CN106282922A - A kind of coevaporation prepares the method for inorganic non-lead halogenide perovskite thin film - Google Patents

A kind of coevaporation prepares the method for inorganic non-lead halogenide perovskite thin film Download PDF

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Publication number
CN106282922A
CN106282922A CN201610806551.6A CN201610806551A CN106282922A CN 106282922 A CN106282922 A CN 106282922A CN 201610806551 A CN201610806551 A CN 201610806551A CN 106282922 A CN106282922 A CN 106282922A
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thin film
inorganic non
perovskite thin
lead
temperature
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杨盼
杨丽军
赵晓冲
王劲川
杨蕊竹
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Institute of Materials of CAEP
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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
    • C23C14/06—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
    • C23C14/22—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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention discloses a kind of method that coevaporation prepares inorganic non-lead halogenide perovskite thin film, including: (1) carries out ultrasonic cleaning to backing material, and nitrogen dries up standby；(2) being put into by backing material on coevaporation equipment sample frame, to evacuation in vacuum chamber, the vacuum to chamber is less than 5 × 10‑4During Pa, heating rotation of substrate material, keep its temperature；(3) regulation CsX evaporation source and SnX2The temperature of evaporation source, makes the two jointly be controlled the evaporation rate of backing material；(4) temperature in source to be evaporated reach setting value and evaporation rate stable after carry out the double source Co-evaporated Deposition of inorganic non-lead halogenide perovskite thin film, be cooled to room temperature, obtain inorganic non-lead halogenide perovskite thin film.Inorganic non-lead halogenide perovskite thin film good stability prepared by the present invention, with low cost, surfacing, internal flaw is less, process repeatability is high, and environmental protection is pollution-free, is suitable for large-scale industrialized production.

