CN113809225A - SnS/C-PEDOT (Poly ethylene diamine thiosulfonic acid) PSS (Poly styrene) flexible thermoelectric film and preparation method thereof - Google Patents
SnS/C-PEDOT (Poly ethylene diamine thiosulfonic acid) PSS (Poly styrene) flexible thermoelectric film and preparation method thereof Download PDFInfo
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Abstract
The invention provides an SnS/C-PEDOT PSS flexible thermoelectric film and a preparation method thereof, wherein the method comprises the step 1 of using SnCl2·2H2Preparing SnCl by using O as a tin source and PVP as a binder through an electrostatic spinning process2/PVP nano-fiber, then SnCl2The PVP nano-fiber is sequentially subjected to pre-oxidation and vulcanization; step 2, carbonizing the obtained SnS/PVP nano-fiber at the temperature of 500-; step 3, ultrasonically dispersing the SnS/C nano-fiber powder in an organic solvent, and then adding a PEDOT (Polytetrafluoroethylene-PSS) aqueous solution to obtain a SnS/C nano-fiber dispersion liquid with the mass fraction of 5-10%; and 4, carrying out vacuum filtration on the SnS/C nanofiber dispersion liquid to obtain the SnS/C-PEDOT (PSS) flexible thermoelectric film.
Description
Technical Field
The invention relates to the technical field of nano energy thermoelectric materials, in particular to a SnS/C-PEDOT/PSS flexible thermoelectric film and a preparation method thereof.
Background
Thermoelectric materials have important value in the field of energy materials as materials capable of directly converting heat into electricity. In recent years, with the great development of wearable devices, flexible thermoelectric materials have become an emerging direction of future thermoelectric materials. Among different flexible thermoelectric material systems, the conductive polymer has the characteristics of strong compatibility, light weight, no toxicity, low cost, good flexibility and the like, so that the conductive polymer becomes a flexible thermoelectric material with the greatest development prospect.
Among the numerous conductive polymers, PEDOT is currently the most interesting conductive polymer due to its high conductivity, good stability, low cost and ease of mass production. However, the insolubility of PEDOT in water and common solvents limits the application thereof, a uniformly dispersed aqueous solution is formed by emulsifying PEDOT and polystyrene sulfonate (PSS), so that it can be used for the preparation of various flexible thermoelectric materials, and the thermoelectric properties of PEDOT: PSS can be better controlled by adjusting the reaction conditions. Poly 3, 4-ethylenedioxythiophene polystyrene sulfonate (PEDOT: PSS) has extremely high electrical conductivity σ and low thermal conductivity κ, but further improvement of thermoelectric performance is limited due to the extremely low Seebeck coefficient S.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the SnS/C-PEDOT/PSS flexible thermoelectric film and the preparation method thereof, wherein an organic-inorganic interface is constructed to improve the S of the original PEDOT/PSS film, so that the thermoelectric property of the PEDOT/PSS film is further improved, and the SnS/C-PEDOT/PSS flexible thermoelectric film can be used in the field of thermoelectric materials.
The invention is realized by the following technical scheme:
a preparation method of a SnS/C-PEDOT/PSS flexible thermoelectric film comprises the following steps:
step 1, SnCl2·2H2O is a tin source and PVP is viscosityA binder, SnCl prepared by an electrostatic spinning process2/PVP nano-fiber, then SnCl2Carrying out preoxidation and vulcanization on the/PVP nano fiber in sequence to obtain SnS/PVP nano fiber;
and 4, carrying out vacuum filtration on the SnS/C nanofiber dispersion liquid to obtain the SnS/C-PEDOT (PSS) flexible thermoelectric film.
Preferably, SnCl described in step 12The PVP nano fiber is obtained by the following steps:
according to (0.9-1.8) g: (0.2-0.5) g: 5mL of SnCl2·2H2Dissolving O and polyvinylpyrrolidone in N, N-dimethylformamide, and performing electrostatic spinning on the obtained mixed solution at a voltage of 16-18kv and a speed of 0.5-1.5mL/min to obtain SnCl2PVP nano fiber.
