CN105870335A - Perovskite solar cell with simple preparation technology and preparation method of perovskite solar cell - Google Patents

Perovskite solar cell with simple preparation technology and preparation method of perovskite solar cell Download PDF

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CN105870335A
CN105870335A CN201610367072.9A CN201610367072A CN105870335A CN 105870335 A CN105870335 A CN 105870335A CN 201610367072 A CN201610367072 A CN 201610367072A CN 105870335 A CN105870335 A CN 105870335A
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solar cell
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perovskite solar
slurry
tio
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CN105870335B (en
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程蓓
范昌烜
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Wuhan University of Technology WUT
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • 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
    • H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

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  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to a perovskite solar cell with a simple preparation technology and a preparation method of the perovskite solar cell. The solar cell is composed of an FTO transparent conductive glass substrate, a TiO2 compact layer, a TiO2 mesoporous layer, a porous Yb2O3 blocking layer and conductive carbon electrodes; CH3NH3PbI3 with a perovskite structure is adopted as a light absorption material and uniformly distributed in the TiO2 mesoporous layer, the porous Yb2O3 blocking layer and the conductive carbon electrodes. According to the perovskite solar cell with the simple preparation technology and the preparation method of the perovskite solar cell, the light absorption material is uniformly distributed between the TiO2 compact layer and the porous Yb2O3 blocking layer through a penetration method, the preparation method is simple, the cell has the good photoelectric conversion efficiency and can be preserved for a long time under the normal temperature condition, and the cell properties are almost not attenuated; above all, due to the fact that no hole transport layer is arranged, the technological process can be simplified, the finished product rate of the cell is significantly increased, and a new thought is provided for large-scale industrialized production in future.

Description

A kind of preparation technology simple perovskite solar cell and preparation method thereof
Technical field
The present invention relates to technical field of solar batteries, be specifically related to a kind of simple perovskite of preparation technology Solar cell and preparation method thereof.
Background technology
Fossil fuel is day by day exhausted and in use causes serious environmental pollution, therefore develops cleaning The energy such as solar cell becomes extremely the most urgent task for maintaining human civilization sustainable development. The industrialization of solar cell is universal needs to overcome two difficult problems: one is to improve photoelectric transformation efficiency, and two are Reduce raw material and process costs.Within 2009, perovskite material is used for light when of solar cell for the first time Photoelectric transformation efficiency only has 3.8%, and the now has had document report efficiency to reach 22%, short several In year, perovskite solar cell one step one step has been over organic solar batteries, dye sensitization The efficiency of solar cell, the monocrystaline silicon solar cell from the most up to 25% is the most within sight.But Along with battery efficiency is constantly bettered a record, we should pay close attention to simultaneously the cost of battery, storage stability, The aspects such as packaging technology, are so just of practical significance to its large-scale industrial production in the future.
In typical solid calcium titanium ore solar cell, its core component is exactly the perovskite of light-absorption layer Material, perovskite material is organic metal three halogenation of the body-centered cubic structure with similar calcium titanate in fact Thing, CH3NH3PbI3It it is most commonly seen one.It is the semiconductor of a kind of direct band gap, forbidden band width Degree is 1.5eV, and when incident light energy is more than 1.5eV, the electronics being in top of valence band is excited, and jumps Adjourning at the bottom of conduction band, stay next hole simultaneously in valence band, such electron-hole pair is claimed Wannier-Mott exciton, different from organic semi-conductor Frenkel exciton.This mode produces photoproduction Electronics can be directly connected to negative electrode by n-type semiconductor, and hole is received by anode by hole mobile material Collection, forms extrinsic current, completes the overall process of photovoltaic effect.Perovskite solar cell typically has two big classes: Mesoporous perovskite solar cell and flat board heterojunction solar battery, every kind has again formal and trans two kinds Version, formal structure be usually electro-conductive glass, negative electrode, electron transfer layer, perovskite light-absorption layer, Hole transmission layer, anode, transconfiguration is usually electro-conductive glass, anode, hole transmission layer, perovskite Light-absorption layer, electron transfer layer, negative electrode.At present it has been reported that the high efficiency perovskite solar cell crossed all It it is to use organic hole transport material (spiro-OMeTAD) and noble metal electrode, although opto-electronic conversion Efficiency is higher, but corresponding preparation cost is the highest, and comprehensive benefit is the most bad.At perovskite solar energy In the preparation technology of battery, generally use right as battery of electron beam evaporation depositing noble metal gold or silver Electrode so that the preparation cost of solar cell is higher, is unfavorable for industrialization large-scale production, Er Qie electricity Son bundle thermal evaporation process condition requires the highest.It addition, the solar cell of preparation at present there is also storage The problem that stability is the best, therefore reduces battery production cost, improves battery efficiency and solve to store surely Qualitative question is the focus of perovskite solar cell research field.
