CN112531097A - N-type bismuth telluride-based thermoelectric material and preparation method thereof - Google Patents
N-type bismuth telluride-based thermoelectric material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an n-type bismuth telluride-based thermoelectric material and a preparation method thereof. The chemical composition of the n-type bismuth telluride-based thermoelectric material is as follows: bi2Te2.7Se0.3+ x% by weight of Sb of which 0<x is less than or equal to 10. In the n-type bismuth telluride-based thermoelectric material, the metal Sb nanophase is dispersed in Bi2Te2.7Se0.3In the presence of Bi2Te2.7Se0.3The energy filtering effect of the Schottky barrier on the Sb contact interface can scatter low-energy carriers, increase the effective mass of electrons and improve the power factor of the material. Meanwhile, the uniformly dispersed Sb can enhance the scattering of low-frequency phonons by the interface and reduce the thermal conductivity of the material. Therefore, the Sb doping can optimize the electric and heat transmission performance at the same time, and the improvement of the ZT value of the n-type bismuth telluride-based thermoelectric material is realized.
Description
Technical Field
The invention relates to the technical field of thermoelectric materials, in particular to an n-type bismuth telluride-based thermoelectric material and a preparation method thereof.
Background
The thermoelectric conversion technology is a novel green energy technology capable of realizing direct interconversion between heat energy and electric energy, and the principle of the thermoelectric conversion technology is based on the Seebeck effect and the Peltier effect and mainly depends on the transmission and interaction of current carriers and phonons in a semiconductor. The thermoelectric device has the advantages of no mechanical transmission part, no noise and no pollution in the working and operating process and the like, has wide application prospect in the field of thermoelectric generation and thermoelectric refrigeration, and the energy conversion efficiency mainly depends on the dimensionless thermoelectric figure of merit (ZT value) of the thermoelectric material: ZT ═ S (S)2σ) T/κ, where S is the Seebeck coefficient, σ is the electrical conductivity, T is the thermodynamic absolute temperature, and κ is the thermal conductivity. Due to the coupling between the parameters, the pursuit of high ZT values has been a very challenging goal for researchers in this field.
The thermoelectric material can be divided into room-temperature thermoelectric material (less than 500K), medium-temperature thermoelectric material (500-900K) and high-temperature thermoelectric material (more than 900K) according to service temperature, and the bismuth telluride-based thermoelectric material is the most mature room-temperature thermoelectric material currently applied. At present, the thermoelectric device is the most common flat-plate type device, thermoelectric arms prepared from p-type thermoelectric materials and n-type thermoelectric materials need to be electrically connected in series, the ZT value of p-type bismuth telluride base materials in the prior research can reach more than 1.3, the ZT value of n-type materials prepared by a commercial zone melting method is only about 1.0, and the development of the p-type materials and the thermoelectric device is severely restricted. How to improve the ZT value of the n-type thermoelectric material is of great significance for improving the energy conversion efficiency of thermoelectric devices and large-scale commercial application of thermoelectric technology.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the invention aims to provide an n-type bismuth telluride-based thermoelectric material and a preparation method thereof. The n-type bismuth telluride-based thermoelectric material can obtain excellent thermoelectric performance by doping Sb.
In one aspect of the invention, an n-type bismuth telluride-based thermoelectric material is provided. According to the inventionIn an illustrative embodiment, the chemical composition of the n-type bismuth telluride-based thermoelectric material is as follows: bi2Te2.7Se0.3+ x% by weight of Sb of which 0<x≤10。
According to the n-type bismuth telluride-based thermoelectric material provided by the embodiment of the invention, the metal Sb nanophase is dispersed in Bi2Te2.7Se0.3In the presence of Bi2Te2.7Se0.3The energy filtering effect of the Schottky barrier on the Sb contact interface can scatter low-energy carriers, increase the effective mass of electrons and improve the power factor of the material. Meanwhile, the uniformly dispersed Sb can enhance the scattering of low-frequency phonons by the interface and reduce the thermal conductivity of the material. Therefore, the Sb doping can optimize the electric and heat transmission performance at the same time, and the improvement of the ZT value of the n-type bismuth telluride-based thermoelectric material is realized.
