CN111446355B - Organic/inorganic composite thermoelectric fiber and preparation and application thereof - Google Patents
Organic/inorganic composite thermoelectric fiber and preparation and application thereof Download PDFInfo
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04B—KNITTING
- D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
- D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04B—KNITTING
- D04B21/00—Warp knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
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- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/10—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects operating with only the Peltier or Seebeck effects
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- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
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- H10N10/856—Thermoelectric active materials comprising organic compositions
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Abstract
The invention relates to an organic/inorganic composite thermoelectric fiber, and preparation and application thereof, wherein the organic component of the thermoelectric fiber is poly (3, 4-ethylenedioxythiophene) -poly (styrene sulfonate) PEDOT: PSS, the inorganic component is tellurium nanowires Te NWs, and the Te NWs are oriented and distributed in the PEDOT: PSS fiber and prepared by wet spinning. The composite fiber prepared by the invention has good thermoelectric performance and wide application prospect in the field of flexible thermoelectric wearability. The preparation method is simple in preparation process and has the potential of continuous production.
Description
Technical Field
The invention belongs to the field of flexible thermoelectric materials and preparation and application thereof, and particularly relates to an organic/inorganic composite thermoelectric fiber and preparation and application thereof.
Background
With the miniaturization of chips, the improvement of adaptability of circuits and hardware and the popularization of mobile networks, a large number of wearable electronic devices and sensors are emerged in the market in recent years, but most of wearable devices are still powered by batteries, and the batteries need to be charged and replaced frequently, while some wearable electronic devices need to be operated autonomously and uninterruptedly, for example, wearable medical sensors used for monitoring physical sign states of patients, and the popularization and application of the wearable medical sensors are limited due to the manual replacement of the batteries and the charging.
Since flexible thermoelectric materials are receiving more and more attention because they can directly convert thermal energy into electric energy and realize continuous self-power supply of wearable electronic devices through the temperature gradient between human skin and the surrounding environment, how to prepare high-performance flexible thermoelectric materials and effectively combine the materials with fabrics is a crucial issue.
Conductive polymer materials are an important branch of flexible thermoelectric materials, and are receiving attention due to their light weight and flexibility. Moreover, the novel commercialized conducting polymer products have low cost, good environmental stability and no toxicity, and are a better choice for constructing flexible thermoelectric materials. The PEDOT and PSS are flexible thermoelectric materials with excellent performance, have good film forming property, can effectively improve the conductivity of the materials after post-treatment, but have limited application in the thermoelectric field due to low Seebeck coefficient. Therefore, researchers use inorganic thermoelectric materials with high Seebeck coefficient to improve the thermoelectric property of PEDOT: PSS, and researchers (Energy,2017,125:519-525) improve the Seebeck coefficient of a PEDOT: PSS composite film by compounding tellurium nanorods with the PEDOT: PSS from 10 to 50 muV.K-1。
At present, the thermoelectric performance of a composite film based on PEDOT: PSS is effectively improved by an organic-inorganic composite method, but the film thermoelectric material has certain problems in wearable application: firstly, the thin-film device usually occupies a large area, which seriously affects the aesthetic feeling of the fabric; second, film devices are generally dense, which affects the breathability and comfort of the fabric. In order to solve the problem, the PEDOT/PSS/Te NWs organic/inorganic composite thermoelectric fiber is constructed by a wet spinning technology, compared with a thermoelectric film, the fiber can be directly sewn into a fabric, the appearance and the air permeability of the fabric are not influenced, and the bonding property of a thermoelectric material and the fabric is improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing an organic/inorganic composite thermoelectric fiber, and preparation and application thereof, and overcoming the problem of poor bonding property between a thin film thermoelectric material and a fabric in the prior art. The invention is prepared by PEDOT, PSS, Te NWs and polyethylene glycol (PEG) through wet spinning.
The invention provides an organic/inorganic composite thermoelectric fiber, which comprises a composite fiber of organic component poly (3, 4-ethylenedioxythiophene) -poly (styrene sulfonate) PEDOT, PSS and inorganic component tellurium nanowire Te NWs.
The mass ratio of PEDOT to PSS to Te NWs is 1: 0.1-1: 1.
The Te NWs is oriented and distributed in the composite fiber.
