CN110171129A - A kind of preparation method of layered polymer base composite thermoelectric material - Google Patents
A kind of preparation method of layered polymer base composite thermoelectric material Download PDFInfo
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- CN110171129A CN110171129A CN201910460363.6A CN201910460363A CN110171129A CN 110171129 A CN110171129 A CN 110171129A CN 201910460363 A CN201910460363 A CN 201910460363A CN 110171129 A CN110171129 A CN 110171129A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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Abstract
The present invention is a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material.First passage solution 3D printing technique of the present invention prepares multilayer laminar polymer matrix composite thermoelectric material.A kind of polymer is added in solvent first, it stirs to it after completely dissolution, add a kind of inorganic material, continue to stir, until inorganic material is dispersed in the solution dissolved with polymer, then first layer polymer matrix composite thermoelectric material is printed by solution 3D printing technique, successively prints the second layer, third layer on the basis of the first layer material again later, until n-th layer polymer matrix composite thermoelectric material, ultimately forms the polymer matrix composite thermoelectric material of multilayer.The first layer that is printed, the second layer, third layer, until the composition of n-th layer polymer matrix composite thermoelectric material may be the same or different.The method have many advantages, such as simple process, it is easy to operate, be suitble to produce in enormous quantities.Prepared multilayer laminar polymer matrix composite thermoelectricity capability is excellent, and in thermoelectric power generation and refrigeration device field has broad application prospects and market value.
Description
Technical field
The invention belongs to field of thermoelectric material technique, a kind of multilayer laminar polymer matrix composite thermoelectric material is related generally to
Preparation method.
Background technique
Electric energy and modern people's life are closely bound up, and the supply of China's electric energy mostlys come from thermal power generation at present, this adds
The speed exhaustion of fossil energy, while also resulting in the serious pollution of environment.Thermoelectric material can pass through solid interior carrier
(electronics or hole) transports the mutual direct conversion realized between thermal energy and electric energy, is a kind of environmentally friendly function material
Material.
Thermo-electric device using inorganic thermoelectric material (such as bismuth telluride based alloys, telluride based alloys) preparation of tradition has
Matter is hard, is difficult to the disadvantages of being bent, and may be only available for the relatively flat heat source in surface, and in real life many heat sources surface
And out-of-flatness, such as: heat transfer pipe, therefore be badly in need of developing thermoelectric material flexible, to be provided to prepare flexible thermo-electric device
Raw material.Compared with the inorganic thermoelectric material of tradition, polymer matrix composite thermoelectric material have light, inexpensive, processing technology is simple,
The advantages that flexible, but its thermoelectricity capability is poor, the main reason is that compound using polymer matrix prepared by traditional handicraft
Thermoelectric material is easy to cause the oxidation of inorganic thermoelectric material (such as bismuth telluride based alloys, telluride based alloys) and in polymer
Disperse non-uniform problem (Du Y, et al.Research progress on polymer-inorganic in matrix
thermoelectric nanocomposite materials[J].Progress in Polymer Science,2012,
37:820)。
Solution 3D printing technique can be quick, direct and accurately converts mock-up for the drawing of three dimensional design,
It is applied in many fields.But up to now using solution 3D printing technique preparation polymer matrix composite thermoelectric material
Research has not been reported substantially, and it is that our team in 2018 by solution 3D printing technique are prepared for list that only research at present, which is reported,
Layer tungsten carbide/polylactic acid composite thermoelectric material (Du Y, et al.Flexible n-type tungsten carbide/
polylactic acid thermoelectric composites fabricated by additive
Manufacturing.Coatings, 2018,8:25), but the thermoelectricity capability of prepared polymer matrix composite is poor, compels
Be essential the thermoelectricity capability of polymer matrix composite to be improved, to meet the production needs of flexible thermo-electric device.
This patent first passage solution 3D printing technique is prepared for the polymer matrix composite thermoelectric material of multilayer, significantly mentions
The high thermoelectricity capability of material, provides the new thinking of one kind for the research and development of polymer matrix composite thermoelectric material.
Summary of the invention
In view of the deficiencies of the prior art, the present invention is prepared for the polymer matrix compound thermal of multilayer by solution 3D printing technique
Electric material.And it demonstrates more poly- than single layer prepared by same process using the multilayer laminar polymer matrix composite of this technique preparation
The thermoelectricity capability for closing object based composites is excellent.The method has many advantages, such as that preparation process is simple, is suitble to produce in enormous quantities, for height
The preparation of performance flexible polymer base composite thermoelectric material provides a kind of completely new technique.
