CN110512271A - A kind of perovskite and its preparation method and application of knitmesh shape - Google Patents
A kind of perovskite and its preparation method and application of knitmesh shape Download PDFInfo
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- CN110512271A CN110512271A CN201910624894.4A CN201910624894A CN110512271A CN 110512271 A CN110512271 A CN 110512271A CN 201910624894 A CN201910624894 A CN 201910624894A CN 110512271 A CN110512271 A CN 110512271A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/20—Changing the shape of the active layer in the devices, e.g. patterning
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The invention belongs to perovskite material technical fields, disclose a kind of perovskite and its preparation method and application of knitmesh shape.This method is that FABr and PbBr is added in solvent, is configured to the precursor liquid of 0.5mol/L~3mol/L, then is added dropwise in FTO Conducting Glass after precursor liquid is diluted 10~30 times, then toluene is added dropwise, and perovskite monocrystalline is prepared in drying；Gained perovskite monocrystalline is soaked in 5~30min in cobalt iso-octoate solution again, sample is then put into drying box drying, finally obtains the perovskite of knitmesh shape.This method uses anti-solvent method, prepares perovskite monocrystalline, and recycling isopropanol is that the cobalt iso-octoate solution of solvent produces knitmesh shape perovskite.The perovskite material can be applicable in area of solar cell.
Description
Technical field
The invention belongs to perovskite material preparation technical field, in particular to the perovskite of a kind of knitmesh shape and its preparation side
Method and application.
Background technique
In recent years, energy crisis became people's major issue urgently to be resolved.Because perovskite material shows uniqueness
Performance, make its solar battery preparation be filled with new vitality.This stern challenge especially is converted in face of solar energy,
This green energy resource of sunlight can be absorbed and utilized to effectively improve the efficiency of solar battery in perovskite material, so that exploitation ratio
The perovskite material that surface area is big, stability is high, optical response range is wide becomes the important content studied instantly.
Perovskite is a kind of functional material with excellent optically and electrically performance, in solar battery, light-emitting diodes
Pipe, the fields such as micro- laser are with a wide range of applications.Metal halide perovskite (MHP) material is due to its excellent photo electric
Matter was quickly grown in photoelectric field in recent years.And FABrBr3It is a kind of current very popular organic and inorganic perovskite material,
Since it is with good light absorpting ability, in a variety of necks such as gas sensor, gas sensor, electrode material and solar battery
Domain has broad application prospects.However as people to FABrBr3Further research, it is found that it is also a kind of good light
Catalyst, more and more people apply it to photocatalysis field.Photocatalysis is in the ultraviolet lighting with higher-energy
Penetrate what lower excitation generated, but due to FABrBr3The specific surface area of monocrystalline is smaller, and the active site that can participate in reaction is less,
So photocatalysis efficiency is limited.In addition, since the photo-generate electron-hole for playing key effect during light-catalysed is to shakiness
Fixed and be easy to compound, which also limits FABrBr3The performance of photocatalysis.Therefore, in order to preferably play FABrBr3In
Effect in photocatalysis field must just solve the problems, such as two aspects: (1) increasing material specific surface area；(2) photoproduction electricity is reduced
Son-hole pair recombination rate.
Summary of the invention
In order to overcome shortcoming and deficiency existing in the prior art, the primary purpose of the present invention is that providing a kind of knitmesh shape
Perovskite preparation method；This method is specifically to use solvent-thermal process method to prepare monocrystalline perovskite material, then made
The perovskite of standby knitmesh shape out, this method preparation process are simple and low in cost.
Another object of the present invention is to provide a kind of perovskite of knitmesh shape that above-mentioned preparation method is prepared.
A further object of the present invention is to provide a kind of applications of the perovskite of above-mentioned knitmesh shape.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the perovskite of knitmesh shape, including following operating procedure: FABr and PbBr is added in solvent,
It is configured to the precursor liquid of 0.5mol/L~3mol/L, then is added dropwise after precursor liquid is diluted 10~30 times in FTO Conducting Glass
On, then toluene is added dropwise, perovskite monocrystalline is prepared in drying；Gained perovskite monocrystalline is soaked in 5 in cobalt iso-octoate solution again~
Then sample is put into drying box drying, finally obtains the perovskite of knitmesh shape by 30min.
The FTO Conducting Glass is cleaned before the use: FTO electro-conductive glass is put into Piranha solution leaching
Then bubble is added deionized water and is diluted to neutrality, obtains clean FTO Conducting Glass.
The time of the immersion is 8~12h；The Piranha solution is the mixture of the concentrated sulfuric acid and 30% hydrogen peroxide.
The solvent is DMF.
The cobalt iso-octoate solution is the solution for being configured to concentration by solvent of isopropanol as 5mmol~50mmol.
It is described will precursor liquid dilute 10~30 times after 1~30ul is added dropwise in FTO Conducting Glass, then be added dropwise 0.5~
1ml toluene is put into 20~50 DEG C of baking oven drying, prepares perovskite monocrystalline.
