CN107799654A - A kind of high efficiency plane perovskite solar cell and preparation method thereof - Google Patents
A kind of high efficiency plane perovskite solar cell and preparation method thereof Download PDFInfo
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- CN107799654A CN107799654A CN201710831998.3A CN201710831998A CN107799654A CN 107799654 A CN107799654 A CN 107799654A CN 201710831998 A CN201710831998 A CN 201710831998A CN 107799654 A CN107799654 A CN 107799654A
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Abstract
The present invention relates to a kind of high efficiency plane perovskite solar cell, the high efficiency plane perovskite solar cell includes transparent conductive substrate, electronic conductive layer, calcium titanium ore bed, hole-conductive layer and metal electrode；The electronic conductive layer is the titanium dioxide dense layer of gallium doping prepared by low temperature process solwution method.The invention further relates to the preparation method of above-mentioned high efficiency plane perovskite solar cell, gallium nitrate and Low Temperature Heat Treatment are added during by preparing titanium dioxide dense layer in hydrolysis titanium tetrachloride, the titanium dioxide dense layer of gallium doping is obtained, and the titanium dioxide dense layer adulterated with the gallium assembles perovskite solar cell.The titanium dioxide dense layer for the gallium doping that plane perovskite solar cell of the present invention is prepared using low temperature process solwution method is as electronic conductive layer, collection and conduction of the titanic oxide electronic conducting shell to light induced electron are promoted by gallium doping, it has the advantages of photoelectric transformation efficiency is high, battery efficiency is high, easily prepares.
Description
Technical field
The invention belongs to technical field of solar batteries, more particularly to a kind of high efficiency plane perovskite solar cell and
Its preparation method.
Background technology
In recent years, perovskite solar cell with higher photoelectric transformation efficiency due to receiving much attention.Perovskite is too
The photoelectric characteristic of electronic conductive layer decides the light absorbs of battery and the conduction of photo-generated carrier and collection, and its in positive energy battery
Micro-structural affects the micro-structural and photoelectric characteristic of calcium titanium ore bed, decides the photoelectric transformation efficiency of battery to a certain extent,
It is therefore particularly important.
Although the perovskite battery highest conversion efficiency by U.S.'s NREL certifications alreadys exceed 22%, current report
Low temperature CH3NH3PbI3-xClxThe photoelectric transformation efficiency of base plane perovskite solar cell typically only 13% or so, can be carried
The space risen is also very big.Promote the conduction of light induced electron and collection from the angle of the photoelectric characteristic of regulation and control electronic conductive layer, with
The photoelectricity transfer efficient for improving battery is one of more feasible thinking.Currently, do not occur the titanium dioxide dense adulterated with gallium also
Plane CH of the layer as electronic conductive layer3NH3PbI3-xClxBased perovskite solar cell, also have no and mixed using low temperature preparation gallium
Miscellaneous titanium dioxide dense layer assembles efficient plane CH3NH3PbI3-xClxThe related report of based perovskite solar cell
Road.
The content of the invention
Based on this, it is an object of the present invention to provide a kind of high efficiency plane perovskite solar cell, it is adulterated with gallium
Titanium dioxide dense layer as electronic conductive layer, the titanium dioxide dense layer of gallium doping has to be prepared by low temperature process, group
The advantages of cell photoelectric high conversion efficiency of dress.
The technical solution adopted by the present invention is as follows：
A kind of high efficiency plane perovskite solar cell, including transparent conductive substrate, electronic conductive layer, calcium titanium ore bed,
Hole-conductive layer and metal electrode；The electronic conductive layer is the titanium dioxide dense layer of gallium doping, the titanium dioxide that the gallium adulterates
Titanium compacted zone is prepared by adding gallium nitrate during lower temperature hydrolytic precipitation method deposition of titanium oxide compacted zone.
