CN106784288B - Preparation method for enhancing performance of composite thermoelectric material - Google Patents
Preparation method for enhancing performance of composite thermoelectric material Download PDFInfo
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Abstract
The invention provides a preparation method of a carbon nano tube/graphene/poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid composite thermoelectric material. Dissolving sodium polystyrene sulfonate in water, adding a proper amount of carbon nano tube and graphene, dispersing uniformly, dropwise adding a proper amount of 3, 4-ethylenedioxythiophene monomer, mixing uniformly, and adding ammonium persulfate and ferric sulfate to initiate polymerization reaction. And after the reaction is finished, centrifuging the product, repeatedly washing the obtained black product by using deionized water, centrifuging, and drying in vacuum. The invention provides a novel preparation method of a carbon nano tube/graphene/poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid composite thermoelectric material, which has the advantages of simple process conditions, low production cost and environmental protection. The preparation method of the invention simultaneously improves the thermoelectric performance of the composite thermoelectric material.
Description
Technical Field
The invention relates to a preparation method of a carbon nano tube/graphene/poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid composite thermoelectric material, in particular to a method for forming the composite thermoelectric material by doping a carbon nano tube and graphene with thiophene through in-situ oxidation polymerization.
Background
With the acceleration of industrialization, it is more and more urgent to solve the problems of environmental pollution and energy shortage. Waste heat is inevitably generated in daily life and production, and if a material capable of utilizing the waste heat can be developed and used, the energy crisis can be greatly alleviated. The thermoelectric material is an environment-friendly functional material capable of recycling waste heat.
The thermoelectric material mainly utilizes the motion of current carriers (holes or electrons) to realize the direct conversion between heat energy and electric energy, has the advantages of small volume, light weight, no transmission part, no noise in work, no environmental pollution, long service life, easy control and the like, is successfully applied to the fields of aerospace, micro sensing, waste heat power generation and the like, and is an energy substitute material with wide prospect and strong competitiveness. The nondimensional thermoelectric figure of merit ZT is an important index for measuring the thermoelectric performance of the material, and the expression is as follows:
wherein S represents the Seebeck coefficient;
is the sum of phonon thermal conductivity and electron thermal conductivity; t represents the absolute temperature. The larger the ZT value is, the better the thermoelectric conversion efficiency is, and therefore, in order to improve the thermoelectric performance, the thermoelectric performance should be improved as much as possible
The alloy based on Bi-Te-Sb can be greatly reduced
The value is not much changed and thus it is still the most widely used thermoelectric material at present. However, inorganic materials have limited resources, high price, difficult processing, serious environmental pollution and toxicity, and cannot become long-term green energy materials.
The conductive polymer has the advantages of rich resources, low price, easy processing, low thermal conductivity and the like, wherein the intrinsic conductive polymer poly (3, 4-ethylenedioxythiophene) becomes one of the most potential organic thermoelectric materials at present due to the advantages of high electrical conductivity, good light transmittance, low cost, good environmental stability, low thermal conductivity, easy control and the like. However, as an organic thermoelectric material, the low electrical conductivity makes the ZT value of the material lower than that of an inorganic thermoelectric material. Scholdt et al (Journal of Electronic Materials 2010; 39(9): 1589-. The carbon nano tube and the graphene have the advantages of high conductivity, good optical property, good mechanical property and the like, and are conductive additives with good prospects in conductive polymers in recent years.
The thermoelectric performance of the composite thermoelectric material prepared by the method of blending the conductive polymer and the carbon nano tube or the graphene is improved to a certain extent, but the composite thermoelectric material has a considerable distance from large-scale commercial application. Therefore, on the premise of ensuring the advantages of simple and convenient preparation method, low cost, environmental friendliness, easy processing and the like, the research on a synthesis method capable of further enhancing the thermoelectric property of the material has very important significance.
Disclosure of Invention
The invention aims to provide a preparation method of a high-performance thermoelectric composite material (poly (3, 4-ethylenedioxythiophene): sodium polystyrene sulfonate/carbon nano tube/graphene), which is simple to operate, green, environment-friendly, low in cost and good in performance. The method is mainly characterized in that a carbon nano tube and graphene are simultaneously doped into poly (3, 4-ethylenedioxythiophene) through in-situ oxidation polymerization reaction, and the thermoelectric property of the composite material is further improved by utilizing the synergistic enhancement effect of the carbon nano tube and the graphene.
