CN110335947A - A kind of controllable perovskite solar battery of PCT ferroelectricity and preparation method thereof - Google Patents
A kind of controllable perovskite solar battery of PCT ferroelectricity and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the controllable perovskite solar battery of PCT ferroelectricity, are specifically implemented according to the following steps: step 1, cleaning FTO electro-conductive glass；Step 2 prepares Pb in FTO conductive glass surface0.8Ca0.2TiO3Electron transfer layer；Step 3, in Pb0.8Ca0.2TiO3Electron-transport layer surface prepares Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer；Step 4, Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface prepares Spiro-OMeTAD hole transmission layer；Gold electrode is deposited in Spiro-OMeTAD hole transport layer surface in step 5.The present invention does electron transfer layer using perovskite ferroelectric sull, constructs and be prepared for a kind of Pb0.8Ca0.2TiO3Base novel high efficiency high stability ferroelectricity is adjustable control multifunctional perovskite solar battery.
Description
Technical field
The invention belongs to the photovoltaic device technical fields in new energy, and in particular to a kind of controllable perovskite of PCT ferroelectricity
Solar battery further relates to a kind of preparation method of controllable PCT perovskite solar battery of P ferroelectricity.
Background technique
As one of most clean energy, solar energy attracts always the attention of vast researcher.Solar-electricity
Pond is the mode of main applied solar energy.Currently, solar battery is broadly divided into three categories: silica-based solar cell, dyestuff
Sensitization solar battery, perovskite solar battery.Wherein, perovskite solar battery is due to its low cost, low temperature preparation etc.
And possess tempting prospect.Since two thousand nine, short 10 year, the efficiency of perovskite solar battery realize from
3.8% to 24.2% swift and violent growth, has been approached the world record of monocrystaline silicon solar cell.It is main to its research at present
Concentrate on stability and functional aspect.
The structure of perovskite solar battery mainly has six parts to constitute: glass, FTO anode, electron transfer layer (ETL),
Light absorbing layer, hole transmission layer (HTL) and cathode.When solar cell device work, light absorption layer material is inhaled under light illumination
It receives photon and generates electron-hole pair, valence-band electrons can transit on conduction band, and electronics is by electron-transport after electron-hole pair separation
Layer extraction, hole are extracted by hole transmission layer, and when connecting external device, electrons and holes generate electricity after being extracted transmission
Stream.The solar cell material converted solar energy into electrical energy need to meet following condition: (1) suitable band gap i.e. 1.1~
1.7 eV；(2) forbidden band allowed transition；(3) high photoelectric conversion efficiency；(4) material structure and performance are stablized.
Organic and inorganic perovskite material since the advent of the world, because of its suitable band gap (1.55eV), the high absorption coefficient of light,
Long carrier diffusion length and higher dielectric constant and have received widespread attention.With ABX3As basic configuration
Perovskite material, wherein A is metal or organic ion (Cs+, MA+, FA+) etc., B is bivalent cation (Pb2+, Sn2+) etc., X is
Halide ion (Cl-, Br-, I-) etc., laboratory production method is mainly solution spin-coating method, blade coating and spraying.Hole transmission layer
It is for stopping electron-transport hole, between perovskite and metal electrode, Spiro-OMeTAD is because it is with very high
Hole mobility and be widely used.Hot evaporation system is mainly used in the preparation of electrode, can deposit to obtain very with it
Smooth metallic film.Electron transfer layer is used to transmit electronics between cathode and perovskite light absorbing layer, while preventing electricity
Compound, the common fine and close TiO in sub- hole2Nano particle.The principal element for restricting its commercial applications at present is its stabilization
Property problem, including thermal stability and air stability.Therefore developing efficient and stable perovskite solar battery is
The hot issue of research.
Summary of the invention
The first purpose of the invention is to provide a kind of preparation method of the controllable perovskite solar battery of PCT ferroelectricity,
Electron transfer layer is done using perovskite ferroelectric sull, constructs and be prepared for a kind of Pb0.8Ca0.2TiO3(PCT) base novel
High efficiency high stability ferroelectricity is adjustable control multifunctional perovskite solar battery.
First technical solution of the present invention is a kind of system of the controllable perovskite solar battery of PCT ferroelectricity
Preparation Method is specifically implemented according to the following steps:
Step 1, cleaning FTO electro-conductive glass；
Step 2 prepares Pb in FTO conductive glass surface0.8Ca0.2TiO3Electron transfer layer；
Step 3, in Pb0.8Ca0.2TiO3Electron-transport layer surface prepares Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorption
Layer；
Step 4, in Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface prepares Spiro-OMeTAD hole transport
Layer；
Gold electrode is deposited in Spiro-OMeTAD hole transport layer surface in step 5.
