CN112607714B - Preparation method of PbSe-based thermoelectric material - Google Patents
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Abstract
The invention discloses a preparation method of an Ag-doped PbSe-based thermoelectric material, and belongs to the technical field of energy conversion. Firstly, pbSe nano particles are synthesized by adopting hydrothermal method, then the PbSe nano particles are compounded with self-made Ag nano particles according to a certain stoichiometric ratio, then the composite nano particles are annealed under proper pressure and temperature, and then the PbSe-xwt% Ag block thermoelectric material is prepared by combining high-frequency furnace heating and hot-pressing sintering processes. The electrical conductivity of the PbSe-xwt% Ag thermoelectric material prepared by the method is 5630.86~11099.02S/m, the thermal conductivity is 0.50-0.70W/mK, and the thermoelectric optimal value is 0.46-0.97. The preparation method has the advantages of short period, simple and convenient operation and low equipment requirement, the obtained thermoelectric material is a p-type semiconductor, and the prepared PbSe-based thermoelectric material has potential application value in the field of energy conversion.
Description
Technical Field
The invention belongs to the technical field of material preparation and energy conversion, and particularly relates to a p-type PbSe nanocomposite material prepared by a method combining annealing and hot pressing, which has excellent thermoelectric performance.
Background
Thermoelectric materials are materials that can achieve the conversion of thermal energy and electrical energy to each other, and can be used for thermoelectric refrigeration and thermoelectric power generation. At present, the thermoelectric device assembled by utilizing p-type and n-type semiconductor thermoelectric materials has the advantages of high stability, small volume, long service life, environmental protection and the like, and therefore, the thermoelectric device has wide application prospects in the fields of sensors, refrigeration, recycling waste heat, aerospace and the like. However, the performance of thermoelectric materials is typically measured by the thermoelectric figure of merit ZT, zt=s 2 σT/k, where S is the Seebeck coefficient, σ is the electrical conductivity, T is the absolute temperature, and k is the thermal conductivity. The power factor of the material is pf=s 2 Sigma. Thus, excellent thermoelectric materials require a combination of high Seebeck coefficient, high electrical conductivity, and low thermal conductivity. The coordination of the relationship between these parameters is critical to improving the final ZT value and achieving thermoelectric material conversion efficiency.
Lead selenide (PbSe) is considered to be an excellent functional material because of its unique optical and electrical properties. The potential use of PbSe in photoresistors, photocatalysis, infrared detectors, solar cells, etc. has been widely explored over the last 20 years. The intrinsic PbSe material is an n-type semiconductor, and the composite or doped PbSe material can change the carrier type of PbSe and is converted into a p-type semiconductor. Compared with large-scale bulk materials, the nanocomposite has the characteristics of multiple components, small size, high density grain boundaries, phase boundaries, lattice defects and the like, can effectively reduce the heat conductivity coefficient of the material, increases phonon scattering of the material, and has synergistic effects on improving the thermoelectric performance of the material. Considering that PbSe is a narrow bandgap semiconductor material with stable physical and chemical properties, pbSe is taken as a matrix in the application, and the doping technology is utilized to dope Ag nano particles into the PbSe nano particles so as to improve the thermoelectric properties of the sample; firstly synthesizing PbSe and Ag nano particles by adopting a liquid phase method, then adopting precursor powder of an annealing treatment thermoelectric material, then adopting a high-frequency furnace heating and hot-pressing sintering process to prepare a block PbSe-xwt% Ag thermoelectric material with high density, and finally testing the electric and thermal conductivity of the prepared PbSe-based thermoelectric material. The results show that the ZT of the 5 wt% Ag doped PbSe-based thermoelectric material is 0.97 at 723K, 8.8 times that of undoped PbSe, and higher than the ZT value at this temperature for most p-type thermoelectric materials.
The prepared composite material is characterized by adopting the technologies of a Scanning Electron Microscope (SEM), an X-ray powder diffractometer (XRD), a high-resolution transmission electron microscope (HRTEM) and the like. The preparation method is simple and easy to operate, the raw materials are relatively cheaper and less toxic than PbTe-based materials, and meanwhile, the p-type PbSe composite material can be rapidly obtained by the method. There is no report of preparing a p-type PbSe-based thermoelectric material by doping PbSe nanoparticles with blended Ag nanoparticles.