The present invention provides a kind of preparation methods of multilayer laminar polymer matrix composite thermoelectric material, include the following steps:
1) a kind of polymer is added in solvent by the step of ingredient, and stirring after completely dissolution, adds one kind to it
Inorganic material continues to stir, until inorganic material is dispersed in the solution dissolved with polymer, prepares solution A；By
Two kinds of polymer are added in solvent, and stirring after completely dissolution, adds second of inorganic material, continue to stir to it, until nothing
Machine material is dispersed in solution, prepares solution B；It is similar with solution A and B, be prepared into respectively solution C, solution D, until
Solution N.
2) solution A is packed into machine, after adjusting parameter, prints the first layer material by the step of printing；
3) solution B is packed into machine, after adjusting parameter, prints the second layer material by the step of printing；
4) solution C is packed into machine, after adjusting parameter, prints third layer material by the step of possible printing；
5) the step of possible printing, it is similar with above-mentioned steps (2), (3), (4), solution N is packed into machine, adjustment
After parameter, n-th layer material is printed；
6) a dry step.
Further, the first layer of the multilayer laminar polymer matrix composite thermoelectric material, second layer, third layer, straight
Composition to n-th layer material may be the same or different.
Further, the lamellar composite thermoelectric material is two or more layers, and every layer with a thickness of 200nm-5mm.
Further, the polymer be conducting polymer (such as: polyaniline, polythiophene, polypyrrole, poly- 3,4- ethylene
One or more kinds of any combination of dioxy thiophene and their derivative etc.), non-conductive polymer (such as: polylactic acid, third
Alkene nitrile-butadiene-styrene copolymer, Kynoar, natural gum, butadiene-styrene rubber, butadiene rubber, isoprene rubber, neoprene rubber
The one or more kinds of of glue, butyl rubber, nitrile rubber, EP rubbers, fluorubber, acrylic rubber, silicon rubber etc. appoint
Meaning combination) or above-mentioned conducting polymer and non-conductive polymer any combination.
Further, the inorganic material is metal material (such as: silver, copper, aluminium, alloy), semiconductor material (Bi-
Te based alloy, Pb-Te based alloy, Sn-Se based alloy, tungsten carbide etc.), carbon material (carbon nanotube, graphene, carbon black, carbon quantum
Point) etc. one or more of materials any combination.
Further, each layer of the polymer and the mass ratio of inorganic material are 0.001-1.
Further, the solvent is any of the one or more of polar solvent, nonpolar solvent, acid, alkali etc.
Combination.
Further, the printing technology are as follows: solution 3D printing technique or the extrusion similar to solution 3D printing technique
Moulding process etc..
The present invention has the advantages that preparation process is simple, thermoelectricity capability is more preferable, can print material of various shapes,
Large-scale production easy to accomplish, prepared polymer matrix composite is in thermoelectric power generation and refrigeration and devices field application prospect
It is huge.
Detailed description of the invention
Fig. 1 uses the schematic diagram of two layers (a) and four layers of (b-d) polymer matrix composite thermoelectric material prepared by the present invention.
Bismuth telluride/silver/PLA composite thermoelectric material digital photograph that Fig. 2 uses embodiment 1 to prepare.
Bismuth telluride/silver/PLA composite thermoelectric material section field emission scanning electron microscope figure that Fig. 3 uses embodiment 1 to prepare
Piece.
Specific embodiment
Embodiment 1
(1) ingredient: polylactic acid is added in chloroform soln, and the mass volume ratio of polylactic acid and chloroform is
0.1g/mL stirs 2h with 100-400 revs/min of rate, after completely dissolution to it, adds bismuth telluride powder, polylactic acid with
The mass ratio of bismuth telluride powder is 0.25, continues to stir 1h with original rate, until bismuth telluride powder is dispersed in solution,
Obtain solution A；Polylactic acid is added in chloroform soln, the mass volume ratio of polylactic acid and chloroform is 0.1g/mL,
2h is stirred with 100-400 revs/min of rate, after completely dissolution to it, adds silver powder, the mass ratio of polylactic acid and silver powder is
0.2, continue to stir 1h with original rate, until silver powder is dispersed in solution, obtains solution B；
(2) dress sample printing: solution A is fitted into solution 3D printer and is printed；
(3) it prints the second layer: solution B is fitted into solution 3D printer, on the first layer side's printing second layer sample；
(4) dry: printed sample is put into natural air drying in electronic moisture-proof cabinet.
