CN117737847A - N-type bismuth telluride-based crystal bar with high electrical property and preparation method thereof - Google Patents
N-type bismuth telluride-based crystal bar with high electrical property and preparation method thereof Download PDFInfo
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- CN117737847A CN117737847A CN202311745546.5A CN202311745546A CN117737847A CN 117737847 A CN117737847 A CN 117737847A CN 202311745546 A CN202311745546 A CN 202311745546A CN 117737847 A CN117737847 A CN 117737847A
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 52
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 52
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000013078 crystal Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000001125 extrusion Methods 0.000 claims abstract description 31
- 238000001192 hot extrusion Methods 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 238000005452 bending Methods 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 22
- 238000007599 discharging Methods 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 10
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 2
- 230000000171 quenching effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 29
- 230000000052 comparative effect Effects 0.000 description 16
- 230000000694 effects Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 230000008602 contraction Effects 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000005266 casting Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000005324 grain boundary diffusion Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention relates to the technical field of thermoelectric materials, and provides an N-type bismuth telluride-based crystal bar with high electrical performance and a preparation method thereof, comprising the following steps: step 1: stoichiometric ratio of Bi 2 Te 3‑x Se x After being put into a reducing hot extrusion die, the die is heated until the temperature reaches 450-500 ℃, and then the die is insulated for 30-6 min0min; x=0.2 to 0.5; step 2: applying pressure, namely applying vertical extrusion force to the precursor in the reducing hot extrusion die, so that the precursor is extruded after passing through a cavity of the reducing hot extrusion die, and a strip-shaped crystal bar is formed; the ratio of the area of the first vertical section to the area of the first horizontal section is: 1.8 to 2.0; the ratio of the area of the second horizontal section to the area of the second vertical section is: 1.4 to 1.6, the preparation method adopts a hot extrusion production process, and improves the mechanical property and the electrical property of the bismuth telluride material by optimizing parameters such as temperature, extrusion rate, extrusion ratio and the like.
Description
Technical Field
The invention relates to the technical field of thermoelectric materials, in particular to an N-type bismuth telluride-based crystal bar with high electrical performance and a preparation method thereof.
Background
Bismuth telluride-based compounds are currently the most widely used thermoelectric materials commercially and perform best near room temperature. The bismuth telluride crystal is a layered structure material, is easily cleaved along the c-axis direction of the crystal, and shows remarkable anisotropic characteristics, however, the electron transport characteristic of the bismuth telluride crystal along the c-axis crystal face is obviously superior to that of other crystal faces, so that the adjustment of the crystal grain orientation realizes the texture as an important research direction for improving the thermoelectric performance.
CN202210604945.9 discloses a method for improving the electrical properties of n-type bismuth telluride-based thermoelectric materials. The invention provides a method for improving the electrical property of an n-type bismuth telluride-based thermoelectric material, which comprises the following steps: nominal composition of Bi 2 Te 3-x Se x The crystal bar is taken as a raw material, the surface is polished, and the clean crystal bar is obtained by cleaning and drying; x=0.2 to 0.5; taking the obtained clean crystal bar, crushing, putting the clean crystal bar into the bottom of a smelting crucible, and performing magnetic suspension smelting until the crushed crystal bar is completely melted; refining, fast casting and cooling to obtain n-type bismuth telluride base alloy; taking the obtained n-type bismuth telluride base alloy, crushing and screening to obtain n-type bismuth telluride base alloy powder; and (5) taking the obtained n-type bismuth telluride base alloy powder, and placing the powder in a die for sintering to obtain the bismuth telluride base alloy. The method of the scheme can prepare the n-type bismuth telluride-based thermoelectric material with preferred orientation along the (00 l) direction, and the electrical property of the n-type bismuth telluride-based thermoelectric material is greatly improved.
However, the finished product of this embodiment is obtained by sintering, and it is difficult to avoid the problem that the quality of the finished product is uneven due to the difference of the molds in mass production.
Based on the above, the technical problems solved by the scheme are as follows: how to mass produce high-performance N-type bismuth telluride base crystal bars, and further improve the electrical performance of the N-type bismuth telluride base alloy crystal bars.
