CN109301060A - A kind of preparation method of composite aerogel thermoelectric material - Google Patents
A kind of preparation method of composite aerogel thermoelectric material Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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Abstract
The present invention relates to a kind of preparation methods of composite aerogel thermoelectric material, which solve PEDOT and carbon material, inorganic material it is compound in caused by thermal conductivity increase, the technical issues of aeroge being made and whole conductivity decline, include the following steps: (1) by bacteria cellulose and EDOT monomer 1:(9~11 in mass ratio) it is mixed in aqueous solution, 1.35~3.51mmol Fe is added after being sufficiently stirred3+24~48h is sufficiently stirred in aqueous solution, is washed with HCL and deionized water, is made into composite material mixture；(2) solution obtained is mixed with the conductive nano filler of different proportion content, stirring, ultrasound, obtained solution freeze at -10~-50 DEG C, and then vacuum freeze drying obtains aeroge；(3) aeroge made from powder compressing machine processing step (2), obtains the BC-PEDOT multiple elements design sheet material of pore structure.The present invention is widely used in thermoelectric material preparation field.
Description
Technical field
The present invention relates to thermoelectric material field, specifically a kind of preparation method of composite aerogel thermoelectric material.
Background technique
Traditional non-renewable energy resources such as petroleum, coal traditional at present have been not enough to support the sustainable development of human society,
Furthermore with advocating environment protection, the cry of sustainable development is higher and higher, and the energy and material and device for developing novel environment friendly also become
Hot spot in scientific research.Thermoelectric material is a kind of material that can be realized thermal energy and electric energy and mutually convert, and thermoelectricity device is made
The advantages that part has small in size, noiseless in work, long service life, not will cause environmental pollution, only relying on the temperature difference can benefit
It is generated electricity with carrier moving.But current transformation efficiency is low, and the common place applied to some low suppling voltages uses, such as people
The power supply etc. of body wearable device.Traditional inorganic material bismuth telluride and its alloy, lead telluride and its alloy etc. are through research and development performance
On had a distinct increment, but content is relatively fewer on earth for this dvielement, and it is big not have a flexible and difficulty of processing, therefore
It is abundant to develop material, it is easy to process, there is high-performance Organic thermoelectric material flexible just to seem most important.
Organic thermoelectric material mostly uses conducting polymer, carbon nanotube and its composite material.PEDOT is current thermoelectricity capability
One of high conductive polymer material need to usually apply and flexible material is made on flexible substrates, and be at present raising
Seebeck coefficient prepares high performance thermoelectric material by composite carbon nanometer tube, inorganic nano material etc., but often this compound
The thermal conductivity of material can be improved.
To further decrease thermal conductivity, thermoelectricity capability is improved, there is research and establishment conductive network in recent years, realizes conductive network
In such a way that the line of micron even Nano grade or lamella are connected, filled between conductive network with air or insulating polymer.
This structure considerably reduces thermal conductivity.Wang et al. prepares tubular graphene alkene skeleton using template and then deposits polyphenyl
Amine prepares high-performance aeroge thermoelectric material.[Wang L,Bi H,Yao Q,et al.Three-dimensional
tubular graphene/polyaniline composites as high-performance elastic
thermoelectrics[J].Composites Science&Technology,2017, 150.135-140]。Shaobo
Han et al. uses PEDOT:PSS and cellulose to carry out being combined the gas that ultralight lower thermal conductivity has temperature sensitive pressure-sensitive dual sense
Gel thermoelectric material [Han S, Jiao F, Khan Z U, et al.Thermoelectric Polymer Aerogels for
Pressure– Temperature Sensing Applications[J].Advanced Functional Materials,
2017,27(44).1-7]。
But material prepared by this mode is since porosity height considerably reduces whole conductivity, and make aeroge
Whole thermoelectricity capability sharp fall.Therefore, in the case where guaranteeing lower thermal conductivity, it is most important to improve conductivity.
Summary of the invention
The present invention be exactly in order to solve PEDOT and carbon material, inorganic material it is compound in caused by thermal conductivity increase, gas is made
Gel again whole conductivity decline the problem of, it is polynary multiple to provide a kind of simple and effective PEDOT, bacteria cellulose, conductive filler
Close the preparation and processing method of aerogel material.