Summary of the invention
The technical problem to be solved is for above-mentioned deficiency present in prior art, it is provided that A kind of novel low-cost perovskite solar cell and preparation method thereof, significantly reduces solar cell Preparation cost, and the photoelectric transformation efficiency of gained solar cell is higher, and storage stability is good.
For solving above-mentioned technical problem, present invention provide the technical scheme that
A kind of preparation technology simple perovskite solar cell is provided, it is characterised in that: the described sun Energy battery is the most successively by FTO transparent conducting glass substrate, TiO2Compacted zone, TiO2Mesoporous layer, Porous Yb2O3Barrier layer and conductive carbon electrode composition, light absorbent is perovskite structure CH3NH3PbI3, the CH of perovskite structure3NH3PbI3It is uniformly distributed in TiO2Mesoporous layer, porous Yb2O3 In barrier layer and conductive carbon electrode.
Preferably, described TiO2Mesoporous layer, porous Yb2O3Barrier layer thickness is respectively 300-800 Nanometer, described conductive carbon electrode thickness is 1-5 micron.
The preparation method of preparation technology of the present invention simple perovskite solar cell, step is as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry, Yb2O3Slurry and C-material slurry；
2) FTO transparent conducting glass substrate surface cleaning being placed in sol evenning machine, surface spin coating causes Close layer solution, obtains TiO at FTO transparent conducting glass substrate surface after the first step sinters2Compacted zone, Then screen process press is utilized to print TiO successively on compacted zone surface2Slurry, Yb2O3Slurry and C-material Slurry, then after second step sinters, put into glove box, from upper end dropping perovskite structure CH3NH3PbI3, every 1cm2Drip this solution of 1-2 microlitre on area, be subsequently heated process and i.e. obtain low Cost perovskite solar cell.
By such scheme, step 1) compound method of described compacted zone solution is: by butyl titanate and Diethanol amine is dissolved in absolute ethyl alcohol, obtains solution 1, wherein volume ratio butyl titanate: diethanol amine: Absolute ethyl alcohol=17:4.5:60；Deionized water and absolute ethyl alcohol 0.9:25 by volume are mixed to get Solution 2；Just solution 1 and solution 2 81.5:25.9 by volume mixes and is sufficiently stirred for, and then seals And obtain compacted zone solution after the most aging 24 hours.
By such scheme, step 1) described TiO2Slurry, Yb2O3Slurry and the system of C-material slurry Preparation Method is: by TiO2Or nanometer Yb2O3Or C-material mixes with terpinol 1:4.5 in mass ratio, Add appropriate absolute ethyl alcohol, use the method for Ultrasonic Pulverization and ball milling to process successively, obtain prefabricated suspended Liquid, adds the ethanol solution of the ethyl cellulose of equal volume in prefabricated suspension, removes after Ultrasonic Pulverization Solvent is gone to obtain TiO2Slurry or Yb2O3Slurry or C-material slurry.
Preferably, described TiO2For nanometer sheet structure, its preparation method is: in butyl titanate Adding mass concentration is the hydrofluoric acid solution of 40%, and butyl titanate and hydrofluoric acid solution volume ratio are 25:3, transfers to after mixing in water heating kettle, in 180 DEG C of Water Under thermal responses 24 hours, centrifugal Remove supernatant liquor, with water and ethanol purge white precipitate 3 times, the most i.e. obtain nanometer sheet structure TiO2。
Preferably, described C-material is obtained by mass mixings such as graphite powder, carbon powder, zirconium dioxides.
By such scheme, step 2) described FTO transparent conducting glass substrate surface cleaning procedure is: By FTO transparent conducting glass substrate surface successively with deionized water, ethanol and acetone ultrasonic cleaning.
By such scheme, step 2) described first step sintering condition is: it is placed in Muffle furnace in 500 DEG C Calcining 30min；Described second step sintering condition is: is placed in Muffle furnace and calcines 1h in 450 DEG C.
By such scheme, step 2) described heating treatment process condition is: it is placed in heating plate in 70 DEG C Stand 3h.