Embodiment 2
(1) ingredient: natural rubber is added in chloroform soln, the mass volume ratio of natural rubber and chloroform
For 0.02g/mL, 2h is stirred with 100-400 revs/min of rate, after completely dissolution to it, adds carbon black, natural rubber with
The mass ratio of carbon black is 0.1, continues to stir 1h with original rate, until hydrocarbon black powder is dispersed in solution, obtains solution
A；Polylactic acid is added in chloroform soln, the mass volume ratio of polylactic acid and chloroform is 0.1g/mL, with 100-
400 revs/min of rate stirs 2h, after completely dissolution to it, adds nickel powder, and the mass ratio of polylactic acid and nickel powder is 0.05,
Continue to stir 1h with original rate, until silver powder is dispersed in solution, obtains solution B；
(2) solution A is packed into machine, after adjusting parameter, prints the first layer material；
(3) solution B is packed into machine, after adjusting parameter, prints the second layer material；
(4) solution A is packed into machine, after adjusting parameter, prints third layer material；
(5) solution B is packed into machine, after adjusting parameter, prints the 4th layer material；
(6) dry: printed sample is put into natural air drying in electronic moisture-proof cabinet.
Embodiment 3
(1) ingredient: natural rubber is added in chloroform soln, the mass volume ratio of natural rubber and chloroform
For 0.02g/mL, 2h is stirred with 100-400 revs/min of rate, after completely dissolution to it, adds carbon black, natural rubber with
The mass ratio of carbon black is 0.01, continues to stir 1h with original rate, until hydrocarbon black powder is dispersed in solution, obtains solution
A；Polylactic acid is added in chloroform soln, the mass volume ratio of polylactic acid and chloroform is 0.1g/mL, with 100-
400 revs/min of rate stirs 2h, after completely dissolution to it, adds nickel powder, and the mass ratio of polylactic acid and nickel powder is 0.05,
Continue to stir 1h with original rate, until nickel powder is dispersed in solution, obtains solution B；By acrylonitrile-butadiene-benzene second
Alkene copolymer is added in chloroform soln, the mass volume ratio of acrylonitrile-butadiene-styrene copolymer and chloroform
For 0.15g/mL, bismuth telluride powder, propylene after completely dissolution to it are added with 100-400 revs/min of rate stirring 2h
The mass ratio of nitrile-butadiene-styrene copolymer and bismuth telluride powder is 0.01, continues to stir 1h with original rate, until tellurium
Change bismuth meal end to be dispersed in solution, obtains solution C；
(2) solution A is packed into machine, after adjusting parameter, prints the first layer material；
(3) solution B is packed into machine, after adjusting parameter, prints the second layer material；
(4) solution C is packed into machine, after adjusting parameter, prints third layer material；
(5) solution A is packed into machine, after adjusting parameter, prints the 4th layer material；
(6) dry: printed sample is put into natural air drying in electronic moisture-proof cabinet.
Embodiment 4
(1) ingredient: natural rubber is added in chloroform soln, the mass volume ratio of natural rubber and chloroform
For 0.02g/mL, 2h is stirred with 100-400 revs/min of rate, after completely dissolution to it, adds carbon black, natural rubber with
The mass ratio of carbon black is 0.5, continues to stir 1h with original rate, until hydrocarbon black powder is dispersed in solution, obtains solution
A；Polylactic acid is added in chloroform soln, the mass volume ratio of polylactic acid and chloroform is 0.1g/mL, with 100-
400 revs/min of rate stirs 2h, after completely dissolution to it, adds nickel powder, and the mass ratio of polylactic acid and nickel powder is 0.4, after
It is continuous that 1h is stirred with original rate, until nickel powder is dispersed in solution, obtain solution B；By acrylonitrile-butadiene-styrene (ABS)
Copolymer is added in chloroform soln, and the mass volume ratio of acrylonitrile-butadiene-styrene copolymer and chloroform is
0.15g/mL after completely dissolution to it adds bismuth telluride powder, acrylonitrile-with 100-400 revs/min of rate stirring 2h
The mass ratio of butadiene-styrene copolymer and bismuth telluride powder is 0.8, continues to stir 1h with original rate, until bismuth telluride
Powder is dispersed in solution, obtains solution C；Natural rubber is added in chloroform soln, natural rubber and trichlorine
The mass volume ratio of methane is 0.02g/mL, after completely dissolution to it is added with 100-400 revs/min of rate stirring 2h
The mass ratio of copper powder, natural rubber and copper powder is 0.7, continues to stir 1h with original rate, until copper powder is dispersed in solution
In, obtain solution D；
(2) solution A is packed into machine, after adjusting parameter, prints the first layer material；
(3) solution B is packed into machine, after adjusting parameter, prints the second layer material；
(4) solution C is packed into machine, after adjusting parameter, prints third layer material；
(5) solution D is packed into machine, after adjusting parameter, prints the 4th layer material；
(6) dry: printed sample is put into natural air drying in electronic moisture-proof cabinet.
