CN104600197B - A kind of preparation method without hole mobile material perovskite thin film hetero-junction solar cell - Google Patents
A kind of preparation method without hole mobile material perovskite thin film hetero-junction solar cell Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims abstract description 12
- 239000010409 thin film Substances 0.000 title claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002002 slurry Substances 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000004528 spin coating Methods 0.000 claims abstract description 19
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 15
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 9
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 claims abstract description 9
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000010408 film Substances 0.000 claims description 20
- 239000002159 nanocrystal Substances 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 239000006193 liquid solution Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 239000012298 atmosphere Substances 0.000 abstract description 6
- 239000002243 precursor Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004078 waterproofing Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000005538 encapsulation Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000009466 transformation Effects 0.000 description 7
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 208000032953 Device battery issue Diseases 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2059—Light-sensitive devices comprising an organic dye as the active light absorbing material, e.g. adsorbed on an electrode or dissolved in solution
-
- 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
- Y02E10/542—Dye sensitized solar cells
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Photovoltaic Devices (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method without hole mobile material perovskite thin film hetero-junction solar cell.The method is in traditional PbI2A small amount of PbCl is added in precursor solution2, to improve PbI2Dissolubility in a solvent, in order to avoid uneven nucleus is formed in spin coating, affects the uniformity of perovskite growth.100 DEG C of sintering scratched upper one kind toward on calcium titanium ore bed and contain CH after 5 minutes in atmosphere3NH3The carbon slurry of I, in atmosphere 100 DEG C of drying scratch last layer again and do not contain CH3NH3The carbon of I is starched to reduce device resistance.The toluene solution of last 50mg/mL PMMA is uniformly dropped on carbon electrode, and dries in atmosphere to reach the effect of encapsulation battery in 100 DEG C.Battery prepared by the present invention has obtained 12.21% peak efficiency and 11.2%（s.d. 1.02）Average efficiency, and a month internal efficiency is without being decreased obviously.This photovoltaic device also shows superior water proofing property simultaneously.
Description
Technical field
The present invention relates to a kind of preparation method without hole mobile material perovskite thin film hetero-junction solar cell, belongs to photovoltaic device
Part technical field.
Background technology
Based on the full solid thin film solaode of perovskite material be one kind by all-solid-state dye-sensitized solar cell
Cheap, the high performance novel photovoltaic device for developing.Notarization efficiency has been promoted to 20.1% at present, and the record has exceeded light
The photoelectric transformation efficiency of the crystal silicon solar batteries product dominated on volt market.Additionally, with conventional solar cell phase
Than its main advantage also has：With low cost, Technology is relatively easy, and plasticity is strong, has broad application prospects.But
The organic hole transport material such as spiro-OMeTAD generally adopted by traditional perovskite solaode is expensive, cost
More than 10 times of golden or platinum, while also needing to prepare gold or silver-colored electricity using evaporation or sputtering method under fine vacuum high energy consumption environment
Pole, so as to inevitably destroy the integrity of device architecture, causes shorted devices, device poor repeatability.Further, since calcium titanium
Ore deposit this core material is easily caused battery failure by the water decomposition in air, and the research of its water proofing property and long-time stability is also very
Urgently.
The content of the invention
The technical problem to be solved is to provide a kind of without hole mobile material perovskite thin film hetero-junctions electricity
The preparation method in pond, the method have synthesized high-quality calcium titanium ore bed first with improved two-step method, and then secondary coating is different
Carbon pastes, finally encapsulated with PMMA, obtained efficiently, stable, the perovskite battery of waterproof.
For the series of problems of existing perovskite battery, we have invented a kind of method that is simple, easily repeating to produce
It is a kind of based on the efficient, cheap, stable of carbon electrode, the perovskite battery without hole mobile material of waterproof.We utilize first
Improved two steps spin-coating method has synthesized high-quality calcium titanium ore bed, compared to the two step spin-coating methods reported by document before, I
In PbI2A small amount of PbCl is added in precursor liquid2To improve PbI2Dissolubility, improve the success rate of high efficiency battery.Separately
Outward, cheap business carbon slurry is mixed into CH by us3NH3Directly coat with calcium titanium ore bed after I, can effectively prevent slurry molten
Agent is destroyed to which, improves perovskite/carbon electrode interface.Subsequently, without CH3NH3The carbon slurry of I applies electric coated with device is reduced again
Resistance.The method of this secondary coating carbon electrode is pioneering at present.Finally, we with solwution method battery surface be prepared for PMMA prevent
Water layer, so as to reach packaging effect, substantially increases the water resistance and stability of battery.
