CN106784288A - A kind of preparation method for strengthening composite thermoelectric material performance - Google Patents
A kind of preparation method for strengthening composite thermoelectric material performance Download PDFInfo
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- CN106784288A CN106784288A CN201611250714.3A CN201611250714A CN106784288A CN 106784288 A CN106784288 A CN 106784288A CN 201611250714 A CN201611250714 A CN 201611250714A CN 106784288 A CN106784288 A CN 106784288A
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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
- H10N10/01—Manufacture or treatment
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
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- 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
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
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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
- H10N10/856—Thermoelectric active materials comprising organic compositions
Abstract
The invention provides a kind of carbon nano tube/graphene/poly- (3,4 ethene dioxythiophene):The preparation method of polystyrolsulfon acid composite thermoelectric material.Kayexalate is soluble in water, appropriate CNT and Graphene are added, after being uniformly dispersed, appropriate 3,4 ethene dioxythiophene monomer is added dropwise, after being well mixed, add ammonium persulfate and ferric sulfate initiated polymerization.After reaction terminates, product is centrifuged, the black product deionized water cyclic washing for obtaining simultaneously is centrifuged, vacuum drying.Simple, low production cost, carbon nano tube/graphene/poly- (3,4 ethene dioxythiophene) of environmental protection the invention provides a kind of process conditions:The novel preparation method of polystyrolsulfon acid composite thermoelectric material.Preparation method of the invention improves the thermoelectricity capability of composite thermoelectric material simultaneously.
Description
Technical field
The present invention relates to a kind of carbon nano tube/graphene/poly- (3,4- ethene dioxythiophenes):Polystyrolsulfon acid compound thermal
The preparation method of electric material, more particularly to thiophene form compound thermoelectricity by in-situ oxidizing-polymerizing doped carbon nanometer pipe and Graphene
The method of material.
Background technology
With industrialized quickening, solve the problems, such as that thing followed environmental pollution and energy shortage are more and more urgent.In day
Used heat can be inevitably produced in often life and production, if can develop and can utilize the material of used heat will be using a kind of
Largely alleviating energy crisis.Thermoelectric material is exactly a kind of environmentally friendly and can recycle the functional material of used heat.
Thermoelectric material mainly uses the motion of carrier (hole or electronics) to realize directly turning between heat energy and electric energy
Change, with small volume, it is lightweight, without noiselessness in drive disk assembly, work, non-environmental-pollution, long service life, easily controllable etc.
Advantage, has been successfully applied to the fields such as Aero-Space, micro sensing, waste-heat power generation, be a class have a extensive future, competitiveness it is strong
Energy substitution material.Dimensionless thermoelectric figure of merit ZT is the important indicator for weighing conducting material thermoelectricity performance, and expression formula is：
Wherein, S represents Seebeck coefficients；It is phonon thermal conductivity rate and electronics thermal conductivity
The sum of rate；T represents absolute temperature.ZT values are bigger, and thermoelectric conversion efficiency is better, therefore, to improve thermoelectricity capability, should try one's best raisingAlloy based on Bi-Te-Sb can be reduced largelyValue changes are not
Greatly, thus be still current most widely used thermoelectric material.But inorganic material resource-constrained, expensive, processing difficulties, ring
Border is seriously polluted and poisonous, can not turn into long-range green energy resource material.
Conducting polymer has aboundresources, cheap, easy processing, the low advantage of thermal conductivity, wherein, intrinsic conduction gathers
Compound poly- (3,4- ethene dioxythiophenes) is because electrical conductivity is high, light transmittance is good, inexpensive, environmental stability is good, lower thermal conductivity and
Easily controllable the advantages of, turns into one of current most potential Organic thermoelectric material.But as Organic thermoelectric material, electrical conductivity
It is low so that material ZT values be less than inorganic thermoelectric material.(the Journal of Electronic Materials such as Scholdt
2010; 39(9):Poly- (3,4- ethene dioxythiophenes) 1589-1592) is adulterated with dimethyl sulfoxide (DMSO):Polystyrolsulfon acid, passes through
Change the concentration of dimethyl sulfoxide (DMSO) and keep Seebeck coefficients and thermal conductivity to keep constant while increasing electrical conductivity, so as to obtain
Obtained ZT values higher.CNT and Graphene have the advantages that electrical conductivity high, good in optical property, good mechanical property, are near
The class conductive additive being had good prospects in conducting polymer over year.
