CN105633266A - Preparation method for composite thermoelectric film with flexible reduced graphene oxide and tellurium nano wires - Google Patents
Preparation method for composite thermoelectric film with flexible reduced graphene oxide and tellurium nano wires Download PDFInfo
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- CN105633266A CN105633266A CN201511023207.1A CN201511023207A CN105633266A CN 105633266 A CN105633266 A CN 105633266A CN 201511023207 A CN201511023207 A CN 201511023207A CN 105633266 A CN105633266 A CN 105633266A
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Abstract
The invention relates to a preparation method for a composite thermoelectric film with flexible reduced graphene oxide (RGO)and tellurium nano wires (Te NWs). The preparation method comprises: reducing preparation is carried out by using oxidized graphene (GO) powder and sodium polystyrene sulfonate (NaPSS) as raw materials according to a hydrothermal method to obtain RGO that can be dispersed in water; reducing preparation is carried out by using sodium tellurite (Na2TeO3) as a raw material and hydrazine hydrate (N2H4.H2O) as a reducing agent according to a hydrothermal method to obtain TeNWs that can be dispersed in watewr; after a certain number of RGO and Na2TeO3 materials are dispersed in water ultrasonically, RGO dispersion liquid and Te NWs dispersion liquid drip on a flexible glass fiber film successively with assistance of vacuum filtration and the glass fiber film is dried in a vacuum environment; annealing is carried out on the glass fiber covered with a composite film at a mixed atmosphere of Ar and H2 under the temperature of 200 DEG C for some time to obtain a composite thermoelectric film with the RGO and Te NWs. The provided preparation method has characteristics of simple and easily controlled process, short reaction time, low energy consumption, high security, good pollution-free performance, and excellent flexible film thermoelectric property and the like.
Description
Technical field
The invention belongs to novel energy resource material technology field, it is specifically related to the preparation method of a kind of flexible reduced graphene and tellurium nano-wire compound thermal conductive film.
Background technology
Thermoelectric material can realize heat energy and material that electric energy is directly changed mutually, based on thermoelectric power generation device and the refrigeration device of thermoelectric material, there is compact equipment, when running without features such as noise, the discarded energy of pollution-free, recoverable, all have broad application prospects in fields such as military affairs, medical science, space flight, microelectronics and even household electrical appliance. Flexible thermal electric material compares business-like block thermoelectric material, have can bend, preparation cost is low, technique is simple, the unique advantage such as applied widely, has attracted the more and more concern of scientific research circle and enterprise circle in recent years.
Reduced graphene has higher carrier concentration and carrier mobility, dispersibles in water after tensio-active agent processes, and is suitable for preparation flexible thermal electric material. But owing to the electronics of reduced graphene and the mobility in hole are almost identical, cause its Seebeck coefficient very low. Many results of study show, energy filtering effect in composite thermoelectric material and interface scattering can reduce the thermal conductivity of material effectively, simultaneously when keeping specific conductivity constant, it is to increase the Seebeck coefficient of material so that the ZT value of material increases significantly. By regulating the reducing degree of reduced graphene can regulate and control work function and the electronic structure of reduced graphene so that it is compound effectively can be carried out with various semiconductor material. But so far, based on the block materials that the composite thermoelectric material of reduced graphene is all made up of conducting polymer or inorganic semiconductor and reduced graphene simple composite, do not realize effective coupling of plural components, have Seebeck coefficient lower, Applicable temperature scope is narrower, without shortcomings such as flexibilities.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of flexible reduced graphene and tellurium nano-wire compound thermal conductive film, the method technique is simple, and preparation cycle is short, and the thin film thermoelectric performance obtained is good.