Preferably, step 1 is to firstly use the SnCl2Vacuum drying/PVP nano-fiber to remove residual N, N-dimethylformamide, drying, and then carrying out vacuum drying on the obtained SnCl2the/PVP nano-fiber is pre-oxidized and vulcanized.
Further, step 1 is to dry SnCl2the/PVP nano-fiber is calcined for 2-4h at the temperature of 230-280 ℃ to obtain the pre-oxidized SnCl2PVP nano fiber.
Preferably, step 1 is performed by pre-oxidizing SnCl2And vulcanizing the/PVP nano fiber at 230-280 ℃ for 2-4h under the action of thiourea to obtain the SnS/PVP nano fiber.
Further, the thiourea is mixed with the SnCl after preoxidation2The mass ratio of the/PVP nano fiber is (5-10): 1.
preferably, the SnS/PVP nano-fiber is carbonized for 4-8h at the temperature in the step 2 to obtain the SnS/C nano-fiber, and then the SnS/C nano-fiber is ground into particles.
Preferably, step (a)The organic solvent in the step 3 is dimethylformamide, ethylene glycol or dimethyl sulfoxide, and the added PEDOT, PSS aqueous solution and SnCl in the step 1 are added2·2H2The proportion of O is (150-400) mu L: (0.9-1.8) g to obtain the SnS/C nanofiber dispersion liquid.
Preferably, the step 4 is to perform vacuum filtration on the SnS/C nanofiber dispersion liquid on an organic nylon membrane with the pore diameter of 0.22 mu m.
The SnS/C-PEDOT/PSS flexible thermoelectric film is prepared by the method for preparing the SnS/C-PEDOT/PSS flexible thermoelectric film.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a preparation method of a SnS/C-PEDOT/PSS flexible thermoelectric film, which uses SnCl2·2H2The SnCl is prepared by using O as a tin source and PVP as a binder and sequentially adopting electrostatic spinning and calcining processes2The flexible film is characterized by comprising/PVP nano-fibers, SnS/PVP nano-fibers and SnS/C nano-fibers, wherein the SnS/C nano-fibers with different weight ratios are mixed with PEDOT/PSS aqueous solution, the SnS/C-PEDOT/PSS flexible films with different weight ratios of the SnS/C nano-fibers are prepared by controlling the weight ratios of the SnS/C nano-fibers to the PEDOT/PSS and a vacuum filtration method, the Seebeck coefficient S is improved on the premise of ensuring high conductivity sigma, and the thermoelectric property of the material is further improved. The SnS/C nano-fiber is used as an inorganic nano-filler with excellent thermoelectric property, and the addition of the SnS/C nano-fiber constructs and optimizes an organic-inorganic interface, so that the Seebeck coefficient of the film is improved, and the thermoelectric property of the material is improved. The invention provides important material support for researching the potential thermoelectric property of the SnS/C-PEDOT PSS flexible film and the application in the related field.
Drawings
FIG. 1 is an XRD pattern of SnS/C nanofibers of example 1.
FIG. 2 is an SEM photograph of SnS/C nanofibers of example 1.
FIG. 3 shows the thermoelectric properties of the SnS/C-PEDOT: PSS flexible thermoelectric film of example 1.
Detailed Description
The invention will be described in detail with reference to the drawings, which are provided for the purpose of illustration and not for the purpose of limitation.
