CN109698280A - Application of the fullerene methylene derivatives I in perovskite solar battery, perovskite solar battery and preparation method thereof - Google Patents
Application of the fullerene methylene derivatives I in perovskite solar battery, perovskite solar battery and preparation method thereof Download PDFInfo
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- CN109698280A CN109698280A CN201811599985.9A CN201811599985A CN109698280A CN 109698280 A CN109698280 A CN 109698280A CN 201811599985 A CN201811599985 A CN 201811599985A CN 109698280 A CN109698280 A CN 109698280A
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- H—ELECTRICITY
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- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
- H10K85/211—Fullerenes, e.g. C60
- H10K85/215—Fullerenes, e.g. C60 comprising substituents, e.g. PCBM
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Abstract
The application and a kind of perovskite solar battery that the invention discloses a kind of fullerene methylene derivatives I in perovskite solar battery, including the conductive layer set gradually by layer structure, electron transfer layer, doped with the calcium titanium ore bed, hole transmission layer and electrode of fullerene methylene derivatives I.The application is by that in solar cells, can effectively raise the photovoltaic performance of solar battery for the application of fullerene methylene derivatives I.
Description
Technical field
The present invention relates to area of solar cell, and in particular to a kind of fullerene methylene derivatives I are in the perovskite sun
Application, perovskite solar battery in energy battery and preparation method thereof.
Background technique
Organic and inorganic perovskite solar battery is since 2009 report for the first time, between short several years, power
Transfer efficiency develops to current peak efficiency 23.3% from 3.8%, becomes the candidate of substitution silicon solar cell.
Perovskite solar battery has the advantages that low manufacturing cost, high photoelectric conversion efficiency, solution processable.
The fast development of its photoelectric conversion efficiency in recent years, which is attributed to, prepares film with big crystal grain and smooth surface and efficient
The development of electron transfer layer and hole transmission layer.The structure of perovskite solar battery mainly has meso-hole structure and plane heterogeneous
Junction structure.Planar heterojunction structure includes n-i-p structure and p-i-n structure again.So far, meso-hole structure is highest certification
The keeper of efficiency 23.3%, the highest authentication efficiency of planar structure n-i-p type are that the highest of 21.5%, p-i-n type authenticates effect
Rate is 20.9%.
The structure of traditional n-i-p type perovskite solar battery are as follows: electro-conductive glass/electron transfer layer/perovskite activity
Layer/hole transmission layer/electrode.
The excellent properties of perovskite solar battery have obtained the extensive concern of the worker of industry, in order to expand calcium titanium
The application field of mine solar battery needs to improve the photoelectric conversion efficiency of solar battery.
In the prior art, the method for improving the photoelectric conversion efficiency of solar battery is mostly complex, and cost of manufacture is high
It is high, such as:
Such as in traditional perovskite active layer FAPbI3Middle doping Cs ion, to control perovskite in annealing process
Phase transition mentions high phase purity.For another example the aqueous isopropanol dissolved with methimazole (MMI) is spun in perovskite film, is passed through
Form MMI-PbI2Compound effectively inhibits Ion transfer and inhibits the diffusion of metal electrode.
Or improved by synthesizing new hole mobile material perovskite solar battery photoelectricity dress change efficiency and
Stability.The hole mobile material for such as synthesizing fluorenes sealing end is applied in perovskite solar battery, realizes that battery device is good
Photoelectric conversion efficiency and stability.
It can be seen that in the prior art, require greatly it is higher at buying and synthesizing relevant decorative material originally, no
The condition for having large-scale production.And the synthetic method of associated materials is complex, and purification of products is difficult, further limits
Therefore how the application of the material designs a kind of preparation method, the lower method of cost of material is to improve solar battery
Photoelectric conversion efficiency, the problem of being this field urgent need to resolve.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of fullerene methylene derivatives I in perovskite solar-electricity
Application, perovskite solar battery in pond and preparation method thereof, the application is by applying fullerene methylene derivatives I
In solar cells, to effectively raise the photovoltaic performance of solar battery.
