CN104409623B - Processing method for improving performance of N-type bismuth telluride base powder sinter block thermoelectric material - Google Patents
Processing method for improving performance of N-type bismuth telluride base powder sinter block thermoelectric material Download PDFInfo
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- CN104409623B CN104409623B CN201410562489.1A CN201410562489A CN104409623B CN 104409623 B CN104409623 B CN 104409623B CN 201410562489 A CN201410562489 A CN 201410562489A CN 104409623 B CN104409623 B CN 104409623B
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- 239000000463 material Substances 0.000 title claims abstract description 41
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 40
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 40
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000003672 processing method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000009413 insulation Methods 0.000 claims abstract description 5
- 239000011669 selenium Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 8
- 229910052714 tellurium Inorganic materials 0.000 claims description 6
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 5
- 229910052711 selenium Inorganic materials 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 3
- 238000003825 pressing Methods 0.000 abstract description 6
- 230000006698 induction Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 description 10
- 230000005619 thermoelectricity Effects 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 8
- 229910001152 Bi alloy Inorganic materials 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000004857 zone melting Methods 0.000 description 3
- 239000013590 bulk material Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001192 hot extrusion Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002908 (Bi,Sb)2(Te,Se)3 Inorganic materials 0.000 description 1
- 229910002899 Bi2Te3 Inorganic materials 0.000 description 1
- 101100379080 Emericella variicolor andB gene Proteins 0.000 description 1
- 229910001370 Se alloy Inorganic materials 0.000 description 1
- 230000005678 Seebeck effect Effects 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000005680 Thomson effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000002305 electric material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
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Abstract
The invention discloses a processing method for improving the performance of an N-type bismuth telluride base powder sinter block thermoelectric material. The method comprises the steps of placing an N-type bismuth telluride base block formed by thermal pressing in a mold, performing low-speed thermal deformation at 500-550 DEG C and under a pressure condition, controlling a change rate of the block in a height direction to be 0.2-3mm/min for 1-10min, then removing the pressure, performing thermal insulation for 2-60min, and repeating the procedure for at least one time. According to the processing method for improving the performance of the N-type bismuth telluride base sinter block thermoelectric material, the thermoelectric performance of the N-type bismuth telluride base material is greatly improved by using a repeated low-speed thermal deformation induction technology, and an optimal value can reach 1.2 which is the reported maximum value of an N-type material in the world at present.
Description
Technical field
The present invention relates to field of thermoelectric material technique, more particularly, to a kind of raising N-type bismuth telluride-base powder sintered block heat
The processing method of electric material performance.
Background technology
Thermoelectric material is a kind of new energy materialses that can be directly realized by heat energy and electric energy mutually conversion, and its mechanism builds on
On Seebeck effect, handkerchief note that effect and these three thermoelectric conversion effect of Thomson effect.In the past few decades, because the energy is asked
Topic is increasingly subject to the concern of people, and the research of thermoelectric material is hence into a new stage.Using p-type and N-type two and half
The series connection of conductor thermoelectric material can make thermoelectric cooling and power generating device.Thermo-electric device has pollution-free, noiseless, without motion portion
Part, without friction many advantages, such as.The conversion efficiency of thermo-electric device depends primarily on the dimensionless thermoelectric figure of merit of material：ZT=(α2
σ/κ)T.Wherein α is Seebeck coefficient, and σ is electrical conductivity, and κ is thermal conductivity, and T is thermodynamic temperature.
Bismuth telluride is current room temperature best performance nearby, commercial applications thermoelectric material the widest.The p-type tellurium of report at present
The ZT value changing bismuth alloy reaches 1.4, and the ZT value of N-type telluride bismuth alloy is relatively low.As Teo Sung Oh etc. (T.S.Oh,
D.B.Hyun,and N.V Kolomoets,Thermoelectric Properties of The Hot-Pressed(Bi,
Sb)2(Te,Se)3Alloys.Scripta Materialia,2000.42(9):Method system 849-854) utilizing powder metallurgy
Standby n type material maximum ZT value is 0.58.And for example, Jiang etc. (J.Jiang, L.D.Chen, Q.Yao, S.Q.Bai,
andQ.Wang,Effect of TeI4Content On The Thermoelectric Properties of n-type-
Bi-Te-Se Crystals Prepared by Zone Melting.Materials Chemistry and Physics,
2005.92(1):39-42.) it is prepared for, using zone-melting process, the N-type bismuth telluride material of Tel4 that adulterates, after doping, the ZT value of sample reaches
To 0.9.
