CN109950048A - A kind of graphene-based thin-film solar cells - Google Patents
A kind of graphene-based thin-film solar cells Download PDFInfo
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Abstract
The invention discloses a kind of graphene-based thin-film solar cells, including transparent electrode, transparent electrode is graphene film, and thickness is not more than 20nm, and graphene sheet layer is conjugated structure, zero defect；Interlayer stack manner is the unordered stacking of random layer.The graphene film is obtained by the graphene film of independent self-supporting through Overheating Treatment, electric treatment.The graphene film of independent self-supporting is gradually warming up to 2000 degree, maintains 1-2 hours, has repaired most defect sturcture, maintains the folded state of graphene sheet layer unrest layer heap.Then it is powered to film, activated carbon promotes carbon atom flowing, to further repair atomic structure defect.The two collective effect, the defect sturcture for greatly reducing graphene film repair temperature.In comparison, graphene has higher electron mobility, and exists without heavy metal pollution problem, reduces costs, improves phototransformation efficiency.
Description
Technical field
The present invention relates to solar battery more particularly to a kind of graphene-based thin-film solar cells.
Background technique
With getting worse for environmental problem, the uncontrolled application bring environmental problem of fossil energy increasingly causes greatly
The concern of people.People are highly desirable to be found renewable, and free of contamination new energy substitutes the fossil energy of heavily contaminated.And too
Sun can be used as the source of earth statement, be always object concerned by people.Wherein solar flexible battery is therein using it
One, it is the light induced electron effect using photoactive substance, converts light into electricity.But traditional solar flexible battery is to answer
It uses ITO as transparent conductive electrode, there are following several respects, first, ITO has heavy metal pollution problem；Its
Two, ITO electric conductivity are bad, and electron mobility is low, are unfavorable for photoelectronic transmission；Third, ITO flexibility is poor, is not suitable for
Do flexible electrode.
The graphene film of macroscopic view assembling graphene oxide or graphene nanometer sheet is the main application of nanoscale graphite alkene
Form, common preparation method are suction methods, scrape embrane method, spin-coating method, spray coating method and dip coating etc..Pass through further high temperature
Processing, can repair the defect of graphene, can effectively improve the electric conductivity and thermal conductance of graphene film, can answer extensively
For in smart phone, intelligence with oneself the accompanied electronics equipment such as hardware, tablet computer, laptop.
But currently, the graphene film thickness crossed of high temperature sintering generally in 1um or more, many gas of enclosed inside,
During high pressure compacting, closed stomata is remained in the form of fold, and the graphene film degree of orientation is caused to be deteriorated, close
Degree becomes smaller, and interlayer AB stacking degree is poor, has seriously affected further increasing for graphene film performance.In addition, there is presently no
The preparation of nanoscale graphite alkene film of the work report based on graphene oxide.Under normal conditions, nanoscale graphite alkene film refers generally to
Be chemical vapor deposition method preparation polycrystalline graphite alkene film, using wet process or dry method transfer after be fixed on some
In substrate, independent self-supporting in air can not achieve.This graphene film itself is polycrystalline structure, and performance is by crystal boundary
It influences very big.
Most of all, the graphene of AB accumulation is prepared more demanding (higher temperature and hold time), and photoelectricity
Non- AB structure is more advantageous to photoelectronic migration in, and there is presently no the graphene films that random layer heap stack structure is dominated.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of graphene-based thin-film solar cells.
The purpose of the present invention is what is be achieved through the following technical solutions: a kind of graphene-based thin-film solar cells, including
Transparent electrode, the transparent electrode are graphene film, wherein graphene sheet layer is conjugated structure, zero defect；Interlayer stacks
Mode is the unordered stacking of random layer.
Further, it is prepared by following steps:
(1) graphene film of independent self-supporting is prepared；The number of plies of thickness direction, graphene film is not more than 200；
(2) graphene film is gradually warming up to 2000 DEG C, heating rate is not more than 60 DEG C/min, maintains 1-2 hours, so
It is powered afterwards to film, size of current 1-20A maintains 1-4h.
