CN110379914B - Sb synthesis based on liquid phase method 2 Te 3 Thermoelectric property improving method of-Te nano heterojunction material - Google Patents
Sb synthesis based on liquid phase method 2 Te 3 Thermoelectric property improving method of-Te nano heterojunction material Download PDFInfo
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Abstract
The invention discloses a method for synthesizing Sb based on a liquid phase method 2 Te 3 The thermoelectric property of the-Te nano heterojunction material is improved by reducing Sb 2 Te 3 Solvothermal reaction temperature to synthesize Sb 2 Te 3 Growing Te nano-wire in situ to make the product show Te nano-wire series hexagonal disc type Sb 2 Te 3 The shape of the sugarcoated haws; and then the synthesized nano powder is further subjected to hydrogen reduction treatment, and the block material is obtained through discharge plasma liquid phase sintering. The invention not only realizes Sb by reducing the reaction temperature 2 Te 3 Self-assembly growth of-Te nano heterojunction, and overcomes the defect of common mechanical composite Sb 2 Te 3 Non-uniformity problems with Te and weak interface bonding problems. Further investigation of its thermoelectric properties revealed that Sb 2 Te 3 the-Te heterojunction shows more excellent thermoelectric performance, the highest ZT value reaches 0.6 at 498K, and the thermoelectric performance is relatively pure Sb 2 Te 3 The block body is improved by 69%.
Description
Technical Field
The invention belongs to the technical field of nano thermoelectric material preparation, and particularly relates to a method for synthesizing Sb based on a liquid phase method 2 Te 3 A thermoelectric property improving method of the-Te nano heterojunction material.
Background
The global energy crisis is becoming more serious, fossil fuels are running to exhaustion, and the development of new clean energy is urgently needed. Thermoelectric materials have been attracting attention and studied as a functional material capable of directly realizing interconversion between functions and thermal energy. Compared with the traditional functional device, the thermoelectric power generation and refrigeration device manufactured by taking the thermoelectric material as the core has the advantages of no noise, no pollution, small volume, low maintenance cost and the like, so that the thermoelectric power generation and refrigeration device has wide application prospect.
The performance of thermoelectric materials is measured by a dimensionless thermoelectric figure of merit, ZT, which can be defined as: ZT ═ S 2 σ T/κ, where S is the Seebeck coefficient, σ is the electrical conductivity, T is the absolute temperature, and κ is the thermal conductivity. It is clear that achieving a high ZT value requires achieving a high S at the same time 2 σ and low κ, however, the electrical and acoustic transport channels in the thermoelectric material are interacting and linked, which makes S, σ, and κ coupled to each other, difficult to optimize simultaneously. In recent decades, both theoretical predictions and experimental studies have found that nanosystems have high density of states and increased phonon scattering or reduced lattice thermal conductivity factors, so "structural nanoscopic" of thermoelectric materials is considered to be one of the most promising strategies for optimizing ZT values. The preparation of the nano thermoelectric material is generally divided into two categories of physics and chemistry, wherein the physics method is a top-down method and comprises a ball milling method and a melt spinning method; the chemical method is a bottom-up method for preparing nano powder, and comprises an electrochemical deposition method, a warm liquid phase synthesis method, an organic solution high-temperature synthesis method, a solvothermal method and the like.
Sb 2 Te 3 Belongs to a tetragonal system and is a binary V with a narrow band gap layered structure 2 VI 3 Group semiconductor compounds, the compound system has been widely studied because of the good ZT value in the low temperature region. But pure Sb 2 Te 3 Due to its own inversion defect (Sb' Te ) A large number of vacancies are generated, resulting in a very low Seebeck coefficient, so that the final ZT value is not high. At present, related documents report that Sb with various morphologies is prepared by several chemical methods 2 Te 3 For example: ren et alProduction of single crystal Sb by surfactant assisted solvothermal method is reported 2 Te 3 A nano-plate; junyou Yang et al reported that Sb is prepared by electrochemical atomic layer epitaxy method 2 Te 3 A nano-film; hongjie Zhang et al report hydrothermal method for preparing single crystal Sb 2 Te 3 A nanoribbon. However, due to Sb 2 Te 3 Spontaneous occupation of part of Sb atoms in Te crystal lattice always occurs, and single Sb with good crystallinity can be synthesized 2 Te 3 Phase is not easy to implement. In addition, most of the current research is focused on different methods for preparing Sb 2 Te 3 On the nano phase, the research on the preparation of nano blocks and the performance improvement is still relatively rare.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for synthesizing Sb based on a liquid phase method 2 Te 3 A thermoelectric property improving method of the-Te nano heterojunction material.