Detailed process is as follows for step 1:
Successively it is cleaned by ultrasonic 30~40min of FTO electro-conductive glass with dish washing liquid, isopropanol, acetone, alcohol, deionized water；
Again with being dried with nitrogen.
Detailed process is as follows for step 2:
Step 2.1, preparation Pb0.8Ca0.2TiO3Precursor solution
(1) calcium acetate and lead acetate are dissolved in ethylene glycol monomethyl ether；PH is adjusted to 4~5 with glacial acetic acid again；It adds
Formamide is modified；It is stirred under heating 0.5~1h, obtains solution A；
(2) the modified solution of tetrabutyl titanate of acetylacetone,2,4-pentanedione is added into solution A；The water-bath reflux 1 at 80~90 DEG C
~2 hours, yellow gum is obtained, prepares the Pb that concentration is 0.3~0.4mol/L0.8Ca0.2TiO3Precursor solution；
Step 2.2, preparation Pb0.8Ca0.2TiO3Electron transfer layer
By Pb0.8Ca0.2TiO3Precursor solution is spun on FTO conductive glass surface；Annealing, obtains Pb0.8Ca0.2TiO3Electricity
Sub- transport layer.
In step 2.1, calcium acetate, lead acetate, formamide, acetylacetone,2,4-pentanedione, butyl titanate the ratio between the amount of substance successively
For 0.2:(0.8~0.88): 1:1:1；Mixing speed is 500~600r/min；
In step 2.2, the revolving speed of spin coating is 3000~4000r/min, spin coating with a thickness of 100~150nm；Annealing item
Part is temperature: 500~550 DEG C, the time: 1~1.5h.
Detailed process is as follows for step 3:
Step 3.1, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution
Precursor powder CsI, FAI, MABr, PbI are weighed in proportion2、PbBr2；Measure presoma solvent two in proportion again
Methylformamide DMF, dimethyl sulfoxide DMSO；Presoma solvent is added in precursor powder；Prepare concentration be 1.2~
The Cs of 1.4mol/L0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution；By Cs0.05FA0.8MA0.15PbI2.55Br0.45Presoma
Solution is sealed together with magneton, 1~2h of magnetic agitation under room temperature；
Step 3.2, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer
Draw Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution is added dropwise to Pb0.8Ca0.2TiO3Film surface；It adopts
Spin coating is carried out with two step spin-coating methods；After spin coating, heated 1~1.5 hour at 100~120 DEG C；It obtains
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer.
In step 3.1, dimethylformamide DMF, dimethyl sulfoxide DMSO volume ratio be DMF:DMSO=(3~4):
(1~2)；The concentration > 99% of dimethylformamide DMF；The concentration > 99% of dimethyl sulfoxide DMSO；Magnetic stirring speed is
600~900r/min；
In step 3.2, two step spin-coating methods specifically:
Step 1: with the revolving speed spin coating 20s of 1000~1200r/min；
Step 2: with the revolving speed spin coating 30s of 5000~6000r/min；The step is carried out to 24~25s, be added dropwise concentration >
Excess of solvent is precipitated in 99% chlorobenzene；
The overall thickness of spin coating is between 200~300nm.
Detailed process is as follows for step 4:
Step 4.1, preparation Spiro-OMeTAD precursor solution
It measures Spiro-OMeTAD powder, 4- tert .-butylpyridine, lithium salts Li-TFSI in proportion to be dissolved in chlorobenzene, room temperature stirs
2~3h is mixed, the Spiro-OMeTAD precursor solution that concentration is 0.08~0.09g/mL is prepared；
Step 4.2, preparation Spiro-OMeTAD hole transmission layer
Filter Spiro-OMeTAD precursor solution；Filtered Spiro-OMeTAD precursor solution is spun on
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface aoxidizes 10~12h in drier, obtains Spiro-OMeTAD sky
Cave transport layer.
In step 4.1, volume accounting of the 4- tert .-butylpyridine TBP in Spiro-OMeTAD precursor solution be 2.2~
2.5%；Volume accounting of the lithium salts Li-TFSI in Spiro-OMeTAD precursor solution is 3.6~4.0%；Lithium salts Li-
The concentration of TFSI is 450~520g/L；Concentration > 99% of chlorobenzene；Purity > 99.5% of Spiro-OMeTAD powder；Stirring speed
Degree is 400~600r/min；
In step 4.2, the revolving speed of spin coating is 4000~5000r/min；Spin coating with a thickness of 150~200nm.
Detailed process is as follows for step 5:
The Au electrode of 60~80nm is deposited in the Au of purity > 99.99% on Spiro-OMeTAD hole transmission layer.
A second object of the present invention is to provide a kind of controllable perovskite solar-electricities of Pb0.8Ca0.2TiO3 ferroelectricity
Pond does electron transfer layer using perovskite ferroelectric sull, constructs and be prepared for a kind of Pb0.8Ca0.2TiO3Base novel is high
Efficiency high stability ferroelectricity is adjustable control multifunctional perovskite solar battery.