Disclosure of Invention
In order to solve the technical problems, the invention provides the N-type bismuth telluride-based crystal bar with high electrical property and the preparation method thereof, wherein the preparation method adopts a hot extrusion production process, and improves the mechanical property and the electrical property of the bismuth telluride material by optimizing parameters such as temperature, extrusion rate, extrusion ratio and the like.
The technical scheme of the invention is as follows:
the preparation method of the N-type bismuth telluride-based crystal bar with high electrical property comprises the following steps:
step 1: stoichiometric ratio of Bi 2 Te 3-x Se x After being put into a reducing hot extrusion die, the die is heated until the temperature reaches 450-500 ℃, and then the die is kept for 30-60 min; x=0.2 to 0.5;
step 2: applying pressure, namely applying vertical extrusion force to the precursor in the reducing hot extrusion die, so that the precursor is extruded after passing through a cavity of the reducing hot extrusion die, and a strip-shaped crystal bar is formed;
the cavity of the reducing hot extrusion die sequentially comprises a feeding section, a reducing section and a discharging section, wherein the axes of the feeding section, the reducing section and the discharging section are positioned on the same plane; the feeding section and the discharging section are vertically downward; the reducing section comprises a first bending section and a second bending section which are connected end to end, wherein the second bending section is connected with the first bending section; the bending angles of the first bending section and the second bending section are equal and are 90-150 degrees;
the ratio of the area of the first vertical section to the area of the first horizontal section is: 1.8 to 2.0;
the ratio of the area of the second horizontal section to the area of the second vertical section is: 1.4 to 1.6.
In the preparation method of the high-electrical-performance N-type bismuth telluride-based crystal ingot,
the first bending section comprises a first vertical section, a first corner section and a first horizontal section which are sequentially connected; the second bending section comprises a second horizontal section, a second corner section and a second vertical section which are sequentially connected; the first horizontal section and the second horizontal section are connected, and the diameters of the first horizontal section and the second horizontal section are the same;
the diameter of the first vertical section is the same as the diameter of the feeding section.
Before extrusion, the temperature is raised and maintained to ensure the temperature stability in the extrusion process, so that on one hand, the uneven temperature distribution of materials is avoided, the uniform heating of the materials is maintained, and the stability and consistency of the extrusion process are further ensured; on the other hand, the plasticity of the bismuth telluride material can be improved by heat preservation at high temperature, so that the grain flow in the subsequent extrusion process is smoother; in addition, the compactness of the material is improved, and the grain boundary diffusion and recrystallization of the material are promoted, so that the grains are finer and more uniform, the grain boundary is tighter, and the electrical property of the bismuth telluride material is improved.
Meanwhile, the method provides a proper stress release place for the crystal bar through multi-section corner extrusion, and is obviously helpful for further improving the preferred orientation along the (00 l) direction.
By the scheme of the invention, the preferential orientation along the (00 l) direction can be improved by combining the heat preservation operation and the reducing extrusion operation, and the electrical property of the material can be improved.
In the above preparation method of the high-electrical-performance N-type bismuth telluride-based crystal ingot, the bending angles of the first bending section and the second bending section are 90 degrees.
In the preparation method of the high-electrical-property N-type bismuth telluride-based crystal ingot, the feeding section, the first horizontal section, the second horizontal section and the discharging section are all cylindrical.
In the preparation method of the high-electrical-performance N-type bismuth telluride-based crystal rod, the preparation method of the precursor comprises the following steps:
smelting, water quenching and crushing the N-type bismuth telluride base alloy, and then carrying out hot-pressing sintering;
the hot-pressing sintering temperature is 180 ℃, the hot-pressing pressure is 70MPa, and the heat preservation and pressure maintaining time is 60min.
In the preparation method of the high-electrical-property N-type bismuth telluride-based crystal rod, in the hot-pressing sintering process, the temperature is raised to the hot-pressing temperature at the speed of 1-4 ℃/min.
In the preparation method of the high-electrical-property N-type bismuth telluride-based crystal bar, the strip-shaped crystal bar is extruded at a speed of 0.2-0.4 mm/min.
In the above method for preparing the high-electrical-performance N-type bismuth telluride-based crystal ingot, x=0.3 to 0.4.
