CN107881472A - A kind of CsPbI3The preparation method of film - Google Patents

A kind of CsPbI3The preparation method of film Download PDF

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Publication number
CN107881472A
CN107881472A CN201711185329.XA CN201711185329A CN107881472A CN 107881472 A CN107881472 A CN 107881472A CN 201711185329 A CN201711185329 A CN 201711185329A CN 107881472 A CN107881472 A CN 107881472A
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cspbi
film
preparation
target
iodine
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张立春
林国琛
薛晓娥
赵风周
徐满
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Ludong University
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Ludong University
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0694—Halides
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

Abstract

The invention provides a kind of CsPbI3The preparation method of film, comprises the following steps：Monocrystalline substrate surface is cleaned, after being dried up with nitrogen, is put into the vacuum growth room of impulse laser deposition system；Target is etched using pulsed laser deposition technique, grows one layer of CsPbI in monocrystalline silicon surface3Film；By the CsPbI3Film is placed under iodine vapor environment and made annealing treatment, i.e., under iodine vapor environment, to CsPbI3Film recrystallization；Growth takes out sample after terminating, and after being cleaned with deionized water, is dried up with nitrogen.The preparation method is simple, and reaction temperature is low, and the reaction time is short, and cost is low, suitable for industrialized production；The CsPbI that large area even compact, crystalline quality are high and photoelectric properties are excellent can be obtained3Film, meet its application in the field of photoelectric devices such as luminescent material, solar cell.

