CN106409935A - MoO3/MoS2/LiF flexible heterojunction solar cell and preparation method thereof - Google Patents
MoO3/MoS2/LiF flexible heterojunction solar cell and preparation method thereof Download PDFInfo
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- CN106409935A CN106409935A CN201610908370.4A CN201610908370A CN106409935A CN 106409935 A CN106409935 A CN 106409935A CN 201610908370 A CN201610908370 A CN 201610908370A CN 106409935 A CN106409935 A CN 106409935A
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 54
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 44
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 230000008569 process Effects 0.000 claims abstract description 31
- 230000005284 excitation Effects 0.000 claims abstract description 12
- 239000004642 Polyimide Substances 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 229920001721 polyimide Polymers 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 239000010408 film Substances 0.000 claims description 29
- 238000004528 spin coating Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 20
- 239000010453 quartz Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000003708 ampul Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 239000010409 thin film Substances 0.000 claims description 14
- 230000005540 biological transmission Effects 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 238000002207 thermal evaporation Methods 0.000 claims description 9
- 238000001771 vacuum deposition Methods 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000005864 Sulphur Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 6
- 229910003208 (NH4)6Mo7O24·4H2O Inorganic materials 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 238000000935 solvent evaporation Methods 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 238000010025 steaming Methods 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 239000011593 sulfur Substances 0.000 claims 1
- 230000008020 evaporation Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 5
- 230000005525 hole transport Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract 1
- 238000011109 contamination Methods 0.000 abstract 1
- 238000004073 vulcanization Methods 0.000 abstract 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 64
- 239000007789 gas Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 210000001142 back Anatomy 0.000 description 3
- 239000012459 cleaning agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- MGCQZNBCJBRZDT-UHFFFAOYSA-N midodrine hydrochloride Chemical compound [H+].[Cl-].COC1=CC=C(OC)C(C(O)CNC(=O)CN)=C1 MGCQZNBCJBRZDT-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- -1 Oxygen Graphite alkene Chemical class 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 241000165940 Houjia Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/06—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier
- H01L31/072—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by at least one potential-jump barrier or surface barrier the potential barriers being only of the PN heterojunction type
- H01L31/0725—Multiple junction or tandem solar cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1864—Annealing
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a MoO3/MoS2/LiF flexible heterojunction solar cell and a preparation method thereof. The solar cell comprises a polyimide (PI) flexible substrate, an Al back pole, a MoO3 hole transport layer, a MoS2 electron hole excitation layer, a LiF electron transport layer, a graphene transparent conductive layer and an Al gate. The MoO3 layer is prepared through a solution method at low temperature, which facilitates mass production in large area. The MoS2 is formed by in-situ vulcanization through a CVD method. The MoO3 layer is annealed to reduce interface defects between the MoO3 hole transport layer and the MoS2 layer. Interface contamination is reduced. Through the heat radiation evaporation LiF layer and the thin hole transport layer and electron transport layer, the series resistance is reduced on the one hand, and on the other hand the great flexible heterojunction solar cell is formed with the MoS2, graphene and other two-dimensional layered materials. The MoO3/MoS2/LiF flexible heterojunction solar cell has the advantages of low temperature preparation, simple process, low cost, high photoelectric conversion efficiency, wide application range and the like.
Description
Technical field
The present invention relates to a kind of flexible solar battery and preparation method thereof, both belonged to flexible thin-film material and led with device
Domain, falls within new energy materialses field.
Background technology
Today's society, energy crisis and environmental pollution become two hang-ups of facing mankind, and solar energy is as preferably may be used
The renewable sources of energy receive the attention of many countries.For solaode, higher conversion efficiency becomes with relatively low production
Originally it is two the most key R＆D targets.At present, silicon is the most frequently used solar cell material, and the solaode of preparation turns
Change efficiency high, technology also relative maturity, but because preparation cost remains high it would be highly desirable to find a kind of novel low-cost high-efficiency rate half
Conductor material and battery.
Molybdenum bisuphide MoS2It is a kind of natural minerals of rich reserves, cheap, there is good heat stability and change
Learn stability, and have the two-dimensional layered structure similar to Graphene；In visible-range, there is wide band gap and band gap is adjustable
The features such as physical property, higher carrier mobility, it is especially suitable for making solaode.Molybdenum trioxide MoO3And lithium fluoride
LiF is widely used in organic polymer solar cell as hole transmission layer and electron transfer layer, MoO3Can be effective
Ground transporting holes to anode and stop electronics to anode transmission, and LiF not only can help to the transmission of electronics moreover it is possible to electronics
Hole excitation layer forms protection.
