CN106486602A - A kind of method that introducing cheap additives prepare high-quality perovskite thin film - Google Patents
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Abstract
The present invention is a kind of to introduce the method that cheap additives prepare high-quality perovskite thin film.This high-quality perovskite material introduces ammonium salt additive in preparation process；Described additive can be incorporated in perovskite precursor solution or in anti-solvent；This kind of perovskite material structural formula is AMX3, wherein A is organic cation, CH3NH3、NH2CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One of or two kinds of mixture, M is Pb2 +Or Sn2 +One of or two kinds of mixture, X is Cl‑, Br‑, I‑Or SCN‑One or more of mixture.The introducing of ammonium salt is reduced thin film internal flaw and decreases surface state by the method, there is provided new prepares approach.Process is simple, with low cost, repeatability is high, and the optics electric property being favorably improved perovskite thin film has a good application prospect.
Description
Technical field
The invention belongs to nano-functional material photovoltaic solar Material Field, it is related to the preparation of high-quality perovskite material, especially
It is a kind of method that introducing cheap additives prepare high-quality perovskite thin film.
Background technology
Human social development still depends on fossil energy so far.But fossil energy distributed pole on earth
Unbalanced, reserves are limited, and fossil energy has been difficult to meet human wants.In addition the combusts fossil energy brings huge environment
Pollution, haze weather and greenhouse effect, the serious sustainable development threatening human society of these negative effects.Solaode energy
Enough it is converted into electric energy using solar energy, can be that human social development provides inexhaustible clean energy resource,
It is human society reply energy crisis, seek the important countermeasure of sustainable development.
At present solaode material therefor mainly has a silica-base material, GaAs material, indium phosphide/InGaP material,
CIGS material, telluride cadmium material, perovskite material, copper-zinc-tin-sulfur material, molecular dye used in dye-sensitized cell,
Vulcanized lead quantum dot or organic material etc..In numerous photovoltaic materials, silicon, GaAs, cadmium telluride and perovskite material preparation
Photovoltaic Device Performance reached 20%, have huge researching value ([1] Polman A, Knight M, Garnett E C,
et al.Science,2016,352:4424.)., according to the selection of different halogens, band gap is in 1.6eV to 3.2eV for perovskite material
Scope is adjustable, has larger specific absorbance, long carrier lifetime, high charge mobility, long migration distance and extremely low defect state
The excellent photoelectric properties such as density ([2] Si H, Liao Q, Zhang Z, et al.Nano Energy, 2016,22:223-
231).Additionally, perovskite material preparation process is simple, perovskite material can be prepared by cheap solwution method.With perovskite
The continuous improvement of quality of materials, Photovoltaic Device Performance achieves important breakthrough ([3] Lee M M, Teuscher J, Miyasaka
T,et al.Science,2012,338:643–647.[4]Burschka J,Pellet N,Moon S J,et
al.Nature,2013,499:316–319.[5]Liu M,Johnston M B,Snaith H J.Nature,2013,501:
395–398.[6]Bi D,Yi C,Luo J,et al.Nat.Energy,2016,1,doi:10.1038/
nenergy.2016.142.).
Perovskite material is with low cost, has huge application potential.Prepare the multiformity of environment yet with solwution method
Have impact on the quality of prepared material, constrain the application further of material, the stability of heavy damage device, limit calcium titanium
The development of ore deposit battery.
Content of the invention
In order to solve the above problems, it is an object of the invention to provide a kind of method preparing high-quality perovskite material, fall
Low material crystals defect, reduces surface state, reduces cost of manufacture as far as possible, for carrying while improving core material crystal property
High Photovoltaic Device Performance provides high-quality perovskite material.
The technical scheme is that：A kind of method that introducing cheap additives prepare high-quality perovskite thin film, the party
Method introduces ammonium salt additive in high-quality perovskite material in preparation process；Described additive can be incorporated into perovskite presoma
In solution or in anti-solvent；Described high-quality perovskite material structural formula is AMX3, wherein A is organic cation, described machine sun
Ion CH3NH3、NH2- CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One of or two kinds of mixture, M
For bivalent metal ion Pb2 +Or Sn2 +One of or two kinds of mixture, X is monovalence halide ion Cl-, Br-, I-Or SCN-In
One or more of mixture.
