CN110205678A - A kind of preparation method of carbon paper load organic and inorganic perovskite crystallite - Google Patents
A kind of preparation method of carbon paper load organic and inorganic perovskite crystallite Download PDFInfo
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- CN110205678A CN110205678A CN201910299043.7A CN201910299043A CN110205678A CN 110205678 A CN110205678 A CN 110205678A CN 201910299043 A CN201910299043 A CN 201910299043A CN 110205678 A CN110205678 A CN 110205678A
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- carbon paper
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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
- C30B29/54—Organic compounds
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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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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 present invention relates to a kind of preparation methods of carbon paper load organic and inorganic perovskite crystallite.The method comprising the steps of: carbon paper being surface-treated to improve surface hydrophilic state;Raw material A, raw material B are mixed and are dissolved in solvent, sealing stirring forms uniformly clear precursor solution, and the raw material A is PbX2, raw material B is CH3NH3X, wherein X=Cl, any one of Br and I;It is sealed being fitted into container together with carbon paper after precursor solution filtering, the carbon paper is placed in precursor solution;The container is put into heating device, steps up heating temperature to keeping the temperature after 50-100 DEG C;The carbon paper for loading organic and inorganic perovskite crystallite is taken out from precursor solution, remained on surface solution is sucked with filter paper, completes preparation.The present invention can prepare the organic and inorganic perovskite monocrystal material that carbon paper loads in lower temperature.Present device is simple, and simple process has broad application prospects.
Description
Technical field
The invention belongs to field of photoelectric material preparation, are specifically related to a kind of carbon paper load organic and inorganic perovskite crystallite
Preparation method.
Background technique
Organic and inorganic perovskite material by its good photoelectric properties be widely used in solar battery, photodetection,
The fields such as laser.In addition to nano materials and knots such as the organic and inorganic perovskite nano wire, the quantum dots that prepare various structures and component
Outside the high large scale perovskite monocrystalline of crystalloid amount, it is always current for how preparing uniform, fine and close and big crystallite dimension film
Research hotspot, it is also extremely important to the realization of its photoelectric functional.At present can use a step solution spin-coating method, two-step method,
Vapour deposition method etc. prepares organic and inorganic perovskite thin film material in ITO (tin indium oxide) glass, FTO (fluorine oxide tin) glass etc.
On substrate.One step solution spin-coating method be by organic and inorganic perovskite precursor solution spin-on deposition on substrate, then by plus
Heat promotes conversion of the presoma to perovskite crystal, and solvent volatilization and the process of perovskite crystallization carry out simultaneously.Two-step method will revolve
It is painted with PbX2Substrate be immersed in CH3NH3It takes out, then passes through after a period of time in X (any one of X=Cl, Br and I) solution
Heating promotes the crystallization of perovskite.Since the reaction time is short, solvent volatilization rapidly, causes perovskite crystal size uneven, thin
Residual pin hole is easy in film.The different method of many research and utilizations obtains the cause without hole turtle shell shape being made of big crystal grain at present
Close film.Vapour deposition method is by CH3NH3X and PbX2It is steamed altogether by double source or the method for alternating deposit is deposited on substrate acquisition crystalline substance
Change good and high coverage rate perovskite thin film, but needs using expensive vacuum equipment.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of preparations of carbon paper load organic and inorganic perovskite crystallite
Method.
In order to achieve the object of the present invention, the invention adopts the following technical scheme:
A kind of preparation method of carbon paper load organic and inorganic perovskite crystallite, comprising the following steps:
Step 1: carbon paper being surface-treated to improve surface hydrophilic state;
Step 2: raw material A, raw material B being mixed and are dissolved in solvent, sealing stirring forms uniformly clear precursor solution;Institute
Stating raw material A is PbX2, raw material B is CH3NH3X, wherein X=Cl, any one of Br and I;
Step 3: being sealed being fitted into container together with carbon paper after precursor solution filtering, the carbon paper is placed in forerunner
In liquid solution;
Step 4: the container being put into heating device, steps up heating temperature to keeping the temperature after 50-100 DEG C;
Step 5: the carbon paper for loading organic and inorganic perovskite crystallite being taken out from precursor solution, sucks table with filter paper
Face residual solution completes preparation.
Further technical solution: surface treatment method described in step 1 includes being impregnated or being heat-treated using strong acid.
Further technical solution: solvent described in step 2 is n,N-Dimethylformamide or gamma-butyrolacton.
Further technical solution: the molar ratio of raw material A described in step 2 and raw material B are 1:(1-1.3).