This patent proposes one kind and is based on MoO3, LiF thin film and MoS2, the novel flexible hetero-junctions of Graphene layer structure
Solaode, using simple preparation method, can prepare the cheap and widely used flexible battery of superior performance.
Content of the invention
Problem solved by the invention is to provide a kind of MoO3/MoS2/ LiF flexibility heterojunction solar battery and preparation
Method, the structure of battery of the present invention is：Polyimide flex substrate/Al backplane/MoO3Hole transmission layer/MoS2Electron hole is swashed
Send out layer/LiF/Graphene transparency conducting layer/Al grid, realize effective conversion of solar energy.With respect to MoS2/ silicon
Heterojunction solar battery, the present invention replaces silicon materials completely and need not loaded down with trivial details technique be doped, and has simple production work
Skill and lower preparation cost and there are the flexibility characteristics being more easy to development and application；With respect to organic polymer solar cell, this
Invention is to have the inorganic MoS of two-dimensional layer of direct band gap and good light abstraction width2Layer is as electron hole excitation layer
Inorganic solar cell, more stability and high efficiency, the life-span longer it is easy to preparation and development and application.
The present invention provide technical scheme be：
A kind of MoO3/MoS2/ LiF flexibility heterojunction solar battery, including flexible substrate, metal backplane, hole transmission layer, no
Machine electron hole excitation layer, electron transfer layer, transparency conducting layer, metal gates, wherein, described inorganic electronic hole excitation layer is
MoS2.
Further, described hole transmission layer is MoO3, described electron transfer layer is LiF.
Further, described flexible substrate is polyimides, and described transparency conducting layer is Graphene.
Further, affiliated metal backplane is Al or Ag, and metal gates are Al or Ag.
Further, described metal Al backplane thickness is 50-100 nm；MoO3Thickness degree is 10-80 nm；MoS2Thickness
Degree 0.65-1.5 nm；LiF thickness degree is 1.5-5 nm；Graphene layer thickness is 0.5-2 nm；Al gate layer thickness is 50-
100 nm.
Meanwhile, present invention also offers a kind of MoO3/MoS2The preparation method of/LiF flexibility heterojunction solar battery, bag
Include following steps：
(1) clean flexible substrate and dry；
(2) with vacuum coating equipment by the way of thermal evaporation evaporating Al thin film on flexible substrates；
(3) prepare MoO3Solution, and with sol evenning machine be spin-coated on steaming have in the flexible substrate of Al film；
(4) in horizontal pipe stove, CVD In-situ sulphiding generation MoS2Layer is simultaneously to MoO3Layer is annealed, in MoO3Above layer
Form MoS2Electron hole excitation layer；
(5) vacuum coating equipment by the way of thermal evaporation in MoS2LiF is deposited with layer；
(6) sol evenning machine is utilized to adopt the method for spin coating to form Graphene transparency conducting layer above LiF；
(7) vacuum coating equipment is deposited with mask above Graphene transparency conducting layer by the way of thermal evaporation and forms grid electricity
Pole.
Further, prepare solwution method MoO3And be spin-coated to steam have Al film flexible substrate formed MoO3Layer flow process be：
(1) by 0.4 g (NH4)6Mo7O24·4H2O is dissolved in 10 ml deionized waters, and adds a small amount of hydrochloric acid solution；
(2) by step（1）In the solution that obtains in atmosphere with 80 DEG C of heating 1 h；
(3) by step（2）In remaining solution deionized water be diluted to the solution of 1-8 mg/mL mass ratio；
(4) by step（3）In the solution that obtains in sol evenning machine with rotating speed spin coating 30 s of 3000 r/min.
Further, the In-situ sulphiding generation MoS of described CVD2Layer is simultaneously to MoO3The flow process annealed of layer be：
(1) quartz boat filling 100 mg-500 mg sulphur powders is placed in stove central authorities, spin coating is had MoO3Print be placed in heating furnace
The dirty low-temperature space of quartz ampoule vent, is filled with protective gas Ar gas 10-15 min with emptying air to quartz ampoule, then heats
To 120 DEG C -150 DEG C, wherein, Ar throughput is 10-100 sccm to quartz ampoule；
(2) keep above-mentioned Ar throughput constant, with 3 DEG C/min-5 DEG C/min slow heating quartz ampoule to 180 DEG C -200 DEG C, permanent
It is cooled to room temperature after warm 5-30 min.
