CN107123739A - A kind of non-lead bismuthino perovskite solar cell light absorption layer and preparation method thereof - Google Patents
A kind of non-lead bismuthino perovskite solar cell light absorption layer and preparation method thereof Download PDFInfo
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- CN107123739A CN107123739A CN201710416978.XA CN201710416978A CN107123739A CN 107123739 A CN107123739 A CN 107123739A CN 201710416978 A CN201710416978 A CN 201710416978A CN 107123739 A CN107123739 A CN 107123739A
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- -1 bismuthino Chemical group 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000031700 light absorption Effects 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 11
- 150000004820 halides Chemical class 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 7
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 claims abstract description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 4
- 239000011630 iodine Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- QEZYDNSACGFLIC-UHFFFAOYSA-N CN.[I] Chemical compound CN.[I] QEZYDNSACGFLIC-UHFFFAOYSA-N 0.000 claims abstract description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 33
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000004528 spin coating Methods 0.000 claims description 15
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 8
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 5
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 claims description 3
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims 3
- 229940113088 dimethylacetamide Drugs 0.000 claims 3
- 239000010408 film Substances 0.000 abstract description 30
- 239000010409 thin film Substances 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000012876 topography Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 229910001451 bismuth ion Inorganic materials 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000009466 transformation Effects 0.000 description 4
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- FBIVEKSMUKWRPT-UHFFFAOYSA-N [BiH2][Ca] Chemical compound [BiH2][Ca] FBIVEKSMUKWRPT-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- CVOFKRWYWCSDMA-UHFFFAOYSA-N 2-chloro-n-(2,6-diethylphenyl)-n-(methoxymethyl)acetamide;2,6-dinitro-n,n-dipropyl-4-(trifluoromethyl)aniline Chemical compound CCC1=CC=CC(CC)=C1N(COC)C(=O)CCl.CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O CVOFKRWYWCSDMA-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- ANAWAQLSSZCNNF-UHFFFAOYSA-N [Ti].[BiH2][Ca] Chemical compound [Ti].[BiH2][Ca] ANAWAQLSSZCNNF-UHFFFAOYSA-N 0.000 description 1
- FGQDLCIITXBKAR-UHFFFAOYSA-K bismuth;triiodate Chemical compound [Bi+3].[O-]I(=O)=O.[O-]I(=O)=O.[O-]I(=O)=O FGQDLCIITXBKAR-UHFFFAOYSA-K 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- 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
- Y02E10/549—Organic PV cells
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- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Non-lead bismuthino perovskite solar cell light absorption layer film prepared the invention discloses a kind of gas phase assisted solution method and preparation method thereof.Non-lead bismuthino perovskite light absorbing layer surface compact prepared by the gas phase assisted solution method, homogeneous grain size, particle diameter are about that 200 300nm, film thickness are 300nm or so.Its preparation method is：The halide solution of bismuth is spin-coated on substrate by solwution method first, then the substrate of halide of the steam that the mixture of iodide powder iodine methylamine, iodine methyl ether and the one or two kinds of in cesium iodide is produced with scribbling bismuth is recycled to be reacted, obtain surface compact, the non-lead bismuthino perovskite light absorbing layer film of homogeneous grain size.The present invention effectively improves the surface topography of non-lead bismuthino perovskite light absorbing layer by using gas phase assisted solution method, makes its transmission advantageously in carrier, and thin film preparation process flow is simple, controllability strong, product repeatability is high.
Description
Technical field
The invention belongs to technical field of solar cells, and in particular to non-lead bismuthino calcium prepared by a kind of gas phase assisted solution method
Titanium ore solar cell light absorption layer and preparation method thereof.
Background technology
In recent years, the lead base halide perovskite battery of organic inorganic hybridization is got the attention.It is 2009, Japanese
DSC expert Miyasaka etc. will have ABX first3The lead base halide hydridization perovskite material (CH of type3NH3PbI3) it is used as light
Absorbed layer is applied on dye-sensitized solar cells, realizes 3.8% photoelectric transformation efficiency (PCE).By short 7 years,
Light absorbs are used as using lead-based perovskite through the certification of regenerative resource National Laboratory of the U.S., Korea Research Institute of Chemical Technology within 2016
The photoelectric transformation efficiency of perovskite solar cell prepared by layer material is up to 22.1%.Although all perovskite sun are electric at present
Chi Zhong, the battery efficiency highest using lead base halide perovskite as light-absorption layer, but lead element is poisonous, and easily environment is caused
Pollution, injury is produced to human body, in addition, the problems such as lead base halide perovskite material property stable in the air is poor, all
It strongly limit its application.Therefore, in order to further expand the technology of preparing of perovskite thin film, it is necessary to develop non-lead perovskite material
Material, and then obtain high stable, nontoxic, efficient perovskite solar cell.Wherein, the bismuth element of V races is a kind of preferably replacement
Pb and then the element for constituting perovskite material, Bi is nontoxic, will not be oxidized, and Bi based perovskites material is with Pb based perovskite material phases
Than with more excellent environmental stability, therefore cause the very big concern of researchers.