The composite thermoelectric material that conducting polymer is prepared with CNT or Graphene by methods such as blendings, certain
The thermoelectricity capability of material is improve in degree, but also has suitable distance apart from large-scale commercial applications.Therefore, ensureing
Preparation method is simple, low cost, it is environment-friendly, easy to process the advantages of on the premise of, research one kind can further enhance material
Expect that the synthetic method of thermoelectricity capability has very important significance.
The content of the invention
It is an object of the invention to provide a kind of simple to operate, environmental protection, high-performance heat with low cost, of good performance
Composite（Poly- (3,4- ethene dioxythiophenes):Kayexalate/carbon nano tube/graphene）Preparation method.Should
Method is mainly is reacted by in-situ oxidizing-polymerizing, and CNT and Graphene are doped into poly- (3,4- ethylene dioxy thiophenes simultaneously
Fen) in, using CNT and the chemiluminescence of Graphene, further improve the thermoelectricity capability of composite.
The present invention uses 3,4 ethene dioxythiophene monomers, CNT and Graphene for raw material, and kayexalate is
Surfactant, ammonium persulfate and ferric sulfate are oxidant, prepare poly- (3,4- by the in-situ oxidizing-polymerizing of thiophene at low temperature
Ethene dioxythiophene):Kayexalate/carbon nano tube/graphene composite thermoelectric material.
Preparation process of the invention is：
(1) dispensing：
Dispensing：(CNT+Graphene) is 250 with the mass ratio of 3,4- ethene dioxythiophenes:1~25:1；Wherein carbon nanometer
Pipe can only add one-component with Graphene, if adding CNT and Graphene simultaneously, its mass ratio can be 99:1~1:99 it
Between arbitrary proportion；
3,4- ethene dioxythiophenes are 2 with kayexalate mass ratio:1~1:1, oxidant and kayexalate matter
Amount is than being 3:1~2:1, described oxidant is ferric sulfate and ammonium persulfate, and wherein ammonium persulfate is with the mass ratio of ferric sulfate
50:1~30:1；
Dispensing order be that surfactant kayexalate is dissolved in deionized water, be subsequently adding CNT and
Graphene, ultrasonic disperse obtains uniform dispersion liquid, adds 3,4-rthylene dioxythiophene monomer, and mechanical agitation is to being uniformly dispersed；
(2) it is polymerized：The ferric sulfate that will have been configured is added in the dispersion liquid obtained by step (1) with ammonium persulfate solution, in 5 DEG C, N2
Atmosphere reacts 48h；
(3) it is centrifuged, washs：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining carries out cyclic washing centrifugal treating,
80-100 DEG C of vacuum drying 12h.
CNT of the present invention is multi-walled carbon nano-tubes (MWCNT) or SWCN, and length is 0.5-2 μ
M, external diameter is 10-20nm；The Graphene is Graphene prepared by solvent stripping method, and the number of plies is 1-4 layers.
Before step (2) of the present invention adds the ferric sulfate and ammonium persulfate solution for having configured, should be to obtained by step (1)
N is passed through in dispersion liquid21h, to remove the O in dispersion liquid2, prevent thiophene peroxidating.
Ammonium persulfate and the mass ratio of ferric sulfate are 50 in step (2) of the present invention:1~30:1.
The present invention further discloses carbon nano tube/graphene/poly- (the 3,4- ethylene dioxy thiophenes prepared using the method
Fen):Polystyrolsulfon acid composite thermoelectric material is improving power factor, improves the application in terms of electrical conductivity.Experimental result shows：
After the present invention adds CNT and Graphene, than adding single nano-carbon material, poly- (3,4-rthylene dioxythiophene):Polyphenyl second
The power factor of alkene sulfonic acid improves 72%, is more beneficial for improving the conversion efficiency of thermoelectric of thermoelectric material.
It is positive that the preparation method of enhancing composite thermoelectric material performance disclosed by the invention has compared with prior art
Effect is：
（1）Preparation method of the invention is simple, and reaction condition is gentle, course of reaction with water as solvent, environmental protection, cost of material
It is cheap, have broad application prospects.