In order to solve the above technical problem, the present invention provides scheme be: fullerene methylene derivatives I are in perovskite
Fullerene methylene derivatives are entrained in the light that solar battery is improved in calcium titanium ore bed by the application in solar battery
Performance is lied prostrate, the structural formula of the fullerene methylene derivatives I is
The application further provides a kind of perovskite solar battery, leads including what is set gradually by layer structure
Electric layer, electron transfer layer, calcium titanium ore bed, hole transmission layer and electrode doped with fullerene methylene derivatives I, the richness
Strangle alkene methylene derivatives I structural formula be
Further, the conductive layer is ITO or FTO.
Further, the electron transfer layer is SnCl2.2H20, tin oxide, vapor deposition C60、TiO2, meso-porous titanium oxide,
[6.6] one or more of-phenyl-C61- methyl butyrate.
Further, the calcium titanium ore bed is MAPbI3、FAPbI3、CsPbI3、CsPbBr3、CsPbI2Br、
CsPbIBr2、MAPbI3-xClx、CsxFA1-xPbI3、MAPbI3-x-yBrxCly、(FAPbI3)x(MAPbBr3)1-x, one of or
It is several, wherein x=0-3, y=0-3；The calcium titanium ore bed with a thickness of 200-700nm.
Further, the hole transmission layer is to be doped with bis- (fluoroform) sulfimide lithium salts and 4- tert-butyl
One of the 2,2' of pyridine, 7,7'- tetra--(dimethoxy diphenylamines)-spiro fluorene, poly- (3- hexyl thiophene), triphen amine polymer
Or it is several.
Further, the electrode is one or more of gold, silver, copper or aluminium.
The application further provides a kind of preparation method of above-mentioned perovskite solar battery: includes the following steps,
S1, electron transfer layer is formed in the conductive substrates；
S2, formation surface doping has fullerene sub- on the surface far from the conductive substrates of the electron transfer layer
The calcium titanium ore bed of methyl-derivatives I；
S3, on the calcium titanium ore bed doped with fullerene methylene derivatives I far from the electron transfer layer one
Face forms hole transmission layer；
S4, electrode is formed on surface of the hole transmission layer far from the calcium titanium ore bed, obtains perovskite solar energy
Battery.
Further, the step S2 specifically includes the following steps:
S201, perovskite presoma is dissolved in DMSO and/or DMF solution, forms the perovskite presoma of 1-1.4M
Solution；
S203, the perovskite precursor solution is spun to table of the electron transfer layer far from the conductive substrates
On face, in spin coating process, the chlorobenzene for the fullerene methylene derivatives I that concentration is 0.05-2mg/mL or chloroformic solution are dripped
It is coated on the perovskite precursor solution；
S204, under conditions of 100-160 DEG C, annealing 30-60min obtain doped with fullerene methylene derivatives I
The calcium titanium ore bed.
Further, the step S2 specifically includes the following steps:
S201, perovskite presoma is dissolved in DMSO and/or DMF solution, it is molten forms 1-1.4M perovskite presoma
Liquid；
S202, the perovskite precursor solution is spun to one of the electron transfer layer far from the conductive substrates
Face, then by chlorobenzene or chloroform drop coating on unannealed calcium titanium ore bed surface, and under conditions of 100-160 DEG C, anneal 30-
60min obtains calcium titanium ore bed；
S203, I chlorobenzene of fullerene methylene derivatives or chloroformic solution that concentration is 0.3-3mg/mL are spun to it is described
One side of the calcium titanium ore bed far from the electron transfer layer；
S204, under conditions of 80-120 DEG C, annealing 3-15min obtain the institute doped with fullerene methylene derivatives I
State calcium titanium ore bed.
Beneficial effects of the present invention: (1) I synthetic method of fullerene methylene derivatives used in the present invention is simple, easily
In purification.
(2) fullerene methylene derivatives I are used in perovskite solar battery, increase crystallite dimension, be passivated crystal grain
Surface defect state reduces carrier mobility, can significantly improve the efficiency of battery.
(3) fullerene methylene derivatives I are used as a kind of hydrophobic material, and moisture in air can be stopped to invade perovskite
Intra-die improves the air stability of battery to reduce destruction of the moisture to battery.