The beneficial effects of the present invention is: at present, prepare perovskite solar cell it is generally required to prepare one Layer nickel oxide etc. improves photoelectric transformation efficiency, compared with prior art, the present invention as hole mobile material Eliminate hole transmission layer, use porous Yb2O3Barrier layer replaces general barrier material, on the one hand fall Low production cost, and because Yb2O3The characteristic of itself, has the biggest specific surface area, pore volume Long-pending very big, therefore, it is possible to store more perovskite material, although lack hole mobile material, but Minimizing due to the number of plies so that the penetrability of sunshine improves, and namely has more luminous energy to shine calcium titanium On ore deposit, thus inspiring more photo-generated carrier, therefore the photoelectric transformation efficiency of final battery is not Reduction is too many, and (short-circuit current density of this perovskite solar cell is 12.22mA/cm2, open-circuit voltage For 0.84V, fill factor, curve factor is 0.55, and photoelectric transformation efficiency is 5.6%), and storage stability is good, Under normal temperature condition, deposit month its structure and performance does not occur significantly to change.The more important thing is, phase Than other battery devices, the technical process of the present invention is more succinct, and the number of plies of battery is less, reduces system The possibility of the appearance human error during Bei, sample can be made to occur, and the probability of substandard products is greatly reduced.
Accompanying drawing explanation
Fig. 1 is the ESEM of the perovskite solar cell cross section prepared by the embodiment of the present invention 1 Picture；
Fig. 2 is the opto-electronic conversion effect of the perovskite solar cell prepared by embodiment 1 and comparative example 1 Rate curve；
Fig. 3 is the monochromatic light photoelectricity of the perovskite solar cell prepared by embodiment 1 and comparative example 1 Conversion efficiency collection of illustrative plates；
Fig. 4 be the perovskite solar cell performance at ambient temperature prepared by embodiment 1 in time The stability test collection of illustrative plates extended；
Fig. 5 is nanometer Yb used in embodiment 12O3Specific surface area and graph of pore diameter distribution.
Detailed description of the invention
For making those skilled in the art be more fully understood that technical scheme, the most right The present invention is described in further detail.
TiO used by the present embodiment2For nanometer sheet structure, its preparation method is: to 25mL metatitanic acid four fourth Adding 3mL mass concentration in ester is the hydrofluoric acid solution of 40%, transfers in water heating kettle after mixing, In 180 DEG C of Water Under thermal responses 24 hours, it is centrifuged off supernatant liquor, by water and ethanol purge white Precipitate 3 times, the most i.e. obtain the TiO of nanometer sheet structure2。
Embodiment 1
A kind of perovskite solar cell of preparation, step is as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry, Yb2O3Slurry and C-material slurry:
The compound method of compacted zone solution is: accurately measure 17mL butyl titanate and 4.5mL diethyl Hydramine, is dissolved in 60mL absolute ethyl alcohol, is sufficiently stirred for, until solution is uniformly clarified, i.e. obtaining solution 1, accurately measure 0.9mL deionized water and 25mL absolute ethyl alcohol is mixed to get solution 2, by solution 1 Mix with solution 2 and be sufficiently stirred for, then seal and obtain compacted zone after the most aging 24 hours Solution, standby；
TiO2Slurry, Yb2O3The preparation method of slurry and C-material slurry is: accurately weigh 4 grams of TiO2 Nanometer sheet or nanometer Yb2O3Or C-material (mass mixing such as graphite powder, carbon powder, zirconium dioxide obtains), Add 18 grams of terpinols and appropriate absolute ethyl alcohol, stir 10 minutes, Ultrasonic Pulverization 50 minutes, repeat Stirring, Ultrasonic Pulverization process three times, be then transferred into ball milling 24 hours in ball grinder, prepares prefabricated molten Liquid, the alcohol suspending liquid adding ethyl cellulose in preformed solution (accurately weighs ethyl cellulose 1.6 Gram, add 16 milliliters of absolute ethyl alcohols dissolve obtain), be sufficiently stirred for, Ultrasonic Pulverization 50 minutes, After transfer to Rotary Evaporators in evaporate solvent, prepare the suitable silk-screen slurry of viscosity；
2) FTO transparent conducting glass is used successively deionized water, ethanol and acetone ultrasonic cleaning, very Empty dry, obtain the electro-conductive glass of clean surface, be subsequently placed in sol evenning machine, surface spin coating compacted zone is molten Liquid, the speed of rotation is set to 2500rpm, spin coating 30s, and each sample spin coating twice, in Muffle furnace TiO is obtained at FTO transparent conducting glass substrate surface after 500 DEG C of sintering 30min2Compacted zone, so After utilize screen process press to print TiO successively on compacted zone surface2Slurry, Yb2O3Slurry and C-material slurry Material, is subsequently placed in Muffle furnace and calcines 1h in 450 DEG C, place in the glove box of full inert gas, Drip the CH of 2 microlitre perovskite structures from carbon film upper end with liquid-transfering gun3NH3PbI3, it is subsequently placed at heating Stand 3h in 70 DEG C on plate, obtain this perovskite solar cell with novel electron barrier layer.