The thermoelectric fiber is obtained by carrying out wet spinning on PEDOT (PSS), Te NWs and polyethylene glycol (PEG)
The invention relates to a preparation method of an organic/inorganic composite thermoelectric fiber, which comprises the following steps:
(1) adding tellurium nanowires Te NWs, PEDOT, PSS conductive particles and polyethylene glycol into deionized water, mixing, stirring and ultrasonically treating to obtain a homogeneous spinning solution, and then carrying out wet spinning to obtain fibers;
(2) and (3) sealing the fibers obtained in the step (2) in a hydrothermal kettle filled with glycol, placing the hydrothermal kettle in an oven for heating treatment, and cooling to obtain the organic/inorganic composite thermoelectric fibers.
The tellurium nanowires Te NWs in the step (1) are specifically as follows: adding tellurium oxide, polyvinylpyrrolidone and potassium hydroxide into an ethylene glycol solvent, carrying out hydrothermal reaction, cooling and washing to obtain Te NWs.
The mass ratio of the tellurium oxide to the polyvinylpyrrolidone to the potassium hydroxide is 1:1: 0.59-1: 3: 1.77; the hydrothermal reaction time is 12-24 h, and the hydrothermal temperature is 140-180 ℃.
The molecular weight of the polyvinylpyrrolidone is 40000.
The concentration of PEDOT to PSS in the spinning solution in the step (1) is 18-25 mg/mL-1(ii) a The mass ratio of PEDOT to PSS to Te NWs to polyethylene glycol is 1:0.1: 0.1-1: 1:5
Further, the preferable value of the mass ratio of PEDOT to PSS to Te NWs to polyethylene glycol is 1:1: 5;
the molecular weight of the polyethylene glycol is 400.
The stirring time in the step (1) is 0.5-2 h, and the ultrasonic time is 0.5-2 h.
Wet spinning in the step (1)The method specifically comprises the following steps: the spinning solution is filled into an injector, the spinning solution is extruded into a coagulating bath at a constant speed by using an injection pump, the spinning solution is kept stand in the coagulating bath for 10-30 min, the specification of a needle head used by the injector is 12-18G, and the extrusion speed of the injection pump is 1-15 mL.h-1The coagulation bath was isopropanol.
And (3) sealing the fibers in the step (2) in a hydrothermal kettle filled with glycol, wherein the mass ratio of the fibers to the glycol is 1: 10-1: 20.
The heating treatment temperature in the step (2) is 150-170 ℃, and the treatment time is 0.5-3 h.
The invention provides an organic/inorganic composite thermoelectric fiber prepared by the method.
The invention provides an application of the organic/inorganic composite thermoelectric fiber, such as the field of thermoelectric wearability.
Advantageous effects
(1) The preparation method is simple and feasible, and has the potential of continuous production;
(2) the organic/inorganic composite thermoelectric fiber has good thermoelectric performance;
(3) the organic/inorganic composite thermoelectric fiber can be directly woven into fabrics, and has good application prospect in the field of thermoelectric wearability.
Drawings
FIG. 1 is a schematic diagram of a self-contained test system;
FIG. 2 is a schematic diagram of a wet spinning process (a) and a digital photograph (b) of the fiber prepared in example 2;
FIG. 3 is a digital photograph of fibers prepared in example 2 woven directly into a fabric;
fig. 4 is an SEM photograph of the composite fiber prepared in example 3, in which (a) is an SEM photograph of a cross section and (b) is an SEM photograph of a surface.
Detailed Description
The invention will be further illustrated with reference to the following 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.
Examples tellurium oxide, sodium hydroxide, polyvinylpyrrolidone (Mw 40000) were produced by alatin technologies ltd; isopropyl alcohol, ethylene glycol, and polyethylene glycol (Mw ═ 400) manufactured by the national pharmaceutical group chemicals limited;
PSS conductive particles are manufactured by Sigma Aldrich, Inc. (Orgacon DRY, DRY re-discrete pellets).