Description

A kind of CsPbI3The preparation method of film
Technical field
The present invention relates to field of semiconductor materials, and in particular to a kind of CsPbI3The preparation method of film.
Background technology
In recent years, the semi-conducting material of some perovskite structures, due to special with excellent optical absorption and charge-conduction Property, turn into the study hotspot of current area of solar cell.Relative to hybrid inorganic-organic perovskite material, full-inorganic halogen Perovskite material (CsPbX3, X=Cl, Br, I) and chemical stability is higher, and (is up to high fluorescence quantum efficiency 90%), wavelength of fluorescence is adjustable and the features such as covering whole visible light wave range, line width, is expected to be applied to a new generation's display and shines In bright technology.In addition, full-inorganic perovskite material has high absorption coefficient, its light absorpting ability is higher than other organic dyestuff More than 10 times；And its octahedra system is also beneficial to the transmission in electronics and hole so that the material has high carrier Mobility and longer carrier lifetime.
It is worth noting that, full-inorganic perovskite material CsPbX3As direct band-gap semicondictor material, except with compared with Outside the high absorption coefficient of light and excellent carrier transmission characteristics, its special luminescent properties also attracts people always for a long time Concern.Full-inorganic perovskite material typically has higher exciton binding energy, special so as to show strong room temperature photoluminescence Property.In addition, ultralow volume defect density also causes perovskite material to show high luminous efficiency.These advantages cause completely without Machine perovskite material also shows wide in light emitting diode, laser device, field-effect transistor and photoelectric detector field Application prospect.
Perovskite material is prepared using chemical methodes such as solwution method, spin-coating methods more at present, and the material prepared easily occurs The defects of pin hole, crackle, it is difficult to obtain the perovskite thin film material of high quality.This causes perovskite material to deposit in actual applications Stability is poor, short life the problems such as, the practical application of perovskite photoelectric device has been had a strong impact on.
The content of the invention
The application is by providing a kind of CsPbI3The preparation method of film, to solve the CsPbI that prior art is prepared3It is thin Film quality is not high, the technical problem such as preparation method complexity.
In order to solve the above technical problems, the application is achieved using following technical scheme：
A kind of CsPbI3The preparation method of film, comprises the following steps：
S1：Monocrystalline substrate surface is cleaned, after being dried up with nitrogen, is put into the vacuum growth of impulse laser deposition system Room；
S2：Target is etched using pulsed laser deposition technique, in one layer of CsPbI of monocrystalline substrate superficial growth3Film；
S3：In order to further improve film quality and crystallinity, by the CsPbI3Film is placed under iodine vapor environment and carried out Annealing, i.e., under iodine vapor environment, to CsPbI3Film recrystallization；
S4：Growth takes out sample after terminating, and after being cleaned with deionized water, is dried up with nitrogen.
Further, the CsPbI grown in step S23The deposit thickness of film is 100nm~400nm.
Further, the concrete technology condition of pulsed laser deposition technique is in step S2：Background vacuum is 1 × 10-6Pa ~5 × 10-6Pa, underlayer temperature are room temperature~400 DEG C, and laser energy is 250mJ~350mJ, and laser frequency is 5Hz~10Hz, Laser power is 1.25w~3.5w, and film growth rates are
Further, room temperature is 25 DEG C~30 DEG C.
Further, the target is CsPbI3Target, the CsPbI3Target is to utilize mol ratio as 1:1 CsI powder and PbI2 After powder mixed grinding is uniform, using a diameter of 1 inch made of 40MPa pressure, thickness as 5mm cylindrical target.
Further, step S2's is specially：CsPbI is etched using high power pulsed laser high temperature3Target, form plasma Plumage brightness, by the adiabatic expansion of plasma, finally orient and be diffused into nucleating growth in monocrystalline substrate, form CsPbI3 Film.
Further, the process conditions made annealing treatment in step S3 are：Annealing region is 90 DEG C~140 DEG C, annealing Time is 30min~120min.
Further, iodine vapor derives from iodine particle in step S3, and the concentration of the iodine particle is 99.5%.
Further, step S3's is specially：By iodine particle and CsPbI3Film is placed in culture dish, by culture dish Sealing, and the culture dish is gently put in heating plate, make iodine grain sublimation, make CsPbI3Iodine vapor of the film in sealing Annealing recrystallization under atmosphere.
Further, the distance between the target and monocrystalline substrate are 5cm.
Compared with prior art, the technical scheme that the application provides, the technique effect or advantage having are：
1) preparation method is simple, and reaction temperature is low, and the reaction time is short, and cost is low, suitable for industrialized production；
2) preparation method can obtain the CsPbI that large area even compact, crystalline quality are high and photoelectric properties are excellent3It is thin Film, meet its application in the field of photoelectric devices such as luminescent material, solar cell；
3) preparation condition of the preparation method is in confined space, it is possible to reduce pollution of the iodine to environment, is a kind of Environmentally friendly preparation method；
4) preparation method provided by the invention, target (CsI powder and PbI are etched using pulsed laser deposition technology2Powder With mol ratio 1：1 is ground and suppresses), the uniform CsPbI of large area is prepared under vacuum3Thin-film material, prepare Technique is compatible with photoelectric device preparation technology.
Brief description of the drawings
Fig. 1 is flow chart of the method for the present invention；
Fig. 2 is the CsPbI prepared according to preparation method of the embodiment of the present invention3The scanning electron microscope (SEM) photograph of membrane structure；
Fig. 3 is the CsPbI prepared according to preparation method of the embodiment of the present invention3The X-ray diffractogram of membrane structure；
Fig. 4 is the CsPbI prepared according to preparation method of the embodiment of the present invention3The photoluminescence spectra figure of membrane structure.
Embodiment
The embodiment of the present application is by providing a kind of CsPbI3The preparation method of film, prepared with to solve prior art CsPbI3Film quality is not high, the technical problem such as preparation method complexity.