Disclosure of Invention
The invention relates to a preparation method of a p-type PbSe-based thermoelectric material. The material has the advantages of simple preparation method, good repeatability and easy mass synthesis. The nano composite material prepared by the method has higher electric conductivity, higher Seebeck coefficient and reduced heat conductivity, silver nano particles and lead selenide nano crystals are mixed by a solution method, and finally the p-type composite material is prepared by hot pressing, so that the material has good thermoelectric performance and potential application in the field of thermoelectric energy conversion.
The invention is realized by the following technical scheme:
a preparation method of a PbSe thermoelectric material doped with Ag nano particles is characterized in that the PbSe nano particles and the Ag nano particles are used as raw materials. Weighing a proper amount of PbSe and self-made Ag nano particles according to the chemical general formula PbSe-xwt% Ag, wherein X is the mass ratio of the Ag nano particles to the PbSe nano particles, and the mass ratio is in the range of X=1-10, uniformly mixing the PbSe and the self-made Ag nano particles in an agate mortar, and fully grinding to obtain a ground mixed sample; then loading the powder into an alumina crucible, placing the alumina crucible into a tube furnace, vacuumizing, and annealing in a flowing weak reducing atmosphere to obtain Ag-doped lead selenide precursor powder; and then the powder is put into a graphite grinding tool, and the PbSe-xwt% Ag block thermoelectric material with good crystallinity and high purity is prepared by heating in a high-frequency furnace, hot-pressing and sintering.
Further, the synthesis method comprises the following specific steps:
(1) Preparation of PbSe nanoparticles: the PbSe nanoparticles are prepared by a hydrothermal method. 0.1-0.3 g selenium source and 1.1-1.2 g lead source are dissolved in 35-45 ml glycol. After stirring for 10-60 minutes, transferring the mixture into a stainless steel autoclave with a polytetrafluoroethylene lining with a volume of 50ml, keeping the autoclave at 180-200 ℃ for 6-12 h, cooling the autoclave to room temperature, washing the precipitate with deionized water and ethanol for 4-6 times, centrifugally collecting the precipitate, and vacuum-drying the obtained sample at 60 ℃ for 12h to obtain the dry PbSe nano particles.
(2) Blending of PbSe and Ag nanoparticles: in order to fully mix the PbSe nanoparticles and the homemade Ag nanoparticles, 5.2-6.2 and g dry PbSe nanoparticle powder is dispersed in 50-ml-150-ml ethanol, then 0.06-0.60-g homemade Ag nanoparticles are added into the ethanol solution, and the mixture solution is fully stirred. The dispersant was then evaporated under vacuum to give a homogeneously mixed PbSe-Xwt% Ag material.
(3) Preparing pellets by annealing treatment and high-frequency furnace heating and hot-pressing sintering processes: annealing the mixed powder at 450-600 ℃ in a weak reducing atmosphere for 1-5 h, then filling the annealed powder into a graphite grinding tool, sealing the graphite grinding tool with carbon rods up and down, wrapping the graphite grinding tool with carbon paper, heating a sample in a glove box by adopting a high-frequency furnace under the axial pressure of 35-65 MPa, and carrying out hot pressing for 10-30 min in the environment of 450-550 ℃ to obtain the PbSe-based block thermoelectric material with high density and purity.
(4) The PbSe-xwt% Ag composite thermoelectric material obtained by the preparation method has good crystallinity, high density and purity, electric conductivity of 5630.86-11099.02S/m, heat conductivity of 0.50-0.70W/mK and thermoelectric optimal value ZT of 0.20-0.97. The thermal conductivity of the material is measured by a Netzsch LFA-467 laser flash method thermal conductivity meter (Germany, resistant Co.); the material conductivity and seebeck coefficient measured the relevant parameters on a germany LSR-3 seebeck coefficient/resistance tester, the thermoelectric optimum ZT using the formula zt=s 2 Sigma T/k, calculated.
The reactant selenium source is selenium powder
The reactant lead source is lead acetate trihydrate
The reaction solvent is distilled water prepared by a laboratory and ethylene glycol purchased by Chinese medicine
The reaction vessel is a purchased high-pressure reaction kettle.