In recent years it has been proposed that a kind of thermoelectricity optimizing bismuth telluride material by new hot extrusion technique and mechanical performance
Method, (S.J.Hong, Y.S.Lee, J.W.Byeon, andB.S.Chun, the Optimum Dopant such as such as Hong and Lee
Content of n-tyPe95%Bi2Te3+ 5%Bi2Se3Compounds Fabricated by Gas Atomization
and Extrusion Process.Journal of Alloys and ComPounds,2006.414(1-2):146-151)
By N-type Bi-Te-Se alloy carries out hot extrusion according to a certain percentage, the highest z-value studying the n type material obtaining is 0.92.
But the Z value being prepared using the method is mostly near 1, lifted more difficult again.
High performance thermo-electric device needs p-type and the thermoelectricity capability of n type material to match, so seek one kind can effectively carry
The processing technology of high N-type telluride bismuth alloy thermoelectricity capability is very meaningful.
Content of the invention
The present invention provides a kind of processing method improving N-type bismuth telluride-base sintering block thermoelectric material performance, using repetition
Low speed thermal deformation induced processes, are substantially improved the thermoelectricity capability of N-type bismuth telluride-base material.
A kind of processing method improving N-type bismuth telluride-base powder sintered block thermoelectric material performance, by hot-forming N-type
Bismuth telluride based bulk is placed in mould, 500～550 DEG C, carry out low speed thermal deformation under pressure condition, and control block is along short transverse
Rate of change be 0.2～3mm/min, after keeping 1～10min, remove pressure, be incubated 2～60min, repeat said process at least
Once.
Research through the present invention finds, the multiple dimensioned microeffect of thermal deformation induction, including micron-sized deformation texture, then
The in-situ nano of crystallization induction is brilliant, and the crystal defect of atom level can be effectively improved the thermoelectricity capability of material.These effects one side
Face can adjust carrier concentration and the transport process of bismuth telluride material internal, improves the electric property of material；On the other hand can
To scatter phonon, reduce the lattice thermal conductivity of material.Both sides collective effect leads to the significant increase of conducting material thermoelectricity performance.This
In invention, further by carrying out to sample repeatedly, low speed thermal deformation-isothermal holding, will effectively strengthen above effect, and then
Significantly lift the thermoelectricity capability of material.Especially in N-type bismuth telluride material, repeat the lifting to thermoelectricity capability for the low speed thermal deformation
Effect is rather notable.
Hot-forming N-type bismuth telluride-base bulk material is put in traditional dies, repeating low speed thermal deformation insulation can
To obtain the alloy sample of multiple deformation.By deformation velocity and the degree of Control Assay, sample is compressed to necessarily by every time
It is incubated after deformation extent.So repeatedly, until sample is completely filled with mould, you can obtain the excellent sample of thermoelectricity capability.
Described hot-forming N-type bismuth telluride based bulk is by being made up through hot pressed sintering of N-type commercialization telluride bismuth alloy
Block；
Or it is that the N-type polycrystal bismuth telluride sill being obtained by high pure element bismuth, tellurium, selenium melting is made through hot pressed sintering
Block.
Preferably, 1.25～2 times of a diameter of hot-forming N-type bismuth telluride based bulk diameter of described mould.?
Under identical rate of deformation, the size of mould affects the deformation extent of sample, and experiment proves that die size is too small, and deformation extent is relatively
Little, texture evolution is insufficient, and die size is excessive, easily because the effect of frictional force causes heterogeneous deformation, is unfavorable for entirety
The optimization of performance.
Preferably, the temperature of insulation is equal to the temperature of low speed thermal deformation.
