CN108365102A - A kind of stability and high efficiency two-dimensional layer perovskite solar cell and preparation method thereof - Google Patents
A kind of stability and high efficiency two-dimensional layer perovskite solar cell and preparation method thereof Download PDFInfo
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- CN108365102A CN108365102A CN201810153988.3A CN201810153988A CN108365102A CN 108365102 A CN108365102 A CN 108365102A CN 201810153988 A CN201810153988 A CN 201810153988A CN 108365102 A CN108365102 A CN 108365102A
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- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
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- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/152—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising zinc oxide, e.g. ZnO
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Abstract
The invention discloses a kind of methods preparing stability and high efficiency two-dimensional layer perovskite solar cell in air, it is characterized in that in air, the growth that micron order perovskite crystal grain is realized by continuous heating in entire spin coating process, prepares the perovskite photovoltaic device of uniform smooth high quality perovskite thin film and stability and high efficiency.The method of " entire spin coating process continuous heating " disclosed in this invention, cause solvent quickly to volatilize and accelerates the growth and conversion of crystal grain, meanwhile being also beneficial to two-dimensional layer perovskite and being grown along perpendicular to substrate direction, ultimately form the uniform perovskite thin film of smooth densification.The method disclosed in the present does not need the protection of inert atmosphere, and prepared by the large area for being advantageously implemented perovskite, reduce cost.
Description
Technical field
The present invention relates to perovskite area of solar cell, more particularly relate to a kind of two-dimensional layer calcium titanium of stability and high efficiency
Mine solar cell and preparation method thereof.
Background technology
In recent years, perovskite solar cell is quickly grown in photovoltaic technology field, and photoelectric efficiency is from initial
3.8%, 22.7% is rapidly reached in a few years time, this growth rate is unprecedented in photovoltaic art.Calcium titanium
Pit wood material itself has the advantages such as light absorptive is strong, carrier mobility is high, carrier diffusion distance, band gap is adjustable so that calcium
Titanium ore material is expected to become optimal solar cell material, or even realizes 33% energy conversion efficiency.Together
When, perovskite solar cell can be prepared by simple low temperature solution polycondensation, and bendable can be made on flexible substrates
Bent flexible device, opposite with other photovoltaic technologies, the production process of perovskite solar cell is simple, at low cost and theoretically
Applicable range is wider.
Current efficient perovskite solar cell is mainly three-dimensional structure, although this structure has excellent photoelectricity
Performance, but it is all very sensitive to water, oxygen, the light in environment, and stability is poor.In three-dimensional perovskite be added long-chain amine or
Two-dimensional layer perovskite, which is made, in the organic molecules such as aromatic amine can greatly improve the hydrophobicity of perovskite, improve it in the environment
Stability, and the amount for changing organic molecule can directly affect the band gap of perovskite so that perovskite band gap can
It adjusts range to substantially increase, is more advantageous to and finds the perovskite material with ideal bandgap.Whether from theoretical research or never
The large-scale application come considers that the development prospect of two-dimensional layer perovskite solar cell is all very open.
It is worth noting that the crystal grain-growth of perovskite and the pattern of film are for the efficiency for improving perovskite thin film
It is vital.The preparation method of traditional two-dimensional layer perovskite thin film, the crystal grain of obtained perovskite can be towards being unfavorable for
The direction of carrier transport is grown so that device efficiency is extremely low.The highest two-dimensional layer perovskite solar cell of efficiency at present
It needs to prepare perovskite thin film in such a way that substrate preheats, the base reservoir temperature of this mode is difficult control in spin coating process
System, poor repeatability, and it is more demanding to the technology of operator.Base reservoir temperature is inhomogenous simultaneously can directly result in perovskite obtained
Film became uneven, homogeneity are deteriorated.Moreover, at present the preparation process of two-dimensional layer perovskite substantially in inert atmosphere into
Capable, it is unfavorable for industrialization large-scale production.
Invention content
The present invention is intended to provide a kind of method that two-dimensional layer perovskite is prepared in air, and realize the calcium of efficient stable
Titanium ore solar cell.