In addition, the n-type bismuth telluride-based thermoelectric material according to the above embodiment of the present invention may also have the following additional technical features:
in some embodiments of the invention, the chemical composition of the n-type bismuth telluride-based thermoelectric material is Bi2Te2.7Se0.3+ x wt% of Sb, wherein x is more than or equal to 4 and less than or equal to 6.
In another aspect of the present invention, the present invention proposes a method of preparing the n-type bismuth telluride-based thermoelectric material of the above embodiment. According to an embodiment of the invention, the method comprises: (1) mixing the raw materials of Bi, Se and Te according to a predetermined stoichiometric ratio and carrying out smelting treatment to obtain Bi2Te2.7Se0.3Casting ingots; (2) the Bi is added2Te2.7Se0.3Pre-grinding the cast ingot, mixing the pre-ground cast ingot with Sb raw material and carrying out ball milling treatment to obtain Bi2Te2.7Se0.3+ x wt% Sb powder; (3) the Bi is added2Te2.7Se0.3And (5) sintering the + x wt% Sb powder to obtain the n-type bismuth telluride-based thermoelectric material.
According to the method for preparing the n-type bismuth telluride-based thermoelectric material of the embodiment of the invention, firstly, Bi prepared from Bi, Se and Te raw materials is utilized2Te2.7Se0.3Ingot casting, which is pre-ground and then ball-milled by mixing with Sb raw material to obtain nanoscaleThe second phase of Sb metal of (1) is introduced into the material, and Bi is utilized2Te2.7Se0.3And energy filtering effect of the Schottky barrier on the Sb contact interface scatters low-energy carriers, so that the effective mass of electrons is increased, and the power factor of the material is improved. Meanwhile, the uniformly dispersed Sb can enhance the scattering of low-frequency phonons by the interface and reduce the thermal conductivity of the material. Therefore, in the n-type bismuth telluride based thermoelectric material prepared by the method, Sb doping can optimize the electric and heat transmission performance at the same time, and the ZT value of the n-type bismuth telluride based thermoelectric material is improved.
In addition, the method for preparing the n-type bismuth telluride-based thermoelectric material according to the embodiment of the invention can also have the following additional technical characteristics:
in some embodiments of the present invention, the purity of the Bi, Se, Te raw materials is no less than 99.999%.
In some embodiments of the invention, the smelting process comprises: heating to 500-700 ℃ at a heating rate of 2-5 ℃/min, preserving heat for 0.5-2 h, heating to 750-950 ℃ at a heating rate of 1-2 ℃/min, preserving heat for 2-10 h, and cooling to room temperature.
In some embodiments of the present invention, the pre-grinding is performed for 0.5 to 2 hours.
In some embodiments of the invention, the ball milling process is performed in an inert gas atmosphere.
In some embodiments of the invention, in the ball milling treatment, the ball-to-material ratio is (10-20): 1, the ball milling rotation speed is 400-500 r/min, and the ball milling time is 2-10 h.
In some embodiments of the invention, the sintering process is spark plasma sintering.
In some embodiments of the present invention, the spark plasma sintering is performed at a pressure of 40 to 50MPa and a temperature of 400 to 500 ℃ for 5 to 8 min.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 shows Bi obtained in example 12Te2.7Se0.3Graphs of high angle annular dark field image (HAADF) and energy spectrum (EDS) characterization results for +5 wt% Sb;
FIG. 2 is a graph showing the ZT value test results of the thermoelectric materials in example 1 and comparative examples 1 and 2;
fig. 3 is a graph showing the results of the maximum ZT values and the average ZT values of the thermoelectric materials in example 1 and comparative examples 1 and 2.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are illustrative only and are not to be construed as limiting the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available. In addition, the room temperature refers to the ambient temperature when the method is performed, for example, 20 to 30 ℃.