The invention relates to a preparation method of an SnS/C-PEDOT/PSS flexible thermoelectric film, which comprises the following steps:
the method comprises the following steps: 0.9-1.8g SnCl2·2H2Dispersing O as a tin source in 5mL of DMF (dimethyl formamide) solvent, and dissolving the O on a magnetic stirrer until the O is a colorless solution;
step two: adding 0.2-0.5g of PVP into the solution obtained in the first step, and stirring on a magnetic stirrer until the PVP is completely dissolved;
step three: putting the solution obtained in the step two into an injector, and preparing SnCl by using electrostatic spinning equipment2The electrostatic spinning voltage is 16-18kv, and the speed is 0.5-1.5 mL/min;
step four: SnCl2The PVP nano-fiber is dried in a vacuum drying box to remove residual solvent, and is pre-oxidized in a muffle furnace after being dried to enable the linear polymer chain to be converted into a heat-resistant trapezoidal annular structure so as to stabilize the fiber appearance, wherein the pre-oxidation temperature is 230-280 ℃, and the time is 2-4 hours;
step five: will contain SnCl after pre-oxidation2Putting the ceramic boat of the/PVP nano-fiber into the gas upstream of the tube furnace, putting the ceramic boat containing thiourea into the gas downstream of the tube furnace, and reacting the pre-oxidized SnCl2sulfurizing/PVP nano fiber at 230-280 deg.c for 2-4 hr, thiourea and pre-oxidized SnCl2The mass ratio of the/PVP fiber membrane is (5-10):1, and Ar/H gas is introduced2The volume ratio is 95:5, and SnS/PVP nano-fiber is generated;
step six: putting the ceramic boat filled with the SnS/PVP nano-fiber into a tube furnace, carbonizing at the temperature of 500-800 ℃ for 4-8H, introducing Ar/H gas2The volume ratio is 95:5, SnS/C nano-fibers are generated and then are ground into powder with uniform particles;
step seven: ultrasonically dispersing SnS/C nanofiber powder in an organic solvent, wherein the organic solvent can be Dimethylformamide (DMF), Ethylene Glycol (EG) or dimethyl sulfoxide (DMOS), and adding the organic solvent into 150-400 mu L of PEDOT: PSS aqueous solution according to different weight ratios for ultrasonic dispersion again to obtain SnS/C nanofiber dispersion liquid with the concentration of 5-10 wt%;
step eight: and (4) filtering the dispersion liquid obtained in the seventh step on an organic nylon membrane with the aperture of 0.22 mu m by a vacuum filtration method to obtain the SnS/C-PEDOT/PSS flexible composite thermoelectric film.
Example 1
The invention relates to a preparation method of an SnS/C-PEDOT/PSS flexible thermoelectric film, which comprises the following steps:
the method comprises the following steps: 0.9g of SnCl2·2H2Dispersing O as a tin source in 5mL of DMF, and dissolving the O on a magnetic stirrer until the O is a colorless solution;
step two: adding 0.2g of PVP into the solution obtained in the first step, and stirring on a magnetic stirrer until the PVP is completely dissolved;
step three: putting the solution obtained in the step two into an injector, and preparing SnCl by using electrostatic spinning equipment2PVP nano-fiber, wherein the voltage is 18kv and the speed is 1 mL/min;
step four: SnCl2Drying the PVP nano-fiber in a vacuum drying oven to remove residual solvent, and pre-oxidizing in a muffle furnace at 280 ℃ for 2h to stabilize the shape of the fiber;
step five: will contain SnCl after pre-oxidation2Putting the ceramic boat of the/PVP nano-fiber into the gas upstream of the tube furnace, putting the ceramic boat containing thiourea into the gas downstream of the tube furnace, and putting thiourea and the SnCl after pre-oxidation2The mass ratio of the/PVP nano fiber is 5:1, and the SnCl is treated at the temperature of 280 DEG C2vulcanizing/PVP nano-fiber for 2H, and introducing Ar/H gas2The ratio is 95:5, and SnS/PVP nano-fiber is generated;
step six: putting the ceramic boat filled with the SnS/PVP nano-fiber into a tube furnace, carbonizing for 8 hours at 650 ℃, introducing Ar/H gas2The SnS/C nano-fibers are generated according to the ratio of 95:5 and then are ground into powder with uniform particles;
step seven: ultrasonically dispersing 1mg of SnS/C nanofiber powder in 10mL of DMF to obtain a dispersion liquid with the concentration of SnS/C nanofibers of 10 wt%, adding 20 mu L of the dispersion liquid of 10 wt% of SnS/C nanofibers into 180 mu L of a PEDOT/PSS aqueous solution, diluting the solution to 10mL with DMF, and ultrasonically dispersing again to obtain the dispersion liquid of 10 wt% of SnS/C nanofibers.
Step eight: and (4) filtering the dispersion liquid obtained in the seventh step on an organic nylon membrane with the aperture of 0.22 mu m by a vacuum filtration method to obtain the SnS/C-PEDOT/PSS flexible thermoelectric film.