The time of the drying is 1~3h, and the temperature of drying is 30~60 DEG C.
A kind of perovskite for the knitmesh shape being prepared according to above-mentioned preparation method.
Application of the perovskite of above-mentioned knitmesh shape in area of solar cell.
The present invention increases its specific surface area, increases the active sites for participating in reaction by preparing the perovskite of knitmesh shape
Point shortens the migration road warp of carrier, reduces hole and electronics is compound, to increase the electrons and holes for participating in reaction
Quantity improves reaction rate.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) present invention uses anti-solvent method, and using DMF as solvent, FABr and PbBr is added, reaction precursor liquid is configured, in FTO
On prepare perovskite monocrystalline, then FTO is soaked in cobalt iso-octoate solution, obtains the perovskite of knitmesh shape.
(2) perovskite for the knitmesh shape that the present invention synthesizes increases specific surface area, can effectively improve the service life of carrier,
Improve the performance of material.
(3) equipment and preparation process needed for the present invention are simple, low in cost, can directly produce in enormous quantities.
Detailed description of the invention
Fig. 1 is what the perovskite of the knitmesh shape prepared in embodiment 1 was observed under 1200 times of scanning electron microscope
Surface SEM photograph.
Fig. 2 is the table that the perovskite of knitmesh shape prepared by embodiment 1 is observed under 3000 times of scanning electron microscope
Face SEM photograph.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Piranha solution used in the following embodiment is the mixture of the concentrated sulfuric acid and 30% hydrogen peroxide.
Embodiment 1
The cleaning of 1.FTO Conducting Glass: by FTO electro-conductive glass be put into Piranha solution impregnate, then be added go from
Sub- water is diluted to neutrality, obtains clean FTO Conducting Glass；
2. FABr and PbBr is added in DMF solvent and configures reaction precursor liquid, it is configured to the precursor liquid of 3mol/L；
3. above-mentioned precursor liquid is diluted 30 times using DMF as solvent；
4. the precursor liquid after above-mentioned dilution is added dropwise on 30ul to clean FTO Conducting Glass conducting surface, then will
The toluene of 0.5ml is added drop-wise in FTO Conducting Glass, is put into 50 DEG C of baking oven drying, is obtained perovskite monocrystalline；
5. preparing the cobalt iso-octoate solution of 50mml using isopropanol as solvent, perovskite monocrystalline obtained above is immersed in
30min in cobalt iso-octoate solution places into 60 DEG C of drying 1h of baking oven, obtains the perovskite of knitmesh shape.
Fig. 1 is the SEM photograph of the perovskite of knitmesh shape manufactured in the present embodiment.As can be known from Fig. 1, in 1200 times of scanning
Observed under electron microscope to perovskite single-crystal surface have knitmesh shape.Fig. 2 is the perovskite of knitmesh shape manufactured in the present embodiment
Surface SEM photograph.As shown in Figure 2, the orderly knitmesh shape perovskite observed under 3000 times of scanning electron microscope.
Embodiment 2
The cleaning of 1.FTO Conducting Glass: by FTO electro-conductive glass be put into Piranha solution impregnate, then be added go from
Sub- water is diluted to neutrality, obtains clean FTO Conducting Glass；
2. FABr and PbBr is added in DMF solvent and configures reaction precursor liquid, it is configured to the precursor liquid of 1mol/L；
3. above-mentioned precursor liquid is diluted 30 times using DMF as solvent；
4. the precursor liquid after above-mentioned dilution is added dropwise on 30ul to clean FTO Conducting Glass conducting surface, then will
The toluene of 0.5ml is added drop-wise in FTO Conducting Glass, is put into 50 DEG C of baking oven drying, is obtained perovskite monocrystalline；
5. preparing the cobalt iso-octoate solution of 50mml using isopropanol as solvent, perovskite monocrystalline obtained above is immersed in
30min in cobalt iso-octoate solution places into 60 DEG C of drying 1h of baking oven, obtains the perovskite of knitmesh shape.Products obtained therefrom is at 1200 times
Scanning electron microscope under the perovskite single-crystal surface observed have knitmesh shape.
Embodiment 3
The cleaning of 1.FTO Conducting Glass: by FTO electro-conductive glass be put into Piranha solution impregnate, then be added go from
Sub- water is diluted to neutrality, obtains clean FTO Conducting Glass；
2. FABr and PbBr is added in DMF solvent and configures reaction precursor liquid, it is configured to the precursor liquid of 3mol/L；
3. above-mentioned precursor liquid is diluted 10 times using DMF as solvent；
4. the precursor liquid after above-mentioned dilution is added dropwise on 30ul to clean FTO Conducting Glass conducting surface, then will
The toluene of 0.5ml is added drop-wise in FTO Conducting Glass, is put into 50 DEG C of baking oven drying, is obtained perovskite monocrystalline；
5. preparing the cobalt iso-octoate solution of 50mml using isopropanol as solvent, perovskite monocrystalline obtained above is immersed in
30min in cobalt iso-octoate solution places into 60 DEG C of drying 1h of baking oven, obtains the perovskite of knitmesh shape.Products obtained therefrom is at 1200 times
Scanning electron microscope under the perovskite single-crystal surface observed have knitmesh shape.
