CN107591481A - The organic metal halide perovskite thin film preparation method of barium titanate doping - Google Patents
The organic metal halide perovskite thin film preparation method of barium titanate doping Download PDFInfo
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Abstract
The invention discloses a kind of organic metal halide perovskite thin film material preparation method of barium titanate doping, belong to photoelectric semiconductor material and hydridization perovskite solar cell preparation field.Barium-titanate material is added among perovskite material using the method for doping, it is set uniformly to be distributed among perovskite solution, then using the method for spin coating, spin coating contains the calcium titanium ore bed of barium titanate on mesoporous titanium dioxide film, light absorption layer material as solar cell, the method that the present invention improves perovskite ferroelectric polarity by adulterating, it is added to having ferroelectric barium-titanate material among calcium titanium ore bed, electric field polarization situation inside during improving perovskite solar cell generation photoelectric effect, improve the stability and photoelectric transformation efficiency of perovskite solar cell.
Description
Technical field
The present invention relates to the technical field of solar cell photoelectric conversion semi-conducting material research, particularly hydridization perovskite
The preparation method of solar cell, belong to photoelectric semiconductor material and hydridization perovskite solar cell preparation field, especially relate to
A kind of and organic metal halide perovskite thin film material preparation method of barium titanate doping.
Background technology
It is progressively depleted with traditional fossil energy, and getting worse ground problem of environmental pollution, efficiently, low energy
Consumption, free of contamination thin-film solar cells were paid attention to by various countries, since DSSC (DSSC in 1991S) quilt
Since Michael Gratzel are invented and efficiency breaks through 7%, DSSCSIt is higher with its low cost, relatively simple preparation technology
Photoelectric transformation efficiency and enjoy people to pay close attention to, hybrid perovskite structure is incorporated into solar cell by scientist
In, in the time of short 7 years, efficiency is improved to 22.1%；It is based particularly on CH3NH3I·PbX2(X Cl, Br or I) etc. has
The efficiency of machine/inorganic hybridization perovskite thin film solar cell climbs up and up, and turns into the focus of our times research.
Existing perovskite material typically has three kinds of crystal structures, including Emission in Cubic, Tetragonal, orthorhombic phase, current research
Generally believe due to its internal ion motion, produce ferroelectricity polarity, influence photovoltaic performance, therefore there can be iron by adding
The material of electrical property reduces or improved its iron electric polarization effect.
Barium titanate (BaTiO3, BTO) and it is a kind of typical Ferroelectrics, its curie point is 120 DEG C, and fusing point is
1625 DEG C, its crystal has good ferroelectricity, high-k and big electro-optic coefficient.Therefore, BTO films and it is nanocrystalline
There is highly important application value in the field such as microelectronics and electro-optic integrated devices.It is the tetragonal of ferroelectric phase at room temperature
It is (4mm point groups) interaction in Tetragonal BTO crystal between the 3d tracks of Ti atoms and O 2p tracks, it is brilliant to produce BTO
The ferroelectricity of body.Therefore, BTO is incorporated into organic metal halide perovskite material, turning into improves perovskite material ferroelectricity
The preferred material of polarity.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of the organic metal halide perovskite thin film of barium titanate doping, pin
To weakening ferroelectricity polarity in above-mentioned perovskite solar cell, by being mixed in calcium titanium ore bed there is ferroelectric barium titanate to receive
Rice grain, to improve the iron electric polarization in perovskite solar cell, improve the opto-electronic conversion performance of perovskite solar cell.
The design concept of the present invention is achieved in that is added to calcium titanium using the method for doping barium-titanate material first
Among pit wood material, it is set uniformly to be distributed among perovskite solution, it is then thin in mesoporous TiO 2 using the method for spin coating
Spin coating contains the calcium titanium ore bed of barium titanate on film, as the light absorption layer material of solar cell, then spin coating hole transmission layer,
Silver electrode in steaming, electrically conducting transparent substrate, semiconductor electronic transport layer, BTO perovskites light absorbing layer, hole transmission layer and silver electricity
Pole, form the perovskite solar cell of barium titanate doping.
