CN115537908A - Preparation method of high-performance bismuth telluride-based thermoelectric material - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 58
- 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
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000013078 crystal Substances 0.000 claims abstract description 43
- 238000004857 zone melting Methods 0.000 claims abstract description 35
- 239000000956 alloy Substances 0.000 claims abstract description 18
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 17
- 238000007711 solidification Methods 0.000 claims abstract description 17
- 230000008023 solidification Effects 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 17
- 238000005520 cutting process Methods 0.000 claims description 14
- 238000003723 Smelting Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000013590 bulk material Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 3
- 238000007709 nanocrystallization Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000930 thermomechanical effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910001215 Te alloy Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
- C30B28/08—Production of homogeneous polycrystalline material with defined structure from liquids by zone-melting
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- Chemical & Material Sciences (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the field of thermoelectric semiconductor materials, and provides a preparation method of a high-performance bismuth telluride-based thermoelectric material aiming at the problem of additional pollution caused in the material nanocrystallization process, which comprises the following steps: 1) Performing zone-melting directional solidification on the bismuth telluride-based alloy cast ingot to obtain a crystal bar; 2) Thermally deforming the crystal bar obtained in the step 1) to obtain a block material, wherein the deformation is larger than 1, and thermally deforming under uniaxial pressure, wherein the pressure direction is vertical to the texture direction of the zone-melting crystal bar. According to the invention, the zone-melting bulk material is thermally deformed by a top-down method, so that pollution caused by material refinement is avoided, nano defects are directly introduced into the bulk material, crystal grains are refined, the thermal conductivity of the material is reduced, and the mechanical property and the thermoelectric property of the material are improved.
Description
Technical Field
The invention relates to the field of thermoelectric semiconductor materials, in particular to a preparation method of a high-performance bismuth telluride-based thermoelectric material.
Background
Thermoelectric materials have great potential in thermoelectric energy conversion and solid state refrigeration, several of which have been in the pastHas attracted the extensive research interest of scholars for ten years. Material performance can be measured by thermoelectric figure of merit ZT, defined as ZT = α 2 σ T/κ, where α, σ, κ, and T are Seebeck coefficient, electrical conductivity, thermal conductivity, and temperature (in Kelvin), respectively. The correlation among the electrical conductivity, seebeck coefficient and thermal conductivity makes it difficult to satisfactorily improve thermoelectric performance.
Bismuth telluride (Bi) 2 Te 3 ) The thermoelectric material is a thermoelectric material with the best performance near room temperature, belongs to a rhombohedral system, and common preparation methods comprise a zone melting method (for example, a patent CN108550689B, a preparation method of an N-type bismuth telluride-based thermoelectric material), a Bridgman method (for example, xudesh, semiconductor refrigeration and application technology, shanghai university of transportation publishing Co., ltd.), a single crystal pulling method (for example, a patent CN113699595A, a recovery and reprocessing method of the bismuth telluride-based thermoelectric material generating donor-like effect), and the like. But the weak van der waals bonds between Te-Te layers in the crystal structure thereof cause it to exhibit poor mechanical properties and high lattice thermal conductance. Nanocrystallization has been demonstrated to improve Bi 2 Te 3 One of the most effective ways for the thermoelectric property and the mechanical property of the polycrystalline bulk material is a mechanical alloying method, but in the preparation process of the polycrystalline bulk material, a donor-like effect is additionally introduced, so that the change of the material carrier concentration is influenced, and the powder is easily oxidized and absorbs moisture along with the powder refinement, so that additional pollution is introduced. Accordingly, an ideal solution is needed.
Disclosure of Invention
The invention provides a preparation method of a high-performance bismuth telluride-based thermoelectric material, aiming at overcoming the problem of additional pollution caused in the process of material nanocrystallization.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-performance bismuth telluride-based thermoelectric material comprises the following steps:
1) Performing zone-melting directional solidification on the bismuth telluride-based alloy cast ingot to obtain a crystal bar;
2) Thermally deforming the crystal bar obtained in the step 1) to obtain a block material, wherein the deformation is larger than 1, and thermally deforming under uniaxial pressure, wherein the pressure direction is vertical to the texture direction of the zone-melting crystal bar.
Preferably, the bismuth telluride-based alloy ingot in the step 1) is obtained by performing swing smelting on metal raw material powder at the temperature of 600-700 ℃. More preferably, the metal raw material powder is a high-purity powder having a purity of not less than 99.99%.