Second technical solution of the present invention is the perovskite solar energy prepared using above-mentioned preparation method
Battery is followed successively by FTO electro-conductive glass, Pb from bottom to top0.8Ca0.2TiO3Electron transfer layer,
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer, Spiro-OMeTAD hole transmission layer, Au electrode；
The resistance value of the FTO electro-conductive glass is 8 Ω/m2；
The Pb0.8Ca0.2TiO3Electron transport layer thickness is 100~150nm；
The Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer is with a thickness of 200~300nm；
The Spiro-OMeTAD thickness of hole transport layer is 150~200nm；
The Au thickness of electrode is 60~80nm.
The beneficial effects of the present invention are:
(1) battery prepared using method of the invention, possesses 18.28% highest photoelectric conversion efficiency, and the calcium titanium
After mine solar battery saves 1440 hours under room temperature environment, battery photoelectric conversion efficiency still with higher and excellent
Stability；
(2) battery prepared using method of the invention in conjunction with iron electric polarization characteristic there is good ferroelectricity to regulate and control photovoltaic
The multifunctionality of performance；
(3) solar battery of the invention, uses Pb0.8Ca0.2TiO3Ferroelectric perovskite replaces previous perovskite solar-electricity
Common TiO in pond2Structure and electrical communication between electron transfer layer and perovskite can be improved, simultaneously in electron transfer layer
The defects of electron transfer layer can be reduced；
(4) solar battery of the invention, iron electric polarization regulate and control to facilitate the separation and extraction of electron hole pair, can
Short-circuit current density is improved, to promote the efficiency of battery；
(5) solar battery of the invention realizes application of the ferroelectric in perovskite solar battery, iron electric polarization
Regulation makes perovskite battery multifunction, has widened battery device in the application range of photoelectricity neighborhood.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the perovskite solar battery that preparation method of the present invention is prepared；
In the perovskite solar battery that Fig. 2, which is preparation method of the present invention, to be prepared according to the condition of embodiment 2
Pb0.8Ca0.2TiO3The XRD diagram of electron transfer layer；
Fig. 3 is the Pb that preparation method of the present invention is prepared according to the condition of embodiment 20.8Ca0.2TiO3Electron transfer layer
Ferroelectric hysteresis loop figure；
The perovskite solar battery that Fig. 4, which is preparation method of the present invention, to be prepared according to the condition of embodiment 2 most efficiently
Rate figure；
Fig. 5 is the perovskite solar battery prepared according to the condition of embodiment 2 of preparation method of the present invention in not homopolarity
Change the efficiency chart under regulation；
Fig. 6 is that the perovskite solar battery that preparation method of the present invention is prepared according to the condition of embodiment 2 exists for a long time
Efficiency Statistics figure under room temperature environment；
Fig. 7 is the perovskite solar battery theoretical calculation that preparation method of the present invention is prepared according to the condition of embodiment 2
Not same polarization under PCT and FAPbI3Between charge transmit integral curve figure.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of the controllable perovskite solar battery of PCT ferroelectricity of the present invention, it is specifically real according to the following steps
It applies:
Step 1, cleaning FTO electro-conductive glass；
Detailed process is as follows:
Successively it is cleaned by ultrasonic 30~40min of FTO electro-conductive glass with dish washing liquid, isopropanol, acetone, alcohol, deionized water；
Again with being dried with nitrogen.
Step 2 prepares Pb in FTO conductive glass surface0.8Ca0.2TiO3Electron transfer layer；
Detailed process is as follows:
Step 2.1, preparation Pb0.8Ca0.2TiO3Precursor solution
(1) calcium acetate and lead acetate are dissolved in ethylene glycol monomethyl ether；PH is adjusted to 4~5 with glacial acetic acid again；It adds
Formamide is modified；It is stirred under heating 0.5~1h, obtains solution A；
(2) the modified solution of tetrabutyl titanate of acetylacetone,2,4-pentanedione is added into solution A；The water-bath reflux 1 at 80~90 DEG C
~2 hours, yellow gum is obtained, prepares the Pb that concentration is 0.3~0.4mol/L0.8Ca0.2TiO3Precursor solution；
Wherein, the ratio between the amount of substance of calcium acetate, lead acetate, formamide, acetylacetone,2,4-pentanedione, butyl titanate is followed successively by
0.2:(0.8~0.88): 1:1:1；Mixing speed is 500~600r/min；
Step 2.2, preparation Pb0.8Ca0.2TiO3Electron transfer layer
By Pb0.8Ca0.2TiO3Precursor solution is spun on FTO conductive glass surface；Annealing, obtains Pb0.8Ca0.2TiO3Electricity
Sub- transport layer；
Wherein, the revolving speed of spin coating be 3000~4000r/min, spin coating with a thickness of 100~150nm；Annealing conditions are,
Temperature: 500~550 DEG C, the time: 1~1.5h.