（2）The method of the present invention takes full advantage of the intrinsic lower thermal conductivity of conducting polymer polythiophene and CNT and stone
The high conductivity of black alkene, and the heat of composite is further increased with the chemiluminescence of Graphene using CNT
Electrical property.
Brief description of the drawings
Fig. 1 is the transmission electron micrograph of the composite of the synthesis of embodiment 1；
Fig. 2 be embodiment it is 2-in-1 into composite transmission electron micrograph；
Fig. 3 is the transmission electron micrograph of the composite of the synthesis of embodiment 3；
Fig. 4 is the electrical conductivity of the composite of the synthesis of embodiment 1,2,3；
Fig. 5 is the Seebeck coefficients of the composite of the synthesis of embodiment 1,2,3；
Fig. 6 is the power factor of the composite of the synthesis of embodiment 1,2,3.
Specific embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention
Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
On the premise of invention spirit and scope, the various changes that are carried out to the material component and consumption in these embodiments or change
Belong to protection scope of the present invention.Raw materials used and reagent of the invention is commercially available.Wherein multi-walled carbon nano-tubes (MWCNT), poly-
SSS (PSSNa), 3,4- ethene dioxythiophenes (EDOT) etc. are commercially available.
Embodiment 1
（1）Dispensing：First by 1g kayexalates (PSSNa) add 145mL deionized waters in, after stirring and dissolving, plus
Enter 0.005g multi-walled carbon nano-tubes (MWCNT) and 0.005g Graphenes (graphene), after ultrasonic disperse is uniform, 1.25g is added dropwise
3,4-rthylene dioxythiophene (EDOT) monomer, mechanical agitation is passed through N to well mixed21h。
（2）Polymerization：During 0.05g ferric sulfate and 2g ammonium persulfates added into 12.5g deionized waters, after stirring, plus
In entering the dispersion liquid obtained by step (1).Course of reaction is N2Atmosphere, mechanical agitation speed is 600rpm, and reaction temperature is 5 DEG C,
Reaction time is 48h.
（3）Centrifugation, washing：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining is carried out at cyclic washing centrifugation
Reason.
（4）Dry：The black precipitate that will be finally given is vacuum dried 12h in 100 DEG C.
The conductivity that the present embodiment is obtained be 2.936 S/cm, Seebeck coefficients be 18.9 μ V/K, power because
Son is 0.105 μ WmK-1.Fig. 1 is the transmission electron micrograph that the present embodiment 1 obtains composite.
Embodiment 2
(1) dispensing：First by 1g kayexalates (PSSNa) add 145mL deionized waters in, after stirring and dissolving, plus
Enter 0.01g multi-walled carbon nano-tubes (MWCNT), after ultrasonic disperse is uniform, 1.25g 3,4-rthylene dioxythiophenes (EDOT) is added dropwise single
Body, mechanical agitation is passed through N to well mixed21h。
(2) it is polymerized：During 0.05g ferric sulfate and 2g ammonium persulfates added into 12.5g deionized waters, after stirring,
In dispersion liquid obtained by addition step (1).Course of reaction is N2Atmosphere, mechanical agitation speed is 600rpm, and reaction temperature is 5
DEG C, the reaction time is 48h.
(3) it is centrifuged, washs：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining is carried out at cyclic washing centrifugation
Reason.
(4) dry：The black precipitate that will be finally given is vacuum dried 12h in 100 DEG C.
The conductivity that the present embodiment is obtained is 2.547 S/cm, and Seebeck coefficients are 16.4 μ V/K, power factor
It is 0.069 μ WmK-1.Fig. 2 is the transmission electron micrograph that the present embodiment 2 obtains composite.
Embodiment 3
(1) dispensing：First by 1g kayexalates (PSSNa) addition 145mL deionized waters, after stirring and dissolving, add
0.01g Graphenes, after ultrasonic disperse is uniform, are added dropwise 1.25g 3,4-rthylene dioxythiophene (EDOT) monomer, and mechanical agitation is to mixed
Close uniform, and be passed through N21h。
(2) it is polymerized：During 0.05g ferric sulfate and 2g ammonium persulfates added into 12.5g deionized waters, after stirring, plus
In entering the dispersion liquid obtained by step (1).Course of reaction is N2Atmosphere, mechanical agitation speed is 600rpm, and reaction temperature is 5 DEG C,
Reaction time is 48h.