Detailed description of the invention
In Fig. 1 (a) be undoped with fullerene methylene derivatives I perovskite battery J-V curve graph, figure (b)~
(e) be respectively the embodiment of the present application 1~4 J-V curve graph.
Fig. 2 is layer structure schematic diagram of the invention.
Figure label explanation: electrode 1, hole transmission layer 2, calcium titanium ore bed 3, electron transfer layer 4, conductive layer 5.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings and specific examples, so that those skilled in the art can
It to better understand the invention and can be practiced, but illustrated embodiment is not as a limitation of the invention.
It should be understood that the following title that the application occurs, is the dedicated technical term in this field, this field skill
Art personnel can be beyond all doubt the following noun of confirmation meaning:
Spiro-OMeTAD:2,2', 7,7'- tetra--(dimethoxy diphenylamines)-spiro fluorene；
DMSO: dimethyl sulfoxide；
DMF:N, dinethylformamide；
ITO: tin indium oxide (electro-conductive glass)；
FTO: the SnO of fluorine is adulterated2；
Li-TFSI: bis- (fluoroform) sulfimide lithium salts；
TBP:4- tert .-butylpyridine.
A kind of perovskite solar battery, including the conductive layer set gradually by layer structure, electron transfer layer,
Doped withCalcium titanium ore bed, hole transmission layer and the electrode of (fullerene methylene derivatives I).
Wherein, conductive layer is ITO or FTO.
Wherein, electron transfer layer SnCl2.2H20, tin oxide, vapor deposition C60、TiO2, meso-porous titanium oxide, [6.6]-phenyl-
One or more of C61- methyl butyrate.
Wherein, calcium titanium ore bed MAPbI3、FAPbI3、CsPbI3、CsPbBr3、CsPbI2Br、CsPbIBr2、 MAPbI3- xClx、CsxFA1-xPbI3、MAPbI3-x-yBrxCly、(FAPbI3)x(MAPbBr3)1-xOne or more of, wherein x=0-
3, y=0-3.
Wherein, hole transmission layer is be doped with bis- (fluoroform) sulfimide lithium salts and 4- tert .-butylpyridine 2,2',
7,7'- tetra--(dimethoxy diphenylamines)-spiro fluorenes, poly- (3- hexyl thiophene), one or more of triphen amine polymer.
Wherein, electrode is one or more of gold, silver, copper or aluminium.
On the basis of the above, for the ease of understanding the application, the application further provides a kind of prepare
The method for stating perovskite solar battery, and provide following several specific embodiments:
It prepares fullerene methylene derivatives I: taking the C of 360mg60(0.5mmol), the bromomalonic acid diethyl of 2390mg
The sarcosine (3mmol) of ester (10mmol) and 2670mg are dissolved in 200mL chlorobenzene (CB) solution, under the conditions of nitrogen protection, are used
100mL dimethyl sulfoxide (DMSO) solution is added dropwise in constant pressure funnel dropwise, after 1 hour is continuously stirred at 10 DEG C, will react
Solution is put into the separatory funnel equipped with 600ml deionized water and is extracted, this process carries out twice that (lower layer's mulberry liquid is
Reaction product), remove DMSO；Lower layer's mulberry reaction product chlorobenzene solution, which is transferred in eggplant type bottle, is spin-dried for chlorobenzene with revolving instrument
Reaction product is obtained, reaction product silica gel post separation first uses carbon disulfide (CS2) go out C60, again with toluene (TL) will production
Object washes out, and is spin-dried for revolving instrument, is dried in vacuo products therefrom.
Then, configuration concentration is the chlorobenzene or chloroformic solution of the fullerene methylene derivatives I of 0.05mg/mL-3mg/mL
It is spare, specifically, the fullerene methylene derivatives I of 0.05-30mg are dissolved in the chlorobenzene or chloroform of 1-10ml, obtain
The chlorobenzene or chloroformic solution solution of fullerene methylene derivatives I.