The invention adopts 3,4 ethylene dioxythiophene monomer, carbon nano tube and graphene as raw materials, sodium polystyrene sulfonate as surfactant, ammonium persulfate and ferric sulfate as oxidant, and prepares poly (3, 4-ethylene dioxythiophene): sodium polystyrene sulfonate/carbon nano tube/graphene composite thermoelectric material by in-situ oxidative polymerization of thiophene at low temperature.
The preparation method comprises the following steps:
(1) preparing materials:
preparing materials: the mass ratio of the (carbon nano tube + graphene) to the 3, 4-ethylenedioxythiophene is 250: 1-25: 1; the carbon nano tube and the graphene can be added with only a single component, and if the carbon nano tube and the graphene are added at the same time, the mass ratio of the carbon nano tube to the graphene can be any ratio of 99: 1-1: 99;
the mass ratio of the 3, 4-ethylenedioxythiophene to the sodium polystyrene sulfonate is 2: 1-1: 1, the mass ratio of the oxidant to the sodium polystyrene sulfonate is 3: 1-2: 1, the oxidant is ferric sulfate and ammonium persulfate, and the mass ratio of the ammonium persulfate to the ferric sulfate is 50: 1-30: 1;
the preparation method comprises the following steps of dissolving a surfactant sodium polystyrene sulfonate in deionized water, adding a carbon nano tube and graphene, performing ultrasonic dispersion to obtain a uniform dispersion liquid, adding a 3, 4-ethylenedioxythiophene monomer, and mechanically stirring until the dispersion liquid is uniformly dispersed;
(2) polymerization: adding the prepared ferric sulfate and ammonium persulfate solution into the dispersion liquid obtained in the step (1), and adding N into the dispersion liquid at the temperature of 5 DEG C2Reacting for 48 hours in an atmosphere;
(3) centrifuging and washing: after the polymerization is finished, centrifuging the product, repeatedly washing and centrifuging the obtained black precipitate, and drying for 12 hours in vacuum at the temperature of 80-100 ℃.
The carbon nano tube is a multi-wall carbon nano tube (MWCNT) or a single-wall carbon nano tube, the length is 0.5-2 mu m, and the outer diameter is 10-20 nm; the graphene is prepared by a solvent stripping method, and the number of layers is 1-4.
Before adding the prepared ferric sulfate and ammonium persulfate solution in the step (2), N is introduced into the dispersion liquid obtained in the step (1)2For 1h to remove O from the dispersion2And the thiophene is prevented from being oxidized.
In the step (2), the mass ratio of ammonium persulfate to ferric sulfate is 50: 1-30: 1.
The invention further discloses application of the carbon nano tube/graphene/poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid composite thermoelectric material prepared by the method in improving power factor and conductivity. The experimental results show that: after the carbon nano tube and the graphene are added, compared with the single nano carbon material, the power factor of poly (3, 4-ethylenedioxythiophene) and polystyrene sulfonic acid is improved by 72 percent, and the thermoelectric conversion efficiency of the thermoelectric material is improved.
Compared with the prior art, the preparation method for enhancing the performance of the composite thermoelectric material has the positive effects that:
(1) the preparation method is simple, the reaction conditions are mild, water is used as a solvent in the reaction process, the preparation method is green and environment-friendly, the raw material cost is low, and the preparation method has a wide application prospect.
(2) The method of the invention fully utilizes the inherent low thermal conductivity of the conductive polymer polythiophene and the high electrical conductivity of the carbon nano tube and the graphene, and further improves the thermoelectric property of the composite material by utilizing the synergistic enhancement effect of the carbon nano tube and the graphene.
Drawings
FIG. 1 is a transmission electron microscope photograph of the composite material synthesized in example 1;
FIG. 2 is a transmission electron microscope photograph of the composite material synthesized in example 2;
FIG. 3 is a transmission electron microscope photograph of the composite material synthesized in example 3;
FIG. 4 is a graph showing the electrical conductivity of the composite material synthesized in examples 1,2 and 3;
FIG. 5 shows Seebeck coefficients of the composite materials synthesized in examples 1,2 and 3;
fig. 6 shows the power factor of the composite material synthesized in examples 1,2 and 3.
Detailed Description
The invention is described below by means of specific embodiments. Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention. The raw materials and reagents used in the present invention are commercially available. Among them, multi-walled carbon nanotubes (MWCNT), sodium polystyrene sulfonate (PSSNa), 3, 4-Ethylenedioxythiophene (EDOT), etc. are commercially available.
