CN106571422B - Bismuth telluride-based N-type thermoelectric material and preparation method thereof - Google Patents
Bismuth telluride-based N-type thermoelectric material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 12
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 11
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000010453 quartz Substances 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000004857 zone melting Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims abstract description 4
- OCVXZQOKBHXGRU-UHFFFAOYSA-N iodine(1+) Chemical compound [I+] OCVXZQOKBHXGRU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 239000011669 selenium Substances 0.000 claims 5
- 238000001816 cooling Methods 0.000 claims 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000004886 process control Methods 0.000 claims 2
- 229910052714 tellurium Inorganic materials 0.000 claims 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims 1
- 238000000137 annealing Methods 0.000 claims 1
- 238000009826 distribution Methods 0.000 claims 1
- 230000005284 excitation Effects 0.000 claims 1
- 229910052711 selenium Inorganic materials 0.000 claims 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical group [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 2
- 239000013590 bulk material Substances 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 229910002899 Bi2Te3 Inorganic materials 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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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- 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
- H10N10/01—Manufacture or treatment
Abstract
The invention discloses a bismuth telluride base N-type thermoelectric material and a preparation method thereof. The synthesis is carried out by adopting a two-step method of melt mixing and zone melting. The synthesis method comprises the following steps: the optional simple substance raw material is added according to Bi2(Te1‑xSex)3X is more than or equal to 0.02 and less than or equal to 0.1, the chemical formula content is weighed, and 0.01 to 0.03 weight percent of metallic antimony (Sb) and 0.03 to 0.06 weight percent of non-metallic iodine (I) are added on the basis of the weighed amount; putting the quartz tube into a quartz tube with a flat sintered bottom for vacuumizing and tube sealing, then putting the quartz tube into a resistance heating swing furnace, placing the quartz tube at a vertical position, and mixing the quartz tube by melting to sinter. After sintering is finished and the quartz tube is naturally cooled to room temperature, the quartz tube is taken out and placed on a vertical zone melting furnace for pulse zone melting. The invention has the advantages that: the preparation method is simple, and the bulk material with high density, near single crystal structure and a small amount of nano-crystalline grain mosaic can be obtained.
Description
Technical Field
The invention relates to a bismuth telluride-based thermoelectric material Bi2(Te1-xSex)3And a preparation method thereof, belonging to the field of inorganic materials.
Background
Bi2Te3The base compound is the first thermoelectric material discovered and studied, and is also the most widely used commercial medium-temperature thermoelectric material at present. The limit ZT of its thermoelectric performance has been around-1 for a long time. With the development of nanotechnology, Bi2Te3The research focus of the base thermoelectric material also turns to the Bi with the nanometer scale2Te3And (3) preparing the base thermoelectric material. Hydrothermal preparation of Bi2Te3Nanotubes and also electrochemically deposited Bi2Te3Preparation of Bi by base nanowire array, laser pulse deposition, metal organic chemical vapor deposition and other methods2Te3A film. Wherein BedPoudel et al grind p-type BiSbTe crystal into nano powder by a ball mill, and then carry out hot pressing, and the ZT value obtained by measurement can reach 1.4 near 370K. However, fromThe nano structure is easy to be damaged in the thermal cycle process and is not easy to be processed into devices, and the like, and the nano Bi2Te3The development of the base thermoelectric material is greatly limited, and it is difficult to implement large-scale industrial application, so that the development of the bulk thermoelectric material with high thermoelectric performance becomes a new trend for the industrial application of the thermoelectric material.
Disclosure of Invention
The invention aims to provide a synthesis method for preparing a bismuth telluride-based N-type thermoelectric material by combining a traditional simple solid-phase reaction method and a zone melting method.
