CN113526545A - Method for preparing tin-based perovskite powder based on mechanochemical method - Google Patents

Method for preparing tin-based perovskite powder based on mechanochemical method Download PDF

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CN113526545A
CN113526545A CN202110804749.1A CN202110804749A CN113526545A CN 113526545 A CN113526545 A CN 113526545A CN 202110804749 A CN202110804749 A CN 202110804749A CN 113526545 A CN113526545 A CN 113526545A
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snx
tin
mechanochemical
perovskite powder
csx
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赵�卓
武俊生
唐美嘉宝
周艳文
张文雷
白星辰
张世丰
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Huzhou Wenlei New Material Co ltd
Liaoning Wenlei Technology Co ltd
Liaoning Xingmei Environmental Protection Science And Trade Co ltd
University of Science and Technology Liaoning USTL
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Huzhou Wenlei New Material Co ltd
Liaoning Wenlei Technology Co ltd
Liaoning Xingmei Environmental Protection Science And Trade Co ltd
University of Science and Technology Liaoning USTL
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Priority to CN202110804749.1A priority Critical patent/CN113526545A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention aims to overcome the problems of perovskite materials in the prior art, provides a method for preparing tin-based perovskite powder based on a mechanochemical method, and belongs to the technical field of photovoltaic materials. The method comprises the following steps: 1) take CsX and SnX2Or CsX and SnX4Mixing uniformly; 2) putting the mixed material into a ball milling tank in a protective atmosphere at room temperature, and ball milling by using a ball mill to obtain CsSnX3Or Cs2SnX6. The method can prepare the tin-based perovskite nano powder with refined crystal grains, high crystallinity and high thermal stability.

