CN107915496A - A kind of preparation method of large-area two-dimensional organic-inorganic perovskite thin film - Google Patents
A kind of preparation method of large-area two-dimensional organic-inorganic perovskite thin film Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 150000004820 halides Chemical class 0.000 claims abstract description 17
- QEZYDNSACGFLIC-UHFFFAOYSA-N CN.[I] Chemical compound CN.[I] QEZYDNSACGFLIC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 19
- 239000012159 carrier gas Substances 0.000 claims description 10
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000010445 mica Substances 0.000 claims description 6
- 229910052618 mica group Inorganic materials 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 241001062009 Indigofera Species 0.000 claims 1
- 239000010437 gem Substances 0.000 claims 1
- 229910001751 gemstone Inorganic materials 0.000 claims 1
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 10
- 230000005693 optoelectronics Effects 0.000 abstract description 4
- 238000011144 upstream manufacturing Methods 0.000 abstract description 4
- 238000000151 deposition Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000007704 wet chemistry method Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052594 sapphire Inorganic materials 0.000 description 3
- 239000010980 sapphire Substances 0.000 description 3
- 238000004630 atomic force microscopy Methods 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 208000035126 Facies Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000003334 potential effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
- C04B41/61—Coating or impregnation
- C04B41/62—Coating or impregnation with organic materials
- C04B41/64—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
Abstract
The invention discloses a kind of preparation method of large-area two-dimensional organic-inorganic perovskite thin film, first according to mass ratio by lead halide powder, iodine methylamine powder is sequentially placed into target substrate upstream, then deposition gases are thermally formed respectively, it is deposited on substrate, pass through the present invention, the high large area perovskite thin film of mass is grown in different growth substrates using a step chemical vapour deposition technique, with quality height, area is big, it is reproducible, the features such as can largely preparing, the research applied for the basic research of New Two Dimensional nano material and the potentiality of related two-dimensional nano opto-electronic device provides the reliable means of sample preparation.
Description
Technical field
The present invention relates to the technology of preparing of two-dimentional organic and inorganic perovskite thin film, be specially a kind of large-area two-dimensional it is organic-
The preparation method of inorganic perovskite thin film.
Background technology
In recent years, one of hybrid inorganic-organic perovskite material most potential as photovoltaic art, receives increasingly
Extensive concern.Within the 7 short years, the energy conversion efficiency of perovskite solar cell is brought up to from 3.8%
22.1%, and achievement in research of the solar cell after decades is commercialized more than polysilicon etc., this is in energy photoelectric field
It is unprecedented.At the same time, since exciton bind energy is small, carrier diffusion distance, fluorescence quantum yield is high, and broadband is inhaled
The features such as receipts, perovskite material equally achieve preliminary progress in the information such as high-performance optical detector field of optoelectronic devices.Calcium
The excellent photoelectric properties of titanium ore material and the breakthrough in optoelectronic device applications field, accelerate the research of its two dimensionization into
Journey.Based on this, find suitable preparation process and obtain the excellent two-dimentional perovskite nano material of photoelectric property, and using it as load
Body, come study physics, optics, electricity, device application etc. property feature, no matter for perovskite material field basis
Research, or exploitation high-performance optical sensitive detection parts, all with particularly important meaning.However, perovskite material as it is a kind of from
Sub- crystal, the two dimension Van der Waals force stratified material such as it and graphene, TMDs, black phosphorus have fundamental difference.Based on this, prepared by tradition
Large area, the maturation method of high-quality two-dimensional layer material are not fully suitable for the preparation of two-dimentional perovskite material, develop
New preparation method is imperative.
At this stage, researcher can pass through wet chemistry method, two step chemical vapour deposition techniques or wet-chemical and chemical gas
The method that phase sedimentary facies combines, obtains component, the two-dimentional perovskite material of thickness change.
Method one：Using (the C of wet chemistry method synthesis atomic-level thickness, lateral dimension at 5 μm or so4H9NH3)2PbBr4Calcium
Perovskite like structure [Science 2015,349 (6255), 1518-1521.].Specifically, by very small amount of (C4H9NH3)2PbBr4Solid is dissolved in dimethylformamide and chlorobenzene solvent, is then added dropwise in Si/SiO2In substrate, 70 DEG C of 10 points of dryings
Clock, obtains ultra-thin (C4H9NH3)2PbBr4.The shortcomings that this method, is that its lateral dimension is generally limited within 5 μm, same with this
When, wet chemistry method limits the accurate control to crystal quality and thickness in preparation process.Therefore, the two dimension that this method is prepared
Perovskite material has application limitation.