The preparation method without hole mobile material perovskite thin film hetero-junction solar cell of the present invention, comprises the steps of：
(1)TiO2The preparation of nano-crystal film substrate；
(2) preparation of calcium titanium ore bed：PbCl containing 0.2M2With 0.6～2.0M PbI2DMF solution in 70 DEG C stir 1h make
For precursor solution, then 6000RPM 30s are spun on TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, it is cooled to room
Temperature, the CH of 7mg/mL3NH3I aqueous isopropanol Deca is in TiO2In nano-crystal film substrate, after reaction 20s, 2000rpm 20s rotations
Apply and dry, then 100 DEG C of sintering 5min, form uniform black thin film；
(3) preparation of carbon electrode：By oiliness carbon starch 120 DEG C at dry, will contain 0.575g/ml dried carbons slurry and 0.005～
0.0375g/mlCH3NH3The chlorobenzene of I is put into ball milling in ball grinder, then uniformly scratches in (2) on gained perovskite thin film,
100 DEG C are dried, and coat the chlorobenzene of the slurry of dried carbon containing 0.575g/ml again, and 100 DEG C are dried；
(4) preparation of encapsulated layer：The toluene solution of uniform Deca 50mg/ml PMMA on carbon-coating obtained by (3), 100 DEG C of bakings
It is dry.
TiO2The preparation process of nano-crystal film substrate is as follows：By 0.15M C16H28O6The butanol solution of Ti is spun on quarter
On the FTO glass for having lost, 150 DEG C of heating 30min, then by TiO2Slurry (1:3 mass ratioes are diluted in ethanol) 2000rpm
Thereon, 450 DEG C sinter 30min, 40mM TiCl for 20s spin coatings4Middle immersion, 30min at 70 DEG C, 500 DEG C sinter 30min again.
TiO2Slurry is TiO2By 1:3 mass ratioes dilute gained in ethanol.
The inventive method is first with a kind of improved two steps spin-coating method in TiO2In nano-crystal film substrate in priority spin coating
PbI2/PbCl2And CH3NH3To form one layer of uniform, high coverage rate perovskite light absorbent, its innovation is I solution
In traditional PbI2A small amount of PbCl is added in precursor solution2, to improve PbI2Dissolubility in a solvent, in order to avoid in spin coating
Uneven nucleus is formed, the uniformity of perovskite growth is affected.In atmosphere 100 DEG C sintering 5 minutes after, toward on calcium titanium ore bed
On blade coating, one kind contains CH3NH3The carbon slurry of I, in atmosphere 100 DEG C of drying scratch last layer again and do not contain CH3NH3The carbon slurry of I.
Coating is containing CH for the first time3NH3The carbon of I is starched to protect perovskite/carbon interface, and second coating is without CH3NH3The carbon of I is starched to reduce
The resistance of device.
Perovskite battery prepared by the inventive method has obtained 12.21% peak efficiency and 11.2% (s.d.1.02)
Average efficiency, after placing one month in air indoors, this transformation efficiency declines little.In addition this photovoltaic device is also showed
Go out extremely superior water proofing property, after washing away under a tap 30 seconds and soaking 30 seconds in water, the efficiency of battery is remained respectively
98.2% originally and 92.47%.Meanwhile, during the independent film forming of this carbon electrode, good pliability is shown, following complete
There is good application prospect in flexible, wearable photovoltaic device.
The present invention has advantages below and beneficial effect：
1st, the calcium titanium ore bed of improved two-step method synthesis is more uniform complete, and directly simple in atmosphere can synthesize, can
It is repeated high.
2nd, without hole mobile material, cost is substantially reduced, and structure more simplifies, and repeatability is greatly improved.
What the 3rd, prepared by cheap carbon slurry does not need expensive vacuum coating equipment to electrode, and it is right to reduce while reduces cost
The infringement of internal material.