Description

Method for preparing tin-based perovskite powder based on mechanochemical method
Technical Field
The invention belongs to the technical field of photovoltaic materials, and particularly relates to a method for preparing tin-based perovskite powder based on a mechanochemical method.
Background
Organic-inorganic lead perovskite halides have been extensively studied in recent years due to their excellent photoelectric and photovoltaic properties. Since the first application of metal halide perovskite materials to solar cells (efficiency of 3.8%) in 2009, researchers have been working on further developing the application of metal halide perovskites in the fields of field effect tubes, solar cells, photodetectors, thermoelectrics, tandem devices, light emitting electrochemical cells, diodes, lasers, and the like.
There are currently two commonly employed methods for fabricating perovskite optoelectronic devices, including solution-based or vapor-based deposition techniques. The former requires dissolving the metal halide precursor in a high boiling polar organic solvent such as Dimethylformamide (DMF) and Dimethylsulfoxide (DMSO), and the latter requires performing under specific equipment and atmosphere. That is, both techniques require stringent operating conditions. Furthermore, it is impractical to manufacture and deploy perovskites over a wide range using these methods. Because of the limited yield in this process, the scale is large. Therefore, there is a need to find a novel and industrially applicable method for preparing perovskite materials.
Disclosure of Invention
The invention aims to overcome the problems of perovskite materials in the prior art and provides a method for preparing tin-based perovskite powder based on a mechanochemical method, and the method can be used for preparing the tin-based perovskite nano powder with refined grains, high crystallinity and high thermal stability.
A method for preparing tin-based perovskite powder based on a mechanochemical method comprises the following steps:
1) take CsX and SnX2Or CsX and SnX4Mixing uniformly;
2) putting the mixed material into a ball milling tank in a protective atmosphere at room temperature, and ball milling by using a ball mill to obtain CsSnX3Or Cs2SnX6。
Further, CsX and SnX are used in the method for preparing tin-based perovskite powder based on the mechanochemical method2The molar ratio of (A) to (B) is 1: 1.
Further, CsX and SnX are used in the method for preparing tin-based perovskite powder based on the mechanochemical method4The molar ratio of (A) to (B) is 2: 1.
Further, in the method for preparing the tin-based perovskite powder based on the mechanochemical method, X is one of I, Cl and Br.
Further, CsX and SnX, the method for preparing the tin-based perovskite powder based on the mechanochemical method2、SnX4The granularity range of the product is 30-50nm, and the purity is more than or equal to 99.99 percent.
Further, in the method for preparing the tin-based perovskite powder based on the mechanochemical method, in the step 2), the mass ratio of the ball materials in the ball-milling tank is 1.5-2: 1.
Further, in the method for preparing the tin-based perovskite powder based on the mechanochemical method, in the step 2), the ball milling frequency of the ball mill is 30-40 Hz, and the ball milling time is 4-5 hours.
Further, CsSnX, the method for preparing tin-based perovskite powder based on the mechanochemical method3Or Cs2SnX6The purity is more than or equal to 99 percent, and the granularity is 800-1000 nm.
Compared with the prior art, the invention has the beneficial effects that:
the invention improves the preparation process and adopts the mechanochemical method to prepare the tin-based perovskite (CsSnX)3、Cs2SnX6) High purity, fine crystal grains to reach nanometer grains and excellent powder heat stability.
Drawings
FIG. 1 shows Cs obtained by the present invention2SnI6Powder X-ray diffraction (XRD) pattern.
FIG. 2 shows Cs obtained by the present invention2SnI6Thermogravimetric analysis (TGA) diagram of the powder.
Detailed Description
Example 1
The method for preparing the tin-based perovskite powder based on the mechanochemical method comprises the following steps:
1) under the protection of nitrogen, taking CsI and SnI with the granularity range of 30-50nm and the purity of 99.99 percent2Mixing thoroughly to obtain mixed powder. Wherein CsI and SnI2The molar ratio of (A) to (B) is 1: 1.
2) The mixed powder was poured into a 10ml zirconia ball mill pot containing 10 zirconia balls with a diameter of 8mm, the mass ratio of the balls to the material being 1.5: 1. Ball milling is carried out for 5 hours at the frequency of 30Hz under the protection of nitrogen at room temperature to obtain the CsSnI3The purity of the nano powder is 99.2%, and the granularity is 800-1000 nm.
Example 2
The method for preparing the tin-based perovskite powder based on the mechanochemical method comprises the following steps:
1) under the protection of nitrogen, taking CsCl and SnCl with the granularity range of 30-50nm and the purity of 99.99 percent2Mixing thoroughly to obtain mixed powder. Wherein CsCl and SnCl2The molar ratio of (A) to (B) is 1: 1.
2) The mixed powder was poured into a 10ml zirconia ball mill jar containing 12 zirconia balls 8mm in diameter at a ball to charge mass ratio of 1.75: 1. Ball milling is carried out for 4 hours at the frequency of 40Hz under the protection of nitrogen at room temperature to obtain CsSnCl3The purity of the nano powder is 99.1%, and the granularity is 800-1000 nm.
Example 3
The method for preparing the tin-based perovskite powder based on the mechanochemical method comprises the following steps:
1) under the protection of nitrogen, taking CsBr and SnBr with the granularity range of 30-50nm and the purity of 99.99 percent2Mixing thoroughly to obtain mixed powder.Wherein CsBr and SnBr2The molar ratio of (A) to (B) is 1: 1.
2) The mixed powder was poured into a 10ml zirconia ball mill pot containing 13 zirconia balls with a diameter of 8mm, the mass ratio of the balls to the material being 2: 1. Ball milling is carried out for 4.5 hours at the frequency of 35Hz under the protection of nitrogen at room temperature to obtain CsSnBr3The purity of the nano powder is 99.4%, and the granularity is 800-1000 nm.
Example 4
The method for preparing the tin-based perovskite powder based on the mechanochemical method comprises the following steps:
1) under the atmospheric condition, taking CsI and SnI with the granularity range of 30-50nm and the purity of 99.99 percent4Mixing thoroughly to obtain mixed powder. Wherein CsI and SnI4The molar ratio of (A) to (B) is 2: 1.
2) The mixed powder was poured into a 10ml zirconia ball mill pot containing 11 zirconia balls with a diameter of 8mm, the mass ratio of the balls to the material being 1.5: 1. Ball milling is carried out for 5 hours at the frequency of 30Hz under the protection of nitrogen at room temperature to obtain Cs2SnI6The purity of the nano powder is 99.0%, and the granularity is 800-1000 nm.
Example 5
The method for preparing the tin-based perovskite powder based on the mechanochemical method comprises the following steps:
1) under the atmospheric condition, taking CsCl and SnCl with the granularity range of 30-50nm and the purity of 99.99 percent4Mixing thoroughly to obtain mixed powder. Wherein CsCl and SnCl4The molar ratio of (A) to (B) is 2: 1.
2) The mixed powder was poured into a 10ml zirconia ball mill pot containing 13 zirconia balls 8mm in diameter at a ball to charge mass ratio of 1.75: 1. Ball milling is carried out for 4 hours at the frequency of 40Hz under the protection of nitrogen at room temperature to obtain Cs2SnCl6The purity of the nano powder is 99.3%, and the granularity is 800-1000 nm.
Example 6
The method for preparing the tin-based perovskite powder based on the mechanochemical method comprises the following steps:
1) under atmospheric conditions, the material with particle size of 30-50nm and purity of 99.99% is takenCsBr and SnBr4Mixing thoroughly to obtain mixed powder. Wherein CsBr and SnBr4The molar ratio of (A) to (B) is 2: 1.
2) The mixed powder was poured into a 10ml zirconia ball mill pot containing 14 zirconia balls with a diameter of 8mm, the mass ratio of the balls to the material being 2: 1. Ball milling is carried out for 4.5 hours at the frequency of 35Hz under the protection of nitrogen at room temperature to obtain Cs2SnBr6The purity of the nano powder is 99.4%, the granularity is 800-1000 nm, and an X-ray diffraction (XRD) diagram and a thermogravimetric analysis (TGA) diagram of the powder are respectively shown in a figure 1 and a figure 2.