In one aspect of the invention, an n-type bismuth telluride-based thermoelectric material is provided. According to an embodiment of the present invention, the chemical composition of the n-type bismuth telluride-based thermoelectric material is as follows: bi2Te2.7Se0.3+ x% by weight of Sb of which 0<x≤10。
Specifically, x may be 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 8, 9, 10, or the like. More preferably, 4. ltoreq. x.ltoreq.6.
According to the n-type bismuth telluride-based thermoelectric material provided by the embodiment of the invention, the metal Sb nanophase is dispersed in Bi2Te2.7Se0.3In the presence of Bi2Te2.7Se0.3The energy filtering effect of the Schottky barrier on the Sb contact interface can scatter low-energy carriers, increase the effective mass of electrons and improve the power factor of the material. Meanwhile, the uniformly dispersed Sb can enhance the scattering of low-frequency phonons by the interface and reduce the thermal conductivity of the material. Thus, Sb dopingThe electric and heat transmission performance can be optimized simultaneously, and the improvement of the ZT value of the n-type bismuth telluride-based thermoelectric material is realized.
In another aspect of the present invention, the present invention proposes a method of preparing the n-type bismuth telluride-based thermoelectric material of the above embodiment. According to an embodiment of the invention, the method comprises: (1) mixing the raw materials of Bi, Se and Te according to a predetermined stoichiometric ratio and carrying out smelting treatment to obtain Bi2Te2.7Se0.3Casting ingots; (2) adding Bi2Te2.7Se0.3Pre-grinding the cast ingot, mixing the pre-ground cast ingot with Sb raw material and carrying out ball milling treatment to obtain Bi2Te2.7Se0.3+ x wt% Sb powder; (3) adding Bi2Te2.7Se0.3And (5) sintering the + x wt% Sb powder to obtain the n-type bismuth telluride-based thermoelectric material.
The method for producing the n-type bismuth telluride-based thermoelectric material according to the embodiment of the present invention is further described in detail below.
Firstly, mixing raw materials of Bi, Se and Te according to a predetermined stoichiometric ratio and carrying out smelting treatment to obtain Bi2Te2.7Se0.3And (5) ingot casting. Specifically, the Bi, Se, Te raw materials can be put into a quartz tube, and the tube can be sealed after being vacuumized (for example, the tube can be vacuumized to a vacuum degree of 1 × 10)-4～9×10-4Pa), and then putting the raw materials into a muffle furnace for smelting treatment.
According to some embodiments of the present invention, the purity of the above-mentioned raw materials of Bi, Se and Te is not less than 99.999%. Specifically, the raw materials of Bi, Se and Te can be particles of elementary substances of Bi, Se and Te respectively.
According to some embodiments of the invention, the smelting process comprises: heating to 500-700 deg.C (e.g. 500 deg.C, 550 deg.C, 600 deg.C, 650 deg.C, 700 deg.C) at a heating rate of 2-5 deg.C/min (e.g. 2 deg.C/min, 3 deg.C/min, 4 deg.C/min, 5 deg.C/min, etc.), maintaining for 0.5-2 h (e.g. 0.5h, 1h, 1.5h, 2h, etc.), heating to 750-950 deg.C (e.g. 750 deg.C, 800 deg.C, 900 deg.C, 950 deg.C) at a heating rate of 1-2 deg.C/min (e.g. 1 deg.C/min, 1.5 deg.C/min, 2 deg.C/min), maintaining for 2-10 h (. By performing the melting treatment under the above-mentioned operating conditions, Bi of high quality can be obtained2Te2.7Se0.3And (4) casting a ingot matrix.
Further, adding Bi2Te2.7Se0.3Pre-grinding the cast ingot, mixing the pre-ground cast ingot with Sb raw material and carrying out ball milling treatment to obtain Bi2Te2.7Se0.3+ x wt% Sb powder.
According to some embodiments of the invention, the pre-grinding is performed for a time of 0.5 to 2 hours, such as 0.5 hour, 1.5 hour, 2 hours, etc. Thus, Bi can be efficiently converted2Te2.7Se0.3And breaking the cast ingot so as to facilitate the subsequent ball milling treatment.