It is right below in conjunction with Figure of description and specific embodiment in order to be better understood from above-mentioned technical proposal Above-mentioned technical proposal is described in detail.
Embodiment
A kind of CsPbI3The preparation method of film, CsPbI is etched using pulsed laser deposition technology3Target, in vacuum condition Under prepare full-inorganic CsPbI3Perovskite thin film, i.e., target is placed in the vacuum growth room of impulse laser deposition system, utilized High power pulsed laser carrys out high temperature etching CsPbI3Target, plasma plume brightness is formed, by the adiabatic expansion mistake of plasma Journey, finally orient and be diffused into nucleating growth on silicon substrate, form CsPbI3Film.
As shown in figure 1, specifically comprise the following steps：
S1：Monocrystalline substrate surface is cleaned, after being dried up with nitrogen, is put into the vacuum growth of impulse laser deposition system Room；
Standard RCA clean is carried out to monocrystalline silicon substrate, removes the organic matter, impurity metal ion and dust on its surface；
S2：Target is etched using pulsed laser deposition technique, grows one layer of CsPbI in monocrystalline silicon surface3Film；Wherein, The concrete technology condition of pulsed laser deposition technique is：Background vacuum is 1 × 10-6Pa~5 × 10-6Pa, underlayer temperature are room temperature ~400 DEG C (room temperatures be 25 DEG C~30 DEG C), laser energy are 250mJ~350mJ, and laser frequency is 5Hz~10Hz, laser power For 1.25w~3.5w, film growth rates areThe target is CsPbI3Target, the CsPbI3Target is to utilize to rub You are than being 1:1 CsI powder and PbI2After powder mixed grinding is uniform, with a diameter of 1 inch, thickness made of 40MPa pressure For 5mm cylindrical target, the distance between substrate and target are 5cm, the CsPbI of growth3The deposit thickness of film be 100nm~ 400nm；
Step S2 be specially：CsPbI is etched using high power pulsed laser high temperature3Target, plasma plume brightness is formed, passed through The adiabatic expansion of plasma, finally orient and be diffused into nucleating growth in monocrystalline substrate, growth deposit thickness is 100nm ~400nm CsPbI3Film；
S3：In order to further improve film quality and crystallinity, by the CsPbI3Film is placed under iodine vapor environment and carried out Annealing, i.e., under iodine vapor environment, to CsPbI3Film recrystallization；Wherein, the process conditions of annealing are：Annealing temperature It is 90 DEG C~140 DEG C to spend scope, and annealing time is 30min~120min, and iodine vapor derives from iodine particle, the iodine The concentration of particle is 99.5%, and the reaction vessel used in annealing process is culture dish；
Step S3 be specially：By iodine particle and CsPbI3Film is placed in culture dish, and culture dish is sealed, and will The culture dish is gently put in heating plate, is made iodine grain sublimation, is made CsPbI3Film moves back under the iodine vapor atmosphere of sealing Fire recrystallization；
S4：Growth takes out sample after terminating, and after being cleaned with deionized water, is dried up with nitrogen.
Below to grow CsPbI of the deposited film thickness as 400nm3Exemplified by film, it is further described, the preparation side Method：
S1：Standard RCA clean is carried out to monocrystalline substrate surface, removes the organic matter, impurity metal ion and ash on surface Dirt, after being dried up with nitrogen, it is put into the vacuum growth room of impulse laser deposition system；
S2：Target is etched using pulsed laser deposition technique, grows one layer of CsPbI in monocrystalline silicon surface3Film；Pulse swashs The concrete technology condition of light deposition technology is：Background vacuum is 5 × 10-6Pa, underlayer temperature are 25 DEG C, laser energy 250mJ, Laser frequency is 5Hz, laser power 1.26W, and the speed of growth isThe target is CsPbI3Target, the CsPbI3Target is It is 1 using mol ratio:1 CsI powder and PbI2After powder mixed grinding is uniform, with a diameter of 1 English made of 40MPa pressure Very little, thickness is 5mm cylindrical target, and the distance between substrate and target are 5cm；
S3：By the CsPbI3Film is placed under iodine vapor environment and made annealing treatment, i.e., right under iodine vapor environment CsPbI3Film recrystallization；
The 0.2g iodine particles weighed up are placed in culture dish first, while by CsPbI3Film is placed in culture dish, Culture dish is sealed, and it is gently put in heating plate, is set 120 DEG C of heating-up temperature, is made iodine grain sublimation, make CsPbI3 Film annealing recrystallization under the iodine vapor atmosphere of sealing, the reaction time is 30min；
Step 4：Growth takes out sample after terminating, and is cleaned with deionized water, is dried up with nitrogen.
Fig. 2 show the CsPbI for characterizing and preparing using SEM3The surface topography of membrane structure, it is prepared Film particles be evenly distributed, size is consistent.Fig. 3 is shown characterizes CsPbI using X-ray diffractometer3Membrane structure Crystalline quality, prepared sample present polycrystalline structure, wherein, 024 direction is CsPbI3Preferred growth direction.Fig. 4 institutes The laser being shown as by the use of 325nm analyzes CsPbI as excitation source3The photoluminescence property of film, CsPbI3Membrane structure Photoluminescence spectra shows the band-edge emission that stronger, centre wavelength is located at 650nm.
In above-described embodiment of the application, by providing a kind of CsPbI3The preparation method of film, comprises the following steps：Clearly Monocrystalline substrate surface is washed, after being dried up with nitrogen, is put into the vacuum growth room of impulse laser deposition system；Swashed using pulse Light deposition technology etches target, grows one layer of CsPbI in monocrystalline silicon surface3Film；By the CsPbI3Film is placed in iodine vapor environment Under made annealing treatment, i.e., under iodine vapor environment, to CsPbI3Film recrystallization；Growth takes out sample after terminating, and spends After ionized water cleaning, dried up with nitrogen.The preparation method is simple, and reaction temperature is low, and the reaction time is short, and cost is low, suitable for work Industry metaplasia is produced；The CsPbI that large area even compact, crystalline quality are high and photoelectric properties are excellent can be obtained3Film, meet its Application in the field of photoelectric devices such as luminescent material, solar cell.
It should be pointed out that it is limitation of the present invention that described above, which is not, the present invention is also not limited to the example above, What those skilled in the art were made in the essential scope of the present invention changes, is modified, adds or replaces, and also should Belong to protection scope of the present invention.