The invention synthesizes Sb based on a liquid phase method 2 Te 3 The thermoelectric property of the-Te nano heterojunction material is improved by reducing Sb 2 Te 3 Solvothermal reaction temperature to synthesize Sb 2 Te 3 Growing Te nano-wire in situ to make the product show Te nano-wire series hexagonal disc type Sb 2 Te 3 The shape of the sugarcoated haws; and then the synthesized nano powder is further subjected to hydrogen reduction treatment, and the block material is obtained through discharge plasma liquid phase sintering. The self-assembly method overcomes the defect of the traditional mechanical mixed Sb 2 Te 3 Heterogeneity with elemental Te, and the resulting sugarcoated haws shape profile illustrates Sb 2 Te 3 The interface with Te is likely to be chemically bonded, which is beneficial to the reduction of thermal conductivity while maintaining as good electrical transport properties as possible. In addition, Sb generated by self-assembly method 2 Te 3 the-Te realizes liquid phase sintering (higher than the melting point of Te) very conveniently and contributes to increase of Sb 2 Te 3 The thermoelectric property of the base material. The method specifically comprises the following steps:
step 1: sb 2 Te 3 -Te nanoPreparation of the powder
0.8g NaOH is weighed out and dissolved in 80ml ethylene glycol, then 2g polyvinylpyrrolidone (PVP) is added, stirring is carried out until complete dissolution, and then 0.664g Na is added to the solution 2 TeO 3 After the mixture was sufficiently dissolved, 0.456g of SbCl was added 3 Stirring and mixing uniformly, transferring the solution into a 100ml reaction kettle, and reacting for 36h at 190 ℃; after the reaction is finished, the product is centrifugally washed by deionized water and absolute ethyl alcohol respectively, and then is placed in a vacuum drying oven to be dried for 48 hours at the temperature of 60 ℃; in step 1, according to Sb 2 Te 3 Weighing Na according to stoichiometric ratio 2 TeO 3 And SbCl 3 。
Step 2: reduction treatment
Reducing the product dried in the step 1 in a hydrogen reduction furnace;
and step 3: sintering
And (3) placing the powder sample reduced in the step (2) in a graphite die, and obtaining a block material through SPS sintering. Cutting the obtained block material into rectangular strips of dimensions 3X 12mm and
wafers were used for thermoelectric performance testing.
In the step 2, the reduction temperature is 300 ℃, and the reduction time is 3 h.
In step 3, the sintering temperature of the spark plasma sintering is 460 ℃ (Te melting point 452 ℃), and the sintering time is 5 minutes.
In step 3, the temperature rise rate of the discharge plasma sintering is 50 ℃/min, the initial sintering pressure is 1MPa, the pressure is increased to 45MPa at 200 ℃, the pressure is maintained for 5 minutes at 460 ℃, and the pressure is released to 1MPa when the temperature is reduced to 250 ℃.
The synthesized product is Sb when the reaction temperature is 220 DEG C 2 Te 3 The material is in a regular hexagonal shape, the edge size is about 600nm, and the thickness is about 10 nm; when the temperature is reduced to 190 ℃, the product is in a series connection of Te nano-wires and hexagonal Sb 2 Te 3 Has a novel shape of "candied gourd" and Sb 2 Te 3 The thickness becomes extremely thin.