Further, the flow process of spin coating Graphene transparency conducting layer is：
(1) weigh graphite oxide, make the graphene oxide solution that mass concentration is 1-8 mg/mL respectively；
(2) spin coating is carried out using sol evenning machine, first by graphene oxide dispersion drop on glass moisten 1 min, then by substrate with
600 r/min rotating speeds rotate 1 min, so that solution is well dispersed in substrate, then rotate 1 min with 800 r/min rotating speeds again,
Make the film thining of formation, finally rotate 1 min with 1600 r/min rotating speeds, accelerate solvent evaporation, so that thin film is become dry；
(3) graphene oxide film adopts a step reducing process, and reducing agent is respectively adopted hydrazine steam and HI solution, a step reduction work
Skill is respectively 60 DEG C of process 24h of hydrazine steam, 100 DEG C of process 3 h of HI solution, graphene oxide film is reduced into Graphene thin
Film, oxidation graphene film, through deionized water and ethanol purge, dries 24 h for 80 DEG C.
Further, LiF and MoO3Purity be more than 99.5%, the purity of sulphur powder S is more than 99.95%.
Beneficial effects of the present invention are as follows：
The present invention adopts solwution method to prepare MoO3Layer, CVD In-situ sulphiding formation MoS2First stage heats up, just to MoO3Layer
Annealed, efficiently utilized the MoO of spin coating3The loose feature of Rotating fields, decreases MoO simultaneously3Hole transmission layer with
MoS2Boundary defect between layer, decreases interface pollution；Evaporate the heating to substrate during LiF layer using heat radiation, also serve as
To MoS2Layer carries out process annealing, has obtained a kind of novel inorganic flexibility heterojunction solar battery and preparation method.MoO3/
MoS2/ LiF flexibility heterojunction solar battery, with respect to MoS2/ silicon heterogenous solaode, preparation cost has significantly
Reduce and possess broader practice prospect；With respect to organic polymer solar cell, stability, life-span and efficiency are all
Improve, cheap and easily prepared and development and application.The method is simple, low cost, and controllability is strong, has good answering
Use prospect.
Brief description
Fig. 1 is MoO3/MoS2The structural representation of/LiF flexibility heterojunction solar battery.
Fig. 2 is MoO3/MoS2The process chart of/LiF flexibility heterojunction solar battery.
Wherein, 1, metal Al grid layer, 2, graphene layer, 3, LiF layer, 4, MoS2Layer, 5, MoO3Layer, 6, Al back electrode, 7,
Polyimide flex substrate.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, and
It is not used in the restriction present invention.
Fig. 1 is MoO provided in an embodiment of the present invention3/MoS2The structural representation of/LiF flexibility hetero-junction solar cell, as Fig. 1 institute
Show, the structure of battery of the present invention is followed successively by metal Al gate electrode layer 1, Graphene transparency conducting layer 2 from top to bottom, and LiF electronics passes
Defeated layer 3, MoS2Electron hole excitation layer 4, MoO3Hole transmission layer 5, Al dorsum electrode layer 6, polyimide flex substrate 7.Preferably
, described metal Al backplane thickness is 50-100 nm；MoO3Thickness degree is 10-80 nm；MoS2Thickness degree 0.65-1.5 nm；
LiF thickness degree is 1.5-5 nm；Graphene layer thickness is 0.5-2 nm；Al gate layer thickness is 50-100 nm.
The MoO of the present invention3/MoS2The preparation method of/LiF flexibility heterojunction solar battery, comprises the following steps：
1 cleaning flexible substrate is simultaneously dried；Above-mentioned to flexible substrate cleaning, shape required for being cut into substrate first, with cleaning
Agent is cleaned, and successively uses tertiary effluent, one-level water to rinse, is and then cleaned by ultrasonic respectively with one-level deionized water, acetone, ethanol successively
10 min, finally use one-level deionized water rinsing again, and dry high purity nitrogen dries up and dries.