Finally, the invention also discloses an N-type bismuth telluride-based crystal bar with improved electrical performance, which is prepared by the method described in any one of the above.
One of the above technical solutions of the present invention has at least one of the following advantages or beneficial effects:
before extrusion, the temperature is raised and maintained to ensure the temperature stability in the extrusion process, so that on one hand, the uneven temperature distribution of materials is avoided, the uniform heating of the materials is maintained, and the stability and consistency of the extrusion process are further ensured; on the other hand, the plasticity of the bismuth telluride material can be improved by heat preservation at high temperature, so that the grain flow in the subsequent extrusion process is smoother; in addition, the compactness of the material is improved, and the grain boundary diffusion and recrystallization of the material are promoted, so that the grains are finer and more uniform, the grain boundary is tighter, and the electrical property of the bismuth telluride material is improved.
Meanwhile, the method provides a proper stress release place for the crystal bar through multi-section corner extrusion, and is obviously helpful for further improving the preferred orientation along the (00 l) direction.
By the scheme of the invention, the preferential orientation along the (00 l) direction can be improved by combining the heat preservation operation and the reducing extrusion operation, and the electrical property of the material can be improved.
Drawings
Fig. 1 is a schematic diagram showing a cavity structure of a hot extrusion die according to embodiment 1 of the present invention;
fig. 2 is a schematic diagram of a cavity structure of a hot extrusion die of comparative example 2 of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the N-type bismuth telluride-based crystal bar with high electrical property comprises the following steps:
step 1: precursor preparation, with stoichiometric ratio of Bi 2 Te 3-x Se x The crystal bar is taken as a raw material, the surface of the raw material is polished, cleaned and dried to obtain a clean crystal bar, the clean crystal bar is crushed, and then the water-cooled copper crucible is adopted for magnetic suspension smelting until the crushed crystal bar is completely melted; wherein the temperature of the magnetic suspension smelting is 790 ℃, and the power rising speed of the smelting power of the magnetic suspension smelting is 50kw/min.
Casting, namely casting the raw materials subjected to magnetic suspension smelting on a metal disc, and cooling to obtain an ingot; the metal disc is a water-cooled copper disc, the water temperature at the bottom of the water-cooled copper disc is 9.8 ℃, and the water pressure is 0.28MPa; the thickness of the cast ingot cast on the water-cooled copper chassis is 15mm, and the diameter is 400mm; wherein the time for pouring the melted raw materials onto the water-cooled copper chassis is less than 5s;
crushing and screening the cast ingot by adopting a ball mill to obtain N-type bismuth telluride base alloy powder;
and (3) carrying out hot-pressing sintering on the N-type bismuth telluride base alloy powder, heating the powder from room temperature to 180 ℃ at a heating rate of 3 ℃/min, preserving heat and pressure for 60min under 70MPa, naturally cooling, and demoulding to obtain the precursor.
Step 2: heating and preserving heat, namely heating the die until the temperature reaches 460 ℃ after the precursor is placed into a reducing hot extrusion die, and preserving heat for 30min;
step 3: and (3) pressing, namely applying vertical extrusion force to the precursor in the reducing hot extrusion die, so that the precursor is extruded after passing through a cavity of the reducing hot extrusion die, and a strip-shaped crystal bar is formed.
Referring to fig. 1, in this embodiment, the cavity of the reducing hot extrusion die sequentially includes a feeding section 1, a reducing section 2, and a discharging section 3 with axes on the same plane; the feeding section 1 and the discharging section 3 are vertically downward; the reducing section 2 comprises a first bending section 21 and a second bending section 22 which are connected end to end; the bending angles of the first bending section 21 and the second bending section 22 are equal and are 90 degrees;
the first bending section 21 comprises a first vertical section 211, a first corner section 212 and a first horizontal section 213 which are sequentially connected; the second bending section 22 comprises a second horizontal section 221, a second corner section 222 and a second vertical section 223 which are sequentially connected; the first horizontal section 213 and the second horizontal section 221 are connected, and the diameters of the first horizontal section 213 and the second horizontal section 221 are the same;
the diameter of the first vertical section 211 is the same as the diameter of the feed section 1;
the ratio of the area of the first vertical section 211 to the area of the first horizontal section 213 is: 1.95;
the ratio of the area of the second horizontal segment 221 to the area of the second vertical segment 223 is: 1.55.
in this embodiment, therefore, the ratio of the areas of the feed section 1 to the discharge section 3, i.e. the total extrusion ratio=1.95×1.55≡3
Specifically, the heating rate in the step 2 is 3 ℃/min; and 3, extruding the strip-shaped crystal bar at a constant speed with an extrusion rate of 0.25 mm/min.