The invention has the beneficial effects that:
by simple reduction of Sb 2 Te 3 The reaction temperature is synthesized by a solvothermal method, so that a small amount of Te nanowires are connected with extremely thin Sb in series in the product 2 Te 3 Novel morphology of the sheet, which may be due to TeO 3- The intermediate Te generated by reduction under alkaline condition can not be completely reduced into Te after the thermodynamic reaction temperature is reduced 2- And Sb 3+ Formation of Sb 2 Te 3 But is saved in small quantities. Sb thus produced 2 Te 3 And the final performance ZT value of the material is improved by 69 percent by liquid phase sintering of the-Te heterojunction.
Drawings
FIG. 1 shows the synthesis of Sb by solvothermal method at 190 ℃ and 220 ℃ 2 Te 3 XRD pattern of (a).
FIG. 2 shows the solvothermal synthesis of Sb at 190 ℃ and 220 ℃ 2 Te 3 Scanning topography.
FIG. 3 is Sb 2 Te 3 -Te liquid phase sintering phenomenon.
FIG. 4 shows Sb 2 Te 3 And Sb 2 Te 3 -fracture morphology of block after Te sintering.
Fig. 5 is a variation relationship between the Seebeck coefficient of the material and the temperature.
Fig. 6 is a graph showing the relationship between the conductivity of a material and the temperature.
FIG. 7 is a graph of the variation of material power factor versus temperature.
Fig. 8 is a graph of material thermal conductivity as a function of temperature.
Fig. 9 is a graph of material ZT versus temperature change.
Detailed Description
The invention synthesizes Sb based on a liquid phase method 2 Te 3 The thermoelectric property improving method of the-Te nano heterojunction material comprises the following steps:
1. pure Sb 2 Te 3 And Sb 2 Te 3 Preparation of-Te nano powder
0.8g NaOH is weighed out and dissolved in 80ml ethylene glycol, then 2g polyvinylpyrrolidone (PVP) is added, stirring is carried out until complete dissolution, and then 0.664g Na is added to the solution 2 TeO 3 After it had dissolved sufficiently, 0.456g of SbCl was added 3 Stirring for 20 minutes, transferring the solution into a 100ml reaction kettle, and reacting at 190 ℃ and 220 ℃ for 36 hours respectively; after the reaction is finished, centrifugally washing the product for a plurality of times by using deionized water and absolute ethyl alcohol, and then placing the product in a vacuum drying oven to dry for 48 hours at the temperature of 60 ℃; to identify the phase composition of the powder, X-ray diffraction analysis was performed. FIG. 1 is a phase XRD spectrum of a mixed powder; in order to observe the morphology and size of the synthesized powder, SEM characterization analysis was performed, and the results are shown in FIG. 2.
2. Reduction treatment
Reducing the product dried in the step 1 in a hydrogen reduction furnace at 300 ℃ for 3 h;
3. sintering
And (3) placing the powder sample reduced in the step (2) in a graphite die, and obtaining a block material through SPS sintering. The SPS sintering process comprises the following steps: the sintering pressure is 40MPa, the temperature is increased to 460 ℃ at the heating rate of 50 ℃/min, the pressure is maintained for 5 minutes, and the pressure is slowly removed when the temperature is reduced to 250 ℃. The liquid phase sintering phenomenon is shown in fig. 3. In order to observe the microstructure of the sintered block material, SEM characterization analysis is carried out on the fracture morphology of the block of the sintered sample, and the result is shown in FIG. 4.
