CN112002796A - Rapid preparation of high-performance Bi easy to cut2Te3Method for producing thermoelectric material - Google Patents
Rapid preparation of high-performance Bi easy to cut2Te3Method for producing thermoelectric material Download PDFInfo
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Abstract
The invention discloses a method for rapidly preparing high-performance p-type or n-type Bi easy to cut2Te3The method of thermoelectric material adopts high-purity simple substance as initial material and melts to obtain p-type or n-type Bi2Te3A base ingot body; then low-speed melt spinning is carried out, the obtained slice is tiled in a mould for spark plasma activated sintering, and high-performance p-type or n-type Bi easy to cut is obtained2Te3A base thermoelectric material. According to the invention, the orientation thin strip obtained by directly sintering the melt and rotary throwing is adopted, so that the orientation of the thin strip is partially retained in the thermoelectric material block obtained by final sintering, and the optimal performance is obtained while the mechanical performance is improvedThe thermoelectric material with the same direction as the zone-melting sample can directly use the cutting and subsequent treatment processes of the zone-melting material which is mature at present, and compared with the conventional polycrystalline material, the utilization rate and the post-treatment efficiency of the material are obviously improved.
Description
Technical Field
The invention belongs to the technical field of energy, and provides a method for rapidly preparing high-performance p-type or n-type Bi easy to cut2Te3A base thermoelectric material method.
Technical Field
The thermoelectric material can realize direct conversion between heat energy and electric energy as a novel clean renewable energy material, has the excellent characteristics of no pollution, no loss, high reliability and the like, is expected to greatly improve the energy utilization rate and relieve the environmental pollution, and attracts the attention of a plurality of researchers. Among a series of materials studied in recent years, bismuth telluride-based compounds are thermoelectric materials which are currently commercially used and have the best performance in the vicinity of room temperature.
The bismuth telluride-based compound is a trigonal system and belongs to a space group R-3 m. Along the crystallographic c-axis direction, bismuth telluride crystals can be regarded as being composed of-Te(1)—Bi—Te(2)—Bi—Te(1)-a repeating arrangement of five atomic layers, wherein Bi-Te(1)Are combined by covalent bond and ionic bond, Bi-Te(2)Are covalent bond therebetween, and Te(1)—Te(1)Are bonded with weak van der Waals force, so Bi2Te3The crystal is easily in Te(1)Cleavage occurs between atomic planes. Due to the special five-element layered structure of the bismuth telluride material, the electrical conductivity of the material along the zone melting direction is about four times that of the material perpendicular to the zone melting direction, and the thermal conductivity of the material is about two times that of the material, so that the thermoelectric performance of the zone melting direction is about two times that of the material perpendicular to the zone melting direction. Since Bi2Te3Crystal of the compound in Te(1)-Te(1)Easy slippage or cleavage between atomic planes along basal planes, resulting in zone melting of Bi2Te3The mechanical properties are poor and it is difficult to obtain the fine particles required for the fabrication of micro devices.
The high demands on mechanical properties have led in the last decade to an increasing focus of research on polycrystalline bismuth telluride based bulk thermoelectric materials. P-type (Bi, Sb) produced by high energy ball milling combined with hot pressing sintering was reported in Science by B.Poudel et al 20082Te3The compound greatly refines the crystal grains of the material by the ball milling process, and introduces high-density lattice defects, so that the crystal grain boundaries and the point defects generate strong scattering to heat phonons, the lattice thermal conductivity of the material is greatly reduced, and the maximum ZT value of the material can reach 1.4 at 400K. From then on, lead toThe over-structure nanocrystallization combined sintering process reduces the thermal conductivity of the material, thereby improving the thermoelectric property to be researched by Bi2Te3The main preparation method of the base thermoelectric material, but on the other hand, in the sintering process, the pressure causes fine grain slippage and rearrangement, and the finally obtained ingot body usually obtains the optimal performance in the direction perpendicular to the pressure direction, which is different from the optimal performance direction of the zone-melting sample, so that the existing mature zone-melting sample cutting process is difficult to apply, and a large amount of material is wasted.