In order to realize above-mentioned purpose, the present invention by the following technical solutions:
A preparation method for flexible reduced graphene and tellurium nano-wire compound thermal conductive film, comprises the following steps:
(1) by a certain amount of graphene oxide and tensio-active agent ultrasonic disperse in water, then adding the acid of 24 times of dispersion liquids in dispersion liquid, mixed solution hydro-thermal reaction at 120 150 DEG C is taken out filter after naturally cooling in 26 hours and is precipitated;
(2) precipitate with deionized water obtained in step (1) is washed till neutrality, is deposited at 60 DEG C vacuum-drying and obtains for 35 hours the reduced graphene dispersibled;
(3) by sodium tellurite and complexing agent stirring and dissolving in water, then adding the ammoniacal liquor of 25% and the hydrazine hydrate of 98% in previous solu, mixed solution cools after hydro-thermal reaction certain time at 180 DEG C;
(4) liquid obtained in step (3) adds a certain amount of acetone and obtains flocks, after centrifugal, abandon the tellurium nano-wire that supernatant liquid obtains dispersibling;
(5) certain density reduced graphene and tellurium nano-wire dispersion liquid is configured respectively;
(6) under vacuum filtration is auxiliary, a certain amount of reduced graphene dispersant liquid drop is coated in the flexible substrates of certain area size, liquid is drained;
(7) under vacuum filtration is auxiliary, the region being coated in step (6) by a certain amount of tellurium nano-wire dispersant liquid drop reduced graphene and covering, drains liquid;
(8) step (7) will be coated with flexible substrates vacuum drying at 30 60 DEG C of laminated film;
(9) glass fibre membrane being coated with laminated film in step (8) is transferred in tube furnace, at Ar/H2Mixed atmosphere (hydrogen content 8%) is annealed certain time at 200 DEG C.
Tensio-active agent used is polystyrene sodium sulfonate (NaPSS), and acid used is Hydrogen bromide or hydroiodic acid HI, and graphene oxide used and sodium polystyrene sulfonate mass ratio are 2:1 1:2;
The hydro-thermal reaction time preparing tellurium nano-wire is 1.5 3 hours, and the type of cooling is water-cooled;
The volume ratio of acetone used and hydro-thermal reaction mixed solution is 24;
Flexible substrates used is glass fibre membrane stable at normal temperature to 500 DEG C;
The concentration of described reduced graphene is 1mg/ml; Tellurium nano-wire is 2mg/ml.
0.15 0.5mg/cm is measured in the painting of dripping of described reduced graphene2, 0.1 2mg/cm is measured in the painting of dripping of tellurium nano-wire2;
Annealing atmosphere is Ar/H2, annealing time is 0.5 2 hours.
The invention has the beneficial effects as follows: reduced graphene can be dispersed in water to make to add sodium polystyrene sulfonate, such that it is able to reduced graphene and tellurium nano-wire are made dispersion liquid; By control reduced graphene and the hydrothermal synthesizing condition of tellurium nano-wire, regulate and control reduced graphene and tellurium nano-wire is electronic structure, enable both mutually mate; The mass ratio different in laminated film from tellurium nano-wire by control reduced graphene and annealing conditions, optimize specific conductivity and the Seebeck coefficient of compound thermal conductive film. The present invention has that preparation cycle is short, technique is simply controlled, safety non-pollution, energy consumption are low, product has the feature such as flexibility and excellent property, according to actual production requirement, this technique can prepare the compound thermal conductive film of different size flexibly according to the size of glass fibre membrane, has wide prospects for commercial application.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the embodiment of the present invention 1.
Fig. 2 is the electron scanning micrograph dispersibling reduced graphene of the embodiment of the present invention 1.
Fig. 3 is the electron scanning micrograph dispersibling tellurium nano-wire of the embodiment of the present invention 1.
Fig. 4 is the electron scanning micrograph of the laminated film of the embodiment of the present invention 1.