B.W.Park et al. is prepared for being based on MA using a step solwution method3Bi2I9And Cs3Bi2I9Solar cell, perovskite
Film surface uniformity is very poor in the network structure being connected with each other, and battery realizes 0.12% and 1.09% opto-electronic conversion effect
Rate.M.Q.Lyu et al. is equally based on a step solwution method in thicker mesoporous TiO2MA is prepared on layer3Bi2I9The perovskite sun
Battery, its photoelectric transformation efficiency is also only 0.19%.H.Z.Chen team systematically have studied precursor solution in solwution method
The influence to battery performance of concentration and substrate, be prepared for structure I TO/c-TiO2/meso-TiO2/A3Bi2I9/Spiro-
MeOTAD/MoO3/ Ag solar cell so that the photoelectric transformation efficiency of battery has obtained larger raising, up to
0.42%.
Although the non-lead bismuthino perovskite efficiency of solar cell prepared at present by a step solwution method reaches 0.42%,
Perovskite surface prepared by this method often forms a kind of network structure of interconnection, and film surface is very coarse and exists big
The pin hole of amount, this uneven film surface substantially increases Carrier recombination probability, and this is also influence non-lead bismuthino calcium
The matter of utmost importance of titanium ore battery performance lifting.In view of the above-mentioned problems, the present invention prepares non-lead by using gas phase assisted solution method
Bismuthino perovskite light absorbing layer film, compared with the film prepared using solwution method, film shows that pattern has obtained very big improvement,
Its surface compact, homogeneous grain size is conducive to the transmission of carrier, and preparation technology flow is simple, controllability strong, product
Repeatability is high.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of easy to operate, repetitive rate is high, surface is caused
Preparation method that is close, being conducive to the good non-lead bismuthino perovskite solar cell light absorption layer of carrier transport, crystallinity.
The concrete technical scheme of the present invention is as follows：
A kind of non-lead bismuthino perovskite solar cell light absorption layer prepared by gas phase assisted solution method, its surface compact is brilliant
Grain is uniform in size, and particle diameter is about 200-300nm, and film thickness is 300nm or so.
The preparation method of above-mentioned non-lead bismuthino perovskite solar cell light absorption layer, comprises the following steps：
(1) halide (BiX of bismuth is weighed3) solid powder, it is dissolved in organic solvent, is fully stirred on heating stirring platform
Mix, it is stand-by after filtering；
(2) step (1) resulting solution is spin-coated on the FTO substrates covered with electron transfer layer, spin coating is stood after terminating,
Place it on warm table and heat after standing.
(3) by after film natural cooling obtained by step (2), it is placed in culture dish, and uniform paving spills iodine around film
Compound powder；
(4) culture dish described in step (3) is placed in vacuum drying chamber, vacuum drying chamber is evacuated to low pressure and added
Heat, heating terminates rear natural cooling；
(5) film obtained by step (4) is cleaned with isopropanol and dried with sol evenning machine, then added on warm table
Heat, you can non-lead bismuthino perovskite solar cell light absorption layer is made.
Further, the halide of bismuth described in step (1) is bismuth chloride (BiCl3), bismuth bromide (BiBr3), bismuth iodide
(BiI3) in one or two kinds of mixture, solvent be DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO),
The mixture of gamma-butyrolacton (GBL) and the one or two kinds of in DMA (DMAC), the temperature of the heating
For 50-80 DEG C, the time of the stirring is 6-12h.
Further, the concentration of spin coating solution described in step (2) is 0.4-1.2mmol/mL, and the amount of spin coating is 30-50 μ L,
Spin coating rotating speed is 2000-5000rpm, and spin-coating time is 20-50s, and time of repose is 5-20min, and heating-up temperature is 50-150 DEG C.
