
- 230000005619 thermoelectricity Effects 0.000 title abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 40
- 239000011669 selenium Substances 0.000 claims abstract description 15
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 7
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004857 zone melting Methods 0.000 claims abstract description 7
- 238000003723 Smelting Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 10
- 230000005611 electricity Effects 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000011344 liquid material Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000002019 doping agent Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000003053 toxin Substances 0.000 abstract 1
- 231100000765 toxin Toxicity 0.000 abstract 1
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002918 waste heat Substances 0.000 description 4
- 229910001369 Brass Inorganic materials 0.000 description 3
- 239000010951 brass Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002001 electrolyte material Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a preparation method for a high-performance n-type bismuth telluride base thermoelectricity power generation material. High-purity tellurium blocks, bismuth blocks and selenium blocks which are industrially produced on a large batch serve as raw materials; after the raw materials are subjected to oxide layer removal and smashing, a proper quantity of dopant is added; the mixture is put into a processed glass tube after being weighed at a certain ratio; and an n-type bismuth telluride base thermoelectricity semiconductor crystal bar is obtained by packaging, smelting and zone-melting growth. At the temperature of 30-300 DEG C, the average ZT value is 0.75, and the average power factor is 4.5*10<-3>W. m. K<-2>. The adopted raw materials are cheap and easy to get, have the advantages of no toxin, environment protection, simple equipment process, low energy consumption and large yield and can be industrially produced on a large scale.
Description
Technical field
The present invention relates to the new material manufacturing, belong to the new energy materials field, particularly a kind of preparation method of high-performance n type bismuth telluride-based thermoelectric electricity generation material.
Background technology
New energy materials and technology are that the 21st century mankind can continue to develop one of indispensable important substance and technical foundation.Thermoelectric material is a kind of novel, eco-friendly new energy materials, and the application aspect thermoelectric cooling and thermoelectric power generation more and more widely.Because thermoelectric power generation possesses special advantages on low-temperature waste heat is recycled, and becomes main force's developing direction of following thermoelectric industry.Therefore, develop a kind of high-performance n type bismuth telluride-base thermoelectric material and satisfy the needs that the preparation of industrialization low-temperature waste heat reclaims the thermoelectric semiconductor generator of generating, it is reduced cost at energy output that institute serviceability temperature section increases unit materials, is in technical know-how and what experimental results show that all is the effective ways that energy utilization rate is improved in the use field of developing thermoelectric semiconductor.
Bismuth telluride-base thermoelectric material is to use best thermoelectric material near the current room temperature, also is the present industrialization raw material of ripe thermoelectric semiconductor industry the most.Though the transfer ratio of thermoelectric device is by the thermoelectric figure of merit of thermoelectric material
ZTThe value decision exists simultaneously
ZTUnder value and the little condition of Seebeck index variation, increase the valid approach that the unit materials energy output becomes reduction thermoelectric power generation device cost by improving its power factor.Guaranteeing under the little condition of Seebeck index variation, realizing reducing unit energy output cost by improving the energy output that internal resistance that conductivity of electrolyte materials reduces the device of doing improves unit materials.Over nearly 50 years, the employed n type of industrialization bismuth telluride-base thermoelectric material obtains maximum thermoelectric figure of merit near room temperature
ZTValue is used it near the thermoelectric cooling device that uses the preparation room temperature and can be obtained maximum conversion efficiency.But, with this material preparation thermoelectric power generation device, unit thermoelectric power generation cost height due to its power factor is low.This is that temperature commonly used is 80 ~ 300 ℃ because the serviceability temperature of power generating device is 30 ~ 400 ℃, and this bismuth telluride-base thermoelectric material average at this temperature section
ZTValue has descended nearly 40%.The room temperature that industrialization is produced in batches
ZTValue 1.1, and 80 ~ 300 ℃ average
ZTValue ability 0.65, the average power factor is 3.0 * 10
-3 W.m.K -2
At present, improve bismuth telluride-base thermoelectric material and be confined to its structure nanoization is reduced its lattice thermal conductivity significantly, increase Seebeck coefficient, and then improve under a certain temperature
ZTValue, rather than a certain serviceability temperature section
ZTThe energy output of value or unit materials.Simultaneously nanometer preparation cost not obvious to the raising of n type bismuth telluride-base material property, nanometer is expensive and need follow-up hot pressing or SPS to sinter block into, can't the large-batch industrial steady production and rest on the scientific research stage always.