Example 2
Substantially the same as in embodiment 1, the difference is that the bending angles of the first bending section 21 and the second bending section 22 are equal and are each 120 °.
Example 3
Substantially the same as in embodiment 1, the difference is that the bending angles of the first bending section 21 and the second bending section 22 are equal and 150 °.
Example 4
Substantially the same as in example 1, except that the temperature was raised until the temperature reached 450℃in step 2, followed by heat preservation for 60 minutes.
Example 5
Substantially the same as in example 1, except that the temperature was raised in the step 2 until the temperature reached 500℃and then the temperature was kept for 60 minutes.
Example 6
Substantially the same as in example 1, except that the extrusion rate in the step 3 was 0.2mm/min.
Example 7
Substantially the same as in example 1, except that the extrusion rate in the step 3 was 0.4mm/min.
Comparative example 1
The same as embodiment 1 basically, except that the reducing section only includes a bending section with a bending angle of 90 ° to perform the reducing of the same compression ratio, the feeding section is vertically downward, and the discharging section is horizontally to one side.
Comparative example 2
Referring to fig. 2, the difference is that the cavity structure of the reducing hot extrusion die is changed to include an input section 4, a shrinkage section 5 and an output section 6 which are sequentially connected with each other, which is basically the same as that of embodiment 1; the contraction section 5 comprises a first contraction section 51, a transition section 52 and a second contraction section 53 which are connected in sequence; the axes of the first contraction section 51 and the second contraction section 53 are overlapped, and the coaxial diameter change is carried out twice by extruding and narrowing the first conical surface and the second conical surface respectively, and the ratio of the area of the input section 4 to the area of the transition section is as follows: 1.95;
the ratio of the area of the transition section to the area of the output section 6 is: 1.55;
in the present embodiment, therefore, the ratio of the area of the input section 4 to the area of the output section 6, i.e. the total extrusion ratio=1.95×1.55≡3.
Comparative example 3
Substantially the same as in example 1, except that the temperature was raised in the step 2 until the temperature reached 350 ℃.
Comparative example 4
Substantially the same as in example 1, except that the extrusion rate was 1.0mm/min.
Comparative example 5
Substantially the same as in example 1, except that,step 1 is not performed: precursor preparation, instead stoichiometric ratio of Bi 0.4 Sb 1.6 Te 3 The crystal bar with +3wt.% Te is taken as a raw material, and the steps 2 and 3 are directly carried out after crushing.
Performance test:
the test items include: seebeck coefficient, conductivity, power factor; the test results can be referred to table 1;
table 1: the materials obtained in each example and comparative example were tested
Analysis of results:
compared with the effect of the embodiment 1 and the comparative embodiment 1, the embodiment 1 has better electric effect, the power factor reaches 4.67, the efficiency is high, and the loss is low. The effects of example 1 and comparative example 2 are compared, the electrical effect of comparative example 2 is poor, the power factor is 2.52, and the power factor is remarkably reduced compared with example 1. The effects of example 1 and comparative example 3 are compared, the electrical effect of comparative example 3 is poor, the power factor is 2.83, and the power factor is remarkably reduced compared with example 1. The effects of example 1 and comparative example 4 are compared, the electrical effect of comparative example 4 is poor, the power factor is 3.63, and the power factor is remarkably reduced compared with example 1. The effects of example 1 and comparative example 5 are compared, the electrical effect of comparative example 5 is poor, the power factor is 2.45, and the power factor is remarkably reduced compared with example 1.
The comparison analysis shows that the quantity of bending, the reducing mode, the temperature control in the extrusion process, the extrusion speed and the precursor orientation optimization have obvious influence on the power factor.
