CN110828650B - Organic-inorganic composite thermoelectric film and preparation method thereof - Google Patents
Organic-inorganic composite thermoelectric film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an organic-inorganic composite thermoelectric film and a preparation method thereof, wherein the film takes a double-pass alumina film as a template, and an inorganic thermoelectric nanoparticle array is prepared on a substrate through physical vapor deposition; and then depositing a conductive polymer film on the surface of the substrate to obtain the conductive polymer film. The method is simple, has high controllability, is beneficial to large-scale rapid preparation of the thermoelectric film, and the inorganic thermoelectric nano particles are uniformly dispersed in the polymer matrix, thereby being beneficial to obtaining high thermoelectric performance and having good application prospect.
Description
Technical Field
The invention belongs to the field of thermoelectric thin film materials and preparation thereof, and particularly relates to an organic-inorganic composite thermoelectric thin film and a preparation method thereof.
Background
The thermoelectric material is a functional material which directly converts thermal energy and electric energy into each other by utilizing the seebeck effect and the peltier effect of a semiconductor material. The thermoelectric conversion technology has the characteristics of small system volume, high reliability, no pollutant emission, wide applicable temperature range and the like, and is applied to the fields of recycling of industrial waste heat and automobile exhaust, micro power supply of aerospace detectors, micro-district cooling, biomedicine and the like. The characteristics of green and environmental protection can effectively relieve the increasingly serious problems of environmental pollution and energy crisis in the world at present, so that high-performance thermoelectric materials and high-efficiency thermoelectric power generation technologies are in wide attention internationally in recent years. The thermoelectric properties of a material are generally evaluated by a dimensionless thermoelectric figure of merit zT, which is σ S2T/kappa, sigma is the electrical conductivity, S is the seebeck coefficient, kappa is the thermal conductivity, T is the absolute temperature, sigma S2Is the power factor. The thermoelectric materials currently studied and used are mainly Bi applied near room temperature2Te3Base thermoelectric material CoSb for use in medium temperature region3PbTe-based thermoelectric materials, SiGe-based thermoelectric materials used in high-temperature regions, and the like. Although these inorganic thermoelectric materials have good thermoelectric properties, their raw materials are expensive, the preparation process is complex and costly, it is difficult to prepare special-shaped and flexible devices, and they are toxic and bring about heavy metal pollution, which greatly limits their wide application.
Since the last 70 th century when conductive polymer materials with high electrical conductivity were reported, more and more researchers began to invest in the research of organic thermoelectric materials. The organic thermoelectric material has unique advantages, such as very low thermal conductivity, low raw material price, flexibility and easy large-scale preparation, and provides a new choice for room-temperature thermoelectric materials. However, the thermoelectric performance of organic thermoelectric materials is much lower than that of conventional inorganic thermoelectric materials. Recent research shows that the preparation of the organic-inorganic nano composite thermoelectric material is an effective way for improving the thermoelectric performance of the organic material, inorganic filling particles with high conductivity or high seebeck coefficient are compounded with a conductive polymer, and the conductivity or the seebeck coefficient of the polymer can be improved by utilizing the synergistic effect of the inorganic filling particles and the conductive polymer; in addition, the Seebeck coefficient of the material can be improved by the energy filtering effect at the interface of the two Materials, and the thermal conductivity is reduced by the phonon interface scattering effect generated by the Nano-filler particles, so that the thermoelectric performance of the conductive polymer is effectively improved (ACS Nano,2010,4, 2445-. However, nanoparticles tend to agglomerate, and the dispersion in organic thermoelectric Materials is not controllable, which limits further improvement of thermoelectric performance (ACS Applied Materials & Interfaces,2010,2, 3170-. CN107964648A discloses a P-type Sb2Te3 composite CH3NH3I thermoelectric film and a preparation method thereof, but the method still cannot finely control the distribution of organic and inorganic thermoelectric materials in the composite film. Although the template is manufactured by etching the single-layer closely-packed polystyrene nanospheres, the organic-inorganic composite thermoelectric film (Nature Communications,2018,9,3817) with monodisperse nano-filler particles can be finally manufactured, but the method has complex process and poor controllability, and is not beneficial to large-scale production and preparation.