Cutting the obtained block material into rectangular strips of dimensions 3X 12mm and
wafers were used for thermoelectric performance testing. And respectively cutting the sintered block sample into rectangular strips with the size of 3 multiplied by 12mm by a diamond slicer to test the electrical property, and cutting a phi 6mm wafer to test the thermal property (thermal diffusion coefficient and density), wherein the test of all the sample properties is along the vertical direction. (Seeebck coefficient and conductivity were both measured using LRS-3 (Linsais, Germany, using 6N-He gas as a protective atmosphere during the test) and the results are shown in FIGS. 5 and 6. FIG. 7 shows the power factor of the material (PF ═ S2. sigma.) as a function of temperature, the thermal diffusion coefficient. lambda. of the material was measured using a laser thermal conductivity meter (LFA-457, Netsch, Germany), the density. rho of the thermally diffused sample was measured using the Archimedes method, and the specific heat of the material was measured during the testHuge errors can be generated, and according to Dulong-Petit law, above the Debye temperature, the specific heat Cp of the material can be obtained by calculation according to formulas 1-2:
Cp＝(3.91×10 -3 xT + 24.35). times.Na/M equation 1
Cp Of composite ＝ΣCp i ×m i % formula 2
Wherein Cp is specific heat of material, Na is number of atoms in molecule, M is relative molecular mass, Cp is specific heat of two or more-phase composite materials i Is the specific heat of i, m i % is mass fraction of phase i. The material thermal conductivity was calculated from κ ═ λ ρ Cp, and the results are shown in fig. 8. The final ZT values of the materials as a function of temperature are shown in fig. 9.
As can be seen from the drawings:
FIG. 1 shows the preparation of Sb by a solvothermal method at different temperatures 2 Te 3 The XRD pattern of the powder shows that the peak position and pure phase Sb of the powder synthesized at the reaction temperature of 220 ℃ are Sb 2 Te 3 (PDF #15-0874) the peak positions are coincident and no impurity peak exists, which indicates that the powder is Sb 2 Te 3 Pure phase. When the reaction temperature is reduced to 190 ℃, xrd of the powder has more second-phase Te peaks, which indicates that the synthesized powder is Sb with hexahedral lamellar structure 2 Te 3 A mixture phase with a small amount of second phase Te belonging to the hexagonal system.
FIG. 2 shows the preparation of Sb by solvothermal method at different temperatures 2 Te 3 SEM photograph of powder, Sb with regular morphology of the synthesized product can be observed from (a) and (b) in FIG. 2 at a reaction temperature of 220 deg.C 2 Te 3 The hexagonal nanosheet is about 600nm in edge size, about 10m in thickness and relatively uniform in appearance; when the temperature is reduced to 190 ℃, as shown in (c) (d) in fig. 2, linear nanocrystals penetrate through the centers of a plurality of nanosheets to form a mixed structure of a shape like a sugarcoated haw, and Sb 2 Te 3 The thickness of the nano-sheet becomes extremely thin and still takes the shape of regular hexagon, and the structure is Sb of series connection of Te nano-wires by combining xrd result analysis 2 Te 3 The novel morphology of (1).
FIG. 3 is Sb 2 Te 3 Liquid phase sintering phenomenon in the blocking of Te powder.
FIG. 4 shows the fracture morphology of the sintered block, wherein (a) in FIG. 4 is Sb 2 Te 3 Fracture morphology, FIG. 4 (b) is Sb 2 Te 3 -Te fracture morphology, observable from the graph, Sb 2 Te 3 The fracture is in the form of micron-sized lath, and Sb 2 Te 3 The fracture of-Te is in the form of nano-scale fine fragments, which is relatively Sb 2 Te 3 In other words, the grain size is significantly smaller, the number of interfaces is increased, and the effect of scattering carriers is significantly enhanced, which is advantageous for reducing the thermal conductivity.
FIG. 5 is a Seebeck coefficient versus temperature curve of a material, and it can be seen that Sb is 2 Te 3 The Seebeck coefficient of the material is about 80 mu VK at room temperature -1 And about 98 μ VK at 498K -1 。Sb 2 Te 3 -Te material vs. Sb 2 Te 3 The Seebeck value is higher overall, and is increased by 55 percent at room temperature, and is about 122 mu VK -1 (ii) a At 498K a maximum of about 170 μ VK -1 And the yield is improved by 76 percent. This is probably due to Sb 2 Te 3 An interface potential barrier formed by the-Te heterojunction generates an energy filtering effect, the transmission of carriers with lower energy is blocked, Seebeck is enhanced, and in addition, Te can inhibit Sb 2 Te 3 The formation of intrinsic defects optimizes the material carrier concentration, which also contributes to the improvement of Seebeck.