XRD analysis and SEM characterization are carried out on the SnS/C-PEDOT and PSS flexible film, the successful compounding of the SnS/C nano-fiber and the PEDOT and PSS is proved, and the thermoelectric property of the flexible film is proved to change along with the temperature through the test of the thermoelectric property. FIG. 1 is an XRD (X-ray diffraction) spectrum of SnS/C nano-fibers in example 1 of the invention, and the comparison of the XRD spectrum and a standard card shows that the prepared SnS/C nano-fibers are SnS pure phases; FIG. 2 is an SEM image of SnS/C nanofibers in example 1 of the present invention, wherein the SnS/C nanofibers are uniformly distributed. FIG. 3 shows the thermoelectric property of the SnS/C-PEDOT: PSS flexible film in example 1 of the present invention from room temperature to 120 ℃, and it can be clearly seen that the conductivity is slightly reduced with the increase of the temperature, but the Seebeck coefficient is increased, and the power factor PF is also increased with the increase of the temperature.
Example 2
The invention relates to a preparation method of an SnS/C-PEDOT/PSS flexible thermoelectric film, which comprises the following steps:
the method comprises the following steps: 1.35g SnCl2·2H2Dispersing O as a tin source in 5mL of DMF, and dissolving the O on a magnetic stirrer until the O is a colorless solution;
step two: adding 0.4g of PVP into the solution obtained in the first step, and stirring on a magnetic stirrer until the PVP is completely dissolved;
step three: putting the solution obtained in the step two into an injector, and preparing SnCl by using electrostatic spinning equipment2PVP nano-fiber, wherein the voltage is 16kv and the speed is 0.8 mL/min;
step four: SnCl2Drying the PVP nano-fiber in a vacuum drying oven to remove residual solvent, and pre-oxidizing in a muffle furnace at 250 ℃ for 3 hours after drying to stabilize the shape of the fiber;
step five: will contain SnCl after pre-oxidation2Ceramic of/PVP nano fiberPlacing the boat in the gas upstream of the tube furnace, placing the ceramic boat containing thiourea in the gas downstream of the tube furnace, thiourea and pre-oxidized SnCl2The mass ratio of the/PVP nano fiber is 8:1, and the SnCl is treated at 230 DEG C2sulfurizing/PVP nano-fiber for 4H, and introducing Ar/H gas2The ratio is 95:5, and SnS/PVP nano-fiber is generated;
step six: putting the ceramic boat containing SnS/PVP nano-fiber into a tube furnace, carbonizing at 750 deg.C for 6H, introducing Ar/H gas2The SnS/C nano-fibers are generated according to the ratio of 95:5 and then are ground into powder with uniform particles;
step seven: ultrasonically dispersing 1mg of SnS/C nanofiber powder in 10mL of DMF to obtain a dispersion liquid with the concentration of SnS/C nanofibers of 10 wt%, adding 10 mu L of the dispersion liquid of 10 wt% of SnS/C nanofibers into 190 mu L of PEDOT: PSS aqueous solution, diluting the solution to 10mL with DMF, and ultrasonically dispersing again to obtain the dispersion liquid of SnS/C nanofibers with the concentration of 5 wt%.
Step eight: and (4) filtering the dispersion liquid obtained in the seventh step on an organic nylon membrane with the aperture of 0.22 mu m by a vacuum filtration method to obtain the SnS/C-PEDOT/PSS flexible thermoelectric film.