In order to solve the above technical problems, the technical solution adopted in the present invention is to provide a kind of organic gold of barium titanate doping
Belong to the preparation method of halide perovskite thin film, step is as follows：
Take metal halide MX2、HC(NH2)2X and CH3NH3X, wherein HC (NH2)2X is abbreviated as FAX, CH3NH3X is abbreviated as
MAX, by metal halide MX2With HC (NH2)2X is added among organic solvent, under the conditions of temperature is 50~150 DEG C, stirring
0.1~24 hour, compound concentration was 0.01~5mol/l FAMX3Solution, by metal halide MX2And CH3NH3X is added to
In organic solvent, under the conditions of temperature is 50~150 DEG C, stir 0.1~24 hour, compound concentration is 0.01~5mol/l's
MAMX3Solution, FAMX3Solution and MAMX3Solution is 1 according to concentration ratio:10~10:1 ratio mixing, temperature be 50~
150 DEG C, stir 0.1~24 hour, obtain (the FAMX that concentration is 0.01~5mol/l3)x(MAMX3)(1-x)Mixed solution；Secondly,
Barium titanate BTO solution is added to (FAMX3)x(MAMX3)(1-x)Among mixed solution, stir 0.1~24 hour, it is dense that BTO is made
Spend the BTO/ (FAMX for 0.01~5mol/L3)x(MAMX3)(1-x)Mixed solution, finally, by BTO/ (FAMX3)x(MAMX3)(1-x)
Mixed solution is added dropwise on substrate film, spin-coating, and rotating speed is 500~7500r/min, 1~150 second spin-coating time,
Sample after spin-coating is heat-treated 5 minutes~60 minutes at 20~150 DEG C.
Further, the metal halide MX in methods described2, middle M can also be Sn, Ge, Cu, Cs etc. a kind of or several
Kind.
Further, the MX in methods described2、HC(NH2)2X and CH3NH3X in X can be I, Br, Cl or
One of which or several mixtures.
Further, organic solvent can be that N-N dimethyl formamide solutions or dimethyl are sub- in methods described
Sulfone, gamma-butyrolacton or two of which or two or more mixtures.
Further, barium titanate can be added in FAMX in methods described3Solution, MAMX can also be added in3Solution, can also
It is added in the two mixed solution, can also be added among organic solvent.
Further, (FAMX in methods described3)x(MAMX3)(1-x)In mixed solution, x numerical value is 1 >=x >=0.
Existing perovskite solar cell typically measures the electric electricity conversion of battery by I-V, but during reverse scan
Fill factor, curve factor bigger during than forward scan can be obtained, so as to obtain higher electricity conversion, this is typically by battery
Caused by the iron electric polarization of internal calcium titanium ore bed, this hesitation is typically as caused by inside battery structure, it is difficult to eliminates.
The present invention has ferroelectric barium titanate nano particle by being mixed in calcium titanium ore bed, to improve in perovskite solar cell
Iron electric polarization, improve perovskite solar cell opto-electronic conversion performance.Experimental method technique of the present invention is simple, operation side
Just, cost is low, and preparation temperature is low, film morphology is controllable, suitable for improving perovskite solar cell ferroelectricity polarity, improves calcium titanium
The stability and electricity conversion of ore deposit solar cell.
Brief description of the drawings
Fig. 1 is the perovskite (FAMX of barium titanate doping3)x(MAMX3)(1-x)Solar cell device structure chart, wherein：1-
Electrically conducting transparent basalis；2- densifications semiconductor/electron transfer layer；3- multi-stage porous semiconductor/electron transfer layer；4- barium titanate dopings
Perovskite light-absorption layer；5- hole transmission layers；6- metal electrode layers；7- perovskites (FAMX3)x(MAMX3)(1-x)Light-absorption layer；8- titaniums
Sour barium.
Fig. 2 is ESEM (SEM) photo of the perovskite thin film of barium titanate doping in embodiment 1.
Fig. 3 is ESEM (SEM) photo for not having in embodiment 2 perovskite thin film of barium titanate doping.
Fig. 4 is X-ray diffraction (XRD) the analysis collection of illustrative plates of the perovskite thin film of barium titanate doping in embodiment 1.
Fig. 5 is in AM1.5,100mW/cm2Under one sun standard illumination condition, the calcium of barium titanate doping in embodiment 1
Titanium
The C-V characteristic J-V curves of ore deposit solar cell.
Table 1 is the perovskite solar cell parameter of barium titanate doping in embodiment 1.
Embodiment
It is below specific embodiment, so as to which the present invention is expanded on further.It will be appreciated that these embodiments are merely to illustrate this
Invention rather than limitation the scope of the present invention, make any change or change to the present invention, these equivalent form of values are equally fallen within
The application appended claims limited range.
