CN105870335B - A kind of simple perovskite solar battery of preparation process and preparation method thereof - Google Patents
A kind of simple perovskite solar battery of preparation process and preparation method thereof Download PDFInfo
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- 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
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Abstract
The present invention relates to simple perovskite solar batteries of a kind of preparation process and preparation method thereof, and the solar battery is by FTO transparent conducting glass substrate, TiO2Compacted zone, TiO2Mesoporous layer, porous Yb2O3Barrier layer and conductive carbon electrode composition, light absorbent are the CH with perovskite structure3NH3PbI3, the CH of perovskite structure3NH3PbI3It is uniformly distributed in TiO2Mesoporous layer, porous Yb2O3In barrier layer and conductive carbon electrode.Light absorbent is uniformly distributed in TiO using osmosis by the present invention2Mesoporous layer and porous Yb2O3Between barrier layer, preparation method is simple, battery has good photoelectric conversion efficiency, and it is almost unattenuated to save under normal temperature conditions some time battery performance, more importantly due to there is no hole transmission layer, it can simplify technical process, greatly improve the yield rate of battery, provide a kind of new approaches for later large-scale industrial production.
Description
Technical field
The present invention relates to technical field of solar batteries, and in particular to a kind of simple perovskite solar-electricity of preparation process
Pond and preparation method thereof.
Background technique
Fossil fuel is increasingly exhausted and causes serious environmental pollution in use, therefore develops clean energy resource as too
Positive energy battery is used to that human civilization sustainable development to be maintained to become current extremely urgent task.The industrialization of solar battery is general
And need to overcome two problems: first is that photoelectric conversion efficiency is improved, second is that reducing raw material and process costs.Perovskite material in 2009
Photoelectric conversion efficiency only has 3.8% when material is used for solar battery for the first time, and now has had document report efficiency
22% is had reached, in a few years, one step of perovskite solar battery, one step has been over organic solar batteries, dye
The efficiency for expecting sensitization solar battery, the monocrystaline silicon solar cell from present up to 25% is also within sight.But with electricity
Pond efficiency is constantly bettered a record, we should pay close attention to cost, storage stability, packaging technology of battery etc. simultaneously, in this way
It is just of practical significance to its large-scale industrial production in the future.
In typical solid perovskite solar battery, core component is exactly the perovskite material of light-absorption layer, calcium titanium
Pit wood material is the organic metal trihalid of the body-centered cubic structure with similar calcium titanate, CH in fact3NH3PbI3It is the most often
The one kind seen.It is a kind of semiconductor of direct band gap, and forbidden bandwidth 1.5eV locates when incident laser energy is greater than 1.5eV
It is excited, is transitted on conduction band bottom in the electronics of top of valence band, while leaving a hole in valence band, such electronics-sky
Cave to by claim Wannier-Mott exciton, it is different from organic semi-conductor Frenkel exciton.This mode generates light induced electron can
To be directly connected to cathode by n-type semiconductor, hole is collected by hole mobile material by anode, forms extrinsic current, is completed
The overall process of photovoltaic effect.Perovskite solar battery generally has two major classes: mesoporous perovskite solar battery and plate are heterogeneous
Joint solar cell, every kind has formal and trans- two kinds of structure type again, and formal structure is usually electro-conductive glass, cathode, electronics
Transport layer, perovskite light-absorption layer, hole transmission layer, anode, transconfiguration are usually electro-conductive glass, anode, hole transmission layer, calcium
Titanium ore light-absorption layer, electron transfer layer, cathode.At present it has been reported that the high efficiency perovskite solar battery crossed all is using organic
Hole mobile material (spiro-OMeTAD) and noble metal electrode are prepared into accordingly although photoelectric conversion efficiency is higher
This is also higher, and comprehensive benefit is simultaneously bad.In the preparation process of perovskite solar battery, it is heavy to generally use electron beam evaporation
Noble metal gold or silver are accumulated as battery to electrode, so that the preparation cost of solar battery is higher, is unfavorable for industrializing big rule
Mould production, and the requirement of electron beam evaporation process conditions is very high.In addition, there is also storages for the solar battery prepared at present
The bad problem of stability, therefore reducing battery production cost, improving battery efficiency and solve problems of stability in storage is calcium
The hot spot of titanium ore solar battery research field.
Summary of the invention
It is a kind of novel low the technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide
Cost perovskite solar battery and preparation method thereof significantly reduces the preparation cost of solar battery, and the gained sun
The photoelectric conversion efficiency of energy battery is higher, and storage stability is good.
