CN107316935A - The preparation method of tellurium bismuthino thermoelectric material - Google Patents
The preparation method of tellurium bismuthino thermoelectric material Download PDFInfo
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- CN107316935A CN107316935A CN201710303830.5A CN201710303830A CN107316935A CN 107316935 A CN107316935 A CN 107316935A CN 201710303830 A CN201710303830 A CN 201710303830A CN 107316935 A CN107316935 A CN 107316935A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
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Abstract
The invention discloses a kind of preparation method of tellurium bismuthino thermoelectric material, the preparation method is first by p-type Bi x Sb 2‑x Te 3‑y Se y Alloy pig carries out a hot pressing, forms an alloy block, wherein 0.4≤x≤ 0.52,0≤y≤0.15;Alloy block is overturn to 90 ° of placements by axle of its length direction again, secondary hot pressing is carried out, obtains tellurium bismuthino thermoelectric material.The present invention obtains qualified tellurium bismuthino thermoelectric material by the way that the alloy pig after melting is directly carried out into hot pressing twice.Preparation method of the present invention is simple, and production efficiency is high, and the electric property and mechanical performance of obtained product are significantly improved.
Description
Technical field
The present invention relates to thermoelectric material field, more particularly, to a kind of preparation method of tellurium bismuthino thermoelectric material.
Background technology
Tellurium bismuthino solid solution alloy is as the best thermoelectric material of near room temperature performance, in thermo-electric generation and semiconductor refrigerating
Field is using quite varied.
At present, production tellurium bismuthino thermoelectric material is mainly two kinds, and one kind is zone refining, and another is to crush powder hot pressing processed
Processing.First method is to be prepared into the alloy pig obtained after melting using zone refining technique to be orientated polycrystalline or monocrystal rod.
This method has cost of investment low, easy large-scale production, the series of advantages such as product thermoelectricity capability is excellent.Though zone refining technique
So there is above-mentioned advantage, but shortcoming is equally obvious:The one side production cycle is longer, is that rod growth rate, crystal bar are melted in strict control zone
Production generally require after ten a few houres, the unqualified part of caput tail performance needs cutting process, causes waste of material;It is another
The machining property of aspect zone refining production sample is poor, and percent defective is high during following process.Second method be by
The alloy pig of melting or area melt rod and crush after powder processed, then using hot-pressing processing.This method can not damage original heat
On the basis of electrical property, the mechanical performance of product is improved.But this method crushes powder in pulverizing process and easily aoxidizes and introduce
Impurity, the fine dusts of generation are harmful, and pressing process is strict, and cost is high, and technological process is long, low production efficiency.
Product mechanical performance can directly be improved by seeking one kind, while maintaining the simple process of the excellent thermoelectricity capability of product is
Popular research direction.Molten alloy ingot is either crushed at powder hot pressing processed generally as intermediate products by subsequent sections melting
Reason, Chinese invention patent CN200810038766.3 discloses a kind of preparation method of bismuth telluride based sintered fuel, is with Bi2Te3
It is parent material that base, which melts rod, and oxide on surface is removed by sandblasting, and precompressed carries out discharge plasma sintering under vacuum
Crystal bar material, obtains agglomerated material.Chinese invention patent CN201410157880.3 discloses a kind of high property of utilization cold forming
Can thermoelectric material manufacture method:After pyroelectric ingot casting, carry out carrying out it under anaerobic up to 400MPa ~
2000MPa cold formings, heat treatment manufacture thermoelectric material.Chinese invention patent CN201410562489.1 discloses a kind of raising N
The processing method of the powder sintered block thermoelectric material performance of type bismuth telluride-base:It is that hot-forming bismuth telluride based bulk is placed in mould
In tool, the rate of change low speed thermal deformation along short transverse is controlled under 500 ~ 550 DEG C, pressure condition.Above-mentioned prior art
Rod is often melted as raw material using hot pressing block either area, pressing process need to prepare cost height, technological process through strict control
It is long.
Accordingly, it is desirable to provide a kind of preparation method of new tellurium bismuthino thermoelectric material.
The content of the invention
In view of this, the invention provides a kind of technique is simple, cost is low, good product performance tellurium bismuthino thermoelectric material
Preparation method.
