CN113707798A - RGO/Cu1.75Preparation method of Te nanowire composite flexible thermoelectric film - Google Patents
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- 239000002070 nanowire Substances 0.000 title claims abstract description 75
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 32
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 18
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 16
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 229910004273 TeO3 Inorganic materials 0.000 claims abstract description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000003825 pressing Methods 0.000 claims description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- FXXMDJFRMDVSCF-RXSVEWSESA-N (2r)-2-[(1s)-1,2-dihydroxyethyl]-3,4-dihydroxy-2h-furan-5-one;hydrate Chemical compound O.OC[C@H](O)[C@H]1OC(=O)C(O)=C1O FXXMDJFRMDVSCF-RXSVEWSESA-N 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 27
- 239000010409 thin film Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910021389 graphene Inorganic materials 0.000 description 9
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/01—Manufacture or treatment
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- H—ELECTRICITY
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- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/852—Thermoelectric active materials comprising inorganic compositions comprising tellurium, selenium or sulfur
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
- H10N10/80—Constructional details
- H10N10/85—Thermoelectric active materials
- H10N10/851—Thermoelectric active materials comprising inorganic compositions
- H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
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Abstract
The invention discloses an RGO/Cu1.75The preparation method of the Te nanowire composite flexible thermoelectric thin film comprises the following steps: mixing ascorbic acid, cetyl trimethyl ammonium bromide, GO dispersion and Na2TeO3Sequentially adding the mixture into deionized water, heating and reacting under the condition of oil bath after stirring, and then naturally cooling to room temperature to obtain RGO/Te nanowire solution; mixing CuSO4And ascorbic acid are respectively dissolved in deionized water, then added into RGO/Te nanowire solution for reaction, centrifuged and washed, and the product is dispersed into absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion; taking RGO/Cu1.75Forming Te nanowire dispersion into film by vacuum filtration, and then cold pressingThen vacuum drying to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film. The composite thermoelectric film prepared by the invention has good flexibility and has a certain application prospect in the field of wearable thermoelectric.
Description
Technical Field
The invention relates to Reduced Graphene Oxide (RGO)/Cu1.75A preparation method of a Te nanowire composite flexible thermoelectric film belongs to the technical field of flexible composite thermoelectric materials.
Background
In recent years, with the increase in energy demand and the increasing depletion of non-renewable energy sources, thermoelectric materials have received increasing attention as an alternative potential. The energy conversion efficiency of the thermoelectric material is represented by a dimensionless thermoelectric figure of merit (ZT), which is expressed as follows:
wherein: s is the Seebeck coefficient of the thermoelectric material; σ is the electrical conductivity of the thermoelectric material; t is the absolute temperature; k is the thermal conductivity of the thermoelectric material. Bulk thermoelectric materials typically suffer from drawbacks such as heavy weight, high stiffness, etc., which limit their use on heat sources with uneven surfaces, while flexible thermoelectric materials avoid the above drawbacks.
At present, the flexible thermoelectric material is mainly an organic thermoelectric material, but is unstable in air, and the thermoelectric performance is also poor compared with an inorganic thermoelectric material. How to prepare inorganic thermoelectric materials into flexible thermoelectric thin films is a technical difficulty in the art. RGO has many excellent properties that can improve the flexibility and durability of the material. Cu1.75Te has excellent conductivity and is expected to be applied to flexible thermoelectric materials. However, at present, no effective method for preparing reduced graphene oxide/Cu exists1.75The Te nanowire is compounded with the flexible thermoelectric film.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: providing an RGO/Cu1.75A preparation method of a Te nanowire composite flexible thermoelectric film.
In order to solve the technical problem, the invention provides RGO/Cu1.75The preparation method of the Te nanowire composite flexible thermoelectric film comprises the following steps:
step 1): adding the ground GO into deionized water, and performing ultrasonic dispersion to obtain a GO dispersion liquid; mixing ascorbic acid, cetyl trimethyl ammonium bromide, GO dispersion and Na2TeO3Sequentially adding into deionized water, stirring, heating in oil bathReacting, and naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step 2): mixing CuSO4And ascorbic acid are respectively dissolved in deionized water, and then are sequentially added into RGO/Te nanowire solution for reaction to obtain RGO/Cu1.75A Te nanowire solution;
step 3): mixing RGO/Cu1.75Centrifuging the Te nanowire solution, adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, dispersing the product into the absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion;
step 4): taking RGO/Cu1.75Forming a film by using Te nanowire dispersion through vacuum filtration, then cold pressing, and finally drying in vacuum to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film.