(3) it is centrifuged, washs：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining is carried out at cyclic washing centrifugation
Reason.
(4) dry：The black precipitate that will be finally given is vacuum dried 12h in 100 DEG C.
The conductivity that the present embodiment is obtained be 2.679 S/cm, Seebeck coefficients be 18.3 μ V/K, power because
Son is 0.090 μ WmK-1.Fig. 3 is the transmission electron micrograph that the present embodiment 3 obtains composite.
Embodiment 4
(1) dispensing：First by 1g kayexalates (PSSNa) addition 145mL deionized waters, after stirring and dissolving, add
0.05g multi-walled carbon nano-tubes (MWCNT), after ultrasonic disperse is uniform, is added dropwise 1.25g 3,4-rthylene dioxythiophene (EDOT) monomer,
Mechanical agitation is passed through N to well mixed21h。
(2) it is polymerized：During 0.05g ferric sulfate and 2g ammonium persulfates added into 12.5g deionized waters, after stirring, plus
In entering the dispersion liquid obtained by step (1).Course of reaction is N2Atmosphere, mechanical agitation speed is 600rpm, and reaction temperature is 5 DEG C,
Reaction time is 48h.
(3) it is centrifuged, washs：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining is carried out at cyclic washing centrifugation
Reason.
(4) dry：The black precipitate that will be finally given is vacuum dried 12h in 100 DEG C.
The conductivity that the present embodiment is obtained is 2.605S/cm, and Seebeck coefficients are 16.9 μ V/K, power factor
It is 0.074 μ WmK-1。
Embodiment 5
(1) dispensing：First by 1g kayexalates (PSSNa) addition 145mL deionized waters, after stirring and dissolving, add
0.05g Graphenes, after ultrasonic disperse is uniform, are added dropwise 1.25g 3,4-rthylene dioxythiophene (EDOT) monomer, and mechanical agitation is to mixed
Close uniform, and be passed through N2 1h。
(2) it is polymerized：During 0.05g ferric sulfate and 2g ammonium persulfates added into 12.5g deionized waters, after stirring, plus
In entering the dispersion liquid obtained by step (1).Course of reaction is N2Atmosphere, mechanical agitation speed is 600rpm, and reaction temperature is 5 DEG C,
Reaction time is 48h.
(3) it is centrifuged, washs：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining is carried out at cyclic washing centrifugation
Reason.
(4) dry：The black precipitate that will be finally given is vacuum dried 12h in 100 DEG C.
The conductivity that the present embodiment is obtained is 2.714 S/cm, and Seebeck coefficients are 18.5 μ V/K, power factor
It is 0.093 μ WmK-1。
Embodiment 6
Contrast test
Conclusion：
(1) after adding 1% CNT, poly- (3,4-rthylene dioxythiophene):The power factor of polystyrolsulfon acid improves 13%.
(2) after adding 1% Graphene, poly- (3,4-rthylene dioxythiophene):The power factor of polystyrolsulfon acid improves
48%。
(3) while after adding CNT and Graphene, poly- (3,4-rthylene dioxythiophene):The power of polystyrolsulfon acid
Factor improves 72%, than adding single carbon material notable.
Claims (5)
1. it is a kind of strengthen composite thermoelectric material performance preparation method, it is characterised in that carried out by the steps：
(1) dispensing：CNT+Graphene is 250 with the mass ratio of 3,4- ethene dioxythiophenes:1~25:1；Wherein carbon nanometer
Pipe can only add one-component with Graphene, if adding CNT and Graphene simultaneously, its mass ratio can be 99:1~1:99；
3,4- ethene dioxythiophenes are 2 with kayexalate mass ratio:1~1:1, oxidant and kayexalate matter
Amount is than being 3:1~2:1, described oxidant is ferric sulfate and ammonium persulfate, and wherein ammonium persulfate is with the mass ratio of ferric sulfate
50:1~30:1；
Surfactant kayexalate is dissolved in deionized water, CNT and Graphene is subsequently adding, ultrasound
Dispersion 1h, adds 3,4-rthylene dioxythiophene monomer, and mechanical agitation obtains uniform dispersion liquid；
(2) it is polymerized：The oxidant that will have been configured is added in the dispersion liquid obtained by step (1), in 5 DEG C, N2Atmosphere reacts 48h；
(3) it is centrifuged, washs：After the completion of polymerization, product is centrifuged, the black precipitate for obtaining carries out cyclic washing centrifugal treating, 80
~ 100 DEG C of vacuum drying 12h.