2 with vacuum coating equipment by the way of thermal evaporation evaporating Al thin film on flexible substrates.
3 preparation MoO3Solution, and with sol evenning machine be spin-coated on steaming have in the flexible substrate of Al film.
Above-mentioned solwution method prepares MoO3And be spin-coated to steam have Al film flexible substrate formed MoO3Layer flow process be：
(1) by 0.4 g (NH4)6Mo7O24·4H2O is dissolved in 10 ml deionized waters, and adds a small amount of hydrochloric acid solution；
(2) by step（1）In the solution that obtains in atmosphere with 80 DEG C of heating 1 h；
(3) by step（2）In remaining solution deionized water be diluted to the solution of 1-8 mg/mL mass ratio；
(4) by step（3）In the solution that obtains in sol evenning machine with rotating speed spin coating 30 s of 3000 r/min.
4 in horizontal pipe stove, CVD In-situ sulphiding generation MoS2Layer is simultaneously to MoO3Layer is annealed, in MoO3Layer
Top half forms MoS2Body material layer.
The In-situ sulphiding generation MoS of above-mentioned CVD2Layer is simultaneously to MoO3The flow process annealed of layer be：
(1) quartz boat filling 100 mg-500 mg sulphur powders is placed in stove central authorities, spin coating is had MoO3Print be placed in heating
The dirty low-temperature space in hearthstone English Gutron air port, is filled with protective gas Ar gas 10-15 min with emptying air, Ran Houjia to quartz ampoule
To 120 DEG C -150 DEG C, wherein, Ar throughput is 10-100 sccm to hot quartz ampoule；
(2) keep above-mentioned Ar throughput constant, with 3 DEG C/min-5 DEG C/min slow heating quartz ampoule to 180 DEG C -200 DEG C,
It is cooled to room temperature after constant temperature 5-30 min.
5 vacuum coating equipments are by the way of thermal evaporation in MoS2LiF is deposited with layer.
6 utilize sol evenning machine to adopt the method for spin coating to form Graphene transparency conducting layer above LiF.
The flow process of above-mentioned spin coating Graphene transparency conducting layer is：
(1) weigh graphite oxide, make the graphene oxide solution that mass concentration is 1-8 mg/mL respectively；
(2) spin coating is carried out using sol evenning machine, first by graphene oxide dispersion drop on glass moisten 1 min, then by substrate with
600 r/min rotating speeds rotate 1 min, so that solution is well dispersed in substrate, then rotate 1 min with 800 r/min rotating speeds again,
Make the film thining of formation, finally rotate 1 min with 1600 r/min rotating speeds, accelerate solvent evaporation, so that thin film is become dry；
(3) graphene oxide film adopts a step reducing process, and reducing agent is respectively adopted hydrazine steam and HI solution, a step reduction work
Skill is respectively 60 DEG C of process 24h of hydrazine steam, 100 DEG C of process 3 h of HI solution, graphene oxide film is reduced into Graphene thin
Film, oxidation graphene film, through deionized water and ethanol purge, dries 24 h for 80 DEG C.
7 vacuum coating equipments are deposited with mask above Graphene transparency conducting layer by the way of thermal evaporation and form grid
Electrode.
Embodiment 1：
（1）Cleaning polyimide flex substrate:First place the substrate into and fill cleaning agent（As found person who is not a member of any political party's liquid detergent）Molten
10 min are soaked, after then repeatedly cleaning, clear water rinses in liquid；It is respectively put into the device equipped with deionized water, acetone and ethanol
Ultrasonic 10 min of difference in ware；After finally putting twice of deionized water rinsing into, dried up with nitrogen gun and put into 80 in baking oven
DEG C dry.
（2）Pass through one layer of Al of heat radiation heating evaporation, voltage 150V, time 10s on flexible substrates.
（3）MoO3Solution is prepared:By 0.4 g (NH4)6Mo7O24·4H2O is dissolved in 10 ml deionized waters, and adds
A small amount of hydrochloric acid solution；Solution is heated 1 hour with 80 DEG C in atmosphere；Remaining solution deionized water is diluted to 1 mg/
The solution of mL mass concentration.