4th, naked layer, compares the similar battery structure delivered and reduces resistance, reduce thickness, and mechanism of being more convenient for is ground
Study carefully and long term growth.
Description of the drawings
Fig. 1 is the device transformation efficiency of embodiment of the present invention 1-5 i.e. with PbI2The efficiency trend graph that amount increases, and this
The device transformation efficiency of bright embodiment 3,6,7,8,9,10 is i.e. with CH in carbon pastes3NH3The efficiency trend graph that I amounts increase.
Fig. 2 be just assembled by the embodiment of the present invention 3 after and rinse 30s respectively under a tap and be soaked in 15min in water
I-V performance charts afterwards, and its transformation efficiency stability trend graph in one month.
Specific embodiment
The present invention, but the present embodiment limit not to its protection domain is explained in more detail below by way of some embodiments
System.
Oiliness carbon slurry is using cheap commercialization carbon slurry (ten JELCON CH-8 types industry conductive carbon pastes of Japan).
Embodiment 1
0.6M PbI2With 0.2M PbCl2It is dissolved in DMF (DMF) simultaneously, 70 DEG C are heated to whole dissolvings,
6000rpm 30s are spun on TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I
Thereon, after reaction 20s, 2000rpm 20s spin coatings are dried solution Deca, and then 100 DEG C of sintering 5min, dry containing 0.575g/ml
Dry industrial carbon slurry, 0.0125g/mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, the industrial carbon slurry of the drying containing 0.575g/ml,
0g/mLCH3NH3The chlorobenzene of I is scratched thereon again, and after 100 DEG C of drying, PMMA is uniformly coated on, and is dried.
Embodiment 2
0.8M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon,
After reaction 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, the industrial carbon slurry of the drying containing 0.575g/ml,
0.0125g/mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3I
Chlorobenzene scratch again thereon, 100 DEG C drying after PMMA uniformly coat on, dry.
Embodiment 3
1.2M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, the industrial carbon slurry of the drying containing 0.575g/ml,
0.0125g/mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3I
Chlorobenzene scratch again thereon, 100 DEG C drying after PMMA uniformly coat on, dry.
Embodiment 4
1.5M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, the industrial carbon slurry of the drying containing 0.575g/ml,
0.0125g/mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3I
Chlorobenzene scratch again thereon, 100 DEG C drying after PMMA uniformly coat on, dry.
Embodiment 5
2.0M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, the industrial carbon slurry of the drying containing 0.575g/ml,
0.0125g/mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3I
Chlorobenzene scratch again thereon, 100 DEG C drying after PMMA uniformly coat on, dry.
Embodiment 6
1.2M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, are dried industrial carbon slurry, 0g/ containing 0.575g/ml
mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3The chlorobenzene of I
Scratch again thereon, after 100 DEG C of drying, PMMA is uniformly coated on, and is dried, as control sample.
Embodiment 7
1.2M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, are dried industrial carbon slurry, 0.005g/ containing 0.575g/ml
mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3The chlorobenzene of I is again
Thereon, after 100 DEG C of drying, PMMA is uniformly coated on secondary blade coating, is dried.
Embodiment 8
1.2M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, are dried industrial carbon slurry, 0.010g/ containing 0.575g/ml
mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3The chlorobenzene of I is again
Thereon, after 100 DEG C of drying, PMMA is uniformly coated on secondary blade coating, is dried.
Embodiment 9
1.2M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, are dried industrial carbon slurry, 0.020g/ containing 0.575g/ml
mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3The chlorobenzene of I is again
Thereon, after 100 DEG C of drying, PMMA is uniformly coated on secondary blade coating, is dried.
Embodiment 10
1.2M PbI2With 0.2M PbCl2It is dissolved in DMF simultaneously, 70 DEG C are heated to whole dissolvings, and 6000rpm 30s are spun on
TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, cold room temperature processed, the CH of 7mg/mL3NH3I solution Deca thereon, instead
After answering 20s, 2000rpm 20s spin coatings are dried, then 100 DEG C of sintering 5min, the industrial carbon slurry of the drying containing 0.575g/ml,
0.0375g/mLCH3NH3The chlorobenzene of I is scratched thereon, 100 DEG C of drying, is dried industrial carbon slurry, 0g/mLCH containing 0.575g/ml3NH3I
Chlorobenzene scratch again thereon, 100 DEG C drying after PMMA uniformly coat on, dry.