Description

A kind of coevaporation prepares the method for inorganic non-lead halogenide perovskite thin film
Technical field
The present invention relates to photovoltaic cell technical field, particularly relate to a kind of coevaporation and prepare inorganic non-lead halogenide calcium The method of titanium ore thin film.
Background technology
Perovskite based on halogenide has the light absorpting ability of excellence, considerable bipolarity carrier mobility, overlength The feature of electron-hole diffusion length, it is one of most important study hotspot in being increasingly becoming current photovoltaic art.Current Halogenide perovskite is predominantly organic-inorganic metal compound methylamine lead iodine (CH3NH3PbX3, X is the one in Cl/Br/I or many Kind), the main synthetic ingredient halogenation methylamine (CH of methylamine lead iodine3NH3X) meet water electrode facile hydrolysis, cause methylamine lead iodine perovskite performance Extremely unstable, and containing poisonous Pb element in methylamine lead iodine perovskite, thus this also greatly limit calcium titanium The development of ore deposit battery.
Therefore, designing a kind of novel perovskite material, enable to be preferably applied for perovskite battery, becoming is one Plant technological trend.
Summary of the invention
It is an object of the invention to provide a kind of method that coevaporation prepares inorganic non-lead halogenide perovskite thin film, mainly Solve existing organic-inorganic metal compound perovskite and there is Organic substance instability and the problem of Pb pollution.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of coevaporation prepares the method for inorganic non-lead halogenide perovskite thin film, comprises the following steps:
(1) backing material is carried out ultrasonic cleaning, then use nitrogen to dry up standby；
(2) the thorough material after drying up is put on the specimen holder of coevaporation equipment, then takes out in vacuum chamber Vacuum, until the vacuum of chamber is less than 5 × 10-4During Pa, heating rotation of substrate material so that it is temperature is maintained at 50～200 ℃；
(3) regulation CsX evaporation source and SnX2The temperature of evaporation source, makes the two jointly carry out the evaporation rate of backing material Controlling, wherein, the range of accommodation of CsX source temperature is 300～900 DEG C, SnX2The range of accommodation of source temperature be 100～ 800℃；Described X is one or more in Cl, Br, I；
(4) temperature in source to be evaporated reach setting value and evaporation rate stable after, open sample baffle plate, carry out inorganic non-lead The double source Co-evaporated Deposition of halogenide perovskite thin film, sedimentation time is 20～60 minutes, is then cooled to room temperature, and obtains inorganic Non-lead halogenide perovskite thin film.
Further, in described step (1), utilize detergent, deionized water, ethanol, acetone, isopropanol the most ultrasonic clearly Wash backing material, each ultrasonic cleaning 5～15 minutes.
Yet further, in described step (1), the nitrogen being dried is used to be dried up by backing material.
As preferably, described backing material is rigid substrate materials.
Or, described backing material is flexible substrate material.
Compared with prior art, the method have the advantages that
(1) present invention utilizes double source coevaporation method to deposited a kind of novel inorganic non-lead halogenide perovskite (CsSnX3 Or Cs2SnX6, X is one or more in halogens Cl, Br, I), owing to it utilizes stable inorganic compound caesium halide (CsX) instead of organic methylamine iodine, thus solve organic-inorganic metal compound perovskite unstable properties well Problem；Further, the present invention utilizes element S n to replace toxic element Pb, also efficiently solves organic-inorganic metal compound calcium titanium The pollution problem in ore deposit.It can be said that the present invention is by the inorganic non-lead halogenide perovskite thin film of double source thermal evaporation deposition preparation Not only surfacing, internal flaw is less, process repeatability is high, and environmental protection is pollution-free, thus is highly suitable for Large-scale industrialized production.
(2) present invention utilizes detergent, deionized water, ethanol, acetone, isopropanol that backing material is carried out ultrasonic cleaning, The most with low cost, and can effectively remove the various impurity in backing material and Organic substance, cleaning performance is the best.
(3) under rational technological design, the backing material in the present invention can use rigid substrate materials (as carried glass Sheet, simple glass, silicon chip etc.), it would however also be possible to employ flexible substrate material (such as PET, PEN, PI etc.), therefore, not only raw material Originate widely, and with low cost, possess the advantage of large-scale promotion application.
Accompanying drawing explanation
Fig. 1 is the structural representation of the coevaporation equipment used in the present invention.
Fig. 2 is the schematic flow sheet of the present invention.
Fig. 3 is inorganic non-lead CsSnI in the present invention-embodiment3The scanning electron microscope (SEM) photograph of perovskite thin film.
Fig. 4 is inorganic non-lead CsSnI3The X-ray diffractogram of perovskite thin film.
Fig. 5 is inorganic non-lead CsSnI3The absorption spectrum curve schematic diagram of perovskite thin film.
Wherein, the parts that reference is corresponding are entitled:
1-vacuum chamber, 2-CsX evaporation source, 3-SnX2Evaporation source, 4-sample baffle plate, the specimen holder of 5-band heating, 6-sample Product rotary shaft.
Detailed description of the invention
The invention will be further described with embodiment in explanation below in conjunction with the accompanying drawings, and the mode of the present invention includes but not only limits In following example.
Embodiment
(chemical formula is CsSnX to the invention provides a kind of inorganic non-lead halogenide3Or Cs2SnX6, X be halogens Cl, One or more in Br or I) perovskite thin film, it is mainly used in perovskite battery aspect.The present invention uses being total to shown in Fig. 1 Evaporation equipment carries out the preparation of inorganic non-lead halogenide perovskite thin film, and this coevaporation equipment includes that vacuum chamber 1, CsX evaporate Source 2, SnX2The specimen holder 5 of evaporation source 3, sample baffle plate 4, band heating, rotary sample axle 6, described CsX evaporation source 2, SnX2Steam Rise 3, the specimen holder 5 of sample baffle plate 4 and band heating is arranged in vacuum chamber 1, and X therein is the one in Cl, Br, I Or it is multiple；Described rotary sample axle 6 is connected with specimen holder 5, for Unscrew vacuum chamber 1, such as the rotation arrows in Fig. 1 Shown in.
As in figure 2 it is shown, the process that the present invention prepares this kind of inorganic non-lead halogenide perovskite thin film is as follows:
One, the pretreatment before coevaporation
(1) utilize successively detergent, deionized water, ethanol, acetone, isopropanol backing material is each carried out ultrasonic clearly Wash, each ultrasonic cleaning 5～15 minutes, then use nitrogen to be dried up by backing material standby；Backing material in the present embodiment Can be rigid substrate materials (such as microscope slide, simple glass, silicon chip etc.), it is also possible to be flexible substrate material (as PET, PEN, PI etc.)；
(2) backing material cleaned and dry up is positioned on the specimen holder of coevaporation, then vacuum chamber is taken out Vacuum, until its vacuum is less than 5 × 10-4During Pa, heat specimen holder, make the temperature of backing material be maintained at 50～200 DEG C.
Two, coevaporation prepares inorganic non-lead halogenide perovskite thin film
(1) regulation CsX evaporation source and SnX2The temperature of evaporation source, makes the two jointly carry out the evaporation rate of backing material Controlling, wherein, the range of accommodation of CsX source temperature is 300～900 DEG C, SnX2The range of accommodation of source temperature be 100～ 800℃；
(2) temperature in source to be evaporated reach setting value and evaporation rate stable after, open sample baffle plate, carry out inorganic non-lead The Co-evaporated Deposition of halogenide perovskite thin film, sedimentation time is 20～60 minutes, is then cooled to room temperature, and obtains inorganic non-lead Halogenide perovskite thin film；In the present embodiment, by composition and the ratio of regulation X element, can realize regulating the forbidden band width of thin film Degree.
Beneficial effects of the present invention is embodied below with an experiment case study.
Evaporation source material is CsI and SnI2, double source coevaporation prepares CsSnI3Inorganic non-lead perovskite thin film.This CsSnI3 The scanning electron microscope of inorganic non-lead perovskite thin film is as it is shown on figure 3, inorganic non-lead CsSnI3The X-ray diffractogram of perovskite thin film is such as Shown in Fig. 4, inorganic non-lead CsSnI3The absorption spectrum curve of perovskite thin film as it is shown in figure 5, from Fig. 5 it can be calculated that this Inorganic non-lead CsSnI of bright preparation3The energy gap of perovskite thin film is about 1.55eV, is therefore highly suitable as photovoltaic cell Absorbed layer material.
The present invention is selected and technological design by rational raw material, has prepared a kind of inorganic non-lead halogenide perovskite thin Film, this perovskite thin film not only preparation cost is cheap, and there is good stability, the characteristic that nontoxic, process repeatability is high, And environmental protection is pollution-free, thus efficiently solves existing organic-inorganic metal compound perovskite and there is Organic substance not The problem that stable and Pb pollutes, and it is advantageously applied to perovskite battery aspect.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit the protection model of the present invention Enclosing, all body design thought in the present invention and the change having no essential meaning made mentally or polishing, it is solved Technical problem is the most consistent with the present invention, within all should being included in protection scope of the present invention.

