CN104495763A - Preparation method of bismuth-telluride-base thermoelectric material - Google Patents

Preparation method of bismuth-telluride-base thermoelectric material Download PDF

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Publication number
CN104495763A
CN104495763A CN201410768207.3A CN201410768207A CN104495763A CN 104495763 A CN104495763 A CN 104495763A CN 201410768207 A CN201410768207 A CN 201410768207A CN 104495763 A CN104495763 A CN 104495763A
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China
Prior art keywords
preparation
ampoule
crystal
thermoelectric material
tellurobismuthite
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CN201410768207.3A
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Chinese (zh)
Inventor
吴燕青
贺贤汉
荒木暉
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Shanghai Shenhe Thermo Magnetics Electronics Co Ltd
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Shanghai Shenhe Thermo Magnetics Electronics Co Ltd
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Priority to CN201410768207.3A priority Critical patent/CN104495763A/en
Publication of CN104495763A publication Critical patent/CN104495763A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/04—Binary compounds including binary selenium-tellurium compounds

Abstract

The invention relates to a preparation method of a bismuth-telluride-base thermoelectric material, which comprises the following steps: 1. carrying out synthesis on raw materials in a vacuum atmosphere; 2. sealing the obtained polycrystal in an ampoule bottle; and 3. putting the ampoule bottle into a crystal growth device, rotating the ampoule bottle, and evacuating the crystal growth device. Ampoule bottle vacuum insulation and Bi2Te3 alloy material rotation are adopted to perform crystal zone melting growth, thereby effectively preventing the growth interface from inclination due to nonuniform circumferential heat transfer; and the ampoule bottle filled with the Bi2Te3 alloy material is always in the vacuum state in the crystal growth process so as to the intercept the heat exchange between the crystal material surface and environment in the convection mode, so that the heat flow transfer direction is effectively controlled in the crystal growth process, the heat flow is led out along the crystal bar growth axis, and the growth interface is smoother, thereby effectively inhibiting the phenomenon of oblique crystallization.