It is believed that the preparation of the precursor can result in an n-type bismuth telluride-based thermoelectric material with a preferred orientation in the (00 l) direction, which is advantageous for improved electrical properties;
the rotation angle extrusion is carried out twice continuously, on one hand, the rotation angle is provided for a stress release position of the crystal, and on the other hand, the rotation angle changes the flow direction of the fluid, so that the fluid realizes preferential orientation along the (00 l) direction in the flow steering process.
The extrusion temperature is critical to the invention, and the extrusion temperature of the n-type bismuth telluride-based thermoelectric material is obviously higher than that of the P-type bismuth telluride-based thermoelectric material, so that the electrical property of the obtained material is better.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. The preparation method of the N-type bismuth telluride-based crystal bar with high electrical property is characterized by comprising the following steps of:
step 1: stoichiometric ratio of Bi 2 Te 3-x Se x After being put into a reducing hot extrusion die, the die is heated until the temperature reaches 450-500 ℃, and then the die is kept for 30-60 min; x=0.2 to 0.5;
step 2: applying pressure, namely applying vertical extrusion force to the precursor in the reducing hot extrusion die, so that the precursor is extruded after passing through a cavity of the reducing hot extrusion die, and a strip-shaped crystal bar is formed;
the cavity of the reducing hot extrusion die sequentially comprises a feeding section, a reducing section and a discharging section, wherein the axes of the feeding section, the reducing section and the discharging section are positioned on the same plane; the feeding section and the discharging section are vertically downward; the reducing section comprises a first bending section and a second bending section which are connected end to end, wherein the second bending section is connected with the first bending section; the bending angles of the first bending section and the second bending section are equal and are 90-150 degrees;
the ratio of the area of the first vertical section to the area of the first horizontal section is: 1.8 to 2.0;
the ratio of the area of the second horizontal section to the area of the second vertical section is: 1.4 to 1.6.
2. The method for preparing the high-electrical-performance N-type bismuth telluride-based crystal ingot according to claim 1, wherein,
the first bending section comprises a first vertical section, a first corner section and a first horizontal section which are sequentially connected; the second bending section comprises a second horizontal section, a second corner section and a second vertical section which are sequentially connected; the first horizontal section and the second horizontal section are connected, and the diameters of the first horizontal section and the second horizontal section are the same;
the diameter of the first vertical section is the same as the diameter of the feeding section.
3. The method for preparing an N-type bismuth telluride based crystal ingot with high electrical performance according to claim 2, wherein the bending angles of the first bending section and the second bending section are 90 °.
4. The method for preparing an N-type bismuth telluride based crystal ingot with high electrical performance according to claim 2, wherein the feeding section, the first horizontal section, the second horizontal section and the discharging section are all cylindrical.
5. The method for preparing the high-electrical-performance N-type bismuth telluride-based crystal ingot according to claim 1, wherein the preparation method of the precursor is as follows:
smelting, water quenching and crushing the N-type bismuth telluride base alloy, and then carrying out hot-pressing sintering;
the hot-pressing sintering temperature is 180 ℃, the hot-pressing pressure is 70MPa, and the heat preservation and pressure maintaining time is 60min.
6. The method for producing a high electrical performance N-type bismuth telluride based crystal ingot according to claim 5, wherein the hot press sintering process is performed at a rate of 1-4 ℃/min to a hot press temperature.
7. The method for producing an N-type bismuth telluride based ingot with high electrical properties according to claim 1, wherein the strip-shaped ingot is extruded at a speed of 0.2mm/min to 0.4mm/min.
8. The method for producing an N-type bismuth telluride-based crystal ingot with high electrical properties according to claim 1, wherein x=0.3 to 0.4.
9. An N-type bismuth telluride-based crystal ingot with improved electrical properties, wherein the N-type bismuth telluride-based crystal ingot is prepared by the method of any one of claims 1 to 8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311745546.5A CN117737847A (en) | 2023-12-15 | 2023-12-15 | N-type bismuth telluride-based crystal bar with high electrical property and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311745546.5A CN117737847A (en) | 2023-12-15 | 2023-12-15 | N-type bismuth telluride-based crystal bar with high electrical property and preparation method thereof |
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| CN117737847A true CN117737847A (en) | 2024-03-22 |
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