CN103579487A - Low-dimensional nano-silver/polyaniline-based thermoelectric material and preparation method thereof - Google Patents

Low-dimensional nano-silver/polyaniline-based thermoelectric material and preparation method thereof Download PDF

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CN103579487A
CN103579487A CN201310566890.8A CN201310566890A CN103579487A CN 103579487 A CN103579487 A CN 103579487A CN 201310566890 A CN201310566890 A CN 201310566890A CN 103579487 A CN103579487 A CN 103579487A
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polyaniline
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silver
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CN103579487B (en
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王连军
王为杰
朱娟娟
江莞
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Donghua University
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Abstract

The invention relates to a low-dimensional nano-silver/polyaniline-based thermoelectric material and a preparation method of the low-dimensional nano-silver/polyaniline-based thermoelectric material. The low-dimensional nano-silver/polyaniline-based thermoelectric material is of a sheet structure in the mode that low-dimensional nano-silver is scattered in polyaniline, and the mass percent of the low-dimensional nano-silver is 2.1%-8.5%. The preparation method of the low-dimensional nano-silver/polyaniline-based thermoelectric material comprises the steps that silver nitrate is added to DBSA to serve as protonic acid, and the protonic acid is doped with aniline to carry out emulsion polymerization to obtain the low-dimensional nano-silver/PANI-based thermoelectric composite material. Compared with a polyaniline-based thermoelectric material, the electrical conductivity of the composite material is remarkably improved under the conditions that the heat conductivity of the composite material is basically unchanged, and the Seebeck coefficient is not greatly reduced, and therefore the thermoelectric performance of the composite material can be greatly improved.