Summary of the invention
The object of the present invention is to provide that a kind of raw material is cheap and easy to get, equipment is simple, technology is simple and easy to control, performance is even, long-term serviceability is stable, and can realize the method for the bar-shaped n bismuth telluride-based thermoelectric electricity generation material that extensive industrialization prepares.
Technical scheme of the present invention is, a kind of preparation method of high-performance n bismuth telluride-based thermoelectric electricity generation material, and its making step is as follows:
A kind of preparation method of high-performance n type bismuth telluride-based thermoelectric electricity generation material is characterized in that its making step is as follows:
(1) be after tellurium piece, bismuth piece and the selenium piece of 4N removed surface oxide layer, to pulverize with pulverizer respectively purity;
(2) be that an end high temperature melting of the glass tube of 10～38mm is shut and annealed with internal diameter, time 〉=1min, other end edge fuses smooth, rinses attachment in the glass tube with clean water, again with absolute ethyl alcohol dehydration back dry for standby;
(3) by stoichiometric proportion Bi
2(Te
1-xSe
x)
3+ ywt%TeI
4, x=0.06 ~ 0.08, y=0.1 ~ 0.17 takes by weighing Bi, Te and Se crushed material and TeI
4Powder places in the glass tube after the oven dry;
(4) vacuum degree that the glass tube of material will be housed be extracted into≤10Pa after, sealing from material plane 〉=3cm place;
(5) glass tube of sealing is placed 600 ~ 700 ℃ the smelting furnace that waves, ° wave by horizontal direction 〉=± 15, to the material fine melt, continue to wave 〉=1min, put into exhaust furnace afterwards, liquid material vibration air exhaust 〉=3min is erected at natural cooling in the air after the exhaust;
(6) glass tube that fusing exhaust aftershaping material is housed that obtains is vertically fixed on the zone melting furnace, by 700～800 ℃ of district's melting temperaturs, and the molten width 3～4cm in district, the speed of growth is 2.5 ± 1.0cm/h growth, natural cooling in the back air of having grown;
(7) break the glass bar of appearance into pieces, with crystal bar tip 30mm ± 10mm and afterbody 25mm ± 10mm excision.
Advantage of the present invention is, adopts bar-shaped n type bismuth telluride-based thermoelectric semiconductor crystal bar that this preparation method the obtains average dimensionless thermoelectricity capability figure of merit at 800 ~ 300 ℃ of temperature sections
ZTValue reaches more than 0.75, constant and the electric cost that increases by 1 times of unit energy output of leading of simultaneously average Seebeck coefficient descends nearly 50%, the power generating device industrialization of reclaiming for low-temperature waste heat provides the raw material of high-performance and low-cost to guarantee, and have that raw material is cheap and easy to get, equipment is simple, technology is simple and easy to control, performance is even, long-term serviceability is stablized, single furnace output 30Kg is with first-class advantage.
Description of drawings
Fig. 1 is a technological process block-diagram of the present invention.
Fig. 2 is prepared sample and the room temperature maximum of the present invention
ZTThe thermoelectricity capability and the temperature relation figure of value sample.
Fig. 3 is prepared sample and the room temperature maximum of the present invention
ZTThe thermoelectricity capability and the temperature relation figure of value sample.
