CN106486602B - A method of it introducing cheap additives and prepares high quality perovskite thin film - Google Patents
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- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
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- H10K71/10—Deposition of organic active material
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Abstract
A kind of method for introducing cheap additives preparation high quality perovskite thin film of the present invention.The high quality perovskite material introduces ammonium salt additive during the preparation process；The additive can be introduced into perovskite precursor solution or in anti-solvent；This kind of perovskite material structural formula is AMX3, wherein A is organic cation, CH3NH3、NH2- CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One or both of mixture, M Pb2 +Or Sn2 +One or both of mixture, X Cl‑, Br‑, I‑Or SCN‑One of or a variety of mixtures.The introducing of ammonium salt is reduced film internal flaw by this method reduces surface state, provides new preparation approach.Simple process and low cost, repeatability is high, and the optics electric property for helping to improve perovskite thin film has a good application prospect.
Description
Technical field
The invention belongs to nano-functional material photovoltaic solar Material Fields, are related to the preparation of high quality perovskite material, especially
It is a kind of method of introducing cheap additives preparation high quality perovskite thin film.
Background technique
Human social development still depends on fossil energy so far.However the distributed pole of fossil energy 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 effects, these negative effects seriously threaten the sustainable development of human society.Solar battery energy
It enough is converted into electric energy using solar energy, inexhaustible clean energy resource can be provided for human social development,
It is human society reply energy crisis, seeks the important countermeasure of sustainable development.
Solar battery material therefor mainly has a silica-base material at present, GaAs material, indium phosphide/InGaP material,
Copper indium gallium selenide 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 have reached 20%, have huge researching value ([1] Polman A, Knight M, Garnett E C,
et al.Science,2016,352:4424.).Perovskite material is according to the selection of different halogens, and band gap is in 1.6eV to 3.2eV
Range is adjustable, has larger absorptivity, 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).In addition, 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 achieve 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 low in cost, has huge application potential.However since solwution method prepares the diversity of environment
The quality for affecting material prepared constrains the further application of material, and the serious stability for destroying device limits calcium titanium
The development of mine battery.
Summary of the invention
To solve the above-mentioned problems, the object of the present invention is to provide a kind of method for preparing high quality perovskite material, drops
Low material crystals defect reduces surface state, cost of manufacture is reduced as far as possible while improving core material crystal property, to mention
High Photovoltaic Device Performance provides high quality perovskite material.
The technical scheme is that a kind of method for introducing cheap additives preparation high quality perovskite thin film, the party
Method introduces ammonium salt additive in high quality perovskite material during the preparation process；The additive can be introduced into perovskite presoma
In solution or in anti-solvent；The high quality perovskite material structural formula is AMX3, wherein A is organic cation, the machine sun
Ion CH3NH3、NH2- CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One or both of mixture, M
For bivalent metal ion Pb2 +Or Sn2 +One or both of mixture, X be monovalence halide ion Cl-, Br-, I-Or SCN-In
One or more mixtures.
Further, the method steps are as follows:
Step 1: substrate being washed by substrate cleaning process, is dried with nitrogen spare；
Step 2: will by step 1, treated that substrate is handled through oxygen plasma etch, 10-40min；
Step 3: by a certain proportion of AX and MX2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained
To with perovskite precursor solution；
Step 4: ammonium salt additive is added in by step 3 treated perovskite precursor solution；
Step 5: using by step 4, treated that one step of precursor solution is spun to by step 2 treated substrate
On, spin coating revolving speed is 100-5000rpm, is operated under the conditions of humidity is lower than 30%；
Step 6: perovskite material will be made annealing treatment after step 5 processing, annealing temperature is 80-150 DEG C, low in humidity
It is operated under the conditions of 30%.
