CN106025075B - The method of high efficiency perovskite solar battery is prepared in a kind of humid air - Google Patents
The method of high efficiency perovskite solar battery is prepared in a kind of humid air Download PDFInfo
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Abstract
The invention discloses one kind to prepare high efficiency planar structure CH in humid air3NH3PbI3‑x(SCN)xThe method of based perovskite solar battery.Method includes the following steps: hydrolysis titanium tetrachloride solution first obtains TiO2Colloid, the colloid that titanium tetrachloride hydrolysis is deposited on FTO electro-conductive glass prepare TiO2Fine and close tunic, secondly using two step solwution methods in TiO2Compacted zone prepares CH3NH3PbI3‑x(SCN)xCalcium titanium ore bed, then on calcium titanium ore bed after spin coating hole-conductive layer, reheating vapor deposition prepares Ag electrode to get perovskite battery is arrived.Compared with the prior art, method of the present invention can prepare high efficiency perovskite battery in wet air, and simple production process, low in cost.
Description
Technical field
The invention belongs to area of solar cell, in particular to one kind is high using low temperature solution polycondensation preparation in humid air
The method of the perovskite solar battery (abbreviation perovskite battery) of efficiency.
Background technique
In recent years, perovskite solar battery is received much attention due to photoelectric conversion efficiency with higher.Currently, it reports
Perovskite Cell Experimentation An highest transfer efficiency alreadys exceed 20% (Yang W S, Noh J H, Jeon N J, et al.High-
performance photovoltaic perovskite layers fabricated through intramolecular
exchange.Science,2015:aaa9272).But CH3NH3PbX3Stabilization of (halogen) calcium titanium ore bed in humid air
Property it is poor, need the inert gas environment preparation low in humidity, and inert atmosphere glove box group is expensive.And if can directly exist
Perovskite solar battery is prepared in wet air, can not only reduce the cost of battery, but also operation side in preparation process
Just.
Thiocyanate (SCN) is a kind of class halide ion that performance is stable, ionic radius and I-It is close, chemical characteristic and halogen
Ion is similar, and SCN-Pb effect is more stronger than I-Pb effect, therefore CH3NH3PbI3-x(SCN)xStructure it is more stable (Q.Jiang,
D.Rebollar,J.Gong,E.L.Piacentino,C.Zheng,T.Xu,Angew.Chem.Int.Ed.,2015,54,
7617).Studies have found that introducing the group containing SCN in dye molecule can be improved its light absorption, promotes carrier conduction
(X.S.Liu,Z.C.Cao,H.L.Huang,X.X.Liu,Y.Z.Tan,H.J.Chen,Y.Pei and S.T.Tan,J.Power
Sources,2014,248,400).Ye You seminar once attempts to replace CH using the part SCN3NH3PbI3I in molecule, discovery
Can increase substantially device preparation repeatability and battery in humid air stability (Y.Chen, B.Li, W.Huang,
D.Gao,Z.Liang,Chem.Commun.,2015,51,11997)。
Currently, the TiO of low temperature solution polycondensation preparation2Planar structure CH3NH3PbI3-x(SCN)xBased perovskite solar battery is also
It has not been reported.
Summary of the invention
The present invention is to solve the deficiencies in the prior art, provides one kind by low temperature solution polycondensation and prepares TiO2It is fine and close
Layer, and CH is prepared in air3NH3PbI3-x(SCN)xCalcium titanium ore bed, to prepare the side of high efficiency perovskite solar battery
Method.
The purpose of the invention is achieved by the following technical solution:
The method of high efficiency perovskite solar battery is prepared in a kind of humid air, comprising the following steps:
(1) titanium tetrachloride solution is hydrolyzed, TiO is obtained2Colloid；
(2) the depositing Ti O on clean FTO (tin oxide of doping F) electro-conductive glass2Colloid prepares TiO2Compacted zone；
(3) 0.3~0.6g/ml of spin coating Pb (SCN) on the sample obtained by step (2)2Methyl sulfoxide solution,
Pb (SCN) is obtained after being heat-treated at 85-95 DEG C2Film；
(4) at Pb (SCN)2On film, with the aqueous isopropanol of 3000~5000r/min spin coating 10mg/ml iodine methylamine；
(5) after repeating step (4) 6~10 times, it is heat-treated obtained film at 75-85 DEG C, obtains
CH3NH3PbI3-x(SCN)xCalcium titanium ore bed；
(6) CH made from step (5)3NH3PbI3-x(SCN)xHole-conductive layer is prepared on calcium titanium ore bed；
(7) one layer of silver electrode is deposited using thermal evaporation on the sample obtained by step (6) to get the perovskite sun is arrived
It can battery.
Further, TiO described in step (1)2Colloid is that addition volume ratio is the four of 1.5-4% in mixture of ice and water
Titanium chloride solution configures.