Example 3
The invention relates to a preparation method of an SnS/C-PEDOT/PSS flexible thermoelectric film, which comprises the following steps:
the method comprises the following steps: 1.8g SnCl2·2H2Dispersing O as a tin source in 5mL of DMF, and dissolving the O on a magnetic stirrer until the O is a colorless solution;
step two: adding 0.4g of PVP into the solution obtained in the first step, and stirring on a magnetic stirrer until the PVP is completely dissolved;
step three: putting the solution obtained in the step two into an injector, and preparing SnCl by using electrostatic spinning equipment2PVP nano-fiber, wherein the voltage is 18kv and the speed is 1.2 mL/min;
step four: SnCl2Drying the PVP nano-fiber in a vacuum drying oven to remove residual solvent, and pre-oxidizing in a muffle furnace at 230 ℃ for 4 hours after drying to stabilize the shape of the fiber;
step five: will contain SnCl after pre-oxidation2Putting the ceramic boat of the/PVP nano-fiber into the gas upstream of the tube furnace, putting the ceramic boat containing thiourea into the gas downstream of the tube furnace, and putting thiourea and the SnCl after pre-oxidation2The mass ratio of the/PVP nano fiber is 10:1, and the SnCl is treated at the temperature of 250 DEG C2vulcanizing/PVP nano-fiber for 3H, and introducing Ar/H gas2The ratio is 95:5, and SnS/PVP nano-fiber is generated;
step six: putting the ceramic boat containing SnS/PVP nano-fiber into a tube furnace, carbonizing at 800 deg.C for 4H, introducing Ar/H gas2The SnS/C nano-fibers are generated according to the ratio of 95:5 and then are ground into powder with uniform particles;
step seven: ultrasonically dispersing 1mg of SnS/C nanofiber powder in 10mL of DMF to obtain a dispersion liquid with the concentration of SnS/C nanofibers of 10 wt%, adding 40 mu L of the dispersion liquid of 10 wt% of SnS/C nanofibers into 360 mu L of PEDOT: PSS aqueous solution, diluting the solution to 10mL with DMF, and ultrasonically dispersing again to obtain the dispersion liquid of 10 wt% of SnS/C nanofibers.
Step eight: and (4) filtering the dispersion liquid obtained in the seventh step on an organic nylon membrane with the aperture of 0.22 mu m by a vacuum filtration method to obtain the SnS/C-PEDOT/PSS flexible thermoelectric film.
Example 4
The invention relates to a preparation method of an SnS/C-PEDOT/PSS flexible thermoelectric film, which comprises the following steps:
the method comprises the following steps: 1.35g SnCl2·2H2Dispersing O as a tin source in 5mL of DMF, and dissolving the O on a magnetic stirrer until the O is a colorless solution;
step two: adding 0.3g of PVP into the solution obtained in the first step, and stirring on a magnetic stirrer until the PVP is completely dissolved;
step three: putting the solution obtained in the step two into an injector, and preparing SnCl by using electrostatic spinning equipment2PVP nano-fiber, wherein the voltage is 16kv and the speed is 1.5 mL/min;
step four: SnCl2Drying the PVP nano-fiber in a vacuum drying oven to remove residual solvent, and pre-oxidizing in a muffle furnace at 280 ℃ for 2h to stabilize the shape of the fiber;
step five: will contain SnCl after pre-oxidation2Putting the ceramic boat of the/PVP nano-fiber into the gas upstream of the tube furnace, putting the ceramic boat containing thiourea into the gas downstream of the tube furnace, and putting thiourea and the SnCl after pre-oxidation2The mass ratio of the/PVP nano fiber is 8:1, and the SnCl is treated at the temperature of 280 DEG C2vulcanizing/PVP nano-fiber for 2H, and introducing Ar/H gas2The ratio is 95:5, and SnS/PVP nano-fiber is generated;
step six: putting the ceramic boat containing SnS/PVP nano-fiber into a tube furnace, carbonizing at 500 deg.C for 8H, introducing Ar/H gas2The SnS/C nano-fibers are generated according to the ratio of 95:5 and then are ground into powder with uniform particles;
step seven: ultrasonically dispersing 1mg of SnS/C nanofiber powder in 10mL of DMF to obtain a dispersion liquid with the concentration of SnS/C nanofibers of 10 wt%, adding 20 mu L of the dispersion liquid of 10 wt% of SnS/C nanofibers into 380 mu L of PEDOT: PSS aqueous solution, diluting the solution to 10mL with DMF, and ultrasonically dispersing again to obtain a dispersion liquid of SnS/C nanofibers with the concentration of 5 wt%.