FIG. 1 is an X-ray diffraction pattern (XRD) of the resulting hot pressed sample
FIG. 2 is a Scanning Electron Microscope (SEM) of the resulting hot pressed sample
FIG. 3 is a high resolution transmission electron microscope image (HRTEM) of the resulting hot pressed sample
FIG. 4 is a graph showing thermal conductance data of the resulting hot pressed samples at different temperatures
FIG. 5 is a graph showing the conductivity and Seebeck coefficient data of the resulting hot pressed samples at different temperatures
FIG. 6 shows thermoelectric optima (ZT) of the resulting hot pressed samples at different temperatures
The specific embodiment is as follows:
the invention is illustrated by the following examples:
example 1:
preparation of X=3% Ag doped PbSe-based thermoelectric material, the specific preparation process is as follows
0.020 g selenium powder and 1.138 g lead acetate trihydrate were dissolved in 42 ml ethylene glycol, after stirring for 30 minutes, the mixture was transferred to a 50ml polytetrafluoroethylene-lined stainless steel autoclave which was kept at 180 ℃ for 12h, then the obtained sample powder was washed with deionized water and ethanol for 6 times, collected by centrifugation, and the sample was dried in vacuo at 60 ℃ for 12 hours; weighing 6.0 g of PbSe and 0.18 g of Ag according to the mass ratio of PbSe to Ag, uniformly mixing the PbSe and the Ag in an agate mortar, fully grinding to obtain a ground mixed sample, then loading the mixed sample into an alumina crucible, placing the alumina crucible into a tube furnace, vacuumizing, and heating to 450 DEG o C, annealing 2h in a flowing weak reducing atmosphere to obtain Ag-doped PbSe precursor powder, namely PbSe-3 wt% Ag thermoelectric material raw material; and (3) loading the PbSe-3 wt% Ag powder into a graphite grinding tool with the inner diameter of 12.7 mm, sealing the graphite grinding tool with a carbon rod up and down, wrapping the graphite grinding tool with carbon paper, hot-pressing the graphite grinding tool for 20 min in an environment with the axial pressure of 55 MPa and the temperature of 500 ℃, then starting to cool down, releasing pressure and closing a hot-pressing instrument, and naturally cooling a sample to obtain the PbSe-3 wt% Ag thermoelectric material.
Example 2: preparation of an x=5 wt% Ag doped PbSe thermoelectric material, the specific preparation process is as follows
Weighing 6.0 g of PbSe and 0.30 g of Ag according to the mass ratio of PbSe to Ag, uniformly mixing the PbSe and the Ag in an agate mortar, and fully grinding to obtain a ground mixed sample. The other steps are the same as in example 1.
Example 3: preparation of x= wt% Ag doped PbSe thermoelectric material, the specific preparation process is as follows
Weighing 6.0 g of PbSe and 0.42 g of Ag according to the mass ratio of PbSe to Ag, uniformly mixing the PbSe and the Ag in an agate mortar, and fully grinding to obtain a ground mixed sample. The other steps are the same as in example 1.
Example 4: pbSe-based composite material thermoelectric performance test
For example 1, example 2, example 3 samples were subjected to phase testing, thermal conductivity and electrical conductivity testing using the Shenyang Ke-Ting STX-20The thermoelectric performance of the 2A diamond wire cutting machine is characterized after the machine is cut into pieces. The test was performed by subjecting a sample of the block PbSe-X wt% Ag (x=3, 5, 7) after hot pressing. As can be seen from the X-ray diffraction pattern (FIG. 1), the phase mainly existing in the sample is the characteristic diffraction peak of PbSe (PDF#06-0354), and Ag is also present in the sample 2 Characteristic peaks of Se (PDF#24-1041), it can be seen that the Ag nanoparticles are heat treated to generate secondary phase Ag 2 Se. Fig. 2 is an SEM image of a PbSe-5 wt% Ag bulk thermoelectric material, and it can be seen that there is a small-sized secondary phase present, as indicated by the circles in the figure. FIG. 3 is a HRTEM image of PbSe-5 wt% Ag bulk thermoelectric material, with significant Ag in the PbSe matrix observed 2 Grain boundaries of the Se secondary phase. Fig. 4 is a graph of thermal conductivity of samples with different doping ratios, and it can be seen that after the samples are compounded with Ag nanoparticles, the thermal conductivity coefficient of the samples gradually decreases with the increase of temperature, and at the temperature of 723 and K, the thermal conductivity of the samples of PbSe-5 and wt% Ag is 0.70W/mK. Fig. 5a and 5b are graphs of the conductivity and seebeck coefficient of samples with different doping ratios with temperature, and as shown in the graph, after the samples are doped with Ag nanoparticles, the conductivity of the samples with three doping ratios is increased and then decreased with the increase of temperature, the seebeck coefficient generally shows an increasing trend, and at the temperature of 723K, the conductivity of the sample PbSe-5 wt% Ag is 11099.02S/m, and the seebeck coefficient is 290.70 μv/K. Fig. 6 is a graph showing the variation of the thermoelectric optimal value ZT of each group of samples with temperature, and it can be found that the performance of the PbSe-5 wt% Ag bulk thermoelectric material is optimal, and the ZT value is 0.97.