Disclosure of Invention
The invention provides an organic-inorganic composite thermoelectric film and a preparation method thereof, wherein inorganic thermoelectric nano-particles are monodisperse and uniformly distributed in an organic matrix, and the defects of complex process and poor controllability of the prior preparation technology are overcome; and then depositing a conductive polymer film on the surface of the film to obtain the organic-inorganic composite thermoelectric film.
The invention relates to an organic-inorganic composite thermoelectric film, which comprises inorganic thermoelectric nano-particle materials distributed in a conductive polymer matrix.
The conductive polymer is one or more of polyaniline, polypyrrole, polythiophene and derivatives thereof, and polyethylene tetrathiol-based metal complex; the inorganic thermoelectric nano-particle material is Bi2Te3、Sb2Te3、SnTe、CoSb3And one or more of PbTe. The content of the inorganic thermoelectric nano particles in the composite thermoelectric film is 1-90 wt%.
The invention relates to a preparation method of an organic-inorganic composite thermoelectric film, which comprises the following steps:
(1) attaching a double-pass alumina film on a substrate;
(2) and (2) depositing the inorganic thermoelectric material on the substrate obtained in the step (1) by using an inorganic thermoelectric material as a target material through a physical vapor deposition method, removing the bi-pass alumina film by using an adhesive tape to obtain an inorganic thermoelectric nanoparticle array, then depositing a conductive polymer, and drying to obtain the organic-inorganic composite thermoelectric film.
The preferred mode of the above preparation method is as follows:
the thickness of the double-pass aluminum oxide film in the step (1) is less than 1 μm, and the diameter of the hole is less than 500 nm; the substrate is a silicon wafer, glass, a polyimide PI film or a polyethylene terephthalate PET film.
The physical vapor deposition method in the step (2) is vacuum thermal evaporation, magnetron sputtering or ion plating; the method for depositing the conductive polymer comprises the following steps: drop coating, spin coating, or electrochemical deposition.
The inorganic thermoelectric material in the step (2) is Bi2Te3Base thermoelectric material, Sb2Te3Base thermoelectric material, SnTe base thermoelectric material, CoSb3One or more of a base thermoelectric material and a PbTe base thermoelectric material; the conductive polymer is one or more of polyaniline, polypyrrole, polythiophene and derivatives thereof, and polyethylene tetrathiol based metal complex.
The thickness of the inorganic thermoelectric material deposited in the step (2) is less than 1 μm.
The drying in the step (2) is carried out for 6-24 hours under the vacuum condition of 60 ℃.
The invention provides an organic-inorganic composite thermoelectric film prepared by the method.
The invention provides an application of the organic-inorganic composite thermoelectric film.
Advantageous effects
The method has the advantages of simple process, low cost, short period and high controllability, and is suitable for large-scale industrial production; the method is also suitable for preparing the organic-inorganic composite thermoelectric film on the flexible substrate, and the composite film has good flexibility and can be bent and applied to the field of wearable electronic devices.
Drawings
FIG. 1 shows the PEDOT: PSS-Bi from example 12Te3A digital photographic image of the composite thermoelectric film;
FIG. 2 shows the PEDOT: PSS-Bi from example 12Te3Scanning electron microscope images of the composite thermoelectric thin film;
FIG. 3 shows the PEDOT: PSS-Bi from example 12Te3Electrical conductivity of the composite thermoelectric film;
FIG. 4 shows the PEDOT: PSS-Bi from example 12Te3The seebeck coefficient of the composite thermoelectric film;
FIG. 5 shows the PEDOT: PSS-Bi from example 12Te3Power factor of the composite thermoelectric film.
Detailed Description
Below isThe invention is further illustrated by reference to specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims. Bi used in the examples of the present invention2Te3Powder and Sb2Te3The powder is prepared from Sichuan high-purity material technology, and is polyethylene dioxythiophene-polystyrene sulfonate (PEDOT: PSS) aqueous solution (type Orgacon)TMICP 1050) and Polyaniline (PANI) powders were produced by Sigma-Aldrich, and bi-pass AAO films were produced by shenzhen topology essence film science and technology ltd.