Preferably, the RGO/Cu1.75The mass fraction of GO in the Te nanowire composite flexible thermoelectric film is 0.01-50%.
Preferably, ascorbic acid, cetyltrimethylammonium bromide, Na in step 1)2TeO3The ratio to deionized water was 5 g: 0.5 g: 0.277 g: 50mL of deionized water was added after mixing in a volume of 3 times.
Preferably, the temperature of the oil bath in the step 1) is 80-150 ℃ and the time is 5-48 h.
Preferably, the CuSO in step 2)4Ascorbic acid and deionized water in a ratio of 0.399 g: 5 g: 40mL, and the volume ratio of the solution to the RGO/Te nanowire solution is 1: 5.
preferably, the reaction temperature in the step 2) is 20-50 ℃ and the reaction time is 1-7 h.
Preferably, the rotation speed of the centrifugation in the step 3) is 6000 rpm, and the time is 5 min.
Preferably, the pressure of the cold pressing in the step 4) is 5-45MPa, the temperature is 10-20 ℃, and the time is 0.5-30 min.
Preferably, the temperature of the vacuum drying in the step 4) is 60 ℃ and the time is 10 h.
The invention synthesizes RGO/Cu in situ1.75Te nanowire composite material, then passingReduced graphene oxide/Cu is prepared by vacuum filtration combined cold pressing treatment process1.75The Te nanowire is compounded with the flexible thermoelectric film. The preparation method is simple in process, and the prepared composite film has good flexibility and thermoelectric property and has wide application prospect in the wearable field.
Drawings
FIG. 1 shows the reduced graphene oxide/Cu prepared in example 21.75SEM picture of Te nanowire composite flexible thermoelectric film;
FIG. 2 shows the reduced graphene oxide/Cu prepared in example 31.75SEM image of Te nanowire composite flexible thermoelectric film.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Reduced graphene oxide/Cu1.75The Te nanowire composite flexible thermoelectric thin film (GO is 0.2wt percent) comprises the following steps:
step (1): adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na are then added2TeO3Sequentially adding the obtained mixture into 150mL of deionized water, carrying out oil bath reaction at 90 ℃ for 20h, and naturally cooling to room temperature to obtain an RGO/Te nanowire solution;
step (2): 0.399g of CuSO4And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, and then are sequentially added into the RGO/Te nanowire solution, and the RGO/Cu is obtained after the reaction of the mixture in oil bath at 40 ℃ for 3 hours1.75A Te nanowire solution;
and (3): mixing RGO/Cu1.75Centrifuging the Te nanowire solution (5 min at 6000 rpm), adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion;
and (4): taking a proper amount of RGO/Cu1.75Forming a film of Te nanowire dispersion by vacuum filtration, and thenCold pressing the film at 35MPa and 15 deg.C for 2min, and vacuum drying at 60 deg.C for 10 hr to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film.
Example 2
Reduced graphene oxide/Cu1.75The Te nanowire composite flexible thermoelectric thin film (GO is 0.4 wt%) comprises the following steps:
step (1): adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na are then added2TeO3Sequentially adding the obtained mixture into 150mL of deionized water, carrying out oil bath reaction at 90 ℃ for 20h, and naturally cooling to room temperature to obtain an RGO/Te nanowire solution;
step (2): 0.399g of CuSO4And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, and then are sequentially added into the RGO/Te nanowire solution, and the RGO/Cu is obtained after the reaction of the mixture in oil bath at 40 ℃ for 3 hours1.75A Te nanowire solution;
and (3): mixing RGO/Cu1.75Centrifuging the Te nanowire solution (5 min at 6000 rpm), adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion;
and (4): taking a proper amount of RGO/Cu1.75Forming a film by vacuum filtration of the Te nanowire dispersion, then cold-pressing the film at 35MPa and 15 ℃ for 2min, and finally vacuum-drying at the temperature of 60 ℃ for 10h to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film.