Further, this method step can also be as follows:
Step 1: substrate being washed by substrate cleaning process, is dried with nitrogen spare；
Step 2: will by step 1, treated that substrate is handled through oxygen plasma etch, 10-40min；
Step 3: by a certain proportion of AX and MX2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained
To with perovskite precursor solution；
Step 4: the ammonium salt additive of 0.1-20% being added in anti-solvent, magnetic agitation to ammonium salt all dissolves, and passes through
It is placed in environment of the humidity lower than 30% after filter plug filtering；
Step 5: one step of precursor solution that step 3 obtains is spun to by step 2 treated substrate, spin coating turns
Speed is 100-5000rpm, and treated the anti-solvent of a dropping step 4 during spin coating is operated under the conditions of humidity is lower than 30%；
Step 6: perovskite material will be made annealing treatment after step 5 processing, annealing temperature is 80-150 DEG C, low in humidity
It is operated under the conditions of 30%.
Further, the ammonium salt concentration is 0.1-20%, and the ammonium salt is NH4I, NH4Cl, NH4Br or NH4F。
Further, the anti-solvent is toluene, chlorobenzene, dimethylbenzene, chloroform, propyl alcohol, ether or ethylene glycol.
Further, the mass fraction of the perovskite precursor solution is 30%-60%.
Further, the AX and MX2Mass ratio be 1:1-3.
Further, the substrate is FTO glass, ito glass, flexible PET base, glass or graphene conductive substrate.
Further, the AX and MX2；Wherein A is organic cation, and the machine cation is CH3NH3、NH2- CH=NH2、
CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One or both of mixture, M be bivalent metal ion Pb2 +Or Sn2 +One or both of mixture, X be monovalence halide ion Cl-, Br-, I-Or SCN-One of or a variety of mixtures.
The beneficial effects of the present invention are: due to the adoption of the above technical scheme, the present invention is based on the introducing of traditional one-step method is novel
Cheap ammonium salt additive realizes the preparation of high quality perovskite material.The introducing of ammonium salt additive improves film morphology rush
It grows up into crystal grain, improves the crystal property of perovskite material.The present invention is thin by 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.To improve perovskite material quality
Provide new preparation approach.This kind of method and process is simple, low in cost, helps to improve the photo electric of perovskite photovoltaic material
Can, it has a good application prospect.
Detailed description of the invention
Present invention introduces the preparation process schematic diagrames of novel ammonium salt additive synthesis perovskite material by Fig. 1.
Present invention introduces NH by Fig. 24The X-ray diffractogram of perovskite material before and after I additive.
Present invention introduces NH by Fig. 34The luminescence generated by light spectrogram of perovskite material before and after I additive.
Present invention introduces NH by Fig. 44Perovskite battery performance figure before and after I additive.
Present invention introduces NH by Fig. 54Perovskite battery performance figure before and after Cl additive.
Present invention introduces NH by Fig. 64Perovskite battery performance figure before and after Br additive.
Specific embodiment
Technical solution of the present invention is described in detail below with reference to example, it is clear that described example is only this
Small part in invention, rather than whole examples.Those skilled in the art are changed under inspiration of the invention and are obtained
Every other example, shall fall within the protection scope of the present invention.
As shown in Figure 1, for a kind of method schematic diagram for introducing cheap additives and preparing high quality perovskite thin film of the present invention,
This method is that the relevant additive of ammonium salt is introduced into perovskite precursor solution or anti-solvent.The present invention also provides a kind of benefits
It is specific to prepare with the method for perovskite presoma or anti-solvent preparation high quality perovskite material after above-mentioned introducing additive
Steps are as follows:
Step 1: substrate being washed by substrate cleaning process, is dried with nitrogen spare；
Step 2: will by step 1, treated that substrate is handled through oxygen plasma etch, 10-40min；
Step 3: by a certain proportion of AX and MX2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained
To with perovskite precursor solution；
Step 4: ammonium salt additive is added in by step 3 treated perovskite precursor solution；
Step 5: using by step 4, treated that one step of precursor solution is spun to by step 2 treated substrate
On, spin coating revolving speed is 100-5000rpm, and anti-solvent is added dropwise during painting, is operated under the conditions of humidity is lower than 30%；
Step 6: perovskite material will be made annealing treatment after step 5 processing, annealing temperature is 80-150 DEG C, low in humidity
It is operated under the conditions of 30%.