Further, the method step is as follows：
Step 1：Substrate is washed by substrate cleaning, nitrogen dries up standby；
Step 2：Substrate after step 1 is processed is processed through oxygen plasma etch, 10-40min；
Step 3：By a certain proportion of AX and MX2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtain
To joining perovskite precursor solution；
Step 4：Ammonium salt additive is added through step 3 in perovskite precursor solution after processing；
Step 5：It is spun to the substrate after step 2 is processed using precursor solution one step after step 4 is processed
On, spin coating rotating speed is 100-5000rpm, is operated under the conditions of humidity is less than 30%；
Step 6：Perovskite material will make annealing treatment after step 5 is processed, annealing temperature is 80-150 DEG C, low in humidity
Operated under the conditions of 30%.
Further, the method step can be also as follows：
Step 1：Substrate is washed by substrate cleaning, nitrogen dries up standby；
Step 2：Substrate after step 1 is processed is processed through oxygen plasma etch, 10-40min；
Step 3：By a certain proportion of AX and MX2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtain
To joining perovskite precursor solution；
Step 4：The ammonium salt additive of 0.1-20% is added in anti-solvent, magnetic agitation all dissolves to ammonium salt, pass through
Filter plug is placed on after filtering and is less than in 30% environment in humidity；
Step 5：Precursor solution one step that step 3 is obtained is spun in the substrate after step 2 is processed, and spin coating turns
Speed is 100-5000rpm, the anti-solvent after Deca step 4 is processed during spin coating, is operated under the conditions of humidity is less than 30%；
Step 6：Perovskite material will make annealing treatment after step 5 is processed, annealing temperature is 80-150 DEG C, low in humidity
Operated under the conditions of 30%.
Further, described ammonium salt concentration is 0.1-20%, and described ammonium salt is NH4I, NH4Cl, NH4Br or NH4F.
Further, described anti-solvent is toluene, chlorobenzene, dimethylbenzene, chloroform, propanol, ether or ethylene glycol.
Further, the mass fraction of described perovskite precursor solution is 30%-60%.
Further, described AX and MX2Mass ratio be 1:1-3.
Further, described substrate be FTO glass, ito glass, flexible PET base, glass or graphene conductive substrate.
Further, described AX and MX2；Wherein A is organic cation, and described machine cation is CH3NH3、NH2- CH=NH2、
CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One of or two kinds of mixture, M is bivalent metal ion Pb2 +Or Sn2 +One of or two kinds of mixture, X is monovalence halide ion Cl-, Br-, I-Or SCN-One or more of mixture.
The invention has the beneficial effects as follows：Due to adopting technique scheme, it is new that the present invention is based on traditional one-step method introducing
Cheap ammonium salt additive achieves the preparation of high-quality perovskite material.The introducing of ammonium salt additive improves film morphology and promotees
Enter crystal grain to grow up, improve the crystal property of perovskite material.It is thin that the present invention passes through ammonium salt additive auxiliary generation perovskite
Film, successfully prepares the high-quality perovskite material of the low defect density of states and long carrier lifetime.For improving perovskite material quality
Provide and new prepare approach.This kind of method process is simple, with low cost, it is favorably improved the photo electric of perovskite photovoltaic material
Can, have a good application prospect.
Brief description
Fig. 1 is present invention introduces new ammonium salt additive synthesizes the preparation process schematic diagram of perovskite material.
Fig. 2 is present invention introduces NH4The X-ray diffractogram of perovskite material before and after I additive.
Fig. 3 is present invention introduces NH4The luminescence generated by light spectrogram of perovskite material before and after I additive.
Fig. 4 is present invention introduces NH4Perovskite battery performance figure before and after I additive.
Fig. 5 is present invention introduces NH4Perovskite battery performance figure before and after Cl additive.
Fig. 6 is present invention introduces NH4Perovskite battery performance figure before and after Br additive.
Specific embodiment
With reference to example, technical scheme is described in detail it is clear that described example is only this
Small part in invention, rather than whole examples.Those skilled in the art are changed being obtained under the inspiration of the present invention
Every other example, broadly fall into the scope of protection of the invention.
As shown in figure 1, introducing, for the present invention is a kind of, the method schematic diagram that cheap additives prepare high-quality perovskite thin film,
The method is that the related additive of ammonium salt is introduced in perovskite precursor solution or anti-solvent.The present invention also provides a kind of profit
The method preparing high-quality perovskite material with the perovskite presoma after above-mentioned introducing additive or anti-solvent, concrete preparation
Step is as follows：
Step 1：Substrate is washed by substrate cleaning, nitrogen dries up standby；
Step 2：Substrate after step 1 is processed is processed through oxygen plasma etch, 10-40min；
Step 3：By a certain proportion of AX and MX2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtain
To joining perovskite precursor solution；
Step 4：Ammonium salt additive is added through step 3 in perovskite precursor solution after processing；
Step 5：It is spun to the substrate after step 2 is processed using precursor solution one step after step 4 is processed
On, spin coating rotating speed is 100-5000rpm, Deca anti-solvent during painting, is operated under the conditions of humidity is less than 30%；
Step 6：Perovskite material will make annealing treatment after step 5 is processed, annealing temperature is 80-150 DEG C, low in humidity
Operated under the conditions of 30%.
