CN108504049A - A kind of preparation method of the compound thermal electric film of macromolecule - Google Patents
A kind of preparation method of the compound thermal electric film of macromolecule Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2365/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The invention discloses a kind of preparation methods of the compound thermal electric film of macromolecule, it is characterized in that, utilize energy filtering effect design conducting polymer and the effective barrier of inorganic semiconductor nanocomposite, by preparing high-performance flexible thermal electric film by depressurizing suction filtration after chemical synthesis conductive polymer nanometer line solution, with inorganic semiconductor nano wire progress physical blending.Power factor is improved 35 70% by content of the present invention by controlling inorganic phase to significantly improve Seebeck coefficient and the thermoelectric (al) power factor.
Description
Technical field
The present invention relates to novel energy field of material technology, relate to the use of energy filtering effect and design nano combined thermoelectricity material
Material, is related to organic conductive polymer and inorganic semiconductor physical blending, more particularly, to a kind of high-performance flexible thermoelectric material
Preparation method.
Background technology
With economical rapid development and social progress, the mankind inevitably face the prestige of environmental degradation and energy shortage
The side of body.Thermo-electric generation shows infinite potentiality as one of green energy resource technology in human kind sustainable development strategy.Utilize temperature
The waste heat such as atural beat or industry and automotive residual heat can be directly changed into electric energy by poor generation technology, have long lifespan, reliability height,
And environment will not be polluted, cost is reduced, substantially increase the utilization rate of the energy the advantages that noiseless when working, have
There are good comprehensive economic results in society, therefore thermoelectric generation becomes Recent study hot spot.
The thermoelectricity capability of inorganic semiconductor material is more excellent, have higher power factor S2 σ, but thermal conductivity compared with
Height, the prices of raw materials are expensive, and its assembly device is more heavy, not Portable belt.Organic thermoelectric material has good flexibility,
And its synthesis is simple, raw material is cheap, rich reserves, lightweight, thermal conductivity are low.Conducting polymer, such as poly- 3,4-ethylene dioxythiophene
(PEDOT) and polyaniline (PANI) has flexible and easy processing in low temperature or room temperature by liquid phase route, and thermoelectricity capability is in recent years
Also it is constantly improved, huge applications potentiality is shown in flexible thermoelectric material.Research shows that：Inorganic by high conductivity is partly led
Body or nano metal material can be obviously improved electric property among being combined to conducting polymer matrix, while keep macromolecule matrix
The lower thermal conductivity feature possessed.If publication number is CN 103311428 A of 102593342 A and CN, by organic conductive
Polymer prepares composite thermoelectric material with inorganic particle by the method for in-situ polymerization, to be finally reached thermoelectricity capability optimization
Purpose.However, the mechanism of such compound system thermoelectricity capability optimization does not become clear elaboration.
Metal is in contact with semiconductor, and since fermi level will be unified, energy band is near metal-semiconductor interface
It can bend.If interface forms carrier accumulation layer, the two is Ohmic contact；If interface forms carrier depletion layer,
Interface forms potential barrier, then the two is Schottky contacts.Effective potential barrier generally is constructed in nano composite system, it can be by low energy
Carrier filter out, i.e. energy filtering effect.Energy filtering effect is as one of carrier scattering mechanism, by high-energy
The ratio of carrier and low energy carrier controls, and then controls mobility, is commonly used to significantly improve Seebeck coefficient
And power factor.The present invention by two kinds of nano wires by the method for physical mixed, by organic with inorganic phase contact interface structure
Effective potential barrier is built, a kind of conducting polymer/inorganic nano combined high-performance flexible heat is theoretically prepared by design of material
Conductive film, technique are simple compared to common in-situ polymerization condition, and controllability is high.
Invention content
Problem to be solved by this invention is：Power factor (the S of existing Organic thermoelectric material2It is σ) relatively low, lead to its heat
The not high technical problem of photoelectric transformation efficiency, provides that a kind of to prepare conducting polymer/inorganic nano combined high-performance flexible thermoelectricity thin
The method of film.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of preparation of the compound thermal electric film of macromolecule
Method, which is characterized in that utilize energy filtering effect design conducting polymer and the effective wall of inorganic semiconductor nanocomposite
It builds, by chemical synthesis conductive polymer nanometer line solution, passes through decompression after carrying out physical blending with inorganic semiconductor nano wire
Suction filtration prepares high-performance flexible thermal electric film.
