CN106981570A - A kind of fast preparation method of perovskite thin film and its application - Google Patents
A kind of fast preparation method of perovskite thin film and its application Download PDFInfo
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Abstract
The present invention announces fast preparation method and its application of a kind of perovskite thin film, realizes rapid growth of crystal using hot gas seasoning, obtains smooth fine and close high-quality perovskite thin film；Including：The mixed solution of lead-containing materials (at least one of lead acetate, lead oxide, lead hydroxide, lead sulfate, ceruse, plumbi nitras, (secondary) lead phosphate, lead chloride, lead iodide, lead bromide) and organic halogen (at least one of methylamine iodine, carbonamidine iodine, methylamine bromine, carbonamidine bromine, methylamine chlorine, carbonamidine chlorine) is prepared, perovskite precursor liquid is used as；It is deposited in substrate；Using dry hot gas, quickly drying is deposited on the perovskite precursor liquid in substrate, forms smooth fine and close perovskite thin film.High efficiency, low cost of the present invention, it is adapted to large-scale industrial production, obtained perovskite thin film can be applied in many photoelectric functional devices fields such as solar cell, light emitting diode, photodiode, laser, thin film transistor (TFT), photodetector, micro sensing device.
Description
Technical field
The invention belongs to photoelectric functional material and devices field, and in particular to a kind of quick method for preparing perovskite material film,
The related application of perovskite thin film and perovskite material film.
Background technology
In recent years, environmental pollution and energy crisis are increasingly sharpened, and are developed and extremely urgent using new cleaning fuel technology.And too
Positive energy battery receives much concern due to possessing the outstanding advantages such as cleaning, efficient, sustainability.In numerous solar cells, have
The perovskite solar cell of machine inorganic hybridization, developed swift and violent photoelectric transformation efficiency from 3.8% lifting of 2009 to now in recent years
Of today 21%.Such solar cell, in 2013 by the U.S.《Science (science)》Magazine be chosen as ten big Progress ＆ New Products it
One, this series of progress shows, organic-inorganic perovskite solar cell can be mainly clean energy resource as future.
Perovskite material is because of its abundant raw material, and photoelectric properties are superior, with low cost, the advantage such as solution processable, in solar energy
The numerous areas such as battery, generating diode, photodiode, laser and transistor have obtained widely studied.It is prepared by tradition
The method of perovskite thin film includes vapour deposition method and solwution method.Vapour deposition method is because its equipment is expensive, and raw material availability is low so that its
Cost is higher and applies less.Solwution method prepares perovskite solar cell and is divided into one-step method and two-step method, traditional handicraft
Based on sol evenning machine by perovskite precursor liquid spin-coating film, then made annealing treatment in thermal station, the solvent in removing solution is simultaneously
Its crystallization is set to obtain film.To obtain smooth fine and close perovskite thin film, it can typically be handled in spin coating process using secondary solvent,
Take off and carry out the method such as DMF solvent or methylamine gas atmosphere regrowth after fire again, to reduce perovskite thin film
Pin hole and acicular crystal etc., so as to improve the quality and corresponding photoelectric property of perovskite thin film.This is not only harsh to environmental requirement,
Typically require in dry air ambient (humidity is less than 20%) or completed in full of nitrogen or inert atmosphere glove box,
And significantly limit the selection of processing technology.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a kind of quick method, calcium titanium for preparing perovskite material film
The related application of ore deposit film and perovskite material film, perovskite thin film is prepared using hot gas seasoning, realizes the fast fast-growing of crystal
It is long, obtain smooth fine and close high-quality thin film；Preparation method high efficiency, low cost of the present invention and technique is simple；Obtained based on the present invention
Perovskite thin film can apply in many photoelectric functional devices fields such as solar cell.
The technical scheme that the present invention is provided is：
A kind of fast preparation method of perovskite thin film, rapid growth of crystal is realized using hot gas seasoning, is prepared smooth
Fine and close high-quality perovskite thin film, comprises the following steps：
1) mixed solution of lead-containing materials and organic halogen is prepared, perovskite precursor liquid is used as；The perovskite precursor liquid is thermosol
Liquid or cold soln；The temperature of the hot solution is 35 DEG C~120 DEG C；The temperature of the cold soln is 20 DEG C~30 DEG C；
2) by deposition process by step 1) the perovskite precursor liquid is deposited in substrate；The substrate include flexible substrates or
Rigid basement；
3) step 2 is quickly dried up using dry hot gas) the perovskite forerunner being deposited in flexible substrates or rigid basement
Liquid, forms smooth fine and close perovskite thin film.