To achieve these goals, technical scheme:A kind of preparation method of tellurium bismuthino thermoelectric material, first by p
Type Bi x Sb 2-x Te 3-y Se y Alloy pig carries out a hot pressing, forms an alloy block, wherein 0.4≤x≤ 0.52,0≤y≤0.15;
Alloy block is overturn to 90 ° of placements by axle of its length direction again, secondary hot pressing is carried out, obtains tellurium bismuthino thermoelectric material.
As a further improvement on the present invention, the temperature of a hot pressing be 250 ~ 350 DEG C, pressure be 5 ~ 30MPa.
As a further improvement on the present invention, the heating rate of a hot pressing is 5 ~ 10 DEG C/min.
As a further improvement on the present invention, the time of a hot pressing is 50 ~ 60min.
As a further improvement on the present invention, the temperature of the secondary hot pressing be 350 ~ 450 DEG C, pressure be 15 ~ 45MPa.
As a further improvement on the present invention, the heating rate of the secondary hot pressing is 10 ~ 20 DEG C/min.
As a further improvement on the present invention, the time of the secondary hot pressing is 5 ~ 60min.
As a further improvement on the present invention, two ends of an alloy block length direction need to cut off 0.5 respectively ~
3mm。
As a further improvement on the present invention, the p-type Bi x Sb 2-x Te 3-y Se y Alloy pig be by by purity be 4N and with
On Bi, Sb, Te, Se simple substance mixed according to stoichiometric proportion after, vacuum melting is formed.
As a further improvement on the present invention, the p-type Bi x Sb 2-x Te 3-y Se y Alloy pig prepare detailed process be:Press
Purity is weighed according to stoichiometric proportion to be placed in the glass tube of an end closure for Bi, Sb, Te, Se simple substance raw material of 4N and the above, with
Vacuum-pumping and sealing, charged glass tube is fixed on the pipe support in rocking furnace afterwards, and rocking furnace heating is until reach setting temperature
Melting is carried out after 650-710 DEG C of degree, smelting time is 10-30 min, and melting terminates, and pipe support is taken out rapidly, coagulated completely in alloy
Gu before beat pipe support and drive bubble in glass tube, it is 0.5-3min to catch up with the bubble time, glass tube then is cooled into room temperature, i.e.,
P-type Bi can be obtained x Sb 2-x Te 3-y Se y Alloy pig.
The present invention obtains qualified tellurium bismuthino thermoelectric material by the way that the alloy pig after melting is directly carried out into hot pressing twice.
Preparation method of the present invention is simple, and production efficiency is high, and the electric property and mechanical performance of obtained product are significantly improved.
Embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
The present invention proposes a kind of preparation method of tellurium bismuthino thermoelectric material, first by p-type Bi x Sb 2-x Te 3-y Se y Alloy pig is carried out
Hot pressing, forms an alloy block, wherein 0.4≤x≤ 0.52,0≤y≤0.15;Again by an alloy block with its length side
90 ° of placements are overturn to for axle, secondary hot pressing is carried out, obtains tellurium bismuthino thermoelectric material.
The present invention is first by p-type Bi x Sb 2-x Te 3-y Se y Alloy pig carries out a hot pressing:According to the big of hot pressing die
It is small, corresponding length is intercepted from alloy pig, a hot pressing is carried out.After after an alloy deblocking temperature cooling, by an alloy block
Two 0.5 ~ 3mm of Bottoming of length direction, then by its along its length for axle overturn 90 ° be placed in hot pressing die, carry out
Secondary hot pressing, obtains tellurium bismuthino thermoelectric material.
In certain embodiments of the present invention, the temperature of a hot pressing be 250 ~ 350 DEG C, pressure be 5 ~ 30MPa.
In certain embodiments of the present invention, the heating rate of a hot pressing is 5 ~ 10 DEG C/min.
In certain embodiments of the present invention, the time of a hot pressing is 50 ~ 60min.
In certain embodiments of the present invention, the temperature of the secondary hot pressing be 350 ~ 450 DEG C, pressure be 15 ~ 45MPa.
In certain embodiments of the present invention, the heating rate of the secondary hot pressing is 10 ~ 20 DEG C/min.
In certain embodiments of the present invention, the time of the secondary hot pressing is 5 ~ 60min.