Further, iodide described in step (3) are one in iodine methylamine (MAI), iodine methyl ether (FAI), cesium iodide (CsI)
Kind or two kinds of mixture, the iodide powder quality are 0.15-0.4g.
Further, the low pressure of vacuum drying chamber described in step (4) is 1-20KPa, and the temperature of the heating is 150-170
DEG C, the time of the heating is 10-120min.
Process is dried described in step (5) and uses sol evenning machine, rotating speed is 2000-5000rpm, and rotational time is 10-30s,
The temperature of the heating is 100-170 DEG C, and the time of the heating is 3-10min.
The present invention develops a kind of gas phase assisted solution method and prepares non-lead bismuthino perovskite solar cell light absorption layer film
Method, the perovskite optical thin film surface compact prepared by this method, homogeneous grain size, carrier transport can be effectively improved
Performance, and then improve the photoelectric properties of battery.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of bismuth iodide film surface prepared by the embodiment of the present invention 1.
The scanning electron for the perovskite light absorbing layer that Fig. 2 is prepared for iodate bismuth thin film in Fig. 1 after vapor phase method is handled shows
Micro mirror photo.
Fig. 3 is the AFM figures on non-lead bismuthino perovskite light absorbing layer surface prepared by the embodiment of the present invention 1.
Fig. 4 is the X-ray diffractogram of non-lead bismuthino perovskite light absorbing layer prepared by the embodiment of the present invention 1.
Embodiment
The present invention is described and illustrated in more detail with reference to specific embodiment, but those skilled in the art understand
, these embodiments are only used for illustrating the present invention, and it does not constitute any limitation to the scope of the present invention.Used in embodiment
Implementation condition further adjustment can be done according to actual conditions, unreceipted condition is usually the condition in normal experiment, with
Under illustrated by embodiment the present invention specific implementation process.
Embodiment 1
By 1mmol BiI3It is dissolved in 1mL DMF solution, the heating stirring 6h on 70 DEG C of heating stirring platform, gained is molten
The concentration of bismuth ion is 1mmol/mL in liquid.Solution is filtered using 0.22 μm of filtering head.40 μ L mistakes are taken with liquid-transfering gun
Solution after filter is dropped on the FTO substrates covered with electron transfer layer, uses sol evenning machine to rotate film with 3000rpm rotating speed
30s.Spin coating completes back substrate and stands 10min, then is placed on 70 DEG C of warm table and heats 30min, and natural cooling.By substrate
It is placed in clean culture dish, weighs 0.2g MAI powder, be equably sprinkled upon substrate perimeter.It is 10KPa, temperature in pressure
In 150 DEG C of vacuum drying chambers, to heat 30min and being cooled to room temperature under air.The substrate for generating film is placed on different
5s is embathed in propanol solution, is subsequently placed on sol evenning machine and 10s is rotated with 3000rpm rotating speeds, finally the substrate with film
5min is heated on the warm table for being placed on 150 DEG C, room temperature is cooled to after removing.
Pass through its table of the non-lead bismuthino perovskite light absorbing layer of gas phase assisted solution method preparation it can be seen from Fig. 1 and Fig. 2
Face densification, homogeneous grain size, particle diameter are about 200-300nm；As seen from Figure 3, the non-lead bismuthino calcium titanium that prepared by this method
Ore deposit light absorbing layer surfacing, roughness very little；Figure 4, it is seen that the knot of non-lead bismuthino perovskite prepared by this method
Brilliant performance is fine.
Embodiment 2
By 1.2mmol BiI3It is dissolved in 0.2mL DMF and 0.8mL DMSO mixed solutions, in 60 DEG C of heating stirring
The concentration of bismuth ion is 1.2mmol/mL in heating stirring 6h on platform, resulting solution.Filtering head using 0.22 μm enters to solution
Row filtering.With liquid-transfering gun take 35 μ L filter after solution drop on the FTO substrates covered with electron transfer layer, use sol evenning machine with
Film is rotated 30s by 3000rpm rotating speed.Spin coating completes back substrate and stands 10min, then is placed into heating on 70 DEG C of warm table
30min, and natural cooling.Substrate is placed in clean culture dish, weighed mixed comprising 0.15g MAI and 0.15g FAI
Powder is closed, substrate perimeter is equably sprinkled upon.It is 10KPa in pressure, temperature is in 150 DEG C of vacuum drying chamber, heating 30min is simultaneously
Room temperature is cooled under air.The substrate for generating film is placed in aqueous isopropanol and embathes 5s, sol evenning machine is subsequently placed at
On with 3000rpm rotating speeds rotate 25s, finally the substrate with film is placed on 150 DEG C of warm table and heats 3min, is removed
After be cooled to room temperature.