Preferably, the bismuth telluride in the step 1) is Bi 0.5 Sb 1.5 Te 3 + x% of wt Te, x being in the range of 0-5, or Bi 2 Te 3-y Se y The value range of y of the N-type bismuth telluride is 0.1-0.4.
Preferably, the conditions of zone-melting directional solidification in the step 1) are as follows: the vacuum degree is 0-2Pa, the temperature is 600-900 ℃, and the directional solidification is carried out at the speed of 8-35 mm/h.
Preferably, the temperature of zone-melting directional solidification of a crystal bar obtained by P-type bismuth telluride base alloy ingot casting is 600-800 ℃; the zone-melting directional solidification temperature of the crystal bar obtained by the N-type bismuth telluride base alloy ingot casting is 700-900 ℃.
Preferably, the zone-melting directional solidification in the step 1) is carried out in a glass tube with the inner diameter of 20-30 mm.
Preferably, before the thermal deformation of the crystal bar in the step 2), the crystal bar is cut into a thermal deformation precursor, wherein the cutting direction is perpendicular to the growth direction of the zone-melting crystal bar and perpendicular to the grain boundary direction of the crystal bar.
Preferably, the thermally deformable precursor is a cylinder with a diameter of 15-30 mm. The size of the precursor can be designed according to the size and the deformation of the mold, and the size is not limited to the shape.
Preferably, the conditions for the hot deformation in step 2) are: thermally deforming at 450-550 deg.C under 30-100 MPa.
Preferably, the deformation amount in step 2) is in the range of 1 to 9.
Preferably, the hot deformation in step 2) is performed in a mold, and the mold is made of graphite, 45 steel or DZ22 alloy.
Therefore, the beneficial effects of the invention are as follows: according to the invention, the zone-melting block material is thermally deformed by a top-down method, so that pollution caused by material refinement is avoided, nano defects are directly introduced into the block material, crystal grains are refined, the thermal conductivity of the material is reduced, the mechanical property and the thermoelectric property of the material are improved, and the thermoelectric property of the material can be improved by more than 20%. The patent CN114031046A uses zone-melting sample to extrude, this patent is on the basis of single crystal zone-melting crystal bar, carries out the thermal deformation of specific direction again, and not hot extrusion, and the deformation direction is inconsistent with the extrusion direction, through introducing nanometer defect, refines the crystalline grain, reduces the thermal conductance to further promote material thermoelectric property and mechanical properties.
Drawings
FIG. 1 is a schematic diagram of precursor preparation according to the present invention;
fig. 2 is a graph comparing thermoelectric properties of the thermally deformable materials (HD 1, HD 2) prepared in example 1 and example 2 and the zone-melting material (ZM) prepared in comparative example 1.
Fig. 3 is a graph comparing mechanical properties of the thermally deformable materials (HD 1, HD 2) prepared in example 1 and example 2 and the float Zone Material (ZM) prepared in comparative example 1.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
General examples
A preparation method of a high-performance bismuth telluride-based thermoelectric material comprises the following steps:
1) Preparation of Bi 0.5 Sb 1.5 Te 3 + x% wt Te of P-type bismuth telluride, wherein x ranges from 0 to 5; or B i2 Te 3-y Se y The value range of y of the N-type bismuth telluride is 0.1-0.4. Weighing Bi powder, te powder, sb powder and Se powder with the purity of more than or equal to 99.99 percent according to the chemical proportionAnd performing high-temperature swing smelting at the temperature of 600-700 ℃ in the air to obtain a P-type bismuth telluride-based alloy ingot or an N-type bismuth telluride-based alloy ingot.
2) The bismuth telluride base alloy ingot is placed in a glass tube with the inner diameter of 20-30 mm, and is subjected to zone-melting directional solidification under the pressure of 0-2Pa, the temperature of 600-900 ℃ (P type is 600-800 ℃, N type is 700-900 ℃) and the speed of 8-35 mm/h to obtain the P type bismuth telluride base crystal rod or the N type bismuth telluride base crystal rod.
3) Thermally deforming the crystal bar obtained in the step 2) in a mold (graphite, 45 steel or DZ22 alloy material) to obtain a block material, wherein the deformation is more than 1 (preferably 1-9), the thermal deformation is carried out at 450-550 ℃ under the uniaxial pressure of 30-100 MPa, and the pressure direction is vertical to the texture direction of the zone-melting crystal bar;
or cutting the crystal bar obtained in the step 2) into a thermal deformation precursor by using a wire cutting machine, wherein the cutting direction is vertical to the growth direction of the zone-melting crystal bar and is vertical to the crystal boundary direction of the crystal bar to obtain a small cylinder with the diameter of 15-30 mm; and then carrying out the thermal deformation treatment on the thermal deformation precursor to obtain the bulk material.