Description

Take Tellurobismuthite as the preparation method of the thermoelectric material of base
Technical field
The invention belongs to thermoelectric material manufacturing technology field, particularly a kind of take Tellurobismuthite as the preparation method of the thermoelectric material of base.
Background technology
Thermoelectric generation technology is a branch of heat-electric direct energy conrersion, it utilizes Sai Beike (Seebeck) effect of material to be used for generating, peltier effect (peltier) carries out refrigeration, and its efficiency of conversion is determined by the index ZT of exosyndrome material thermoelectricity capability, wherein (wherein (α: the seebeck coefficient of material; σ: the specific conductivity of material; κ: the thermal conductivity of material); Earnestly explore through scientists since the 1950's, in succession occur Bi 2te 3, PbTe, CoSb 3, a series of excellent property such as SiGe thermoelectric material; Bi 2te 3and with Bi 2te 3thermoelectric material for base is still the thermo-electric conversion functional materials that working temperature is best near room temperature performance, commercialization degree is the highest up to now.Be widely used in fields such as optical communication, microelectronics, bio-instruments, aerospace.Along with the progress of related application technology, more and more higher expectation is proposed to the Performance And Reliability of thermo-electric device, also for thermoelectric material practitioner specifies the direction of effort.
Bi 2te 3crystalline structure belong to trigonal system (rhombohedral system), spacer as shown in Figure 1, can be considered hexahedron laminate structure along C direction of principal axis, have identical atom at same layer, layer and interlayer are in-Te (1)-Bi-Te (2)-Bi-Te (1)-Atomic Arrangement mode, wherein Te (1)-Bi is that covalent linkage and ionic linkage combine, Bi-Te (2)for covalent bonds, Te (1)-Te (1)cohesive Energy is more weak, closes, therefore Bi with Van der Waals bond 2te 3crystal is easy to, along the face perpendicular to crystal C axle, cleavage occurs.Bi 2te 3the anisotropy of crystalline structure, causes the strong anisotropy on thermoelectricity capability, has bibliographical information in the parallel and vertical cleavage difference to its thermoelectricity capability on direction:
Specific conductivity: σ /// σ ⊥≈ 4 ~ 10
Seebeck coefficient: α /// α ⊥≈ 1
Thermal conductivity: κ /// κ ⊥≈ 3 ~ 5
Figure of merit: Z /// Z ⊥≈ 2
The performance of monocrystal material is best theoretically, but due to manufacturing cost high, and be easy to cleavage, crack degradation, for obtaining the crystalline material having commercial value, the generally growing crystal from melt by Bridgman method or zone melting method.Xu Desheng " conductor refrigeration and utilisation technology " press of Shanghai Communications University 1991 describes Bridgman and zone melting growth Bi 2te 3the method of material, due to the arrangement mode between this crystal atoms and associative key form, easily along (00l) face cleavage.And the direction in (00l) face is relevant with the shape of solid-liquid interface during crystal growth, and the shape of solid-liquid interface is relevant with heat exchange between crystal and environment, desirable solid-liquid growth interface should be a plane, and normal direction is parallel with the desired direction of growth, from melt, obtained oriented crystal growth method all effectively do not control its growth interface form on one's own initiative in the past, no matter be Bridgman method or zone melting method, owing to being subject to heat exchange method, the particularly impact of thermal convection, its solid-liquid growth interface often center to the curved surface of melt inner projection, as shown in Figure 2, again due to the impact of circumferential heat exchange inequality, growth interface is asymmetric often, sometimes be tilt, larger angle is had in this case between the direction of growth of crystal and C axle, not only its thermoelectricity capability is subject to certain impact, and easily there is oblique crackle or corner incompleteness in thermoelectric element.
Chinese patent " a kind of preparation method of bismuth telluride-base thermoelectric material " (application number: 03150425.6) (hereinafter referred to as: D1) and Chinese patent " a kind of preparation method of bismuth telluride based sintered fuel " (application number: 200810038766.3) (hereinafter referred to as: D2) describe the method that sintering method prepares thermoelectric material, it is raw material that crystal bar is melted in these two kinds of method Dou Yi districts, D1 adopts powder sintered method, D2 adopts district to melt the method for the direct hot pressing of rear block, method described in D1 can not obtain the crystal of certain orientation degree, thermoelectricity capability is lower, the method of D2, though avoid in D1 the problem of the material orientation degree forfeiture adopting pressed by powder to bring, but processing power is by device-restrictive, inefficiency, be difficult to realize producing in enormous quantities, commercial value is little.
Summary of the invention