Preferably, above-mentioned preparation method includes the following steps：
Step 1)：Prepare conductive polymer nanometer line solution：First by surfactant-dispersed to deionized water, then will
Conducting polymer monomer is added in surfactant solution, adds oxidant, after being reacted by magnetic agitation, by mixture
After filtering and use deionized water, organic solvent to clean 2~9 times in turn successively, dispersion is in organic solvent；
Step 2：Prepare conducting polymer/inorganic semiconductor mixed solution：By nanowire solution and one-dimensional inorganic semiconductor
Nano material mixes, and ultrasonic disperse is uniform；Wherein, the mass concentration of one-dimensional inorganic semiconductor nano material is 10~90%；
The chemical synthesis conducting polymer can be realized by the method for electrochemical polymerization.
Step 3)：Prepare thermal electric film：Conducting polymer/inorganic semiconductor mixed solution is made by sand core filter device
It is filtered and is formed a film with vacuum pump, filtered and terminate to be placed on the drying 5~24 hours of 25~80 DEG C of vacuum drying oven.It is described that prepare thermoelectricity thin
Film can be realized by the method for spin coating.
It is highly preferred that in the step 1) conducting polymer monomer using 3,4-ethylene dioxythiophene (EDOT), aniline or
Pyrroles.
It is highly preferred that the surfactant in the step 1) is using dodecyl sodium sulfate (SDS), cetyl front three
Base ammonium bromide (CTAB), dodecyl trimethyl ammonium bromide (DTAB) or alkyl trimethyl ammonium bromide (OTAB).
It is highly preferred that the oxidant in the step 1) uses ferric trichloride (FeCl3), p-methyl benzenesulfonic acid iron (Fe
(tos)3) or ammonium persulfate (APS).
It is highly preferred that in the step 1) in conductive polymer nanometer line solution surfactant a concentration of 0~40mM,
A concentration of 5~30mM of conducting polymer monomer, oxidant concentration are 5~60mM.
It is highly preferred that cleaning organic solvent uses any one in ethyl alcohol, methanol and acetone in the step 1)
Or it is several；Dispersion uses ethyl alcohol, methanol or acetone with organic solvent.
It is highly preferred that one-dimensional inorganic semiconductor nano material is using tellurium (Te), semi-conductor type carbon nanometer in the step 2)
Manage (CNT) or bismuth (Bi).
Use aperture for 0.22 micron of nylon leaching film it is highly preferred that being filtered in the step 3).
It is highly preferred that the film weight that the step 3) obtains is 10~90mg.
Compared with prior art, the beneficial effects of the present invention are：
1, thermoelectricity nanocomposite design is carried out using energy filtering effect, sets about thermoelectric material from performance optimisation mechanism
Selection；
2, there is film good flexibility, power factor to be obviously improved 20~300 times compared to pure conducting polymer；
3, preparation method is quick and easy, easy to spread；
4, the flexible thermo-electric device haveing excellent performance can be obtained.
Specific implementation mode
In order to make the present invention more obvious and understandable, it is hereby described in detail below with preferred embodiment.