The method that traditional room temperature prepares perovskite is unfavorable for perovskite crystal grain and is grown towards beneficial direction, and solvent
Volatilization is slow, remains the problems such as more.And the mode of substrate preheating, that there are base reservoir temperatures is inhomogenous, solvent evaporation rate is inhomogenous
The problems such as.In order to overcome the problems, such as these, the present invention uses the lower ionic liquid of boiling point as solvent, with entire spin coating process
Continuous heating stablizes the mode in a suitable temperature range, by the adjusting solubility of two-dimensional layer perovskite, spin coating rotating speed,
Spin coating temperature and time, annealing time and temperature can effectively regulate and control two-dimensional layer to realize the quick uniform volatilization of solvent
The average grain size of perovskite, at the same make crystal grain towards perpendicular to the direction of substrate grow, finally obtain surface uniformly, cause
Film close, crystallinity is high improves the electricity conversion and stability of perovskite.Further for traditional N, N- dimethyl
Formamide (DMF), Dimethyl Asian Maple (DMSO) equal solvent, acetic acid methylamine (MAAc) used, formic acid methylamine (MAFA) plasma are molten
The toxicity of agent substantially reduces, to more environment-friendly;The film of entire two-dimensional layer perovskite carries out in air completely, reduces
Production cost, is more advantageous to industrialization large-scale production.
In order to solve the above-mentioned technical problem, technical solution proposed by the present invention is:A kind of stability and high efficiency two-dimensional layer calcium titanium
The preparation process of the preparation method of mine solar cell, the perovskite light-absorption layer carries out in air completely and whole process is held
The device architecture of continuous heating, the perovskite solar cell includes transparent conductive substrate, hole transmission layer, perovskite suction successively
Photosphere, electron transfer layer, interface-modifying layer and metal electrode, the hole transmission layer and electron transfer layer are prepared by solwution method,
The interface-modifying layer and metal electrode are prepared by thermal evaporation deposition process, and the preparation of the perovskite light-absorption layer includes following step
Suddenly:
A, by metal halide, methylamine salt and macromolecular amine salt according to stoichiometric ratio (n:n-1:2, n=1~∞, n
∈ R) it dissolves in a solvent, 60 DEG C of stirring 1-18h obtain the perovskite precursor solution of clear;The perovskite presoma
The concentration of solution is in 100-400mg/ml;
B, in air, precursor solution is preheated at 60 DEG C, 70-200 μ L precursor solutions is taken to be added drop-wise to 60-200 DEG C
In the substrate and rapidly spin coating 10s -3min under 2000-8000rmp rotating speeds, entire spin coating process keep base reservoir temperature in 60-
200 DEG C, obtain uniform smooth perovskite thin film;
C, gained perovskite thin film at 60-150 DEG C is made annealing treatment to 0-10min, obtain the two-dimensional layer calcium titanium of high quality
Mine film.
Preferably, the transparent conductive substrate is in ITO electro-conductive glass or polyethylene terephthalate (PET)
It is a kind of.
Preferably, the hole transmission layer is poly- (3,4-rthylene dioxythiophene)-polystyrolsulfon acid (PEDOT:PSS)、
CuSCN、CuI、NiOx, one kind in RGO or GO, the electron transfer layer is one in fullerene derivate PCBM or ZnO
Kind, the interface-modifying layer is LiF, MoO3、BCP、C60One such, the metal electrode is in Al, Ag or Au
It is a kind of.
Preferably, the perovskite light-absorption layer precursor solution solvent for use is one or more of DMF, DMSO, MAAc
Mixture.
Preferably, the perovskite light-absorption layer is A '2An-1MnX3n+1(n=1~∞, n ∈ R), wherein A ' be long-chain amine from
Son or aromatic amine ion, A are methylamine ion, and M is the metal ions such as lead, tin, one or more of X Cl, Br, I.