Example 3
Reduced graphene oxide/Cu1.75The Te nanowire composite flexible thermoelectric thin film (GO is 1.0 wt%) comprises the following steps:
step (1): adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na are then added2TeO3Sequentially adding into 150mL of deionized water, and carrying out oil bath at 90 DEG CNaturally cooling to room temperature after 20h to obtain RGO/Te nanowire solution;
step (2): 0.399g of CuSO4And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, and then are sequentially added into the RGO/Te nanowire solution, and the RGO/Cu is obtained after the reaction of the mixture in oil bath at 40 ℃ for 3 hours1.75A Te nanowire solution;
and (3): mixing RGO/Cu1.75Centrifuging the Te nanowire solution (5 min at 6000 rpm), adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion;
and (4): taking a proper amount of RGO/Cu1.75Forming a film by vacuum filtration of the Te nanowire dispersion, then cold-pressing the film at 35MPa and 15 ℃ for 2min, and finally vacuum-drying at the temperature of 60 ℃ for 10h to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film.
Example 4
Reduced graphene oxide/Cu1.75The Te nanowire composite flexible thermoelectric thin film (GO is 50wt percent) comprises the following steps:
step (1): adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na are then added2TeO3Sequentially adding the obtained mixture into 150mL of deionized water, carrying out oil bath reaction at 150 ℃ for 48h, and naturally cooling to room temperature to obtain an RGO/Te nanowire solution;
step (2): 0.399g of CuSO4And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, and then are sequentially added into the RGO/Te nanowire solution, and the RGO/Cu is obtained after the reaction for 7 hours in an oil bath at 50 DEG C1.75A Te nanowire solution;
and (3): mixing RGO/Cu1.75Centrifuging the Te nanowire solution (5 min at 6000 rpm), adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion;
and (4): taking a proper amount of RGO/Cu1.75Forming a film by vacuum filtration of the Te nanowire dispersion, then cold-pressing the film at 15 ℃ under 45MPa for 30min, and finally vacuum-drying at 60 ℃ for 10h to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film.
Claims (9)
1. RGO/Cu1.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized by comprising the following steps:
step 1): adding the ground GO into deionized water, and performing ultrasonic dispersion to obtain a GO dispersion liquid; mixing ascorbic acid, cetyl trimethyl ammonium bromide, GO dispersion and Na2TeO3Sequentially adding the mixture into deionized water, heating and reacting under the condition of oil bath after stirring, and then naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step 2): mixing CuSO4And ascorbic acid are respectively dissolved in deionized water, and then are sequentially added into RGO/Te nanowire solution for reaction to obtain RGO/Cu1.75A Te nanowire solution;
step 3): mixing RGO/Cu1.75Centrifuging the Te nanowire solution, adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, dispersing the product into the absolute ethyl alcohol to obtain RGO/Cu1.75A Te nanowire dispersion;
step 4): taking RGO/Cu1.75Forming a film by using Te nanowire dispersion through vacuum filtration, then cold pressing, and finally drying in vacuum to obtain RGO/Cu1.75The Te nanowire is compounded with the flexible thermoelectric film.
2. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the RGO/Cu1.75The mass fraction of GO in the Te nanowire composite flexible thermoelectric film is 0.01-50%.
3. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that ascorbic acid and hexadecyl trimethyl are adopted in the step 1)Ammonium bromide, Na2TeO3The ratio to deionized water was 5 g: 0.5 g: 0.277 g: 50mL of deionized water was added after mixing in a volume of 3 times.
4. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the temperature of the oil bath in the step 1) is 80-150 ℃, and the time is 5-48 h.
5. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that CuSO in the step 2)4Ascorbic acid and deionized water in a ratio of 0.399 g: 5 g: 40mL, and the volume ratio of the solution to the RGO/Te nanowire solution is 1: 5.
6. the RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the reaction temperature in the step 2) is 20-50 ℃ and the reaction time is 1-7 h.
7. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the rotation speed of centrifugation in the step 3) is 6000 rpm, and the time is 5 min.
8. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the pressure of cold pressing in the step 4) is 5-45MPa, the temperature is 10-20 ℃, and the time is 0.5-30 min.
9. The RGO/Cu of claim 11.75The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the temperature of vacuum drying in the step 4) is 60 ℃, and the time is 10 hours.
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| Title |
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