Step 3, in Pb0.8Ca0.2TiO3Electron-transport layer surface prepares Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorption
Layer；
Detailed process is as follows:
Step 3.1, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution
Precursor powder CsI, FAI, MABr, PbI are weighed in proportion2、PbBr2；Measure presoma solvent two in proportion again
Methylformamide DMF, dimethyl sulfoxide DMSO；Presoma solvent is added in precursor powder；Prepare concentration be 1.2~
The Cs of 1.4mol/L0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution；By Cs0.05FA0.8MA0.15PbI2.55Br0.45Presoma
Solution is sealed together with magneton, 1~2h of magnetic agitation under room temperature；
Wherein, dimethylformamide DMF, dimethyl sulfoxide DMSO volume ratio be DMF:DMSO=(3~4): (1~
2)；The concentration > 99% of dimethylformamide DMF；The concentration > 99% of dimethyl sulfoxide DMSO；Magnetic stirring speed is 600
~900r/min；
Step 3.2, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer
Draw Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution is added dropwise to Pb0.8Ca0.2TiO3Film surface；It adopts
Spin coating is carried out with two step spin-coating methods；After spin coating, heated 1~1.5 hour at 100~120 DEG C；It obtains
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer；
Two step spin-coating methods specifically:
Step 1: with the revolving speed spin coating 20s of 1000~1200r/min；
Step 2: with the revolving speed spin coating 30s of 5000~6000r/min；The step is carried out to 24~25s, be added dropwise concentration >
Excess of solvent is precipitated in 99% chlorobenzene；
The overall thickness of spin coating is between 200~300nm.
Step 4, in Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface prepares Spiro-OMeTAD hole transport
Layer；
Detailed process is as follows:
Step 4.1, preparation Spiro-OMeTAD precursor solution
It weighs Spiro-OMeTAD powder, 4- tert .-butylpyridine, lithium salts Li-TFSI in proportion to be dissolved in chlorobenzene, room temperature stirs
2~3h is mixed, the Spiro-OMeTAD precursor solution that concentration is 0.08~0.09g/mL is prepared；
Wherein, volume accounting of the 4- tert .-butylpyridine TBP in Spiro-OMeTAD precursor solution be 2.2~
2.5%；Volume accounting of the lithium salts Li-TFSI in Spiro-OMeTAD precursor solution is 3.6~4.0%；Lithium salts Li-
The concentration of TFSI is 450~520g/L；Concentration > 99% of chlorobenzene；Purity > 99.5% of Spiro-OMeTAD powder；Stirring speed
Degree is 400~600r/min；
Step 4.2, preparation Spiro-OMeTAD hole transmission layer
Filter Spiro-OMeTAD precursor solution；Filtered Spiro-OMeTAD precursor solution is spun on
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface aoxidizes 10~12h in drier, obtains Spiro-OMeTAD
Hole transmission layer；
Wherein, the revolving speed of spin coating is 4000~5000r/min；Spin coating with a thickness of 150~200nm.
Gold electrode is deposited in Spiro-OMeTAD hole transport layer surface in step 5
Detailed process is as follows:
The Au electrode of 60~80nm is deposited in the Au of purity > 99.99% on Spiro-OMeTAD hole transmission layer.
The perovskite solar battery prepared using above-mentioned preparation method, be followed successively by from bottom to top FTO electro-conductive glass,
Pb0.8Ca0.2TiO3Electron transfer layer, Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer, Spiro-OMeTAD hole transport
Layer, Au electrode；
The resistance value of FTO electro-conductive glass is 8 Ω/m2；
Pb0.8Ca0.2TiO3Electron transport layer thickness is 100~150nm；
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer is with a thickness of 200~300nm；
Spiro-OMeTAD thickness of hole transport layer is 150~200nm；
Au thickness of electrode is 60~80nm.
Embodiment 1
Step 1, cleaning FTO electro-conductive glass；
Successively it is cleaned by ultrasonic 30~40min of FTO electro-conductive glass with dish washing liquid, isopropanol, acetone, alcohol, deionized water；
Again with being dried with nitrogen.