Embodiment 1:
S1, the SnCl for being 0.1mg/mL by concentration2.2H20 ethanol solution is spin-coated to the surface ITO, spincoating conditions 2000r,
Spin-coating time 30s, first 150 DEG C of annealing 30min, then 180 DEG C of annealing 60min.
S2, use the type of perovskite active layer for (FAPbI3)x(MAPbBr3)1-x, perovskite presoma is dissolved in
In the mixed solution of DMF:DMSO=4:1, it is configured to the perovskite precursor solution of 1.35M, with spin coating revolving speed 6000r, spin coating
Perovskite presoma is spun to electron-transport layer surface by the spincoating conditions of time 40s, and in 20s, 0.05mg/mL is added dropwise
Fullerene methylene derivatives I chlorobenzene (CB) solution 100uL.After spin coating, 100 DEG C of annealing 60min obtain surface
Doped with the calcium titanium ore bed of fullerene methylene derivatives I.
The spiro-OMeTAD solution doped with Li-TFSI and tBP that concentration is 80mg/mL is spun to calcium titanium by S3,
Ore bed surface, air oxidation for 24 hours, obtain hole transmission layer.
S4, electrode evaporation silver 8nm, obtain perovskite solar battery.
J-V test is carried out to the device prepared, J-V curve is shown in Fig. 1 (b), it is found that compared with Fig. 1 (a), device
Voltage (V), electric current (J), fill factor (FF), photoelectric conversion efficiency (PCE) all significantly improves.Further relate to the material energy
It is enough passivated crystal boundary, so that device surface defect state is reduced, Carrier recombination is reduced, and charge-extraction efficiency improves.
Embodiment 2:
S1, the surface ITO spin coating concentration be 0.1mg/mL SnCl2.2H20 ethanol solution, spincoating conditions 2000r,
30s.In 150 DEG C of annealing 30min, 180 DEG C of annealing 60min after the completion of spin coating.
S2, use the type of perovskite active layer for (FAPbI3)x(MAPbBr3)1-x, perovskite presoma is dissolved in
In the mixed solution of DMF:DMSO=4:1, it is configured to the perovskite precursor solution of 1.35M, with revolving speed 6000r, spin-coating time
Perovskite presoma is spun to electron-transport layer surface by the condition of 40s, and in 20s, the fullerene methylene of 2mg/mL is added dropwise
Chlorobenzene (CB) the solution 100uL of radical derivative I.After spin coating, 100 DEG C of annealing 60min.
S3, the spiro-OMeTAD solution (doping Li-TFSI and tBP) that concentration is 80mg/mL is spun to perovskite table
Face, air oxidation is for 24 hours.
S4, electrode evaporation silver 8nm, obtain perovskite solar battery.
J-V test is carried out to the device prepared, J-V curve is shown in Fig. 1 (c), it is found that compared with Fig. 1 (a), device
Voltage (V), electric current (J), fill factor (FF), photoelectric conversion efficiency (PCE) all significantly improves.Further relate to the material energy
It is enough passivated crystal boundary, so that device surface defect state is reduced, Carrier recombination is reduced, and charge-extraction efficiency improves.
Embodiment 3:
S1, the surface ITO spin coating concentration be 0.1mg/mL SnCl2.2H20 ethanol solution, spincoating conditions 2000r,
30s, and 150 DEG C of annealing 30min, 180 DEG C of annealing 60min.
S2, use the type of perovskite active layer for (FAPbI3)x(MAPbBr3)1-x, perovskite presoma is dissolved in
In the mixed solution of DMF:DMSO=4:1, it is configured to the perovskite precursor solution of 1.35M, and with revolving speed 6000r, when spin coating
Between the spincoating conditions of 40s perovskite presoma is spun to electron-transport layer surface, in 20s, it is anti-that 100uL chlorobenzene is added dropwise
Solvent solution.After spin coating, 100 DEG C of annealing 60min.
By chlorobenzene (CB) solution for the fullerene methylene derivatives I that 30uL concentration is 0.3mg/mL with 2000r, 30s's
Spincoating conditions are spun to perovskite activity layer surface, 100 DEG C of annealing 10min.
