CN105024007B - A kind of method prepared by thermoelectricity thick film - Google Patents
A kind of method prepared by thermoelectricity thick film Download PDFInfo
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- CN105024007B CN105024007B CN201510352375.9A CN201510352375A CN105024007B CN 105024007 B CN105024007 B CN 105024007B CN 201510352375 A CN201510352375 A CN 201510352375A CN 105024007 B CN105024007 B CN 105024007B
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- 230000005619 thermoelectricity Effects 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000012528 membrane Substances 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 20
- 229920000297 Rayon Polymers 0.000 claims abstract description 15
- 239000003292 glue Substances 0.000 claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000008187 granular material Substances 0.000 claims abstract description 8
- 239000010408 film Substances 0.000 claims description 78
- 230000000694 effects Effects 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000011889 copper foil Substances 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 229910002899 Bi2Te3 Inorganic materials 0.000 description 9
- 239000000956 alloy Substances 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- 238000005325 percolation Methods 0.000 description 5
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 5
- 239000004020 conductor Substances 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- 238000007639 printing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000001856 Ethyl cellulose Substances 0.000 description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 3
- 239000011231 conductive filler Substances 0.000 description 3
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- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 2
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- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The present invention relates to a kind of methods prepared by thermoelectricity thick film.The thermoelectricity thick film ink of the present invention is made of thermoelectric material particle, polymer and organic solvent, the polymer ratio that the present invention uses, it does not fall off voluntarily after only drying the thermoelectricity thick film ink being printed on flexible substrate, there is the one side of viscose glue closely to be covered using high-temperature resistant membrane after thermoelectricity thick film ink is fully dry, the thermoelectricity thick film of acquisition function admirable is handled by isostatic cool pressing.Since the ratio of Inventive polymers is only to make to be printed on the minimum ratio not fallen off voluntarily after the thermoelectricity thick film ink on flexible substrate is dried; attachment and molding of the thermoelectricity thick film on flexible substrate are handled by the high-temperature resistant membrane and isostatic cool pressing that closely cover to be obtained; thermoelectric granules are abundant and are closely contacted; the conductivity s close to bulk is not only obtained to improve its thermoelectricity capability; and due to the protection of high-temperature resistant membrane, even if thermoelectricity thick film works long hours in room temperature to 230oC is not easy to aoxidize.
Description
Technical field
The present invention relates to the technical field of material preparation, a kind of method prepared more particularly, to thermoelectricity thick film.
Background technology
The temperature difference is to determine the important parameter of thermopower generation efficiency, traditional bulk thermoelectric arm limited length, it is not easy to establish
The larger temperature difference, therefore the making of the membranaceous thermoelectric arm of strip is to improve the feasible method of thermopower generation efficiency.The preparation of conductor thick film
Method flexible design invests small, at low cost, dependable performance, has been used for that voltage is high, electric current is big, powerful occasion, is suitable for heat
The preparation of electric thick film.
Good thermoelectric material must have higher Seebeck coefficient S and conductivity s, to ensure have obvious thermoelectricity to imitate
It answers, while keeping the joule's heat energy of generation small.
Attachment and molding of the thermoelectricity thick film on substrate need use to have polymeric binder, the presence pair of polymeric matrix
Seebeck coefficient S influences less, but makes the reduction that contacts with each other between thermoelectricity thick film particle, and flow conductive decline, makes thermoelectricity thick film
Conductivity s decline 2~3 orders of magnitude, thermoelectricity capability is decreased obviously.