Advantageous effect:Compared with the preparation method of other perovskite solar cells, the present invention can prepare calcium in air
Titanium ore active layer, and do not influenced completely by environmental factor, solvent for use is the organic solvent of hypotoxicity, meets Green Chemistry
Theory.In addition to this, grown along the direction of vertical substrate using the crystal grain of two-dimentional perovskite thin film produced by the present invention, crystal grain compared with
Greatly, defect is less so that short circuit current significantly improves the two-dimentional perovskite solar cell, it can be achieved that stability and high efficiency.These are special
Property is advantageous to realize large-scale commercial applications.
Description of the drawings
Fig. 1 is a kind of two-dimensional layer perovskite solar battery structure schematic diagram of efficient stable in the embodiment of the present invention.
Fig. 2 is that DMF traditional in the embodiment of the present invention makees solvent using two-dimensional layer calcium titanium made from substrate preheating method
J-V curves, photoelectric properties parameter and the traditional DMF of mine solar cell make solvent using two dimension made from substrate preheating method
The atomic force microscopy diagram of laminated perovskite film.
Fig. 3 is that MAAc makees solvent using the two-dimensional layer perovskite sun made from heating spin coating mode in the embodiment of the present invention
J-V curves, photoelectric properties parameter and the MAAc of energy battery make solvent using two-dimensional layer perovskite made from heating spin coating mode
The atomic force microscopy diagram of film.
Fig. 4 is the scanning electron microscope diagram using two-dimensional layer perovskite thin film surface made from substrate preheating method
Specific implementation method
Embodiment 1
The present invention provides a kind of two-dimensional layer perovskite solar cell of efficient stable, and structure is conductive, transparent successively
Substrate (ITO, PET etc.), hole transmission layer (PEDOT:PSS、CuI、CuSCN、NiOX, RGO, GO etc.), two-dimensional layer perovskite
Active layer A '2An-1MnX3n+1(n=1~∞), electron transfer layer (PCBM, ZnO etc.), interface-modifying layer (LiF, MoO3、BCP、C60
Deng), metal electrode (Au, Ag, Al etc.).
The method that two-dimensional layer perovskite solar cell is prepared in a kind of air provided by the present invention, primary operational step
It is rapid as follows:
Step 1:The conductive transparent substrate crossed by clean process is dried up with nitrogen, and hydrophilic treated is done to it.
Step 2:On the conductive transparent substrate handled by step 1, pass through solution spin coating proceeding deposition of hole
Transport layer.
Step 3:The device handled by step 2 is placed on heating spin coating instrument, heating spin coating work is continued through
Skill deposits two-dimensional layer perovskite active layer.
Step 4:The device handled by step 3 is transferred in inert atmosphere, solution is continued through on surface
Spin coating proceeding deposits electron transfer layer.
Step 5:The device handled by step 4 is transferred in evaporated device, boundary is deposited with certain rate
Face decorative layer and metal electrode.
The step 1 includes the following steps:A, conductive transparent substrate is one kind in ITO or PET;B, clean with washing successively
Agent, deionized water, acetone, EtOH Sonicate clean 20min, are then dried up with nitrogen gun;C, some transparent substrates will be arrived with ultraviolet smelly
Oxygen machine handles 15min~30min.
The step 2 includes the following steps:A, PETDOT is selected:In the materials such as PSS, CuSCN, CuI, NiOx, RGO, GO
The composite materials of one or several kinds of compositions be pre-configured to certain density solution.B, use spin coating instrument with certain spin coating
Rotating speed and time, in the hole transport that deposition thickness is 10nm~100nm on conductive transparent substrate after step 1 is processed
Layer.
The step 3 includes the following steps:A, by macromolecular amine salt, MACl and PbI2150mg is stoichiometrically made
mL-1~350mg mL-1Perovskite precursor solution, 1h~for 24 hours is stirred under the conditions of 50 DEG C~80 DEG C;B, in air, 60
DEG C~130 DEG C under conditions of, with rotating speed spin coating 10s~1min of 3000rmp~6000rmp during step 3 handles to obtain
Surface obtains two-dimensional layer perovskite thin film, and in 60 DEG C~100 DEG C stepped annealing 3min~10min.
The step 4 includes the following steps:A, the compound of one or several kinds of compositions in the materials such as PCBM, ZnO is selected
Material is pre-configured to certain density solution;B, use spin coating instrument with certain spin coating rotating speed and time, by step 1
Deposition thickness is the electron transfer layer of 10nm~100nm on conductive transparent substrate after processed.