For this purpose, the present invention provides a kind of preparation methods of composite aerogel thermoelectric material comprising following steps:
(1) prepared by composite material mixture: by bacteria cellulose and EDOT monomer in mass ratio 1:
(9~11) mix in aqueous solution, and 1.35~3.51mmol Fe is added after being sufficiently stirred3+Aqueous solution is sufficiently stirred
24~48h is washed with HCL and deionized water, is made into composite material mixture；(2) preparation of aeroge: by the step (1)
In composite material mixture obtained mixed with the conductive nano filler of different proportion content, stirring, ultrasound, obtained solution
4h is freezed at -10~-50 DEG C, then vacuum freeze drying obtains aeroge；(3) processing of aeroge: powder compressing machine is used
Aeroge made from the step (2) is handled, the BC-PEDOT multiple elements design sheet material of pore structure is obtained.
Preferably, in step (1), composite material mixture can be carried out mixing system with PEDOT:PSS solution by BC solution
It is standby.
Preferably, the nm-class conducting wire filler in step (2) is single-walled carbon nanotube, double-walled carbon nano-tube, multi-wall carbon nano-tube
One of pipe, tellurium nano-wire are a variety of.
Preferably, pressure is 5~50MPa in step (3), and pressing time is 0.1~30min, and pressed temperature is 0~100
℃。
Helpfulness of the invention:
(1) present invention makees backing material using the bacteria cellulose itself with lower thermal conductivity and forms three-dimensional network skeleton,
In-situ polymerization is carried out with EDOT monomer or the conductive network that cladding forms a connection is carried out using PEDOT:PSS, and nanometer is added
Conductive filler forms another conductive network being connected to after reaching percolation threshold, while interface and conductive network joint are due to material
The difference of material can form energy filtering effect and improve Seebeck, and whole system constitutes biconnected network structure, form one
The thermoelectric material of P type.
(2) composite sheet of the invention carries out thermoelectricity capability test, by p-type sheet material prepared by the present invention and N-shaped sheet material according to
Thermo-electric device has just been made in secondary connect.Both ends keep the different temperatures temperature difference, carry out device performance test.
(3) present invention prepares biconnected porous sheet composite thermoelectric material using freeze-drying, has manufacture craft
It is simple and convenient, abundant raw material is cheap, environmental-friendly, product has the characteristics that preferable flexibility.
(4) present invention uses simple aeroge tabletting mode, and porosity remains to reach 40% or so after tabletting, makes
The conductivity of aeroge thermoelectricity increases substantially, and thermal conductivity rises less, further, since eliminating during vacuum freeze drying
Peroxidating phenomenon caused by oxygen in air, compared to vacuum filtration film forming the present invention made of sheet material Seebeck coefficient more
Height is a bit.
Detailed description of the invention
Fig. 1 a is the tearing section SEM figure of BC-PEDOT lamella composite thermoelectric material prepared by the embodiment of the present invention 1；
Fig. 1 b is the high power SEM figure of BC-PEDOT lamella composite thermoelectric material prepared by the embodiment of the present invention 1；
Fig. 1 c be the embodiment of the present invention 1 prepare BC/PEDOT aeroge pressurization at sheet material Seebeck coefficient at any time
Variation changes over time comparison diagram with the Seebeck coefficient that film is made is filtered.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies content described in example and is merely to illustrate the present invention, without this hair described in claims should will not be limited
It is bright.
Embodiment 1
(1) prepared by composite material mixture: the bacteria cellulose of 10ml (2mg/ml) being gone with 20ml deionized water dilute
It releases, is mixed in aqueous solution with 1.27mmolEDOT monomer later, nine water of 1.35mmol and nitric acid are added after being sufficiently stirred
The aqueous solution that iron and 3ml deionized water are made into, is sufficiently stirred for 24 hours, uses HCL (0.1mol/L) respectively, deionized water washing at least 3
It is secondary, finally it is made into the composite material mixture that concentration is 2mg/ml.
(2) preparation of aeroge: obtained solution carries out -50 DEG C and freezes 4 hours, then obtains within vacuum freeze drying 48 hours
To aeroge.
(3) processing of aeroge: with powder compressing machine in 5MPa, 50 DEG C of pushing 15min, the BC- of pore structure is obtained
PEDOT multiple elements design sheet material.
Embodiment 2
(1) prepared by composite material mixture: the bacteria cellulose of 10ml (2mg/ml) being gone with 20ml deionized water dilute
It releases, is mixed in aqueous solution with 1.27mmolEDOT monomer later, nine water of 1.35mmol and nitric acid are added after being sufficiently stirred
The aqueous solution that iron and 3ml deionized water are made into, is sufficiently stirred for 24 hours, uses HCL (0.1mol/L) respectively, deionized water washing at least 3
It is secondary, finally it is made into the composite material mixture that concentration is 2mg/ml.