Embodiment 3
By 0.2mmol BiI3With 0.8mmol BiCl3It is dissolved in 1mL DMF solution, on 70 DEG C of heating stirring platform
Heating stirring 6h, the concentration of resulting solution bismuth ion is 1mmol/mL.Solution is filtered using 0.22 μm of filtering head.With
Liquid-transfering gun takes the solution after 40 μ L filterings to drop on the FTO substrates covered with electron transfer layer, uses sol evenning machine with 3000rpm's
Film is rotated 30s by rotating speed.Spin coating completes back substrate and stands 20min, then is placed on 70 DEG C of warm table and heats 30min, and
Natural cooling.Substrate is placed in clean culture dish, weighs 0.2g MAI powder, be equably sprinkled upon substrate perimeter.In pressure
It is 15KPa by force, temperature is in 160 DEG C of vacuum drying chamber, heats 35min and is cooled to room temperature in atmosphere.Film will be generated
Substrate be placed in aqueous isopropanol and embathe 5s, be subsequently placed on sol evenning machine and 10s rotated with 3000rpm rotating speeds, finally handle
Substrate with film is placed on 100 DEG C of warm table and heats 5min, and room temperature is cooled to after removing.
Embodiment 4
By 0.5mmol BiI3It is dissolved in 0.8mL DMF and 0.2mL GBL mixed solutions, in 70 DEG C of heating stirring
The concentration of bismuth ion is 0.5mmol/mL in heating stirring 6h on platform, resulting solution.Filtering head using 0.22 μm enters to solution
Row filtering.With liquid-transfering gun take 45 μ L filter after solution drop on the FTO substrates covered with electron transfer layer, use sol evenning machine with
3000rpm rotating speed rotation 30s.Spin coating completes back substrate and stands 10min, then is placed into heating on 150 DEG C of warm table
30min, and natural cooling.Substrate is placed in clean culture dish, weighs 0.2g MAI powder, be equably sprinkled upon substrate
Around.In the vacuum drying chamber that pressure is 10KPa, temperature is 150 DEG C, heat 35min and be cooled to room temperature under air.Will
The substrate of generation film, which is placed in aqueous isopropanol, embathes 5s, is subsequently placed on sol evenning machine and is rotated with 3000rpm rotating speeds
20s, is finally placed on the substrate with film on 150 DEG C of warm table and heats 5min, room temperature is cooled to after removing.
Embodiment 5
By 0.7mmol BiI3With 0.3mmol BiBr3It is dissolved in 0.5mL DMF and 0.5mL DMAC mixed solutions,
The concentration of bismuth ion is 1mmol/mL in the heating stirring 12h on 80 DEG C of heating stirring platform, resulting solution.With 0.22 μm of mistake
Filter is filtered to solution.The solution after 40 μ L filterings is taken to drop on the FTO substrates covered with electron transfer layer with liquid-transfering gun,
Sol evenning machine is used to rotate 40s with 3000rpm rotating speed.Spin coating completes back substrate and stands 10min, then is placed into 70 DEG C of warm table
Upper heating 10min, and natural cooling.Substrate is placed in clean culture dish, weighs 0.2g MAI powder, equably spill
In substrate perimeter.It is 10KPa in pressure, temperature is in 150 DEG C of vacuum drying chamber, heating 35min is simultaneously cooled under air
Room temperature.The substrate for generating film is placed in aqueous isopropanol and embathes 5s, is subsequently placed on sol evenning machine with 2500rpm rotating speeds
10s is rotated, finally the substrate with film is placed on 120 DEG C of warm table and heats 5min, room temperature is cooled to after removing.