The solar cell prepared by the present embodiment deposits month its structure and photoelectricity under normal temperature condition Performance does not occur significantly to change, and illustrates that its storage stability is good.
It is illustrated in figure 1 the cross-sectional scans Electronic Speculum of perovskite solar cell prepared by the present embodiment Picture, it can be seen that battery is FTO electro-conductive glass substrate, TiO the most respectively2Cause Close layer, TiO2Mesoporous layer, porous Yb2O3Barrier layer and conductive carbon, to electrode (carbon-coating), have substantially Layer structure, TiO2Mesoporous layer, porous Yb2O3Barrier layer thickness is 300-800 nanometer, and carbon-coating is thick Degree is 1-5 micron.
In Shanghai occasion China, INSTRUMENT MODEL is the electrochemical workstation of CHI660C, uses three-electrode structure pair Perovskite solar cell prepared by the present embodiment carries out photoelectric transformation efficiency test.It is illustrated in figure 2 calcium Titanium ore solar cell is tested under standard solar simulator and is obtained photoelectric transformation efficiency curve, records short Road current density is 12.22mA/cm2, open-circuit voltage is 0.84V, and fill factor, curve factor is 0.55, and photoelectricity turns Changing efficiency is 5.6%.
It is illustrated in figure 3 the monochromatic light opto-electronic conversion effect of perovskite solar cell prepared by the present embodiment Rate.Test be U.S. Newport (Newport) be equipped with monochromator monochromatic light conversion quantum efficiency test system Draw on system (QE/IPCE).It can be seen that this battery has higher photoelectric conversion capacity.
Fig. 4 is that Sample Cell carried out photoelectricity at interval of 72 hours under AM 1.5G simulated solar irradiation and turns Changing the test of efficiency, because there being the protection of thicker carbon-coating, the photoelectric transformation efficiency of battery can be longer Time in maintain higher level, in front ten days preserved, battery efficiency occurs in that a certain degree of ripple Dynamic, this is the result of the further crystallization of perovskite, this shows compared to other batteries, the present invention Can effectively solve a difficult problem for not shelf-stable after cell package.
Fig. 5 is nanometer Yb used by the present embodiment2O3Nitrogen adsorption-desorption isotherm and corresponding hole Footpath distribution map, it is seen that nanometer Yb2O3The thermoisopleth of particle is IV type, has obvious delayed winding, Surface sample exists mesoporous (2-50nm).Nitrogen adsorption-detachment assays has drawn the BET of sample (Brunauer-Emmett-Teller) specific surface area (SBET), wherein the specific surface area of ytterbium oxide reaches 891m2/ g, this explanation ytterbium oxide nano particle has a biggest specific surface area, thus ytterbium oxide particle Aperture volume that middle existence is bigger and the surface area of exposure.Obviously, bigger specific surface area can carry more The perovskite of volume, this is advantageous for the absorption of perovskite, thus is conducive to increasing perovskite solar-electricity The pond utilization rate to luminous energy.
Comparative example 1
Preparation contrast perovskite solar cell sample, step is as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry and C-material slurry:
The compound method of compacted zone solution is: accurately measure 17mL butyl titanate and 4.5mL diethyl Hydramine, is dissolved in 60mL absolute ethyl alcohol, is sufficiently stirred for, until solution is uniformly clarified, i.e. obtaining solution 1, accurately measure 0.9mL deionized water and 25mL absolute ethyl alcohol is mixed to get solution 2, by solution 1 Mix with solution 2 and be sufficiently stirred for, then seal and obtain compacted zone after the most aging 24 hours Solution, standby；
TiO2The preparation method of slurry and C-material slurry is: accurately weigh TiO2Or C-material 4 grams, Add 18 grams of terpinols and appropriate absolute ethyl alcohol, stir 10 minutes, Ultrasonic Pulverization 50 minutes, repeat Stirring, Ultrasonic Pulverization process three times, be then transferred into ball milling 24 hours in ball grinder, prepares prefabricated molten Liquid, to paying the ethanol solution adding ethyl cellulose in solution in advance, is sufficiently stirred for, Ultrasonic Pulverization 50 points Clock, evaporates solvent in being finally transferred to Rotary Evaporators, prepares silk-screen slurry；
2) FTO transparent conducting glass is used successively deionized water, ethanol and acetone ultrasonic cleaning, very Empty dry, obtain the electro-conductive glass of clean surface, be subsequently placed in sol evenning machine, surface spin coating compacted zone is molten Liquid, the speed of rotation is set to 2500rpm, spin coating 30s, and each sample spin coating twice, in Muffle furnace TiO is obtained at FTO transparent conducting glass substrate surface after 500 DEG C of sintering 30min2Compacted zone, so After utilize screen process press to print TiO successively on compacted zone surface2Slurry and C-material slurry, then put In Muffle furnace in 450 DEG C calcine 1h, place in the glove box of full inert gas, with liquid-transfering gun from The CH of carbon film upper end dropping 1-2 microlitre perovskite structure3NH3PbI3, it is subsequently placed in heating plate in 70 DEG C Stand 3h, obtain contrasting perovskite solar cell sample.
