CN106328813B - A kind of high stability mixes caesium Ca-Ti ore type solar cell and preparation method thereof - Google Patents
A kind of high stability mixes caesium Ca-Ti ore type solar cell and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of high stabilities to mix caesium Ca-Ti ore type solar cell and preparation method thereof.The solar cell includes successively from bottom to top：Light anode mixes caesium perovskite light-absorption layer, hole transmission layer and to electrode.The preparation for mixing caesium perovskite light-absorption layer includes：1) by PbI2DMF solution be applied to TiO2The surface of porous membrane layer, heating remove DMF, form PbI2Film；2) by CH3NH3I and caesium source are dissolved in organic solvent formation and contain CH3NH3The solution of I and caesium source, by the solution coating to the PbI2Caesium perovskite light-absorption layer is mixed in the surface heating reaction of film, formation.The present invention mixes caesium using two-step method, first deposits PbI2, after removing DMF, be coated with the aqueous isopropanol of cesium acetate and MAI, under heating condition with PbI2Reacted, avoid occur DMF decompose generate by-product, crystallization and the film forming of perovskite are influenced, to obtain higher efficiency.
Description
Technical field
The invention belongs to Ca-Ti ore type area of solar cell, and in particular to a kind of high stability mixes the caesium Ca-Ti ore type sun
Energy battery and preparation method thereof.
Background technology
After 21 century, economy and society are fast-developing, and demand of the mankind to the energy is increasing, energy problem at
For the major issue of relationship human survival.However, traditional fossil fuel (coal, oil, natural gas) is positive because constantly largely disappearing
It consumes and exhaustion increasingly.The exploitation of renewable new energy helps to alleviate the pressure of world energy sources and environment, and solar energy is resource
Amount is maximum, is distributed most commonly used green regenerative energy sources.
Solar cell can be converted into luminous energy electric energy, and the exploitation of solar cell is most effective using solar energy
One of approach.Solar cell is small, conveniently moving, uses not limited by regions.We both can be the sun
Energy battery makes large-scale power station, and realization is generated electricity by way of merging two or more grid systems, and can be easily with less battery component to remote
Regional user provides life electric energy, or provides electric power safeguard to mobile communication equipment.Currently, occupying leading position on the market
Solar cell be mainly monocrystalline silicon and polysilicon solar cell, the production technology comparative maturity of both batteries, battery
Photoelectric conversion efficiency it is higher, stability is good (service life is all at 15 years or more).But silicon systems solar cell is to raw material
It is required that harsh, purity generally will be 99.9999% or more, and complex manufacturing technology, cost remain high, cost of electricity-generating compared with
Height cannot achieve ultra-large functionization.
For the cost problem of silicon systems solar cell at this stage, since last century the nineties, a kind of novel has
Solar cell-dye-sensitized solar cells of machine-inorganic compounding is of low cost with its, prepares easy feature and causes
The extensive concern of people.It is also considered as a kind of up-and-coming technology using solar energy.
1991, Lausanne, SUI Gao Deng engineering institutesThe computer MSR Information system of professor is by porous TiO2Film is applied to this
In kind battery, the photoelectric conversion efficiency of this battery is made to be greatly improved, made breakthrough progress (Deng,
United States Patent (USP), publication number, WO9116719A-31 Oct 1991；Deng, United States Patent (USP), publication number,
US005350644A-27 Sep 1994).The dye-sensitized solar cells of single-junction structure and laminated construction respectively obtains at present
The photoelectric conversion efficiency of 11.18% and 15.09% (Progress In Photovoltaics:Research And
Applications, 2006.V.14.429-442, Applied Physics Letters, 2006.V.88.203103-1-3).
Ca-Ti ore type organic-inorganic composition CH3NH3PbI3And its derivative, there is high molar absorption coefficient and wider spectrum to inhale
Receive range, the conventional dyes being used in substituted dyes sensitization solar battery.