Method two：Using two step chemical vapour deposition techniques [Adv.Opt.Mater., 2014,2,838-844.] or humidifying
Learn the method [ACS Nano, 2016,10,3536-3542.] being combined with chemical vapor deposition and go out two-dimentional calcium in grown on substrates
Perovskite like structure.Specifically, the first step obtains wet chemistry method using chemical vapour deposition technique and prepares two-dimentional lead halide presoma, by
In the two-dimensional layered structure attribute of presoma lead halide, its thickness change is easy to regulate and control, so that the thickness of two-dimentional perovskite
Regulation and control are achieved.Second step, using chemical vapour deposition technique by the organic steams such as iodine methylamine and preamble two dimension lead halide forerunner
Precursor reactant, realizes conversion of the lead halide to perovskite material.The shortcomings that this method, is, difficult since chemical reaction substep carries out
In the large area deposition for realizing two-dimentional perovskite material, its lateral dimension is generally limited within 20 μm.
For two-dimensional material, realizing prepared by high-quality, large area and the controllable material of thickness is expanded in device
The precondition of application.In consideration of it, continuing to optimize or develop technology of preparing, large area, uniformly two-dimentional organic and inorganic calcium titanium are realized
The controllable preparation of ore deposit film is a major challenge in current flow of research.In the present invention, we utilize a step chemical vapor deposition
Area method (silicon/oxidative silicon, mica, sapphire) on appropriate substrate, passes through forerunner's weight, growth temperature, growth time, load
Throughput, ceramic boat spacing and air pressure etc. regulate and control, and prepare large area (lateral dimension is in grade), thickness uniform, controllable (20
Nanometer is following) two-dimentional perovskite thin film material.
The content of the invention
The technical problems to be solved by the invention are to overcome the deficiencies of the prior art and provide a kind of large area, thickness equal
The preparation method of even controllable two-dimentional perovskite thin film material.This method can prepare that uniformity is good, quality is high, area is larger
Two-dimentional perovskite thin film, has the characteristics that prepared by reproducible and batch.
The present invention specifically comprises the following steps：A kind of preparation method of large-area two-dimensional organic and inorganic perovskite thin film, bag
Include following steps：
(1) the lead halide powder of 1 parts by weight, the iodine methylamine powder of 1.8~2.2 parts by weight, target substrate are sequentially placed into
In quartz ampoule, the spacing of iodine methylamine powder and target substrate is controlled in 10-20cm；The spacing of lead halide powder and iodine methylamine powder
Control is in 5-10cm.
(2) carrier gas (argon gas or nitrogen) is passed through after sealing, it is 30-100sccm to control flow；By lead halide powder location
Domain rises to 200-250 DEG C；Iodine methylamine powder region is risen to 120-180 DEG C；Basal region is warming up to 150-180 DEG C,
Deposition obtains two-dimentional perovskite thin film material after 30-40 minutes, and vacuum tube furnace quartz intraductal atmospheric pressure is kept in whole process
Keep environment under low pressure 30-80mTorr.
Further, the selected target substrate is silicon/oxidative silicon, mica or sapphire.
The technique effect of the present invention is as follows:
(1) method of a step chemical vapor deposition of the invention successfully prepares large-area two-dimensional perovskite thin film.This method
The perovskite thin film of preparation has quality high, and area is big, reproducible, the features such as can largely preparing.
(4) fluorescence spectrum and light microscope show that this method achieves breakthrough, are existed using a step chemical vapour deposition technique
The high large area perovskite thin film of mass is grown in different growth substrates.
(3) present invention for New Two Dimensional nano material basic research and related two-dimensional nano opto-electronic device it is potential
Property application research provide the reliable means of sample preparation.
Brief description of the drawings
Fig. 1 is the grower used in the present invention.
Fig. 2 is the X-ray diffraction pattern for the two-dimentional perovskite thin film prepared in the present invention.
Fig. 3 is the optical microscope photograph for the two-dimentional perovskite thin film prepared in the present invention.
Fig. 4 is the atomic force microscopy for two perovskite thin films prepared in the present invention.
Embodiment
The present invention is expanded on further with reference to the accompanying drawings and examples, but is not therefore limited the present invention to described
Within scope of embodiments.
Embodiment 1
20mg iodine methylamine powder and 10mg lead halide powder are weighed, is individually positioned in 40 DEG C of vacuum drying chambers and preserved
3 it is small when；Growth substrates mica sheet is put into the middle position of vacuum tube furnace furnace chamber；By iodine methylamine powder uniformly dispersing in ceramics
In boat 1, the position of carrier gas upstream distance objective substrate 10cm is placed on；By lead halide powder uniformly dispersing in ceramic boat 2, put
Put in carrier gas upstream apart from the position of previous ceramic boat 5cm；Vacuum tube furnace quartz pipe flange is sealed, then passes to carrier gas (argon
Gas), kept for 30 minutes under the flow of 50sccm.Carrier gas is successively by the lead halide powder region (heating zone of most upstream
Domain 1), iodine methylamine powder region (heating region 2), growth substrates mica sheet；Then vacuum tube furnace halogenation lead powder is set
The heating rate of last region (heating region 1) is 20 DEG C/min, rises to 200 DEG C；Vacuum tube furnace iodine methylamine powder is set
The heating rate of region (heating region 2) is 10 DEG C/min, rises to 120 DEG C；The liter of vacuum tube furnace middle section is set
Warm speed is 10 DEG C/min, from room temperature to 150 DEG C of growth temperature, keeps being grown for 30 minutes under growth temperature, so
After make vacuum tube furnace cooled to room temperature, it be 30sccm that carrier gas flux is kept in whole process, and vacuum tube furnace is quartzy
Manage (a diameter of 60mm) interior air pressure and keep environment under low pressure 30mTorr, referring to Fig. 1.
