CN110459670B - Method for preparing magnetic nano composite thermoelectric material based on amorphous material in situ - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 94
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 48
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000002122 magnetic nanoparticle Substances 0.000 claims abstract description 16
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 12
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 229910002771 BaFe12O19 Inorganic materials 0.000 claims description 2
- 229910002899 Bi2Te3 Inorganic materials 0.000 claims description 2
- 229910005331 FeSi2 Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910000577 Silicon-germanium Inorganic materials 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 229910052711 selenium Inorganic materials 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- 229910052714 tellurium Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000005676 thermoelectric effect Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
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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
- H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Physics & Mathematics (AREA)
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Abstract
The invention provides a method for preparing a magnetic nano composite thermoelectric material in situ based on an amorphous material, which comprises the following steps: carrying out heat treatment on the amorphous material above the crystallization temperature, and obtaining the magnetic nano composite thermoelectric material in situ; the magnetic nano composite thermoelectric material consists of a thermoelectric matrix material and magnetic nano particles. The invention takes the amorphous material as the raw material, carries out heat treatment above the crystallization temperature of the amorphous material, and obtains the magnetic nano composite thermoelectric material consisting of the thermoelectric base material and the magnetic nano particles in situ, the magnetic nano particles in the obtained magnetic nano composite thermoelectric material are uniformly distributed, the size is controllable, the performance repeatability is good, the preparation process is greatly simplified, and further, the preparation cost is greatly reduced, the invention is suitable for industrial production, and has important economic and scientific values for preparing the magnetic nano composite thermoelectric material.
Description
Technical Field
The invention relates to the technical field of thermoelectric material preparation, in particular to a method for preparing a magnetic nano composite thermoelectric material in situ based on an amorphous material.
Background
With the rapid development of the world economy, the rapid increase of the population and the continuous expansion of the industrial scale, the demand of people for energy sources is continuously increased. The thermoelectric material can directly perform reversible conversion of electric energy and heat energy by utilizing the thermoelectric effect, and a thermoelectric device formed by the thermoelectric material has the advantages of small volume, no noise, no transmission, no pollution, long service life and the like, so that the thermoelectric material has a very considerable application prospect as an environment-friendly material in solving the worldwide sustainable energy development policy.
The nano-composite is an important direction for optimizing thermoelectric performance of materials, the conventional nano-composite thermoelectric material is generally prepared by mixing and sintering matrix powder and nano-particles, and if the nano-particles are magnetic nano-particles, the problems of magnetic nano-particle agglomeration, uneven distribution and the like are easy to occur. Although the problem of agglomeration can be solved when the magnetic nanoparticles are prepared by methods such as surface modification and the like and then mixed with matrix powder to prepare the magnetic nanocomposite material, the process has a long preparation period, high cost and a complex preparation process, so that the wider application of the process is limited to a certain extent.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for in-situ preparation of a magnetic nanocomposite thermoelectric material based on an amorphous material, so as to solve the problems of easy occurrence of agglomeration and uneven distribution of magnetic nanoparticles and complicated preparation process in the existing preparation process of the magnetic nanocomposite thermoelectric material.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for preparing a magnetic nano composite thermoelectric material in situ based on an amorphous material comprises the following steps:
carrying out heat treatment on the amorphous material above the crystallization temperature, and obtaining the magnetic nano composite thermoelectric material in situ; the magnetic nano composite thermoelectric material consists of a thermoelectric matrix material and magnetic nano particles.
Optionally, the thermoelectric matrix material is Bi2Te3、PbX、Mg2X、SiGe、MX3、MNiSn、MCoSb、XFeSb、FeSi2、FexSiyB100-x-yOne of (1); x in the PbX is one of S, Se and Te; the Mg2X in X is one of Si, Ge and Sn; said MX3Wherein M is one of Co, Rh and Ir, and X is one of P, As and Sb; m in the MNiSn is one of Ti, Zr and Hf; m in the MCoSb is one of Ti, Zr and Hf; x in XFESb is one of V, Nb and Ta.
Optionally, the magnetic nanoparticles are Fe, Co, Ni, Mn, Gd, BaFe12O19、Gd5Si2Ge2、LaFe11.6Si1.4One kind of (1).
Optionally, the heat treating the amorphous material above the crystallization temperature includes: annealing the amorphous material above the crystallization temperature.
Optionally, the annealing time of the annealing treatment is 20-60 min.