The test methods involved in the examples: based on the previous work in the laboratory (Advanced Functional Materials,2019,29:1900304), the seebeck coefficient of thermoelectric fibers was tested with a self-built test system. The temperature across the sample was controlled using a Peltier cooler and heater, the open circuit voltage across the fiber was measured using a KEITHLEY 2700(a Tektronix) data acquisition system, the real time temperature across the fiber was measured using a thermocouple, and the seebeck coefficient was obtained after calculation. Cutting 10cm thermoelectric fiber, coating silver paste as electrode on two ends of the fiber, and using universal meter (VC 890C)+) And measuring the resistance at two ends of the fiber, calculating the sectional area of the thermoelectric fiber by using a scanning electron microscope and image J, calculating the resistivity of the fiber according to the length, the resistance and the sectional area of the fiber, and converting the resistivity into the conductivity.
Example 1
0.0335g of tellurium oxide, 0.0355g of potassium hydroxide and 0.02g of polyvinylpyrrolidone are dissolved in 30mL of ethylene glycol solvent, the mixture is cooled and washed after reacting for 24 hours at 160 ℃ to obtain Te NWs, 266mg of PEDOT, PSS conductive particles and 26mg of polyethylene glycol are weighed respectively for standby, the prepared Te NWs, PEDOT, PSS and polyethylene glycol are added into 14.7mL of deionized water and stirred for 1 hour, and ultrasonic treatment is carried out for 1 hour to obtain homogeneous spinning solution. The homogeneous PEDOT: PSS/Te NWs spinning solution was filled into a syringe and 3 mL. h using a syringe pump-1Extruding the mixture into an isopropanol coagulating bath at a speed of 14G, standing for 20min to obtain the PEDOT/PSS/Te NWs composite fiber, sealing the obtained fiber in a hydrothermal kettle filled with 10 times of glycol by mass of the fiber, heating at 160 ℃ for 1h, and cooling to obtain the PEDOT/PSS/Te NWs composite fiber.
The electrical conductivity of the PEDOT PSS fiber prepared in this example was 296S cm-1Seebeck coefficient of 16 μ V.K-1The power factor is 7.5 μ W.m-1·K-2。
Example 2
0.1675g of tellurium oxide, 0.1675g of potassium hydroxide and 0.1g of polyvinylpyrrolidone are dissolved in 60mL of ethylene glycol solvent, the mixture is cooled and cleaned after reacting for 12h at 140 ℃ to obtain Te NWs, 170mg of PEDOT, PSS conductive particles and 390mg of polyethylene glycol are respectively weighed and reserved for standby application, the prepared Te NWs, PEDOT, PSS and polyethylene glycol are added into 8mL of deionized water and stirred for 1h, and ultrasonic treatment is carried out for 1h to obtain homogeneous spinning solution. The homogeneous PEDOT: PSS/Te NWs spinning solution was filled into a syringe and 3 mL. h using a syringe pump-1Extruding the mixture into isopropanol coagulating bath from a needle head of 14G, standing for 20min to obtain the PEDOT/PSS/Te NWs composite fiber, sealing the obtained fiber in a hydrothermal kettle filled with 15 times of glycol by mass of the fiber, heating for 1h at 160 ℃, and cooling to obtain the PEDOT/PSS/Te NWs composite fiber.
As shown in FIG. 2, wherein (a) is a schematic diagram of a wet spinning process, and (b) is a digital photograph of the PEDOT: PSS/Te NWs composite fiber prepared in this example.
FIG. 3 shows a digital photograph of the composite PEDOT/PSS/Te NWs fiber woven into the fabric prepared in this example.
The conductivity of the PEDOT/PSS/Te NWs fiber prepared in this example was 273S-cm-1Seebeck coefficient of 32 μ V.K-1The power factor is 28 μ W.m-1·K-2。
Example 3
0.1675g of tellurium oxide, 0.5025g of potassium hydroxide and 0.29g of polyvinylpyrrolidone are dissolved in 60mL of ethylene glycol solvent, the mixture is cooled and washed after reacting for 24h at 180 ℃ to obtain Te NWs, 130mg of PEDOT, PSS conductive particles and 650mg of polyethylene glycol are respectively weighed and reserved for later use, the prepared Te NWs, PEDOT, PSS and polyethylene glycol are added into 5.2mL of deionized water and stirred for 2h, and ultrasonic treatment is carried out for 2h to obtain homogeneous spinning solution. Homogeneous PEDOT: PSS/Te NWs dope was loaded into a syringe using a syringe pump at 15 mL. h-1Is extruded from a 18G needle toAnd (3) standing in an isopropanol coagulating bath for 30min to obtain the PEDOT (PSS)/Te NWs composite fiber, sealing the obtained fiber in a hydrothermal kettle filled with 20 times of glycol by mass of the fiber, heating at 170 ℃ for 3h, and cooling to obtain the PEDOT/Te NWs composite fiber.