Embodiment
Further specify preparation method's process of the present invention below by drawings and Examples, referring to Fig. 1, a kind of preparation method of high-performance n type bismuth telluride-based thermoelectric electricity generation material is a raw material with business-like high purity tellurium piece, bismuth piece and selenium piece, adds a certain amount of TeI
4After deoxidation layer, pulverizing, weighing according to a certain percentage is placed in the glass tube of handling well, through encapsulation, fusing, growing by zone melting, obtains n type bismuth telluride-based thermoelectric semiconductor crystal bar.Its making step is as follows:
(1) be after tellurium piece, bismuth piece and the selenium piece of 4N removed surface oxide layer with brass wire brush or blade, to pulverize with pulverizer respectively commercialization purity;
(2) be that an end of the glass tube of 10 ~ 38mm adopts propane or gas lamp to shut and anneal fully with internal diameter, time 〉=1min, other end edge fuses smooth, rinse attachment in the glass tube with clean water, after using glass cleaner, running water, washed with de-ionized water totally again, at last with dry for standby behind the dehydration of alcohol;
(3) by stoichiometric proportion Bi
2(Te
1-xSe
x)
3+ ywt%TeI
4, x=0.06 ~ 0.08, y=0.1 ~ 0.17 takes by weighing Bi, Te and Se crushed material and TeI
4Powder places in the glass tube after the oven dry;
(4) vacuum degree that the glass tube of material will be housed be extracted into≤10Pa after, sealing from material plane 〉=3cm place;
(5) glass tube of sealing is placed 600 ~ 700 ℃ the smelting furnace that waves, ° wave by horizontal direction 〉=± 15, to the material fine melt, continue to wave 〉=1min, make material mixing even, put into exhaust furnace afterwards, liquid material vibration air exhaust 〉=3min is erected at natural cooling in the air after the exhaust;
(6) glass tube that fusing exhaust aftershaping material is housed that obtains is vertically fixed on the zone melting furnace, by 700 ~ 800 ℃ of district's melting temperaturs, and the molten width 3 ~ 4cm in district, the speed of growth is 2.5 ± 1.0cm/h growth, natural cooling in the back air of having grown;
(7) break the glass bar of appearance into pieces,, promptly obtain the uniform and stable n type bismuth telluride-based thermoelectric semiconductor crystal bar of performance crystal bar tip 30mm ± 10mm and afterbody 25mm ± 10mm excision.
Embodiment 1:
Referring to Fig. 2, a kind of preparation method of high-performance n type bismuth telluride-based thermoelectric electricity generation material, its making step is as follows:
(1) be after tellurium piece, bismuth piece and the selenium piece of 4N removed surface oxide layer with brass wire brush or blade, to pulverize with pulverizer respectively commercialization purity;
(2) be that an end of the glass tube of 32mm adopts the propane lamp to shut and anneal fully with internal diameter, time 2min, other end edge fuses smooth, rinse foul in the glass tube with clean water, after using glass cleaner, running water, washed with de-ionized water totally again, at last with dry for standby behind the dehydration of alcohol;
(3) by stoichiometric proportion Bi
2(Te
1-xSe
x)
3+ ywt%TeI
4, x=0.07, y=0.15 gets Bi, Se and Te crushed material 1.70Kg altogether, adds the TeI of 0.15wt%
4Put in the glass tube after the oven dry;
(4) after the vacuum degree that the glass tube of material will be housed is extracted into 4Pa, sealing from material plane 3cm place;
(5) glass tube of sealing is placed 600 ~ 700 ℃ the smelting furnace that waves, ° wave, continue to wave 3min after putting the material fine melt by horizontal direction ± 15, make material mixing even, put into exhaust furnace afterwards, vibration air exhaust 3min is erected at natural cooling in the air after the exhaust;
The glass tube that fusing exhaust aftershaping material is housed that (6) will obtain is vertically fixed on the zone melting furnace, by 720 ℃ of district's melting temperaturs, and the molten width 3.5cm in district, the speed of growth is the 2.8cm/h growth, natural cooling in the back air of having grown;
(7) break the glass bar of appearance and excise tip 30mm into pieces, afterbody 25mm promptly obtains single long 280mm, the uniform and stable n type bismuth telluride-based thermoelectric semiconductor crystal bar of heavy 1.52Kg left and right sides performance.