Using and test the battery of example gained with the identical method of example 1, its photoelectricity turns Changing efficiency curve as shown in Fig. 2 curve, IPCE collection of illustrative plates is as graphically shown in fig. 3.The photoelectricity of its battery turns Transducing power, efficiency are all weak than the sample in embodiment 1.

Claims (9)

1. a preparation technology simple perovskite solar cell, it is characterised in that: described solar energy Battery is the most successively by FTO transparent conducting glass substrate, TiO2Compacted zone, TiO2Mesoporous layer, Porous Yb2O3Barrier layer and conductive carbon electrode composition, light absorbent is perovskite structure CH3NH3PbI3, the CH of perovskite structure3NH3PbI3It is uniformly distributed in TiO2Mesoporous layer, porous Yb2O3 In barrier layer and conductive carbon electrode.
Perovskite solar cell the most according to claim 1, it is characterised in that: described TiO2 Mesoporous layer, porous Yb2O3Barrier layer thickness is respectively 300-800 nanometer, described conductive carbon electrode thickness For 1-5 micron.
3. a preparation method for perovskite solar cell according to claim 1 and 2, its It is characterised by that step is as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry, Yb2O3Slurry and C-material slurry；
2) FTO transparent conducting glass substrate surface cleaning being placed in sol evenning machine, surface spin coating causes Close layer solution, obtains TiO at FTO transparent conducting glass substrate surface after the first step sinters2Compacted zone, Then screen process press is utilized to print TiO successively on compacted zone surface2Slurry, Yb2O3Slurry and C-material Slurry, then after second step sinters, put into glove box, from upper end dropping perovskite structure CH3NH3PbI3, every 1cm2Drip this solution of 1-2 microlitre on area, be subsequently heated process and i.e. obtain low Cost perovskite solar cell.
The preparation method of perovskite solar cell the most according to claim 3, it is characterised in that Step 1) compound method of described compacted zone solution is: butyl titanate and diethanol amine is dissolved in anhydrous In ethanol, obtain solution 1；Deionized water and absolute ethyl alcohol are mixed to get solution 2；Just solution 1 Mix in specific proportions with solution 2 and be sufficiently stirred for, then sealing and after the most aging 24 hours Obtain compacted zone solution.
The preparation method of calcium ore deposit the most according to claim 3 solar cell, it is characterised in that Step 1) described TiO2Slurry, Yb2O3The preparation method of slurry and C-material slurry is: by TiO2 Nanometer sheet or nanometer Yb2O3Or C-material mixes with terpinol 1:4.5 in mass ratio, add anhydrous Ethanol, uses the method for Ultrasonic Pulverization and ball milling to process successively, obtains prefabricated suspension, to prefabricated suspended Liquid adds the ethanol solution of the ethyl cellulose of equal volume, removes solvent after Ultrasonic Pulverization and obtain TiO2 Slurry or Yb2O3Slurry or C-material slurry.
The preparation method of perovskite solar cell the most according to claim 5, it is characterised in that Described C-material is obtained by mass mixings such as graphite powder, carbon powder, zirconium dioxides.
The preparation method of perovskite solar cell the most according to claim 3, it is characterised in that Step 2) described FTO transparent conducting glass substrate surface cleaning procedure is: by FTO electrically conducting transparent glass Glass substrate surface is successively with deionized water, ethanol and acetone ultrasonic cleaning.
The preparation method of perovskite solar cell the most according to claim 3, it is characterised in that Step 2) described first step sintering condition is: it is placed in Muffle furnace and calcines 30min in 500 DEG C；Described Two-step sintering condition is: is placed in Muffle furnace and calcines 1h in 450 DEG C.
The preparation method of perovskite solar cell the most according to claim 3, it is characterised in that Step 2) described heating treatment process condition is: it is placed in heating plate and stands 3h in 70 DEG C.
CN201610367072.9A 2016-05-27 2016-05-27 A kind of simple perovskite solar battery of preparation process and preparation method thereof Expired - Fee Related CN105870335B (en)

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