P-type Bi x Sb 2-x Te 3-y Se y The preparation of alloy pig be by by Te, Bi, Sb simple substance that purity is 4N and the above according to
After stoichiometric proportion mixing, melting under vacuum is formed.
Above-mentioned p-type Bi x Sb 2-x Te 3-y Se y The specific forming process of alloy pig is:It is 4N to weigh purity according to stoichiometric proportion
And the Bi of the above, Sb, Te, Se simple substance raw material is placed in the glass tube of an end closure, sealing is subsequently vacuumed out, by charged glass
Glass pipe is fixed on the pipe support in rocking furnace, and rocking furnace heating carries out melting, melting until reaching after 650-710 DEG C of design temperature
Time is 10-30 min, and melting terminates, pipe support is taken out rapidly, pipe support is beaten before alloy solidifies completely and drives in glass tube
Bubble, it is 0.5-3min to catch up with the bubble time, and glass tube then is cooled into room temperature, you can obtain p-type Bi x Sb 2-x Te 3-y Se y Alloy
Ingot.
The preparation method for the tellurium bismuthino thermoelectric material that the present invention is provided, the alloy pig obtained after melting is directly carried out twice
Hot pressing, melts without area or crushes powder processed, so that it may obtain tellurium bismuthino thermoelectric material of good performance.The method that the present invention is provided,
Technique is simple, and production efficiency is high, and the product electric property and mechanical performance of preparation are significantly improved.
Embodiment 1.
P-type Bi0.52Sb1.48Te2.85Se0.15The preparation method of tellurium bismuthino thermoelectric material, comprises the following steps.
The first step, molten alloy ingot.
According to p-type Bi0.52Sb1.48Te2.85Se0.15Stoichiometric proportion weigh purity for 4N Bi, Sb, Te, Se simple substance in
In glass tube, by glass tube vacuum-pumping and sealing.Then the glass tube after sealing two ends is fixed on pipe support and is placed in rocking furnace
Melting 10min at a temperature of inherent 710 DEG C.Melting terminates, and pipe support is taken out rapidly, and pipe is beaten from lower to upper before alloy solidifies completely
Frame drives the bubble in glass tube, and it is 3min to catch up with the bubble time, is then cooled to room temperature, smashes glass tube and takes out alloy pig, i.e.,
P-type Bi can be obtained0.52Sb1.48Te2.85Se0.15Alloy pig.
Second step, forging and stamping processing.
By p-type Bi0.52Sb1.48Te2.85Se0.15Alloy pig interception is placed in hot-pressing processing in mould, is heated up with 5 DEG C/min fast
Degree rises to 250 DEG C and carries out an a hot pressing alloy block of formation, and the soaking time of a hot pressing is 50min, and pressure is
30MPa.Alloy block is overturn to 90 ° of placements by axle of its length direction, it is each end to end along its length to cut 0.5mm, with 10
DEG C/min programming rates rise to 450 DEG C of progress secondary hot pressings, the soaking time of secondary hot pressing is 5min, and pressure is 45MPa, i.e.,
Obtain p-type Bi0.52Sb1.48Te2.85Se0.15Tellurium bismuthino thermoelectric material.
Thermoelectricity capability test result according to the preparation-obtained sample of preparation method of the present invention is shown, originates melting sample
The electrical conductivity of product is 940 S/cm, and electromotive force rate is 180 μ V/K, and the electrical conductivity of sample is 820 S/cm after hot pressing twice,
Electromotive force rate value is 206 μ V/K.The bending tensile strength of sample brought up to by 30 MPa before hot pressing after hot pressing twice 50
MPa。
As a comparison, same composition raw material passes through 6h ball millings, and the electrical conductivity obtained after 360 DEG C of hot pressing 2h is 460
S/cm, electromotive force rate is 231 μ V/K.Electrical property according to the preparation-obtained sample of preparation method of the present invention is much better than ball milling
Obtained sample.
Embodiment 2.
P-type Bi0.4Sb1.6Te3The preparation method of tellurium bismuthino thermoelectric material, comprises the following steps.
The first step, molten alloy ingot.