Example 1
(1) Attaching a double-pass alumina film with the hole diameter of about 100nm, the thickness of about 200nm and the hole spacing of about 250nm to a silicon wafer substrate with the size of about 10mm by 10 mm;
(2) with P-type Bi2Te3The powder is used as a target material, and the pressure intensity in the cavity is 10-5mbar, evaporation rate of 0.5nm/s and evaporation time of 2min, and performing vacuum thermal evaporation on the silicon wafer substrate attached with the Bi-pass alumina film in the step (1), wherein Bi is2Te3The thickness is about 60 nm;
(3) slowly sticking a polyimide high-temperature adhesive tape on the surface of the sample obtained in the step (2), slightly pressing the whole surface to enable the adhesive tape to be fully adhered with the alumina film, and then tearing off the adhesive tape to obtain Bi2Te3An array of nanoparticles;
(4) mixing a poly (ethylenedioxythiophene) -polystyrene sulfonate) (PEDOT: PSS) aqueous solution with a DMSO solvent with the volume fraction of 5%, magnetically stirring for 30min, dripping and covering the obtained solution on the surface of the sample obtained in the step (3), spin-coating to prepare a PEDOT: PSS film at the rotating speed of 3000rpm and the spin-coating time of 45s, then putting the PEDOT: PSS film into a vacuum drying oven, and drying at 60 ℃ for 6h to obtain the PEDOT: PSS-Bi2Te3Compounding a thermoelectric film;
prepared PEDOT PSS-Bi2Te3Digital photo of composite thermoelectric filmThe surface of the material is flat and smooth as shown in figure 1;
prepared PEDOT PSS-Bi2Te3SEM image of the composite thermoelectric film, as shown in FIG. 2, monodisperse Bi2Te3The nano particles are uniformly distributed in a PEDOT PSS matrix;
shown in FIGS. 3-5 are PEDOT PSS-Bi2Te3The electric conductivity, the seebeck coefficient and the power factor of the composite thermoelectric film are respectively about 630S/cm, 82 muV/K and 425 muW/mK at room temperature2。
Example 2
(1) Attaching a double-pass alumina film with the hole diameter of about 100nm, the thickness of about 200nm and the hole spacing of about 250nm to a silicon wafer substrate with the size of about 10mm by 10 mm;
(2) with P type Sb2Te3The powder is used as a target material, and the pressure intensity in the cavity is 10-5mbar, evaporation rate of 0.5nm/s and evaporation time of 2min, and carrying out vacuum thermal evaporation on the silicon wafer substrate attached with the bi-pass alumina film in the step (1), wherein Sb is2Te3The thickness is about 60 nm;
(3) slowly sticking a polyimide high-temperature adhesive tape on the surface of the sample obtained in the step (2), slightly pressing the whole surface to enable the adhesive tape to be fully adhered with the alumina film, and then tearing off the adhesive tape to obtain Sb2Te3An array of nanoparticles;
(4) mixing a PEDOT/PSS aqueous solution with a DMSO solvent with the volume fraction of 5%, magnetically stirring for 30min, dripping the obtained solution on the surface of the sample obtained in the step (3), coating the sample with the solution in a rotating manner at the rotating speed of 3000rpm for 45s to prepare a PEDOT/PSS film, then putting the film into a vacuum drying oven, and drying the film at the temperature of 60 ℃ for 6h to obtain the PEDOT/PSS-Sb2Te3And compounding the thermoelectric film.
PEDOT:PSS-Sb2Te3The electric conductivity, the Seebeck coefficient and the power factor of the composite thermoelectric film at room temperature are respectively about 578S/cm, 76 muV/K and 334 muW/mK2。
Example 3
(1) Attaching a double-pass alumina film with the hole diameter of about 100nm, the thickness of about 200nm and the hole spacing of about 250nm to a silicon wafer substrate with the size of about 10mm by 10 mm;
(2) with P-type Bi2Te3The powder is used as a target material, and the pressure intensity in the cavity is 10-5mbar, evaporation rate of 0.5nm/s and evaporation time of 2min, and performing vacuum thermal evaporation on the silicon wafer substrate attached with the Bi-pass alumina film in the step (1), wherein Bi is2Te3The thickness is about 60 nm;
(3) slowly sticking a polyimide high-temperature adhesive tape on the surface of the sample obtained in the step (2), slightly pressing the whole surface to enable the adhesive tape to be fully adhered with the alumina film, and then tearing off the adhesive tape to obtain Bi2Te3An array of nanoparticles;
(4) mixing 0.1g of eigenstate Polyaniline (PANI) powder and camphorsulfonic acid according to the molar ratio of 2:1, placing the mixture in an agate mortar for fully grinding for 30min, then adding the mixture into 10mL of m-cresol solvent, stirring for 6h to fully dissolve the mixture in the solvent, dripping the obtained solution on and covering the surface of the sample obtained in the step (3), preparing a PANI film by spin coating at the rotating speed of 3000rpm and the spin coating time of 45s, then placing the film in a vacuum drying oven, and drying the film for 12h at the temperature of 60 ℃ to obtain PANI-Bi2Te3And compounding the thermoelectric film.