Relative to prior art, plane perovskite solar cell of the present invention is caused using the titanium dioxide of gallium doping
Close layer is (referred to as：(Ga)TiO2Compacted zone) electronic conductive layer is used as, the mobility of electronic shell is improved by gallium doping, to promote
The conduction and collection of light induced electron, so as to improve the photoelectric transformation efficiency of battery.Plane perovskite solar energy of the present invention
The battery efficiency of battery apparently higher than by the use of undoped with titanium dioxide dense layer as electronic conductive layer the plane perovskite sun
Can battery.
Further, the mol ratio 3-9 of gallium atom and titanium atom in the titanium dioxide dense layer of the gallium doping:100.It is logical
The doping of adjustment gallium is crossed in optimum range, it is ensured that the plane perovskite solar cell possesses high battery efficiency.
Further, the transparent conductive substrate is described to adulterate the tin dioxide conductive glass (FTO electro-conductive glass) of fluorine
Calcium titanium ore bed is CH3NH3PbI3-xClxBased perovskite layer, the hole-conductive layer are Spiro-OMeTAD layers, the metal electrode
For silver electrode.
The present invention also provides the preparation method of any of the above-described high efficiency plane perovskite solar cell, the preparation method
Comprise the following steps：
(1) preparation of electronic conductive layer：Gallium nitrate is first added in mixture of ice and water, adds titanium tetrachloride aqueous solution,
Configure the titania-doped colloidal solution of gallium, then take cleaning transparent conductive substrate be put into 60~80 DEG C gallium doping titanium dioxide
Soaked 40~60 minutes in titanium colloidal solution, use deionized water and alcohol flushing after taking-up successively, then entered with 180~220 DEG C
Row heat treatment 30~60 minutes, obtain preparing the titanium dioxide that the gallium as electronic conductive layer in transparent conductive substrate adulterates
Compacted zone；
(2) preparation of calcium titanium ore bed：It is 3 by mol ratio:1 CH3NH3I and PbCl2It is dissolved in dimethylformamide, obtains
To perovskite precursor liquid, treatment with ultraviolet light is carried out 8~15 minutes to the titanium dioxide dense layer that the gallium obtained by step (1) adulterates,
Then perovskite precursor liquid is being added dropwise thereon, is carrying out heat treatment 50~70 minutes with 80~120 DEG C after spin coating, obtain preparing in gallium
The CH as calcium titanium ore bed on the titanium dioxide dense layer of doping3NH3PbI3-xClxBased perovskite layer；
(3) preparation of hole-conductive layer：In the CH obtained by step (2)3NH3PbI3-xClxSpin coating contains on based perovskite layer
The fluorenes (Spiro-OMeTAD) of 0.08M 2,2', 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9,9'- spiral shells two, 0.064M
Double trifluoromethanesulfonimide lithium salts (LiTFSI) and the chlorobenzene mixed solution of 0.064M tetrabutyls pyridine (TBP), then will
It is placed in the air of lucifuge drying 6~8 hours, obtains preparing in CH3NH3PbI3-xClxConduct on based perovskite layer is empty
The Spiro-OMeTAD layers of cave conducting shell；
(4) preparation of metal electrode：One thickness is being deposited on Spiro-OMeTAD layers obtained by step (3) using thermal evaporation
After 80~150nm metal electrode, the high efficiency plane perovskite solar cell is made.
Further, in step (1), the volume ratio of titanium tetrachloride and water is 1.5~4 in the titanium tetrachloride aqueous solution:
100, gained gallium doping titanium dioxide dense layer in the mol ratio of gallium atom and titanium atom be 3~9:100.By adjusting nitric acid
The dosage of gallium, make the doping of gallium in optimum range, it is ensured that the plane perovskite solar cell possesses high battery efficiency.
Further, in step (1), (FTO is conductive to adulterate the tin dioxide conductive glass of fluorine for the transparent conductive substrate
Glass), after the tin dioxide conductive glass of the doping fluorine first passes through treatment with ultraviolet light 10~20 minutes, place into gallium doping dioxy
Change and soaked in titanium colloidal solution.