The absorption of large-area two-dimensional organic inorganic hybridization perovskite thin film (No. 1 sample) prepared by embodiment 1, fluorescence light
Spectrum, optical microscope photograph and atomic force microscopy difference are as shown in Figure 2, Figure 3 and Figure 4.The results show that two-dimentional perovskite
The lateral dimension of thin-film material is 2.1 nanometers in grade, thickness.
The present embodiment has also further investigated a step chemical vapour deposition technique and has prepared large-area two-dimensional perovskite thin film process
In, can forerunner's weight, growth temperature, growth time, carrier gas flux, ceramic boat spacing and air pressure in growth course to obtain
Large-area two-dimensional perovskite thin film or the influence to sample quality.For specific implementation process with embodiment 1, difference lies in change respectively
Become forerunner's weight, growth temperature, growth time, carrier gas flux, ceramic boat spacing, air pressure, target substrate, obtain 2-23
Number product, as shown in table 1.Table 1
From the foregoing, it will be observed that must be strictly controlled the ratio of two kinds of steam, reaction temperature, intermediate is generated, then by intermediate
Deposit under suitable conditions in substrate, can just obtain two-dimentional perovskite thin film.It is specific as follows：
1. the mass ratio of iodine methylamine and lead halide is 1.8~2.2；
2. the spacing of iodine methylamine powder and target substrate is controlled in 10-20cm；Between lead halide powder and iodine methylamine powder
Away from control in 5-10cm；
3. the temperature range of lead halide powder region is 200-250 DEG C；The temperature model of iodine methylamine powder region
Enclose for 120-180 DEG C；The temperature range of target substrate region is 150-180 DEG C.Kept for 30-40 minutes under growth temperature
Grown, it is 30-100sccm that carrier gas flux is kept in whole process, and vacuum tube furnace quartz intraductal atmospheric pressure keeps low pressure
Environment 30-80mTorr；
4. target substrate is silicon/oxidative silicon, mica, sapphire.
Claims (2)
1. a kind of preparation method of large-area two-dimensional organic and inorganic perovskite thin film, it is characterised in that comprise the following steps：
(1) the lead halide powder of 1 parts by weight, the iodine methylamine powder of 1.8~2.2 parts by weight, target substrate are sequentially placed into quartz
The spacing of Guan Zhong, iodine methylamine powder and target substrate is controlled in 10-20cm；Lead halide powder and the spacing of iodine methylamine powder control
In 5-10cm.
(2) carrier gas (argon gas or nitrogen) is passed through after sealing, it is 30-100sccm to control flow；By lead halide powder region liter
To 200-250 DEG C；Iodine methylamine powder region is risen to 120-180 DEG C；Basal region is warming up to 150-180 DEG C, deposition
Two-dimentional perovskite thin film material is obtained after 30-40 minutes, keeps vacuum tube furnace quartz intraductal atmospheric pressure to keep in whole process
Environment under low pressure 30-80mTorr.
2. according to the method described in claim 1, it is characterized in that, the selected target substrate is silicon/oxidative silicon, mica or indigo plant
Jewel.
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| CN109052470A (en) * | 2018-10-15 | 2018-12-21 | 郑州大学 | A kind of inorganic non-lead caesium bismuth halogen Cs3Bi2X9Perovskite micron disk and its synthetic method |
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| CN113484341A (en) * | 2021-07-01 | 2021-10-08 | 南京工业大学 | Method for preparing TEM sample based on hybrid lead-based perovskite nanosheets |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109052470A (en) * | 2018-10-15 | 2018-12-21 | 郑州大学 | A kind of inorganic non-lead caesium bismuth halogen Cs3Bi2X9Perovskite micron disk and its synthetic method |
| CN111864080A (en) * | 2020-09-07 | 2020-10-30 | 天津理工大学 | Two-dimensional organic-inorganic hybrid perovskite crystal photoelectric detector and preparation method thereof |
| CN113484341A (en) * | 2021-07-01 | 2021-10-08 | 南京工业大学 | Method for preparing TEM sample based on hybrid lead-based perovskite nanosheets |
| CN113484341B (en) * | 2021-07-01 | 2022-10-25 | 南京工业大学 | Method for preparing TEM sample based on hybrid lead-based perovskite nanosheets |
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