In order to achieve the purpose, the invention adopts the technical scheme that: bismuth telluride-based N-type thermoelectric material Bi2(Te1-xSex)3The preparation method of (1). Bi with higher ZT value is prepared by traditional simple solid phase reaction and doping and zone melting combined method2Te3An N-type thermoelectric material. By adding Bi2(Te1-xSex)3Properly changing Bi content in normal chemical proportion of base thermoelectric material to synthesize Bi2(Te1-xSex)3A compound polymorph. The bismuth telluride-based N-type thermoelectric material Bi of the invention2(Te1-xSex)3The preparation method and the test method comprise the following steps:
1. the preparation method comprises the following steps:
1) the optional simple substance raw material is added according to Bi2(Te1-xSex)3X is more than or equal to 0.02 and less than or equal to 0.1, the chemical formula content is weighed, and the Bi content can be increased by 0.3 to 0.8 percent by weight on the basis of normal chemical mixture ratio; adding 0.01-0.03 wt% of metallic antimony (Sb) and 0.03-0.06 wt% of non-metallic iodine (I) on the basis of the weighed amount, wherein the purity of all simple substance raw materials is more than 4N;
2) loading the weighed materials into a quartz tube with a flat sintered bottom for vacuumizing and tube sealing, then loading into a resistance heating swing furnace, vertically placing the quartz tube, reacting at 810 +/-10 ℃ for 10-15 hours, swinging the furnace body irregularly in the reaction process, controlling the swing frequency at 0.04-0.08Hz, and swinging the furnace field until the temperature indicated value is constant, wherein the swing time fluctuates from the beginning of swinging due to the temperature of the furnace field; the time interval of the two adjacent swaying times is 0.5 to 1 hour, and the relaxation time required for the uniformity of the components of the melt is achieved mainly according to the full combination of different simple substance atoms in the melt and the mutual transmission and diffusion among the melts;
3) after the reaction is finished, the quartz tube is placed at a vertical position, then the temperature is slowly reduced to 700 +/-5 ℃ at the speed of 3 ℃/h +/-1 ℃/h, the temperature is maintained for 1 to 2 hours, then the temperature is reduced to 650 +/-5 ℃ at the speed of 5 ℃/h +/-0.5 ℃/h, and then the quartz tube is naturally cooled to the room temperature after being annealed for 3 hours at the temperature;
4) taking out the quartz tube with the temperature reduced to room temperature from the resistance-heated rocking furnace, placing the quartz tube on a vertical zone melting furnace for pulse zone melting, and moving a heating body from bottom to top. The zone melting process comprises the following steps: the zone melting temperature is 780-810 ℃, the quartz tube is static, and the heating body is driven by a variable frequency control motor to move from bottom to top at the moving speed of 0.06-0.12 mm/min; secondly, in the zone melting process, the quartz tube is transversely vibrated for 2-3 minutes by a vibration pump every 1-1.5 hours, the amplitude is 0.5-1 mm, and the frequency is 50 Hz. The polycrystalline material crystallized according to the process comprises grain mosaic of 100nm to 300nm, reduces the thermal conductivity of the material, improves the Seebeck coefficient of the material at the same time,
5) and after the heating body is lifted to the position above the top of the material in the tube, the material synthesis is finished after the material in the quartz tube is observed to be crystallized.
2. The test method comprises the following steps: the electrical conductivity and seebeck coefficient measurements were performed on ULVAC ZEM-3, the thermal diffusivity test was performed on a relaxation-resistant laser thermal conductivity meter (Netzsch LFA 467) (argon atmosphere, pyroceram9606 as standard), and the thermal conductivity was calculated from the formula κ (T) ═ α (T) × cp (T) × ρ (T). Wherein α (T) denotes a thermal diffusion coefficient, cp (T) denotes a pressure heat capacity, and ρ (T) denotes a density of the test sample.
The invention has the following beneficial effects:
1. the requirement on the purity of raw materials is low (only 4N), the preparation process is simple, and the traditional solid-phase reaction combined with a zone melting method can directly obtain the block material with high density and good uniformity.
2. Because a pulse zone melting method is adopted, crystal grains of 100nm to 300nm are introduced into the polycrystalline material for embedding, the thermal conductivity of the material is reduced, the Seebeck coefficient of the material is improved, and the remarkable improvement of the thermoelectric property of the block material is realized;
3. bi of the present invention2(Te1-xSex)3The compound has outstanding thermoelectric performance and high compactness, and is likely to be applied to the fields of waste heat recovery, space exploration and the like.
Drawings
FIG. 1 shows Bi2(Te1-xSex)3A graph of seebeck coefficient versus temperature;
FIG. 2 shows Bi2(Te1-xSex)3A plot of resistivity versus temperature;
FIG. 3 shows Bi2(Te1-xSex)3Graph of thermal conductivity versus temperature;
FIG. 4 shows Bi2(Te1-xSex)3Graph of thermoelectric performance values (ZT values).