（4）In the gas tank of inert gas shielding, with the side of spin coating whirl coating on the Al film steam the flexible substrate having Al film
Method gets rid of one layer of thick MoO of about 10 nm3.Wherein, rotating speed is 500 turns every point of low speed, gets rid of 6 seconds；3000 r/min at a high speed,
Get rid of 30 s, then obtain the MoO that thickness is about 10 nanometers3Layer.
（5）The quartz boat filling 100mg sulphur powder S is placed in stove central authorities, surface fills MoO3Print be placed in heating hearthstone
The dirty low-temperature space in English Gutron air port, is filled with protective gas Ar 10 min with emptying air to quartz ampoule, and then heated quarty tube is extremely
120℃.Wherein Ar throughput is 100 sccm.
（6）Keep above-mentioned Ar throughput constant, with 3 DEG C/min slow heating quartz ampoule to 180 DEG C, cold after constant temperature 5 min
But to room temperature.
（7）In MoS2The upper LiF controlling one layer of about 1.5nm thickness of evaporation by thickness monitoring instrument.
（8）Graphene solution is prepared：Weigh a certain amount of graphite oxide, add deionized water supersound process 1 h, will aoxidize
Graphite peels off into graphene oxide, makes the graphene oxide solution that mass concentration is 1 mg/mL.By being centrifuged at a high speed
Go out and there is no scattered graphene oxide, the graphene oxide solution obtaining stable dispersion is standby.
（9）Spin coating is carried out using sol evenning machine, first graphene oxide dispersion is dropped in and moisten 1 min on glass, then by base
Bottom rotates 1 min with 600 r/min rotating speeds, so that solution is well dispersed in substrate, then rotates 1 with 800 r/min rotating speeds again
Min, makes the film thining of formation, finally rotates 1 min with 1600 r/min rotating speeds, accelerates solvent evaporation, so that thin film is become dry.Oxygen
Graphite alkene thin film adopts a step reducing process. and reducing agent is respectively hydrazine steam and HI solution.One step reducing process is respectively hydrazine
60 DEG C of process 24h of steam, 100 DEG C of process 3 h of HI solution, graphene oxide film is reduced into graphene film, reduction-oxidation
Graphene film is through deionized water and ethanol purge, 80 DEG C of drying 24 h.
（10）The preparation of electrode：In the metallic aluminium that graphenic surface evaporation about 50 nm is thick.By under inert gas shielding
After annealing（150 DEG C of baking 5 min）.Obtain the flexible heterojunction solar battery battery of structure as shown in Fig. 1：Metal Al
Gate electrode layer 1, Graphene transparency conducting layer 2, LiF 3, MoS2Electron hole excitation layer 4, MoO3Hole transmission layer,
Al dorsum electrode layer 6, polyimide flex substrate 7.
Embodiment 2：
（1）Cleaning polyimide flex substrate:First place the substrate into and fill cleaning agent（As found person who is not a member of any political party's liquid detergent）Molten
10 min are soaked, after then repeatedly cleaning, clear water rinses in liquid；It is respectively put into the device equipped with deionized water, acetone and ethanol
Ultrasonic 10 min of difference in ware；After finally putting twice of deionized water rinsing into, dried up with nitrogen gun and put into 80 in baking oven
DEG C dry.
（2）Pass through one layer of Al of heat radiation heating evaporation, voltage 150V, time 20s on flexible substrates.
（3）MoO3Solution is prepared:By 0.4 g (NH4)6Mo7O24·4H2O is dissolved in 10 ml deionized waters, and adds
A small amount of hydrochloric acid solution；Solution is heated 1 hour with 80 DEG C in atmosphere；Remaining solution deionized water is diluted to 2mg/ml
The solution of mass ratio.
（4）In the gas tank of inert gas shielding, get rid of one layer of about 20 nm with the method for spin coating whirl coating on being coated with Al thick
MoO3.Wherein, rotating speed is 500 turns every point of low speed, gets rid of 6 seconds；3000 turns every point at a high speed, get rid of 30 seconds.Finally obtain
The MoO of thickness about 20 nm3Layer.
（5）The quartz boat filling 100mg sulphur powder S is placed in stove central authorities, surface fills MoO3Print be placed in heating hearthstone
English Gutron air port upstream low-temperature space, is filled with protective gas Ar 10 min with emptying air to quartz ampoule, and then heated quarty tube is extremely
150℃.Wherein Ar throughput is 80 sccm.