Embodiment 1
A kind of preparation method of PEDOT/Te high-performance nanos composite and flexible thermal electric film：
Step 1：Dodecyl sodium sulfate (SDS) will be dissolved in deionized water, glass bar is used in combination to stir to colourless
Ferric trichloride (FeCl is added after bright shape3), it is placed on magnetic stirring apparatus in 50~65 DEG C of stirrings, by 3,4 enedioxies after 1 hour
Thiophene (EDOT) is slowly added into above-mentioned solution, is stirred 6 hours at 50 DEG C.Wherein paratoluenesulfonic acid sodium salt dosage be 0.30M, three
Iron chloride dosage is 0.16M, a concentration of 0.07M of 3,4 ethylenedioxy thiophenes.Mixed solution is in navy blue after reaction；
Step 2：Appropriate amount of deionized water is added in step 1 acquired solution, ultrasonic vibration 20~after sixty minutes pours into sand core mistake
Device is filtered, remaining solid proper amount of methanol is disperseed after carrying out decompression suction filtration, is filtered again after ultrasonic vibration, repeats above-mentioned mistake
The nano wire cleaned up, is finally dispersed in 500mL methanol solutions by 6 cycles of journey again；
Step 3：It takes above-mentioned solution 35mL, ultrasonic vibration 40 minutes after tellurium nano-wire is added, pour into sand core filter device, into
Row decompression filters.Wherein, the mass fraction of tellurium nano-wire is 90%, and the nylon for the use of aperture being 0.22 micron during filtering is filtered
Film；
Step 4：The filter membrane that above-mentioned end filters is placed in vacuum drying oven drying, the wherein temperature of baking oven is 50 DEG C, drying
Time is 12 hours.
Step 5：The thermoelectricity capability of the prepared film of test, seebeck coefficient Ss are 87.3 μ V/K, and conductivityσ is
151.8S/cm, power factor (S2σ) it is 115.69 μ W m-1 K-2, it is pure PEDOT nano wire films (19.1 μ W m-1K-2)
6.06 again.
Embodiment 2
A kind of preparation method of PEDOT/MWNTs high-performance nanos composite and flexible thermal electric film：
Step 1：Dodecyl sodium sulfate (SDS) will be dissolved in deionized water, glass bar is used in combination to stir to colourless
Ferric trichloride (FeCl is added after bright shape3), it is placed on magnetic stirring apparatus in 50 DEG C of stirrings, by 3,4 ethylenedioxy thiophenes after 1 hour
(EDOT) it is slowly added into above-mentioned solution, is stirred 6 hours at 50 DEG C.Wherein paratoluenesulfonic acid sodium salt dosage is 0.30M, tri-chlorination
Iron dosage is 0.16M, a concentration of 0.07M of 3,4 ethylenedioxy thiophenes.Mixed solution is in navy blue after reaction；
Step 2：Appropriate amount of deionized water is added in step 1 acquired solution, ultrasonic vibration after forty minutes, pours into sand core filtering dress
It sets, remaining solid proper amount of methanol is disperseed after carrying out decompression suction filtration, is filtered again after ultrasonic vibration, repeats the above process 6
The nano wire cleaned up is finally dispersed in 500mL methanol solutions by a cycle again；
Step 3：It takes above-mentioned solution 35mL, ultrasonic vibration 40 minutes after multi-walled carbon nanotube is added, pour into sand core filtering dress
It sets, carries out decompression suction filtration.Wherein, the mass fraction of multi-walled carbon nanotube is 10%, micro- for 0.22 using aperture during filtering
The nylon leaching film of rice；
Step 4：The filter membrane that above-mentioned end filters is placed in vacuum drying oven drying, the wherein temperature of baking oven is 50 DEG C, drying
Time is 12 hours；
Step 5：The thermoelectricity capability of the prepared film of test, seebeck coefficient Ss are 33.2 μ V/K, and conductivityσ is
674.5S/cm, power factor (S2σ) it is 74.35 μ Wm-1K-2, it is pure PEDOT nano wire films (19.1 μ W m-1K-2) 3.89
Times.