According to some embodiments of the invention, the ball milling process is performed in an inert gas atmosphere. Specifically, after the raw materials are put into ball milling equipment (such as a ball milling tank), the ball milling equipment is vacuumized to 1-9 Pa, and then inert gas (such as nitrogen, argon and the like) is filled into the ball milling equipment so as to perform the ball milling treatment. Thus, the Sb nanophase in Bi can be further favorably formed2Te2.7Se0.3The dispersion in the formula (I) further improves the thermoelectric performance of the material.
According to some embodiments of the invention, in the ball milling treatment, the ball-to-material ratio is (10-20): 1, the ball milling rotation speed is 400-500 r/min, and the ball milling time is 2-10 h. Specifically, the ball-material ratio can be 10:1, 12:1, 15:1, 18:1, 20:1 and the like, the ball milling rotation speed can be 400r/min, 425r/min, 450r/min, 475r/min, 500r/min and the like, and the ball milling time can be 2h, 4h, 6h, 8h, 10h and the like. The ball milling treatment under the above conditions can further contribute to the Sb nanophase in Bi2Te2.7Se0.3The dispersion in the formula (I) further improves the thermoelectric performance of the material.
Further, adding Bi2Te2.7Se0.3And (5) sintering the + x wt% Sb powder to obtain the n-type bismuth telluride-based thermoelectric material.
Preferably, according to some embodiments of the invention, the sintering process is spark plasma sintering. Therefore, the material with fine and uniform tissue and high density can be obtained at relatively low sintering temperature; low sintering energy consumption and good product quality.
According to some embodiments of the present invention, the spark plasma sintering may be performed at a pressure of 40 to 50MPa and a temperature of 400 to 500 ℃ for 5 to 8 min. Specifically, the sintering pressure can be 40MPa, 42MPa, 45MPa, 48MPa, 50MPa, etc., the sintering temperature can be 400 ℃, 425 ℃, 450 ℃, 475 ℃, 500 ℃, etc., and the sintering time can be 5min, 6min, 7min, 8min, etc. By subjecting Bi to the above conditions2Te2.7Se0.3+ x wt% Sb powder sintering to obtain compact and homogeneous Bi2Te2.7Se0.3+ x wt% Sb block.
In addition, it should be noted that all the features and advantages described above for the n-type bismuth telluride-based thermoelectric material are also applicable to the method for preparing the n-type bismuth telluride-based thermoelectric material, and are not described in detail herein.
In summary, the n-type bismuth telluride-based thermoelectric material and the preparation method thereof provided by the invention can have at least one of the following advantages:
1. dispersing metal Sb nano-phase in Bi by ball milling2Te2.7Se0.3In the method, the mass percent of Sb (namely the value of x) is adjusted to regulate and control the electron and phonon transmission of the material.
2. By using Bi2Te2.7Se0.3Energy filtering effect of Schottky barrier on the Sb contact interface scatters low-energy carriers, effective electron quality is increased, and power factor of the material is improved; and the uniformly dispersed Sb is utilized to enhance the scattering of low-frequency phonons by the interface and reduce the thermal conductivity of the material.
3. Meanwhile, the electricity and heat transmission performance is optimized, and the ZT value of the N-type bismuth telluride thermoelectric material is improved.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
High-purity Bi, Te and Se particles are prepared according to Bi2Te2.7Se0.3Of (2) is stoichiometricMixing and carrying out smelting treatment, wherein the smelting treatment comprises the following steps: heating to 600 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 850 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 5h, and cooling to room temperature to obtain Bi2Te2.7Se0.3And (5) ingot casting.
Adding Bi2Te2.7Se0.3Pre-grinding the cast ingot, mixing the cast ingot with 5 wt% of high-purity Sb particles, and ball-milling the mixture for 10 hours at the rotating speed of 450r/min to obtain Bi2Te2.7Se0.3+ 5% by weight of Sb powder.