Claims (10)

  1. A kind of 1. CsPbI3The preparation method of film, it is characterised in that comprise the following steps：
    S1：Monocrystalline substrate surface is cleaned, after being dried up with nitrogen, is put into the vacuum growth room of impulse laser deposition system；
    S2：Target is etched using pulsed laser deposition technique, in one layer of CsPbI of monocrystalline substrate superficial growth3Film；
    S3：By the CsPbI3Film is placed under iodine vapor environment and made annealing treatment, i.e., under iodine vapor environment, to CsPbI3It is thin Film recrystallizes；
    S4：Growth takes out sample after terminating, and after being cleaned with deionized water, is dried up with nitrogen.
  2. 2. CsPbI according to claim 13The preparation method of film, it is characterised in that the CsPbI grown in step S23 The deposit thickness of film is 100nm~400nm.
  3. 3. CsPbI according to claim 13The preparation method of film, it is characterised in that pulsed laser deposition in step S2 The concrete technology condition of technology is：Background vacuum is 1 × 10-6Pa~5 × 10-6Pa, underlayer temperature are room temperature~400 DEG C, laser Energy is 250mJ~350mJ, and laser frequency is 5Hz~10Hz, and laser power is 1.25w~3.5w, and film growth rates are
  4. 4. CsPbI according to claim 33The preparation method of film, it is characterised in that room temperature is 25 DEG C~30 DEG C.
  5. 5. CsPbI according to claim 13The preparation method of film, it is characterised in that the target is CsPbI3Target, should CsPbI3Target is to utilize mol ratio as 1:1 CsI powder and PbI2After powder mixed grinding is uniform, with straight made of 40MPa pressure The cylindrical target that footpath is 1 inch, thickness is 5mm.
  6. 6. the CsPbI according to any claim in claim 1 to 53The preparation method of film, it is characterised in that step S2 be specially：CsPbI is etched using high power pulsed laser high temperature3Target, plasma plume brightness is formed, by the exhausted of plasma Thermal expansion process, finally orient and be diffused into nucleating growth in monocrystalline substrate, form CsPbI3Film.
  7. 7. CsPbI according to claim 13The preparation method of film, it is characterised in that the work made annealing treatment in step S3 Skill condition is：Annealing region is 90 DEG C~140 DEG C, and annealing time is 30min~120min.
  8. 8. CsPbI according to claim 13The preparation method of film, it is characterised in that iodine vapor derives from step S3 Iodine particle, the concentration of the iodine particle is 99.5%.
  9. 9. the CsPbI according to claim 7 or 83The preparation method of film, it is characterised in that step S3 be specially：Will Iodine particle and CsPbI3Film is placed in culture dish, and culture dish is sealed, and the culture dish is gently put in heating plate, Make iodine grain sublimation, make CsPbI3Film annealing recrystallization under the iodine vapor atmosphere of sealing.
  10. 10. CsPbI according to claim 13The preparation method of film, it is characterised in that the target and monocrystalline substrate The distance between be 5cm.
CN201711185329.XA 2017-11-23 2017-11-23 A kind of CsPbI3The preparation method of film Pending CN107881472A (en)