Embodiment 3
A kind of preparation method of PPY/MWNTs high-performance nanos composite and flexible thermal electric film：
Step 1：In deionized water by cetyl trimethylammonium bromide (CTAB) dissolving, it is used in combination glass bar to stir evenly
After pyrroles is added, be placed on magnetic stirring apparatus in 0~5 DEG C of stirring, be slowly added into ammonium persulfate (ABS) after 1 hour above-mentioned
In solution, reacted 6 hours at 0~5 DEG C.Wherein pyrrole concentrations are 15mM, are 1: 1 with ammonium persulfate molar ratio；Cetyl three
Methyl bromide ammonium concentration is 0.87mM；
Step 2：Appropriate amount of deionized water is added in step 1 acquired solution, ultrasonic vibration after forty minutes, pours into sand core filtering dress
It sets, remaining solid ethanol in proper amount is disperseed after carrying out decompression suction filtration, is filtered again after ultrasonic vibration, repeats the above process 6
The nano wire cleaned up is finally dispersed in 500mL ethanol solutions by a cycle again；
Step 3：It takes above-mentioned solution 35mL, ultrasonic vibration 40 minutes after multi-walled carbon nanotube is added, pour into sand core filtering dress
It sets, carries out decompression suction filtration；Wherein, the mass fraction of multi-walled carbon nanotube is 20%, micro- for 0.22 using aperture during filtering
The nylon leaching film of rice；
Step 4：The filter membrane that above-mentioned end filters is placed in vacuum drying oven drying, the wherein temperature of baking oven is 50 DEG C, drying
Time is 12 hours；
Step 5：The thermoelectricity capability of the prepared film of test, seebeck coefficient Ss are 21.6 μ V/K, and conductivityσ is
100.3S/cm, power factor (S2σ) it is 4.68 μ Wm-1K-2, it is pure PPY nano wire films (0.02 μ Wm-1K-2) 220 times.
Embodiment 4
A kind of preparation method of PPY/Te high-performance nanos composite and flexible thermal electric film：
Step 1：In deionized water by cetyl trimethylammonium bromide (CTAB) dissolving, it is used in combination glass bar to stir evenly
After pyrroles is added, be placed on magnetic stirring apparatus in 0~5 DEG C of stirring, be slowly added into ammonium persulfate (ABS) after 1 hour above-mentioned
In solution, reacted 6 hours at 0~5 DEG C.Wherein pyrrole concentrations are 15mM, are 1: 1 with ammonium persulfate molar ratio；Cetyl three
Methyl bromide ammonium concentration is 0.87mM；
Step 2：Appropriate amount of deionized water is added in step 1 acquired solution, ultrasonic vibration after forty minutes, pours into sand core filtering dress
It sets, remaining solid ethanol in proper amount is disperseed after carrying out decompression suction filtration, is filtered again after ultrasonic vibration, repeats the above process 6
The nano wire cleaned up is finally dispersed in 500mL ethanol solutions by a cycle again；
Step 3：It takes above-mentioned solution 35mL, ultrasonic vibration 40 minutes after tellurium nano-wire is added, pour into sand core filter device, into
Row decompression filters；Wherein, the mass fraction of tellurium nano-wire is 70%, and the nylon for the use of aperture being 0.22 micron during filtering is filtered
Film；
Step 4：The filter membrane that above-mentioned end filters is placed in vacuum drying oven drying, the wherein temperature of baking oven is 50 DEG C, drying
Time is 12 hours；
Step 5：The thermoelectricity capability of the prepared film of test, seebeck coefficient Ss are 120.7 μ V/K, and conductivityσ is
0.52S/cm, power factor (S2σ) it is 0.76 μ W m-1K-2, it is pure PPY nano wire films (0.02 μ W m-1K-2) 38 times.
Claims (10)
1. a kind of preparation method of the compound thermal electric film of macromolecule, which is characterized in that designed using energy filtering effect conductive poly-
Object and the effective barrier of inorganic semiconductor nanocomposite are closed, it is and inorganic by chemical synthesis conductive polymer nanometer line solution
After semiconductor nanowires progress physical blending high-performance flexible thermal electric film is prepared by depressurizing suction filtration.