Invention content
The present invention is at least one defect overcome described in the above-mentioned prior art, provides a kind of side prepared by thermoelectricity thick film
Method can not only obtain the conductivity s of bulk to improve its thermoelectricity capability, even if but also thermoelectricity thick film work long hours in room
Temperature is not easy to aoxidize to 230 DEG C.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of method prepared by thermoelectricity thick film, thermoelectricity
Thick film ink is made of thermoelectric material particle, polymer and organic solvent, the polymer ratio that the present invention uses, and only makes to be printed on
It does not fall off voluntarily after thermoelectricity thick film ink drying on flexible substrate, thermoelectricity thick film ink uses high-temperature resistant membrane after fully drying
There is the one side of viscose glue closely to be covered, the thermoelectricity thick film for obtaining function admirable is handled by isostatic cool pressing, thermoelectric granules are abundant
And be closely contacted, obtain the conductivity s of bulk and protect thermoelectricity thick film work long hours room temperature to 230 DEG C it is not oxidizable
Effect.
The thermoelectric material particle is the good thermoelectricity of the near room temperatures thermoelectricity capability such as p-type or N-type Bi2Te3 based alloys
Material granule；The polymer is the polymer such as polystyrene or ethyl cellulose；The organic solvent is toluene, lemon
The organic solvents such as alkene, terpinol；The flexible substrate is that mica sheet etc. can bear isostatic pressing and thermal conductivity is low, high temperature resistant
Substrate；The printing is the printing processes such as mask printing, silk-screen printing, spraying, printing；The present invention uses poly-
Complex ratios are only to make to be printed on the minimum polymer ratio not fallen off voluntarily after the thermoelectricity thick film ink on flexible substrate is dried
Example；The high-temperature resistant membrane, which is Kapton films (Kapton) etc., can bear isostatic pressing and have viscose glue on one side
High-temperature resistant membrane；It is described there is the one side of viscose glue to carry out close covering using high-temperature resistant membrane to be high-temperature resistant membrane have the one of viscose glue
Face is covered towards thermoelectricity thick film, and cover after high-temperature resistant membrane without apparent bubble；The isostatic cool pressing processing is room
Make the isostatic pressed of 1MPa or more and pressurize 10 seconds or more under temperature to fully dry and closely covering high-temperature resistant membrane thermoelectricity thick film
Processing；The electrode is silver electrode being printed on flexible substrate etc. or is sticked to high-temperature resistant membrane and has the one side of viscose glue, then
The electrodes such as the copper foil, the silver foil that are covered towards thermoelectricity thick film.
The preparation method flexible design of conductor thick film invests small, at low cost, dependable performance, has been used for voltage height, electric current
Greatly, powerful occasion is suitable for the preparation of thermoelectricity thick film.Metallic is typically added in conductor thick film in a polymer matrix
It waits conductive fillers to prepare, realizes that conduction, electrical conduction mechanism can be solved with percolation is theoretical with tunneling effect by conductive filler
It releases：Percolation theory thinks, after the loading of conductive filler reaches percolation threshold value, is in the clipped wire of independent dispersion state originally
Son starts to contact with each other, and forms continuous network structure, makes the conductive energy of conductive thick film；And tunneling effect is then considered to gather
Close the insulating properties of object, it is believed that the organic film that one layer of insulation is covered on metallic only passes through grain between particle and particle
Tunneling effect between son, electronics could pass through insulating layer, achieve the effect that conduction.
The polymer ratio that the present invention uses, after only drying the thermoelectricity thick film ink being printed on flexible substrate not voluntarily
It falls off, there is the one side of viscose glue closely to be covered using high-temperature resistant membrane after thermoelectricity thick film ink is fully dry, it is quiet through being subcooled etc.
Pressure processing obtains the thermoelectricity thick film of function admirable.Under the double action that the ratio and isostatic cool pressing of polymer are handled, thermoelectricity
Grain is abundant and is closely contacted, and can increase substantially percolation conductive effect, the conductivity s of bulk be obtained, to improve it
Thermoelectricity capability is not easy to 230 DEG C even if thermoelectricity thick film works long hours in room temperature in addition, due to the protection of high-temperature resistant membrane
Oxidation.