Further, in step (1), transparent conductive substrate, which is put into 70 DEG C of the titania-doped colloidal solution of gallium, soaks
50 minutes, deionized water and alcohol flushing are used after taking-up successively, is then heat-treated with 200 DEG C.
Further, in step (2), CH in the perovskite precursor liquid3NH3I and PbCl2Gross mass percentage be
40%.
Further, in step (2), the time of the treatment with ultraviolet light is 10 minutes；The speed of the spin coating is 3000
Rev/min, the time is 30 seconds；The temperature of the heat treatment is 100 DEG C, and the time is 60 minutes；The spin coating and heat treatment exist
Carried out in glove box.
Further, in step (4), the metal electrode is silver electrode, and the thermal evaporation is carried out in thermal evaporation instrument, and
(6 × 10-6)~(1 × 10-8) millitorr air pressure under, be deposited with 1~10nm/min speed.
Preparation method of the present invention prepares TiO in hydrolysis titanium tetrachloride2Added during compacted zone appropriate
Gallium nitrate, (Ga) TiO is then obtained by Low Temperature Heat Treatment2Compacted zone, and utilize and be somebody's turn to do (Ga) TiO2Compacted zone conducts as electronics
Layer, obtained structure are：FTO/(Ga)TiO2/CH3NH3PbI3-xClx/ Spiro-OMeTAD/Ag high efficiency plane perovskite electricity
Pond.Preparation method of the present invention easily realizes that the Parameter Conditions of each step are easily controllable, and it is low to prepare cost.
The present invention is not limited solely to using FTO electro-conductive glass as transparent conductive substrate, using CH3NH3PbI3Base calcium titanium
Ore bed, as metal electrode, owns as calcium titanium ore bed, using Spiro-OMeTAD layers as hole-conductive layer, using silver electrode
The TiO of gallium doping is prepared using low temperature process of the present invention2Electronic shell, and the perovskite sun for any structure being assembled into
Energy battery belongs to protection scope of the present invention.
In order to more fully understand and implement, the invention will now be described in detail with reference to the accompanying drawings.
Brief description of the drawings
Fig. 1 is the structural representation of the high efficiency plane perovskite solar cell of the present invention.
Embodiment
As shown in figure 1, high efficiency plane perovskite solar cell provided by the invention transparent leading of including stacking gradually
Electric substrate 1, electronic conductive layer 2, calcium titanium ore bed 3, hole-conductive layer 4 and metal electrode 5.
Specifically, the transparent conductive substrate 1 is the tin dioxide conductive glass of doping fluorine.The electronic conductive layer 2 is
The titanium dioxide dense layer of gallium doping, the wherein mol ratio of gallium atom and titanium atom are 3~9:100.The calcium titanium ore bed 3 is
CH3NH3PbI3-xClxBased perovskite layer.The hole-conductive layer 4 is Spiro-OMeTAD layers.The metal electrode 5 be 80~
Silver electrode thick 150nm.
The preparation method of high efficiency plane perovskite solar cell provided by the invention comprises the following steps：
(1) preparation of electronic conductive layer：Gallium nitrate is first added in mixture of ice and water, adds titanium tetrachloride aqueous solution,
Configure the titania-doped colloidal solution of gallium.Then take cleaning transparent conductive substrate be put into 60~80 DEG C gallium doping titanium dioxide
Soaked 40~60 minutes in titanium colloidal solution, use deionized water and alcohol flushing after taking-up successively, then entered with 180~220 DEG C
Row heat treatment 30~60 minutes, obtain preparing the titanium dioxide that the gallium as electronic conductive layer in transparent conductive substrate adulterates
Compacted zone.