Claims (7)

1. A method for preparing tin-based perovskite powder based on a mechanochemical method is characterized by comprising the following steps:
1) take CsX and SnX2Or CsX and SnX4Mixing uniformly;
2) putting the mixed material into a ball milling tank in a protective atmosphere at room temperature, and ball milling by using a ball mill to obtain CsSnX3Or Cs2SnX6。
2. The method for preparing tin-based perovskite powder based on mechanochemical method according to claim 1, wherein CsX is mixed with SnX2The molar ratio of (A) to (B) is 1: 1; CsX and SnX4The molar ratio of (A) to (B) is 2: 1.
3. The method for preparing tin-based perovskite powder based on a mechanochemical method according to claim 1, wherein X is one of I, Cl and Br.
4. The method for preparing tin-based perovskite powder based on mechanochemical method according to claim 1, wherein CsX and SnX2、SnX4The granularity range of the product is 30-50nm, and the purity is more than or equal to 99.99 percent.
5. The method for preparing tin-based perovskite powder based on the mechanochemical method according to claim 1, wherein in the step 2), the ball-to-material ratio in the ball milling tank is 1.5-2: 1.
6. The method for preparing tin-based perovskite powder based on the mechanochemical method according to claim 1, wherein in the step 2), the ball milling frequency of the ball mill is 30-40 Hz, and the ball milling time is 4-5 hours.
7. The method for preparing tin-based perovskite powder based on mechanochemical method according to claim 1, wherein CsSnX3Or Cs2SnX6The purity is more than or equal to 99 percent, and the granularity is 800-1000 nm.
CN202110804749.1A 2021-07-16 2021-07-16 Method for preparing tin-based perovskite powder based on mechanochemical method Withdrawn CN113526545A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160122634A1 (en) * 2014-10-31 2016-05-05 Sun Harmonics, Ltd SYNTHESIS OF CsSnI3 BY A SOLUTION BASED METHOD
CN106675559A (en) * 2016-12-27 2017-05-17 南京理工大学 Method for preparing high-stability perovskite composite fluorescent powder by ball milling
WO2019067900A1 (en) * 2017-09-28 2019-04-04 Brown University Titanium (iv)-based halide double-perovskites with tunable 1.0 to 1.8 ev bandgaps for photovoltaic applications
CN109929537A (en) * 2017-12-15 2019-06-25 Tcl集团股份有限公司 Quantum dot and preparation method thereof
CN110526280A (en) * 2019-07-18 2019-12-03 河南大学 A kind of Cs2SnI6Powder and preparation method thereof
CN111924874A (en) * 2020-08-17 2020-11-13 华北理工大学 Preparation method of copper-zinc-tin-based powder
CN112334758A (en) * 2018-04-27 2021-02-05 华盛顿大学 Metal halide semiconductor optical and electronic device and method for manufacturing the same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160122634A1 (en) * 2014-10-31 2016-05-05 Sun Harmonics, Ltd SYNTHESIS OF CsSnI3 BY A SOLUTION BASED METHOD
CN106675559A (en) * 2016-12-27 2017-05-17 南京理工大学 Method for preparing high-stability perovskite composite fluorescent powder by ball milling
WO2019067900A1 (en) * 2017-09-28 2019-04-04 Brown University Titanium (iv)-based halide double-perovskites with tunable 1.0 to 1.8 ev bandgaps for photovoltaic applications
CN109929537A (en) * 2017-12-15 2019-06-25 Tcl集团股份有限公司 Quantum dot and preparation method thereof
CN112334758A (en) * 2018-04-27 2021-02-05 华盛顿大学 Metal halide semiconductor optical and electronic device and method for manufacturing the same
CN110526280A (en) * 2019-07-18 2019-12-03 河南大学 A kind of Cs2SnI6Powder and preparation method thereof
CN111924874A (en) * 2020-08-17 2020-11-13 华北理工大学 Preparation method of copper-zinc-tin-based powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZONGHAN HONG ET AL.: "Completely Solvent-free Protocols to Access Phase-Pure, Metastable Metal Halide Perovskites and Functional Photodetectors from the Precursor Salts", 《ISCIENCE》 *

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Application publication date: 20211022