The melt spinning process is a mature processing process capable of introducing nanostructures with different scales. The melt spinning process is to fast quench the molten metal to obtain thin strip sample with cooling rate up to 104-106K/s, the prepared thermoelectric material thin strip contains a large amount of amorphous or nanocrystalline structures, and the whole thin strip shows obvious orientation due to different cooling processes of the contact surface and the free surface of the thin strip. At present, the research on melt spinning is mainly to perform SPS sintering after grinding a thin strip to obtain a compact block material, and the method is the same as the structural nanocrystallization method such as the high-energy ball milling, and the like, so that the optimal performance direction of the finally obtained thermoelectric material is still perpendicular to the sintering pressure direction, and is not consistent with the existing mature cutting process of zone-melting materials.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for rapidly preparing high-performance p-type or n-type Bi easy to cut aiming at the defects in the prior art2Te3Method for producing base thermoelectric material, p-type or n-type Bi obtained2Te3The base thermoelectric material has excellent thermoelectric properties in a direction parallel to the pressure direction.
The technical scheme adopted by the invention for solving the technical problems is as follows:
rapid preparation of high-performance p-type or n-type Bi easy to cut2Te3A method of fabricating a thermoelectric material, comprising the steps of:
(1) high-purity simple substance is adopted as initial raw material, and p-type Bi and n-type Bi are obtained by melting2Te3A base ingot body;
(2) bi obtained in the step (1)2Te3Carrying out low-speed melt spinning on the base ingot body to obtain a thin strip;
(3) flatly paving the thin strip obtained in the step (2) in a mould to carry out spark plasma activated sintering (SPS) to obtain high-performance p-type or n-type Bi easy to cut2Te3A base thermoelectric material.
According to the scheme, the p-type Bi2Te3The chemical composition of the base thermoelectric material is BixSb2-xTe3(x is 0.4 to 0.6); n-type Bi2Te3The chemical composition of the base thermoelectric material is Bi2SeyTe3-y(y＝0.2～0.3)。
According to the scheme, the purity of the high-purity simple substance is more than 99 percent; according to p-type or n-type Bi2Te3The elements and the stoichiometric ratio thereof contained in the base thermoelectric material select high-purity simple substances as initial raw materials, and the elements are mainly selected from Bi, Sb, Te, Se and the like.
According to the scheme, the melting temperature is 1073-1273K, and the melting time is 6-12 h.
According to the scheme, the melt rotary-throwing rotating speed is 2-10 m/s, preferably 2-6 m/s, inert atmosphere such as nitrogen or argon is adopted, and the spraying caliber is 0.3-0.4 mm.
According to the method, the spark plasma activated sintering (SPS) is carried out under the conditions that the sintering pressure is 20-60 MPa, the sintering temperature is 400-500 ℃, the temperature rising speed is 50-150 ℃/min, and the sintering time is 2-10 min.
Compared with the prior art, the invention has the beneficial effects that: according to the method, the orientation thin strip obtained by directly sintering the melt and rotary throwing is adopted, so that the orientation of the thin strip is partially retained in the finally obtained thermoelectric material block, the mechanical performance is improved, meanwhile, the base thermoelectric material with the optimal performance direction consistent with that of a zone melting sample is obtained, the existing mature cutting and subsequent treatment process of the zone melting material can be directly used, and the utilization rate and the post-treatment efficiency of the material are obviously improved compared with those of the conventional polycrystalline material.
Drawings
FIG. 1 is a graph showing the change of conductance of the test sample with temperature in the direction parallel to the pressure direction and perpendicular to the pressure direction in example 1, in the direction parallel to the pressure direction in example 2, and in the direction parallel to the pressure direction in example 3, respectively.
FIG. 2 is a graph showing the Seebeck coefficient as a function of temperature for the samples tested in example 1 in the direction parallel to the pressure and in the direction perpendicular to the pressure, in example 2 in the direction parallel to the pressure, and in example 3 in the direction parallel to the pressure, respectively;
FIG. 3 is a graph showing the power factor of samples tested in example 1 parallel to the pressure direction and perpendicular to the pressure direction, example 2 parallel to the pressure direction, and example 3 parallel to the pressure direction as a function of temperature, respectively.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
In the following examples, high performance p-type or n-type Bi2Te3The method for preparing the base thermoelectric material comprises the following specific preparation processes: high-purity simple substances Bi, Te and Se or Sb are used as initial raw materials and are mixed according to a p-type BixSb2-xTe3(x is 0.4 to 0.6) or n-type Bi2SeyTe3-y(y is 0.2-0.3), weighing simple substances according to the stoichiometric ratio of elements, vacuum-sealing the weighed simple substances in a quartz tube, placing the quartz tube in a melting furnace, melting for 6-12 hours at 1073-1273K, and cooling along with the furnace; melt spinning is carried out on the ingot obtained by melting, the rotating speed of a copper rod is 2-10 m/s, the spraying caliber is 0.35mm under the argon atmosphere; directly spreading the thin strip obtained by spin-spinning the collected melt in a graphite mold with the inner diameter of 10-40 mm for SPS sintering, wherein the sintering pressure is 20-60 MPa, the sintering temperature is 400-500 ℃, the temperature rising speed is 50-150 ℃/min, and the temperature is kept for 2-10 min to obtain the high-performance p-type or n-type Bi easy to cut2Te3A base thermoelectric material.