For the fast preparation method of above-mentioned perovskite thin film, further, step 1) lead-containing materials be lead acetate, oxygen
Change in lead, lead hydroxide, lead sulfate, ceruse, plumbi nitras, (secondary) lead phosphate, lead chloride, lead iodide, lead bromide at least
It is a kind of；Organic halogen is at least one of methylamine iodine, carbonamidine iodine, methylamine bromine, carbonamidine bromine, methylamine chlorine, carbonamidine chlorine.
For the fast preparation method of above-mentioned perovskite thin film, further, step 1) the solvent bag of the perovskite precursor liquid
Include N,N-dimethylformamide, dimethyl sulfoxide (DMSO), gamma-butyrolacton, 1-METHYLPYRROLIDONE, isopropanol, methanol, ethanol, two-
One or more in methyl cellosolve, two-ethoxy ethanol, chloroform, toluene, chlorobenzene and dichloro-benzenes.
For the fast preparation method of above-mentioned perovskite thin film, further, in step 1) it is optional in the perovskite precursor liquid
In selecting property incorporation water, hydrochloric acid, hydroiodic acid, phosphoric acid, hypophosphorous acid, acetic acid, cesium chloride, cesium bromide, cesium iodide, cesium carbonate
One or more, are used as additive.
For the fast preparation method of above-mentioned perovskite thin film, further, step 2) substrate before the deposition can be advance
It is heat-treated；The flexible substrates are PET (PET), PEN (PEN) or poly-
Etherimide (PEI)；The rigid basement is ito transparent electrode, FTO transparency electrodes, metal nanometer line/oxide mixing are saturating
Prescribed electrode, oxide/metal/oxide multilevel hierarchy transparency electrode, alloy, metal electrode and carbon material, white glass rigid basement
At least one of；The deposition process include slot coated, silk-screen printing, printing, spraying, blade coating and spin coating in one kind or
It is a variety of.
For the fast preparation method of above-mentioned perovskite thin film, further, in step 2) it is described by deposition process by calcium titanium
Before ore deposit precursor liquid is deposited in substrate, first in upper surface of substrate deposition of titanium oxide, zinc oxide, poly- 3,4-ethylene dioxythiophene:
Poly styrene sulfonate, zinc-tin oxide, tin ash, poly- [double (4- phenyl) (4- butyl phenyls) amine, 4- butyl-N, N- diphenyl benzene
Amine homopolymer, polyvinylcarbazole, metal phthalein mountain valley with clumps of trees and bamboo molecular material, fullerene, graphene, nickel oxide, vanadic anhydride, sulphur cyanogen
Change copper, cuprous iodide, zinc sulphide, molybdenum disulfide, chromium oxide, molybdenum oxide, fullerene derivate, 2,2', the [(4- of N, N- bis- of 7,7'- tetra-
Methoxyphenyl) amino] two fluorenes of -9,9'- spiral shells, poly- [double (4- phenyl) (2,4,6- trimethylphenyls) amine], 2,3,5,6- tetra- fluoro- 7,7', 8,8'-
One or more in four cyanogen dimethyl-parabenzoquinones.
For the fast preparation method of above-mentioned perovskite thin film, further, step 3) hot gas of the drying include argon gas,
Nitrogen, oxygen, the one or more dried in hot-air.
For the fast preparation method of above-mentioned perovskite thin film, further, in step 3) it is described formation perovskite thin film after,
50 DEG C~150 DEG C of 1~120min of thermal anneal process is carried out to the perovskite thin film of formation.
The perovskite that the fast preparation method that the present invention also provides perovskite thin film described in a kind of utilization claim 1 is prepared is thin
Film.In addition, the perovskite thin film that can prepare the fast preparation method using above-mentioned perovskite thin film is applied to solar-electricity
Pond, light emitting diode, photodiode, laser, thin film transistor (TFT), the preparation of photodetector or micro sensing device.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention prepares perovskite thin film using hot gas seasoning, it is possible to achieve organic-inorganic perovskite crystal fast-growth, obtains
Smooth fine and close high-quality thin film has been arrived, while operating procedure is simple, it is relatively low to environment and equipment requirement.Eliminate secondary solvent
The process such as processing or the post processing of crystal diauxic growth, simplifies film preparation flow.Therefore, high efficiency, low cost of the present invention, is fitted
Should in large-scale industrial production, the perovskite thin film obtained based on the present invention can apply solar cell, light emitting diode,
Many photoelectric functional devices fields such as photodiode, laser, thin film transistor (TFT), photodetector, micro sensing device.
Brief description of the drawings
Fig. 1 prepares the FB(flow block) of perovskite thin film for the hot gas seasoning that the present invention is provided.