Preferably, during described low speed thermal deformation, control block is 0.2～2.5mm/min along the rate of change of short transverse,
The time keeping is 1～2min.Further preferably, described hot-forming N-type bismuth telluride based bulk be by high pure element bismuth,
The block that the N-type polycrystal bismuth telluride sill that tellurium, selenium melting obtain is made through hot pressed sintering, control block under 550 DEG C, pressure
Rate of change along short transverse is 2.5mm/min, and time of holding is 1min, remove the temperature retention time after pressure be 2～
50min.Further preferably, removing the temperature retention time after pressure is 50min.It is further preferred that described N-type bismuth telluride-base bulk material is by height
Pure element bismuth, tellurium, selenium are according to chemical formula Bi2Te2.2Se0.8Proportioning is smelting, hot pressed sintering prepares.
Preferably, the number of times of described low speed thermal deformation-isothermal holding is 2～4 times.
The invention has the beneficial effects as follows：
The carrier concentration of multiple dimensioned microeffect controllable material of thermal deformation induction and material microstructure.Repeatedly, low
Speed heat deformation can effectively strengthen this effect, thus significantly improving the thermoelectricity capability of N-type bismuth telluride material, the present invention is successfully
The ZT value of n type material is brought up to 1.2, is the peak of the n type material reported in the world at present.
After high-performance P-type material composition device, conversion efficiency of thermoelectric can significantly be lifted.And entirely repeatedly
Can complete in same mould in low speed thermal deformation insulating process, production efficiency is greatly improved.
The processing method favorable repeatability of the present invention, effect is significant, regulation and control are simple, are that one kind produces high-performance N effectively
The method of type bismuth telluride material, has certain industrial utility value and theoretical significance.
Specific embodiment
Carry out next step below in conjunction with example to the present invention to elaborate：
Reference Example 1
From the N-type commercialization telluride bismuth alloy of zone-melting process preparation, the mould of Ф 12.6mm is put in ball mill grinding after sieving
Block is made after hot pressed sintering.The ZT value of sintered specimen reaches maximum 0.57 in 500K.
Reference Example 2
Using high pure element bismuth, tellurium, selenium according to chemical formula Bi2Te2.2Se0.8Proportioning, vacuum melting obtains ingot casting, ball milling mistake
Block is made after the mould heat pressure sintering putting into Ф 12.6mm after sieve.The ZT value of sintered specimen reaches maximum 0.52 in 450K.
Embodiment 1
Take in Reference Example 1 block of preparation, put in the mould of Ф 20mm, 500 DEG C, carry out low speed heat under pressure condition and become
Shape, control block is 0.3mm/min along the rate of change of short transverse, after keeping 2min, stops applying pressure, is incubated at 500 DEG C
5min.Then apply pressure again and carry out low speed thermal deformation, control block is 0.3mm/min along the rate of change of short transverse, becomes
Shape, to the complete mold filling of sample, obtains secondary thermal deformation sample.This sample ZT value in 500K is 0.87, sinters compared with Reference Example 1
Sample lifting 53%.
Embodiment 2
Take in Reference Example 1 block of preparation, put in the mould of Ф 20mm, 500 DEG C, carry out low speed heat under pressure condition and become
Shape, control block is 0.3mm/min along the rate of change of short transverse, after keeping 2min, stops applying pressure, is incubated at 500 DEG C
5min.Repeat identical operation, control block is 0.3mm/min along the rate of change of short transverse, holding 2min again, release,
It is incubated 5min at 500 DEG C.Last control block is 0.3mm/min along the rate of change of short transverse, is deformed into the complete mold filling of sample,
Obtain three thermal deformation samples.Recording this sample ZT value in 500K is 0.92, improves compared with sintered specimen in Reference Example 1
61%.
Embodiment 3
Take in Reference Example 1 block of preparation, put in the mould of Ф 20mm, 500 DEG C, carry out low speed heat under pressure condition and become
Shape, control block is 0.3mm/min along the rate of change of short transverse, after keeping 2min, stops applying pressure, is incubated at 500 DEG C
5min.Repeat identical and operate twice, control block is 0.3mm/min along the rate of change of short transverse, keeps 2min again,
Release, is incubated 5min at 500 DEG C.Last control block is 0.3mm/min along the rate of change of short transverse, is deformed into sample complete
Mold filling, obtains four thermal deformation samples.Recording the ZT value in 500K for this sample is 1.00, carries compared with sintered specimen in Reference Example 1
Rise 75.4%.