The method can be also following steps：
Step 1：Substrate is washed by substrate cleaning, nitrogen dries up standby；
Step 2：Substrate after step 1 is processed is processed through oxygen plasma etch, 10-40min；
Step 3：By a certain proportion of AX and MX2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtain
To joining perovskite precursor solution；
Step 4：Ammonium salt additive is added in anti-solvent, magnetic agitation all dissolves to ammonium salt, after filtering through filtering plug
It is placed on and be less than in 30% environment in humidity；
Step 5：Precursor solution one step that step 3 is obtained is spun in the substrate after step 2 is processed, and spin coating turns
Speed is 100-5000rpm, the anti-solvent after Deca step 4 is processed during spin coating, is operated under the conditions of humidity is less than 30%；
Step 6：Perovskite material will make annealing treatment after step 5 is processed, annealing temperature is 80-150 DEG C, low in humidity
Operated under the conditions of 30%.
Described organic cation A is CH3NH3、NH2- CH=NH2One of or two kinds of mixture, M is bivalence gold
Belong to ion Pb2 +Or Sn2 +One of or two kinds of mixture, X is monovalence halide ion Cl-, Br-, I-Or SCN-One of or
Multiple mixture.
Described ammonium salt concentration is 0.1-20%, and described ammonium salt is NH4I, NH4Cl, NH4Br or NH4F.
Described anti-solvent is toluene, chlorobenzene, dimethylbenzene, chloroform, propanol, ether, ethylene glycol etc..
The mass fraction of described perovskite precursor solution is 30%-60%.
Example 1：Introduce cheap NH4I prepares high-quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethanol, acetone, isopropanol replace ultrasonic 15min, and nitrogen dries up standby.Will
The substrate cleaning up is processed through oxygen plasma etch, 15min.Configuration perovskite precursor solution, by 1:1 CH3NH3I
And PbI (MAI)2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, add 1% NH4It is molten that I obtains presoma
Liquid.This precursor solution one step is spun in the substrate after process, spin coating rotating speed is 2000rpm, is less than 30% in humidity
Operated under part.No ammonium salt additive perovskite thin film preparation method ibid.Spin coating hole mobile material, gold evaporation electricity
Pole.Test.
Before and after contrast interpolation, the X-ray diffractogram of perovskite is as shown in Figure 2.
Before and after contrast interpolation, the luminescence generated by light spectrogram of perovskite is as shown in Figure 3.
Before and after contrast is added, perovskite battery performance figure is as shown in Figure 4.
Example 2：Introduce cheap NH4Cl prepares high-quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethanol, acetone, isopropanol replace ultrasonic 15min, and nitrogen dries up standby.Will
The substrate cleaning up is processed through oxygen plasma etch, 15min.Configuration perovskite precursor solution, by 1:1 NH2- CH=
NH2I (FAI) and PbI2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, add 15% NH4Before Cl obtains
Drive liquid solution.This precursor solution one step is spun in the substrate after process, spin coating rotating speed is 2000rpm, is less than in humidity
Operated under the conditions of 30%.No ammonium salt additive perovskite thin film preparation method ibid.Spin coating hole mobile material, evaporation
Gold electrode.Test.
Before and after contrast is added, perovskite battery performance figure is as shown in Figure 5.
Example 3：Introduce cheap NH4Br prepares high-quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethanol, acetone, isopropanol replace ultrasonic 15min, and nitrogen dries up standby.Will
The substrate cleaning up is processed through oxygen plasma etch, 15min.Configuration perovskite precursor solution, by 1:1 CH3NH3Cl
And PbI2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, add 5% NH4Br obtains precursor solution.Will
This precursor solution one step is spun in the substrate after process, and spin coating rotating speed is 2000rpm, enters under the conditions of humidity is less than 30%
Row operation.No ammonium salt additive perovskite thin film preparation method ibid.Spin coating hole mobile material, is deposited with gold electrode.Test.