Fig. 5 is specific conductivity and the Seebeck coefficient of the laminated film of the embodiment of the present invention 1
Embodiment
The substantive distinguishing features of the present invention and significant progress is set forth further, but the present invention is not limited only to the following examples below by embodiment:
Embodiment 1:
As shown in Figure 1, the preparation method of a kind of flexible reduced graphene/tellurium nano-wire compound thermal conductive film, it comprises the following steps:
(1) by 25mg graphene oxide (GO) and 12.5mg sodium polystyrene sulfonate (NaPSS) ultrasonic disperse in the deionized water of 12.5mL, adding the saturated hydrobromic acid solution of 25mL again in dispersion liquid, naturally cooling is precipitated to be transferred in the reactor of 50mL by mixed solution at 120 DEG C hydro-thermal reaction after 2 hours; After precipitation being rinsed 35 times with deionized water, at 60 DEG C, vacuum-drying precipitates the reduced graphene obtaining dispersibling for 3 hours, and the electron scanning micrograph dispersibling reduced graphene is as shown in Figure 2;
(2) by 0.369g sodium tellurite and 2g polyvinylpyrrolidone stirring and dissolving in 70mL deionized water, in solution, add the ammoniacal liquor of 6.6mL25% and the hydrazine hydrate of 3.4mL98% again, it is transferred in the reactor of 100mL by mixed solution at 180 DEG C hydro-thermal reaction after 3 hours with the tap water cooling reactor of flowing; After adding the acetone of 160mL in the mixed solution after cooling, centrifugal for mixture and abandoning supernatant obtaining the tellurium nano-wire dispersibled, the electron scanning micrograph dispersibling tellurium nano-wire is as shown in Figure 3;
(3) the reduced graphene dispersion liquid of 1mg/mL and the tellurium nano-wire dispersion liquid of 2mg/mL is configured respectively; Under vacuum filtration is auxiliary, the reduced graphene dispersion liquid of 0.15mL is evenly dripped on the glass fibre membrane being coated in 2cm �� 0.5cm, liquid is drained; Again under vacuum filtration is auxiliary, the tellurium nano-wire dispersion liquid of 0.1mL is evenly dripped the region being coated with reduced graphene and covering, after waiting liquid to drain, glass fibre membrane vacuum drying at 60 DEG C of laminated film will be coated with;
(4) glass fibre membrane dried is transferred in tube furnace, at Ar/H2Annealing 2 hours at 200 DEG C in mixed atmosphere (hydrogen content 8%), as shown in Figure 4, specific conductivity and Seebeck coefficient are as shown in Figure 5 for the electron scanning micrograph of laminated film.
Embodiment 2:
(1) by 25mg graphene oxide (GO) and 50mg sodium polystyrene sulfonate (NaPSS) ultrasonic disperse in the deionized water of 12.5mL, adding the saturated hydrobromic acid solution of 50mL again in dispersion liquid, naturally cooling is precipitated to be transferred in the reactor of 100mL by mixed solution at 150 DEG C hydro-thermal reaction after 2 hours; After precipitation being rinsed 35 times with deionized water, at 60 DEG C, vacuum-drying precipitates the reduced graphene obtaining dispersibling for 3 hours;
(2) by 0.369g sodium tellurite and 2g polyvinylpyrrolidone stirring and dissolving in 70mL deionized water, in solution, add the ammoniacal liquor of 6.6mL25% and the hydrazine hydrate of 3.4mL98% again, it is transferred in the reactor of 100mL by mixed solution at 180 DEG C hydro-thermal reaction after 1.5 hours with the tap water cooling reactor of flowing; After adding the acetone of 320mL in the mixed solution after cooling, centrifugal for mixture and abandoning supernatant is obtained the tellurium nano-wire dispersibled;
(3) the reduced graphene dispersion liquid of 1mg/mL and the tellurium nano-wire dispersion liquid of 2mg/mL is configured respectively; Under vacuum filtration is auxiliary, the reduced graphene dispersion liquid of 0.15mL is evenly dripped on the glass fibre membrane being coated in 2cm �� 0.5cm, liquid is drained; Again under vacuum filtration is auxiliary, the tellurium nano-wire dispersion liquid of 0.1mL is evenly dripped the region being coated with reduced graphene and covering, after waiting liquid to drain, glass fibre membrane vacuum drying at 60 DEG C of laminated film will be coated with;
(4) glass fibre membrane dried is transferred in tube furnace, at Ar/H2Mixed atmosphere (hydrogen content 8%) is annealed 2 hours at 200 DEG C.