Further, the graphene film of independent self-supporting is prepared using solid transfer method.
Further, the solid transfer method includes the following steps:
(1.1) graphene oxide is configured to concentration is 0.5-10ug/mL graphene oxide water solution, to mix fiber
Plain ester (MCE) is that substrate filters film forming.
(1.2) graphene oxide membrane for being attached at MCE film is placed in closed container, 60-100 degree HI high temperature fumigation 1-
10h。
(1.3) the solid transfer agent even application of thawing is cold in redox graphene film surface, and at room temperature
But.
(1.4) graphene film for being coated with solid transfer agent is placed in the good solvent of MCE film, etches away MCE film.
(1.5) graphene film that solid transfer agent obtained above supports is waved at a temperature of solid transfer agent volatilizees
Hair falls solid transfer agent, obtains the graphene film of independent self-supporting.
Further, the solid transfer agent is selected from following substance, such as paraffin, aluminium chloride, iodine, naphthalene, three oxidations
Two arsenic, phosphorus pentachloride, acrylamide, ferric trichloride, sulphur, red phosphorus, ammonium chloride, ammonium hydrogen carbonate, potassium iodide, norbornene, coffee
The small molecule solid-state that cause, melamine, water, rosin, the tert-butyl alcohol, sulfur trioxide etc. can distil or volatilize under certain conditions
Substance.
Further, the good solvent of the MCE film is selected from one of acetone, n-butanol, ethyl alcohol, isopropanol or a variety of.
Further, the graphene film of independent self-supporting is prepared using water stripping means, the preparation method is as follows:
(1.1) graphene film is removed from AAO basilar memebrane, specifically: surface is fitted with to the AAO base of graphene film
Counterdie is placed on the water surface with face-up where graphene film；AAO basilar memebrane is pressed, so that AAO basilar memebrane sinks, graphene
Film floats on the water surface.
(1.2) graphene film for floating on the water surface is picked up from the bottom up using a substrate, so that graphene film is laid in
Substrate surface, and there is one layer of aqueous medium between graphene film and substrate.
(1.3) substrate that surface is loaded with graphene film is freeze-dried, graphene film self-supporting, and divided with substrate
From.
Further, the porosity on the surface of the AAO basilar memebrane is not less than 40%.
Further, substrate described in step 2 is hydrophobic substrate.
Further, the upper surface of substrate described in step 2 has sunk area.
The beneficial effects of the present invention are: the graphene film of independent self-supporting is gradually warming up to 2000 degree of (1- by the present invention
60 degree are per minute), it maintains 1-2 hours, has repaired most defect sturcture, it is folded to maintain graphene sheet layer unrest layer heap
State.Then it is powered to film, activated carbon promotes carbon atom flowing, to further repair atomic structure defect.
The two collective effect, the defect sturcture for greatly reducing graphene film repair temperature.Non- ab structure subtracts interlaminar action power
It is weak, phonon, which is reduced, in the conduction of vertical direction increases the thermal conductivity of horizontal direction to increase horizontal transport.Zero defect structure
The transmission for being conducive to electronics and phonon, not will form resistance and thermal resistance.While guaranteeing transparent, great conduction ensure that
Rate and mechanics load-carrying properties can bear tension force effect of the battery in discharge process and cell flexible bending process.It uses
When, the film as light anode, to electrode etc.；In comparison, graphene has higher electron mobility, and without weight
Rnetal contamination problem exists, and reduces costs, and improves phototransformation efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the graphene film of independent self-supporting prepared by embodiment 1；
Fig. 2 is the Raman figure of film prepared by embodiment 1；
Fig. 3 is the TEM figure of film prepared by embodiment 1；
Fig. 4 is the flow diagram of AAO substrate film stripping graphene film.