Claims (4)

1. the method that a coevaporation prepares inorganic non-lead halogenide perovskite thin film, it is characterised in that comprise the following steps:
(1) backing material is carried out ultrasonic cleaning, then use nitrogen to dry up standby；
(2) the thorough material after drying up is put on the specimen holder of coevaporation equipment, then to carrying out evacuation in vacuum chamber, Until the vacuum of chamber is less than 5 × 10-4During Pa, heating rotation of substrate material so that it is temperature is maintained at 50～200 DEG C；
(3) regulation CsX evaporation source and SnX2The temperature of evaporation source, makes the two jointly be controlled the evaporation rate of backing material, Wherein, the range of accommodation of CsX source temperature is 300～900 DEG C, SnX2The range of accommodation of source temperature is 100～800 ℃；Described X is one or more in Cl, Br, I；
(4) temperature in source to be evaporated reach setting value and evaporation rate stable after, open sample baffle plate, carry out inorganic non-lead halogenation The double source Co-evaporated Deposition of thing perovskite thin film, sedimentation time is 20～60 minutes, is then cooled to room temperature, and obtains inorganic non-lead Halogenide perovskite thin film.
A kind of coevaporation the most according to claim 1 prepares the method for inorganic non-lead halogenide perovskite thin film, its feature It is, in described step (1), utilizes detergent, deionized water, ethanol, acetone, isopropanol ultrasonic cleaning backing material successively, Every time ultrasonic cleaning 5～15 minutes.
A kind of coevaporation the most according to claim 2 prepares the method for inorganic non-lead halogenide perovskite thin film, its feature Being, described backing material is rigid substrate materials.
A kind of coevaporation the most according to claim 3 prepares the method for inorganic non-lead halogenide perovskite thin film, its feature Being, described backing material is flexible substrate material.
CN201610806551.6A 2016-09-07 2016-09-07 A kind of coevaporation prepares the method for inorganic non-lead halogenide perovskite thin film Pending CN106282922A (en)