Fig. 2 is the Characterization for Microstructure figure of the perovskite thin film prepared in the embodiment of the present invention one using hot gas seasoning；
Wherein, (a) is the X-ray diffractogram (X-ray diffraction, XRD) of film crystal structure, and wherein abscissa is X
X ray diffraction angle, ordinate is diffracted intensity；(b) for SEM shape appearance figure (Scanning electron microscope,
SEM schemes), wherein white scale size in the lower right corner is 1 micron.
Embodiment
Below in conjunction with the accompanying drawings, the present invention, the scope of but do not limit the invention in any way are further described by embodiment.
The invention provides a kind of method that directly can quickly prepare perovskite thin film in atmosphere, the heat that Fig. 1 provides for the present invention
Gas seasoning prepares the FB(flow block) of perovskite thin film, including：The mixed solution of lead-containing materials and organic halogen is prepared first,
Lead-containing materials be lead acetate, lead oxide, lead hydroxide, lead sulfate, ceruse, plumbi nitras, (secondary) lead phosphate, lead chloride,
At least one of lead iodide, lead bromide；Organic halogen is methylamine iodine, carbonamidine iodine, methylamine bromine, carbonamidine bromine, methylamine chlorine, carbonamidine
At least one of chlorine.Then using mixed solution as precursor liquid, by slot coated, silk-screen printing is printed, sprayed, blade coating,
Precursor liquid is deposited in flexible substrates or rigid basement by the technologies such as spin coating, recycles dry hot gas quickly to dry up, and forms flat
Whole fine and close perovskite thin film.
It is used as one embodiment of the present invention, it is preferred that the lead-containing materials in precursor liquid include lead acetate, lead oxide, hydrogen-oxygen
Change the one or more in lead, lead sulfate, ceruse, plumbi nitras, (secondary) lead phosphate, lead chloride, lead iodide, lead bromide；
It is one or more that organic halogen includes methylamine iodine, carbonamidine iodine, methylamine bromine, carbonamidine bromine, methylamine chlorine, carbonamidine chlorine.
Precursor liquid solvent include N,N-dimethylformamide, dimethyl sulfoxide (DMSO), gamma-butyrolacton, 1-METHYLPYRROLIDONE, isopropanol,
Methanol, ethanol, cellosolvo, chloroform, toluene, chlorobenzene and dichloro-benzenes etc., it is preferred that can select single solvent,
The allotment of two kinds or two or more solvents can suitably be carried out.The concentration of precursor aqueous solution is mole dense with lead source (lead-containing materials)
On the basis of degree, concentration range is 0.05M~1M.
It is used as one embodiment of the present invention, it is preferred that the deposition process of precursor liquid includes slot coated, silk-screen printing, beaten
At least one of print, spraying, blade coating, spin coating.
It is used as one embodiment of the present invention, it is preferred that the substrate of deposition film includes ito transparent electrode, the transparent electricity of FTO
Pole, metal nanometer line/oxide mixed transparent electrode, oxide/metal/oxide multilevel hierarchy transparency electrode, alloy, metal
At least one of rigid basement such as electrode and carbon material, white glass；Or PET, poly- naphthalenedicarboxylic acid ethylene glycol
At least one of ester, PEI flexible substrates.
As one embodiment of the present invention, in device fabrication process, it is alternative substrate surface preferential deposition titanium dioxide,
Zinc oxide, poly- 3,4- ethylenedioxy thiophenes: poly styrene sulfonate, zinc-tin oxide, tin ash, poly- [double (4- phenyl) (4- butyl
Phenyl) amine, 4- butyl-N, N- diphenyl aniline homopolymer, polyvinylcarbazole, metal phthalein mountain valley with clumps of trees and bamboo molecular material, fullerene, graphene,
Nickel oxide, vanadic anhydride, copper rhodanide, cuprous iodide, zinc sulphide, molybdenum disulfide, chromium oxide, molybdenum oxide, fullerene
Derivative, 2,2', the fluorenes of 7,7'- tetra- [N, N- bis- (4- methoxyphenyls) amino] -9,9'- spiral shells two, poly- [double (4- phenyl) (2,4,6- trimethylphenyls)
Amine], 2,3,5,6- tetra- fluoro- 7,7', one or more boundary layers in 8,8'- tetra- cyanogen dimethyl-parabenzoquinones, then redeposited perovskite thin film.
As one embodiment of the present invention, in hot gas drying process, it is preferred that the gas used can be that argon gas etc. is lazy
Property gas or nitrogen, oxygen or dry air.Gas pressure intensity is 0.1~5MPa, and gas temperature is 0~250 DEG C,
Gas outlet is 0~40cm with deposition substrate distance, while requiring that jet area is more than film size in principle.