Example 1
A preparation method of a high-performance bismuth telluride-based thermoelectric material comprises the following steps:
(1) Batch smelting/material preparation
Preparation of Bi 0.5 Sb 1.5 Te 3 The P-type bismuth telluride with + x% wt Te, wherein x is 3, bi powder, sb powder and Te powder with the purity of more than or equal to 99.99% are weighed according to the chemical proportion, and the P-type Bi is obtained by high-temperature swing smelting at 650 ℃ in vacuum 0.5 Sb 1.5 Te 3 +3% wt Te alloy ingot.
(2) Zone melting
And (2) placing the alloy ingot obtained in the step (1) in a glass tube with the inner diameter of 28 cm, and performing zone-melting directional solidification under the pressure of 0-2Pa, the temperature of 600 ℃ and the speed of 25mm/h to obtain the bismuth telluride-based P-type crystal rod.
(3) Thermal deformation precursor preparation
And (3) cutting the zone-melting crystal bar obtained in the step (2) by using a wire cutting machine to prepare a thermal deformation precursor, wherein the cutting direction is vertical to the crystal boundary direction of the crystal bar as shown in figure 1, so as to obtain a small cylinder with the diameter of 16mm and h28 mm.
(4) Thermomechanical production
And (3) placing the thermally deformable precursor obtained in the step (3) in a graphite mold (30 mm, the deformation amount is 1.5), heating to 500 ℃, and thermally deforming under 40MPa uniaxial pressure to obtain a block material (HD 1) of (30mm, h111mm).
Example 2
The difference from example 1 is in steps (3) and (4):
(3) Thermal deformation precursor preparation
Cutting the zone-melting crystal bar obtained in the step (2) in the embodiment 1 by using a wire cutting machine to prepare a thermal deformation precursor, wherein the cutting direction is vertical to the crystal boundary direction of the crystal bar, so as to obtain a small cylinder (16 mm, h18 mm).
(4) Thermomechanical production
And (3) placing the thermal deformation precursor obtained in the step (3) in a graphite mold (20 mm, the deformation amount is 1.5), heating to 500 ℃, and thermally deforming under 40MPa uniaxial pressure to obtain a block material (HD 2) with the thickness of 20mm and h8 mm.
Comparative example 1
The difference from example 1 is that step (4) was not carried out, i.e., no hot deformation treatment was carried out, and the resulting product was a zone-melting material (ZM).
Example 3
A preparation method of a high-performance bismuth telluride-based thermoelectric material comprises the following steps:
(1) Batch smelting/Material preparation
Preparation of Bi 2 Te 3-y Se y The bismuth telluride N has y of 0.3, bi powder, se powder and Te powder with purity of more than or equal to 99.99 percent are weighed according to the chemical proportion, and the bismuth telluride N is smelted in a high-temperature swing mode at 700 ℃ under vacuum to obtain the bismuth telluride N 0.5 Te 2.7 Se 0.3 The alloy ingot of (1).
(2) Zone melting
And (2) placing the alloy ingot obtained in the step (1) in a glass tube with the inner diameter of 28 cm, and performing zone-melting directional solidification at the pressure of 0-2Pa, the temperature of 700 ℃ and the speed of 25mm/h to obtain the bismuth telluride-based N-type crystal rod.
(3) Thermal deformation precursor preparation
And (3) cutting the zone-melting crystal bar obtained in the step (2) by using a wire cutting machine to prepare a thermal deformation precursor, wherein the cutting direction is vertical to the crystal boundary direction of the crystal bar, so as to obtain a small cylinder (16 mm, h18 mm).
(4) Thermomechanical production
Placing the thermally deformable precursor obtained in step (3) in a graphite mold (20 mm, deformation amount is 1.5), heating to 500 ℃, and thermally deforming under 40MPa uniaxial pressure to obtain a block material (HD 1) (20mm, h111mm).
Example 4
(1) Batch smelting/Material preparation
Preparation of Bi 0.5 Sb 1.5 Te 3 + x% of wt Te P-type bismuth telluride, wherein x is 3, bi powder, sb powder and Te powder with the purity of more than or equal to 99.99% are weighed according to the chemical proportion, and are subjected to high-temperature swing smelting at 650 ℃ under vacuum to obtain the P-type Bi 0.5 Sb 1.5 Te 3 +3% wt Te alloy ingot.