Detailed Description
Example 1:
the optional simple substance raw material is added according to Bi2(Te0.92Se0.08)3Weighing the chemical formula, wherein Te is 500 g, and the Bi content can be increased by 0.4 percent by weight on the basis of normal chemical mixture ratio; adding 0.02 wt% of metal antimony (Sb) and 0.03 wt% of non-metal iodine (I) on the basis of the weighed amount, wherein the purity of all elementary substance raw materials is more than 4N;
the weighed materials are put into a quartz tube with a flat sintered bottom for vacuumizing and tube sealing, then the quartz tube is put into a resistance heating swing furnace, the quartz tube is vertically placed for reaction at 800 ℃ for 12 hours, the furnace body is swung irregularly in the reaction process, firstly, the swing frequency is controlled at 0.04Hz, the swing time fluctuates from the beginning of swing of the furnace field temperature until the temperature indicated value is constant; secondly, the interval of the two adjacent swinging times is 50 minutes, after the reaction is finished, the quartz tube is placed at a vertical position, then the temperature is slowly reduced to 700 ℃ at the speed of 3 ℃/h, the temperature is maintained for 1 hour, then the temperature is reduced to 65 ℃ at the speed of 5 ℃/h, and then the quartz tube is naturally cooled to the room temperature after being annealed for 3 hours at the temperature; taking out the quartz tube with the temperature reduced to room temperature from the resistance-heated rocking furnace, placing the quartz tube on a vertical zone melting furnace for pulse zone melting, and moving a heating body from bottom to top. The zone melting process comprises the following steps: the zone melting temperature is 790 ℃, the quartz tube is static, and the heating body is driven by a variable frequency control motor to move from bottom to top at the moving speed of 0.08 mm/min; secondly, in the zone melting process, transverse vibration is applied to the quartz tube for 2 minutes by a vibration pump every 1.5 hours, the amplitude is 0.5mm, and the frequency is 50 Hz. And after the heating body is lifted to the position above the top of the material in the tube, the material synthesis is finished after the material in the quartz tube is observed to be crystallized.
Example 2:
cutting and polishing sample (Bi)1-xSbx)2Te3And performing thermoelectric performance test. (Bi) prepared by the above method1- xSbx)2Te3The block samples were cut with a wire cutter and then sanded. Cutting basic wafers and cuboid samples by a cutting machine, and then polishing by abrasive paper; the disc samples were 2.0mm thick and 12.0mm in diameter. The cross-sectional area of the cuboid was 2.5 x 2.5mm2 and the wafers were tested for thermal diffusivity on a relaxation resistant (NETZSCH) LFA467 laser thermal conductivity meter using pyropream 9606 as a standard and tested under an argon atmosphere. The samples were tested for conductivity and seebeck coefficient on ULVAC ZEM-3.
Example 3:
sample (Bi)1-xSbx)2Te3Thermoelectric performance test results of
The above test results show that the resistivity increases with increasing temperature, from 10.1 x 10-6 Ω m at room temperature to 2.7 x 10-5 Ω m at 480K. The absolute value of the Seebeck coefficient increases with the temperature, and reaches a maximum of 247 muV/K at 320KAnd then decreased. Seebeck coefficient is positive (Bi)1-xSbx)2Te3Is a hole. The thermal conductivity becomes smaller with increasing temperature, wherein the thermal conductivity around room temperature is 1.3W/m.K. According to the figure of merit calculation formula of the thermoelectric material: (Bi) S2 sigma/K, where S is the Seebeck coefficient of the material, sigma is the electrical conductivity, and K is the thermal conductivity, can be obtained1-xSbx)2Te3The ZT value of the sample was 1.33 at 340K.
Claims (4)
1. Bismuth telluride-based N-type thermoelectric material Bi2(Te1-xSex)3The preparation method is characterized by comprising the following process steps: the optional simple substance raw material is added according to Bi2(Te1-xSex)3X is more than or equal to 0.02 and less than or equal to 0.1, the chemical formula content is weighed, 0.01 to 0.03 weight percent of metallic antimony (Sb) and 0.03 to 0.06 weight percent of non-metallic iodine (I) are added on the basis of the weighed amount, and the purity of all elementary substance raw materials is more than 4N; loading the quartz tube into a quartz tube with a flat sintered bottom for vacuumizing and tube sealing, then loading the quartz tube into a resistance heating swing furnace, vertically placing the quartz tube, reacting for 20 to 30 hours at 810 +/-10 ℃, swinging the furnace body irregularly during the reaction process, placing the quartz tube to a vertical position after the reaction is finished, slowly cooling to 700 +/-5 ℃ at the speed of 3 ℃/h +/-1 ℃/h, preserving heat for 1 to 2 hours, then cooling to 650 +/-5 ℃ at the speed of 5 ℃/h +/-0.5 ℃/h, then annealing for 3 hours, naturally cooling to room temperature, taking out the quartz tube, and placing the quartz tube on a vertical zone melting furnace for pulse zone melting;
the untimely swinging of the furnace body in the reaction process is realized by the following process control: a. the swinging frequency is controlled to be 0.04-0.08Hz, the temperature of the furnace body fluctuates after the swinging is started, and the swinging time is determined by the balance relaxation time of the temperature of the furnace body; b. the time interval between the adjacent two times of swinging is 0.5 to 1 hour;
the pulse zone melting is characterized in that transverse pulse vibration excitation is carried out under the framework of the traditional zone melting, and the pulse zone melting is realized through the following process control: a. the zone melting temperature is 780-810 ℃, the quartz tube is static, and the heating body controls the motor to drive to move from bottom to top in a frequency conversion way, and the moving speed is 0.06-0.12 mm/min; b. in the zone melting process, transverse vibration with amplitude of 0.5mm-1mm and frequency of 50Hz is applied to the quartz tube by the vibration pump every 1 hour-1.5 hours for 2 minutes-3 minutes.