Embodiment 1
(1) calcium titanium ore bed preparation process
Take PbI2、HC(NH2)2I is put into beaker, adds anhydrous level N-N dimethylformamides and dimethyl sulfoxide (DMSO), temperature 70
DEG C, stir 12 hours, compound concentration is 1.3mol/l FAPbI3Liquid, take PbI2、CH3NH3I is put into beaker, adds nothing
Water level N-N dimethylformamides and dimethyl sulfoxide (DMSO), temperature are 70 DEG C, are stirred 12 hours, and compound concentration is 1.3mol/l's
MAPbI3Liquid, by above-mentioned solution by volume 5:1 mixing, temperature are 70 DEG C, stir 12 hours, prepare (FAPbI3)0.83
(MAPbI)0.17Solution, barium titanate is added among above-mentioned solution, the concentration of barium titanate is 0.23 mg/mL, by above-mentioned solution
It is added dropwise on the mesoporous TiO 2 handled well, spin-coating, rotating speed 1500r/min, spin-coating time 30 seconds, after spin coating
Sample at 150 DEG C, be heat-treated 30 minutes.Pass through Fig. 2 SEM photograph, it can be seen that it is thin that BTO has been incorporated into perovskite
In film；Fig. 4 XRD data demonstrate BTO and are already present in the laminated film of embodiment 1；Fig. 5 J-V test datas are shown
The perovskite solar battery efficiency for adulterating BTO is 10.72%.
Table 1
Embodiment 2
(1) calcium titanium ore bed preparation process
Take PbI2、HC(NH2)2I is put into beaker, adds anhydrous level N-N dimethylformamides and dimethyl sulfoxide (DMSO), temperature
For 70 DEG C, stir 12 hours, compound concentration is 1.3mol/l FAPbI3Liquid, take PbI2、CH3NH3I is put into beaker, is added
Anhydrous level N-N dimethylformamides and dimethyl sulfoxide (DMSO), temperature are 70 DEG C, are stirred 12 hours, and compound concentration is 1.3mol/l's
MAPbI3Liquid, by above-mentioned solution by volume 5:1 mixing, temperature are 70 DEG C, stir 12 hours, prepare (FAPbI3) 0.83
(MAPbI3)0.17Solution, barium titanate is added among above-mentioned solution, the concentration of barium titanate is 0.23mg/mL, by above-mentioned solution
It is added dropwise on the mesoporous TiO 2 handled well, spin-coating, rotating speed 1500r/min, spin-coating time 30 seconds, after spin coating
Sample is heat-treated 30 minutes at 150 DEG C.
In a word, the present invention has ferroelectric barium titanate nano particle by being mixed in calcium titanium ore bed, to improve calcium titanium
Iron electric polarization in ore deposit solar cell, improve the opto-electronic conversion performance of perovskite solar cell.Experimental method work of the present invention
Skill is simple, easy to operate, and cost is low, and preparation temperature is low, film morphology is controllable, suitable for improving perovskite solar cell ferroelectricity
Polarity, improve the stability and electricity conversion of perovskite solar cell.
Claims (5)
1. the preparation method of the organohalogen compounds perovskite thin film of a kind of barium titanate doping, it is characterised in that comprise the following steps：
First, metal halide MX is taken2、HC(NH2)2X and CH3NH3X, wherein HC (NH2)2X is abbreviated as FAX, CH3NH3X is abbreviated as
MAX, by metal halide MX2With HC (NH2)2X is added among organic solvent, under the conditions of temperature is 50~150 DEG C, stirring
0.1~24 hour, compound concentration was 0.01~5mol/l FAMX3Solution, by metal halide MX2And CH3NH3X is added to
In organic solvent, under the conditions of temperature is 50~150 DEG C, stir 0.1~24 hour, compound concentration is 0.01~5mol/l's
MAMX3Solution, FAMX3Solution and MAMX3Solution is 1 according to concentration ratio:10~10:1 ratio mixing, temperature be 50~
150 DEG C, stir 0.1~24 hour, obtain (the FAMX that concentration is 0.01~5mol/l3)x(MAMX3)(1-x)Mixed solution；Secondly,
Barium titanate BTO solution is added to (FAMX3)x(MAMX3)(1-x)Among mixed solution, stir 0.1~24 hour, it is dense that BTO is made
Spend the BTO/ (FAMX for 0.01~5mol/L3)x(MAMX3)(1-x)Mixed solution, finally, by BTO/ (FAMX3)x(MAMX3)(1-x)
Mixed solution is added dropwise on substrate film, spin-coating, and rotating speed is 500~7500r/min, 1~150 second spin-coating time,
Sample after spin-coating is heat-treated 5 minutes~60 minutes at 20~150 DEG C.
2. the preparation method of the organohalogen compounds perovskite thin film of barium titanate doping according to claim 1, its feature exist
In：The metal halide MX2Middle M can be more than one or both of Sn, Ge, Cu and Cs.
3. the preparation method of the organohalogen compounds perovskite thin film of barium titanate doping according to claim 1, its feature exist
In the MX2、HC(NH2)2X and CH3NH3X in X can be I, Br and Cl, in one or more kinds of mixtures.