（6）Keep above-mentioned Ar throughput constant, with 5 DEG C/min slow heating quartz ampoule to 200 DEG C, cold after constant temperature 5 min
But to room temperature.
（7）In MoS2The upper LiF controlling one layer of about 2.5 nm thickness of evaporation by thickness monitoring instrument.
（8）Graphene solution is prepared：Weigh a certain amount of graphite oxide, add deionized water supersound process 1 h, will aoxidize
Graphite peels off into graphene oxide, makes the graphene oxide solution that mass concentration is 2mg/mL.By being centrifuged at a high speed
Go out and there is no scattered graphene oxide, the graphene oxide solution obtaining stable dispersion is standby.
（9）Spin coating is carried out using sol evenning machine, first graphene oxide dispersion is dropped in and moisten 1 min on glass, then by base
Bottom rotates 1 min with 600 r/min rotating speeds, so that solution is well dispersed in substrate, then rotates 1 with 800 r/min rotating speeds again
Min, makes the film thining of formation, finally rotates 1 min with 1600 r/min rotating speeds, accelerates solvent evaporation, so that thin film is become dry.Oxygen
Graphite alkene thin film adopts a step reducing process. and reducing agent is respectively hydrazine steam and HI solution.One step reducing process is respectively hydrazine
60 DEG C of process 24h of steam, 100 DEG C of process 3 h of HI solution, graphene oxide film is reduced into graphene film, reduction-oxidation
Graphene film is through deionized water and ethanol purge, 80 DEG C of drying 24 h.
（10）The preparation of electrode：In the metallic aluminium that graphenic surface evaporation about 60 nm is thick.By under inert gas shielding
After annealing（150 DEG C of baking 5 min）.Obtain the flexible heterojunction solar battery battery of structure as shown in Fig. 1：Metal Al
Gate electrode layer 1, Graphene transparency conducting layer 2, LiF 3, MoS2Electron hole excitation layer 4, MoO3Hole transmission layer,
Al dorsum electrode layer 6, polyimide flex substrate 7.
Table 1 is MoO3/MoS2The preparation method embodiment of/LiF flexibility heterojunction solar battery, as shown in table 1 below.
Table one
The invention discloses a kind of MoO3/MoS2/ LiF flexibility heterojunction solar battery and preparation method, MoS2Using CVD
In-situ sulphiding formation, simultaneously to MoO3Layer is annealed, and efficiently utilizes the MoO of spin coating3The loose feature of Rotating fields is permissible
Reduce MoO3Hole transmission layer and MoS2Boundary defect between layer, decreases interface pollution；To lining during heat radiation evaporation LiF layer
The heating at bottom, also serves as to MoS2The process annealing of layer, optimizes MoS2Rotating fields decrease preparation technology；Relatively thin hole
Transport layer and electron transfer layer thickness, on the one hand decrease series resistance, on the other hand achieve and MoS2, the two dimension such as Graphene
Stratified material forms good flexibility heterojunction solar battery.MoO3/MoS2/ LiF flexibility heterojunction solar battery, with respect to
MoS2/ Si heterojunction solar battery, preparation cost has and obvious reduces and possess broader practice prospect；With respect to having
Machine polymer solar battery, stability, life-span and efficiency all increase, cheap and easily prepared and development and application.
The method is simple, low cost, and controllability is strong, has a good application prospect.
Be the present invention to be further described above in conjunction with the embodiments, this description be intended merely to better illustrate the present invention and not
It is to be limited.The present invention is not limited to particular example as described herein and embodiment.Skill in any this area
Art personnel are easy to be further improved without departing from the spirit and scope of the present invention and perfect, both fall within this
Bright protection domain.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should comprise
Within protection scope of the present invention.
Claims (10)
1. a kind of MoO3/MoS2/ LiF flexibility heterojunction solar battery is it is characterised in that include flexible substrate (7), the metal back of the body
Pole (6), hole transmission layer (5), inorganic electronic hole excitation layer (4), electron transfer layer (3), transparency conducting layer (2), metal gate
Pole (1), wherein, described electron hole excitation layer is MoS2.
2. flexibility heterojunction solar battery according to claim 1 is it is characterised in that described hole transmission layer is
MoO3, described electron transfer layer is LiF.
3. flexibility heterojunction solar battery according to claim 1 and 2 is it is characterised in that described flexible substrate is
Polyimides, described transparency conducting layer is Graphene.