CH at present3NH3PbI3There are mainly of two types for dye-sensitized solar cells：One kind is liquid sensitization solar electricity
Pond, using liquid I-/I3 -Electricity reaches 6.5%, but the corrosion due to iodine electrolyte to perovskite to making electrolyte, peak efficiency,
Therefore stability test is poor, limits the development of such battery.Another kind of is all solid state sensitization solar battery, using hole
Transmission material solves the problems, such as that electrolyte corrodes sensitizer instead of liquid iodophor electrolyte.Hole mobile material have compared with
Low lumo energy, can effectively improve the open-circuit voltage of battery, and common hole mobile material has spiro-MeOTAD, PTAA
Deng such battery highest transfer efficiency has reached 20.1% at present.
Perovskite CH3NH3PbI3And its there are three kinds for the preparation method of derivative：The first is to utilize successive sedimentation method,
I.e. first in TiO2Spin coating PbI on film2Solution, then the film is immersed into CH3NH3In the solution of I, perovskite is ultimately formed；Second
Kind is by two kinds of presoma PbI2(PbBr2Or PbCl2) and CH3NH3I mixed preparings are solution, can be with by solvent drying after spin coating
Obtain perovskite；The third is to steam two kinds of presoma double sources altogether, reacts to form perovskite in film surface.
In battery structure, the crystallization of perovskite and film forming are the key that influence perovskite solar cell properties.Previous
Mostly research is the film-forming process for optimizing perovskite, and the lead source of presoma mostlys come from PbI2And PbCl2, type is relatively simple.
Invention content
The object of the present invention is to provide one kind mixing caesium Ca-Ti ore type solar cell and preparation method thereof.
It is provided by the present invention to mix caesium Ca-Ti ore type solar cell, include successively from bottom to top：Light anode, light-absorption layer,
Hole transmission layer and to electrode.
The light anode is by TiO2Compact film and TiO2Porous membrane layer forms, and the TiO2Porous membrane layer is located at described
TiO2On compact film.
The TiO2The thickness of compact film is 40nm-60nm.
The TiO2The thickness of porous membrane layer is 50-600nm, aperture 5-60nm.
The light-absorption layer is to mix caesium perovskite light-absorption layer.
The thickness of the light-absorption layer is 200-700nm.
The thickness of the hole transmission layer is 80nm-120nm.
Concretely spiro-OMeTAD and pair mixing of trifluoromethanesulfonimide lithiums of the material of the hole transmission layer
Object.
The thickness to electrode is 55nm-65nm.
The material to electrode is concretely golden.
It is above-mentioned to mix in caesium Ca-Ti ore type solar cell, the light anode, hole transmission layer and the preparation method to electrode
It is conventional method, can be prepared according to existing preparation method.
The light-absorption layer is prepared by the method comprising the following steps：
1) by PbI2DMF solution be applied to the TiO2The surface of porous membrane layer, heating remove DMF, to described
TiO2Porous membrane layer surface forms PbI2Film；
2) by CH3NH3I and caesium source are dissolved in organic solvent formation and contain CH3NH3The solution of I and caesium source contain by described in
CH3NH3The solution coating in I and caesium source is to the PbI2The surface of film is reacted under heating condition, in the TiO2It is porous
The surface of film layer, which is formed, mixes caesium perovskite light-absorption layer.
In above method step 1), the PbI2DMF solution a concentration of 200-750mg/mL.
The rotating speed of the coating concretely spin coating, the spin coating is 1000-8000rpm, time 20-90s.
The temperature of the heating is 50-150 degree, time 5-60min.
In above method step 2), the caesium source can be selected from following at least one：CsOAc and CsI.
The organic solvent is the organic solvent that can dissolve the caesium source.
When the caesium source is CsOAc, the organic solvent is isopropanol.
It is described to contain CH3NH3In I and the solution in caesium source, CH3NH3A concentration of 5-40mg/mL of I, caesium source it is a concentration of
0.2-10mg/mL。
It is described to contain CH3NH3The solution coating in I and caesium source is to the PbI2The concrete operations on the surface of film are：By institute
It states containing CH3NH3I and the solution in caesium source are added drop-wise to the PbI2The surface of film, 2000-7000rmp rejection films 30-90s.
In step 2), the condition of the heating is：10-90min is first heated at a temperature of 50-100 DEG C, then in 100-
5-15min is heated at a temperature of 150 DEG C.
The thickness for mixing caesium perovskite light-absorption layer being prepared is 200-700nm.