Before and after contrast is added, perovskite battery performance figure is as shown in Figure 6.
Example 4：Introduce cheap NH4F prepares high-quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethanol, acetone, isopropanol replace ultrasonic 15min, and nitrogen dries up standby.Will
The substrate cleaning up is processed through oxygen plasma etch, 15min.Configuration perovskite precursor solution, by 1:3 (MAI,
) and PbI FAI2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtains in precursor solution, add 5%
NH4Br is in chlorobenzene.This precursor solution one step is spun in the substrate after process, spin coating rotating speed is 2000rpm, the spin coating phase
Between Deca be added with NH4The anti-solvent of F, is operated under the conditions of humidity is less than 30%.The perovskite of no ammonium salt additive is thin
Membrane preparation method is ibid.Spin coating hole mobile material, is deposited with gold electrode.Test.
Claims (9)
1. a kind of cheap additives that introduce prepare the method for high-quality perovskite thin film it is characterised in that this high-quality perovskite
Material introduces ammonium salt additive in preparation process；Described additive can be incorporated in perovskite precursor solution or anti-solvent
In；Described high-quality perovskite material structural formula is AMX3, wherein A is organic cation, and described organic cation is CH3NH3、
NH2- CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One of or two kinds of mixture, M is divalent metal
Ion Pb2 +Or Sn2 +One of or two kinds of mixture, X is monovalence halide ion Cl-, Br-, I-Or SCN-One of or many
The mixture planted.
2. method according to claim 1 is it is characterised in that the method step is as follows：
Step 1：Substrate is washed by substrate cleaning, nitrogen dries up standby；
Step 2：Substrate after step 1 is processed is processed through oxygen plasma etch, 10-40min；
Step 3：By a certain proportion of AX and MX2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtain joining calcium
Titanium ore precursor solution；
Step 4：Ammonium salt additive is added through step 3 in perovskite precursor solution after processing；
Step 5：It is spun in the substrate after step 2 is processed using precursor solution one step after step 4 is processed, rotation
Painting rotating speed is 100-5000rpm, Deca anti-solvent during painting, is operated under the conditions of humidity is less than 30%；
Step 6：Perovskite material will make annealing treatment after step 5 is processed, annealing temperature is 80-150 DEG C, is less than in humidity
Operated under the conditions of 30%.
3. method according to claim 1 is it is characterised in that the method step is as follows：
Step 1：Substrate is washed by substrate cleaning, nitrogen dries up standby；
Step 2：Substrate after step 1 is processed is processed through oxygen plasma etch, 10-40min；
Step 3：By a certain proportion of AX and MX2It is dissolved in dimethyl sulfoxide and the mixed solvent of dimethylformamide, obtain joining calcium
Titanium ore precursor solution；
Step 4：Ammonium salt additive is added in anti-solvent, magnetic agitation all dissolves to ammonium salt, place after filtering through filtering plug
In the environment being less than 30% in humidity；
Step 5：Precursor solution one step that step 3 is obtained is spun in the substrate after step 2 is processed, and spin coating rotating speed is
100-5000rpm, the anti-solvent after Deca step 4 is processed during spin coating, operated under the conditions of humidity is less than 30%；
Step 6：Perovskite material will make annealing treatment after step 5 is processed, annealing temperature is 80-150 DEG C, is less than in humidity
Operated under the conditions of 30%.
4. according to claim 1-3 any one methods described it is characterised in that described ammonium salt concentration is 0.1-20%, described
Ammonium salt is NH4I, NH4Cl, NH4Br or NH4F.
5. method according to claim 3 it is characterised in that described anti-solvent be toluene, chlorobenzene, dimethylbenzene, chloroform, third
Alcohol, ether or ethylene glycol.
6. according to the method in claim 2 or 3 it is characterised in that the mass fraction of described perovskite precursor solution
For 30%-60%.
7. according to the method in claim 2 or 3 it is characterised in that described substrate is FTO glass, ito glass, flexibility
PET base, glass or graphene conductive substrate.
8. according to the method in claim 2 or 3 it is characterised in that described AX and MX2Mass ratio be 1:1-3.
9. according to the method in claim 2 or 3 it is characterised in that described AX and MX2；Wherein A is organic cation, described
Organic cation is CH3NH3、NH2- CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One of or two kinds
Mixture, M is bivalent metal ion Pb2 +Or Sn2 +One of or two kinds of mixture, X is monovalence halide ion Cl-, Br-,
I-Or SCN-One or more of mixture.
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