4. flexibility heterojunction solar battery according to claim 1 and 2 is it is characterised in that affiliated metal backplane is
Al or Ag, metal gates are Al or Ag.
5. the flexible heterojunction solar battery according to claim 1-4 is it is characterised in that described metal Al backplane（6）
Thickness is 50-100 nm；MoO3Layer（5）Thickness is 10-80 nm；MoS2Layer (4) thickness 0.65-1.5 nm；LiF layer（3）Thickness
For 1.5-5 nm；Graphene layer (2) thickness is 0.5-2 nm；Al grid layer (1) thickness is 50-100 nm.
6. as claimed in one of claims 1-5 described flexibility heterojunction solar battery preparation method it is characterised in that
Comprise the steps：
(1) clean flexible substrate and dry；
(2) with vacuum coating equipment by the way of thermal evaporation evaporating Al thin film on flexible substrates；
(3) prepare MoO3Solution, and with sol evenning machine be spin-coated on steaming have in the flexible substrate of Al film；
(4) in horizontal pipe stove, CVD In-situ sulphiding generation MoS2Layer is simultaneously to MoO3Layer is annealed, in MoO3Above layer
Form MoS2Electron hole excitation layer；
(5) vacuum coating equipment by the way of thermal evaporation in MoS2LiF is deposited with layer；
(6) sol evenning machine is utilized to adopt the method for spin coating to form Graphene transparency conducting layer above LiF；
(7) vacuum coating equipment is deposited with mask above Graphene transparency conducting layer by the way of thermal evaporation and forms grid electricity
Pole.
7. preparation method as claimed in claim 6 is it is characterised in that prepare solwution method MoO3And be spin-coated to steaming have the soft of Al film
Property substrate formed MoO3Layer flow process be：
(1) by 0.4 g (NH4)6Mo7O24·4H2O is dissolved in 10 ml deionized waters, and adds a small amount of hydrochloric acid solution；
(2) by step（1）In the solution that obtains in atmosphere with 80 DEG C of heating 1 h；
(3) by step（2）In remaining solution deionized water be diluted to the solution of 1-8 mg/mL mass ratio；
(4) by step（3）In the solution that obtains in sol evenning machine with rotating speed spin coating 30 s of 3000 r/min.
8. preparation method as claimed in claim 6, is characterized in that, the In-situ sulphiding generation MoS of described CVD2Layer is simultaneously to MoO3
The flow process annealed of layer be：
(1) quartz boat filling 100 mg-500 mg sulphur powders is placed in stove central authorities, spin coating is had MoO3Print be placed in heating furnace
The dirty low-temperature space of quartz ampoule vent, is filled with protective gas Ar gas 10-15 min with emptying air to quartz ampoule, then heats
To 120 DEG C -150 DEG C, wherein, Ar throughput is 10-100 sccm to quartz ampoule；
(2) keep above-mentioned Ar throughput constant, with 3 DEG C/min-5 DEG C/min slow heating quartz ampoule to 180 DEG C -200 DEG C, permanent
It is cooled to room temperature after warm 5-30 min.
9. preparation method as claimed in claim 6 is it is characterised in that the flow process of spin coating Graphene transparency conducting layer is：
(1) weigh graphite oxide, make the graphene oxide solution that mass concentration is 1-8 mg/mL respectively；
(2) spin coating is carried out using sol evenning machine, first by graphene oxide dispersion drop on glass moisten 1 min, then by substrate with
600 r/min rotating speeds rotate 1 min, so that solution is well dispersed in substrate, then rotate 1 min with 800 r/min rotating speeds again,
Make the film thining of formation, finally rotate 1 min with 1600 r/min rotating speeds, accelerate solvent evaporation, so that thin film is become dry；
(3) graphene oxide film adopts a step reducing process, and reducing agent is respectively hydrazine steam and HI solution, a step reducing process
It is respectively 60 DEG C of process 24h of hydrazine steam, 100 DEG C of process 3 h of HI solution, graphene oxide film is reduced into graphene film,
Oxidation graphene film, through deionized water and ethanol purge, dries 24 h for 80 DEG C.
10. battery preparation method as claimed in claim 6 is it is characterised in that LiF and MoO3Purity be the sulfur more than 99.5%
The purity of powder S is more than 99.95%.
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