The object of the present invention is to provide a kind of take Tellurobismuthite as the preparation method of the thermoelectric material of base, should can grow the crystalline material with excellent thermoelectricity capability and mechanical property in this way.
For solving the problems of the technologies described above, the present invention take Tellurobismuthite as the preparation method of the thermoelectric material of base, comprises the steps: the first step, is synthesized by starting material under vacuum atmosphere; Second step, polycrystal sealing-in synthesis obtained is in ampoule; 3rd step, puts into crystal growing apparatus by ampoule, rotates ampoule, and bleeds to crystal growing apparatus.
In the described the first step, the temperature of synthesis is 700 DEG C ~ 800 DEG C.
In the described the first step, the time of synthesis is 60 minutes.
In described second step, the atmosphere in ampoule is vacuum or rare gas element.
In described 3rd step, ampoule to be arranged on crystal growing apparatus and to rotate ampoule by crystal growing apparatus.
In described 3rd step, by crystal growing apparatus, ampoule is heated in the process of bleeding.
In described 3rd step, the temperature of heating is 650 DEG C ~ 750 DEG C.
In described 3rd step, the velocity of rotation of rotation is 2RPM ~ 100RPM.
In described 3rd step, in described 3rd step, bleed until the pressure in silica tube in described crystal growing apparatus is less than 100Pa.
Crystalline growth velocity be 10 milli m/h ~ 35 milli m/h.
The present invention is that the preparation method of the thermoelectric material of base adopts ampoule vacuum insulation, Bi with Tellurobismuthite 2te 3the method that alloy material rotates carries out crystal growing by zone melting, and effectively prevent because circumference heat transfer is uneven, growth interface run-off the straight, makes Bi is housed 2te 3the ampoule of alloy material is located all the time under vacuum conditions in crystal growing process, block the heat exchange of convection type between crystalline material surface and environment, the direction of transfer of hot-fluid in crystal growth ground process is made to obtain effective control, hot-fluid is derived along boule growth direction of principal axis, growth interface is more tending towards smooth, effectively suppresses the phenomenon of oblique crystallization.Improve the thermoelectricity capability of material, suppress the oblique crackle of thermoelectric element because oblique crystallization causes or SOL; Not only increase thermoelectric element materials serviceability rate and utilization ratio, but also improve the maximum temperature difference of device.
Accompanying drawing explanation
Fig. 1 is Tellurobismuthite crystalline structure figure;
Growing crystal schematic diagram in Fig. 2 conventional melt;
Preparation method's crystal growing apparatus structural representation of Fig. 3 to be the present invention with Tellurobismuthite be thermoelectric material of base.
Embodiment
Be that the preparation method of the thermoelectric material of base is described in further detail with Tellurobismuthite to the present invention below in conjunction with accompanying drawing.
The present invention take Tellurobismuthite as the preparation method of the thermoelectric material of base, and concrete steps are:
1) material formulation:
A) P type, N-type is become to form Te, Sb, Bi, Se preparation of raw material:
P type: (Sb, Bi) 2te 3+ doping agent; N-type: Bi 2(Te, Se) 3+ doping agent.
B) by starting material by a certain percentage, under vacuum atmosphere, alloy material is synthesized.Synthesis temperature is 700 DEG C ~ 800 DEG C, and generated time is 60 minutes.
2) crystal growth:
A) synthesize the polycrystal sealing-in obtained in quartz or thermal glass ampoule, in ampoule, the atmosphere of bottle is vacuum or rare gas element.
B) be placed on crystal growing apparatus as shown in Figure 3 by the ampoule through sealing-in, vacuumize, pressure is less than 100Pa, furnace temp 650 DEG C ~ 750 DEG C.
C) turning axle velocity of rotation 2RPM ~ 100RPM.
D) crystalline growth velocity 10 milli m/h ~ 35 milli m/h.
The performance evaluation of material comprises: 1) obtained crystalline material through cutting, selected after the serviceability rate of element; 2) maximum temperature difference of device postevaluation device is assembled into the element of gained. the maximum temperature difference of device reflects the performance index Z value of material indirectly.
Adopt the material obtained by above-mentioned processing condition, the raising of its element serviceability rate reaches 75% ~ 85%, and the maximum temperature difference of device reaches 74.2 DEG C ~ 75.2 DEG C.
Experiment one
To consist of Sb 1.48bi 0.52te 3the P-type material of+3%Te is example, takes various starting material first according to the above ratio, puts into ampoule, vacuumize, and vacuum tightness is better than sealing-in after 5Pa; Ampoule after sealing-in is complete puts into the synthetic furnace that temperature is 800 DEG C, and generated time is 60 minutes; Ampoule after synthesis is put on the lower support frame 1 shown in Fig. 2, zone-melting temperature 750 DEG C, crystalline growth velocity 25 milli m/h.