(2) preparation of calcium titanium ore bed：It is 3 by mol ratio:1 CH3NH3I and PbCl2It is dissolved in dimethylformamide, obtains
To perovskite precursor liquid, treatment with ultraviolet light is carried out 8~15 minutes to the titanium dioxide dense layer that the gallium obtained by step (1) adulterates,
Then perovskite precursor liquid is being added dropwise thereon, is carrying out heat treatment 50~70 minutes with 80~120 DEG C after spin coating, obtain preparing in gallium
The CH as calcium titanium ore bed on the titanium dioxide dense layer of doping3NH3PbI3-xClxBased perovskite layer.
(3) preparation of hole-conductive layer：In the CH obtained by step (2)3NH3PbI3-xClxSpin coating contains on based perovskite layer
0.08M Spiro-OMeTAD, 0.064M LiTFSI and 0.064M Spiro-OMeTAD chlorobenzene mixed solution, then will
It is placed in the air of lucifuge drying 6~8 hours, obtains preparing in CH3NH3PbI3-xClxConduct on based perovskite layer is empty
The Spiro-OMeTAD layers of cave conducting shell.
(4) preparation of metal electrode：One thickness is being deposited on Spiro-OMeTAD layers obtained by step (3) using thermal evaporation
80~150nm metal electrode, the high efficiency plane perovskite solar cell is made.
Embodiment 1
The present embodiment prepares high efficiency plane perovskite solar cell and specifically carried out according to the following steps：
(1) preparation of the titanium dioxide dense layer of gallium doping：Gallium nitrate is first added in mixture of ice and water, adds tetrachloro
The volume ratio for changing titanium and water is 1.5~4:100 titanium tetrachloride aqueous solution, configure the titania-doped colloidal solution of gallium.Then
After taking the tin dioxide conductive glass uviol lamp of the doping fluorine of cleaning to shine 10~20 minutes, 70 DEG C of gallium doping titanium dioxide is put into
Soaked 50 minutes in titanium colloidal solution, use deionized water and alcohol flushing after taking-up successively, then carry out heat treatment 30 with 200 DEG C
~60 minutes, obtain preparing the titanium dioxide dense layer of the gallium doping on the tin dioxide conductive glass of doping fluorine, the gallium is mixed
The mol ratio of gallium atom and titanium atom is 5 in miscellaneous titanium dioxide dense layer:100.
(2)CH3NH3PbI3-xClxThe preparation of based perovskite layer：It is 3 by mol ratio:1 CH3NH3I and PbCl2It is dissolved in two
In NMF, CH is obtained3NH3I and PbCl2Gross mass percentage be 40% perovskite precursor liquid.To step (1) institute
The titanium dioxide dense layer of the gallium doping obtained carries out treatment with ultraviolet light 10 minutes, and perovskite precursor liquid is then being added dropwise thereon, then
After 3000 revs/min of speed spin coating 30 seconds, heat treatment 60 minutes is carried out with 100 DEG C, obtains preparing the dioxy in gallium doping
Change the CH on titanium compacted zone3NH3PbI3-xClxBased perovskite layer.The spin coating and heat treatment are carried out in glove box.
(3) preparation of Spiro-OMeTAD layers：In the CH obtained by step (2)3NH3PbI3-xClxSpin coating on based perovskite layer
Chlorobenzene mixed solution containing 0.08M Spiro-OMeTAD, 0.064M LiTFSI and 0.064M Spiro-OMeTAD, so
6~8 hours are placed it in the air of lucifuge drying afterwards with fully oxidized, obtain preparing in CH3NH3PbI3-xClxBase calcium titanium
Spiro-OMeTAD layers on ore bed.
(4) preparation of silver electrode：In thermal evaporation instrument, (6 × 10-6)~(1 × 10-8) millitorr air pressure under with 1~
The silver electrode of a 80~150nm of thickness, Ran Houqu is being deposited in 10nm/min speed on Spiro-OMeTAD layers obtained by step (3)
Go out the battery of steamed silver electrode, that is, the high efficiency plane perovskite solar cell prepared.