Embodiment 6
By 1mmol BiI3It is dissolved in 1mL DMF solution, the heating stirring 6h on 70 DEG C of heating stirring platform, gained is molten
The concentration of bismuth ion is 1mmol/mL in liquid.Solution is filtered with 0.22 μm of filtering head.35 μ L are taken to filter with liquid-transfering gun
Solution afterwards is dropped on the FTO substrates covered with electron transfer layer, uses sol evenning machine to rotate 30s with 3000rpm rotating speed.Spin coating
After the completion of substrate stand 10min, then be placed on 70 DEG C of warm table and heat 30min, and natural cooling.Substrate is placed on
In clean culture dish, the mixed-powder for including 0.15g MAI and 0.1g CsI is weighed, substrate perimeter is equably sprinkled upon.In pressure
Strong is 20KPa, in the vacuum drying chamber that temperature is 150 DEG C, and heating 50min is simultaneously cooled to room temperature in atmosphere.Film will be generated
Substrate be placed in aqueous isopropanol and embathe 5s, be subsequently placed on sol evenning machine and 10s rotated with 3000rpm rotating speeds, finally will
Substrate with film is placed on 75 DEG C of warm table and heats 5min, and room temperature is cooled to after removing.
Claims (7)
1. non-lead bismuthino perovskite solar cell light absorption layer prepared by a kind of gas phase assisted solution method, it is characterised in that described
Light absorbing layer surface compact, homogeneous grain size, particle diameter is about 200-300nm, and film thickness is 300nm or so.
2. a kind of preparation method of non-lead bismuthino perovskite solar cell light absorption layer according to claim 1, its feature exists
In specifically including following steps：
(1) the halide solid powder of bismuth is weighed, is dissolved in organic solvent, it is stand-by after heating stirring and filtering；
(2) step (1) resulting solution is spin-coated on the FTO substrates covered with electron transfer layer, obtains BiX3Film is simultaneously stood,
Then heat；
(3) by after film natural cooling obtained by step (2), it is placed in culture dish, and uniform paving spills iodide around film
Powder；
(4) culture dish described in step (3) is placed in vacuum drying chamber, vacuum drying chamber is evacuated to low pressure and heated,
Heating terminates rear natural cooling；
(5) film obtained by step (4) is cleaned, dried, non-lead bismuthino perovskite solar cell light absorbs are made in heating
Layer.
3. preparation method according to claim 2, it is characterised in that the halide of bismuth described in step (1) is bismuth chloride
(BiCl3), bismuth bromide (BiBr3) and bismuth iodide (BiI3) in one or two kinds of mixture, the organic solvent be N, N-
In dimethylformamide (DMF), dimethyl sulfoxide (DMSO) (DMSO), gamma-butyrolacton (GBL) and DMAC N,N' dimethyl acetamide (DMAC)
The mixture of one or two kinds of, the temperature of the heating is 50-80 DEG C, and the time of the stirring is 6-12h.
4. preparation method according to claim 2, it is characterised in that the concentration of spin coating solution is described in step (2)
0.4-1.2mmol/mL, the amount of spin coating is 30-50 μ L, and spin coating rotating speed is 2000-5000rpm, and spin-coating time is 20-50s, is stood
Time is 5-20min, and heating-up temperature is 50-150 DEG C.
5. preparation method according to claim 2, it is characterised in that iodide described in step (3) are iodine methylamine
(MAI), iodine methyl ether (FAI), the mixture of one or two kinds of in cesium iodide (CsI), the iodide powder quality is
0.15-0.4g。
6. preparation method according to claim 2, it is characterised in that the low pressure of vacuum drying chamber is described in step (4)
1-20KPa, the temperature of the heating is 150-170 DEG C, and the time of the heating is 10-120min.
7. preparation method according to claim 2, it is characterised in that the process that dried described in step (5) uses sol evenning machine,
Rotating speed is 2000-5000rpm, and rotational time is 10-30s, and the temperature of the heating is 100-170 DEG C, the time of the heating
For 3-10min.
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| CN105820055A (en) * | 2016-01-25 | 2016-08-03 | 湖北大学 | Methyl amino lead iodide bismuth perovskite crystal light absorption layer material and preparation method thereof |
| WO2017009688A1 (en) * | 2015-07-13 | 2017-01-19 | Tubitak | Perovskite thin film production method and optoelectronic device |
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| WO2017009688A1 (en) * | 2015-07-13 | 2017-01-19 | Tubitak | Perovskite thin film production method and optoelectronic device |
| CN105820055A (en) * | 2016-01-25 | 2016-08-03 | 湖北大学 | Methyl amino lead iodide bismuth perovskite crystal light absorption layer material and preparation method thereof |
| CN106601917A (en) * | 2016-12-02 | 2017-04-26 | 广州光鼎科技有限公司 | Preparation method of lead-free organic and inorganic cation common hybridization perovskite material and film thereof |
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