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Cited By (10)

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CN109097741A (en) * 2018-08-31 2018-12-28 鲁东大学 A kind of CsPbBr3The preparation method of film
CN109256471A (en) * 2018-12-10 2019-01-22 合肥工业大学 A kind of unleaded full-inorganic perovskite caesium bismuth iodine film/n-type silicon heterojunction photoelectric detector and preparation method thereof
CN109266344A (en) * 2018-11-21 2019-01-25 南京邮电大学 The preparation method of one type halogen perovskite quanta point material
CN109301072A (en) * 2018-09-27 2019-02-01 深圳大学 A kind of preparation method of solvent-free perovskite photoelectric device
CN109904257A (en) * 2019-02-28 2019-06-18 杭州电子科技大学 A kind of preparation and purification method of caesium lead iodine
CN110350094A (en) * 2019-06-12 2019-10-18 安徽鑫民玻璃股份有限公司 A method of it iodinates and improves perovskite thin film stability
JP2022500873A (en) * 2018-09-20 2022-01-04 ジョイント ストック カンパニー クラスノヤルスク ハイドロパワー プラント（ジェイエスシー クラスノヤルスク エイチピーピー） Methods for Forming Films of Perovskite-Like Materials
CN116705893A (en) * 2023-08-02 2023-09-05 济南大学 MSM type photoelectric detector and preparation method thereof
CN116722059A (en) * 2023-08-01 2023-09-08 济南大学 Semiconductor CsPbX 3 Thin film material, preparation method and application thereof, and solar cell
CN116847665A (en) * 2023-09-01 2023-10-03 济南大学 Silicon-based epitaxial perovskite heterogeneous PN junction photoelectric detector and preparation method thereof

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097741A (en) * 2018-08-31 2018-12-28 鲁东大学 A kind of CsPbBr3The preparation method of film
JP2022500873A (en) * 2018-09-20 2022-01-04 ジョイント ストック カンパニー クラスノヤルスク ハイドロパワー プラント（ジェイエスシー クラスノヤルスク エイチピーピー） Methods for Forming Films of Perovskite-Like Materials
JP7429687B2 (en) 2018-09-20 2024-02-08 ジョイント ストック カンパニー クラスノヤルスク ハイドロパワー プラント（ジェイエスシー クラスノヤルスク エイチピーピー） Method for forming films of perovskite-like materials
CN109301072A (en) * 2018-09-27 2019-02-01 深圳大学 A kind of preparation method of solvent-free perovskite photoelectric device
CN109301072B (en) * 2018-09-27 2022-11-18 深圳大学 Preparation method of solvent-free perovskite photoelectric device
CN109266344A (en) * 2018-11-21 2019-01-25 南京邮电大学 The preparation method of one type halogen perovskite quanta point material
CN109256471A (en) * 2018-12-10 2019-01-22 合肥工业大学 A kind of unleaded full-inorganic perovskite caesium bismuth iodine film/n-type silicon heterojunction photoelectric detector and preparation method thereof
CN109904257B (en) * 2019-02-28 2020-09-01 杭州电子科技大学 Preparation and purification method of cesium-lead-iodine
CN109904257A (en) * 2019-02-28 2019-06-18 杭州电子科技大学 A kind of preparation and purification method of caesium lead iodine
CN110350094A (en) * 2019-06-12 2019-10-18 安徽鑫民玻璃股份有限公司 A method of it iodinates and improves perovskite thin film stability
CN116722059A (en) * 2023-08-01 2023-09-08 济南大学 Semiconductor CsPbX 3 Thin film material, preparation method and application thereof, and solar cell
CN116705893A (en) * 2023-08-02 2023-09-05 济南大学 MSM type photoelectric detector and preparation method thereof
CN116847665A (en) * 2023-09-01 2023-10-03 济南大学 Silicon-based epitaxial perovskite heterogeneous PN junction photoelectric detector and preparation method thereof
CN116847665B (en) * 2023-09-01 2023-12-19 济南大学 Silicon-based epitaxial perovskite heterogeneous PN junction photoelectric detector and preparation method thereof

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