Example 1
(1) Preparing materials: firstly, 1g of sodium polystyrene sulfonate (PSSNa) is added into 145mL of deionized water, after stirring and dissolving, 0.005g of multi-walled carbon nanotube (MWCNT) and 0.005g of graphene (graphene) are added, after uniform ultrasonic dispersion, 1.25g of 3, 4-Ethylenedioxythiophene (EDOT) monomer is added dropwise, mechanical stirring is carried out until uniform mixing is achieved, and N is introduced21h。
(2) Polymerization: 0.05g of ferric sulfate and 2g of ammonium persulfate are added into 12.5g of deionized water, and after uniform stirring, the mixture is added into the dispersion liquid obtained in the step (1). The reaction process isN2The atmosphere, mechanical stirring speed is 600rpm, reaction temperature is 5 ℃, and reaction time is 48 h.
(3) Centrifuging and washing: after the polymerization is completed, the product is centrifuged, and the obtained black precipitate is repeatedly washed and centrifuged.
(4) And (3) drying: the finally obtained black precipitate was dried in vacuo at 100 ℃ for 12 h.
The sample obtained in this example had an electrical conductivity of 2.936S/cm, a Seebeck coefficient of 18.9. mu.V/K, and a power factor of 0.105. mu.W.mK-1. FIG. 1 is a transmission electron microscope photograph of the composite material obtained in example 1.
Example 2
(1) Preparing materials: firstly, 1g of sodium polystyrene sulfonate (PSSNa) is added into 145mL of deionized water, after stirring and dissolving, 0.01g of multi-walled carbon nanotube (MWCNT) is added, after uniform ultrasonic dispersion, 1.25g of 3, 4-Ethylenedioxythiophene (EDOT) monomer is dripped, mechanical stirring is carried out until uniform mixing is achieved, and N is introduced21h。
(2) Polymerization: 0.05g of ferric sulfate and 2g of ammonium persulfate are added into 12.5g of deionized water, and after uniform stirring, the mixture is added into the dispersion liquid obtained in the step (1). The reaction process is N2The atmosphere, mechanical stirring speed is 600rpm, reaction temperature is 5 ℃, and reaction time is 48 h.
(3) Centrifuging and washing: after the polymerization is completed, the product is centrifuged, and the obtained black precipitate is repeatedly washed and centrifuged.
(4) And (3) drying: the finally obtained black precipitate was dried in vacuo at 100 ℃ for 12 h.
The sample obtained in the example has the conductivity of 2.547S/cm, the Seebeck coefficient of 16.4 mu V/K and the power factor of 0.069 mu W-mK-1. FIG. 2 is a TEM image of the composite material obtained in example 2.
Example 3
(1) Preparing materials: firstly, 1g of sodium polystyrene sulfonate (PSSNa) is added into 145mL of deionized water, 0.01g of graphene is added after stirring and dissolving, 1.25g of 3, 4-Ethylenedioxythiophene (EDOT) monomer is dropwise added after uniform ultrasonic dispersion, mechanical stirring is carried out until uniform mixing is achieved, and N is introduced21h。
(2) Polymerization: 0.05g of ferric sulfate and 2g of ammonium persulfate are added into 12.5g of deionized water, and after uniform stirring, the mixture is added into the dispersion liquid obtained in the step (1). The reaction process is N2The atmosphere, mechanical stirring speed is 600rpm, reaction temperature is 5 ℃, and reaction time is 48 h.
(3) Centrifuging and washing: after the polymerization is completed, the product is centrifuged, and the obtained black precipitate is repeatedly washed and centrifuged.
(4) And (3) drying: the finally obtained black precipitate was dried in vacuo at 100 ℃ for 12 h.
The sample obtained in this example had an electrical conductivity of 2.679S/cm, a Seebeck coefficient of 18.3. mu.V/K, and a power factor of 0.090. mu.W.mK-1. FIG. 3 is a TEM image of the composite material obtained in example 3.
Example 4
(1) Preparing materials: firstly, 1g of sodium polystyrene sulfonate (PSSNa) is added into 145mL of deionized water, after stirring and dissolving, 0.05g of multi-walled carbon nanotube (MWCNT) is added, after uniform ultrasonic dispersion, 1.25g of 3, 4-Ethylenedioxythiophene (EDOT) monomer is dripped, mechanical stirring is carried out until uniform mixing is achieved, and N is introduced21h。
(2) Polymerization: 0.05g of ferric sulfate and 2g of ammonium persulfate are added into 12.5g of deionized water, and after uniform stirring, the mixture is added into the dispersion liquid obtained in the step (1). The reaction process is N2The atmosphere, mechanical stirring speed is 600rpm, reaction temperature is 5 ℃, and reaction time is 48 h.