S3, the spiro-OMeTAD solution (doping Li-TFSI and tBP) that concentration is 80mg/mL is spun to perovskite table
Face, air oxidation is for 24 hours.
S4, electrode evaporation silver 8nm, obtain perovskite solar battery.
J-V test is carried out to the device prepared, J-V curve is shown in Fig. 1 (d), it is found that compared with Fig. 1 (a), device
Voltage (V), electric current (J), fill factor (FF), photoelectric conversion efficiency (PCE) all significantly improves.Further relate to the material energy
It is enough passivated crystal boundary, so that device surface defect state is reduced, Carrier recombination is reduced, and charge-extraction efficiency improves.
Embodiment 4.
S1, the surface ITO spin coating concentration be 0.1mg/mL SnCl2.2H20 ethanol solution, spincoating conditions 2000r,
30s, and 150 DEG C of annealing 30min, 180 DEG C of annealing 60min form electron transfer layer.
S2, use the type of perovskite active layer for (FAPbI3)x(MAPbBr3)1-x, perovskite presoma is dissolved in
In the mixed solution of DMF:DMSO=4:1, it is configured to the perovskite precursor solution of 1.35M, with revolving speed 6000r, spin-coating time
The spincoating conditions of 40s are spun to electron-transport layer surface, and in 20s, 100uL chlorobenzene anti-solvent solution is added dropwise.Spin coating terminates
Afterwards, 100 DEG C of annealing 60min.
By chlorobenzene (CB) solution for the fullerene methylene derivatives I that 30uL concentration is 3mg/mL with 2000r, the rotation of 30s
Painting condition is spun to perovskite activity layer surface, 100 DEG C of annealing 10min.
S3, the spiro-OMeTAD solution (doping Li-TFSI and tBP) that concentration is 80mg/mL is spun to perovskite table
Face, air oxidation is for 24 hours.
S4, electrode evaporation silver 8nm, obtain perovskite solar battery.
J-V test is carried out to the device prepared, J-V curve is shown in Fig. 1 (e), it is found that compared with Fig. 1 (a), device
Voltage (V), electric current (J), fill factor (FF), photoelectric conversion efficiency (PCE) all significantly improves.Further relate to the material energy
It is enough passivated crystal boundary, so that device surface defect state is reduced, Carrier recombination is reduced, and charge-extraction efficiency improves.
It can be seen that by above-mentioned each embodiment and mix the fullerene methylene derivatives I by described two modes
It is miscellaneous in perovskite solar battery, device photovoltaic performance can be significantly improved.
The application creativeness applies fullerene methylene derivatives I in perovskite solar battery, can significantly
Improve perovskite.
The application will with the mode for being directly spun to perovskite activity layer surface by the way of a step spin-coating method anti-solvent
This is material doped to perovskite activity layer surface, improves the crystallinity of perovskite solar battery, passivation crystal boundary, reduction defect
State reduces Carrier recombination, charge-extraction efficiency is improved, and moisture in air is inhibited to invade, to improve efficiency steady with air
It is qualitative.
Fullerene methylene derivatives I applied by the application, the material synthesis method is simple, is easy to purify.
Fullerene methylene derivatives I are used in perovskite solar battery, crystallite dimension is capable of increasing, passivation is brilliant
Grain surface defect state, reduces carrier mobility, significantly improves the efficiency of battery.
The fullerene methylene derivatives I are used as a kind of hydrophobic material, and moisture in air invasion perovskite can be stopped brilliant
The air stability of battery is improved to reduce destruction of the moisture to battery in intragranular portion.
Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, of the invention
Within protection scope.Protection scope of the present invention is subject to claims.
Claims (10)
1. application of the fullerene methylene derivatives I in perovskite solar battery, the fullerene methylene derivatives I
Structural formula is
2. a kind of perovskite solar battery, which is characterized in that including set gradually by layer structure conductive layer, electron-transport
Layer, doped with the calcium titanium ore bed, hole transmission layer and electrode of fullerene methylene derivatives I, the fullerene methylene is derivative
The structural formula of object I is
3. perovskite solar battery as described in claim 1, which is characterized in that the conductive layer is ITO or FTO.