Experiment two
To consist of Bi 2te 2.79se 0.21+ 0.087%TeI 4n type material be example, take various starting material first according to the above ratio, put into ampoule, vacuumize, vacuum tightness is better than sealing-in after 5Pa; Put into the synthetic furnace that temperature is 700 DEG C, generated time is 60 minutes; Ampoule after synthesis is put on the lower support frame 1 shown in lower Fig. 2; Zone-melting temperature 650 DEG C, crystalline growth velocity 20 milli m/h.
Experiment three,
To consist of Sb 1.48bi 0.52te 3the P-type material of+3%Te is example, takes various starting material first according to the above ratio, puts into ampoule, vacuumize, and vacuum tightness is better than sealing-in after 5Pa; Put into the synthetic furnace that temperature is 800 DEG C, generated time is 60 minutes; Ampoule after synthesis puts into the silica tube 2 shown in Fig. 3, is supported by ampoule undersetting, and vacuumize in silica tube 2, vacuum tightness is better than 100Pa; Zone-melting temperature 750 DEG C, crystalline growth velocity 35 milli m/h, back shaft rotating speed 100RPM.
Experiment four
To consist of Bi 2te 2.79se 0.21+ 0.087%TeI 4n type material be example, take various starting material first according to the above ratio, put into ampoule, vacuumize, vacuum tightness is better than sealing-in after 5Pa; Put into the synthetic furnace that temperature is 700 DEG C, generated time is 60 minutes; Ampoule after synthesis puts into the silica tube 2 shown in Fig. 3, is supported by ampoule undersetting, and vacuumize in silica tube 2, vacuum tightness is better than 100Pa; Zone-melting temperature 700 DEG C, crystalline growth velocity 10 milli m/h, back shaft rotating speed 50RPM.
Experiment five,
To consist of Sb 1.48bi 0.52te 3the P-type material of+3%Te is example, takes various starting material first according to the above ratio, puts into ampoule, vacuumize, and vacuum tightness is better than sealing-in after 5Pa; Put into the synthetic furnace that temperature is 800 DEG C, generated time is 60 minutes; Ampoule after synthesis puts into the silica tube 2 shown in Fig. 3, is supported by ampoule undersetting, and vacuumize in silica tube 2, vacuum tightness is better than 100Pa; Zone-melting temperature 750 DEG C, crystalline growth velocity 20 milli m/h, back shaft rotating speed 20RPM.
Experiment six
To consist of Bi 2te 2.79se 0.21+ 0.087%TeI 4n type material be example, take various starting material first according to the above ratio, put into ampoule, vacuumize, vacuum tightness is better than sealing-in after 5Pa; Put into the synthetic furnace that temperature is 700 DEG C, generated time is 60 minutes; Ampoule after synthesis puts into the silica tube 2 shown in Fig. 3, is supported by ampoule undersetting, and vacuumize in silica tube 2, vacuum tightness is better than 100Pa; Zone-melting temperature 700 DEG C, crystalline growth velocity 20 milli m/h, back shaft rotating speed 2RPM.
Experimental result
1) element serviceability rate:
Experiment one Experiment two Experiment three Experiment four Experiment five Experiment six
68.20％ 80.00％ 75.10％ 83.30％ 78.60％ 85.40％
2) device maximum temperature difference:
P material and the n type material of experiment two of experiment one are assembled into the maximum temperature difference 73.3 DEG C of device.
P material and the n type material of experiment four of experiment three are assembled into the maximum temperature difference 74.6 DEG C of device.
P material and the n type material of experiment two of experiment six are assembled into the maximum temperature difference 75.2 DEG C of device.
The present invention is that the preparation method of the thermoelectric material of base adopts ampoule vacuum insulation, Bi with Tellurobismuthite 2te 3the method that alloy material rotates carries out crystal growing by zone melting, and effectively prevent because circumference heat transfer is uneven, growth interface run-off the straight, makes Bi is housed 2te 3the ampoule of alloy material is located all the time under vacuum conditions in crystal growing process, block the heat exchange of convection type between crystalline material surface and environment, the direction of transfer of hot-fluid in crystal growth ground process is made to obtain effective control, hot-fluid is derived along boule growth direction of principal axis, growth interface is more tending towards smooth, effectively suppresses the phenomenon of oblique crystallization.Improve the thermoelectricity capability of material, suppress the oblique crackle of thermoelectric element because oblique crystallization causes or SOL; Not only increase thermoelectric element materials serviceability rate and utilization ratio, but also improve the maximum temperature difference of device.
Below the preferred embodiment of the invention is illustrated, but the invention is not limited to described embodiment, those of ordinary skill in the art also can make all equivalent modification or replacement under the prerequisite without prejudice to the invention spirit, and these equivalent modification or replacement are all included in the application's claim limited range.