Step 2 prepares Pb in FTO conductive glass surface0.8Ca0.2TiO3Electron transfer layer；
Step 2.1, preparation Pb0.8Ca0.2TiO3Precursor solution
(1) calcium acetate and lead acetate are dissolved in ethylene glycol monomethyl ether；PH is adjusted to 4~5 with glacial acetic acid again；It adds
Formamide is modified；It is stirred under heating 0.5~1h, obtains solution A；
(2) the modified solution of tetrabutyl titanate of acetylacetone,2,4-pentanedione is added into solution A；The water-bath reflux 1 at 80~90 DEG C
~2 hours, yellow gum is obtained, prepares the Pb that concentration is 0.3mol/L0.8Ca0.2TiO3Precursor solution；
Wherein, the ratio between the amount of substance of calcium acetate, lead acetate, formamide, acetylacetone,2,4-pentanedione, butyl titanate is followed successively by
0.2:0.8:1:1:1；Mixing speed is 500~600r/min；
Step 2.2, preparation Pb0.8Ca0.2TiO3Electron transfer layer
By Pb0.8Ca0.2TiO3Precursor solution is spun on FTO conductive glass surface；Annealing, obtains Pb0.8Ca0.2TiO3Electricity
Sub- transport layer；
Wherein, the revolving speed of spin coating be 3000~4000r/min, spin coating with a thickness of 100nm；Annealing conditions are temperature:
500~550 DEG C, the time: 1~1.5h.
Step 3, in Pb0.8Ca0.2TiO3Electron-transport layer surface prepares Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorption
Layer；
Step 3.1, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution
Precursor powder CsI, FAI, MABr, PbI are weighed in proportion2、PbBr2；Measure presoma solvent two in proportion again
Methylformamide DMF, dimethyl sulfoxide DMSO；Presoma solvent is added in precursor powder；Preparing concentration is
The Cs of 1.2mol/L0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution；By Cs0.05FA0.8MA0.15PbI2.55Br0.45Presoma
Solution is sealed together with magneton, 1~2h of magnetic agitation under room temperature；
Wherein, dimethylformamide DMF, dimethyl sulfoxide DMSO volume ratio be DMF:DMSO=3:2；Dimethyl methyl
The concentration > 99% of amide DMF；The concentration > 99% of dimethyl sulfoxide DMSO；Magnetic stirring speed is 600~900r/min；
Step 3.2, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer
Draw Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution is added dropwise to Pb0.8Ca0.2TiO3Film surface；It adopts
Spin coating is carried out with two step spin-coating methods；After spin coating, heated 1~1.5 hour at 100~120 DEG C；It obtains
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer；
Two step spin-coating methods specifically:
Step 1: with the revolving speed spin coating 20s of 1000~1200r/min；
Step 2: with the revolving speed spin coating 30s of 5000~6000r/min；The step is carried out to 24~25s, be added dropwise concentration >
Excess of solvent is precipitated in 99% chlorobenzene；
The overall thickness of spin coating is 200nm.
Step 4, in Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface prepares Spiro-OMeTAD hole transport
Layer；
Step 4.1, preparation Spiro-OMeTAD precursor solution
It weighs Spiro-OMeTAD powder, 4- tert .-butylpyridine, lithium salts Li-TFSI in proportion to be dissolved in chlorobenzene, room temperature stirs
2~3h is mixed, the Spiro-OMeTAD precursor solution that concentration is 0.08g/mL is prepared；
Wherein, volume accounting of the 4- tert .-butylpyridine TBP in Spiro-OMeTAD precursor solution is 2.2%；Lithium salts
Volume accounting of the Li-TFSI in Spiro-OMeTAD precursor solution is 3.6%；The concentration of lithium salts Li-TFSI is 450g/
L；Concentration > 99% of chlorobenzene；Purity > 99.5% of Spiro-OMeTAD powder；Mixing speed is 400~600r/min；
Step 4.2, preparation Spiro-OMeTAD hole transmission layer
Filter Spiro-OMeTAD precursor solution；Filtered Spiro-OMeTAD precursor solution is spun on
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface aoxidizes 10~12h in drier, obtains Spiro-OMeTAD
Hole transmission layer；
Wherein, the revolving speed of spin coating is 4000~5000r/min；Spin coating with a thickness of 150nm.
Gold electrode is deposited in Spiro-OMeTAD hole transport layer surface in step 5
The Au electrode of 60nm is deposited in the Au of purity > 99.99% on Spiro-OMeTAD hole transmission layer.
The perovskite solar battery prepared using above-mentioned preparation method, be followed successively by from bottom to top FTO electro-conductive glass,
Pb0.8Ca0.2TiO3Electron transfer layer, Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer, Spiro-OMeTAD hole transport
Layer, Au electrode；
The resistance value of FTO electro-conductive glass is 8 Ω/m2；
Pb0.8Ca0.2TiO3Electron transport layer thickness is 100nm；
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer is with a thickness of 200nm；
Spiro-OMeTAD thickness of hole transport layer is 150nm；
Au thickness of electrode is 60nm.
Embodiment 2
It is step 1, identical as the step 1 of embodiment 1.