Description

A kind of low-dimensional Nano Silver/polyaniline thermoelectric material and preparation method thereof
Technical field
The invention belongs to thermoelectric material and preparation field thereof, particularly a kind of low-dimensional Nano Silver/polyaniline thermoelectric material and preparation method thereof.
Background technology
Thermoelectric material is the specific function material that a class can realize thermoelectricity and the direct conversion of electric energy, and application comprises thermoelectric power generation and two aspects of thermoelectric cooling.Thermoelectric material be by the Seebeck effect of semi-conducting material and paltie effect realize heat energy and electric energy directly intercouples, mutually conversion a class functional material., noiseless pollution-free because himself having, volume is little, the life-span is long, high reliability, and is widely used in the fields such as waste-heat power generation, Aero-Space, military equipment, household electrical appliance.
The thermoelectricity capability of material and three relating to parameters: Seebeck factor alpha, conductivity б and thermal conductivity κ.Have figureofmerit Z to represent the overall thermal electrical property of material, its pass is: Z=α simultaneously 2б/κ, also represents with dimensionless figure of merit ZT conventionally.Yet, research at present and the thermoelectric material overwhelming majority who uses are inorganic semiconductor, expensive raw material price, processing difficulties, the element containing may be poisonous, and current inorganic heat electric material is generally applicable to high temperature and middle temperature, the optional kind of low-temperature inorganic thermoelectric material is less, and these have all limited the industrialized development of thermoelectric material greatly.
Nearly ten years, along with the fast development of organic conductive material, organic thermoelectric material is more and more noticeable as a kind of potential new type low temperature thermoelectric material.Compare with inorganic semiconductor thermoelectric material, organic thermoelectric material not only raw material is cheap and easy to get, and processing is simple, be easy to prepare the opposite sex and flexible device, and thermal conductivity is extremely low, than the little order of magnitude of general inorganic semiconductor material.Conducting polymer is important organic thermoelectric material, and it is to be formed after chemistry and electrochemical doping by the polymer with conjugatedπbond, comprises polyacetylene, polyaniline, polypyrrole, polythiophene etc.In conducting polymer, polyaniline is electrical transmission excellent performance not only, and preparation is simple, structure diversification, has good stability.But the polyaniline of eigenstate is nonconducting, after overdoping, its conductivity can obtain the raising of several orders of magnitude, particularly in polyaniline, add inorganic nanoparticles (as metal, oxide and material with carbon element etc.), by the compound electrical transmission performance that can significantly improve polymer of organic/inorganic.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of low-dimensional Nano Silver/polyaniline thermoelectric material and preparation method thereof, and the inventive method simple and fast is with low cost, can increase the utilance of material, improve generating process, reduce manufacturing cost, there is good industrialization prospect.
A kind of low-dimensional Nano Silver/polyaniline thermoelectric material of the present invention, described thermoelectric material is that low-dimensional Nano Silver is dispersed in the laminated structure of polyaniline, the mass percent of Nano Silver is 2.1%~8.5%.
Described low-dimensional Nano Silver is one or both in nano particle AgNPs, nano silver wire AgNWs.
The preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material of the present invention, comprising:
(1) DBSA DBSA is added in deionized water, stir, dissolve, obtain translucent milky DBSA solution;
(2) compound containing silver element is dissolved in deionized water, obtains containing Ag +solution, then dropwise adds in above-mentioned DBSA solution, stirs, and obtains mixed solution;
(3) aniline monomer is dropwise added in above-mentioned mixed solution, stir, solution can become white emulsion from translucent milky white solution, is then placed in ice bath;
(4) ammonium persulfate APS is dissolved in deionized water, obtain APS solution, then dropwise add in above-mentioned emulsion, stir 3-5h, in course of reaction, can observe, solution becomes light green color from milky, become again light blue, finally become navy blue, a lot of bubbles in solution, then add acetone breakdown of emulsion, stir, filter, washing, freeze drying, grind, compressing tablet, obtain low-dimensional Nano Silver/polyaniline thermoelectric material, detergent alkylate naphthenic acid DBSA wherein, Ag element, aniline monomer, ammonium persulfate APS, the proportionate relationship of acetone is 0.0336 mole: 0.001-0.004 mole: 0.0322 mole: 0.0328 mole: 300 milliliters.
In described step (1), mixing time is 30-60min.
In the middle DBSA solution of described step (1), the ratio of DBSA DBSA and deionized water is 11g:600g.
In described step (2), containing the compound of silver element, be a kind of in silver nitrate, silver sulfate, silver acetate.
In described step (2), mixing time is 20-40min.
Aniline monomer in described step (3) need to be purified the aniline monomer of purchase by decompression distillation, after purifying, aniline monomer has the light brown transparent solution that becomes colorless.
In described step (3), ice bath temperature is 4 ℃, and mixing time is 1-3h.