Claims (8)
1. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material, it is characterised in that comprising steps of
(1) ingredient: a kind of polymer is added in solvent, and stirring after completely dissolution, adds a kind of inorganic material to it, is continued
Stirring prepares solution A until inorganic material is dispersed in the solution dissolved with polymer；By second polymer plus
Into solvent, stirring after completely dissolution, adds second of inorganic material, continues to stir to it, until inorganic material is uniformly divided
It is dispersed in solution, prepares solution B；It is similar with solution A and B, it is prepared into solution C, solution D respectively, until solution N；
(2) solution A is packed into machine, after adjusting parameter, prints the first layer material；
(3) solution B is packed into machine, after adjusting parameter, prints the second layer material；
(4) solution C is packed into machine, after adjusting parameter, prints third layer material；
(5) similar with above-mentioned steps (2), (3), (4), solution N is packed into machine, after adjusting parameter, prints n-th layer material；
(6) sample drying.
2. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: the first layer that is printed, the second layer, third layer, until the composition of n-th layer polymer matrix composite thermoelectric material can be identical,
It can also be different.
3. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: layered composite thermoelectric material is two or more layers, and every layer with a thickness of 200nm-5mm.
4. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: the polymer be conducting polymer (such as: polyaniline, polythiophene, polypyrrole, poly- 3,4- ethylenedioxy thiophene and they
Derivative etc. one or more kinds of any combination), non-conductive polymer (such as: polylactic acid, acrylonitrile-butadiene-benzene second
Alkene copolymer, Kynoar, natural gum, butadiene-styrene rubber, butadiene rubber, isoprene rubber, neoprene, butyl rubber, butyronitrile
One or more kinds of any combination of rubber, EP rubbers, fluorubber, acrylic rubber, silicon rubber etc.) or above-mentioned lead
Any combination of electric polymer and non-conductive polymer.
5. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: the inorganic material is metal material (such as: silver, copper, aluminium, alloy), semiconductor material (Bi-Te based alloy, Pb-Te
Based alloy, Sn-Se based alloy, tungsten carbide etc.), in the materials such as carbon material (carbon nanotube, graphene, carbon black, carbon quantum dot)
One or more kinds of any combination.
6. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: the mass ratio of each layer of the polymer and inorganic material is 0.001-1.
7. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: the solvent is one or more kinds of any combination of polar solvent, nonpolar solvent, acid, alkali etc..
8. a kind of preparation method of multilayer laminar polymer matrix composite thermoelectric material according to claim 1, feature exist
In: the printing technology are as follows: solution 3D printing technique or the extrusion molding process etc. similar to solution 3D printing technique.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111319256A (en) * | 2020-04-07 | 2020-06-23 | 常州大学 | Method for directly manufacturing organic polymer PTC thermosensitive device through 3D printing |
| CN113571698A (en) * | 2021-09-23 | 2021-10-29 | 中南大学 | Carbon point regulated metal selenide/carbon composite material and preparation method and application thereof |
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| CN107634137A (en) * | 2017-08-28 | 2018-01-26 | 上海应用技术大学 | A kind of preparation method of polymer matrix composite thermoelectric material |
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| CN111319256A (en) * | 2020-04-07 | 2020-06-23 | 常州大学 | Method for directly manufacturing organic polymer PTC thermosensitive device through 3D printing |
| CN113571698A (en) * | 2021-09-23 | 2021-10-29 | 中南大学 | Carbon point regulated metal selenide/carbon composite material and preparation method and application thereof |
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Application publication date: 20190827 |