The step 5 includes the following steps:A, vacuum degree is extracted into<5×10-4Pa;B, MoO3, LiF, BCP, C are selected60
It is a kind of as modifying interface layer material in equal materials, it selects a kind of as metal electrode electrode material in the materials such as Au, Ag, Al
Material, withSpeed evaporation thickness be about 1~10nm modifying interface layer material and thickness be 80~150nm
Metal electrode.
Embodiment 2
In the embodiment of the present invention two-dimensional layer perovskite solar cell structure as shown in Figure 1, set gradually for:ITO
Transparent conducting glass, hole transmission layer (PEDOT:PSS), two-dimensional layer perovskite active layer (BA2MA3Pb4IXCl13-x), electronics
Transport layer (PCBM), interface-modifying layer (LiF), metal electrode (Al).
1, the processing of two-dimensional layer perovskite solar cell conductive transparent substrates
(1) transparent electro-conductive glass once 20min, deionized water, acetone, ethyl alcohol is ultrasonically treated with abluent to distinguish
Ultrasonic 10min;(2) cleaning transparent electro-conductive glass is handled into 20min in UV ozone machine.
2, the preparation of two-dimensional layer perovskite solar cell hole transmission layer
(1) by hole transport layer material PEDOT:PSS is first filtered with 0.22 μm of water system filtering head, is then turned with liquid-transfering gun
It moves to by the processed ITO conductive glass surfaces of step 1, is paved with surface.(2) spin coating instrument is used to turn with 3000~5000rmp
Fast spin coating 30s~60s, annealing 15min~30min obtains thickness as 50nm or so calcium at 120 DEG C~140 DEG C after spin coating
Titanium ore hole transmission layer.
3, the preparation of two-dimensional layer perovskite solar cell photoactive layer
(1) tradition DMF makees solvent using the preparation of substrate preheating method
A, by BAI, MACl, PbI2According to 2:3:4 molar ratio is dissolved in DMF, and 1h~be made for 24 hours is stirred at 60 DEG C
200mg mL-1Precursor solution;B, precursor solution is preheated to 50 DEG C~100 DEG C, device is preheated to 60 made from step 1
DEG C~130 DEG C, the substrate of heat is quickly transferred on room temperature spin coating instrument, and be paved with precursor solution, spin coating 10s~60s, 60
DEG C~100 DEG C of Gradient annealing 3min~10min.
(2) MAAc make solvent using heating spin coating mode prepare
A, by BAI, MACl, PbI2According to 2:3:4 molar ratio is dissolved in MAAc, and 1h~be made for 24 hours is stirred at 60 DEG C
200mg mL-1Precursor solution;B, precursor solution is preheated to 50 DEG C~100 DEG C, device is transferred to 60 made from step 1
DEG C~130 DEG C of heating spin coating instrument on, and be paved with precursor solution, spin coating 10s~60s, entire spin coating process continuous heating,
60 DEG C~100 DEG C Gradient annealing 3min~10min.
4, the preparation of two-dimensional layer perovskite solar cell electron transfer layer
(1) electron transport layer materials PCBM is dissolved in anhydrous chlorobenzene, configuration concentration is the solution of 10~30mg/ml, 60
Magnetic agitation 24 hours at~70 DEG C;(2) device made from step 3 is transferred in inert atmosphere;(3) PCBM that will have been configured
Solution takes out the full device surface by step 3 processing of drop with liquid-transfering gun, is revolved with the rotating speed of 1000~3000rmp with spin coating instrument
Apply 30s~60s spin coatings.
5, the preparation of two-dimensional layer perovskite solar cell interface decorative layer and metal electrode
(1) device made from step 4 is transferred in evaporated device, and vacuum degree is evacuated to<5×10-4Pa;(2) firstRate obtain the LiF layers of 1nm~10nm, then with Rate obtain 80nm~
The Al electrodes of 150nm.