Adopt preparation method of the present invention, single stove can once prepare 20, can obtain the uniform and stable n type bismuth telluride-based thermoelectric semiconductor crystal bar of performance of total weight 〉=30Kg.
Embodiment 2:
A kind of preparation method of high-performance n type bismuth telluride-based thermoelectric electricity generation material, its making step is as follows:
(1) be after tellurium piece, bismuth piece and the selenium piece of 4N removed surface oxide layer with brass wire brush or blade, to pulverize with pulverizer respectively commercialization purity;
(2) be that an end of the glass tube of 35mm adopts gas lamp to shut and anneal fully with internal diameter, time 〉=3min, other end edge fuses smooth, rinse attachment in the glass tube with running water, after using glass cleaner, running water, washed with de-ionized water totally again, at last with dry for standby behind the dehydration of alcohol;
(3) by stoichiometric proportion Bi
2(Te
1-xSe
x)
3+ ywt%TeI
4, x=0.06, y=0.14, Bi, Se and Te crushed material be 1.9Kg altogether, adds the TeI of 0.14wt%
4Put in the glass tube after the oven dry;
(4) after the vacuum degree that the glass tube of material will be housed is extracted into 3Pa, sealing from material plane 4cm place;
(5) glass tube of sealing is placed 600 ~ 700 ℃ the smelting furnace that waves, ° wave, to the material fine melt, continue to wave 2min by horizontal direction ± 20, make material mixing even, put into exhaust furnace afterwards, liquid material vibration air exhaust 4min is erected at natural cooling in the air after the exhaust;
(6) glass tube that fusing exhaust aftershaping material is housed that obtains is vertically fixed on the zone melting furnace, by 750 ℃ of district's melting temperaturs, and the molten width 4cm in district, the speed of growth is the 3.0cm/h growth, natural cooling in the back air of having grown;
(7) break the glass bar of appearance into pieces,, promptly obtain the uniform and stable n type bismuth telluride-based thermoelectric semiconductor crystal bar of performance crystal bar tip 35mm and afterbody 30mm excision.
In sum, preparation method's of the present invention advantage is:
(1) but employed raw material is cheap and easy to get, asepsis environment-protecting, apparatus and process is simple, energy consumption is low, the big large-scale industrial production of output;
(2) N-shaped bismuth telluride-based thermoelectric semi-conducting material is the bar-shaped of diameter 10 ~ 38mm, and length can reach 40cm, does not have obvious crackle, inner pore-free, and satisfactory mechanical property can directly be used for cutting the preparation thermoelectric semiconductor power generator;
(3) the bismuth telluride-based thermoelectric semiconductor material performance is uniform and stable, in the average dimensionless thermoelectricity capability figure of merit of 30 ~ 300 ℃ of temperature sectionsZTValue reaches more than 0.75, and the mean power factor reaches 4.5 * 10-3 W.m.K -2 Strengthened the serviceability temperature scope of power generating device, improved energy conversion rate and lowered the cost of unit thermoelectric power generation, solved low-temperature waste heat and reclaimed the technical barrier of thermoelectric power generation industrialization;
(4) serviceability temperature endZTBe worth controlled: by regulating the proportioning of raw material, obtain the average dimensionless thermoelectricity capability figure of merit of 30-400 ℃ interior certain section serviceability temperature of temperature rangeZTValue and the constant lower power factor maximum of Seebeck coefficient, acquisition is applicable to the material of temperature required section use.