The present invention by two-step method mix caesium be prepared it is novel mix caesium perovskite, compared with one-step method mixes caesium, in a step
During method mixes caesium, heating can cause Cs ionic catalysis decomposing D MF, generate formamide disruption perovskite structure, device is caused to be imitated
Rate reduces.The present invention mixes caesium using two-step method, first deposits PbI2, after removing DMF, the isopropanol for being coated cesium acetate and MAI is molten
Liquid, under heating condition with PbI2Reacted, avoid occur DMF decompose generate by-product, influence the crystallization of perovskite
And film forming, to obtain higher efficiency.
The all solid state sensitization solar battery using the present invention for mixing caesium perovskite light-absorption layer is in AM1.5,100mW/cm2Light
According under, the short-circuit current density of battery is 15.9mA/cm2, open-circuit voltage 0.91V, fill factor 0.77, opto-electronic conversion effect
Rate is 11.0%.With under same illumination condition caesium perovskite is mixed using what one-step method mixed that caesium is prepared as all solid state of light-absorption layer
Sensitization solar battery is compared, and photoelectric conversion efficiency is significantly improved.
The present invention provides the basic technology methods that perovskite is prepared using novel precursor.Such persursor material and
Preparation method can prepare stable calcium titanium ore bed, effectively perovskite be inhibited to decompose in a heated condition.This method is grasped
Make method simplicity, is easy to control.Such material and method are the research of all solid state Ca-Ti ore type solar cell of high stability
Provide new approaches.In short, the present invention can be obviously improved the stability and photoelectric conversion efficiency of device, and it is of low cost,
It is of great significance for the practical application of all solid state Ca-Ti ore type solar cell.
Description of the drawings
Fig. 1 is the structural schematic diagram for mixing caesium Ca-Ti ore type solar cell of the present invention.
Fig. 2 is that the J-V performances of all solid state sensitization solar battery prepared in comparative example 1, comparative example 2 and embodiment are bent
Line, wherein 1 be in comparative example 1 using undoped with perovskite as the J-V performance curves of all solid state sensitization solar battery of light-absorption layer,
2 be to mix all solid state sensitization solar battery for mixing caesium perovskite as light-absorption layer that caesium is prepared using one-step method in comparative example 2
J-V performance curves, 3 for using the two-step method of the present invention mix that caesium is prepared mix caesium perovskite as all solid state sensitization of light-absorption layer too
The J-V performance curves of positive energy battery.
Fig. 3 is the stability curve of all solid state sensitization solar battery prepared in comparative example 1, comparative example 2 and embodiment.
Specific implementation mode
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
Comparative example 1, using undoped with perovskite as the preparation of all solid state sensitization solar battery of light-absorption layer
1) light anode is prepared
a、TiO2The preparation of compact film
The TiO2Compacted zone is prepared according to the method that following documents provide：Lead Iodide Perovskite
Sensitized All-Solid-State Submicron Thin Film Mesoscopic Solar Cell with
Efficiency Exceeding 9%, H.S.Kim, C.R.Lee, J.H.Im, K.B.Lee, T.Moehl, A.Marchioro,
S.J.Moon,R.Humphry-Baker,J.H.Yum,J.E.Moser,M.Gratzel and N.G.Park,Scientific
Reports,2012,2,591.
The specific steps are：
Titanium dioxide dense film is prepared using spin-coating method, by the precursor solution (1mL isopropyl titanate+0.5mL second of dense film
Hydramine+5mL glycol monoethyl ethers) conductive glass surface is filled, rejection film 30s under the conditions of rotating speed is 3000rpm.After immediately
Film is placed into be preheating on 80 degree of hot plate and heats 30min and is fully hydrolyzed, and at 500 degree, heating 30min, TiO2It is fine and close
The thickness 50nm of film layer；
b、TiO2The preparation of porous membrane layer
The TiO2Porous membrane layer is prepared according to the method that following documents provide：Sequential deposition
as a route to high-performanceperovskite-sensitized solar cells,J.Burschka,
N.Pellet,S.Moon,R.H.Baker,P.Gao,M.K.Nazeeruddin,M.Graetze,Nature2013,499,316.