4. the preparation method of the organohalogen compounds perovskite thin film of barium titanate doping according to claim 1, its feature exist
In the organic solvent can be one or both of N-N dimethyl formamide solutions, dimethyl sulfoxide (DMSO) and gamma-butyrolacton
Mixture above.
5. a kind of preparation method of the organohalogen compounds calcium titanium ore bed of barium titanate doping according to claim 1, its feature
It is, (the FAMX3)x(MAMX3)(1-x)In mixed solution, x numerical value is 1 >=x >=0.
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Cited By (9)
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| CN108281555A (en) * | 2018-01-27 | 2018-07-13 | 吉林大学 | It is a kind of using titanium oxide and barium titanate composite material as the perovskite solar cell of electron transfer layer and preparation method thereof |
| CN108470836A (en) * | 2018-04-10 | 2018-08-31 | 南京邮电大学 | A kind of preparation method and solar cell of perovskite thin film |
| CN108948089A (en) * | 2018-07-16 | 2018-12-07 | 天津师范大学 | One kind having photoelectric metal organic hybrid perovskite material and application |
| CN109560197A (en) * | 2018-11-21 | 2019-04-02 | 苏州大学 | Ferroelectric perovskite solar cell based on polarization and preparation method thereof |
| CN109755147A (en) * | 2018-11-26 | 2019-05-14 | 北京铂阳顶荣光伏科技有限公司 | Membrane photovoltaic component test method and membrane photovoltaic component |
| CN113594356A (en) * | 2020-04-30 | 2021-11-02 | 南京理工大学 | Ferroelectric oxide and MAxFA1-xPbI30-3 composite film material |
| CN113790744A (en) * | 2021-09-10 | 2021-12-14 | 华能新能源股份有限公司 | Optical detection method and optical detector |
| CN114914318A (en) * | 2022-04-29 | 2022-08-16 | 复旦大学 | Barium titanate @ mesoporous titanium dioxide heterojunction two-dimensional film and preparation method and application thereof |
| WO2024109770A1 (en) * | 2022-11-24 | 2024-05-30 | 中国科学院深圳先进技术研究院 | Current-capacitor dual-working mode direct x-ray detector and preparation method |
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|---|---|---|---|---|
| CN108281555A (en) * | 2018-01-27 | 2018-07-13 | 吉林大学 | It is a kind of using titanium oxide and barium titanate composite material as the perovskite solar cell of electron transfer layer and preparation method thereof |
| CN108470836B (en) * | 2018-04-10 | 2021-08-24 | 南京邮电大学 | Preparation method of perovskite thin film and solar cell |
| CN108470836A (en) * | 2018-04-10 | 2018-08-31 | 南京邮电大学 | A kind of preparation method and solar cell of perovskite thin film |
| CN108948089A (en) * | 2018-07-16 | 2018-12-07 | 天津师范大学 | One kind having photoelectric metal organic hybrid perovskite material and application |
| CN109560197A (en) * | 2018-11-21 | 2019-04-02 | 苏州大学 | Ferroelectric perovskite solar cell based on polarization and preparation method thereof |
| CN109560197B (en) * | 2018-11-21 | 2021-08-06 | 苏州大学 | Ferroelectric perovskite solar cell based on polarization and preparation method thereof |
| CN109755147A (en) * | 2018-11-26 | 2019-05-14 | 北京铂阳顶荣光伏科技有限公司 | Membrane photovoltaic component test method and membrane photovoltaic component |
| CN113594356A (en) * | 2020-04-30 | 2021-11-02 | 南京理工大学 | Ferroelectric oxide and MAxFA1-xPbI30-3 composite film material |
| CN113790744A (en) * | 2021-09-10 | 2021-12-14 | 华能新能源股份有限公司 | Optical detection method and optical detector |
| WO2023035445A1 (en) * | 2021-09-10 | 2023-03-16 | 中国华能集团清洁能源技术研究院有限公司 | Photodetection method and photodetector |
| CN114914318A (en) * | 2022-04-29 | 2022-08-16 | 复旦大学 | Barium titanate @ mesoporous titanium dioxide heterojunction two-dimensional film and preparation method and application thereof |
| CN114914318B (en) * | 2022-04-29 | 2023-09-22 | 复旦大学 | Barium titanate@mesoporous titanium dioxide heterojunction two-dimensional film and preparation method and application thereof |
| WO2024109770A1 (en) * | 2022-11-24 | 2024-05-30 | 中国科学院深圳先进技术研究院 | Current-capacitor dual-working mode direct x-ray detector and preparation method |
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