(2) Zone melting
And (2) placing the alloy ingot obtained in the step (1) in a glass tube with the inner diameter of 28 cm, and performing zone-melting directional solidification at the pressure of 0-2Pa, the temperature of 600 ℃ and the speed of 25mm/h to obtain the bismuth telluride-based P-type crystal rod.
(3) Thermomechanical production
And (3) placing the crystal bar obtained in the step (2) in a square mold with the length, width and height of 40 × 60 × 50 mm, wherein the deformation amount is 2.2, heating to 500 ℃, and carrying out thermal deformation under 40MPa uniaxial pressure to obtain a block material with the length, width and height of 40 × 60 × 12 mm.
Performance characterization
As shown in figures 2 and 3, the bismuth telluride-based thermoelectric material prepared by the method has excellent mechanical property and thermoelectric property, and the thermoelectric property of the material can be improved by more than 20%. Wherein the hardness test condition is that the residual indentation on the block sample is obtained by calculating the length of the diagonal of the indentation by using a 0.3kg force conical head, and the larger the numerical value is, the higher the hardness is represented.
Although the present invention has been described with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the present invention.
Claims (10)
1. A preparation method of a high-performance bismuth telluride-based thermoelectric material is characterized by comprising the following steps:
1) Performing zone-melting directional solidification on the bismuth telluride base alloy cast ingot to obtain a crystal bar;
2) Thermally deforming the crystal bar obtained in the step 1) to obtain a block material, wherein the deformation is larger than 1, and thermally deforming under uniaxial pressure, wherein the pressure direction is vertical to the texture direction of the zone-melting crystal bar.
2. The method for preparing the high-performance bismuth telluride-based thermoelectric material as claimed in claim 1, wherein the bismuth telluride-based alloy ingot in the step 1) is obtained by performing swing smelting on metal raw material powder at 600-700 ℃.
3. The method for preparing a high-performance bismuth telluride-based thermoelectric material as claimed in claim 1 or 2, wherein the bismuth telluride in the step 1) is Bi 0.5 Sb 1.5 Te 3 (ii) P-type bismuth telluride having + x% wt of Te, wherein x is in the range of 0-5, or Bi 2 Te 3-y Se y The value range of y of the N-type bismuth telluride is 0.1-0.4.
4. The preparation method of the high-performance bismuth telluride-based thermoelectric material as claimed in claim 1, wherein the conditions of zone-melting directional solidification in the step 1) are as follows: the vacuum degree is 0-2Pa, the temperature is 600-900 ℃, and the directional solidification is carried out at the speed of 8-35 mm/h.
5. The preparation method of the high-performance bismuth telluride-based thermoelectric material as claimed in claim 3, wherein the temperature of zone-melting directional solidification of a boule obtained from the P-type bismuth telluride-based alloy ingot is 600-800 ℃; the temperature of zone-melting directional solidification of a crystal bar obtained by casting the N-type bismuth telluride-based alloy ingot is 700-900 ℃.
6. The preparation method of the high-performance bismuth telluride-based thermoelectric material as in claim 1, wherein the step 1) of zone-melting directional solidification is carried out in a glass tube with an inner diameter of 20-30 mm.
7. The preparation method of the high-performance bismuth telluride-based thermoelectric material as claimed in claim 1, wherein before the thermal deformation of the ingot in the step 2), the ingot is cut into a thermal deformation precursor, wherein the cutting direction is perpendicular to the growth direction of the zone-melting ingot and perpendicular to the grain boundary direction of the ingot.
8. The method for preparing a high-performance bismuth telluride-based thermoelectric material as claimed in claim 7, wherein the thermally deformable precursor is a cylinder with a diameter of 15-30 mm.
9. The preparation method of the high-performance bismuth telluride-based thermoelectric material as claimed in claim 1, wherein the thermal deformation conditions in step 2) are as follows: thermally deforming at 450-550 deg.C under 30-100 MPa.
10. The method for preparing a high-performance bismuth telluride-based thermoelectric material as in claim 1 or 9, wherein the deformation in step 2) is in the range of 1-9.
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| CN116804288A (en) * | 2023-08-21 | 2023-09-26 | 杭州大和热磁电子有限公司 | Preparation method of N-type bismuth telluride zone-melting cast ingot for thermoelectric refrigerator |
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| CN116804288B (en) * | 2023-08-21 | 2023-12-12 | 杭州大和热磁电子有限公司 | Preparation method of N-type bismuth telluride zone-melting cast ingot for thermoelectric refrigerator |
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