Claims (1)
1. the preparation method of a high-performance n type bismuth telluride-based thermoelectric electricity generation material is characterized in that its making step is as follows:
(1) be after tellurium piece, bismuth piece and the selenium piece of 4N removed surface oxide layer, to pulverize with pulverizer respectively purity;
(2) be that an end high temperature melting of the glass tube of 10～38mm is shut and annealed with internal diameter, time 〉=1min, other end edge fuses smooth, rinses attachment in the glass tube with clean water, again with absolute ethyl alcohol dehydration back dry for standby;
(3) by stoichiometric proportion Bi
2(Te
1-xSe
x)
3+ ywt%TeI
4, x=0.06 ~ 0.08, y=0.1 ~ 0.17 takes by weighing Bi, Te and Se crushed material and TeI
4Powder places in the glass tube after the oven dry;
(4) vacuum degree that the glass tube of material will be housed be extracted into≤10Pa after, sealing from material plane 〉=3cm place;
(5) glass tube of sealing is placed 600 ~ 700 ℃ the smelting furnace that waves, ° wave by horizontal direction 〉=± 15, to the material fine melt, continue to wave 〉=1min, put into exhaust furnace afterwards, liquid material vibration air exhaust 〉=3min is erected at natural cooling in the air after the exhaust;
(6) glass tube that fusing exhaust aftershaping material is housed that obtains is vertically fixed on the zone melting furnace, by 700～800 ℃ of district's melting temperaturs, and the molten width 3～4cm in district, the speed of growth is 2.5 ± 1.0cm/h growth, natural cooling in the back air of having grown;
(7) break the glass bar of appearance into pieces, with crystal bar tip 30mm ± 10mm and afterbody 25mm ± 10mm excision.
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Cited By (7)
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| CN103456877A (en) * | 2013-06-25 | 2013-12-18 | 陈志明 | Manufacturing method of N type semiconductor element for refrigeration or heating device |
| CN104831344A (en) * | 2015-04-29 | 2015-08-12 | 河南鸿昌电子有限公司 | Crystal pulling method of semiconductor crystal bar |
| CN105060260A (en) * | 2015-08-27 | 2015-11-18 | 广东先导稀材股份有限公司 | Method for preparing tellurium tetraiodide |
| CN106571422A (en) * | 2016-11-09 | 2017-04-19 | 苏州科技大学 | Bismuth telluride based N type thermoelectric material and preparation method thereof |
| CN110002412A (en) * | 2019-04-22 | 2019-07-12 | 武汉科技大学 | A kind of preparation method of preferred orientation N-shaped bismuth telluride-base polycrystalline bulk thermoelectric material |
| CN112289919A (en) * | 2020-10-30 | 2021-01-29 | 中国电子科技集团公司第十八研究所 | Preparation method of N-type bismuth telluride polycrystalline block thermoelectric material |
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| JP2016529188A (en) * | 2013-06-25 | 2016-09-23 | ジミン チェン、 | Method for manufacturing n-type semiconductor element for cooling or heating device |
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| CN105060260A (en) * | 2015-08-27 | 2015-11-18 | 广东先导稀材股份有限公司 | Method for preparing tellurium tetraiodide |
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| CN106571422B (en) * | 2016-11-09 | 2022-03-22 | 苏州科技大学 | Bismuth telluride-based N-type thermoelectric material and preparation method thereof |
| CN110002412A (en) * | 2019-04-22 | 2019-07-12 | 武汉科技大学 | A kind of preparation method of preferred orientation N-shaped bismuth telluride-base polycrystalline bulk thermoelectric material |
| CN112289919A (en) * | 2020-10-30 | 2021-01-29 | 中国电子科技集团公司第十八研究所 | Preparation method of N-type bismuth telluride polycrystalline block thermoelectric material |
| CN114835495A (en) * | 2021-02-01 | 2022-08-02 | 中国科学院宁波材料技术与工程研究所 | Preferentially oriented n-type bismuth telluride sintered material and preparation method and application thereof |
| CN114835495B (en) * | 2021-02-01 | 2024-02-23 | 中国科学院宁波材料技术与工程研究所 | Preferred orientation n-type bismuth telluride sintered material and preparation method and application thereof |
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