Claims (2)
1. A preparation method of a PbSe-based thermoelectric material is characterized by comprising the following steps:
(1) Firstly synthesizing PbSe nano particles by a liquid phase method, then blending the PbSe nano particles with self-made Ag nano particles, carrying out annealing treatment, preparing pellets by a hot-press sintering process, and obtaining the PbSe-based thermoelectric material, wherein the chemical formula of the thermoelectric material is PbSe-xwt% Ag, and X=1-10;
(2) The specific synthesis steps are as follows: pbSe nano particles are prepared by a hydrothermal method, 0.1-0.3 g of selenium source and 1.1-1.2 g of lead source are dissolved in 35-45 ml of ethylene glycol, after stirring for 10-60 minutes, the mixture is transferred into a stainless steel autoclave with a polytetrafluoroethylene lining with the volume of 50ml, the autoclave is kept at 180-200 ℃ for 6-12 hours, then the autoclave is cooled to room temperature, precipitation is washed for 4-6 times by deionized water and ethanol, centrifugal collection is carried out, the obtained sample is dried in vacuum for 12 hours at 60 ℃ to obtain dry PbSe nano particles; dispersing 5.2-6.2 g of dry PbSe nano particle powder in 50-150 ml of ethanol, then adding 0.06-0.6 g of self-made Ag nano particles into the ethanol solution, fully stirring the mixture solution, and then evaporating the dispersing agent in vacuum atmosphere to obtain a uniformly mixed PbSe-Xwt% Ag material;
(3) Preparing pellets by annealing treatment and high-frequency furnace heating and hot-pressing sintering processes: annealing the mixed PbSe-Xwt% Ag material for 1-5 hours in a weak reducing atmosphere at 450-600 ℃, then filling the annealed powder into a graphite grinding tool, sealing the powder up and down by using a carbon rod, wrapping the powder by using carbon paper, heating a sample in a glove box by adopting a high-frequency furnace under the axial pressure of 35-65 MPa, and carrying out hot pressing for 10-30 minutes in the environment of 450-550 ℃ to obtain the PbSe-based block thermoelectric material with high density and high purity; the PbSe-Xwt% Ag composite thermoelectric material obtained by the preparation method has good crystallinity, high density and purity, electric conductivity of 5630-11099S/m, heat conductivity of 0.5-0.7W/mK and thermoelectric optimal value ZT of 0.2-0.97.
2. The method for preparing a PbSe-based thermoelectric material according to claim 1, wherein: the selenium source is selenium powder; the lead source is lead acetate trihydrate.
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| US2995613A (en) * | 1959-07-13 | 1961-08-08 | Bell Telephone Labor Inc | Semiconductive materials exhibiting thermoelectric properties |
| CN103180982A (en) * | 2010-10-19 | 2013-06-26 | 加利福尼亚理工学院 | Self-tuning of carrier concentration for high thermoelectric performance |
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| US7586033B2 (en) * | 2005-05-03 | 2009-09-08 | Massachusetts Institute Of Technology | Metal-doped semiconductor nanoparticles and methods of synthesis thereof |
| JP5173433B2 (en) * | 2005-12-07 | 2013-04-03 | トヨタ自動車株式会社 | Thermoelectric conversion material and manufacturing method thereof |
| US8067259B2 (en) * | 2009-05-12 | 2011-11-29 | Evident Technologies | Method of producing high performance photovoltaic and thermoelectric nanostructured bulk and thin films |
| CN101549405A (en) * | 2009-05-19 | 2009-10-07 | 燕山大学 | High-pressure sintering preparation method of high-densification high-performance nano crystal block thermoelectric material |
| US20130180561A1 (en) * | 2010-01-29 | 2013-07-18 | California Institute Of Technology | Nanocomposites with high thermoelectric performance and methods |
| CN103219515B (en) * | 2013-03-28 | 2014-12-17 | 浙江大学 | PbSe cubic particle/graphene composite material as well as preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US2995613A (en) * | 1959-07-13 | 1961-08-08 | Bell Telephone Labor Inc | Semiconductive materials exhibiting thermoelectric properties |
| CN103180982A (en) * | 2010-10-19 | 2013-06-26 | 加利福尼亚理工学院 | Self-tuning of carrier concentration for high thermoelectric performance |
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| Exploring the doping effects of Ag in p-type PbSe compounds with enhanced thermoelectric performance;ShanyuWang等;《JOURNAL OF PHYSICS D: APPLIED PHYSICS》(第44期);1-10 * |
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