2. the preparation method described in claim 1, wherein CNT are multi-walled carbon nano-tubes, and length is 0.5-2, external diameter
It is 10-20nm.
3. before the preparation method described in claim 1, wherein step (2) add the ferric sulfate and ammonium persulfate solution for having configured,
Should be to being passed through N in the dispersion liquid obtained by step (1)2, the time is 1h.
4. the preparation method described in claim 1, wherein oxidant is alternatively ferric sulfate and sodium peroxydisulfate.
5. carbon nano tube/graphene/poly- (3,4- ethene dioxythiophenes) is prepared using claim 1 methods described:Polystyrene
Application of the sulfonic acid composite thermoelectric material in terms of power factor is improved.
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| CN110284322A (en) * | 2019-07-01 | 2019-09-27 | 深圳市尼森实业有限公司 | Carbon-based fire-retardant compound fabric of a kind of compliant conductive fever and preparation method thereof |
| CN110808329A (en) * | 2019-11-13 | 2020-02-18 | 四川大学 | Phthalocyanine copper sulfonic acid doped polymer-based thermoelectric material and preparation method and application thereof |
| CN112358772A (en) * | 2020-11-12 | 2021-02-12 | 华南理工大学 | Flexible flame-retardant coating with sensitive temperature sensing and fire early warning functions and preparation method and application thereof |
| CN112509729A (en) * | 2019-09-16 | 2021-03-16 | 天津工业大学 | Poly (3, 4-ethylenedioxythiophene)/graphene oxide-carbon nanotube flexible transparent conductive film with double-layer structure and preparation method thereof |
| CN113215814A (en) * | 2020-01-21 | 2021-08-06 | 天津工业大学 | Low-temperature interfacial polymerization organic textile thermoelectric material and preparation method thereof |
| CN116156988A (en) * | 2023-01-12 | 2023-05-23 | 江苏上达半导体有限公司 | Flexible thermoelectric material for semiconductor device and preparation method thereof |
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| CN110284322A (en) * | 2019-07-01 | 2019-09-27 | 深圳市尼森实业有限公司 | Carbon-based fire-retardant compound fabric of a kind of compliant conductive fever and preparation method thereof |
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| CN110808329A (en) * | 2019-11-13 | 2020-02-18 | 四川大学 | Phthalocyanine copper sulfonic acid doped polymer-based thermoelectric material and preparation method and application thereof |
| CN110808329B (en) * | 2019-11-13 | 2021-03-23 | 四川大学 | Phthalocyanine copper sulfonic acid doped polymer-based thermoelectric material and preparation method and application thereof |
| CN113215814A (en) * | 2020-01-21 | 2021-08-06 | 天津工业大学 | Low-temperature interfacial polymerization organic textile thermoelectric material and preparation method thereof |
| CN112358772A (en) * | 2020-11-12 | 2021-02-12 | 华南理工大学 | Flexible flame-retardant coating with sensitive temperature sensing and fire early warning functions and preparation method and application thereof |
| CN112358772B (en) * | 2020-11-12 | 2022-05-24 | 华南理工大学 | Flexible flame-retardant coating with sensitive temperature sensing and fire early warning functions and preparation method and application thereof |
| CN116156988A (en) * | 2023-01-12 | 2023-05-23 | 江苏上达半导体有限公司 | Flexible thermoelectric material for semiconductor device and preparation method thereof |
| CN116156988B (en) * | 2023-01-12 | 2023-10-20 | 江苏上达半导体有限公司 | Flexible thermoelectric material for semiconductor device and preparation method thereof |
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