Step 2, roughly the same with the step 2 of embodiment 1, difference is only that:
In step 2.1, Pb0.8Ca0.2TiO3The concentration of precursor solution is 0.35mol/L；Calcium acetate, lead acetate, formyl
The ratio between amine, acetylacetone,2,4-pentanedione, amount of substance of butyl titanate are followed successively by 0.2:0.84:1:1:1；
In step 2.2, spin coating with a thickness of 125nm.
Step 3, roughly the same with the step 3 of embodiment 1, difference is only that:
In step 3.1, Cs0.05FA0.8MA0.15PbI2.55Br0.45The concentration of precursor solution is 1.3mol/L；Dimethyl
Formamide DMF, dimethyl sulfoxide DMSO volume ratio be DMF:DMSO=3.5:1.5；
In step 3.2, the overall thickness of spin coating is 250nm.
Step 4, roughly the same with the step 4 of embodiment 1, difference is only that:
In step 4.1, the concentration of Spiro-OMeTAD precursor solution is 0.085g/mL；4- tert .-butylpyridine TBP exists
Volume accounting in Spiro-OMeTAD precursor solution is 2.35%；Lithium salts Li-TFSI is molten in Spiro-OMeTAD presoma
Volume accounting in liquid is 3.8%；The concentration of lithium salts Li-TFSI is 485g/L；
In step 4.2, spin coating with a thickness of 175nm.
Step 5, roughly the same with the step 5 of embodiment 1, difference is only that: the Au electrode of 70nm is deposited.
The perovskite solar battery prepared, is followed successively by FTO electro-conductive glass, Pb from bottom to top0.8Ca0.2TiO3Electronics
Transport layer, Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer, Spiro-OMeTAD hole transmission layer, Au electrode；
The resistance value of FTO electro-conductive glass is 8 Ω/m2；
Pb0.8Ca0.2TiO3Electron transport layer thickness is 125nm；
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer is with a thickness of 250nm；
Spiro-OMeTAD thickness of hole transport layer is 175nm；
Au thickness of electrode is 70nm.
Embodiment 3
It is step 1, identical as the step 1 of embodiment 1.
Step 2, roughly the same with the step 2 of embodiment 1, difference is only that:
In step 2.1, Pb0.8Ca0.2TiO3The concentration of precursor solution is 0.4mol/L；Calcium acetate, lead acetate, formyl
The ratio between amine, acetylacetone,2,4-pentanedione, amount of substance of butyl titanate are followed successively by 0.2:0.88:1:1:1；
In step 2.2, spin coating with a thickness of 150nm.
Step 3, roughly the same with the step 3 of embodiment 1, difference is only that:
In step 3.1, Cs0.05FA0.8MA0.15PbI2.55Br0.45The concentration of precursor solution is 1.4mol/L；Dimethyl
Formamide DMF, dimethyl sulfoxide DMSO volume ratio be DMF:DMSO=4:1；
In step 3.2, the overall thickness of spin coating is 300nm.
Step 4, roughly the same with the step 4 of embodiment 1, difference is only that:
In step 4.1, the concentration of Spiro-OMeTAD precursor solution is 0.09g/mL；4- tert .-butylpyridine TBP exists
Volume accounting in Spiro-OMeTAD precursor solution is 2.5%；Lithium salts Li-TFSI is molten in Spiro-OMeTAD presoma
Volume accounting in liquid is 4.0%；The concentration of lithium salts Li-TFSI is 520g/L；
In step 4.2, spin coating with a thickness of 200nm.
Step 5, roughly the same with the step 5 of embodiment 1, difference is only that: the Au electrode of 80nm is deposited.
The perovskite solar battery prepared, is followed successively by FTO electro-conductive glass, Pb from bottom to top0.8Ca0.2TiO3Electronics
Transport layer, Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer, Spiro-OMeTAD hole transmission layer, Au electrode；
Wherein, the resistance value of FTO electro-conductive glass is 8 Ω/m2；
Pb0.8Ca0.2TiO3Electron transport layer thickness is 150nm；
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer is with a thickness of 300nm；
Spiro-OMeTAD thickness of hole transport layer is 200nm；
Au thickness of electrode is 80nm.
It should be understood that
One, the area for the FTO electro-conductive glass that embodiment 1- embodiment 3 uses is 2.5cm*2.5cm.
Two, device efficiency will increase when applying positive polarization to ferroelectric thin film, and device efficiency can subtract when applying reverse polarization
It is small；The transmission direction of the charge obtained by first-principles calculations is consistent with the ferroelectricity regulation in experiment.
Three, efficiency test experiment is specific as follows:
The scheme of embodiment 1-3 is prepared for three different perovskite solar cell devices, passes through J-V test macro
The performance of three kinds of battery devices is tested, related data is as follows:
Four, attached drawing 2-7 is summarized as follows:
Fig. 2: the Pb of preparation is tested0.8Ca0.2TiO3The XRD diffraction pattern of film, the Pb prepared in experiment0.8Ca0.2TiO3
Film can be highly corresponding with PDF card, illustrates Pb0.8Ca0.2TiO3The formation of Perovskite Phase, obtained lenticular, uniformly/
The Pb of pure phase0.8Ca0.2TiO3Film.