The making of the membranaceous thermoelectric arm of strip is to improve the feasible method of thermopower generation efficiency, and the preparation method of conductor thick film is suitable
Preparation for thermoelectricity thick film.Attachment and molding of the thermoelectricity thick film on substrate need use to have polymeric binder, polymer
The presence of matrix influences less Seebeck coefficient S, but will make the reduction that contacts with each other between thermoelectricity thick film particle, keeps percolation conductive
Decline, the conductivity s of thermoelectricity thick film declines 2~3 orders of magnitude, and thermoelectricity capability is decreased obviously.
Compared with prior art, advantageous effect is：The polymer ratio that the present invention uses only makes to be printed on to be printed on electrode
It does not fall off voluntarily after thermoelectricity thick film ink drying on flexible substrate, thermoelectricity thick film ink uses high-temperature resistant membrane after fully drying
There is the one side of viscose glue closely to be covered, the thermoelectricity thick film for obtaining function admirable is handled by isostatic cool pressing.Since the present invention is poly-
The ratio for closing object is only to make to be printed on the minimum ratio not fallen off voluntarily after the thermoelectricity thick film ink on flexible substrate is dried, thermoelectricity
Attachment and molding of the thick film on flexible substrate are handled by the high-temperature resistant membrane and isostatic cool pressing that closely cover to be obtained, thermoelectric granules
It fully and is closely contacted, not only obtains the conductivity s of bulk to improve its thermoelectricity capability, but also due to high-temperature resistant membrane
Protection, be not easy to aoxidize to 230 DEG C in room temperature even if thermoelectricity thick film works long hours.
Description of the drawings
Fig. 1 is present invention process flow diagram.
Fig. 2 is p-type Bi2Te3 based alloys bar-shaped sample Seebeck coefficient S test data curves at room temperature.
Fig. 3 is p-type Bi2Te3 based alloys thermoelectricity thick film Seebeck coefficient S test data curves at room temperature.
Specific implementation mode
The attached figures are only used for illustrative purposes and cannot be understood as limitating the patent；It is attached in order to more preferably illustrate the present embodiment
Scheme certain components to have omission, zoom in or out, does not represent the size of actual product；To those skilled in the art,
The omitting of some known structures and their instructions in the attached drawings are understandable.Being given for example only property of position relationship described in attached drawing
Illustrate, should not be understood as the limitation to this patent.
Include flexible substrate 1, electrode 2, mask 3, thermoelectricity thickness as shown in Figure 1, for the process flow diagram of the present invention
Film 4, high-temperature resistant membrane 5.
Thermoelectric material particle, polymer and organic solvent are ground into the suitable thermoelectricity thick film ink of viscosity, wherein using
Polymer ratio, be only printed on using mask 3 after thermoelectricity thick film 4 on the flexible substrate 1 for being printed on electrode 2 is dried not from
Row falls off, and has the one side of viscose glue closely to be covered using high-temperature resistant membrane 5 after thermoelectricity thick film ink is fully dry, through being subcooled etc.
Static pressure processing obtains the thermoelectricity thick film of function admirable, and thermoelectric granules are abundant and are closely contacted, and obtain the conductivity s of bulk simultaneously
Thermoelectricity thick film is protected to work long hours in room temperature to 230 DEG C of not oxidizable effects.
Embodiment 1
Illustrate that the ratio of invention polymer is only to make the heat being printed on flexible substrate below by experiment
The minimum ratio not fallen off voluntarily after electric thick film ink drying, attachment and molding of the thermoelectricity thick film on flexible substrate are by closely covering
High-temperature resistant membrane and the isostatic cool pressing processing of lid obtain, and the conductivity s of bulk is not only obtained to improve it with the verification present invention
The advantages of thermoelectricity capability：
Include flexible substrate 1, electrode 2, mask 3, thermoelectricity thickness as shown in Figure 1, for the process flow diagram of the present invention
Film 4, high-temperature resistant membrane 5.