In order to solve the above technical problems, present invention provide the technical scheme that
There is provided a kind of simple perovskite solar battery of preparation process, it is characterised in that: the solar battery is under
It is supreme successively by FTO transparent conducting glass substrate, TiO2Compacted zone, TiO2Mesoporous layer, porous Yb2O3Barrier layer and conductive carbon electricity
Pole composition, light absorbent are the CH of perovskite structure3NH3PbI3, the CH of perovskite structure3NH3PbI3It is uniformly distributed in TiO2It is situated between
Aperture layer, porous Yb2O3In barrier layer and conductive carbon electrode.
Preferably, the TiO2Mesoporous layer, porous Yb2O3Barrier layer thickness is respectively 300-800 nanometers, the conduction
Carbon electrode is with a thickness of 1-5 microns.
The preparation method of the simple perovskite solar battery of preparation process of the present invention, steps are as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry, Yb2O3Slurry and C-material slurry；
2) cleaning of FTO transparent conducting glass substrate surface is placed in sol evenning machine, surface spin coating compacted zone solution, through the
TiO is obtained in FTO transparent conducting glass substrate surface after the sintering of one step2Then compacted zone utilizes screen printing in fine and close layer surface
Brush machine successively prints TiO2Slurry, Yb2O3Slurry and C-material slurry, then it is put into glove box after second step is sintered, it is dripped from upper end
Add the CH of perovskite structure3NH3PbI3, every 1cm2On area be added dropwise the 1-2 microlitres of solution, then heat treatment i.e. obtain it is low at
This perovskite solar battery.
According to the above scheme, the preparation method of step 1) the compacted zone solution are as follows: butyl titanate and diethanol amine is molten
In dehydrated alcohol, solution 1 is obtained, wherein volume ratio butyl titanate: diethanol amine: dehydrated alcohol=17:4.5:60；It will go
0.9:25 is mixed to get solution 2 by volume for ionized water and dehydrated alcohol；It will be by solution 1 and solution 2 81.5:25.9 by volume
It mixes and is sufficiently stirred, then seal and aging obtains compacted zone solution at room temperature after 24 hours.
According to the above scheme, the step 1) TiO2Slurry, Yb2O3Slurry and C-material slurry the preparation method comprises the following steps: by TiO2
Or nanometer Yb2O3Or C-material is mixed with terpinol 1:4.5 in mass ratio, adds appropriate dehydrated alcohol, successively using ultrasonic powder
Broken and ball milling method is handled, and obtains prefabricated suspension, and the second of the ethyl cellulose of equal volume is added into prefabricated suspension
Alcoholic solution removes solvent after Ultrasonic Pulverization and obtains TiO2Slurry or Yb2O3Slurry or C-material slurry.
Preferably, the TiO2For nanometer chip architecture, preparation method are as follows: mass concentration is added into butyl titanate
For 40% hydrofluoric acid solution, butyl titanate and hydrofluoric acid solution volume ratio are 25:3, are transferred to water heating kettle after mixing
In, hydro-thermal reaction 24 hours, are centrifuged off supernatant liquor under the conditions of 180 DEG C, are cleaned white precipitate 3 times with water and ethyl alcohol, do
The TiO of nanometer sheet structure is obtained after dry2。
Preferably, the C-material is obtained by mass mixings such as graphite powder, carbon black powder, zirconium dioxides.
According to the above scheme, step 2) the FTO transparent conducting glass substrate surface cleaning procedure are as follows: by FTO electrically conducting transparent
Glass basic surface successively uses deionized water, ethyl alcohol and acetone ultrasonic cleaning.
According to the above scheme, the step 2) first step sintering condition are as follows: be placed in Muffle furnace in 500 DEG C of calcining 30min；Institute
State second step sintering condition are as follows: be placed in Muffle furnace in 450 DEG C of calcining 1h.
According to the above scheme, the step 2) heating treatment process condition are as follows: be placed in heating plate in 70 DEG C of standing 3h.