Fig. 3: test Pb0.8Ca0.2TiO3The ferroelectric hysteresis loop of film, the film that we prepare have iron electric polarization, maximum pole
Change value is 18C/cm2, regulation can be played the role of to battery.
Fig. 4: the Pb prepared under optimal preparation method0.8Ca0.2TiO3The positive and negative of based perovskite battery device is swept.Device
Anti- peak efficiency of sweeping is 18.28%, and corresponding efficiency of just sweeping reaches 16.34%, illustrates the hesitation of battery to cell performance
The influence of energy is smaller.
Fig. 5: it indicates to Pb0.8Ca0.2TiO3Based perovskite battery device applies different iron electric polarizations and carries out ferroelectricity regulation
Influence to device performance, the results showed that the performance of device can gradually be promoted with the increase of iron electric polarization, it was confirmed that ferroelectricity
The separation that regulation facilitates electron hole pair improves the photovoltaic performance of battery to improve short-circuit current density.
Fig. 6: to Pb0.8Ca0.2TiO3Based perovskite battery device is tested under 25 DEG C, the room temperature environment of 35% humidity
After 60 days (test in every 10 days is primary), battery device photoelectric conversion efficiency is still able to maintain 80%, illustrates Pb0.8Ca0.2TiO3Base calcium
Titanium ore battery stability with higher.
Fig. 7: utilizing first principle, through theoretical calculation explanation under conditions of positive polarization and negative polarization, photogenerated charge
It is entirely different in perovskite and the transmission direction in electron transfer layer, so that further the Pb of preparation is tested in confirmation0.8Ca0.2TiO3
The Modulatory character energy of based perovskite battery device.
The advantages of solar battery prepared by the present invention are as follows:
(1) solar battery of the invention possesses 18.28% high photoelectric conversion efficiency, and compared in batch device
In conventional Ti O2Based perovskite solar battery obtains efficiency with higher；And there is preferable time and environmental stability.
(2) solar battery of the invention has good ferroelectricity regulating and controlling effect, by the way that ferroelectric material is added into device
As electron transfer layer to which regulating and controlling effect can be played to device performance.Ferroelectric thin film must be added so that in not same polarization feelings
Under condition, device parameter performance generation is different to be changed.
(3) solar battery of the invention must be polarized by theoretical calculation and two aspect mutual authentication ferroelectric materials of experiment
Device performance must be influenced, ferroelectric effect is explained from mechanism must influence charge transmission and device performance.
Claims (10)
1. a kind of preparation method of the controllable perovskite solar battery of PCT ferroelectricity, which is characterized in that specifically according to the following steps
Implement:
Step 1, cleaning FTO electro-conductive glass；
Step 2 prepares Pb in FTO conductive glass surface0.8Ca0.2TiO3Electron transfer layer；
Step 3, in Pb0.8Ca0.2TiO3Electron-transport layer surface prepares Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer；
Step 4, in Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface prepares Spiro-OMeTAD hole transmission layer；
Gold electrode is deposited in Spiro-OMeTAD hole transport layer surface in step 5.
2. the preparation method of perovskite solar battery as described in claim 1, which is characterized in that the step 1 it is specific
Process is as follows:
Successively it is cleaned by ultrasonic 30~40min of FTO electro-conductive glass with dish washing liquid, isopropanol, acetone, alcohol, deionized water；Nitrogen is used again
Air-blowing is dry.
3. the preparation method of perovskite solar battery as claimed in claim 2, which is characterized in that the step 2 it is specific
Process is as follows:
Step 2.1, preparation Pb0.8Ca0.2TiO3Precursor solution
(1) calcium acetate and lead acetate are dissolved in ethylene glycol monomethyl ether；PH is adjusted to 4~5 with glacial acetic acid again；Add formamide
It is modified；It is stirred under heating 0.5~1h, obtains solution A；
(2) the modified solution of tetrabutyl titanate of acetylacetone,2,4-pentanedione is added into solution A；Water-bath reflux 1~2 is small at 80~90 DEG C
When, yellow gum is obtained, the Pb that concentration is 0.3~0.4mol/L is prepared0.8Ca0.2TiO3Precursor solution；
Step 2.2, preparation Pb0.8Ca0.2TiO3Electron transfer layer
By Pb0.8Ca0.2TiO3Precursor solution is spun on FTO conductive glass surface；Annealing, obtains Pb0.8Ca0.2TiO3Electronics passes
Defeated layer.