(3) Centrifuging and washing: after the polymerization is completed, the product is centrifuged, and the obtained black precipitate is repeatedly washed and centrifuged.
(4) And (3) drying: the finally obtained black precipitate was dried in vacuo at 100 ℃ for 12 h.
The sample obtained in the example has the conductivity of 2.605S/cm, the Seebeck coefficient of 16.9 mu V/K and the power factor of 0.074 mu W.mK-1。
Example 5
(1) Preparing materials: firstly, 1g of sodium polystyrene sulfonate (PSSNa) is added into 145mL of deionized water, 0.05g of graphene is added after stirring and dissolving, 1.25g of 3, 4-ethylenedioxythia is dripped after uniform ultrasonic dispersionThiophene (EDOT) monomer, mechanically stirring until the mixture is uniform, and introducing N2 1h。
(2) Polymerization: 0.05g of ferric sulfate and 2g of ammonium persulfate are added into 12.5g of deionized water, and after uniform stirring, the mixture is added into the dispersion liquid obtained in the step (1). The reaction process is N2The atmosphere, mechanical stirring speed is 600rpm, reaction temperature is 5 ℃, and reaction time is 48 h.
(3) Centrifuging and washing: after the polymerization is completed, the product is centrifuged, and the obtained black precipitate is repeatedly washed and centrifuged.
(4) And (3) drying: the finally obtained black precipitate was dried in vacuo at 100 ℃ for 12 h.
The sample obtained in the example has the conductivity of 2.714S/cm, the Seebeck coefficient of 18.5 mu V/K and the power factor of 0.093 mu W-mK-1。
Example 6
Comparative test
And (4) conclusion:
(1) after 1% of carbon nano tube is added, the power factor of poly (3, 4-ethylenedioxythiophene) and polystyrene sulfonic acid is improved by 13%.
(2) After 1% of graphene is added, the power factor of poly (3, 4-ethylenedioxythiophene): polystyrene sulfonic acid is improved by 48%.
(3) After the carbon nano tube and the graphene are added, the power factor of the poly (3, 4-ethylenedioxythiophene) and the polystyrene sulfonic acid is improved by 72 percent, which is more obvious than that of adding a single carbon material.
Claims (5)
1. A preparation method for enhancing the performance of a composite thermoelectric material is characterized by comprising the following steps:
(1) preparing materials: the mass ratio of the 3, 4-ethylenedioxythiophene to the carbon nano tube and the graphene is 250: 1-25: 1; the mass ratio of the carbon nano tube to the graphene is 1: 1;
the mass ratio of the 3, 4-ethylenedioxythiophene to the sodium polystyrene sulfonate is 2: 1-1: 1, the mass ratio of the oxidant to the sodium polystyrene sulfonate is 3: 1-2: 1, the oxidant is ferric sulfate and ammonium persulfate, and the mass ratio of the ammonium persulfate to the ferric sulfate is 50: 1-30: 1;
dissolving a surfactant sodium polystyrene sulfonate in deionized water, adding a carbon nano tube and graphene, performing ultrasonic dispersion for 1h, adding a 3, 4-ethylenedioxythiophene monomer, and performing mechanical stirring to obtain a uniform dispersion liquid;
(2) polymerization: adding the prepared oxidant into the dispersion liquid obtained in the step (1), and adding N at 5 DEG C2Reacting for 48 hours in an atmosphere;
(3) centrifuging and washing: after the polymerization is finished, centrifuging the product, repeatedly washing and centrifuging the obtained black precipitate, and vacuum-drying at 80-100 ℃ for 12 h; the carbon nano tube/graphene/poly (3, 4-ethylenedioxythiophene) prepared by the preparation method comprises the following steps: the power factor of the sodium polystyrene sulfonate composite thermoelectric material is improved by 72 percent.
2. The method of claim 1, wherein the carbon nanotubes are multi-walled carbon nanotubes having a length of 0.5 to 2 and an outer diameter of 10 to 20 nm.
3. The preparation process according to claim 1, wherein N is introduced into the dispersion obtained in step (1) before the prepared solution of ferric sulfate and ammonium persulfate is added in step (2)2The time is 1 h.
4. The method of claim 1, wherein the oxidizing agent is selected from the group consisting of iron sulfate and sodium persulfate.
5. Preparing carbon nanotubes/graphene/poly (3, 4-ethylenedioxythiophene) using the method of claim 1: the application of the sodium polystyrene sulfonate composite thermoelectric material in improving the power factor.
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