Fig. 5 is the experimentation figure of embodiment 4AAO substrate film stripping graphene film.
Fig. 6 is the photo for the self-supporting graphene film that embodiment 4 is prepared.
Fig. 7 is the atomic force microscopy diagram for the self-supporting graphene film that embodiment 4 is prepared.
Fig. 8 is the substrate schematic diagram of embodiment 5, and in figure, the substrate being recessed centered on 1,2 be graphene film, and 3 be water.
Fig. 9 is graphene-based dye sensitization transparent solar cell structural schematic diagram, wherein graphene film is as light sun
Pole.
Figure 10 is graphene-based dye sensitization transparent solar cell structural schematic diagram, wherein graphene film is as positive electricity
Pole.
In figure, quartz glass 1, graphene film 2, positive 3, ITO4.
Specific embodiment
Embodiment 1:
(1) graphene oxide is configured to concentration is 0.5ug/mL graphene oxide water solution, to mix cellulose esters
(MCE) film forming is filtered for substrate.
(2) graphene oxide membrane for being attached at MCE film is placed in closed container, 60 degree of HI high temperature fumigation 1h.
(3) use the methods of vapor deposition, curtain coating by the paraffin even application of thawing in redox graphene film surface, and in
Slow cooling at room temperature.
(4) graphene film for being coated with solid transfer agent is slowly washed with ethyl alcohol, dissolves MCE film.
(5) graphene film that solid transfer agent obtained above supports slowly is vapored away into solid transfer under 120 degree
Agent, obtains the graphene film of independent self-supporting, the graphene film with a thickness of 30 atomic layers or so, transparency 95%.
(6) graphene film is gradually warming up to 2000 DEG C, 60 DEG C/min of heating rate, maintains 2 hours, then gives film
It is powered, size of current 1A maintains 4h.
As shown in Figure 1, graphene has a small amount of fold.As can be seen that defect peak is substantially not present in Raman in Fig. 2, demonstrate,prove
The zero defect structure of graphene film is illustrated.Fig. 3 TEM electron diffraction diagram spectrum shows that stack manner is random layer between graphene sheet layer
It stacks.The thermal conductivity of its horizontal direction reaches 2500W/mK, and conductivity reaches 1.5MS/m, and the wave-length coverage of photodetection reaches
Terahertz.
As shown in figure 9,1. using above-mentioned graphene film as light anode assembly organic thin film solar cell, compared to adopting
2., photoelectric conversion efficiency improves 5% to dye sensitization transparent solar cell ITO is used as light anode assembled, compared to
The dye sensitization transparent solar cell that ordinary graphite alkene film (spin coating on ITO) is assembled as light anode 3., photoelectric conversion
Efficiency improves 37%.And when using ordinary graphite alkene film (in spin coating on ITO) as light anode, after 2400h, graphene film
It may be destroyed due to microstructure, conductivity decline 23%, the photoelectric conversion efficiency of solar battery 3. drops to
17%；And the graphene film of the application is using after 3600h, conductivity is maintained at original 90% or more, and solar battery is 1.
Photoelectric conversion efficiency be maintained at original 95% or more.
Embodiment 2:
(1) graphene oxide is configured to concentration is 10ug/mL graphene oxide water solution, to mix cellulose esters
(MCE) film forming is filtered for substrate.
(2) graphene oxide membrane for being attached at MCE film is placed in closed container, 100 degree of HI high temperature fumigation 10h.
(3) use the methods of vapor deposition, curtain coating by the rosin even application of thawing in redox graphene film surface, and in
Slow cooling at room temperature.
(4) graphene film for being coated with solid transfer agent is placed in acetone, removes MCE film.
(5) graphene film that solid transfer agent obtained above supports slowly is vapored away into rosin under 300 degree, obtained
The graphene film of independent self-supporting, with a thickness of 60 atomic layers or so, transparent is 10%.