Step eight: and (4) filtering the dispersion liquid obtained in the seventh step on an organic nylon membrane with the aperture of 0.22 mu m by a vacuum filtration method to obtain the SnS/C-PEDOT/PSS flexible membrane.
Claims (10)
1. A preparation method of SnS/C-PEDOT/PSS flexible thermoelectric film is characterized by comprising the following steps:
step 1, SnCl2·2H2Preparing SnCl by using O as a tin source and PVP as a binder through an electrostatic spinning process2/PVP nano-fiber, then SnCl2Carrying out preoxidation and vulcanization on the/PVP nano fiber in sequence to obtain SnS/PVP nano fiber;
step 2, carbonizing the SnS/PVP nano-fiber at the temperature of 500-800 ℃, and then grinding the SnS/PVP nano-fiber into particles to obtain SnS/C nano-fiber powder;
step 3, ultrasonically dispersing the SnS/C nano-fiber powder in an organic solvent, and then adding a PEDOT (Polytetrafluoroethylene-PSS) aqueous solution to obtain a SnS/C nano-fiber dispersion liquid with the mass fraction of 5-10%;
and 4, carrying out vacuum filtration on the SnS/C nanofiber dispersion liquid to obtain the SnS/C-PEDOT (PSS) flexible thermoelectric film.
2. The method for preparing the SnS/C-PEDOT PSS flexible thermoelectric film according to claim 1, wherein the SnCl in the step 12The PVP nano fiber is obtained by the following steps:
according to (0.9-1.8) g: (0.2-0.5) g: 5mL of SnCl2·2H2Dissolving O and polyvinylpyrrolidone in N, N-dimethylformamide, and performing electrostatic spinning on the obtained mixed solution at a voltage of 16-18kv and a speed of 0.5-1.5mL/min to obtain SnCl2PVP nano fiber.
3. The method for preparing the SnS/C-PEDOT PSS flexible thermoelectric film according to claim 1, wherein the SnCl is firstly prepared in step 12Vacuum drying/PVP nano-fiber to remove residual N, N-dimethylformamide, drying, and then carrying out vacuum drying on the obtained SnCl2the/PVP nano-fiber is pre-oxidized and vulcanized.
4. The method for preparing the SnS/C-PEDOT PSS flexible thermoelectric film according to the claim 3, wherein the step 1 is to dry SnCl2the/PVP nano-fiber is calcined for 2-4h at the temperature of 230-280 ℃ to obtain the pre-oxidized SnCl2PVP nano fiber.
5. The method for preparing the SnS/C-PEDOT PSS flexible thermoelectric film according to the claim 1, wherein the step 1 is to pre-oxidize SnCl2And vulcanizing the/PVP nano fiber at 230-280 ℃ for 2-4h under the action of thiourea to obtain the SnS/PVP nano fiber.
6. The method for preparing the SnS/C-PEDOT PSS flexible thermoelectric film according to claim 5, wherein the thiourea and the pre-oxidized SnCl are used2The mass ratio of the/PVP nano fiber is (5-10): 1.
7. the method for preparing the SnS/C-PEDOT: PSS flexible thermoelectric film according to claim 1, wherein the SnS/PVP nano-fiber is carbonized for 4-8h at the temperature in the step 2 to obtain the SnS/C nano-fiber, and then the SnS/C nano-fiber is ground into particles.
8. The method for preparing the SnS/C-PEDOT PSS flexible thermoelectric film according to claim 1, wherein the organic solvent in step 3 is dimethylformamide, ethylene glycol or dimethyl sulfoxide, the added aqueous solution of PEDOT PSS and the SnCl in step 1 are added2·2H2The proportion of O is (150-400) mu L: (0.9-1.8) g to obtain the SnS/C nanofiber dispersion liquid.
9. The method for preparing the SnS/C-PEDOT: PSS flexible thermoelectric film according to claim 1, wherein the step 4 comprises vacuum filtering the SnS/C nano-fiber dispersion on an organic nylon membrane with the pore diameter of 0.22 μm.
10. The SnS/C-PEDOT: PSS flexible thermoelectric film prepared by the method for preparing the SnS/C-PEDOT: PSS flexible thermoelectric film according to any one of claims 1 to 9.
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