Embodiment 2
The step of the present embodiment preparation high efficiency plane perovskite solar cell, is substantially the same manner as Example 1, difference
Be in：In step (1), the mol ratio of gallium atom and titanium atom is 7 in the titanium dioxide dense layer of obtained gallium doping:100.
Embodiment 3
The step of the present embodiment preparation high efficiency plane perovskite solar cell, is substantially the same manner as Example 1, difference
Be in：In step (1), the mol ratio of gallium atom and titanium atom is 9 in the titanium dioxide dense layer of obtained gallium doping:100.
Comparative example
The step of this comparative example preparation high efficiency plane perovskite solar cell, is roughly the same with embodiment 1, difference
Be in：Step (1) is the preparation process of titanium dioxide dense layer, does not add gallium nitrate in mixture of ice and water, obtained to be
Undoped with titanium dioxide dense layer.
It is 100mW/cm in light intensity using 91159 solar simulators of Newport companies under room temperature environment2Condition
It is lower that performance test is carried out to plane perovskite solar cell made from embodiment 1-3 and comparative example respectively.
Test result is：(mol ratio of gallium and titanium is 5 to the titanium dioxide dense layer adulterated with gallium of embodiment 1:100) group
The photoelectric efficiency of the plane perovskite solar cell of dress is 16.06%.The titanium dioxide dense layer adulterated with gallium of embodiment 2
(mol ratio of gallium and titanium is 7:100) photoelectric efficiency of the plane perovskite solar cell of assembling is 17.09%.Embodiment 3
With gallium adulterate titanium dioxide dense layer (mol ratio of gallium and titanium be 9:100) the plane perovskite solar cell of assembling
Photoelectric efficiency is 14.19%.The photoelectricity of the plane perovskite solar cell assembled with titanium dioxide dense layer of comparative example is imitated
Rate is 14.22%.
Above-mentioned test result shows, the plane of the invention by the use of the titanium dioxide dense layer that gallium adulterates as electronic conductive layer
The battery efficiency of perovskite solar cell apparently higher than by the use of undoped with titanium dioxide dense layer be used as the flat of electronic conductive layer
Face perovskite solar cell.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.
The perovskite solar cell that electronic shell prepared by all low temperature process using the application assembles, the category present invention
Protection domain.
Claims (10)
1. a kind of high efficiency plane perovskite solar cell, including transparent conductive substrate, electronic conductive layer, calcium titanium ore bed, sky
Cave conducting shell and metal electrode；It is characterized in that：The electronic conductive layer is the titanium dioxide dense layer of gallium doping, and the gallium adulterates
Titanium dioxide dense layer by during lower temperature hydrolytic precipitation method deposition of titanium oxide compacted zone add gallium nitrate be prepared.
2. high efficiency plane perovskite solar cell according to claim 1, it is characterised in that：The two of the gallium doping
The mol ratio 3-9 of gallium atom and titanium atom in titanium oxide compacted zone:100.
3. the high efficiency plane perovskite solar cell according to any one of claim 1 or 2, it is characterised in that：It is described
Transparent conductive substrate is the tin dioxide conductive glass of doping fluorine, and the calcium titanium ore bed is CH3NH3PbI3-xClxBased perovskite layer,
The hole-conductive layer is Spiro-OMeTAD layers, and the metal electrode is silver electrode.
