CN113707798B - RGO/Cu 1.75 Preparation method of Te nanowire composite flexible thermoelectric film - Google Patents
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- 239000002070 nanowire Substances 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 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 40
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000006185 dispersion Substances 0.000 claims abstract description 24
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 20
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 20
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 230000001568 sexual effect Effects 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000003828 vacuum filtration Methods 0.000 abstract description 4
- 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
- 238000000034 method Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002156 mixing 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
- 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
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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/Cu 1.75 The preparation method of the Te nanowire composite flexible thermoelectric film comprises the following steps: ascorbic acid, cetyltrimethylammonium bromide, GO dispersion and Na 2 TeO 3 Sequentially adding the solution into deionized water, stirring, heating for reaction under the condition of an oil bath, and naturally cooling to room temperature to obtain RGO/Te nanowire solution; cuSO is performed 4 Respectively dissolving ascorbic acid in deionized water, adding into RGO/Te nanowire solution for reaction, centrifuging, washing, dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion; RGO/Cu is taken 1.75 Te nanowire dispersion liquid is subjected to vacuum filtration to form a film, then cold pressing is carried out, and finally vacuum drying is carried out, thus obtaining RGO/Cu 1.75 Te nano-wire composite 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 a Reduced Graphene Oxide (RGO)/Cu 1.75 A 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 increasing demand for energy and the increasing depletion of non-renewable energy sources, thermoelectric materials have received increasing attention as an alternative potential solution. The energy conversion efficiency of a 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 absolute temperature; k is the thermal conductivity of the thermoelectric material. Bulk thermoelectric materials generally suffer from disadvantages such as high mass and rigidity, which limit their use on heat sources with uneven surfaces, while flexible thermoelectric materials avoid the disadvantages described above.
Currently flexible thermoelectric materials are based on organic thermoelectric materials, but they are unstable in air and have poor thermoelectric properties compared to inorganic thermoelectric materials. How to prepare inorganic thermoelectric materials into flexible thermoelectric films is a technical difficulty in the art. RGO has many excellent properties that can improve the flexibility and durability of the material. Cu (Cu) 1.75 Te has excellent conductivity and is expected to be applied to flexible thermoelectric materials. However, no effective method for preparing reduced graphene oxide/Cu exists at present 1.75 Te nano-wire composite flexible thermoelectric film.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: provide an RGO/Cu 1.75 A preparation method of Te nanowire composite flexible thermoelectric film.
In order to solve the technical problems, the invention provides an RGO/Cu 1.75 The 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 GO dispersion; ascorbic acid, cetyltrimethylammonium bromide, GO dispersion and Na 2 TeO 3 Sequentially adding the solution into deionized water, stirring, heating for reaction under the condition of an oil bath, and naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step 2): cuSO is performed 4 Respectively dissolving ascorbic acid in deionized water, sequentially adding into RGO/Te nanowire solution for reaction to obtain RGO/Cu 1.75 Te nanowire solution;
step 3): RGO/Cu 1.75 Centrifuging Te nanowire solution, adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion;
step 4): RGO/Cu is taken 1.75 Te nanowire dispersion liquid is subjected to vacuum filtration to form a film, then cold pressing is carried out, and finally vacuum drying is carried out, thus obtaining RGO/Cu 1.75 Te nano-wire composite flexible thermoelectric film.
Preferably, the RGO/Cu 1.75 The mass fraction of GO in the Te nanowire composite flexible thermoelectric film is 0.01-50%.
Preferably, in the step 1), ascorbic acid, cetyltrimethylammonium bromide and Na 2 TeO 3 The proportion of deionized water is 5g:0.5g:0.277g:50mL, and 3 volumes of deionized water were added after mixing.
Preferably, the temperature of the oil bath in the step 1) is 80-150 ℃ and the time is 5-48h.
Preferably, the CuSO in step 2) 4 The ratio of ascorbic acid to deionized water was 0.399g:5g:40mL of the volume ratio of the solution to RGO/Te nanowire solution is 1:5.
preferably, the temperature of the reaction in step 2) is 20-50 ℃ and the time is 1-7h.
Preferably, the rotational speed of the centrifugation in the step 3) is 6000 rpm and the time is 5min.
Preferably, the cold pressing pressure in the step 4) is 5-45MPa, the temperature is 10-20 ℃ and the time is 0.5-30min.