4. perovskite solar battery as described in claim 1, which is characterized in that the electron transfer layer is SnCl2.2H20、
Tin oxide, vapor deposition C60、TiO2, meso-porous titanium oxide, one or more of [6.6]-phenyl-C61- methyl butyrate.
5. perovskite solar battery as described in claim 1, which is characterized in that the calcium titanium ore bed is MAPbI3、
FAPbI3、CsPbI3、CsPbBr3、CsPbI2Br、CsPbIBr2、MAPbI3-xClx、CsxFA1-xPbI3、MAPbI3-x-yBrxCly、
(FAPbI3)x(MAPbBr3)1-xOne or more of, wherein x=0-3, y=0-3；The calcium titanium ore bed with a thickness of
200-700nm。
6. perovskite solar battery as described in claim 1, which is characterized in that the hole transmission layer is double to be doped with
The 2,2' of (fluoroform) sulfimide lithium salts and 4- tert .-butylpyridine, 7,7'- tetra--(dimethoxy diphenylamines)-spiro fluorene is gathered
One or more of (3- hexyl thiophene), triphen amine polymer.
7. perovskite solar battery as described in claim 1, which is characterized in that the electrode is in gold, silver, copper or aluminium
It is one or more of.
8. a kind of method for preparing any perovskite solar battery in claim 1~6, which is characterized in that including following step
Suddenly,
S1, electron transfer layer is formed in the conductive substrates；
S2, formation surface doping has fullerene methylene to spread out on the surface far from the conductive substrates of the electron transfer layer
The calcium titanium ore bed of biology I；
S3, on the calcium titanium ore bed doped with fullerene methylene derivatives I far from the electron transfer layer one side shape
At hole transmission layer；
S4, electrode is formed on surface of the hole transmission layer far from the calcium titanium ore bed, obtains perovskite solar battery.
9. preparation method as claimed in claim 8, which is characterized in that the step S2 specifically includes the following steps:
S201, perovskite presoma is dissolved in DMSO and/or DMF solution, forms the perovskite precursor solution of 1-1.4M；
S202, the perovskite precursor solution is spun on surface of the electron transfer layer far from the conductive substrates,
In spin coating process, by concentration for the fullerene methylene derivatives I of 0.05-2mg/mL chlorobenzene or chloroformic solution drop coating to institute
It states on perovskite precursor solution；
S203, under conditions of 100-160 DEG C, annealing 30-60min obtain doped with described in fullerene methylene derivatives I
Calcium titanium ore bed.
10. preparation method as claimed in claim 8, which is characterized in that the step S2 specifically includes the following steps:
S201, perovskite presoma is dissolved in DMSO and/or DMF solution, forms 1-1.4M perovskite precursor solution；
S202, the perovskite precursor solution is spun to one side of the electron transfer layer far from the conductive substrates, and
Afterwards by chlorobenzene or chloroform drop coating on unannealed calcium titanium ore bed surface, and under conditions of 100-160 DEG C, anneal 30-60min,
Obtain calcium titanium ore bed；
S203, I chlorobenzene of fullerene methylene derivatives or chloroformic solution that concentration is 0.3-3mg/mL are spun to the calcium titanium
One side of the ore bed far from the electron transfer layer；
S204, under conditions of 80-120 DEG C, annealing 3-15min obtain the calcium doped with fullerene methylene derivatives I
Titanium ore layer.
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| CN110635052A (en) * | 2019-09-27 | 2019-12-31 | 西南大学 | With a PC61Preparation method of positive perovskite battery with BM as electron transport layer |
| CN113651825A (en) * | 2021-08-17 | 2021-11-16 | 华侨大学 | Fullerene derivative, preparation method thereof and perovskite solar cell |
| CN113651825B (en) * | 2021-08-17 | 2022-07-26 | 华侨大学 | Fullerene derivative, preparation method thereof and perovskite solar cell |
| CN114899322A (en) * | 2022-04-25 | 2022-08-12 | 华侨大学 | Fullerene di (ethoxycarbonyl) methylene derivative electron transport material, application, solar cell and preparation method thereof |
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