4. the preparation method of the high efficiency plane perovskite solar cell described in claim any one of 1-3, it is characterised in that：
Comprise the following steps：
(1) preparation of electronic conductive layer：Gallium nitrate is first added in mixture of ice and water, adds titanium tetrachloride aqueous solution, is configured
The titania-doped colloidal solution of gallium, the transparent conductive substrate of cleaning is then taken to be put into 60~80 DEG C of the titania-doped glue of gallium
Soaked 40~60 minutes in liquid solution, use deionized water and alcohol flushing after taking-up successively, then carry out heat with 180~220 DEG C
Processing 30~60 minutes, obtain preparing the titanium dioxide dense that the gallium as electronic conductive layer in transparent conductive substrate adulterates
Layer；
(2) preparation of calcium titanium ore bed：It is 3 by mol ratio:1 CH3NH3I and PbCl2It is dissolved in dimethylformamide, obtains calcium
Titanium ore precursor liquid, treatment with ultraviolet light is carried out 8~15 minutes to the titanium dioxide dense layer that the gallium obtained by step (1) adulterates, then
Perovskite precursor liquid is being added dropwise thereon, heat treatment is carried out 50~70 minutes with 80~120 DEG C after spin coating, is obtaining preparing and is adulterated in gallium
Titanium dioxide dense layer on the CH as calcium titanium ore bed3NH3PbI3-xClxBased perovskite layer；
(3) preparation of hole-conductive layer：In the CH obtained by step (2)3NH3PbI3-xClxSpin coating contains 0.08M on based perovskite layer
Spiro-OMeTAD, 0.064M LiTFSI and 0.064M Spiro-OMeTAD chlorobenzene mixed solution, are then placed
6~8 hours in the air that lucifuge is dried, obtain preparing in CH3NH3PbI3-xClxConduct hole-conductive on based perovskite layer
The Spiro-OMeTAD layers of layer；
(4) preparation of metal electrode：Be deposited using thermal evaporation on Spiro-OMeTAD layers obtained by the step (3) thickness 80~
150nm metal electrode, the high efficiency plane perovskite solar cell is made.
5. the preparation method of high efficiency plane perovskite solar cell according to claim 4, it is characterised in that：Step
(1) in, the volume ratio of titanium tetrachloride and water is 1.5~4 in the titanium tetrachloride aqueous solution:100, the titanium dioxide of gained gallium doping
The mol ratio 3~9 of gallium atom and titanium atom in titanium compacted zone:100.
6. the preparation method of high efficiency plane perovskite solar cell according to claim 5, it is characterised in that：Step
(1) in, the transparent conductive substrate is the tin dioxide conductive glass of doping fluorine, and the tin dioxide conductive glass of the doping fluorine is first
After treatment with ultraviolet light 10~20 minutes, place into the titania-doped colloidal solution of gallium and soak.
7. the preparation method of high efficiency plane perovskite solar cell according to claim 6, it is characterised in that：Step
(1) in, transparent conductive substrate, which is put into 70 DEG C of the titania-doped colloidal solution of gallium, soaks 50 minutes, is spent successively after taking-up
Ionized water and alcohol flushing, then it is heat-treated with 200 DEG C.
8. the preparation method of high efficiency plane perovskite solar cell according to claim 4, it is characterised in that：Step
(2) in, CH in the perovskite precursor liquid3NH3I and PbCl2Gross mass percentage be 40%.
9. the preparation method of high efficiency plane perovskite solar cell according to claim 8, it is characterised in that：Step
(2) in, the time of the treatment with ultraviolet light is 10 minutes；The speed of the spin coating is 3000 revs/min, and the time is 30 seconds；Institute
The temperature for stating heat treatment is 100 DEG C, and the time is 60 minutes；The spin coating and heat treatment are carried out in glove box.
10. the preparation method of high efficiency plane perovskite solar cell according to claim 4, it is characterised in that：Step
Suddenly in (4), the metal electrode is silver electrode, and the thermal evaporation is carried out in thermal evaporation instrument, and (6 × 10-6)~(1 × 10-8) millitorr air pressure under, be deposited with 1~10nm/min speed.
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| CN110672579A (en) * | 2019-09-26 | 2020-01-10 | 南通大学 | Method for detecting surface morphology of perovskite layer of solar cell by utilizing Raman spectrum |
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