The specific steps are：
Acid process slurry (18NR-T, Dysol) is using ethyl alcohol according to mass ratio 2：7 dilutions obtain perforated membrane slurry, it will be more
Pore membrane slurry is coated on the film surface that step a is obtained, rotating speed spin coating 30s under the conditions of 6500rpm.After, film is turned
It moves on on hot plate, the thickness of 430 degree of heating 30min, porous membrane layer are 150nm, aperture 10nm；
2) light-absorption layer is prepared
By the presoma PbI of perovskite2It is dissolved in DMF (n,N-Dimethylformamide) according to 463mg/ml concentration, it will
The film surface that the solution coating of 20 μ l is obtained to step b, spin coating rotating speed are 6500rpm, time 90s.After immediately will
Film is transferred to pre- be warming up on 70 degree of hot plate and heats 30min；
The slice, thin piece heated above is cooled to room temperature, by the 10mg/ml CH of 300 μ L3NH3The aqueous isopropanol of I is added dropwise negative
PbI is carried2Film surface, spin coating rotating speed be 3000rpm, time 30s.Obtained brown film is placed on 70 degree of hot plate
After heating 30min, through 110 degree of heat treatment 10min, perovskite light-absorption layer, thickness 450nm are obtained.
3) hole transmission layer is prepared
Perovskite extinction layer surface one layer of hole mobile material of spin coating that step 2) is obtained, when spin coating, are accelerated to using 1s
4000rpm keeps 30s, and thickness is about 100nm.Spin coating carries out in air,
Wherein, the composition of hole mobile material is as follows：spiro-OMeTAD(2,29,7,79-tetrakis(N,N-di-p-
Methoxyphenylamine) -9,99-spirobifluorene) 37.5 μ L of 0.072g, 4- tert .-butylpyridine, double fluoroforms
The 37.5 μ L and chlorobenzene 1mL of acetonitrile solution (520mg/1ml acetonitriles) of sulfimide lithium.
4) it prepares to electrode
Vacuum evaporation gold is carried out on the film that step 3) obtains, steaming golden speed isVacuum degree is 1.0 × 10- 3Pa is hereinafter, gold electrode thickness is 60nm.
By the battery in AM1.5,100mW/cm2The J-V performance curves of battery are tested under illumination with ZAHNER CIMPS,
As shown in 1 in Fig. 2, the short-circuit current density for obtaining battery is 6.09mA/cm2, open-circuit voltage 0.82V, fill factor is
0.64, photoelectric conversion efficiency 3.2%.
Comparative example 2 uses PbI2, MAI and CsI mix caesium preparation as presoma one-step method and mix caesium perovskite light-absorption layer and adopt
Caesium perovskite light-absorption layer, which is mixed, with this prepares all solid state perovskite solar cell
Preparation method and comparative example 1 are essentially identical, the difference is that：The preparation method of light-absorption layer uses one in step 2)
Spin-coating method is walked, i.e.,：By PbI2, MAI and CsI (wherein, PbI is dissolved in DMF2A concentration of 463mg/mL, MAI it is a concentration of
A concentration of 1mg/mL of 10mg/mL, CsI), in the TiO that step b is obtained2PbI is added dropwise in porous membrane surface2, MAI and CsI DMF
200 μ L, 3000rpm rejection films 30s of solution.Obtained brown film is placed on 110 degree of hot plate and heats 30min, obtains mixing caesium calcium
Titanium ore light-absorption layer, thickness 500nm.
By the battery in AM1.5,100mW/cm2The J-V performance curves of battery are tested under illumination with ZAHNER CIMPS,
As shown in 2 in Fig. 2, the short-circuit current density for obtaining battery is 14.6mA/cm2, open-circuit voltage 0.88V, fill factor is
0.74, photoelectric conversion efficiency 9.56%.
Embodiment, two-step method mix caesium preparation and mix caesium perovskite light-absorption layer and mix the preparation of caesium perovskite light-absorption layer entirely admittedly using this
State perovskite solar cell
Preparation method and comparative example 1 are essentially identical, the difference is that：In the PbI prepared2200 μ are added dropwise in film surface
The CH of L3NH3Aqueous isopropanol (the CH of I and CsOAc3NH3A concentration of 1mg/ml of a concentration of 10mg/ml of I, CsOAc),
3000rpm rejection films 30s.Obtained brown film is placed on 70 degree of hot plates after heating 30min, then is heated on 110 degree of hot plate
10min obtains mixing caesium perovskite light-absorption layer, thickness 450nm.