The beneficial effects of the present invention are: currently, preparing perovskite solar battery generally requires one layer of nickel oxide of preparation
Photoelectric conversion efficiency is improved Deng as hole mobile material, compared with prior art, present invention omits hole transmission layers, use
Porous Yb2O3Barrier layer replaces general barrier material, on the one hand reduces production cost, and because Yb2O3The spy of itself
Property, there is very big specific surface area, pore volume is very big, therefore can store more perovskite materials, although lacking sky
Hole transport materials, but due to the reduction of the number of plies, so that the penetrability of sunlight improves, that is, there are more luminous energy to shine calcium
On titanium ore, to inspire more photo-generated carriers, therefore there is no reduce too many (be somebody's turn to do for the photoelectric conversion efficiency of final battery
The short-circuit current density of perovskite solar battery is 12.22mA/cm2, open-circuit voltage 0.84V, fill factor 0.55, light
Photoelectric transformation efficiency is that 5.6%), and storage stability is good, stores month its structure under normal temperature conditions and performance is not sent out
Raw apparent change.Importantly, comparing other battery devices, technical process of the invention is more succinct, the number of plies of battery
Less, a possibility that reducing the appearance human error in preparation process, the probability that sample can be made substandard products occur is greatly reduced.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of perovskite solar battery cross section prepared by the embodiment of the present invention 1；
Fig. 2 is the photoelectric conversion efficiency curve of perovskite solar battery prepared by embodiment 1；
Fig. 3 is the monochromatic light ray photoelectric transformation efficiency figure of perovskite solar battery prepared by embodiment 1 and comparative example 1
Spectrum；
Fig. 4 is the performance extended stabilization at any time at room temperature of perovskite solar battery prepared by embodiment 1
Property test map；
Fig. 5 is nanometer Yb used in embodiment 12O3Specific surface area and graph of pore diameter distribution.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing to the present invention make into
One step detailed description.
TiO used in the present embodiment2For nanometer chip architecture, preparation method are as follows: 3mL matter is added into 25mL butyl titanate
The hydrofluoric acid solution that concentration is 40% is measured, is transferred in water heating kettle after mixing, hydro-thermal reaction 24 is small under the conditions of 180 DEG C
When, it is centrifuged off supernatant liquor, is cleaned white precipitate 3 times with water and ethyl alcohol, obtains the TiO of nanometer sheet structure after dry2。
Embodiment 1
A kind of perovskite solar battery is prepared, steps are as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry, Yb2O3Slurry and C-material slurry:
The preparation method of compacted zone solution are as follows: it is accurate to measure 17mL butyl titanate and 4.5mL diethanol amine, it is dissolved in
In 60mL dehydrated alcohol, be sufficiently stirred until solution is uniformly clarified to get to solution 1, it is accurate measure 0.9mL deionized water and
25mL dehydrated alcohol is mixed to get solution 2, and solution 1 and solution 2 are mixed and is sufficiently stirred, then sealing and aging at room temperature
Compacted zone solution is obtained after 24 hours, it is spare；
TiO2Slurry, Yb2O3Slurry and C-material slurry the preparation method comprises the following steps: accurately weighing 4 grams of TiO2Nanometer sheet or nanometer
Yb2O3Or C-material (mass mixings such as graphite powder, carbon black powder, zirconium dioxide obtain), 18 grams of terpinols and appropriate anhydrous second are added
Alcohol stirs 10 minutes, Ultrasonic Pulverization 50 minutes, repeats stirring, Ultrasonic Pulverization process three times, be then transferred into ball milling in ball grinder
24 hours, preformed solution is made, the alcohol suspending liquid that ethyl cellulose is added into preformed solution (accurately weighs ethyl cellulose
1.6 grams, be added in 16 milliliters of dehydrated alcohols to dissolve obtain), be sufficiently stirred, Ultrasonic Pulverization 50 minutes, be finally transferred to rotation steam
Solvent is evaporated in hair instrument, the suitable silk-screen slurry of viscosity is made；
2) deionized water, ethyl alcohol and acetone is successively used to be cleaned by ultrasonic FTO transparent conducting glass, vacuum drying obtains table
The electro-conductive glass of face cleaning, is subsequently placed in sol evenning machine, and surface spin coating compacted zone solution, the speed of rotation is set as 2500rpm, rotation
Apply 30s, each sample spin coating twice, in FTO transparent conducting glass substrate surface after 500 DEG C of sintering 30min in Muffle furnace
Obtain TiO2Then compacted zone successively prints TiO using screen process press in fine and close layer surface2Slurry, Yb2O3Slurry and C-material
Slurry is subsequently placed in Muffle furnace in 450 DEG C of calcining 1h, places into the glove box full of inert gas, with liquid-transfering gun from carbon
The CH of 2 microlitres of perovskite structures is added dropwise in film upper end3NH3PbI3, it is subsequently placed in heating plate in 70 DEG C of standing 3h, obtains this tool
There is the perovskite solar battery on novel electron barrier layer.
Solar battery manufactured in the present embodiment is stored into month its structure under normal temperature conditions and photoelectric properties are not sent out
Raw apparent change, illustrates that its storage stability is good.