As one embodiment of the present invention, hot gas drying prepares perovskite thin film, can be according to precursor liquid, dry gas temperature
The difference of degree and gas flow rate etc., selective carry out thermal anneal process.Fiery 50~150 DEG C of temperature is taken off, annealing time is
1~120min.
As one embodiment of the present invention, hot gas drying prepares perovskite thin film, in preparation process, used calcium
Titanium ore precursor liquid can be hot solution (being heated to precursor liquid, 35 DEG C~120 DEG C) or cold soln (without heating, 20 DEG C~30 DEG C)
In any one；Perovskite thin film institute is prepared using substrate without being heat-treated in advance, can also be carried out in advance (30 DEG C~200 DEG C)
Heat treatment, size of foundation base size is unrestricted.
In perovskite thin film preparation process, depositional mode, gas componant, gas temperature and flow velocity can be according in different components
In application and flexibly choose, the perovskite thin film prepared can be applied to perovskite solar cell, light emitting diode, light
Quick diode, laser, thin film transistor (TFT), photodetector or micro sensing device etc..
Illustrate the method for preparing perovskite thin film that the present invention is provided below by way of specific embodiment.
Embodiment one：Perovskite thin film is prepared based on hot gas rapid dry process, for preparing trans solar cell
Ito transparent electrode is cleaned by ultrasonic with glass cleaner, deionized water, acetone, methanol successively, added using 60 DEG C
Heat drying, to improve the wellability and cleanliness factor on FTO surfaces；Using slot coated printing hole mobile material PEDOT:PSS,
The lower 130 DEG C of thermal annealing 20min of atmospheric environment；The methylamine iodine of 0.45mmol lead acetate and 1.35mmol is placed in 1ml DMF
In, it is stirred at room temperature to solute and is completely dissolved, forms transparent mixing precursor liquid, printed precursor liquid using slot coated or knife coating
Brush ITO/PEDOT:It is fast with 100 DEG C of drying hot-air directly over ITO at 5cm distance in PSS substrates
Speed drying solvent, obtains dark-brown perovskite thin film, XRD and SEM test structures such as Fig. 2 of resulting perovskite thin film
It is shown.As can be seen that obtained film composition mainly CH3NH3PbI3, crystallinity is preferable.It is also noted that using hot gas
Seasoning can obtain opposed flattened perovskite thin film；Pass through slot coated printed electronic transmission material such as fullerene derivate again
(PC61BM), last vacuum (<4*10-4Pa silver electrode) is deposited；Complete based on hot gas rapid dry process perovskite thin film
The preparation of trans solar cell.
Embodiment two
Carry out ultrasonic clear, 60 DEG C of heating, dryings with glass cleaner, deionized water, acetone, methanol successively to ito transparent electrode,
To improve the wellability and cleanliness factor on FTO surfaces.And then organic alcoholic solution of finely dispersed titania nanoparticles
FTO upper surfaces are spun to, 150 DEG C are heated 20min and complete the preparation of titanic oxide electronic collecting layer.Configure 0.8M chlorination
Lead and 2.4M methylamine iodine mixed solution are in DMF, and 70 DEG C of stirrings are to being completely dissolved.Using knife coating procedure titania-based
Perovskite thin film is prepared on bottom, then perovskite thin film is placed at dry hot-air gas outlet 5cm positions, hot-air is being dried
The lower real solvent of (100 DEG C) auxiliary quickly volatilizees, and accelerates the chemical reaction between lead chloride and methylamine iodine, so as to realize hot gas
It is prepared by dry high-quality perovskite thin film.
Embodiment three
Transparency electrode carries out ultrasonic clear, 60 DEG C of heating, dryings, to change with glass cleaner, deionized water, acetone, methanol successively
The wellability and cleanliness factor on kind FTO surfaces.0.8M lead chloride and 2.4M carbonamidine iodine mixed solution are configured in DMF,
70 DEG C of stirrings are to being completely dissolved, on blade coating to substrate of glass, then with 150 DEG C of drying hot-air in the 5cm directly over glass
Distance at, quickly dry up solvent, obtain dark-brown perovskite thin film.
Example IV
It is cleaned by ultrasonic PET flexible substrates, after drying, configures 0.8M lead iodide and 0.8M methylamine iodine mixed solution in DMF
In, it is stirred at room temperature to being completely dissolved, on blade coating to PET base, then with 100 DEG C of drying hot nitrogen apart from PET bases
Bottom 10cm distance, quickly dries up solvent, obtains dark-brown perovskite thin film.