This method can be also following steps:
Step 1: substrate being washed by substrate cleaning process, is dried with nitrogen spare；
Step 2: will by step 1, treated that substrate is handled through oxygen plasma etch, 10-40min；
Step 3: by a certain proportion of AX and MX2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained
To with perovskite precursor solution；
Step 4: ammonium salt additive being added in anti-solvent, magnetic agitation to ammonium salt all dissolves, after filtering plug filters
It is placed in environment of the humidity lower than 30%；
Step 5: one step of precursor solution that step 3 obtains is spun to by step 2 treated substrate, spin coating turns
Speed is 100-5000rpm, and treated the anti-solvent of a dropping step 4 during spin coating is operated under the conditions of humidity is lower than 30%；
Step 6: perovskite material will be made annealing treatment after step 5 processing, annealing temperature is 80-150 DEG C, low in humidity
It is operated under the conditions of 30%.
The organic cation A is CH3NH3、NH2- CH=NH2One or both of mixture, M be divalent gold
Belong to ion Pb2 +Or Sn2 +One or both of mixture, X be monovalence halide ion Cl-, Br-, I-Or SCN-One of or
A variety of mixtures.
The ammonium salt concentration is 0.1-20%, and the ammonium salt is NH4I, NH4Cl, NH4Br or NH4F。
The anti-solvent is toluene, chlorobenzene, dimethylbenzene, chloroform, propyl alcohol, ether, ethylene glycol etc..
The mass fraction of the perovskite precursor solution is 30%-60%.
Example 1: cheap NH is introduced4I prepares high quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethyl alcohol, acetone, isopropanol alternating ultrasound 15min are dried with nitrogen spare.It will
The substrate cleaned up is handled through oxygen plasma etch, 15min.Perovskite precursor solution is configured, by the CH of 1:13NH3I
(MAI) and PbI2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, adds 1% NH4It is molten that I obtains presoma
Liquid.By in one step of the precursor solution substrate that is spun to that treated, spin coating revolving speed is 2000rpm, is lower than 30% in humidity
It is operated under part.The perovskite thin film preparation method of no ammonium salt additive is same as above.Gold electricity is deposited in spin coating hole mobile material
Pole.Test.
The X-ray diffractogram of comparison addition front and back perovskite is as shown in Figure 2.
The luminescence generated by light spectrogram of comparison addition front and back perovskite is as shown in Figure 3.
Comparison addition front and back perovskite battery performance figure is as shown in Figure 4.
Example 2: cheap NH is introduced4Cl prepares high quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethyl alcohol, acetone, isopropanol alternating ultrasound 15min are dried with nitrogen spare.It will
The substrate cleaned up is handled through oxygen plasma etch, 15min.Perovskite precursor solution is configured, by the NH of 1:12- CH=
NH2I (FAI) and PbI2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, adds 15% NH4Before Cl is obtained
Drive liquid solution.By in one step of the precursor solution substrate that is spun to that treated, spin coating revolving speed is 2000rpm, is lower than in humidity
It is operated under the conditions of 30%.The perovskite thin film preparation method of no ammonium salt additive is same as above.Spin coating hole mobile material, vapor deposition
Gold electrode.Test.
Comparison addition front and back perovskite battery performance figure is as shown in Figure 5.
Example 3: cheap NH is introduced4Br prepares high quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethyl alcohol, acetone, isopropanol alternating ultrasound 15min are dried with nitrogen spare.It will
The substrate cleaned up is handled through oxygen plasma etch, 15min.Perovskite precursor solution is configured, by the CH of 1:13NH3Cl
And PbI2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, adds 5% NH4Br obtains precursor solution.It will
In substrate that one step of precursor solution is spun to that treated, spin coating revolving speed is 2000rpm, under the conditions of humidity is lower than 30% into
Row operation.The perovskite thin film preparation method of no ammonium salt additive is same as above.Gold electrode is deposited in spin coating hole mobile material.Test.
Comparison addition front and back perovskite battery performance figure is as shown in Figure 6.