Claims (10)

1. be the preparation method of the thermoelectric material of base with Tellurobismuthite, it is characterized in that, comprise the steps:
Starting material are synthesized by the first step under vacuum atmosphere;
Second step, polycrystal sealing-in synthesis obtained is in ampoule;
3rd step, puts into crystal growing apparatus by ampoule, rotates ampoule, and bleeds to crystal growing apparatus.
2. according to claim 1 take Tellurobismuthite as the preparation method of the thermoelectric material of base, and it is characterized in that, in the described the first step, the temperature of synthesis is 700 DEG C ~ 800 DEG C.
3. according to claim 2 take Tellurobismuthite as the preparation method of the thermoelectric material of base, and it is characterized in that, in the described the first step, the time of synthesis is 60 minutes.
4. according to claim 1 take Tellurobismuthite as the preparation method of the thermoelectric material of base, and it is characterized in that, in described second step, the atmosphere in ampoule is vacuum or rare gas element.
5. according to claim 1 take Tellurobismuthite as the preparation method of the thermoelectric material of base, it is characterized in that, in described 3rd step, to be arranged on by ampoule on crystal growing apparatus and to rotate ampoule by crystal growing apparatus.
6. according to claim 5 take Tellurobismuthite as the preparation method of the thermoelectric material of base, it is characterized in that, in described 3rd step, is heated in the process of bleeding by crystal growing apparatus to ampoule.
7. according to claim 6 take Tellurobismuthite as the preparation method of the thermoelectric material of base, and it is characterized in that, in described 3rd step, the temperature of heating is 650 DEG C ~ 750 DEG C.
8. according to claim 6 take Tellurobismuthite as the preparation method of the thermoelectric material of base, and it is characterized in that, in described 3rd step, the velocity of rotation of rotation is 2RPM ~ 100RPM.
9. according to claim 1 take Tellurobismuthite as the preparation method of the thermoelectric material of base, it is characterized in that, in described 3rd step, bleeds until the pressure in silica tube in described crystal growing apparatus is less than 100Pa.
10. according to claim 1 take Tellurobismuthite as the preparation method of the thermoelectric material of base, it is characterized in that, crystalline growth velocity is 10 millis m/h ~ 35 millis m/h.
CN201410768207.3A 2014-12-12 2014-12-12 Preparation method of bismuth-telluride-base thermoelectric material Pending CN104495763A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109399579A (en) * 2018-11-14 2019-03-01 有研工程技术研究院有限公司 A kind of chalcogenide compound synthesis uniforming device
CN114293260A (en) * 2021-11-24 2022-04-08 上海申和投资有限公司 Directional growth method of bismuth telluride thermoelectric material

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CN103046114A (en) * 2012-10-24 2013-04-17 上海大学 Preparation method of FeSb2 mono-crystal with superhigh Seebeck coefficient
CN103194790A (en) * 2013-04-03 2013-07-10 中山大学 Growth device and method for phosphorus-germanium-zinc single crystal
CN103555986A (en) * 2013-11-08 2014-02-05 河南城建学院 Method for preparing (Bi0.8Sb0.2)2Te3 nano thermoelectric material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101168836A (en) * 2006-10-25 2008-04-30 国家纳米技术与工程研究院 Method for preparing bismuth telluride alloy thin film by employing cosputtering sedimentation method
CN101656291A (en) * 2009-09-21 2010-02-24 吉林大学 Functional grade thermoelectric material n-PbTe and preparation method thereof
CN101956158A (en) * 2009-11-18 2011-01-26 九江学院 Preparation method of rare earth doped Bi2Te3 based thermoelectric film material
CN102403445A (en) * 2010-09-07 2012-04-04 中国科学院福建物质结构研究所 Bismuth telluride-based thermoelectric material and preparation method thereof
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CN103046114A (en) * 2012-10-24 2013-04-17 上海大学 Preparation method of FeSb2 mono-crystal with superhigh Seebeck coefficient
CN103194790A (en) * 2013-04-03 2013-07-10 中山大学 Growth device and method for phosphorus-germanium-zinc single crystal
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109399579A (en) * 2018-11-14 2019-03-01 有研工程技术研究院有限公司 A kind of chalcogenide compound synthesis uniforming device
CN114293260A (en) * 2021-11-24 2022-04-08 上海申和投资有限公司 Directional growth method of bismuth telluride thermoelectric material

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Application publication date: 20150408