PANI-Bi2Te3The electric conductivity, the Seebeck coefficient and the power factor of the composite thermoelectric film at room temperature are about 235S/cm, 77 mu V/K and 139 mu W/mK respectively2。
Comparative example
The thermoelectric properties of the organic-inorganic composite thermoelectric thin films in examples 1 to 3 were far superior to those of the literature (ACS Applied Materials)&PSS-Bi PEDOT mentioned in Interfaces,2010,2, 3170-3178))2Te3Thermoelectric properties of the composite film (thermoelectric power factor 47 μ W/mK at room temperature2)。
Claims (7)
1. An organic-inorganic composite thermoelectric film, characterized in that the film comprises an array of inorganic thermoelectric nanoparticle materials uniformly distributed in a conductive polymer matrix; the conductive polymer is polyaniline, polypyrrole, polythiophene and derivatives thereof, and polyethylene tetrathiol groupOne or more of metal complexes; the inorganic thermoelectric nano-particle material is Bi2Te3、Sb2Te3、SnTe、CoSb3One or more of PbTe;
wherein the organic-inorganic thermoelectric film is prepared by the following method:
(1) attaching a double-pass alumina film on a substrate;
(2) depositing an inorganic thermoelectric material on the substrate obtained in the step (1) by a physical vapor deposition method, removing the bi-pass alumina film to obtain an inorganic thermoelectric nanoparticle array, then depositing a conductive polymer, and drying to obtain the organic-inorganic composite thermoelectric film.
2. The composite thermoelectric film according to claim 1, wherein the content of the inorganic thermoelectric nanoparticles in the composite thermoelectric film is 1 to 90 wt%.
3. A preparation method of an organic-inorganic composite thermoelectric film comprises the following steps:
(1) attaching a double-pass alumina film on a substrate;
(2) depositing an inorganic thermoelectric material on the substrate obtained in the step (1) by a physical vapor deposition method, removing the bi-pass alumina film to obtain an inorganic thermoelectric nanoparticle array, then depositing a conductive polymer, and drying to obtain an organic-inorganic composite thermoelectric film; wherein the inorganic thermoelectric material is Bi2Te3Base thermoelectric material, Sb2Te3Base thermoelectric material, SnTe base thermoelectric material, CoSb3One or more of a base thermoelectric material and a PbTe base thermoelectric material; the conductive polymer is one or more of polyaniline, polypyrrole, polythiophene and derivatives thereof, and polyethylene tetrathiol based metal complex.
4. The preparation method according to claim 3, wherein the thickness of the two-pass aluminum oxide film in the step (1) is less than 1 μm, and the diameter of the pores is less than 500 nm; the substrate is a silicon wafer, glass, a polyimide PI film or a polyethylene terephthalate PET film.
5. The preparation method according to claim 3, wherein the physical vapor deposition method in the step (2) is vacuum thermal evaporation, magnetron sputtering or ion plating; the method for depositing the conductive polymer comprises the following steps: drop coating, spin coating, or electrochemical deposition.
6. The method of claim 3, wherein the inorganic thermoelectric material deposited in step (2) has a thickness of less than 1 μm.
7. Use of the organic-inorganic composite thermoelectric film according to claim 1.
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| CN102376868A (en) * | 2011-11-24 | 2012-03-14 | 上海第二工业大学 | Preparing method for conductive polymer nanoparticle composite TiO2-base thermoelectric material |
| CN104538540A (en) * | 2015-01-16 | 2015-04-22 | 武汉大学 | Antimony telluride/poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) thermoelectric composite material and manufacturing method thereof |
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| CN102376868A (en) * | 2011-11-24 | 2012-03-14 | 上海第二工业大学 | Preparing method for conductive polymer nanoparticle composite TiO2-base thermoelectric material |
| CN104538540A (en) * | 2015-01-16 | 2015-04-22 | 武汉大学 | Antimony telluride/poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) thermoelectric composite material and manufacturing method thereof |
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