Embodiment 3:
(1) by 25mg graphene oxide (GO) and 25mg sodium polystyrene sulfonate (NaPSS) ultrasonic disperse in the deionized water of 12.5mL, adding the saturated hydrobromic acid solution of 25mL again in dispersion liquid, naturally cooling is precipitated to be transferred in the reactor of 50mL by mixed solution at 120 DEG C hydro-thermal reaction after 2 hours; After precipitation being rinsed 35 times with deionized water, at 60 DEG C, vacuum-drying precipitates the reduced graphene obtaining dispersibling for 3 hours;
(2) by 0.369g sodium tellurite and 2g polyvinylpyrrolidone stirring and dissolving in 70mL deionized water, in solution, add the ammoniacal liquor of 6.6mL25% and the hydrazine hydrate of 3.4mL98% again, it is transferred in the reactor of 100mL by mixed solution at 180 DEG C hydro-thermal reaction after 3 hours with the tap water cooling reactor of flowing; After adding the acetone of 160mL in the mixed solution after cooling, centrifugal for mixture and abandoning supernatant is obtained the tellurium nano-wire dispersibled;
(3) the reduced graphene dispersion liquid of 1mg/mL and the tellurium nano-wire dispersion liquid of 2mg/mL is configured respectively; Under vacuum filtration is auxiliary, the reduced graphene dispersion liquid of 0.5mL is evenly dripped on the glass fibre membrane being coated in 2cm �� 0.5cm, liquid is drained; Again under vacuum filtration is auxiliary, the tellurium nano-wire dispersion liquid of 1mL is evenly dripped the region being coated with reduced graphene and covering, after waiting liquid to drain, glass fibre membrane vacuum drying at 60 DEG C of laminated film will be coated with;
(4) glass fibre membrane dried is transferred in tube furnace, at Ar/H2Mixed atmosphere (hydrogen content 8%) is annealed 0.5 hour at 200 DEG C.
Embodiment 4:
(1) by 25mg graphene oxide (GO) and 12.5mg sodium polystyrene sulfonate (NaPSS) ultrasonic disperse in the deionized water of 12.5mL, adding the saturated hydroiodic acid HI solution of 25mL again in dispersion liquid, naturally cooling is precipitated to be transferred in the reactor of 50mL by mixed solution at 150 DEG C hydro-thermal reaction after 6 hours; After precipitation being rinsed 35 times with deionized water, at 60 DEG C, vacuum-drying precipitates the reduced graphene obtaining dispersibling for 3 hours;
(2) by 0.178g sodium tellurite and 1g polyvinylpyrrolidone stirring and dissolving in 35mL deionized water, in solution, add the ammoniacal liquor of 3.3mL25% and the hydrazine hydrate of 1.7mL98% again, it is transferred in the reactor of 50mL by mixed solution at 180 DEG C hydro-thermal reaction after 3 hours with the tap water cooling reactor of flowing; After adding the acetone of 80mL in the mixed solution after cooling, centrifugal for mixture and abandoning supernatant is obtained the tellurium nano-wire dispersibled;
(3) the reduced graphene dispersion liquid of 1mg/mL and the tellurium nano-wire dispersion liquid of 2mg/mL is configured respectively; Under vacuum filtration is auxiliary, the reduced graphene dispersion liquid of 0.5mL is evenly dripped on the glass fibre membrane being coated in 1cm �� 1cm, liquid is drained; Again under vacuum filtration is auxiliary, the tellurium nano-wire dispersion liquid of 1mL is evenly dripped the region being coated with reduced graphene and covering, after waiting liquid to drain, glass fibre membrane vacuum drying at 60 DEG C of laminated film will be coated with;
(4) glass fibre membrane dried is transferred in tube furnace, at Ar/H2Mixed atmosphere (hydrogen content 8%) is annealed 2 hours at 200 DEG C.
Embodiment 5:
(1) by 25mg graphene oxide (GO) and 12.5mg sodium polystyrene sulfonate (NaPSS) ultrasonic disperse in the deionized water of 12.5mL, adding the saturated hydroiodic acid HI solution of 50mL again in dispersion liquid, naturally cooling is precipitated to be transferred in the reactor of 100mL by mixed solution at 150 DEG C hydro-thermal reaction after 2 hours; After precipitation being rinsed 35 times with deionized water, at 60 DEG C, vacuum-drying precipitates the reduced graphene obtaining dispersibling for 3 hours;
(2) by 0.178g sodium tellurite and 1g polyvinylpyrrolidone stirring and dissolving in 35mL deionized water, in solution, add the ammoniacal liquor of 3.3mL25% and the hydrazine hydrate of 1.7mL98% again, it is transferred in the reactor of 50mL by mixed solution at 180 DEG C hydro-thermal reaction after 1.5 hours with the tap water cooling reactor of flowing; After adding the acetone of 80mL in the mixed solution after cooling, centrifugal for mixture and abandoning supernatant is obtained the tellurium nano-wire dispersibled;
(3) the reduced graphene dispersion liquid of 1mg/mL and the tellurium nano-wire dispersion liquid of 2mg/mL is configured respectively; Under vacuum filtration is auxiliary, the reduced graphene dispersion liquid of 0.15mL is evenly dripped on the glass fibre membrane being coated in 1cm �� 1cm, liquid is drained; Again under vacuum filtration is auxiliary, the tellurium nano-wire dispersion liquid of 1mL is evenly dripped the region being coated with reduced graphene and covering, after waiting liquid to drain, glass fibre membrane vacuum drying at 60 DEG C of laminated film will be coated with;
(4) glass fibre membrane dried is transferred in tube furnace, at Ar/H2Mixed atmosphere (hydrogen content 8%) is annealed 0.5 hour at 200 DEG C.