By the battery in AM1.5,100mW/cm2The J-V performance curves of battery are tested under illumination with ZAHNER CIMPS,
As shown in 3 in Fig. 2, the short-circuit current density for obtaining battery is 15.9mA/cm2, open-circuit voltage 0.91V, fill factor is
0.77, photoelectric conversion efficiency 11.0%.
The all solid state sensitization solar battery for mixing caesium perovskite light-absorption layer that two-step method using the present invention mixes caesium preparation exists
AM1.5,100mW/cm2Under illumination, the short-circuit current density of battery is 15.9mA/cm2, open-circuit voltage 0.91V, fill factor
It is 0.77, photoelectric conversion efficiency 11.0%.With the perovskite not mix caesium under same illumination condition as the complete solid of light-absorption layer
State sensitization solar battery (comparative example 1) and caesium perovskite is mixed as all solid state quick of light-absorption layer using what one-step method mixed that caesium is prepared
Change solar cell (comparative example 2) to compare, photoelectric conversion efficiency is significantly improved.
Fig. 3 is the stability curve of all solid state sensitization solar battery prepared in comparative example 1, comparative example 2 and embodiment.
As seen from Figure 3, two-step method through the invention mix caesium preparation mix all solid state quick of caesium perovskite light-absorption layer
Change stability of the stability significantly better than all solid state sensitization solar battery that comparative example 1,2 is prepared of solar cell.
Claims (5)
1. the method for preparing the light-absorption layer for mixing caesium Ca-Ti ore type solar cell, includes the following steps：
1) by PbI2DMF solution be applied to TiO2The surface of porous membrane layer, heating remove DMF, in the TiO2Perforated membrane
Layer surface forms PbI2Film；
2) by CH3NH3I and caesium source are dissolved in organic solvent formation and contain CH3NH3The solution of I and caesium source contain CH by described3NH3I
With the solution coating in caesium source to the PbI2The surface of film, heating reaction, in the TiO2The surface of porous membrane layer is formed
Mix caesium perovskite light-absorption layer；
The caesium source is CsOAc, and the organic solvent is isopropanol.
2. according to the method described in claim 1, it is characterized in that：In step 1), the PbI2DMF solution it is a concentration of
200-750mg/mL；
The coating is spin coating, and the rotating speed of the spin coating is 1000-8000rpm, time 20-90s；
The temperature of the heating is 50-150 degree, time 5-60min.
3. method according to claim 1 or 2, it is characterised in that：It is described to contain CH3NH3In I and the solution in caesium source,
CH3NH3A concentration of 5-40mg/mL of I, a concentration of 0.2-10mg/mL in caesium source.
4. method according to claim 1 or 2, it is characterised in that：It is described to contain CH3NH3The solution coating of I and caesium source
To the PbI2The operation on the surface of film is：Contain CH by described3NH3I and the solution in caesium source are added drop-wise to the PbI2Film
Surface, 2000-7000rmp rejection films 30-90s.
5. one kind mixing caesium Ca-Ti ore type solar cell, it is characterised in that：Light-absorption layer is by any side in claim 1-4
Method is prepared.
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| US9880458B1 (en) * | 2017-04-17 | 2018-01-30 | Hee Solar, L.L.C. | Hybrid perovskite material processing |
| CN111170649A (en) * | 2018-11-09 | 2020-05-19 | 上海交通大学 | Method for preparing cesium-based all-inorganic perovskite material through low-temperature reaction |
| CN109638162B (en) * | 2018-12-14 | 2022-07-05 | 江西理工大学 | High-quality CsPbI2Preparation method of Br inorganic perovskite film |
| CN113106552B (en) * | 2020-01-13 | 2024-01-02 | 吉林大学 | Surface-doped modified perovskite monocrystal, preparation method, application and solar cell |
| CN117242922A (en) * | 2022-03-03 | 2023-12-15 | 宁德时代新能源科技股份有限公司 | Radioactive perovskite, photovoltaic cell containing same and preparation method |
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