(6) graphene film is gradually warming up to 2000 DEG C, 45 DEG C/min of heating rate, maintains 1 hour, then gives film
It is powered, size of current 20A maintains 1h.
After tested, defect peak is substantially not present in Raman, it was demonstrated that the zero defect structure of graphene film.TEM electronic diffraction
Map shows that stack manner is folded for random layer heap between graphene sheet layer.The thermal conductivity of its horizontal direction reaches 2100W/mK, electricity
Conductance reaches 1.3MS/m, and the wave-length coverage of photodetection reaches Terahertz.
1. using above-mentioned graphene film as light anode assembly dye-sensitized film solar battery, make compared to using ITO
For light anode assembling dye sensitization transparent solar cell 2., photoelectric conversion efficiency improves 10%, compared to conventional stone
3., photoelectric conversion efficiency mentions the dye sensitization transparent solar cell that black alkene film (spin coating on ITO) assembles as light anode
It is high by 8%.After using 3600h, conductivity is 91% originally, and the photoelectric conversion efficiency of solar battery 1. is original
96%.
Embodiment 3:
(1) graphene oxide is configured to concentration is 8ug/mL graphene oxide water solution, to mix cellulose esters
(MCE) film forming is filtered for substrate.
(2) graphene oxide membrane for being attached at MCE film is placed in closed container, 80 degree of HI high temperature fumigation 8h.
(3) with the methods of vapor deposition, curtain coating by the norbornene even application of thawing in redox graphene film surface,
And Slow cooling at room temperature.
(4) graphene film for being coated with solid transfer agent is placed in isopropanol, removes MCE film.
(5) graphene film that solid transfer agent obtained above supports slowly is vapored away into solid transfer under 100 degree
Agent obtains the graphene film of independent self-supporting, with a thickness of 200 atomic layers or so.
(6) graphene film is gradually warming up to 2000 DEG C, 20 DEG C/min of heating rate, maintains 1 hour, then gives film
It is powered, size of current 10A maintains 1h.
After tested, defect peak is substantially not present in Raman, it was demonstrated that the zero defect structure of graphene film.TEM electronic diffraction
Map shows that stack manner is folded for random layer heap between graphene sheet layer.The thermal conductivity of its horizontal direction reaches 1800W/mK, electricity
Conductance reaches 1.1MS/m, and the wave-length coverage of photodetection reaches Terahertz.
As shown in Figure 10, using above-mentioned graphene film as anode, organic thin film solar electricity is assembled by light anode of ITO
Pond 1., compared to using platinum electrode as anode assemble dye sensitization transparent solar cell 2., photoelectric conversion efficiency mentions
It is high by 26%, compared to the dye sensitization transparent solar cell for using ordinary graphite alkene film (spin coating on ITO) to assemble as anode
3. photoelectric conversion efficiency improves 17%.After using 3600h, conductivity is 93% originally, the light of solar battery 1.
Photoelectric transformation efficiency is 96% originally.
Embodiment 4:
(1) it by the concentration of control graphene solution, filters to obtain ultra-thin go back in AAO basilar memebrane by suction filtration method
Former graphene oxide membrane.
(2) graphene film is removed from AAO basilar memebrane, specifically: surface is fitted with redox graphene film
AAO basilar memebrane (porosity 40%) is placed on the water surface, such as Figure 4 and 5 a with face-up where graphene film；Press AAO
Substrate film edge, such as Fig. 5 b, AAO basilar memebrane starts to sink, and such as Fig. 5 c, finally, AAO basilar memebrane is sunken to bottom of a cup, graphene film floats
It bubbles through the water column (in virtual coil), such as Fig. 5 b and 5d.
(3) substrate of glass that " Zhejiang University " is printed on using a surface will float on the graphene film of the water surface from the bottom up
It picks up, so that graphene film is laid in substrate surface, and there is one layer of aqueous medium between graphene film and substrate.