In described step (4), the ammonium persulfate APS of APS solution and the ratio of deionized water are 7.5g:50g.
In described step (4), freeze drying temperature is-80 ℃, and sublimation drying is 12-24h, can be because of the structural failure of polyaniline in the situation of high temperature drying.
Acetone breakdown of emulsion process can heat release in described step (4), needs to continue stir on the one hand as early as possible breakdown of emulsion and can as early as possible the waste heat of generation be distributed with electric mixer.
In described step (4), mixing time is 20-30min.
In described step (4), washing is deionized water washing 3-5 time.
In described step (4), compressing tablet is discharge plasma sintering SPS compressing tablet pressurize 10-15min, and SPS sintering is mainly the function of utilizing the extrusion forming of SPS energy, but does not heat up sintering.
What in SPS sintering, use in described step (4) is the cylinder graphite grinding tool of Φ 10, so what finally obtain is that diameter is the disk of Φ 10.
The present invention adopts one-step method original position to synthesize low-dimensional Nano Silver composite polyphenylene amine, and in this course of reaction, polyaniline is adulterated by DBSA.Aniline monomer restores low-dimensional Nano Silver in the lamellar structure that is attached to polyaniline, has increased the conductive path of polyaniline, and the thermoelectric material obtaining has excellent thermoelectricity capability.
The present invention adopts said method one-step synthesis silver nano-grain composite polyphenylene amine, low-dimensional Nano Silver/PANI (polyaniline) base thermoelectrical composite material of preparation, conductivity is higher, and conductivity is lower, thereby the ZT value of composite material is significantly improved in whole warm area, and maximum amplification is 281%.
beneficial effect
(1) the present invention, in the situation that to maintain the thermal conductivity that matrix thermoelectric material is lower substantially constant, reduces although Sai Beike (Seeneck) coefficient has by a small margin, and conductivity increases considerably, thus the thermoelectricity capability of raising material by a relatively large margin;
(2) the present invention adopts one-step method original position to synthesize low-dimensional Nano Silver/PANI (polyaniline), and method is simple and convenient, with low cost, can increase the utilance of material, improves production technology, reduces production costs, and has good industrialization prospect.
Accompanying drawing explanation
The infrared spectrogram of AgNPs/PANI (polyaniline) composite material powder of the silver nitrate of Fig. 1 gained different content of the present invention;
The X-ray diffractogram of AgNPs/PANI (polyaniline) composite material powder of Fig. 2 gained different content of the present invention silver nitrate;
The field emission scanning electron microscope figure of Fig. 3 gained 8.5%wt of the present invention AgNPs/PANI (polyaniline) composite material powder different multiples; Field emission scanning electron microscope figure when wherein, figure a is 20000 times; B, c, field emission scanning electron microscope figure when d is 30000 times;
The conductivity of different AgNPs/PANI (polyaniline) composite material of Fig. 4 gained of the present invention block and the relation of temperature;
The Seebeck coefficient of different AgNPs/PANI (polyaniline) composite material of Fig. 5 gained of the present invention block and the relation of temperature;
The thermal conductivity of different AgNPs/PANI (polyaniline) composite material of Fig. 6 gained of the present invention block and the relation of temperature;
The ZT value of different AgNPs/PANI (polyaniline) composite material of Fig. 7 gained of the present invention block and the relation of temperature.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Component is P type PANI matrix powder
Get 11gDBSA (DBSA) and 600g deionized water in the beaker of 2L after electric stirring DBSA be dissolved in uniformly in deionized water, last solution is translucent milky DBSA solution.Get 3g aniline monomer and dropwise join in this solution, electric stirring 3h, solution can become white emulsion from translucent milky white solution.Above-mentioned solution is placed in to the ice bath of 4 ℃, configuration solution B: 7.5gAPS (ammonium persulfate) is dissolved in 50g deionized water.B liquid is dropwise added drop-wise in above-mentioned solution.Electric stirring 5h, can observe in course of reaction, and solution becomes light green color from milky, then becomes light bluely, finally becomes navy blue, a lot of bubbles in solution.In solution, add 300ml acetone breakdown of emulsion, and electric stirring 30 minutes, then filter, and with deionized water washing for several times, freeze drying 24h.
By the above-mentioned dry powder mortar porphyrize obtaining, with SPS(discharge plasma sintering) compressing tablet.Pressurize 10 minutes.The maximum ZT value of the block materials of gained is 1.98 * 10 -5.
Embodiment 2
Component is P type PANI matrix powder+2.1wt%AgNPs
Get 11gDBSA (DBSA) and 600g deionized water in the beaker of 2L after electric stirring DBSA be dissolved in uniformly in deionized water, last solution is translucent milky DBSA solution.Get silver nitrate 0.17g and be dissolved in 50g deionized water, and be dropwise added drop-wise in above-mentioned solution, and electric stirring 30 minutes.Get 3g aniline monomer and dropwise join in this solution, electric stirring 3h, solution can become white emulsion from translucent milky white solution.Above-mentioned solution is placed in to the ice bath of 4 ℃, configuration solution B: 7.5gAPS (ammonium persulfate) is dissolved in 50g deionized water.B liquid is dropwise added drop-wise in above-mentioned solution.Electric stirring 5h, can observe in course of reaction, and solution becomes light green color from milky, then becomes light bluely, finally becomes navy blue, a lot of bubbles in solution.In solution, add 300ml acetone breakdown of emulsion, and electric stirring 30 minutes, then filter, and with deionized water washing for several times, freeze drying 24h.