Embodiment 4
The cleaning of 1.FTO Conducting Glass: by FTO electro-conductive glass be put into Piranha solution impregnate, then be added go from
Sub- water is diluted to neutrality, obtains clean FTO Conducting Glass；
2. FABr and PbBr is added in DMF solvent and configures reaction precursor liquid, it is configured to the precursor liquid of 1mol/L；
3. above-mentioned precursor liquid is diluted 10 times using DMF as solvent；
4. the precursor liquid after above-mentioned dilution is added dropwise on 30ul to clean FTO Conducting Glass conducting surface, then will
The toluene of 0.5ml is added drop-wise in FTO Conducting Glass, is put into 50 DEG C of baking oven drying, is obtained perovskite monocrystalline；
Using isopropanol as solvent, cobalt iso-octoate is configured to the precursor liquid of 50mml, perovskite monocrystalline obtained above is soaked
Bubble 30min in cobalt iso-octoate precursor liquid, places into 60 DEG C of drying 1h of baking oven, obtains the perovskite of knitmesh shape.Products obtained therefrom exists
The perovskite single-crystal surface observed under 1200 times of scanning electron microscope has knitmesh shape.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of the perovskite of knitmesh shape, it is characterised in that including following operating procedure: FABr and PbBr are added
Enter in solvent, be configured to the precursor liquid of 0.5mol/L~3mol/L, then is added dropwise after precursor liquid is diluted 10~30 times in FTO conduction
In glass substrate, then toluene is added dropwise, perovskite monocrystalline is prepared in drying；It is molten that gained perovskite monocrystalline is soaked in cobalt iso-octoate again
Then sample is put into drying box drying, finally obtains the perovskite of knitmesh shape by 5~30min in liquid.
2. preparation method according to claim 1, it is characterised in that: the FTO Conducting Glass before the use into
Row cleaning: being put into Piranha solution for FTO electro-conductive glass and impregnate, and deionized water is then added and is diluted to neutrality, obtains clean
FTO Conducting Glass.
3. preparation method according to claim 2, it is characterised in that: the time of the immersion is 8~12h；The anthropophagy
Fish solution is the mixture of the concentrated sulfuric acid and 30% hydrogen peroxide.
4. preparation method according to claim 1, it is characterised in that: the solvent is DMF.
5. preparation method according to claim 1, it is characterised in that: the cobalt iso-octoate solution is using isopropanol as solvent
It is configured to the solution that concentration is 5mmol~50mmol.
6. preparation method according to claim 1, it is characterised in that: described to be added dropwise 1 after 10~30 times of precursor liquid dilution
~30ul is in FTO Conducting Glass, then 0.5~1ml toluene is added dropwise, and is put into 20~50 DEG C of baking oven drying, prepares calcium titanium
Mine monocrystalline.
7. preparation method according to claim 1, it is characterised in that: the time of the drying is 1~3h, the temperature of drying
It is 30~60 DEG C.
8. a kind of perovskite for the knitmesh shape that preparation methods described in any item according to claim 1~7 are prepared.
9. application of the perovskite of knitmesh shape according to claim 8 in area of solar cell.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106356456A (en) * | 2016-10-17 | 2017-01-25 | 北京科技大学 | Solar cell based on high-quality perovskite heterojunctions and preparation method thereof |
| US20170152608A1 (en) * | 2015-11-30 | 2017-06-01 | Wisconsin Alumni Research Foundation | Solution growth of single-crystal perovskite structures |
| CN109545970A (en) * | 2018-12-24 | 2019-03-29 | 南京工业大学 | A kind of method and perovskite solar battery improving perovskite solar battery efficiency and stability |
| CN109768163A (en) * | 2018-12-07 | 2019-05-17 | 南京邮电大学 | A kind of TiO2/ CdS perovskite solar battery and preparation method |
-
2019
- 2019-07-11 CN CN201910624894.4A patent/CN110512271B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170152608A1 (en) * | 2015-11-30 | 2017-06-01 | Wisconsin Alumni Research Foundation | Solution growth of single-crystal perovskite structures |
| CN106356456A (en) * | 2016-10-17 | 2017-01-25 | 北京科技大学 | Solar cell based on high-quality perovskite heterojunctions and preparation method thereof |
| CN109768163A (en) * | 2018-12-07 | 2019-05-17 | 南京邮电大学 | A kind of TiO2/ CdS perovskite solar battery and preparation method |
| CN109545970A (en) * | 2018-12-24 | 2019-03-29 | 南京工业大学 | A kind of method and perovskite solar battery improving perovskite solar battery efficiency and stability |
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