Compared with the prior art, the method for preparing the magnetic nano composite thermoelectric material in situ based on the amorphous material has the following advantages:
the invention takes the amorphous material as the raw material, carries out heat treatment above the crystallization temperature of the amorphous material, and obtains the magnetic nano composite thermoelectric material consisting of the thermoelectric base material and the magnetic nano particles in situ, the magnetic nano particles in the obtained magnetic nano composite thermoelectric material are uniformly distributed, the size is controllable, the performance repeatability is good, the preparation process is greatly simplified, and further, the preparation cost is greatly reduced, the invention is suitable for industrial production, and has important economic and scientific values for preparing the magnetic nano composite thermoelectric material.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a DSC of magnetic nanocomposite thermoelectric materials of examples 1 and 2 of the present invention;
fig. 2 is an XRD spectrum of the magnetic nanocomposite thermoelectric material of example 1 and example 2 of the present invention;
FIG. 3 is an SEM photograph of an unannealed amorphous material of a comparative example of the present invention;
FIG. 4 is an SEM photograph of a magnetic nanocomposite thermoelectric material of example 1 of the present invention;
FIG. 5 is an SEM photograph of a magnetic nanocomposite thermoelectric material of example 2 of the invention;
FIG. 6 is a hysteresis loop plot of magnetic nanocomposite thermoelectric materials of examples 1 and 2 of the present invention;
FIG. 7 is a graph of power factor versus temperature for magnetic nanocomposite thermoelectric materials of examples 1 and 2 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be described in detail below with reference to the drawings and examples.
Example 1
A method for preparing a magnetic nano composite thermoelectric material in situ based on an amorphous material specifically comprises the following steps:
amorphous material, i.e. Fe, produced by high vacuum melt-spun machines78Si9B13Placing the amorphous ribbon into a quartz tube, and vacuum sealing the tube under a vacuum degree of less than 10Pa, wherein, as can be seen from FIG. 1, Fe78Si9B13Two obvious exothermic peaks exist in a DSC graph of the amorphous thin band, the first peak is a crystallization peak of alpha-Fe, the crystallization temperature is 498 ℃, and the second peak is Fe2The crystallization peak of B, the crystallization temperature is 540 ℃;
will contain Fe78Si9B13Putting the amorphous thin-belt quartz tube into a resistance furnace at 520 ℃, annealing for 40min, and then cooling along with the furnace to obtain the magnetic nano composite thermoelectric material in situ, wherein the magnetic nano composite thermoelectric material is prepared from a thermoelectric base material (Fe)xSiyB100-x-y) And magnetic nanoparticles (Fe), i.e. amorphous materials (Fe)78Si9B13) The magnetic nano composite thermoelectric material can be obtained in situ after heat treatment of elements comprising thermoelectric base materials and magnetic nano particles in the magnetic nano composite thermoelectric material.
Example 2
This example differs from example 1 in that: in the method for in-situ preparation of the magnetic nanocomposite thermoelectric material based on the amorphous material, the annealing time is 60 min.
XRD testing was performed on the magnetic nanocomposite thermoelectric materials obtained in examples 1 and 2 of the present invention, and the materials were mixed with non-annealed amorphous material (Fe)78Si9B13Amorphous thin bands), comparative example, the test results are shown in fig. 2.
As can be seen from FIG. 2, no significant crystal phase peak was observed in the XRD pattern of the comparative example, indicating that Fe was selected78Si9B13The amorphous ribbon is indeed an amorphous material, and compared to the comparative example, a distinct crystalline phase peak is found in both inventive example 1 and inventive example 2, and the main precipitate is α -Fe (corresponding to PDF card number #)06-0696), with small amounts of Fe also present2The B precipitate phase (corresponding to PDF card number #03-1053) demonstrates that the annealing heat treatment of the present invention can precipitate α -Fe magnetic crystals.
The magnetic nanocomposite thermoelectric materials obtained in examples 1 and 2 of the present invention were subjected to SEM test and were mixed with an unannealed amorphous material (Fe)78Si9B13Amorphous ribbons), i.e., comparative examples, were compared and the test results are shown in fig. 3 (comparative example), fig. 4 (example 1), and fig. 5 (example 2), respectively.