(4) substrate that surface is loaded with graphene film is freeze-dried, graphene film self-supporting, as shown in Fig. 6, and
It is separated with substrate.It is tested through atomic force microscope, with a thickness of 4nm, as shown in Figure 7.
(5) graphene film is gradually warming up to 2000 DEG C, 60 DEG C/min of heating rate, maintains 2 hours, then gives film
It is powered, size of current 20A maintains 1h.
After tested, defect peak is substantially not present in Raman, it was demonstrated that the zero defect structure of graphene film.TEM electronic diffraction
Map shows that stack manner is folded for random layer heap between graphene sheet layer.
1. using above-mentioned graphene film as light anode assembly dye-sensitized film solar battery, make compared to using ITO
For light anode assembling dye sensitization transparent solar cell 2., photoelectric conversion efficiency improves 3%, compared to conventional stone
3., photoelectric conversion efficiency mentions the dye sensitization transparent solar cell that black alkene film (spin coating on ITO) assembles as light anode
It is high by 3%.After using 3600h, conductivity is 84% originally, and the photoelectric conversion efficiency of solar battery 1. is original
90%.
Embodiment 5
(1) it by the concentration of control graphene solution, filters to obtain ultra-thin oxygen in AAO basilar memebrane by suction filtration method
Graphite alkene film.
(2) graphene film is removed from AAO basilar memebrane, specifically: surface is fitted with to the AAO of graphene oxide membrane
Basilar memebrane (porosity 60%) is placed on the water surface with face-up where graphene film, presses AAO substrate film edge, AAO
Basilar memebrane starts to sink, finally, AAO basilar memebrane is sunken to bottom of a cup, graphene film floats on the water surface, and graphene film is successfully removed.
(3) hydrophilic silicon base (silicon face hydrophilic treated, the central concave, such as figure of " Zhejiang University " are printed on using a surface
Shown in 8) graphene film for floating on the water surface is picked up from the bottom up, so that graphene film is laid in base center position, graphite
There is aqueous medium at the center of alkene film and recess.
(4) substrate that surface is loaded with graphene film is freeze-dried, graphene film self-supporting, and is separated with substrate.
It is tested through atomic force microscope, with a thickness of 14nm.
(5) graphene film is gradually warming up to 2000 DEG C, 4 DEG C/min of heating rate, is maintained 2 hours, it is then logical to film
Electricity, size of current 1A maintain 4h.
After tested, defect peak is substantially not present in Raman, it was demonstrated that the zero defect structure of graphene film.TEM electronic diffraction
Map shows that stack manner is folded for random layer heap between graphene sheet layer.
1. using above-mentioned graphene film as light anode assembly dye-sensitized film solar battery, make compared to using ITO
For light anode assembling dye sensitization transparent solar cell 2., photoelectric conversion efficiency improves 7%, compared to conventional stone
3., photoelectric conversion efficiency mentions the dye sensitization transparent solar cell that black alkene film (spin coating on ITO) assembles as light anode
It is high by 5%.After using 3600h, conductivity is 90% originally, and the photoelectric conversion efficiency of solar battery 1. is original
95%.
It should be noted that suction method is the method for most uniformly preparing graphene film generally acknowledged at present, in certain suction filtration
Under liquid measure, concentration can be regulated and controled to control the thickness of graphene film, thickness is minimum to can be one layer of graphene, with
The increase of graphene concentration, under pressure, newly-increased graphene are gradually filled into the gap of first layer graphene, so that
First layer graphene is gradually filled up completely, and then develops into the second layer, constantly repeatedly above step, can prepare thickness across 2
Layer arrives the graphene nano film of up to ten thousand layers of graphene.Therefore, those skilled in the art can be adjusted by simple experiment parameter is
It can get the graphene film with a thickness of 4nm.