It should be noted that the purpose for publicizing and implementing example is that help further understands the present invention, but those skilled in the art
It is appreciated that：Do not departing from the present invention and spirit and scope of the appended claims, various substitutions and modifications are all possible.
Therefore, the present invention should not be limited to embodiment disclosure of that, and the scope of protection of present invention is defined with claims
Scope is defined.
Claims (10)
1. a kind of fast preparation method of perovskite thin film, rapid growth of crystal is realized using hot gas seasoning, prepare flat
Whole fine and close high-quality perovskite thin film, comprises the following steps：
1) mixed solution of lead-containing materials and organic halogen is prepared, perovskite precursor liquid is used as；The perovskite precursor liquid is thermosol
Liquid or cold soln；The temperature of the hot solution is 35 DEG C~120 DEG C；The temperature of the cold soln is 20 DEG C~30 DEG C；
2) by deposition process by step 1) the perovskite precursor liquid is deposited in substrate；The substrate include flexible substrates or
Rigid basement；
3) step 2 is quickly dried up using dry hot gas) the perovskite forerunner being deposited in flexible substrates or rigid basement
Liquid, forms smooth fine and close perovskite thin film.
2. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, step 1) lead-containing materials are
Lead acetate, lead oxide, lead hydroxide, lead sulfate, ceruse, plumbi nitras, (secondary) lead phosphate, lead chloride, lead iodide, bromine
Change at least one of lead；Organic halogen be methylamine iodine, carbonamidine iodine, methylamine bromine, carbonamidine bromine, methylamine chlorine, carbonamidine chlorine in extremely
Few one kind.
3. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, step 1) the perovskite forerunner
The solvent of liquid include N,N-dimethylformamide, dimethyl sulfoxide (DMSO), gamma-butyrolacton, 1-METHYLPYRROLIDONE, isopropanol, methanol,
One or more in ethanol, two-methyl cellosolve, two-ethoxy ethanol, chloroform, toluene, chlorobenzene and dichloro-benzenes.
4. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, in step 1) before the perovskite
Drive in liquid in incorporation water, hydrochloric acid, hydroiodic acid, phosphoric acid, hypophosphorous acid, acetic acid, cesium chloride, cesium bromide, cesium iodide, cesium carbonate
One or more be used as additive.
5. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, step 2) substrate is in deposition
It can be heat-treated in advance before；The flexible substrates are PET (PET), PEN
Or PEI (PEI) (PEN)；The rigid basement is ito transparent electrode, FTO transparency electrodes, metal nanometer line
/ oxide mixed transparent electrode, oxide/metal/oxide multilevel hierarchy transparency electrode, alloy, metal electrode and carbon material,
At least one of white glass；The deposition process is included in slot coated, silk-screen printing, printing, spraying, blade coating and spin coating
It is one or more.
6. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, in step 2) described pass through deposition
Before perovskite precursor liquid is deposited in substrate by method, first in upper surface of substrate deposition of titanium oxide, zinc oxide, poly- 3,4- second
Support dioxy thiophene：Poly styrene sulfonate, zinc-tin oxide, tin ash, poly- [double (4- phenyl) (4- butyl phenyls) amine, 4- butyl-N, N-
Diphenyl aniline homopolymer, polyvinylcarbazole, metal phthalein mountain valley with clumps of trees and bamboo molecular material, fullerene, graphene, nickel oxide, five oxidations two
Vanadium, copper rhodanide, cuprous iodide, zinc sulphide, molybdenum disulfide, chromium oxide, molybdenum oxide, fullerene derivate, 2,2', 7,7'-
The fluorenes of four [N, N- bis- (4- methoxyphenyls) amino] -9,9'- spiral shells two, poly- [double (4- phenyl) (2,4,6- trimethylphenyls) amine], 2,3,5,6-
One or more in the cyanogen dimethyl-parabenzoquinone of four fluoro- 7,7', 8,8'- tetra-.
7. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, step 3) drying hot gas
Body includes argon gas, nitrogen, oxygen, the one or more dried in hot-air.
8. the fast preparation method of perovskite thin film as claimed in claim 1, it is characterized in that, in step 3) the formation calcium titanium
After ore deposit film, 50 DEG C~150 DEG C of 1~120min of thermal anneal process is carried out to the perovskite thin film of formation.
9. the perovskite thin film that the fast preparation method of perovskite thin film described in a kind of utilization claim 1 is prepared.
10. the perovskite thin film that the fast preparation method using perovskite thin film described in claim 1 is prepared is applied to too
It is positive can battery, light emitting diode, photodiode, laser, thin film transistor (TFT), the system of photodetector or micro sensing device
It is standby.
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