(2) preparation of aeroge: (1) solution is mixed with the DWCNT of different proportion content, stirring, ultrasound.What is obtained is molten
Liquid carries out -10 DEG C and freezes 4 hours, then obtains aeroge within vacuum freeze drying 48 hours.
(3) processing of aeroge: with powder compressing machine in 50MPa, 0 DEG C of pushing 0.1min, the BC- of pore structure is obtained
PEDOT multiple elements design sheet material.
Embodiment 3
(1) prepared by composite material mixture: the bacteria cellulose of 10ml (2mg/ml) being gone with 20ml deionized water dilute
It releases, is mixed in aqueous solution with 1.41mmolEDOT monomer later, nine water of 2.43mmol and nitric acid are added after being sufficiently stirred
The aqueous solution that iron and 3ml deionized water are made into, is sufficiently stirred 36h, uses HCL (0.1mol/L) respectively, and deionized water 3 times, finally
It is made into the composite material mixture that concentration is 2mg/ml.
(2) preparation of aeroge: (1) solution is mixed with the MWNT of different proportion content, stirring, ultrasound.What is obtained is molten
Liquid carries out -30 DEG C and freezes 4 hours, then obtains aeroge within vacuum freeze drying 48 hours.
(3) processing of aeroge: with powder compressing machine in 25MPa, 50 DEG C of pushing 10min, the BC- of pore structure is obtained
PEDOT multiple elements design sheet material.
Embodiment 4
(1) prepared by composite material mixture: by the bacteria cellulose of 10ml (2mg/ml) and different proportion PEDOT:PSS
(PH1000) it is mixed, is sufficiently stirred.
(2) preparation of aeroge: obtained solution carries out -50 DEG C and freezes 4 hours, then obtains within vacuum freeze drying 48 hours
To aeroge.
(3) processing of aeroge: powder compressing machine 10MPa, 100 DEG C of pushing 0.1min are used, the BC- of pore structure is obtained
PEDOT multiple elements design sheet material.
Embodiment 5
(1) prepared by composite material mixture: the bacteria cellulose of 10ml (2mg/ml) being gone with 20ml deionized water dilute
Release, mixed in aqueous solution with 1.55mmolEDOT monomer later, after being sufficiently stirred be added 3.51mmol ferric trichloride with
48h is sufficiently stirred in the aqueous solution that 8ml deionized water is made into, and uses HCL (0.1mol/L) respectively, deionized water 3 times, is finally made into
Concentration is the composite material mixture of 2mg/ml.
(2) preparation of aeroge: (1) solution is mixed with the SWCNT of different proportion content, stirring, ultrasound.What is obtained is molten
Liquid carries out -30 DEG C and freezes 4 hours, then obtains aeroge within vacuum freeze drying 48 hours.
(3) processing of aeroge: with powder compressing machine in 5MPa, 100 DEG C of pushing 0.5min, the BC- of pore structure is obtained
PEDOT multiple elements design sheet material.
Embodiment 6
(1) prepared by composite material mixture: the bacteria cellulose of 10ml (2mg/ml) being gone with 20ml deionized water dilute
It releases, is mixed in aqueous solution with 1.55mmolEDOT monomer later, nine water of 3.51mmol and nitric acid are added after being sufficiently stirred
The aqueous solution that iron and 8ml deionized water are made into, is sufficiently stirred 48h, uses HCL (0.1mol/L) respectively, and deionized water 3 times, finally
It is made into the composite material mixture that concentration is 2mg/ml.
(2) preparation of aeroge: by the SWCNT and different proportion content tellurium nano-wire of (1) solution and certain proportion content
Mixing, stirring, ultrasound.Obtained solution carries out -50 DEG C and freezes 4 hours, then obtains aeroge within vacuum freeze drying 48 hours.
(3) processing of aeroge: powder compressing machine 25MPa, 50 DEG C of pushing 30min are used, the BC- of pore structure is obtained
PEDOT multiple elements design sheet material.