Example 1
Rapid preparation of high-performance p-type Bi easy to cut2Te3A method of fabricating a thermoelectric material, comprising the steps of:
(1) high-purity simple substances Bi, Sb and Te are used as initial raw materials according to chemical compositionBi0.5Sb1.5Te3Weighing simple substances according to the stoichiometric ratio of the elements, vacuum sealing the weighed simple substances in a quartz tube, putting the quartz tube in a melting furnace, and melting to obtain p-type Bi2Te3A base ingot body; wherein the melting temperature is 1123K, and the melting time is 10 h;
(2) the obtained p-type Bi2Te3Carrying out low-speed melt spinning on the base ingot body to obtain a thin strip; wherein the melt spinning speed is 4m/s, argon atmosphere is adopted, and the jet caliber is 0.35 mm;
(3) laying the thin strip in a mould for spark plasma activated sintering (SPS) to obtain high-performance p-type Bi easy to cut2Te3A base thermoelectric material; wherein the sintering pressure is 24MPa, the sintering temperature is 400 ℃, the heating rate is 80 ℃/min, and the sintering time is 5 min.
For the p-type Bi prepared in example 12Te3The performance test is carried out on the base thermoelectric material, the performance test direction is parallel to the pressure direction, and the electric conductivity, the Seebeck coefficient and the power factor within the range of 300K-400K are shown in Table 1; the performance test direction is perpendicular to the pressure direction, and the conductivity, the Seebeck coefficient and the power factor within the range of 300K-400K are shown in Table 2. As is clear from Table 1-2, the p-type Bi prepared in example 12Te3The base thermoelectric material sample obtains more excellent performance in the direction parallel to the pressure direction.
TABLE 1
TABLE 2
| 300K | 350K | 400K | |
| Electrical conductivity (10)4S/m) | 8.58 | 6.34 | 4.79 |
| Seebeck coefficient (μ V/K) | 211 | 227 | 225 |
| Power factor (mV/mK)2) | 3.82 | 3.26 | 2.42 |
Example 2
The present embodiment is different from embodiment 1 in that: the SPS sintering pressure is 24MPa, the sintering temperature is 450 ℃, and the temperature is kept for 5 min.
For the p-type Bi prepared in example 22Te3The performance test of the base thermoelectric material is carried out, the performance test direction is parallel to the pressure direction, and the electric conductivity, the Seebeck coefficient and the power factor within the range of 300K-400K are shown in Table 3.
TABLE 3
| 300K | 350K | 400K | |
| Electrical conductivity (10)4S/m) | 10.9 | 8.4 | 6.3 |
| Seebeck coefficient (μ V/K) | 196 | 213 | 213 |
| Power factor (mV/mK)2) | 4.2 | 3.8 | 2.86 |
Example 3
The present embodiment is different from embodiment 1 in that: the SPS sintering pressure is 40MPa, the sintering temperature is 450 ℃, and the temperature is kept for 5 min.
For the p-type Bi prepared in example 32Te3The performance test of the base thermoelectric material is carried out, the performance test direction is parallel to the pressure direction, and the electric conductivity, the Seebeck coefficient and the power factor within the range of 300K-400K are shown in Table 4.
TABLE 4
| 300K | 350K | 400K | |
| Electrical conductivity (10)4S/m) | 10.6 | 7.8 | 5.87 |
| Seebeck coefficient (μ V/K) | 198 | 214 | 215 |
| Power factor (mV/mK)2) | 4.15 | 3.55 | 2.72 |
Example 4
Rapid preparation of high-performance n-type Bi easy to cut2Te3A method of fabricating a thermoelectric material, comprising the steps of:
(1) high-purity elementary substances Bi, Se and Te are used as initial raw materials, and Bi is chemically formed2Se0.3Te2.7Weighing simple substances according to the stoichiometric ratio of the elements, vacuum sealing in a quartz tube after weighing, placing the quartz tube in a melting furnace, and melting to obtain n-type Bi2Te3The ingot body is based, the melting temperature is 1123K, and the melting time is 10 h;
(2) subjecting the obtained n-type Bi2Te3Carrying out low-speed melt spinning on the base ingot body to obtain a thin strip; wherein the melt spinning rotating speed is 4m/s, the jet caliber is 0.35mm under argon atmosphere;
(3) laying the thin strip in a mould for spark plasma activated sintering (SPS) to obtain the high-performance n-type Bi easy to cut2Te3A base thermoelectric material; wherein the sintering pressure is 40MPa, the sintering temperature is 450 ℃, the heating rate is 80 ℃/min, and the sintering time is 5 min.