Preferably, the temperature of the vacuum drying in the step 4) is 60 ℃ and the time is 10 hours.
The invention synthesizes RGO/Cu in situ 1.75 Te nanowire composite material, and then preparing reduced graphene oxide/Cu through vacuum filtration and cold pressing treatment process 1.75 Te nano-wire composite flexible thermoelectric film. The preparation method is simple in process, and the prepared composite film has good flexibility and thermoelectric performance and has wide application prospect in the wearable field.
Drawings
FIG. 1 is a reduced graphene oxide/Cu prepared using example 2 1.75 SEM image of Te nanowire composite flexible thermoelectric film;
FIG. 2 is a reduced graphene oxide/Cu prepared using example 3 1.75 SEM image of Te nanowire composite flexible thermoelectric film.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Example 1
Reduced graphene oxide/Cu 1.75 The Te nanowire composite flexible thermoelectric film (the mass fraction of GO is 0.2 wt%) comprises the following steps:
step (1): and adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. Next, 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na 2 TeO 3 Sequentially adding the solution into 150mL of deionized water, carrying out oil bath reaction at 90 ℃ for 20 hours, and naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step (2): 0.399g of CuSO 4 And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, then are sequentially added into the RGO/Te nanowire solution, and are subjected to oil bath reaction at 40 ℃ for 3 hours to obtain RGO/Cu 1.75 Te nanowire solution;
step (3): RGO/Cu 1.75 Centrifuging Te nanowire solution (with the time of 5min and the rotating speed of 6000 rpm), adding deionized water and absolute ethyl alcohol, alternatively centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion;
step (4): taking a proper amount of RGO/Cu 1.75 Te nanowire dispersion liquid is filtered in vacuum to form a film, then the film is cold-pressed for 2min at the temperature of 15 ℃ under 35MPa, and finally the film is vacuum-dried for 10h at the temperature of 60 ℃ to obtain RGO/Cu 1.75 Te nano-wire composite flexible thermoelectric film.
Example 2
Reduced graphene oxide/Cu 1.75 The Te nanowire composite flexible thermoelectric film (the mass fraction of GO is 0.4 wt%) comprises the following steps:
step (1): and adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. Next, 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na 2 TeO 3 Sequentially adding the solution into 150mL of deionized water, carrying out oil bath reaction at 90 ℃ for 20 hours, and naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step (2):0.399g of CuSO 4 And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, then are sequentially added into the RGO/Te nanowire solution, and are subjected to oil bath reaction at 40 ℃ for 3 hours to obtain RGO/Cu 1.75 Te nanowire solution;
step (3): RGO/Cu 1.75 Centrifuging Te nanowire solution (with the time of 5min and the rotating speed of 6000 rpm), adding deionized water and absolute ethyl alcohol, alternatively centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion;
step (4): taking a proper amount of RGO/Cu 1.75 Te nanowire dispersion liquid is filtered in vacuum to form a film, then the film is cold-pressed for 2min at the temperature of 15 ℃ under 35MPa, and finally the film is vacuum-dried for 10h at the temperature of 60 ℃ to obtain RGO/Cu 1.75 Te nano-wire composite flexible thermoelectric film.
Example 3
Reduced graphene oxide/Cu 1.75 The Te nanowire composite flexible thermoelectric film (the mass fraction of GO is 1.0 wt%) comprises the following steps:
step (1): and adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. Next, 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na 2 TeO 3 Sequentially adding the solution into 150mL of deionized water, carrying out oil bath reaction at 90 ℃ for 20 hours, and naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step (2): 0.399g of CuSO 4 And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, then are sequentially added into the RGO/Te nanowire solution, and are subjected to oil bath reaction at 40 ℃ for 3 hours to obtain RGO/Cu 1.75 Te nanowire solution;
step (3): RGO/Cu 1.75 Centrifuging Te nanowire solution (with the time of 5min and the rotating speed of 6000 rpm), adding deionized water and absolute ethyl alcohol, alternatively centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion;
step (4): taking a proper amount of RGO/Cu 1.75 Te nanowire dispersion, film forming by vacuum filtration, and then film forming in 3Cold pressing at 15deg.C under 5MPa for 2min, and vacuum drying at 60deg.C for 10 hr to obtain RGO/Cu 1.75 Te nano-wire composite flexible thermoelectric film.