The SEM characterization of the composite fiber obtained in this example is shown in fig. 4, in which (a) SEM photograph of the cross section of the composite fiber and (b) SEM photograph of the surface of the composite fiber, it can be clearly seen from the (b) that the Te NWs orientation is distributed in the composite fiber.
The conductivity of the PEDOT/PSS/Te NWs fiber prepared in this example was 249S cm-1Seebeck coefficient of 56 μ V.K-1The power factor is 78 μ W.m-1·K-2。
Comparative example 1
Compared with the PEDOT: PSS thermoelectric fiber prepared in the literature (ACS Applied Polymer Materials,2019,1:1257--1·K-2It can be seen that the thermoelectric performance of the thermoelectric fiber prepared in example 3 of the present invention is much better than that of the thermoelectric fiber prepared in the literature.
Comparative example 2
Compared with the PEDOT: PSS/Te organic-inorganic composite thermoelectric film prepared in the literature (Energy,2017,125:519-525), the power factor of the thermoelectric film prepared in the literature is 51.2 muW.m-1·K-2It can be seen that the thermoelectric properties of the thermoelectric fiber prepared in example 3 of the present invention are superior to those of the thermoelectric thin film prepared in the literature.
Claims (9)
1. An organic/inorganic composite thermoelectric fiber, characterized in that the fiber comprises a composite fiber of poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonate) PEDOT, PSS and tellurium nanowires Te NWs;
wherein the organic/inorganic composite thermoelectric fiber is prepared by the following method:
(1) adding tellurium nanowires Te NWs, PEDOT, PSS conductive particles and polyethylene glycol into deionized water, mixing, stirring and ultrasonically treating to obtain a spinning solution, and then carrying out wet spinning to obtain fibers;
(2) sealing the fibers obtained in the step (1) in a hydrothermal kettle filled with glycol, heating, and cooling to obtain organic/inorganic composite thermoelectric fibers; wherein the heating treatment temperature is 170 ℃, and the treatment time is 0.5-3 h.
2. The thermoelectric fiber according to claim 1, wherein the mass ratio of PEDOT to PSS to Te NWs is 1:0.1 to 1: 1.
3. The thermoelectric fiber of claim 1, wherein the Te NWs is oriented in the composite fiber.
4. The thermoelectric fiber according to claim 1, wherein the thermoelectric fiber is obtained by wet spinning of PEDOT PSS, Te NWs, polyethylene glycol PEG.
5. A preparation method of an organic/inorganic composite thermoelectric fiber comprises the following steps:
(1) adding tellurium nanowires Te NWs, PEDOT, PSS conductive particles and polyethylene glycol into deionized water, mixing, stirring and ultrasonically treating to obtain a spinning solution, and then carrying out wet spinning to obtain fibers;
(2) sealing the fibers obtained in the step (1) in a hydrothermal kettle filled with glycol, heating, and cooling to obtain organic/inorganic composite thermoelectric fibers; wherein the heating treatment temperature is 170 ℃, and the treatment time is 0.5-3 h.
6. The preparation method according to claim 5, wherein the tellurium nanowires Te NWs in the step (1) are specifically as follows: adding tellurium oxide, polyvinylpyrrolidone and potassium hydroxide into an ethylene glycol solvent, carrying out hydrothermal reaction, cooling and washing to obtain Te NWs.
7. The method according to claim 5, wherein the concentration of PEDOT/PSS in the dope of step (1) is 18 to 25 mg/mL-1；PPSS, Te NWs and polyethylene glycol in a mass ratio of 1:0.1: 0.1-1: 1: 5.
8. The preparation method according to claim 5, wherein the wet spinning in the step (1) is specifically: the spinning solution is filled into an injector, the spinning solution is extruded into a coagulating bath at a constant speed by using an injection pump, the spinning solution is kept stand in the coagulating bath for 10-30 min, the specification of a needle head used by the injector is 12-18G, and the extrusion speed of the injection pump is 1-15 mL.h-1The coagulation bath was isopropanol.
9. Use of the organic/inorganic composite thermoelectric fiber according to claim 1 in the field of thermoelectric wearability.
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