By the above-mentioned dry powder mortar porphyrize obtaining, with SPS(discharge plasma sintering) compressing tablet.Pressurize 10 minutes.The maximum ZT value of the block materials of gained is 3.72 * 10 -5.
Embodiment 3
Component is P type PANI matrix powder+4.2wt%AgNPs
Get 11gDBSA (DBSA) and 600g deionized water in the beaker of 2L after electric stirring DBSA be dissolved in uniformly in deionized water, last solution is translucent milky DBSA solution.Get silver nitrate 0.334g and be dissolved in 50g deionized water, and be dropwise added drop-wise in above-mentioned solution, and electric stirring 30 minutes.Get 3g aniline monomer and dropwise join in this solution, electric stirring 3h, solution can become white emulsion from translucent milky white solution.Above-mentioned solution is placed in to the ice bath of 4 ℃, configuration solution B: 7.5gAPS (ammonium persulfate) is dissolved in 50g deionized water.B liquid is dropwise added drop-wise in above-mentioned solution.Electric stirring 5h, can observe in course of reaction, and solution becomes light green color from milky, then becomes light bluely, finally becomes navy blue, a lot of bubbles in solution.In solution, add 300ml acetone breakdown of emulsion, and electric stirring 30 minutes, then filter, and with deionized water washing for several times, freeze drying 24h.
By the above-mentioned dry powder mortar porphyrize obtaining, with SPS(discharge plasma sintering) compressing tablet.Pressurize 10 minutes.The maximum ZT value of the block materials of gained is 3.28 * 10 -5.
Embodiment 4
Component is P type PANI matrix powder+6.3wt%AgNPs
Get 11gDBSA (DBSA) and 600g deionized water in the beaker of 2L after electric stirring DBSA be dissolved in uniformly in deionized water, last solution is translucent milky DBSA solution.Get silver nitrate 0.509g and be dissolved in 50g deionized water, and be dropwise added drop-wise in above-mentioned solution, and electric stirring 30 minutes.Get 3g aniline monomer and dropwise join in this solution, electric stirring 3h, solution can become white emulsion from translucent milky white solution.Above-mentioned solution is placed in to the ice bath of 4 ℃, configuration solution B: 7.5gAPS (ammonium persulfate) is dissolved in 50g deionized water.B liquid is dropwise added drop-wise in above-mentioned solution.Electric stirring 5h, can observe in course of reaction, and solution becomes light green color from milky, then becomes light bluely, finally becomes navy blue, a lot of bubbles in solution.In solution, add 300ml acetone breakdown of emulsion, and electric stirring 30 minutes, then filter, and with deionized water washing for several times, freeze drying 24h.
By the above-mentioned dry powder mortar porphyrize obtaining, with SPS(discharge plasma sintering) compressing tablet.Pressurize 10 minutes.The maximum ZT value of the block materials of gained is 5.73 * 10 -5.
Embodiment 5
Component is P type PANI matrix powder+8.5%wtAgNPs
Get 11gDBSA (DBSA) and 600g deionized water in the beaker of 2L after electric stirring DBSA be dissolved in uniformly in deionized water, last solution is translucent milky DBSA solution.Get silver nitrate 0.679g and be dissolved in 50g deionized water, and be dropwise added drop-wise in above-mentioned solution, and electric stirring 30 minutes.Get 3g aniline monomer and dropwise join in this solution, electric stirring 3h, solution can become white emulsion from translucent milky white solution.Above-mentioned solution is placed in to the ice bath of 4 ℃, configuration solution B: 7.5gAPS (ammonium persulfate) is dissolved in 50g deionized water.B liquid is dropwise added drop-wise in above-mentioned solution.Electric stirring 5h, can observe in course of reaction, and solution becomes light green color from milky, then becomes light bluely, finally becomes navy blue, a lot of bubbles in solution.In solution, add 300ml acetone breakdown of emulsion, and electric stirring 30 minutes, then filter, and with deionized water washing for several times, freeze drying 24h.
By the above-mentioned dry powder mortar porphyrize obtaining, with SPS(discharge plasma sintering) compressing tablet.Pressurize 10 minutes.The maximum ZT value of the block materials of gained is 4.46 * 10 -5.
Fig. 3 is the field emission scanning electron microscope figure of 8.5%wt AgNPs/PANI (polyaniline) composite material powder different multiples; Field emission scanning electron microscope figure when figure a is 20000 times, can find out in the lamellar structure that is distributed in polyaniline of AgNPs, size is in 30-60 nanometer; B, c, field emission scanning electron microscope figure when d is 30000 times can find out that PANI powder presents irregular graininess, size is about 30-60nm, and the sign that has secondary growth, nano grain surface regrows nano particle, and integral body is bonded together and presents random network configuration.After compound with silver, we can be clear that silver is graininess at polyaniline and exists, and what have is even coated on inside polyaniline particle.
Adopt the silver nano-grain in nano silver wire alternate embodiment 2~example 5, after testing, the conductivity of gained composite material raises, and composite material thermoelectricity capability value is improved.