Comparative example
(1) prepared by composite material mixture: the bacteria cellulose of 10ml (2mg/ml) being gone with 20ml deionized water dilute
It releases, is mixed in aqueous solution with 1.27mmolEDOT monomer later, nine water of 1.35mmol and nitric acid are added after being sufficiently stirred
The aqueous solution that iron and 3ml deionized water are made into, prepares the sample of stirring 24,39,42,45,48h, with HCL (0.1mol/ respectively
L), deionized water is washed at least 3 times, is finally made into the composite material mixture that concentration is 2mg/ml.
(2) solution that (1) obtains is filtered by the way of vacuum decompression suction filtration on nanofiber filter membrane, then in room
It is dried to obtain the BC-PEDOT laminated film of self-supporting under temperature, as a comparison sample.
1 thin-film material performance parameter of table
Conclusion: comparative example is to use the BC-PEDOT solution for reacting 39h prepared simultaneously with the data of embodiment 1,
Aeroge tabletting method of the invention and traditional suction filtration method preparation gained is respectively adopted, it can be found that method system of the invention
The Seebeck coefficient obtained is higher, and thermal conductivity is lower, more advantageous to thermoelectricity capability.
Claims (4)
1. a kind of preparation method of composite aerogel thermoelectric material, it is characterized in that including the following steps:
(1) prepared by composite material mixture: by bacteria cellulose and EDOT monomer 1:(9~11 in mass ratio) it is mixed in aqueous solution
It closes, 1.35~3.51mmol Fe is added after being sufficiently stirred3+24~48h is sufficiently stirred in aqueous solution, is washed with HCL and deionization
It washs, is made into composite material mixture；
(2) preparation of aeroge: the nanometer of composite material mixture obtained in the step (1) and different proportion content is led
Electric filler mixing, stirring, ultrasound, obtained solution freeze at -10~-50 DEG C, and then vacuum freeze drying obtains aeroge；
(3) processing of aeroge: aeroge made from the step (2) is handled with powder compressing machine, obtains the BC- of pore structure
PEDOT multiple elements design sheet material.
2. the preparation method of composite aerogel thermoelectric material according to claim 1, which is characterized in that the step (1)
In, composite material mixture can be mixed with by BC solution and PEDOT:PSS solution.
3. the preparation method of composite aerogel thermoelectric material according to claim 1, which is characterized in that the step
(2) the nm-class conducting wire filler in is one of single-walled carbon nanotube, double-walled carbon nano-tube, multi-walled carbon nanotube, tellurium nano-wire
Or it is a variety of.
4. the preparation method of composite aerogel thermoelectric material according to claim 1, which is characterized in that the step
(3) pressure is 5~50MPa in, and pressing time is 0.1~30min, and pressed temperature is 0~100 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112002459A (en) * | 2020-08-07 | 2020-11-27 | 中国科学院理化技术研究所 | Flexible conductive material preparation method and flexible conductive material prepared by using same |
| CN115259166A (en) * | 2022-07-13 | 2022-11-01 | 武汉理工大学 | Super-soft conductive silicon aerogel, preparation method thereof and application thereof in sensor |
| CN115710137A (en) * | 2022-10-31 | 2023-02-24 | 西安建筑科技大学 | Calcium cobaltate thermoelectric ceramic with oriented micro-nano through holes and preparation method thereof |
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| CN102807357A (en) * | 2012-07-13 | 2012-12-05 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
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| CN107674421A (en) * | 2017-09-29 | 2018-02-09 | 江苏理工学院 | A kind of preparation method and applications of graphene/carbon nano-tube aerogel polymer conducing composite material |
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| CN102807357A (en) * | 2012-07-13 | 2012-12-05 | 中国科学院研究生院 | Block aerogel composite material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112002459A (en) * | 2020-08-07 | 2020-11-27 | 中国科学院理化技术研究所 | Flexible conductive material preparation method and flexible conductive material prepared by using same |
| CN115259166A (en) * | 2022-07-13 | 2022-11-01 | 武汉理工大学 | Super-soft conductive silicon aerogel, preparation method thereof and application thereof in sensor |
| CN115259166B (en) * | 2022-07-13 | 2024-01-16 | 武汉理工大学 | Super-flexible conductive silicon aerogel, preparation method thereof and application thereof in sensor |
| CN115710137A (en) * | 2022-10-31 | 2023-02-24 | 西安建筑科技大学 | Calcium cobaltate thermoelectric ceramic with oriented micro-nano through holes and preparation method thereof |
| CN115710137B (en) * | 2022-10-31 | 2023-05-12 | 西安建筑科技大学 | Calcium cobaltate thermoelectric ceramic with directional micro-nano through holes and preparation method thereof |
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