The Bi is added2Te2.7Se0.3And (3) performing discharge plasma sintering on the +5 wt% Sb powder, wherein the sintering temperature is 450 ℃, the sintering pressure is 50MPa, and the sintering time is 5min, so as to prepare the phi 10 x 10 columnar block. After cutting, the maximum ZT value is 1.3(400K), and the average ZT value is ZTaveIs 1.0(300 to 575K).
The prepared product is characterized by high-angle annular dark field image (HAADF) and energy spectrum (EDS), and the result is shown in figure 1.
Comparative example 1
High-purity Bi, Te and Se particles are prepared according to Bi2Te2.7Se0.3Mixing the stoichiometric ratios of (a) and carrying out a smelting process, the smelting process comprising: heating to 600 ℃ at the heating rate of 3 ℃/min, preserving heat for 1h, heating to 850 ℃ at the heating rate of 1.5 ℃/min, preserving heat for 5h, and cooling to room temperature to obtain Bi2Te2.7Se0.3And (5) ingot casting.
The Bi is added2Te2.7Se0.3And (3) performing discharge plasma sintering on the powder, wherein the sintering temperature is 450 ℃, the sintering pressure is 50MPa, and the sintering time is 5min, so as to prepare the phi 10 x 10 columnar block. After cutting, the maximum ZT value is 0.9(400K), and the average ZT value is ZTaveIs 0.8(300 to 575K).
Comparative example 2
The commercial n-type bismuth telluride alloy prepared by adopting a zone melting method has the maximum ZT value of 1.0(400K) and the average ZT value of ZTaveIs 0.7(300 to 575K).
Materials of example 1, comparative examples 1 and 2The results of the material ZT value test are summarized in fig. 2 and 3. It can be seen that Bi of the present invention2Te2.7Se0.3The material is doped by Sb, compared with undoped Bi2Te2.7Se0.3The material and the commercial n-type bismuth telluride alloy by the zone melting method have improved maximum ZT value and average ZT value, and better thermoelectric property.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. An n-type bismuth telluride-based thermoelectric material is characterized by comprising the following chemical components: bi2Te2.7Se0.3+ x% by weight of Sb of which 0<x≤10。
2. The n-type bismuth telluride-based thermoelectric material as claimed in claim 1, wherein x is 4. ltoreq. x.ltoreq.6.
3. A method for producing the n-type bismuth telluride-based thermoelectric material as claimed in claim 1 or 2, characterized by comprising:
(1) mixing the raw materials of Bi, Se and Te according to a predetermined stoichiometric ratio and carrying out smelting treatment to obtain Bi2Te2.7Se0.3Casting ingots;
(2) the Bi is added2Te2.7Se0.3Pre-grinding the cast ingot, mixing the pre-ground cast ingot with Sb raw material and carrying out ball milling treatment to obtain Bi2Te2.7Se0.3+ x wt% Sb powder;
(3) the Bi is added2Te2.7Se0.3And (5) sintering the + x wt% Sb powder to obtain the n-type bismuth telluride-based thermoelectric material.
4. The method as claimed in claim 3, wherein the purity of the Bi, Se, Te raw materials is not less than 99.999%.
5. The method defined in claim 3 wherein the smelting process comprises: heating to 500-700 ℃ at a heating rate of 2-5 ℃/min, preserving heat for 0.5-2 h, heating to 750-950 ℃ at a heating rate of 1-2 ℃/min, preserving heat for 2-10 h, and cooling to room temperature.
6. The method according to claim 3, wherein the pre-grinding is performed for a time of 0.5 to 2 hours.
7. The method of claim 3, wherein the ball milling process is performed in an inert gas atmosphere.
8. The method according to claim 3, wherein in the ball milling treatment, the ball-to-material ratio is (10-20): 1, the ball milling rotation speed is 400-500 r/min, and the ball milling time is 2-10 h.
9. A method according to claim 3, wherein the sintering process is spark plasma sintering.
10. The method according to claim 9, wherein the spark plasma sintering is performed at a pressure of 40 to 50MPa and a temperature of 400 to 500 ℃ for 5 to 8 min.
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