Further, TiO described in step (2)2Compacted zone is made by following steps: by clean FTO electro-conductive glass
After shining 10~30min with ultraviolet lamp, it is put into the TiO that temperature is 65~75 DEG C240~70min, Zhi Houqu are impregnated in colloidal solution
It is heat-treated 30~60min at 180~200 DEG C out and after rinsing, obtains TiO2Compacted zone.
Preferably, the heat treatment time in step (3) is 30~60min.
Preferably, the heat treatment time in step (5) is 10~30min.
Further, hole-conductive layer described in step (6) is made: made from step (5) as following steps
CH3NH3PbI3-x(SCN)xThe 2,2' of spin coating 0.08M on calcium titanium ore bed, 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) amino]-
9,9'- spiral shell, two fluorenes (spiro-OMeTAD), double trifluoromethanesulfonimide lithium salts (LiTFSI) of 0.064M and tetra- fourth of 0.064M
Chlorobenzene (TBP) mixed solution of yl pyridines, obtained sample place 8~12h in being protected from light dry air.
Preferably, silver electrode described in step (7) is with a thickness of 80~150nm.
Preferably, thermal evaporation described in step (7) carries out in thermal evaporation instrument, and in 6 × 10-6~1 × 10-8 millitorr
Air pressure under, be deposited with the speed of 1~10nm/min.
Compared with the prior art, the side of high efficiency perovskite solar battery is prepared in humid air provided by the invention
Method has the following advantages and beneficial effects:
(1) this method belongs to solwution method, easy to operate, is easy to control；And the perovskite battery of entire planar structure is all
It prepares at low temperature, maximum heat treatment temperature is no more than 200 DEG C.
(2)CH3NH3PbI3-x(SCN)xCalcium titanium ore bed is (70% or more the humidity) prepared in the air of high humility, nothing
The inert gas environment of low humidity is needed, it is simple, convenient, do not depend on expensive glove box group.
The present invention also provides a kind of high efficiency perovskite solar battery according to made from above-mentioned preparation method.
Compared with the prior art, high efficiency perovskite solar battery of the present invention passes through cryogenic fluid legal system
It is standby, it is easy to operate, it is easy to control, cost is relatively low, and the photoelectric conversion efficiency of battery is high.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but the embodiment invented is without being limited thereto.
Embodiment 1
In the present embodiment, a kind of method that high efficiency perovskite solar battery is prepared in humid air, including following step
It is rapid:
(1) titanium tetrachloride solution of 5ml is added in the mixture of ice and water of 200ml, is configured to TiO2Colloid；
(2) after clean FTO electro-conductive glass being shone 15min with ultraviolet lamp, it is put into the TiO that temperature is 70 DEG C2Colloidal solution
Middle immersion 60min, is heat-treated 30min at 200 DEG C after taking out and rinse later, obtains TiO2Compacted zone；
(3) by Pb (SCN)2It is dissolved in methyl sulfoxide, is configured to the solution that concentration is 0.5g/ml, be made in step (2)
TiO2Spin coating Pb (SCN) on compacted zone2Then solution is heat-treated 30min at 90 DEG C and obtains Pb (SCN)2Film；
(4) at Pb (SCN)2On film, with the aqueous isopropanol of the revolving speed spin coating 10mg/ml iodine methylamine of 3000r/min.
(5) after being repeated 6 times step (4), it is heat-treated obtained film 20min at 80 DEG C, obtains CH3NH3PbI3-x
(SCN)xCalcium titanium ore bed；
(6) CH prepared by step (5)3NH3PbI3-x(SCN)xThe 2,2' of spin coating 0.08M on calcium titanium ore bed, 7,7'- tetra-
[N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell, two fluorenes, the double trifluoromethanesulfonimide lithium salts and 0.064M of 0.064M
The chlorobenzene mixed solution of tetrabutyl pyridine, obtained sample place an evening in being protected from light dry air；
(7) silver (Ag) electrode of a 80~150nm of thickness is deposited on the sample obtained by step (6) using thermal evaporation, takes
Out the battery of steamed electrode to get arrive perovskite solar battery.
It is 100mW/cm in light intensity using 91159 solar simulators of Newport company under room temperature environment2Condition
Under, the obtained battery of analysis test, the effective area of battery is 0.06cm2.Test result is shown using described in the present embodiment
Cell photoelectric transfer efficiency made from method is 10.12%.