For the n-type Bi prepared in example 42Te3The performance test of the base thermoelectric material is carried out, the performance test direction is parallel to the pressure direction, and the electric conductivity, the Seebeck coefficient and the power factor within the range of 300K-400K are shown in Table 4.
TABLE 4
| 300K | 350K | 400K | |
| Electrical conductivity (10)4S/m) | 10.1 | 8.2 | 6.8 |
| Seebeck coefficient (μ V/K) | -198 | -207 | -211 |
| Power factor (mV/mK)2) | 3.96 | 3.5 | 3.03 |
In the prior art, polycrystalline Bi obtained by sintering is often used2Te3The direction of optimum performance of the base thermoelectric material is perpendicular to the pressure direction, while the sintered ingot body is generally cylindrical in order to ensure uniform pressure and temperature. In order to obtain suitable particles by cutting, in this case, first, sheets with the same thickness need to be cut from the sintered ingot body along the vertical direction, and then square particles need to be cut from the sheets with different sizes. The optimal performance direction of the sintered ingot body prepared by the method is parallel to the pressure direction, is consistent with the commercial zone-melting bar material, and can be directly used by the existing mature cutting process, namely, the ingot body is cut into completely consistent wafers along the horizontal direction, and then the wafers are cut into square particles without changing the cutting program, so that the cutting is easier while the loss rate is reduced.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (8)
1. Rapid preparation of high-performance Bi easy to cut2Te3A method of forming a thermoelectric material, comprising the steps of:
(1) according to Bi2Te3The chemical composition of the base thermoelectric material adopts simple substance as initial raw material, and Bi is obtained by melting2Te3A base ingot body;
(2) bi obtained in the step (1)2Te3Proceeding from a basic ingot bodyMelt spinning to obtain a thin strip;
(3) paving the thin strip obtained in the step (2) in a mould for spark plasma activation sintering to obtain high-performance Bi easy to cut2Te3A base thermoelectric material.
2. The rapid preparation of high-performance Bi easy to cut as claimed in claim 12Te3A method for producing a thermoelectric material, characterized in that Bi is used2Te3The base thermoelectric material is either p-type or n-type.
3. The rapid preparation of high-performance Bi easy to cut as claimed in claim 22Te3Method for producing thermoelectric materials, characterized in that p-type Bi2Te3The chemical composition of the base thermoelectric material is BixSb2-xTe3X = 0.4-0.6; n-type Bi2Te3The chemical composition of the base thermoelectric material is Bi2SeyTe3-y，y=0.2~0.3。
4. The rapid preparation of high-performance Bi easy to cut as claimed in claim 22Te3A method for producing a thermoelectric material, characterized in that the elementary substance has a purity of more than 99%; according to p-type or n-type Bi2Te3The element contained in the base thermoelectric material is selected as a simple substance as a starting material.
5. The rapid preparation of high-performance Bi easy to cut as claimed in claim 12Te3The method for preparing the base thermoelectric material is characterized in that the melting temperature is 1073-1273K, and the melting time is 6-12 h.
6. The rapid preparation of high-performance Bi easy to cut as claimed in claim 12Te3The method for preparing the base thermoelectric material is characterized in that the rotating speed of melt spinning is 2-6 m/s, and the melt spinning is performed in an inert atmosphere or a nitrogen atmosphere.
7. The rapid preparation of claim 1 is easyHigh performance Bi for cutting2Te3The method for preparing the base thermoelectric material is characterized in that the discharge plasma activation sintering is carried out, the sintering pressure is 20-60 MPa, the sintering temperature is 400-500 ℃, and the sintering time is 2-10 min.
8. Easily cuttable high-performance Bi prepared by the method of claim 12Te3A base thermoelectric material.
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| CN113735582A (en) * | 2021-09-09 | 2021-12-03 | 武汉科技大学 | Preparation method of bismuth telluride-based thermoelectric material |
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