2. the preparation method of the compound thermal electric film of macromolecule as described in claim 1, which is characterized in that include the following steps：
Step 1)：Prepare conductive polymer nanometer line solution：It, then will be conductive first by surfactant-dispersed to deionized water
Polymer monomer is added in surfactant solution, adds oxidant, and after being reacted by magnetic agitation, mixture is filtered
After being used in combination deionized water, organic solvent to clean 2~9 times in turn successively, dispersion is in organic solvent；
Step 2：Prepare conducting polymer/inorganic semiconductor mixed solution：By nanowire solution and one-dimensional inorganic semiconductor nano
Material mixes, and ultrasonic disperse is uniform；Wherein, the mass concentration of one-dimensional inorganic semiconductor nano material is 10~90%；
Step 3)：Prepare thermal electric film：Conducting polymer/inorganic semiconductor mixed solution is used very by sand core filter device
Empty pumping filter film forming filters and terminates to be placed on the drying 5~24 hours of 25~80 DEG C of vacuum drying oven.
3. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that led in the step 1)
Electric polymer monomer uses 3,4-ethylene dioxythiophene, aniline or pyrroles.
4. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that in the step 1)
Surfactant uses dodecyl sodium sulfate, cetyl trimethylammonium bromide, dodecyl trimethyl ammonium bromide or alkyl
Trimethylammonium bromide.
5. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that in the step 1)
Oxidant uses ferric trichloride, p-methyl benzenesulfonic acid iron or ammonium persulfate.
6. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that led in the step 1)
A concentration of 0~40mM of surfactant in electric polymer nanowire solution, a concentration of 5~30mM of conducting polymer monomer,
Oxidant concentration is 5~60mM.
7. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that in the step 1)
Cleaning uses any one or a few in ethyl alcohol, methanol and acetone with organic solvent；Dispersion is with organic solvent using ethyl alcohol, first
Alcohol or acetone.
8. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that one in the step 2)
It ties up inorganic semiconductor nanometer material and uses tellurium, semiconductor type carbon nano-tube or bismuth.
9. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that taken out in the step 3)
Filter uses aperture for 0.22 micron of nylon leaching film.
10. the preparation method of the compound thermal electric film of macromolecule as claimed in claim 2, which is characterized in that the step 3)
The film weight arrived is 10~90mg.
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Cited By (5)
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| CN109293962A (en) * | 2018-09-19 | 2019-02-01 | 同济大学 | A kind of preparation method of high thermoelectricity capability silver selenide/flexible nylon laminated film |
| CN110130096A (en) * | 2019-05-30 | 2019-08-16 | 上海应用技术大学 | A kind of preparation method of flexible fiber fabric composite thermoelectric material |
| CN110182767A (en) * | 2019-06-19 | 2019-08-30 | 江西科技师范大学 | A kind of preparation method of aciculiform tellurium nano pyroelectric material |
| CN111446355A (en) * | 2020-03-13 | 2020-07-24 | 东华大学 | Organic/inorganic composite thermoelectric fiber and preparation and application thereof |
| CN117402390A (en) * | 2023-12-14 | 2024-01-16 | 上海德赟电热材料科技有限公司 | Preparation method of carbon fiber and carbon nanotube based composite electric heating film and film thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293962A (en) * | 2018-09-19 | 2019-02-01 | 同济大学 | A kind of preparation method of high thermoelectricity capability silver selenide/flexible nylon laminated film |
| CN110130096A (en) * | 2019-05-30 | 2019-08-16 | 上海应用技术大学 | A kind of preparation method of flexible fiber fabric composite thermoelectric material |
| CN110182767A (en) * | 2019-06-19 | 2019-08-30 | 江西科技师范大学 | A kind of preparation method of aciculiform tellurium nano pyroelectric material |
| CN110182767B (en) * | 2019-06-19 | 2022-07-19 | 江西科技师范大学 | Preparation method of needle-shaped tellurium nano thermoelectric material |
| CN111446355A (en) * | 2020-03-13 | 2020-07-24 | 东华大学 | Organic/inorganic composite thermoelectric fiber and preparation and application thereof |
| CN117402390A (en) * | 2023-12-14 | 2024-01-16 | 上海德赟电热材料科技有限公司 | Preparation method of carbon fiber and carbon nanotube based composite electric heating film and film thereof |
| CN117402390B (en) * | 2023-12-14 | 2024-03-29 | 上海德赟电热材料科技有限公司 | Preparation method of carbon fiber and carbon nanotube based composite electric heating film and film thereof |
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Application publication date: 20180907 |