2. The bismuth telluride-based N-type thermoelectric material Bi as claimed in claim 12(Te1-xSex)3The preparation method is characterized by comprising the following steps: the purity of the selected elementary substance raw materials Bi, Te and Sb reaches 4N, wherein the ratio of Bi: nominal molar ratio of (TeSe) 2: 3, doping trace selenium (Se) at the position of tellurium (Te), wherein x is more than or equal to 0.02 and less than or equal to 0.1, and the content of Bi can be increased by 0.3 to 0.8 percent by weight on the basis of normal chemical mixture ratio.
3. The production method according to claim 1 or 2, characterized in that: the bismuth telluride-based N-type polycrystalline material obtained by the process has the following microstructure characteristics: a. grain size distribution range: 100nm to centimeter, wherein the crystal grain of 100nm-300nm accounts for 1-3% of the volume ratio; b. the density of the material reaches 96.5 percent.
4. The production method according to claim 3, characterized in that: the non-dimensionality figure of merit ZT of the prepared bismuth telluride base N-type polycrystal reaches 1.33 at 340K.
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| CN108550689B (en) * | 2018-05-25 | 2021-10-22 | 北京石油化工学院 | Preparation method of N-type bismuth telluride-based thermoelectric material |
| CN111477736B (en) * | 2019-01-24 | 2022-09-16 | 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 |
| CN110408986B (en) * | 2019-07-16 | 2020-08-04 | 江阴市赛贝克半导体科技有限公司 | Zone melting-directional solidification furnace and synthesis method of semiconductor 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 |
| 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 |
| CN113716531B (en) * | 2021-09-01 | 2024-02-09 | 中国科学技术大学 | Solid-phase synthesis method of narrow-bandgap semiconductor MTeI |
| CN114561687B (en) * | 2022-02-28 | 2023-11-17 | 福建师范大学 | S-doped MnBi 2 Te 4 Method for producing single crystal |
| CN115196965B (en) * | 2022-07-25 | 2023-07-25 | 深圳先进电子材料国际创新研究院 | N-type bismuth telluride thermoelectric material and preparation method thereof |
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| CN101994155A (en) * | 2010-11-18 | 2011-03-30 | 中国科学院宁波材料技术与工程研究所 | Nanophase doped bismuth telluride-based thermoelectric material and preparation method thereof |
| CN102024899A (en) * | 2010-09-22 | 2011-04-20 | 中国科学院宁波材料技术与工程研究所 | Nanoparticle composite bismuth telluride-based thermoelectric material and preparation method thereof |
| CN102088058A (en) * | 2010-11-30 | 2011-06-08 | 江西纳米克热电电子股份有限公司 | Preparation method for high-performance n-type bismuth telluride base thermoelectricity power generation material |
| CN102108554A (en) * | 2010-11-30 | 2011-06-29 | 江西纳米克热电电子股份有限公司 | Method for preparing high-performance p-type bismuth telluride-based thermoelectric materials |
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| CN102024899A (en) * | 2010-09-22 | 2011-04-20 | 中国科学院宁波材料技术与工程研究所 | Nanoparticle composite bismuth telluride-based thermoelectric material and preparation method thereof |
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| CN102088058A (en) * | 2010-11-30 | 2011-06-08 | 江西纳米克热电电子股份有限公司 | Preparation method for high-performance n-type bismuth telluride base thermoelectricity power generation material |
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