Claims (10)
1. the preparation method of a flexible reduced graphene and tellurium nano-wire compound thermal conductive film, it is characterized in that: by regulating the shape looks of the reducing degree of reduced graphene and tellurium nano-wire to be that they can mutually mate in composite coated, preparation method comprises the steps:
(1) by a certain amount of graphene oxide and tensio-active agent ultrasonic disperse in water, then adding the acid of 24 times of dispersion liquid volumes in dispersion liquid, mixed solution hydro-thermal reaction at 120 150 DEG C is taken out filter after naturally cooling in 26 hours and is precipitated;
(2) precipitate with deionized water obtained in step (1) is washed till neutrality, is deposited at 60 DEG C vacuum-drying and obtains for 35 hours the reduced graphene dispersibled;
(3) by sodium tellurite and complexing agent stirring and dissolving in water, then adding the ammoniacal liquor of 25% and the hydrazine hydrate of 98% in previous solu, mixed solution cools after hydro-thermal reaction certain time at 180 DEG C;
(4) liquid obtained in step (3) adds a certain amount of acetone and obtains flocks, after centrifugal, abandon the tellurium nano-wire that supernatant liquid obtains dispersibling;
(5) certain density reduced graphene and tellurium nano-wire dispersion liquid is configured respectively;
(6) under vacuum filtration is auxiliary, a certain amount of reduced graphene dispersant liquid drop is coated in the flexible substrates of certain area size, liquid is drained;
(7) under vacuum filtration is auxiliary, the region being coated in step (6) by a certain amount of tellurium nano-wire dispersant liquid drop reduced graphene and covering, drains liquid;
(8) step (7) will be coated with flexible substrates vacuum drying at 30 60 DEG C of laminated film;
(9) glass fibre membrane being coated with laminated film in step (8) is transferred in tube furnace, at Ar/H2Mixed atmosphere (hydrogen content 8%) is annealed certain time at 200 DEG C.
2. according to the preparation method described in claim 1, it is characterised in that in step (1), the mass ratio of graphene oxide and tensio-active agent is 2:1 1:2.
3., according to the preparation method described in claim 1, it is characterised in that in step (1), tensio-active agent is sodium polystyrene sulfonate, acid is Hydrogen bromide or hydroiodic acid HI.
4. according to the preparation method described in claim 1, it is characterised in that in step (3), the hydro-thermal reaction time is 1.5 3 hours, and the type of cooling is water-cooled.
5. according to the preparation method described in claim 1, it is characterised in that in step (4) 24 times that add that volume is the liquid that step (3) obtains of acetone.
6. according to the preparation method described in claim 1, it is characterised in that the concentration of step (5) described reduced graphene is 1mg/ml; Tellurium nano-wire is 2mg/ml.
7. according to the preparation method described in claim 1, it is characterised in that the flexible substrates used in step (6) is glass fibre membrane stable at normal temperature to 500 DEG C.
8. according to the preparation method described in claim 1, it is characterised in that in step (6), 0.15 0.5mg/cm is measured in the painting of dripping of reduced graphene2��
9. according to the preparation method described in claim 1, it is characterised in that in step (7), 0.1 2mg/cm is measured in the painting of dripping of tellurium nano-wire2��
10. according to the preparation method described in claim 1, it is characterised in that in step (8), annealing atmosphere is Ar/H2, annealing time is 0.5 2 hours.
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CN108772083A (en) * | 2018-08-17 | 2018-11-09 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of graphene oxide-houghite laminated film |
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CN113707798A (en) * | 2021-08-17 | 2021-11-26 | 上海应用技术大学 | RGO/Cu1.75Preparation method of Te nanowire composite flexible thermoelectric film |
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