The length and width of p-type Bi2Te3 based alloy bar-shaped samples, thick respectively 29.3mm, 3.5mm and 2.1mm make at room temperature
With four-end method, the resistance for measuring sample with accurate LCR self-balancing bridge circuits with the AC signal of 60Hz calculates for 0.116 ohm
It is 343S/cm to obtain conductivity s；At room temperature, bar-shaped sample one end is heated with PTC heating plates, is measured with multiplex inspector
The potential difference DV at sample both ends is with the change procedure of temperature difference between the two ends DT, and slope is Seebeck coefficient S (as shown in Figure 2), by Fig. 2's
Data can obtain, and Seebeck coefficient S is 382mV/K, and it is 50mW/cm × K2 that power factor S2s, which is calculated,.
200 mesh sieve is crossed after p-type Bi2Te3 based alloy bar-shaped sample attrition grindings, mixed with ethyl cellulose and terpinol
It is ground into the suitable thermoelectricity thick film ink of viscosity, the wherein mass ratio of ethyl cellulose and p-type Bi2Te3 base alloy powders is
0.52%, using the film mask 3 that thickness is 0.10mm thickness, thermoelectricity thick film ink is printed on the mica-based for being printed on silver electrode 2
On piece 1, the thickness of mica substrate is 0.20mm, after removing mask 3, obtains molding thermoelectricity thick film 4, thermoelectricity thick film 4 is fully dry
It does not fall off voluntarily after dry, have viscose glue using heat safe Kapton (polyimides) film 5 one carries out tightly in face of thermoelectricity thick film 4
The thickness of close covering, Kapton (polyimides) film 5 is 0.055mm, then the isostatic cool pressing Jing Guo 10MPa pressurizes 1 minute
Processing, acquisition length and width, thickness (deducting mica substrate and Kapton film thicknesses) are respectively the P of 25.2mm, 4.0mm and 0.027mm
Type Bi2Te3 based alloy thermoelectricity thick films.At room temperature, using four-end method, believed with the exchange of 60Hz with accurate LCR self-balancing bridge circuits
The resistance for number measuring sample is 13.4 ohm, and it is 174S/cm that conductivity s, which is calculated,.Since thermoelectric granules are fully and close
Ground contacts, compared with p-type Bi2Te3 based alloy bar-shaped samples, the conductivity s only drop by half of thermoelectricity thick film.At room temperature, thermoelectricity
Thick film sample one end is heated with PTC heating plates, and the potential difference DV at sample both ends is measured with temperature difference between the two ends with multiplex inspector
The change procedure of DT, data and curves by the data of Fig. 3 as shown in figure 3, can be obtained, and Seebeck coefficient S is 385mV/K, with p-type
Bi2Te3 based alloy bar-shaped samples are compared, and the Seebeck coefficient S of thermoelectricity thick film is almost unchanged, and power factor S2s is calculated and is
26mW/cm×K2。
The polymer ratio that the present invention uses is can be seen that by above embodiment, only makes to be printed on to be printed on electrode
It does not fall off voluntarily after thermoelectricity thick film ink drying on flexible substrate, thermoelectricity thick film ink uses high-temperature resistant membrane after fully drying
There is the one side of viscose glue closely to be covered, the thermoelectricity thick film for obtaining function admirable is handled by isostatic cool pressing.In the ratio of polymer
Under the double action of example and isostatic cool pressing processing, thermoelectric granules are abundant and are closely contacted, and conductivity s is 174S/cm, thermoelectricity
Coefficient S is 385mV/K, and power factor S2s is 26mW/cm × K2, and thermoelectricity thick film prepared by the present invention obtains the conductivity of bulk
S has higher thermoelectricity capability.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
All any modification, equivalent and improvement etc., should be included in the claims in the present invention made by within the spirit and principle of invention
Protection domain within.