Example 4
Reduced graphene oxide/Cu 1.75 The Te nanowire composite flexible thermoelectric film (the mass fraction of GO is 50 wt%) comprises the following steps:
step (1): and adding a proper amount of ground GO into 50mL of deionized water, and performing ultrasonic dispersion. Next, 5g of ascorbic acid, 0.5g of cetyltrimethylammonium bromide, the GO dispersion described above and 0.277g of Na 2 TeO 3 Sequentially adding the solution into 150mL of deionized water, carrying out oil bath reaction at 150 ℃ for 48 hours, and naturally cooling to room temperature to obtain RGO/Te nanowire solution;
step (2): 0.399g of CuSO 4 And 5g of ascorbic acid are respectively dissolved in 40mL of deionized water, then are sequentially added into the RGO/Te nanowire solution, and are subjected to oil bath reaction at 50 ℃ for 7 hours to obtain RGO/Cu 1.75 Te nanowire solution;
step (3): RGO/Cu 1.75 Centrifuging Te nanowire solution (with the time of 5min and the rotating speed of 6000 rpm), adding deionized water and absolute ethyl alcohol, alternatively centrifuging and washing for 6 times, and dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion;
step (4): taking a proper amount of RGO/Cu 1.75 Te nanowire dispersion liquid is filtered in vacuum to form a film, then the film is cold-pressed for 30min at the temperature of 15 ℃ under 45MPa, and finally the film is vacuum-dried for 10h at the temperature of 60 ℃ to obtain RGO/Cu 1.75 Te nano-wire composite flexible thermoelectric film.
Claims (6)
1. RGO/Cu 1.75 The preparation method of the Te nanowire composite flexible thermoelectric film is characterized by comprising the following steps of:
step 1): adding the ground GO into deionized water, and performing ultrasonic dispersion to obtain GO dispersion; ascorbic acid, cetyltrimethylammonium bromide, GO dispersion and Na 2 TeO 3 Sequentially adding into deionized water, stirring, heating under oil bath, reacting, and naturally coolingCooling to room temperature to obtain RGO/Te nanowire solution; the ascorbic acid, cetyl trimethyl ammonium bromide and Na 2 TeO 3 The ratio of deionized water in the GO dispersion and the deionized water added for the second time was 5g:0.5g:0.277g:50mL:150mL;
step 2): cuSO is performed 4 Respectively dissolving ascorbic acid in deionized water, sequentially adding into RGO/Te nanowire solution for reaction to obtain RGO/Cu 1.75 Te nanowire solution; the CuSO 4 The proportion of deionized water dissolved therein was 0.399g:40mL, ratio of ascorbic acid to deionized water dissolved therein was 5g:40mL; ascorbic acid, cetyltrimethylammonium bromide, na in said step 1) 2 TeO 3 、CuSO 4 The proportion of ascorbic acid in step 2) was 5g:0.5g:0.277g:0.399g:5g;
step 3): RGO/Cu 1.75 Centrifuging Te nanowire solution, adding deionized water and absolute ethyl alcohol, alternately centrifuging and washing for 6 times, dispersing the product into absolute ethyl alcohol to obtain RGO/Cu 1.75 Te nanowire dispersion;
step 4): RGO/Cu is taken 1.75 Vacuum filtering Te nano-wire dispersion to form film, cold pressing at 5-45MPa and 10-20deg.C for 0.5-30min, and vacuum drying to obtain RGO/Cu 1.75 Te nano-wire composite flexible thermoelectric film.
2. The RGO/Cu of claim 1 1.75 The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the RGO/Cu 1.75 The mass fraction of GO in the Te nanowire composite flexible thermoelectric film is 0.01-50%.
3. The RGO/Cu of claim 1 1.75 The 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 5-48h.
4. The RGO/Cu of claim 1 1.75 Te nanowire composite flexibleThe preparation method of the sexual thermoelectric film is characterized in that the reaction temperature in the step 2) is 20-50 ℃ and the reaction time is 1-7h.
5. The RGO/Cu of claim 1 1.75 The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the centrifugal rotating speed in the step 3) is 6000 rpm, and the time is 5min.
6. The RGO/Cu of claim 1 1.75 The preparation method of the Te nanowire composite flexible thermoelectric film is characterized in that the vacuum drying temperature in the step 4) is 60 ℃ and the time is 10 hours.
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