6, the test of two-dimensional layer perovskite active layer surface topography and two-dimensional layer perovskite solar cell properties ginseng
Several tests
Using JSM-7800F scanning electron microscope test two-dimensional layer perovskite active layer Cross Section Morphologies, such as Fig. 2 and figure
Shown in 3, makees solvent using MAAc and the perovskite active layer crystal grain being prepared using the method for heating spin coating is obviously grown up, it is thin
Membrane crystallization Quality advance, while surface is finer and close smooth.
The test of two-dimensional layer perovskite solar cell properties parameter using solar simulator (Oriel Newport,
150W, AM 1.5) it is used as light source, light intensity to be calibrated with standard silicon reference cell (Oriel Newport PN91150V).Intensity is
100mW cm-2The anode of the simulated solar irradiation of (AM 1.5) from two-dimensional layer perovskite solar cell is incident, uses Keithley
2400 digital sourcemeters record photoelectric current-voltage curve of battery.Give cell photoelectric performance parameter as shown in Figures 2 and 3
Test result, it is seen that make solvent with MAAc and using two-dimensional layer perovskite active layer battery made from the method for heating spin coating
Photoelectric conversion efficiency is improved significantly.
Embodiments of the present invention are described in detail in above example, and still, present invention is not limited to the embodiments described above
In detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention,
These simple variants all belong to the scope of protection of the present invention.
Claims (5)
1. a kind of preparation method of stability and high efficiency two-dimensional layer perovskite solar cell, which is characterized in that the perovskite is inhaled
The preparation process of photosphere carries out in air completely and whole process continuous heating, the device junction of the perovskite solar cell
Structure includes transparent conductive substrate, hole transmission layer, perovskite light-absorption layer, electron transfer layer, interface-modifying layer and metal electricity successively
Pole, the hole transmission layer and electron transfer layer are prepared by solwution method, and the interface-modifying layer and metal electrode are sunk by thermal evaporation
Prepared by product method, the preparation of the perovskite light-absorption layer comprises the steps of:
A, by metal halide, methylamine salt and macromolecular amine salt according to stoichiometric ratio (n:n-1:2, n=1~∞, n ∈ R)
In a solvent, 60 DEG C of stirring 1-18h obtain the perovskite precursor solution of clear for dissolving;The perovskite precursor solution
Concentration in 100-400mg/ml;
B, in air, precursor solution is preheated at 60 DEG C, 70-200 μ L precursor solutions is taken to be added drop-wise to 60-200 DEG C of substrate
Above and rapidly the spin coating 10s -3min under 2000-8000rmp rotating speeds, entire spin coating process keep base reservoir temperature in 60-200
DEG C, obtain uniform smooth perovskite thin film;
C, gained perovskite thin film is made annealing treatment to 0-10min at 60-150 DEG C, the two-dimensional layer perovskite for obtaining high quality is thin
Film.
2. the preparation method of stability and high efficiency two-dimensional layer perovskite solar cell as described in claim 1, which is characterized in that
The transparent conductive substrate is one kind in ITO electro-conductive glass or polyethylene terephthalate (PET).
3. the preparation method of stability and high efficiency two-dimensional layer perovskite solar cell as described in claim 1, which is characterized in that
The hole transmission layer is poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid (PEDOT:PSS)、CuSCN、CuI、NiOx、
One kind in RGO or GO, the electron transfer layer are one kind in fullerene derivate PCBM or ZnO, and the interface is repaiied
It is LiF, MoO to adorn layer3、BCP、C60One such, the metal electrode is one kind in Al, Ag or Au.
4. the preparation method of stability and high efficiency two-dimensional layer perovskite solar cell as described in claim 1, which is characterized in that
The perovskite light-absorption layer precursor solution solvent for use is the mixture of one or more of DMF, DMSO, MAAc.
5. the preparation method of stability and high efficiency two-dimensional layer perovskite solar cell as described in claim 1, which is characterized in that
The perovskite light-absorption layer is A '2An-1MnX3n+1(n=1~∞, n ∈ R), wherein A ' are long-chain amine ion or aromatic amine ion, A
For methylamine ion, M is the metal ions such as lead, tin, one or more of X Cl, Br, I.
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