According to p-type Bi0.4Sb1.6Te3Stoichiometric proportion weigh Bi, Sb, Te simple substance of the purity for 4N in glass tube, will
Glass tube vacuum-pumping and sealing.Then the glass tube after sealing two ends is fixed on pipe support and is placed in rocking furnace in 680 DEG C of temperature
The lower melting 20min of degree.Melting terminates, and pipe support is taken out rapidly, beats pipe support from lower to upper before alloy solidifies completely and drives glass
Bubble in pipe, it is 1min to catch up with the bubble time, is then cooled to room temperature, smashes glass tube and takes out alloy pig, you can obtains p-type
Bi0.4Sb1.6Te3Alloy pig.
Second step, forging and stamping processing.
By p-type Bi0.4Sb1.6Te3Alloy pig interception is placed in hot-pressing processing in mould, is risen to 10 DEG C/min programming rates
300 DEG C carry out a hot pressing and form an alloy block, and the soaking time of a hot pressing is 55min, and pressure is 15MPa.Will once
Alloy block overturns 90 ° of placements by axle of its length direction, each end to end along its length to cut 3mm, with 20 DEG C/min programming rates
400 DEG C of progress secondary hot pressings are risen to, the soaking time of secondary hot pressing is 30min, and pressure is 30MPa, that is, obtains p-type
Bi0.4Sb1.6Te3Tellurium bismuthino thermoelectric material.
Thermoelectricity capability test result according to the preparation-obtained sample of preparation method of the present invention is shown, originates melting sample
The electrical conductivity of product is 1000 S/cm, and electromotive force rate is 175 μ V/K, and the electrical conductivity of sample is 910 S/ after secondary hot pressing
Cm, electromotive force rate value is 196 μ V/K.The bending tensile strength of sample brought up to by 35 MPa before hot pressing after hot pressing twice 60
MPa。
As a comparison, same composition raw material passes through 6h ball millings, and the electrical conductivity obtained after 360 DEG C of hot pressing 2h is 560
S/cm, electromotive force rate is 217 μ V/K.Electrical property according to the preparation-obtained sample of preparation method of the present invention is much better than ball milling
Obtained sample.
Embodiment 3.
P-type Bi0.48Sb1.52Te2.9Se0.1The preparation method of tellurium bismuthino thermoelectric material, comprises the following steps.
The first step, molten alloy ingot.
According to p-type Bi0.48Sb1.52Te2.9Se0.1Stoichiometric proportion weigh purity for 4N Bi, Sb, Te, Se simple substance in glass
In glass pipe, by glass tube vacuum-pumping and sealing.Then the glass tube after sealing two ends is fixed on pipe support and is placed in rocking furnace
The melting 30min at a temperature of 650 DEG C.Melting terminates, and pipe support is taken out rapidly, and pipe support is beaten from lower to upper before alloy solidifies completely
The bubble in glass tube is driven, it is 0.5min to catch up with the bubble time, is then cooled to room temperature, smash glass tube and take out alloy pig, i.e.,
P-type Bi can be obtained0.48Sb1.52Te2.9Se0.1Alloy pig.
Second step, forging and stamping processing.
By p-type Bi0.48Sb1.52Te2.9Se0.1Alloy pig interception is placed in hot-pressing processing in mould, with 8 DEG C/min programming rates
Rise to 350 DEG C and carry out a hot pressing and obtain an alloy block, the soaking time of a hot pressing is that 60min, pressure are 5MPa.Will
Alloy block overturns 90 ° of placements by axle of its length direction, each end to end along its length to cut 2mm, is heated up with 15 DEG C/min
Speed rises to 350 DEG C of progress secondary hot pressings, and the soaking time of secondary hot pressing is that 60min, pressure are 15MPa, that is, obtains p-type
Bi0.48Sb1.52Te2.9Se0.1Tellurium bismuthino thermoelectric material.
Thermoelectricity capability test result according to the preparation-obtained sample of preparation method of the present invention is shown, originates melting sample
The electrical conductivity of product is 1100 S/cm, and electromotive force rate is 167 μ V/K, and the electrical conductivity of sample is 950 S/ after secondary compacting
Cm, electromotive force rate value is 193 μ V/K.The bending tensile strength of sample brought up to by 28 MPa before hot pressing after hot pressing twice 55
MPa。
As a comparison, same composition raw material passes through 6h ball millings, and the electrical conductivity obtained after 360 DEG C of hot pressing 2h is 680
S/cm, electromotive force rate is 227 μ V/K.Electrical property according to the preparation-obtained sample of preparation method of the present invention is much better than ball milling
Obtained sample.