It is as shown in Figure 1 the cross-sectional scans electron microscopic picture of perovskite solar battery prepared by the present embodiment, from figure
In as can be seen that battery be FTO electro-conductive glass substrate, TiO respectively from bottom to up2Compacted zone, TiO2Mesoporous layer, porous Yb2O3Resistance
Barrier and conductive carbon have apparent layer structure, TiO to electrode (carbon-coating)2Mesoporous layer, porous Yb2O3Barrier layer thickness is
300-800 nanometers, carbon layers having thicknesses are 1-5 microns.
In the electrochemical workstation that Shanghai Chen Hua instrument model is CHI660C, using three-electrode structure to the present embodiment system
Standby perovskite solar battery carries out photoelectric conversion efficiency test.Be illustrated in figure 2 perovskite solar battery standard too
Test obtains photoelectric conversion efficiency curve under sunlight simulator, and measuring short-circuit current density is 12.22mA/cm2, open-circuit voltage is
0.84V, fill factor 0.55, photoelectric conversion efficiency 5.6%.
It is illustrated in figure 3 the monochromatic light ray photoelectric transformation efficiency of perovskite solar battery manufactured in the present embodiment.Test is
It is obtained in the monochromatic light conversion quantum efficiency test macro (QE/IPCE) that U.S. Newport (Newport) is equipped with monochromator.From
As can be seen that battery photoelectric conversion capacity with higher in figure.
Fig. 4 is the survey that Sample Cell carries out photoelectric conversion efficiency at interval of 72 hours under AM 1.5G simulated solar irradiation
Examination, because there is the protection of thicker carbon-coating, the photoelectric conversion efficiency of battery can maintain higher level in a longer period of time,
There is a degree of fluctuation in battery efficiency in preceding ten days of preservation, this is the further crystallization of perovskite as a result, thus
It can be seen that compared to other batteries, the present invention can effectively solve after cell package the not problem of shelf-stable.
Fig. 5 is nanometer Yb used in the present embodiment2O3Nitrogen adsorption-desorption isotherm and corresponding graph of pore diameter distribution, can
See a nanometer Yb2O3The thermoisopleth of particle is IV type, has and significantly lags winding, and there are mesoporous (2-50nm) in surface sample.Nitrogen
Aspiration is attached-and detachment assays have obtained BET (Brunauer-Emmett-Teller) specific surface area (S of sampleBET), wherein aoxidizing
The specific surface area of ytterbium reaches 891m2/ g, this illustrates that ytterbium oxide nano particle has very big specific surface area, thus ytterbium oxide
There is the surface area of bigger aperture volume and exposure in grain.Obviously, bigger specific surface area can carry further amounts of calcium titanium
Mine, this is advantageous for the absorption of perovskite, to be conducive to increase perovskite solar battery to the utilization rate of luminous energy.
Comparative example 1
Preparation comparison perovskite solar cell sample, steps are as follows:
1) compacted zone solution and TiO are prepared respectively2Slurry and C-material slurry:
The preparation method of compacted zone solution are as follows: it is accurate to measure 17mL butyl titanate and 4.5mL diethanol amine, it is dissolved in
In 60mL dehydrated alcohol, be sufficiently stirred until solution is uniformly clarified to get to solution 1, it is accurate measure 0.9mL deionized water and
25mL dehydrated alcohol is mixed to get solution 2, and solution 1 and solution 2 are mixed and is sufficiently stirred, then sealing and aging at room temperature
Compacted zone solution is obtained after 24 hours, it is spare；
TiO2Slurry and C-material slurry the preparation method comprises the following steps: accurately weighing TiO2Or 4 grams of C-material, 18 grams of terpinols are added
With appropriate dehydrated alcohol, stirs 10 minutes, Ultrasonic Pulverization 50 minutes, repeat stirring, Ultrasonic Pulverization process three times, be then transferred into
Preformed solution is made in ball milling 24 hours in ball grinder, to the ethanol solution that ethyl cellulose is added in solution is paid in advance, sufficiently stirs
It mixes, Ultrasonic Pulverization 50 minutes, is finally transferred to evaporate solvent in Rotary Evaporators, silk-screen slurry is made；
2) deionized water, ethyl alcohol and acetone is successively used to be cleaned by ultrasonic FTO transparent conducting glass, vacuum drying obtains table
The electro-conductive glass of face cleaning, is subsequently placed in sol evenning machine, and surface spin coating compacted zone solution, the speed of rotation is set as 2500rpm, rotation
Apply 30s, each sample spin coating twice, in FTO transparent conducting glass substrate surface after 500 DEG C of sintering 30min in Muffle furnace
Obtain TiO2Then compacted zone successively prints TiO using screen process press in fine and close layer surface2Slurry and C-material slurry, then
It is placed in Muffle furnace in 450 DEG C of calcining 1h, places into the glove box full of inert gas, be added dropwise with liquid-transfering gun from carbon film upper end
The CH of 1-2 microlitres of perovskite structure3NH3PbI3, it is subsequently placed in heating plate in 70 DEG C of standing 3h, obtains the comparison perovskite sun
It can battery sample.