Claims (10)
1. a kind of graphene-based thin-film solar cells, which is characterized in that including transparent electrode, the transparent electrode is graphene
Film, in graphene film, graphene sheet layer is conjugated structure, zero defect；Interlayer stack manner is the unordered stacking of random layer.
2. graphene-based thin-film solar cells according to claim 1, which is characterized in that graphene film passes through following
Step is prepared:
(1) graphene film of independent self-supporting is prepared；The number of plies of thickness direction, graphene film is not more than 200；
(2) graphene film is gradually warming up to 2000 DEG C, heating rate is not more than 60 DEG C/min, maintains 1-2 hours, then to thin
Film is powered, size of current 1-20A, maintains 1-4h.
3. graphene-based thin-film solar cells according to claim 2, which is characterized in that prepared using solid transfer method
The graphene film of the independent self-supporting.
4. graphene-based thin-film solar cells according to claim 3, which is characterized in that the solid transfer method includes
Following steps:
(1.1) graphene oxide is configured to concentration is 0.5-10ug/mL graphene oxide water solution, to mix cellulose esters
(MCE) film forming is filtered for substrate.
(1.2) graphene oxide membrane for being attached at MCE film is placed in closed container, 60-100 degree HI high temperature fumigation 1-10h.
(1.3) the solid transfer agent even application of thawing is cooled down in redox graphene film surface, and at room temperature.
(1.4) graphene film for being coated with solid transfer agent is placed in the good solvent of MCE film, etches away MCE film.
(1.5) graphene film that solid transfer agent obtained above supports is vapored away at a temperature of solid transfer agent volatilizees solid
Body transfer agent obtains the graphene film of independent self-supporting.
5. graphene-based thin-film solar cells as claimed in claim 4, which is characterized in that the solid transfer agent, choosing
From following substance, for example, it is paraffin, aluminium chloride, iodine, naphthalene, arsenic trioxide, phosphorus pentachloride, acrylamide, ferric trichloride, sulphur, red
Phosphorus, ammonium chloride, ammonium hydrogen carbonate, potassium iodide, norbornene, caffeine, melamine, water, rosin, the tert-butyl alcohol, sulfur trioxide etc.
The small molecule solid matter that can be distilled or volatilize under certain conditions.
6. graphene-based thin-film solar cells according to claim 4, which is characterized in that the good solvent of the MCE film
Selected from one of acetone, n-butanol, ethyl alcohol, isopropanol or a variety of.
7. graphene-based thin-film solar cells according to claim 2, which is characterized in that prepared using water stripping means
The graphene film of the independent self-supporting, the preparation method is as follows:
(1.1) graphene film is removed from AAO basilar memebrane, specifically: by surface be fitted with the AAO basilar memebrane of graphene film with
It is face-up where graphene film, it is placed on the water surface；AAO basilar memebrane is pressed, so that AAO basilar memebrane sinks, graphene film floating
In the water surface.
(1.2) graphene film for floating on the water surface is picked up from the bottom up using a substrate, so that graphene film is laid in substrate
Surface, and there is one layer of aqueous medium between graphene film and substrate.
(1.3) substrate that surface is loaded with graphene film is freeze-dried, graphene film self-supporting, and is separated with substrate.
8. graphene-based thin-film solar cells according to claim 7, which is characterized in that the table of the AAO basilar memebrane
The porosity in face is not less than 40%.
9. graphene-based thin-film solar cells according to claim 7, which is characterized in that substrate described in step 2
For hydrophobic substrate.
10. graphene-based thin-film solar cells according to claim 7, which is characterized in that substrate described in step 2
Upper surface have sunk area.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020187332A1 (en) * | 2019-03-17 | 2020-09-24 | 杭州高烯科技有限公司 | Method for electrocatalytic preparation of defect-free disorderly stacked graphene nanofilms and application |
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| CN107857252A (en) * | 2017-10-13 | 2018-03-30 | 浙江大学 | A kind of preparation method of independent self-supporting graphene film |
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Application publication date: 20190628 |