Claims (10)

1. low-dimensional Nano Silver/polyaniline thermoelectric material, is characterized in that: described thermoelectric material is that low-dimensional Nano Silver is dispersed in the laminated structure of polyaniline, and the mass percent of Nano Silver is 2.1%~8.5%.
2. a kind of low-dimensional Nano Silver/polyaniline thermoelectric material according to claim 1, is characterized in that: described low-dimensional Nano Silver is one or both in nano particle AgNPs, nano silver wire AgNWs.
3. a preparation method for low-dimensional Nano Silver/polyaniline thermo electric material as claimed in claim 1, comprising:
(1) DBSA DBSA is added in deionized water, stir, dissolve, obtain DBSA solution;
(2) compound containing silver element is dissolved in deionized water, obtains containing Ag +solution, then dropwise adds in above-mentioned DBSA solution, stirs, and obtains mixed solution;
(3) aniline monomer is dropwise added in above-mentioned mixed solution, stir, obtain emulsion, be then placed in ice bath;
(4) ammonium persulfate APS is dissolved in deionized water, obtains APS solution, then dropwise add in above-mentioned emulsion, stir 3-5h, then add acetone breakdown of emulsion, stir, filter, washing, freeze drying, grinds compressing tablet, obtain low-dimensional Nano Silver/polyaniline thermoelectric material, wherein the proportionate relationship of detergent alkylate naphthenic acid DBSA, Ag element, aniline monomer, ammonium persulfate APS, acetone is 0.0336 mole: 0.001-0.004 mole: 0.0322 mole: 0.0328 that: 300ml.
4. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: the DBSA in described step (1) DBSA solution and the mass ratio of deionized water are 11:600; Mixing time is 30-60min.
5. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: in described step (2), containing the compound of silver element, be a kind of in silver nitrate, silver sulfate, silver acetate.
6. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: in described step (2), mixing time is 20-40min.
7. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: in described step (3), ice bath temperature is 4 ℃, and mixing time is 1-3h.
8. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: in described step (4) APS solution, the mass ratio of APS and deionized water is 7.5g:50g.
9. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: in described step (4), freeze drying temperature is-80 ℃, and sublimation drying is 12-24h; Mixing time is 20-30min.
10. the preparation method of a kind of low-dimensional Nano Silver/polyaniline thermo electric material according to claim 3, is characterized in that: in described step (4), compressing tablet is discharge plasma sintering SPS compressing tablet pressurize 10-15min.
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CN108767105A (en) * 2018-05-18 2018-11-06 徐冬 A kind of preparation method of nano composite thermoelectric materials

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CN106771706A (en) * 2016-11-22 2017-05-31 武汉理工大学 A kind of method of the thermoelectric material of quick screenability optimization
CN106771706B (en) * 2016-11-22 2019-10-25 武汉理工大学 A kind of method of the thermoelectric material of quick screenability optimization
CN108649196A (en) * 2018-04-28 2018-10-12 河南工业大学 Lithium vanadate combination electrode material and the preparation method and application thereof
CN108649196B (en) * 2018-04-28 2021-03-16 河南工业大学 Lithium vanadate composite electrode material and preparation method and application thereof
CN108767105A (en) * 2018-05-18 2018-11-06 徐冬 A kind of preparation method of nano composite thermoelectric materials

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