Claims (3)
1. a kind of method prepared by thermoelectricity thick film, which is characterized in that thermoelectricity thick film ink is by thermoelectric material particle, polymer and has
Solvent forms, and the mass ratio of the polymer and thermoelectric material that use is 0.52%, only makes to be printed on the flexible substrate for being printed on electrode
On the drying of thermoelectricity thick film ink after do not fall off voluntarily, have viscose glue using high-temperature resistant membrane after thermoelectricity thick film ink is fully dry
It is closely covered on one side, the thermoelectricity thick film for obtaining function admirable is handled by isostatic cool pressing, thermoelectric granules are fully and close
Ground contacts, and obtains the conductivity s of bulk and thermoelectricity thick film is protected to work long hours in room temperature to 230 DEG C of not oxidizable effects.
2. method prepared by a kind of thermoelectricity thick film according to claim 1, it is characterised in that：The use high temperature resistant is thin
Film has being covered towards thermoelectricity thick film when carrying out close covering to be high-temperature resistant membrane having viscose glue for viscose glue, and covers
High-temperature resistant membrane is without apparent bubble after lid.
3. method prepared by a kind of thermoelectricity thick film according to claim 1, it is characterised in that：The isostatic cool pressing processing
Be at room temperature to fully dry and closely covering high-temperature resistant membrane thermoelectricity thick film make 1MPa or more and pressurize 10 seconds or more etc.
Static pressure processing；The electrode is the silver electrode being printed on flexible substrate or is sticked to high-temperature resistant membrane and has the one side of viscose glue, so
Thermoelectric thick film is covered below copper foil, silver foil electrode.
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| CN201510352375.9A CN105024007B (en) | 2015-06-24 | 2015-06-24 | A kind of method prepared by thermoelectricity thick film |
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| CN201510352375.9A CN105024007B (en) | 2015-06-24 | 2015-06-24 | A kind of method prepared by thermoelectricity thick film |
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| CN105024007A CN105024007A (en) | 2015-11-04 |
| CN105024007B true CN105024007B (en) | 2018-09-25 |
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| CN105789425B (en) * | 2016-01-05 | 2019-01-18 | 中国科学院金属研究所 | A kind of cellulose paper/Bi2Te3Thermal electric film composite material and preparation method |
| CN106549096B (en) * | 2016-12-08 | 2019-03-26 | 苏州鸿凌达电子科技有限公司 | Thermoelectric film material and its manufacture craft |
| CN107377023B (en) * | 2017-09-08 | 2020-02-14 | 上海萃励电子科技有限公司 | Manufacturing method of temperature-controllable micro-fluidic chip |
| CN107732000B (en) * | 2017-10-23 | 2020-01-31 | 武汉理工大学 | Pressurizing device applied to thick film hot-pressing sintering, thermoelectric thick film and flexible thermoelectric device |
| CN113437208B (en) * | 2020-03-23 | 2023-12-26 | 中国科学院上海硅酸盐研究所 | Method for preparing thermoelectric thick film |
Citations (4)
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|---|---|---|---|---|
| CN102460754A (en) * | 2009-04-06 | 2012-05-16 | 3M创新有限公司 | Composite thermoelectric material and method for producing the same |
| CN102544348A (en) * | 2010-12-10 | 2012-07-04 | 原子能和代替能源委员会 | Deposition of thermoelectric materials by stamping |
| CN104115295A (en) * | 2012-02-24 | 2014-10-22 | 国立大学法人九州工业大学 | Thermoelectric conversion material |
| CN104538540A (en) * | 2015-01-16 | 2015-04-22 | 武汉大学 | Antimony telluride/poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) thermoelectric composite material and manufacturing method thereof |
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2015
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102460754A (en) * | 2009-04-06 | 2012-05-16 | 3M创新有限公司 | Composite thermoelectric material and method for producing the same |
| CN102544348A (en) * | 2010-12-10 | 2012-07-04 | 原子能和代替能源委员会 | Deposition of thermoelectric materials by stamping |
| CN104115295A (en) * | 2012-02-24 | 2014-10-22 | 国立大学法人九州工业大学 | Thermoelectric conversion material |
| CN104538540A (en) * | 2015-01-16 | 2015-04-22 | 武汉大学 | Antimony telluride/poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) thermoelectric composite material and manufacturing method thereof |
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