Embodiment 2
In the present embodiment, a kind of method that high efficiency perovskite solar battery is prepared in humid air, including following step
It is rapid:
(1) titanium tetrachloride solution of 5ml is added in the mixture of ice and water of 200ml, is configured to TiO2Colloid；
(2) after clean FTO electro-conductive glass being shone 30min with ultraviolet lamp, it is put into the TiO that temperature is 70 DEG C2Colloidal solution
Middle immersion 40min, is heat-treated 40min at 190 DEG C after taking out and rinse later, obtains TiO2Compacted zone；
(3) by Pb (SCN)2It is dissolved in methyl sulfoxide, is configured to the solution that concentration is 0.6g/ml, be made in step (2)
TiO2Spin coating Pb (SCN) on compacted zone2Then solution is heat-treated 60min at 90 DEG C and obtains Pb (SCN)2Film；
(4) at Pb (SCN)2On film, with the aqueous isopropanol of the revolving speed spin coating 10mg/ml iodine methylamine of 4000r/min.
(5) after being repeated 8 times step (4), it is heat-treated obtained film 30min at 85 DEG C, obtains CH3NH3PbI3-x
(SCN)xCalcium titanium ore bed；
(6) CH prepared by step (5)3NH3PbI3-x(SCN)xThe 2,2' of spin coating 0.08M on calcium titanium ore bed, 7,7'- tetra-
[N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell, two fluorenes, the double trifluoromethanesulfonimide lithium salts and 0.064M of 0.064M
The chlorobenzene mixed solution of tetrabutyl pyridine, obtained sample place an evening in being protected from light dry air；
(7) silver (Ag) electrode of a 80~150nm of thickness is deposited on the sample obtained by step (6) using thermal evaporation, takes
Out the battery of steamed electrode to get arrive perovskite solar battery.
It is 100mW/cm in light intensity using 91159 solar simulators of Newport company under room temperature environment2Condition
Under, the obtained battery of analysis test, the effective area of battery is 0.06cm2.Test result is shown using described in the present embodiment
Cell photoelectric transfer efficiency made from method is 9.02%.
Embodiment 3
In the present embodiment, a kind of method that high efficiency perovskite solar battery is prepared in humid air, including following step
It is rapid:
(1) titanium tetrachloride solution of 3ml is added in the mixture of ice and water of 200ml, is configured to TiO2Colloid；
(2) after clean FTO electro-conductive glass being shone 10min with ultraviolet lamp, it is put into the TiO that temperature is 70 DEG C2Colloidal solution
Middle immersion 70min, is heat-treated 60min at 180 DEG C after taking out and rinse later, obtains TiO2Compacted zone；
(3) by Pb (SCN)2It is dissolved in methyl sulfoxide, is configured to the solution that concentration is 0.3g/ml, be made in step (2)
TiO2Spin coating Pb (SCN) on compacted zone2Then solution is heat-treated 60min at 90 DEG C and obtains Pb (SCN)2Film；
(4) at Pb (SCN)2On film, with the aqueous isopropanol of the revolving speed spin coating 10mg/ml iodine methylamine of 5000r/min.
(5) after being repeated 10 times step (4), it is heat-treated obtained film 10min at 75 DEG C, obtains CH3NH3PbI3-x
(SCN)xCalcium titanium ore bed；
(6) CH prepared by step (5)3NH3PbI3-x(SCN)xThe 2,2' of spin coating 0.08M on calcium titanium ore bed, 7,7'- tetra-
[N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell, two fluorenes, the double trifluoromethanesulfonimide lithium salts and 0.064M of 0.064M
The chlorobenzene mixed solution of tetrabutyl pyridine, obtained sample place an evening in being protected from light dry air；
(7) silver (Ag) electrode of a 80~150nm of thickness is deposited on the sample obtained by step (6) using thermal evaporation, takes
Out the battery of steamed electrode to get arrive perovskite solar battery.
It is 100mW/cm in light intensity using 91159 solar simulators of Newport company under room temperature environment2Condition
Under, the obtained battery of analysis test, the effective area of battery is 0.06cm2.Test result is shown using described in the present embodiment
Cell photoelectric transfer efficiency made from method is 6.74%.
In above-mentioned 3 embodiments, embodiment 1 is most preferred embodiment.
It should be noted that preparing the side of high efficiency perovskite solar battery in a kind of humid air of the present invention
In method, the temperature of heat treatment influences battery performance parameter obtained smaller, wherein in step (3) heat treatment temperature 75~
Effect is preferable within the scope of 95 DEG C；Heat treatment temperature in step (5) effect within the scope of 75~85 DEG C is preferable.In addition, step (2)
In TiO2The temperature of colloidal solution controls within the scope of 65~75 DEG C.Thermal evaporation described in step (7) is in thermal evaporation
It carries out in instrument, and under the air pressure of 6 × 10-6~1 × 10-8 millitorr, is deposited with the speed of 1~10nm/min.
The heat treatment temperature of above-mentioned 3 embodiments selects optimal parameter, is only presently preferred embodiments of the present invention,
Limitation in any form not is done to the present invention, content selects preferable other parameters to those skilled in the art according to the present invention
Also it can reach the purpose of the present invention.