4. the preparation method of perovskite solar battery as claimed in claim 3, which is characterized in that in the step 2.1, vinegar
The ratio between sour calcium, lead acetate, formamide, acetylacetone,2,4-pentanedione, amount of substance of butyl titanate are followed successively by 0.2:(0.8~0.88): 1:
1:1；Mixing speed is 500~600r/min；
In the step 2.2, the revolving speed of spin coating is 3000~4000r/min, spin coating with a thickness of 100~150nm；Annealing conditions
For temperature: 500~550 DEG C, the time: 1~1.5h.
5. the preparation method of perovskite solar battery as claimed in claim 4, which is characterized in that the step 3 it is specific
Process is as follows:
Step 3.1, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution
Precursor powder CsI, FAI, MABr, PbI are weighed in proportion2、PbBr2；Measure presoma solvent dimethyl methyl in proportion again
Amide DMF, dimethyl sulfoxide DMSO；Presoma solvent is added in precursor powder；Preparing concentration is 1.2~1.4mol/L
Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution；By Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution and magnetic
Son is sealed together, 1~2h of magnetic agitation under room temperature；
Step 3.2, preparation Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer
Draw Cs0.05FA0.8MA0.15PbI2.55Br0.45Precursor solution is added dropwise to Pb0.8Ca0.2TiO3Film surface；Using two steps
Spin-coating method carries out spin coating；After spin coating, heated 1~1.5 hour at 100~120 DEG C；It obtains
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer.
6. the preparation method of perovskite solar battery as claimed in claim 5, which is characterized in that in the step 3.1, two
Methylformamide DMF, dimethyl sulfoxide DMSO volume ratio be DMF:DMSO=(3~4): (1~2)；Dimethylformamide DMF
Concentration > 99%；The concentration > 99% of dimethyl sulfoxide DMSO；Magnetic stirring speed is 600~900r/min；
In the step 3.2, two step spin-coating methods specifically:
Step 1: with the revolving speed spin coating 20s of 1000~1200r/min；
Step 2: with the revolving speed spin coating 30s of 5000~6000r/min；The step is carried out to 24~25s, and the chlorine of concentration > 99% is added dropwise
Excess of solvent is precipitated in benzene；
The overall thickness of spin coating is between 200~300nm.
7. the preparation method of perovskite solar battery as claimed in claim 6, which is characterized in that the step 4 it is specific
Process is as follows:
Step 4.1, preparation Spiro-OMeTAD precursor solution
Spiro-OMeTAD powder, 4- tert .-butylpyridine, lithium salts Li-TFSI is weighed in proportion to be dissolved in chlorobenzene, stirring at normal temperature 2~
3h prepares the Spiro-OMeTAD precursor solution that concentration is 0.08~0.09g/mL；
Step 4.2, preparation Spiro-OMeTAD hole transmission layer
Filter Spiro-OMeTAD precursor solution；Filtered Spiro-OMeTAD precursor solution is spun on
Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer surface aoxidizes 10~12h in drier, obtains Spiro-OMeTAD sky
Cave transport layer.
8. the preparation method of perovskite solar battery as claimed in claim 7, which is characterized in that in the step 4.1,4-
Volume accounting of the tert .-butylpyridine TBP in Spiro-OMeTAD precursor solution is 2.2~2.5%；Lithium salts Li-TFSI exists
Volume accounting in Spiro-OMeTAD precursor solution is 3.6~4.0%；The concentration of lithium salts Li-TFSI is 450~520g/
L；Concentration > 99% of chlorobenzene；Purity > 99.5% of Spiro-OMeTAD powder；Mixing speed is 400~600r/min；
In the step 4.2, the revolving speed of spin coating is 4000~5000r/min；Spin coating with a thickness of 150~200nm.
9. the preparation method of perovskite solar battery as claimed in claim 8, which is characterized in that the step 5 it is specific
Process is as follows:
The Au electrode of 60~80nm is deposited in the Au of purity > 99.99% on Spiro-OMeTAD hole transmission layer.
10. the perovskite solar battery prepared using the described in any item preparation methods of claim 1-9, feature are existed
In being followed successively by FTO electro-conductive glass, Pb from bottom to top0.8Ca0.2TiO3Electron transfer layer, Cs0.05FA0.8MA0.15PbI2.55Br0.45Light
Absorbed layer, Spiro-OMeTAD hole transmission layer, Au electrode；
The resistance value of the FTO electro-conductive glass is 8 Ω/m2；
The Pb0.8Ca0.2TiO3Electron transport layer thickness is 100~150nm；
The Cs0.05FA0.8MA0.15PbI2.55Br0.45Light absorbing layer is with a thickness of 200~300nm；
The Spiro-OMeTAD thickness of hole transport layer is 150~200nm；
The Au thickness of electrode is 60~80nm.
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| CN114314670A (en) * | 2021-12-29 | 2022-04-12 | 西北大学 | Modification method of copper ion implanted zinc battery anode material delta-manganese dioxide |
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