Example 4: cheap NH is introduced4F prepares high quality perovskite thin film
Substrate (FTO/ITO) is cleaned up, ethyl alcohol, acetone, isopropanol alternating ultrasound 15min are dried with nitrogen spare.It will
The substrate cleaned up is handled through oxygen plasma etch, 15min.Configure perovskite precursor solution, by 1:3 (MAI,
) and PbI FAI2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained in precursor solution, adds 5%
NH4Br is into chlorobenzene.By in one step of the precursor solution substrate that is spun to that treated, spin coating revolving speed is 2000rpm, spin coating phase
Between be added dropwise be added with NH4The anti-solvent of F is operated under the conditions of humidity is lower than 30%.Perovskite without ammonium salt additive is thin
Membrane preparation method is same as above.Gold electrode is deposited in spin coating hole mobile material.Test.
Claims (9)
1. a kind of method for introducing cheap additives preparation high quality perovskite thin film, which is characterized in that the high quality perovskite
Material introduces ammonium salt additive during the preparation process；The additive is introduced into perovskite precursor solution or in anti-solvent；
The high quality perovskite material structural formula is AMX3, wherein A is organic cation, and the organic cation is CH3NH3、NH2-
CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3One or both of mixture, M is bivalent metal ion
Pb2 +Or Sn2 +One or both of mixture, X be monovalence halide ion Cl-, Br-, I-Or SCN-One of or it is a variety of
Mixture.
2. the method according to claim 1, wherein the method steps are as follows:
Step 1: substrate being washed by substrate cleaning process, is dried with nitrogen spare；
Step 2: will by step 1, treated that substrate is handled through oxygen plasma etch, 10-40min；
Step 3: by a certain proportion of AX and MX2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained with calcium
Titanium ore precursor solution；
Step 4: ammonium salt additive is added in by step 3 treated perovskite precursor solution；
Step 5: using by step 4, treated that one step of precursor solution is spun to by step 2 treated substrate, rotation
Painting revolving speed is 100-5000rpm, and anti-solvent is added dropwise during painting, is operated under the conditions of humidity is lower than 30%；
Step 6: perovskite material will be made annealing treatment after step 5 processing, annealing temperature is 80-150 DEG C, is lower than in humidity
It is operated under the conditions of 30%.
3. the method according to claim 1, wherein the method steps are as follows:
Step 1: substrate being washed by substrate cleaning process, is dried with nitrogen spare；
Step 2: will by step 1, treated that substrate is handled through oxygen plasma etch, 10-40min；
Step 3: by a certain proportion of AX and MX2It is dissolved in the in the mixed solvent of dimethyl sulfoxide and dimethylformamide, is obtained with calcium
Titanium ore precursor solution；
Step 4: ammonium salt additive being added in anti-solvent, magnetic agitation to ammonium salt all dissolves, and places after filtering plug filters
In environment of the humidity lower than 30%；
Step 5: one step of precursor solution that step 3 obtains is spun to by step 2 treated substrate, spin coating revolving speed is
100-5000rpm, treated the anti-solvent of a dropping step 4 during spin coating, is operated under the conditions of humidity is lower than 30%；
Step 6: perovskite material will be made annealing treatment after step 5 processing, annealing temperature is 80-150 DEG C, is lower than in humidity
It is operated under the conditions of 30%.
4. method according to claim 1 to 3, which is characterized in that the ammonium salt concentration is 0.1-20%, the ammonium
Salt is NH4I, NH4Cl, NH4Br or NH4F。
5. according to the method described in claim 3, it is characterized in that, the anti-solvent be toluene, chlorobenzene, dimethylbenzene, chloroform, third
Alcohol, ether or ethylene glycol.
6. according to the method in claim 2 or 3, which is characterized in that the mass fraction of the perovskite precursor solution
For 30%-60%.
7. according to the method in claim 2 or 3, which is characterized in that the substrate is FTO glass, ito glass, flexibility
PET base, glass or graphene conductive substrate.
8. according to the method in claim 2 or 3, which is characterized in that the AX and MX2Mass ratio be 1:1-3.
9. according to the method in claim 2 or 3, which is characterized in that the AX and MX2；Its
Middle A is organic cation, and the organic cation is CH3NH3、NH2-CH=NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3
(CH2)3NH3One or both of mixture, M be bivalent metal ion Pb2 +Or Sn2 +One or both of mixing
Object, X are monovalence halide ion Cl-, Br-, I-Or SCN-One of or a variety of mixtures.
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