Embodiment 4
Take in Reference Example 2 block of preparation, put in the mould of Ф 20mm, 550 DEG C, carry out low speed heat under pressure condition and become
Shape, control block is 2.5mm/min along the rate of change of short transverse, after keeping 1min, stops applying pressure, is incubated at 550 DEG C
50min.Then again control block along short transverse rate of change be 2.5mm/min, be deformed into the complete mold filling of sample, obtain secondary
Thermal deformation sample.This sample ZT value in 450K is 1.1, improves 104% compared with sintered specimen in Reference Example 2.
Embodiment 5
Take in Reference Example 2 block of preparation, put in the mould of Ф 20mm, 550 DEG C, carry out low speed heat under pressure condition and become
Shape, control block is 2.5mm/min along the rate of change of short transverse, after keeping 1min, stops applying pressure, is incubated at 550 DEG C
50min.Repeat this process once, last control block is 2.5mm/min along the rate of change of short transverse, is deformed into sample complete
Mold filling, obtains three thermal deformation samples.This sample ZT value in 450K reaches 1.2, improves compared with sintered specimen in Reference Example 2
125%.
Comparative example 1
Take the block of preparation in Reference Example 1, put in the mould of Ф 20mm, the technique adopting forge hot at 550 DEG C, 80Mpa
The ZT value that pressurize 30min obtains final products is 0.82.
Comparative example 2
Take the block of preparation in Reference Example 2, put in the mould of Ф 20mm, the technique adopting forge hot at 550 DEG C, 80MPa
The ZT value that pressurize 30min obtains final products is 0.97.
Claims (6)
1. a kind of improve N-type bismuth telluride-base powder sintered block thermoelectric material performance processing method it is characterised in that step such as
Under：
Hot-forming N-type bismuth telluride based bulk is placed in mould, 500～550 DEG C, carry out low speed heat under pressure condition and become
Shape, control block is 0.2～3mm/min along the rate of change of short transverse, after keeping 1～10min, removes pressure, insulation 2～
60min, repeats said process at least one times；
1.25～2 times of a diameter of hot-forming N-type bismuth telluride based bulk diameter of described mould；
The temperature of insulation is equal to the temperature of low speed thermal deformation.
2. the processing method improving N-type bismuth telluride-base powder sintered block thermoelectric material performance according to claim 1, its
It is characterised by, described hot-forming N-type bismuth telluride based bulk is the N-type polycrystalline being obtained by high pure element bismuth, tellurium, selenium melting
The block that bismuth telluride-base material is made through hot pressed sintering.
3. the processing method improving N-type bismuth telluride-base powder sintered block thermoelectric material performance according to claim 1, its
Be characterised by, during described low speed thermal deformation, control block along short transverse rate of change be 0.2～2.5mm/min, holding when
Between be 1～2min.
4. the processing method improving N-type bismuth telluride-base powder sintered block thermoelectric material performance according to claim 3, its
It is characterised by, 550 DEG C, control block is 2.5mm/min along the rate of change of short transverse under pressure, the time of holding is 1min.
5. the processing method improving N-type bismuth telluride-base powder sintered block thermoelectric material performance according to claim 4, its
It is characterised by, removing the temperature retention time after pressure is 2～50min.
6. the processing method improving N-type bismuth telluride-base powder sintered block thermoelectric material performance according to claim 5, its
It is characterised by, the number of times of described low speed thermal deformation-isothermal holding is 2～4 times.
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| CN111435698A (en) * | 2019-01-14 | 2020-07-21 | 中国科学院宁波材料技术与工程研究所 | Bismuth telluride-based thermoelectric material and preparation method thereof |
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| CN115215658B (en) * | 2022-07-15 | 2023-08-08 | 湖北赛格瑞新能源科技有限公司 | Preparation method of n-type bismuth telluride-based ultrafine-grain thermoelectric material based on copper-assisted extrusion molding |
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Effective date of registration: 20171211 Address after: 310016 room B, room 1808, Sam Wo business square, No. 238, Jianggan District nautical Road, Hangzhou, Zhejiang Patentee after: Zhejiang electrical union Mining Technology Development Co., Ltd. Address before: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Patentee before: Zhejiang University |
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