The above described is only a preferred embodiment of the present invention, limitation in any form not is done to the present invention, therefore
All contents without departing from technical solution of the present invention, it is made to the above embodiment according to the technical essence of the invention any simply to repair
Change, equivalent variations and modification, all of which are still within the scope of the technical scheme of the invention.
Claims (8)
1. preparing the method for high efficiency perovskite solar battery in a kind of humid air, which comprises the following steps:
(1) titanium tetrachloride solution is hydrolyzed, TiO is obtained2Colloid；
(2) the depositing Ti O on clean FTO electro-conductive glass2Colloid prepares TiO2Compacted zone, the TiO2Compacted zone by with
Lower step is made: after clean FTO electro-conductive glass is shone 10~30min with ultraviolet lamp, being put into the TiO that temperature is 65~75 DEG C2
40~70min is impregnated in colloidal solution, is heat-treated 30~60min after taking out and rinse later at 180~200 DEG C, is obtained
TiO2Compacted zone；
(3) 0.3~0.6g/ml of spin coating Pb (SCN) on the sample obtained by step (2)2Methyl sulfoxide solution, in 85-95
Pb (SCN) is obtained after being heat-treated at DEG C2Film；
(4) at Pb (SCN)2On film, with the aqueous isopropanol of 3000~5000r/min spin coating 10mg/ml iodine methylamine；
(5) after repeating step (4) 6~10 times, it is heat-treated obtained film at 75-85 DEG C, obtains CH3NH3PbI3-x
(SCN)xCalcium titanium ore bed；
(6) CH made from step (5)3NH3PbI3-x(SCN)xHole-conductive layer is prepared on calcium titanium ore bed；
(7) one layer of silver electrode is deposited using thermal evaporation on the sample obtained by step (6) to get perovskite solar-electricity is arrived
Pond.
2. the method for preparing high efficiency perovskite solar battery in humid air according to claim 1, feature exist
In: TiO described in step (1)2Colloid is that the titanium tetrachloride solution configuration that volume ratio is 1.5-4% is added in mixture of ice and water
It forms.
3. the method for preparing high efficiency perovskite solar battery in humid air according to claim 1, feature exist
In: the heat treatment time in step (3) is 30~60min.
4. the method for preparing high efficiency perovskite solar battery in humid air according to claim 1, feature exist
In: the heat treatment time in step (5) is 10~30min.
5. the method for preparing high efficiency perovskite solar battery in humid air according to claim 1, feature exist
In: hole-conductive layer described in step (6) is made: the CH made from step (5) as following steps3NH3PbI3-x(SCN)xCalcium
The 2,2' of spin coating 0.08M on titanium ore layer, 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell, two fluorenes, 0.064M
Double trifluoromethanesulfonimide lithium salts and 0.064M tetrabutyl pyridine chlorobenzene mixed solution, obtained sample is being protected from light drying
Air in place 8~12h.
6. the method for preparing high efficiency perovskite solar battery in humid air according to claim 1, feature exist
In: silver electrode described in step (7) is with a thickness of 80~150nm.
7. the method for preparing high efficiency perovskite solar battery in humid air according to claim 1, feature exist
In: thermal evaporation described in step (7) carries out in thermal evaporation instrument, and 6 × 10-6~1 × 10-8Under the air pressure of millitorr, with 1
The speed of~10nm/min is deposited.
8. a kind of high efficiency perovskite solar battery, it is characterised in that: pass through the described in any item methods of claim 1~7
It is prepared.
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| CN106784317B (en) * | 2016-11-29 | 2019-08-09 | 宁波大学 | The manufacturing method of the perovskite solar battery of super-thin electronic transport layer structure |
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| CN107146852B (en) * | 2017-04-06 | 2020-02-28 | 华南师范大学 | Method for preparing high-efficiency perovskite solar cell in humid air by introducing ammonium salt |
| CN107170889A (en) * | 2017-05-04 | 2017-09-15 | 华南师范大学 | It is a kind of by being introduced into the method that alkali metal ion prepares high efficiency perovskite solar cell in humid air |
| CN107706309B (en) * | 2017-09-15 | 2020-05-26 | 华南师范大学 | Preparation method of planar perovskite solar cell |
| CN107799654B (en) * | 2017-09-15 | 2020-10-09 | 华南师范大学 | High-efficiency planar perovskite solar cell and preparation method thereof |
| CN108054284A (en) * | 2017-12-19 | 2018-05-18 | 天津大学 | A kind of preparation method of big crystal grain perovskite thin film |
| CN109638161B (en) * | 2018-12-04 | 2022-11-29 | 储天新能源科技（长春）有限公司 | Preparation method of efficient perovskite solar cell and perovskite solar cell |
| CN111129314B (en) * | 2019-12-30 | 2023-01-31 | 电子科技大学 | Preparation method of perovskite electron transport layer |
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