The preparation flow of above-mentioned all embodiments is as shown in Figure 1；Perovskite electricity described in above-described embodiment 1,2,3,4,5
Shown in the transformation efficiency result such as Fig. 1 (a) in pond；The conversion effect of the perovskite battery described in above-described embodiment 3,6,7,8,9,10
Shown in rate result such as Fig. 1 (b)；30s is washed away before the battery of embodiment 3 is washed and under a tap respectively and is soaked in water
Transformation efficiency after 15min to such as Fig. 2 (a) Suo Shi, shown in the stabilised efficiency such as Fig. 2 (b) in embodiment 3 one months.
Test condition：Using the U.S. 91192 models of Oriel standard 500W simulated solar irradiation xenon lamp as light source, spoke
It is 100W/cm according to intensity2, battery is 0.114cm by illuminating area2。
Table 1
| PbI2Concentration (M) | 0.6 | 0.8 | 1.2 | 1.5 | 2.0 | —— |
| Battery efficiency (%) | 6.19 | 9.99 | 12.51 | 9.99 | 8.50 | —— |
| CH3NH3The addition (g) of I | 0 | 0.04 | 0.08 | 0.10 | 0.16 | 1.30 |
| Battery efficiency (%) | 7.30 | 9.80 | 11.16 | 12.51 | 11.35 | 9.89 |
Table 2
Fig. 1 (a) is as shown in table 1 with the concrete efficiency data corresponding to Fig. 1 (b), from table 1 it follows that embodiment 3
Battery prepared by formula is best performance；Concrete photovoltaic performance ginseng of the corresponding optimum battery before and after water process in Fig. 2 (a)
Number is as shown in table 2, illustrates that the battery prepared by the method for the present invention has very superior photovoltaic performance, and does not almost receive completely
The impact of water, and possess long-term stability, this has very big value in following commercial application.
Claims (3)
1. a kind of preparation method without hole mobile material perovskite thin film hetero-junction solar cell, comprises the steps of：
（1）TiO2The preparation of nano-crystal film substrate；
（2）The preparation of calcium titanium ore bed：PbCl containing 0.2M2With 0.6～2.0M PbI2DMF solution in 70 DEG C stir 1h as front
Liquid solution is driven, then 6000RPM 30s are spun on TiO2In nano-crystal film substrate, after 100 DEG C of baking 5min, it is cooled to room temperature,
The CH of 7mg/mL3NH3I aqueous isopropanol Deca is in TiO2In nano-crystal film substrate, after reaction 20s, 2000rpm 20s spin coatings
Dry, then 100 DEG C of sintering 5min, form uniform black thin film；
（3）The preparation of carbon electrode：By oiliness carbon starch 120 DEG C at dry, will contain 0.575g/ml dried carbons slurry and 0.005～
0.0375g/mlCH3NH3The chlorobenzene of I is put into ball milling in ball grinder, then uniformly scratch in（2）On middle gained perovskite thin film,
100 DEG C are dried, and coat the chlorobenzene of the slurry of dried carbon containing 0.575g/ml again, and 100 DEG C are dried；
（4）The preparation of encapsulated layer：In（3）The toluene solution of uniform Deca 50mg/ml PMMA on gained carbon-coating, 100 DEG C of drying.
2. preparation method according to claim 1, it is characterised in that TiO2The preparation process of nano-crystal film substrate is as follows：
By 0.15M C16H28O6The butanol solution of Ti is spun on the FTO glass for having etched, 150 DEG C of heating 30min, then will
TiO2Thereon, 450 DEG C sinter 30min, 40mM TiCl for slurry 2000rpm 20s spin coatings4Middle immersion, 30min at 70 DEG C, again
500 DEG C of sintering 30min.
3. preparation method according to claim 2, it is characterised in that TiO2Slurry is TiO2By 1:3 mass ratioes are in ethanol
Dilution gained.
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