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CN108198941A (en) * 2018-01-08 2018-06-22 苏州大学 Full-inorganic perovskite solar cell with ultraviolet light strainability and preparation method thereof and its application in optical field
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
CN109518161A (en) * 2018-11-29 2019-03-26 中国科学院长春光学精密机械与物理研究所 The preparation method of caesium tin halogen perovskite thin film material
WO2019141045A1 (en) * 2018-01-17 2019-07-25 杭州纤纳光电科技有限公司 Apparatus for immersion-based preparation of perovskite thin film, use method and application thereof
CN111370998A (en) * 2020-01-06 2020-07-03 武汉大学 Method for preparing perovskite array micro resonant cavity laser by femtosecond laser
CN112647047A (en) * 2020-12-02 2021-04-13 河南大学 Preparation method and application of cesium tin iodine film
CN114481032A (en) * 2021-12-17 2022-05-13 无锡极电光能科技有限公司 Device and method for preparing perovskite film layer, solar cell and preparation method

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108198941A (en) * 2018-01-08 2018-06-22 苏州大学 Full-inorganic perovskite solar cell with ultraviolet light strainability and preparation method thereof and its application in optical field
CN108198941B (en) * 2018-01-08 2022-08-12 苏州大学 All-inorganic perovskite solar cell with ultraviolet light filtering performance and preparation thereof
WO2019141045A1 (en) * 2018-01-17 2019-07-25 杭州纤纳光电科技有限公司 Apparatus for immersion-based preparation of perovskite thin film, use method and application thereof
JP2021507542A (en) * 2018-01-17 2021-02-22 杭州繊納光電科技有限公司Ｈａｎｇｚｈｏｕ Ｍｉｃｒｏｑｕａｎｔａ Ｓｅｍｉｃｏｎｄｕｃｔｏｒ Ｃｏ．，Ｌｔｄ Immersion device for producing perovskite film, usage and its use
JP7037838B2 (en) 2018-01-17 2022-03-17 杭州繊納光電科技有限公司 A vapor deposition device for manufacturing perovskite film, its usage, and a method for manufacturing perovskite solar cells.
JP7037838B6 (en) 2018-01-17 2022-04-01 杭州繊納光電科技有限公司 A vapor deposition device for manufacturing perovskite film, its usage, and a method for manufacturing perovskite solar cells.
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
CN109518161A (en) * 2018-11-29 2019-03-26 中国科学院长春光学精密机械与物理研究所 The preparation method of caesium tin halogen perovskite thin film material
CN111370998A (en) * 2020-01-06 2020-07-03 武汉大学 Method for preparing perovskite array micro resonant cavity laser by femtosecond laser
CN112647047A (en) * 2020-12-02 2021-04-13 河南大学 Preparation method and application of cesium tin iodine film
CN112647047B (en) * 2020-12-02 2022-02-15 河南大学 Preparation method and application of cesium tin iodine film
CN114481032A (en) * 2021-12-17 2022-05-13 无锡极电光能科技有限公司 Device and method for preparing perovskite film layer, solar cell and preparation method

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Application publication date: 20170104