The present invention obtains qualified tellurium bismuthino thermoelectric material by the way that the alloy pig after melting is directly carried out into hot pressing twice.
Preparation method of the present invention is simple, and production efficiency is high, and the electric property and mechanical performance of obtained product are significantly improved.
Although for example purpose, having been disclosed for the preferred embodiment of the present invention, the ordinary skill people of this area
Member will realize in the case of scope and spirit of the present invention disclosed in not departing from by appended claims, various to change
It is possible for entering, increasing and replacing.
Claims (10)
1. a kind of preparation method of tellurium bismuthino thermoelectric material, it is characterised in that:
First by p-type Bi x Sb 2-x Te 3-y Se y Alloy pig carries out a hot pressing, forms an alloy block, wherein 0.4≤x≤ 0.52,0
≤y≤0.15;
Alloy block is overturn to 90 ° of placements by axle of its length direction again, secondary hot pressing is carried out, obtains tellurium bismuthino thermoelectricity material
Material.
2. the preparation method of tellurium bismuthino thermoelectric material according to claim 1, it is characterised in that:The temperature of hot pressing
It is 5 ~ 30MPa to spend for 250 ~ 350 DEG C, pressure.
3. the preparation method of tellurium bismuthino thermoelectric material according to claim 2, it is characterised in that:The liter of hot pressing
Warm speed is 5 ~ 10 DEG C/min.
4. the preparation method of tellurium bismuthino thermoelectric material according to claim 2, it is characterised in that:Hot pressing when
Between be 50 ~ 60min.
5. the preparation method of tellurium bismuthino thermoelectric material according to claim 1, it is characterised in that:The temperature of the secondary hot pressing
It is 15 ~ 45MPa to spend for 350 ~ 450 DEG C, pressure.
6. the preparation method of tellurium bismuthino thermoelectric material according to claim 5, it is characterised in that:The liter of the secondary hot pressing
Warm speed is 10 ~ 20 DEG C/min.
7. the preparation method of tellurium bismuthino thermoelectric material according to claim 5, it is characterised in that:The secondary hot pressing when
Between be 5 ~ 60min.
8. the preparation method of tellurium bismuthino thermoelectric material according to claim 1, it is characterised in that:Alloy block length
Two ends in degree direction need to cut off 0.5 ~ 3mm respectively.
9. according to the preparation method of any described tellurium bismuthino thermoelectric material of claim 1 ~ 8, it is characterised in that:The p-type
Bi x Sb 2-x Te 3-y Se y Alloy pig is to be mixed by Bi, Sb, Te, Se simple substance by purity for 4N and the above according to stoichiometric proportion
Afterwards, vacuum melting is formed.
10. the preparation method of tellurium bismuthino thermoelectric material according to claim 9, it is characterised in that:The p-type Bi x Sb 2- x Te 3-y Se y Alloy pig prepare detailed process be:It is mono- for Bi, Sb, Te, Se of 4N and the above that purity is weighed according to stoichiometric proportion
Matter raw material is placed in the glass tube of an end closure, is subsequently vacuumed out sealing, charged glass tube is fixed in rocking furnace
On pipe support, rocking furnace heating carries out melting until reaching after 650-710 DEG C of design temperature, and smelting time is 10-30 min, melting
Terminate, pipe support is taken out rapidly, pipe support is beaten before alloy solidifies completely and drives bubble in glass tube, it is 0.5- to catch up with the bubble time
3min, is then cooled to room temperature by glass tube, you can obtain p-type Bi x Sb 2-x Te 3-y Se y Alloy pig.
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CN112079638A (en) * | 2020-09-22 | 2020-12-15 | 哈尔滨工业大学 | P-type bismuth telluride-based thermoelectric material with high thermoelectric and mechanical properties and preparation method thereof |
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 |
CN115141019A (en) * | 2022-07-15 | 2022-10-04 | 湖北赛格瑞新能源科技有限公司 | Method for preparing p-type bismuth telluride-based thermoelectric material by utilizing accumulated hot heading |
CN115141019B (en) * | 2022-07-15 | 2023-09-08 | 湖北赛格瑞新能源科技有限公司 | Method for preparing p-type bismuth telluride-based thermoelectric material by utilizing accumulated hot heading |
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