Further technical solution: the heating rate of heating device described in step 4 is 2-5 DEG C/day.
Further technical solution: the time of heat preservation described in step 4 is 2-5 days.
The beneficial effects of the present invention are:
(1) present invention can prepare the organic and inorganic perovskite list that carbon paper loads in lower temperature (being lower than 100 DEG C)
Brilliant material.Present device is simple, simple process.Carbon paper of the present invention is cheap and resistance very little flexible substrate,
Organic and inorganic perovskite material with excellent photoelectric properties is supported on carbon paper, so as to by organic and inorganic perovskite
The electronics that material generates under the environment such as illumination quickly exports, therefore has broad application prospects.
(2) present invention first by carbon paper lead to peracid treatment or heating so that its surface is modified to hydrophily after, be put into and match
In the organic and inorganic perovskite growth solution set.Utilize solubility of the organic and inorganic perovskite material in specific solvent
With temperature raising, its forming core crystallization on carbon paper fiber is precipitated in reduced principle, final uniform load to high conductivity flexibility
On carbon paper.By slowly heating up and final insulating process, the growth of organic and inorganic perovskite crystallite can be effectively controlled, no
Appear in the case where certain a large amount of precipitations in place cause accumulation and certain local crystallite undue growths on carbon paper fiber.It utilizes
Organic and inorganic perovskite crystallite prepared by the present invention and carbon paper binding force are strong, and have biggish surface area, good electric conductivity
And the advantages that stability.
(3) present invention realize on carbon paper payload size uniformly, without the organic and inorganic perovskite crystallite obviously reunited.Benefit
Organic and inorganic perovskite material is loaded on the carbon paper of high conductivity with method described in the invention, can effectively expand it
Application in the photoelectric devices such as solar cell, sensor, detector.
Detailed description of the invention
Fig. 1 is carbon paper load organic and inorganic perovskite crystallite preparation method schematic diagram provided by the invention.
Fig. 2 is carbon paper load C H3NH3PbBr3The electron scanning micrograph (embodiment 1) of crystallite.
Fig. 3 is carbon paper load C H3NH3PbBr3The X-ray diffraction result (embodiment 2) of crystallite.
Specific embodiment
It makes below with reference to preparation method of the embodiment to carbon paper of the present invention load organic and inorganic perovskite crystallite and more having
The explanation of body:
Embodiment 1
Step 1: by carbon paper in sulfuric acid (98%) and nitric acid (65%) mixed solution (volume ratio 3:1), 60 DEG C of immersions 1 are small
When to improve surface hydrophilic state;
Step 2: raw material A, raw material B being mixed and are dissolved in solvent gamma-butyrolacton, sealing stirring forms uniformly clarification for 12 hours
Precursor solution;The raw material A is PbBr2, raw material B is CH3NH3The molar ratio of Br, raw material A and raw material B are 1:1;
Step 3: the precursor solution is fitted into container together with carbon paper using after polytetrafluoroethylene filter filtering
Sealing, the carbon paper are placed in precursor solution;
Step 4: the container is put into heating device (baking oven or thermal station), with the heating rate of 2 DEG C/day from room temperature by
Step improves heating temperature to keeping the temperature 3 days after 60 DEG C;During heating as temperature is gradually increased, organic and inorganic perovskite is micro-
Crystalline substance is gradually precipitated on carbon paper, grows up;
Step 5: organic and inorganic perovskite material CH will be loaded3NH3PbBr3The carbon paper of crystallite takes from precursor solution
Out, remained on surface solution is sucked with filter paper, completes preparation.
Embodiment 2
Step 1: carbon paper handle 16 hours for 400 DEG C in air, to improve surface hydrophilic state;
Step 2: raw material A, raw material B being mixed and are dissolved in solvent gamma-butyrolacton, sealing stirring forms uniformly clarification for 12 hours
Precursor solution;The raw material A is PbBr2, raw material B is CH3NH3The molar ratio of Br, raw material A and raw material B are 1:1;
Step 3: the precursor solution is fitted into container together with carbon paper using after polytetrafluoroethylene filter filtering
Sealing, the carbon paper are placed in precursor solution;
Step 4: the container is put into heating device (baking oven or thermal station), with the heating rate of 2 DEG C/day from room temperature by
Step improves heating temperature to keeping the temperature 2 days after 60 DEG C;
Step 5: by load C H3NH3PbBr3The carbon paper of crystallite takes out from precursor solution, sucks remained on surface with filter paper
Solution completes preparation.