FIG. 6 is a graph of the electrical conductivity σ of the material as a function of temperature, and Sb as a whole 2 Te 3 And Sb 2 Te 3 The conductivity of Te materials decreases with increasing temperature, which characterizes degenerate semiconductors. Sb probably due to the reduction of the carrier concentration 2 Te 3 The conductivity of-Te was substantially maintained at 2X10 although somewhat lower than that of the pure phase 4 Sm -1 About, still higher than that of Sb synthesized by solvothermal method 2 Te 3 Levels reported in the relevant literature.
FIG. 7 is a plot of power factor PF versus temperature for a material due to Sb 2 Te 3 The Seebeck coefficient of the-Te material is greatly improved, so that the power factor of the-Te material is improvedThe PF is also obviously improved in a high-temperature region, and the maximum value of 4.9mWK can be reached at 498K - 2 cm -1 Comparatively pure Sb 2 Te 3 The height is 44 percent higher.
FIG. 8 is a plot of thermal conductivity κ of the material versus temperature, Sb 2 Te 3 The lowest thermal conductivity of the-Te material with the thermal conductivity K of 497K is 0.44W m -1 K -1 Therefore, the liquid phase sintering has the advantages that the organization structure is refined, the interface concentration is increased, and the scattering effect on carriers and phonons is enhanced due to the liquid phase sintering effect.
Fig. 9 shows the temperature dependence of the material ZT. Due to Sb 2 Te 3 The enhanced power factor PF and lower thermal conductivity kappa of the-Te material in a high-temperature region enable the-Te material to reach a ZT maximum value of 0.56 at 498K, compared with pure phase Sb prepared by a solvothermal method 2 Te 3 The highest ZT value of the thermoelectric performance is improved by 69%.
Claims (4)
1. Sb synthesis based on liquid phase method 2 Te 3 The thermoelectric property improving method of the-Te nano heterojunction material is characterized in that:
first by reducing Sb 2 Te 3 Solvothermal reaction temperature to synthesize Sb 2 Te 3 Growing Te nano-wire in situ to make the product show Te nano-wire series hexagonal disc type Sb 2 Te 3 The shape of the sugarcoated haws; then the synthesized nano powder is further subjected to hydrogen reduction treatment, and a block material is obtained through discharge plasma liquid phase sintering; the method comprises the following steps:
step 1: sb 2 Te 3 Preparation of-Te nano powder
0.8g NaOH is weighed and dissolved in 80mL ethylene glycol, then 2g polyvinylpyrrolidone is added, stirring is carried out until the polyvinylpyrrolidone is completely dissolved, and then 0.664g Na is added to the solution 2 TeO 3 After the mixture was sufficiently dissolved, 0.456g of SbCl was added 3 Stirring and mixing uniformly, transferring the solution into a 100mL reaction kettle, and reacting for 36h at 190 ℃; after the reaction is finished, the product is centrifugally washed by deionized water and absolute ethyl alcohol respectively, and then is placed in a vacuum drying oven to be dried for 48 hours at the temperature of 60 ℃;
and 2, step: reduction treatment
Reducing the product dried in the step 1 in a hydrogen reduction furnace;
and step 3: sintering
And (3) placing the powder sample reduced in the step (2) in a graphite die, and obtaining a block material through SPS sintering.
2. The method of claim 1, wherein:
in the step 2, the reduction temperature is 300 ℃, and the reduction time is 3 h.
3. The method of claim 1, wherein:
in the step 3, the sintering temperature of the spark plasma sintering is 460 ℃, and the sintering time is 5 minutes.
4. A method according to claim 1 or 3, characterized in that:
in step 3, the temperature rise rate of the discharge plasma sintering is 50 ℃/min, the initial sintering pressure is 1MPa, the pressure is increased to 45MPa at 200 ℃, the pressure is maintained for 5 minutes at 460 ℃, and the pressure is released to 1MPa when the temperature is reduced to 250 ℃.
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