As can be seen from FIGS. 3, 4 and 5, the amorphous material (Fe) in the SEM images of the comparative examples78Si9B13Amorphous thin strip), while the magnetic nanocomposite thermoelectric materials of examples 1 and 2 have no significant contrast change, uniformly distributed nanocrystalline grains were observed, and it can be seen from the XRD analysis result of fig. 1 that the nanocrystalline grains are α -Fe magnetic grains, indicating that the magnetic nanocrystalline can be precipitated in situ by the annealing treatment of the present invention, to obtain the magnetic nanocomposite material. Furthermore, as can be seen from fig. 4 and 5, the average size of the nanocrystals in example 1 was about 95nm, and the average size of the nanocrystals in example 2 was about 180nm, indicating that good control of the nanocrystal size in the magnetic nanocomposite thermoelectric material can be achieved by controlling the annealing time of the present invention.
The magnetic nanocomposite thermoelectric materials obtained in examples 1 and 2 of the present invention were subjected to a magnetic test, and were mixed with an unannealed amorphous material (Fe)78Si9B13Amorphous thin bands), comparative example, the test results are shown in fig. 6.
As can be seen from fig. 6, the magnetic nanocomposite thermoelectric materials of examples 1 and 2 and the amorphous material of the comparative example both exhibited significant ferromagnetism, and the magnetic nanocomposite thermoelectric materials of examples 1 and 2 had a higher saturation magnetic strength than the amorphous material of the comparative example, and it can be seen from the XRD analysis of fig. 2 that the amorphous material (Fe) was annealed by the present invention (Fe)78Si9B13Amorphous thin band) is magnetic nanoparticles.
For example 1 and practice of the inventionExample 2 the magnetic nanocomposite thermoelectric material obtained was subjected to a thermoelectric performance test and was mixed with an unannealed amorphous material (Fe)78Si9B13Amorphous thin bands), comparative example, the test results are shown in fig. 7.
As can be seen from fig. 7, the power factors of the magnetic nanocomposite thermoelectric materials obtained by annealing treatment in examples 1 and 2 of the present invention were both greatly improved as compared with the comparative example, indicating that the magnetic nanocomposite thermoelectric materials having certain thermoelectric properties can be obtained by the production method of the present invention.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A method for preparing a magnetic nano composite thermoelectric material in situ based on an amorphous material is characterized by comprising the following steps:
carrying out heat treatment on the amorphous material above the crystallization temperature, and obtaining the magnetic nano composite thermoelectric material in situ; the magnetic nano composite thermoelectric material consists of a thermoelectric base material and magnetic nano particles;
the thermoelectric base material is Bi2Te3、PbX、Mg2X、SiGe、MX3、MNiSn、MCoSb、XFeSb、FeSi2、FexSiyB100-x-yOne of (1); x in the PbX is one of S, Se and Te; the Mg2X in X is one of Si, Ge and Sn; said MX3Wherein M is one of Co, Rh and Ir, and X is one of P, As and Sb; m in the MNiSn is one of Ti, Zr and Hf; m in the MCoSb is one of Ti, Zr and Hf; x in the XFeSb is one of V, Nb and Ta;
the magnetic nanoparticles are Fe, Co, Ni, Mn, Gd, BaFe12O19、Gd5Si2Ge2、LaFe11.6Si1.4One of (1);
the heat treatment of the amorphous material above the crystallization temperature comprises the following steps: annealing the amorphous material above the crystallization temperature.
2. The method for in-situ preparation of the magnetic nanocomposite thermoelectric material based on the amorphous material as claimed in claim 1, wherein the annealing time of the annealing treatment is 20-60 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557448A (en) * | 2010-12-24 | 2012-07-11 | 株式会社日立制作所 | Thermoelectric conversion material |
| CN103165810A (en) * | 2013-03-22 | 2013-06-19 | 东北农业大学 | Carbon-coated class V-VI compound semiconductor nano sheet and preparation method thereof |
| CN109071324A (en) * | 2016-04-15 | 2018-12-21 | 株式会社小糸制作所 | The manufacturing method of nanocomposite and nanocomposite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557448A (en) * | 2010-12-24 | 2012-07-11 | 株式会社日立制作所 | Thermoelectric conversion material |
| CN103165810A (en) * | 2013-03-22 | 2013-06-19 | 东北农业大学 | Carbon-coated class V-VI compound semiconductor nano sheet and preparation method thereof |
| CN109071324A (en) * | 2016-04-15 | 2018-12-21 | 株式会社小糸制作所 | The manufacturing method of nanocomposite and nanocomposite |
Non-Patent Citations (1)
| Title |
|---|
| Stress effects on magnetic property of Fe-based metallic glasses;M.G.Ri;《Journal of Non-Crystalline Solids》;20180514;全文 * |
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