Embodiment 3
Step 1: by carbon paper in sulfuric acid (98%) and nitric acid (65%) mixed solution (volume ratio 3:1), 60 DEG C of immersions 1 are small
When to improve surface hydrophilic state;
Step 2: raw material A, raw material B being mixed and are dissolved in solvent gamma-butyrolacton, sealing stirring forms uniformly clarification for 12 hours
Precursor solution;The raw material A is PbCl2, raw material B is CH3NH3The molar ratio of Cl, raw material A and raw material B are 1:1.3;
Step 3: the precursor solution is fitted into container together with carbon paper using after polytetrafluoroethylene filter filtering
Sealing, the carbon paper are placed in precursor solution;
Step 4: the container is put into heating device (baking oven or thermal station), with the heating rate of 5 DEG C/day from room temperature by
Step improves heating temperature to keeping the temperature 5 days after 50 DEG C;During heating as temperature is gradually increased, organic and inorganic perovskite is micro-
Crystalline substance is gradually precipitated on carbon paper, grows up;
Step 5: by load C H3NH3PbCl3The carbon paper of crystallite takes out from precursor solution, sucks remained on surface with filter paper
Solution completes preparation.
Embodiment 4
Step 1: by carbon paper in sulfuric acid (98%) and nitric acid (65%) mixed solution (volume ratio 3:1), 60 DEG C of immersions 1 are small
When to improve surface hydrophilic state;
Step 2: raw material A, raw material B being mixed and are dissolved in solvent n,N-Dimethylformamide, sealing stirring is formed for 12 hours
Uniform clear precursor solution;The raw material A is PbI2, raw material B is CH3NH3The molar ratio of I, raw material A and raw material B are 1:
1.2;
Step 3: the precursor solution is fitted into container together with carbon paper using after polytetrafluoroethylene filter filtering
Sealing, the carbon paper are placed in precursor solution;
Step 4: the container is put into heating device (baking oven or thermal station), with the heating rate of 3 DEG C/day from room temperature by
Step improves heating temperature to keeping the temperature 4 days after 100 DEG C;During heating as temperature is gradually increased, organic and inorganic perovskite is micro-
Crystalline substance is gradually precipitated on carbon paper, grows up;
Step 5: by load C H3NH3PbI3The carbon paper of crystallite takes out from precursor solution, sucks remained on surface with filter paper
Solution completes preparation.
Sample after loading organic and inorganic perovskite crystallite to carbon paper carries out the observation of surface sweeping Electronic Speculum, finds in carbon paper fiber
It grown the largely organic and inorganic perovskite crystallite (Fig. 2) having a size of 5-15 microns between upper and fiber, reached uniform load
Purpose.
Claims (6)
1. a kind of preparation method of carbon paper load organic and inorganic perovskite crystallite, it is characterised in that the following steps are included:
Step 1: carbon paper being surface-treated to improve surface hydrophilic state;
Step 2: raw material A, raw material B being mixed and are dissolved in solvent, sealing stirring forms uniformly clear precursor solution;The original
Material A is PbX2, raw material B is CH3NH3X, wherein X=Cl, any one of Br and I;
Step 3: being sealed being fitted into container together with carbon paper after precursor solution filtering, it is molten that the carbon paper is placed in presoma
In liquid;
Step 4: the container being put into heating device, steps up heating temperature to keeping the temperature after 50-100 DEG C;
Step 5: the carbon paper for loading organic and inorganic perovskite crystallite being taken out from precursor solution, it is residual to suck surface with filter paper
Solution is stayed, preparation is completed.
2. the preparation method of carbon paper load organic and inorganic perovskite crystallite as described in claim 1, it is characterised in that: step 1
Described in surface treatment method include using strong acid impregnate or be heat-treated.
3. the preparation method of carbon paper load organic and inorganic perovskite crystallite as described in claim 1, it is characterised in that: step 2
Described in solvent be n,N-Dimethylformamide or gamma-butyrolacton.
4. the preparation method of carbon paper load organic and inorganic perovskite crystallite as described in claim 1, it is characterised in that: step 2
Described in the molar ratio of raw material A and raw material B be 1:(1-1.3).
5. the preparation method of carbon paper load organic and inorganic perovskite crystallite as described in claim 1, it is characterised in that: step 4
Described in heating device heating rate be 2-5 DEG C/day.
6. the preparation method of carbon paper load organic and inorganic perovskite crystallite as described in claim 1, it is characterised in that: step 4
Described in heat preservation time be 2-5 days.
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Application publication date: 20190906 |