The resulting battery of example is tested using same example 1 identical method, IPCE map such as Fig. 3 curve
It is shown.The photoelectric conversion capacity of its battery, efficiency are all weaker than the sample in embodiment 1.
Claims (9)
1. a kind of simple perovskite solar battery of preparation process, it is characterised in that: the solar battery from bottom to up according to
It is secondary by FTO transparent conducting glass substrate, TiO2Compacted zone, TiO2Mesoporous layer, porous Yb2O3Barrier layer and conductive carbon electrode composition,
Light absorbent is the CH of perovskite structure3NH3PbI3, the CH of perovskite structure3NH3PbI3It is uniformly distributed in TiO2It is mesoporous layer, more
Hole Yb2O3In barrier layer and conductive carbon electrode.
2. perovskite solar battery according to claim 1, it is characterised in that: the TiO2Mesoporous layer, porous Yb2O3
Barrier layer thickness is respectively 300-800 nanometers, and the conductive carbon electrode is with a thickness of 1-5 microns.
3. a kind of preparation method of perovskite solar battery according to claim 1 or 2, it is characterised in that step is such as
Under:
1) compacted zone solution and TiO are prepared respectively2Slurry, Yb2O3Slurry and C-material slurry；
2) cleaning of FTO transparent conducting glass substrate surface is placed in sol evenning machine, surface spin coating compacted zone solution, through the first step
TiO is obtained in FTO transparent conducting glass substrate surface after sintering2Then compacted zone utilizes screen process press in fine and close layer surface
Successively print TiO2Slurry, Yb2O3Slurry and C-material slurry, then it is put into glove box after second step is sintered, calcium is added dropwise from upper end
The CH of perovskite like structure3NH3PbI3, every 1cm2The CH of 1-2 microlitres of perovskite structure is added dropwise on area3NH3PbI3, then heat
Obtain inexpensive perovskite solar battery.
4. the preparation method of perovskite solar battery according to claim 3, which is characterized in that the step 1) densification
The preparation method of layer solution are as follows: butyl titanate and diethanol amine are dissolved in dehydrated alcohol, obtain solution 1；By deionized water
Solution 2 is mixed to get with dehydrated alcohol；Solution 1 and solution 2 are mixed and are sufficiently stirred in specific proportions, is then sealed and in room
Compacted zone solution is obtained after temperature is aging 24 hours lower.
5. the preparation method of perovskite solar battery according to claim 3, which is characterized in that the step 1) TiO2
Slurry, Yb2O3Slurry and C-material slurry the preparation method comprises the following steps: by TiO2Nanometer sheet or nanometer Yb2O3Or C-material is pressed with terpinol
Mass ratio 1:4.5 mixing, adds dehydrated alcohol, successively using Ultrasonic Pulverization and the processing of the method for ball milling, obtains prefabricated suspended
The ethanol solution of the ethyl cellulose of equal volume is added into prefabricated suspension, removes solvent after Ultrasonic Pulverization and obtains for liquid
TiO2Slurry or Yb2O3Slurry or C-material slurry.
6. the preparation method of perovskite solar battery according to claim 5, which is characterized in that the C-material is by stone
The mass mixings such as ink powder, carbon black powder, zirconium dioxide obtain.
7. the preparation method of perovskite solar battery according to claim 3, which is characterized in that the step 2) FTO
Transparent conducting glass substrate surface cleaning procedure are as follows: by FTO transparent conducting glass substrate surface successively use deionized water, ethyl alcohol and
Acetone ultrasonic cleaning.
8. the preparation method of perovskite solar battery according to claim 3, which is characterized in that step 2) described first
Walk sintering condition are as follows: be placed in Muffle furnace in 500 DEG C of calcining 30min；The second step sintering condition are as follows: be placed in Muffle furnace in
450 DEG C of calcining 1h.
9. the preparation method of perovskite solar battery according to claim 3, which is characterized in that the step 2) heating
Treatment process condition are as follows: be placed in heating plate in 70 DEG C of standing 3h.
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