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A kind of preparation method of perovskite type compound

A perovskite type and compound technology, applied in the direction of tin halide, etc., can solve the problems of harsh process conditions, expensive raw materials, and impure products, and achieve the effects of simple synthesis process, simple process reduction, and convenient operation

Inactive Publication Date: 2017-07-14
SHANGHAI ZAOFU NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of expensive raw materials, harsh process conditions, impure products and difficult separation problems in the current preparation method of trihalide tin cesium CsSnX3 (X represents Cl, Br or I), the first purpose of the present invention is to propose a "Four-step" preparation method

Method used

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  • A kind of preparation method of perovskite type compound
  • A kind of preparation method of perovskite type compound
  • A kind of preparation method of perovskite type compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation method of perovskite type compound, specifically the method for preparing tin cesium trihalide, its technological process is as follows figure 1 As shown, the specific steps are as follows:

[0050] Preparation of High Purity CsSnI3 Solid

[0051] 1. Synthesis of CsSnI3 (Cs2SnI6):

[0052] 1) Reaction formula:

[0053] SnI2+CsI---------CsSnI3

[0054] SnI4 (a small amount)+2CsI--------Cs2SnI6 (a small amount)

[0055] 2) specific method

[0056] First, commercialized SnI2 (0.01 mol, 3.725 g) and CsI (0.01 mol, 2.598 g) were mixed in equimolar amounts, placed in a heating tube with a switch, and vacuumed for 40 minutes to remove the moisture in the tube React with air at 500°C for 45 minutes, then control the temperature and slowly cool down to room temperature within 5 hours to obtain a black solid. The material was used directly in the next preparation without treatment. Yield 100%. According to XRD analysis, the substance is composed of CsSnI3 ...

Embodiment 2

[0074] Preparation of High Purity CsSnBr3

[0075] 1. Synthesis of CsSnBr3 (Cs2SnBr6):

[0076] 1) Reaction formula:

[0077] SnBr2+CsBr---------CsSnBr3

[0078] SnBr4 (a small amount)+2CsB--------Cs2SnBr6 (a small amount)

[0079] 2) specific method

[0080] Similar to step 1(2) of Example 1. The difference is that the reactant SnBr2 replaces SnI2, and CsBr replaces CsI, wherein the amount of commercialized SnBr2 is 0.01 mole, 2.785 grams, and the amount of CsBr is 0.01 mole, 2.128 grams.

[0081] 2. Synthesis of CsSnBr3(Sn):

[0082] 1) Reaction formula:

[0083] CsSnBr3+Sn (excess) ------ no reaction

[0084] Cs2SnBr6 (a small amount) + Sn (excessive) ---- 2CsSnBr3 + Sn (excessive)

[0085] 2) Specific methods:

[0086] The mixture (5.0 grams) of CsSnBr3 (Cs2SnBr6) obtained above was added with a small amount of Sn powder (0.1 grams), and placed in a heating tube together, and reacted at 450 degrees under vacuum for 30 minutes, and then slowly within 3 hours. Afte...

Embodiment 3

[0098] Preparation of High Purity CsSnCl3

[0099] 1. Synthesis of CsSnCl3 (Cs2SnCl6):

[0100] 1) Reaction formula:

[0101] SnCl2+CsCl---------CsSnCl3

[0102] SnCl4 (a small amount)+2CsCl-------Cs2SnCl6 (a small amount)

[0103] 2) specific method

[0104] First, commercialized SnCl2 (0.01 mol, 1.896 g) and CsCl (0.01 mol, 1.684 g) were mixed in equimolar amounts, placed in a heating tube with a switch, and vacuumed for 30 minutes to remove moisture in the tube With air, react at 550 degree temperature for 60 minutes, then control the temperature and slowly cool down to room temperature within 4 hours to obtain a black solid substance. The material was used in the next preparation without treatment. Yield 100%. According to XRD analysis, the substance is composed of CsSnCl3 and Cs2SnCl6.

[0105] 2. Synthesis of CsSnCl3(Sn):

[0106] 1) Reaction formula:

[0107] CsSnCl3+Sn (excess) ------ no reaction

[0108] Cs2SnCl6 (a small amount) + Sn (excessive) ---- 2CsSnC...

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Abstract

The present invention relates to a kind of preparation method of perovskite type compound, adopts four-step method, comprises the synthesis of CsSnX3 (Cs2SnX6), the synthesis of CsSnX3 (Sn), the removal of tin in CsSnX3 (Sn), the preparation of high-purity CsSnX3, in addition A preparation and sealing method of a cesium trihalide tin cesium CsSnX3 liquid is also proposed. The invention solves the problems of expensive raw materials, harsh process conditions, impure products and difficult separation in the current preparation method of trihalide tin cesium CsSnX3, and can obtain high-quality products without using high-purity raw materials and harsh purification processes. And the process is simple, not only suitable for laboratory preparation, but also suitable for industrial batch production.

Description

technical field [0001] The invention belongs to the field of optoelectronic materials, and in particular relates to a preparation method of a perovskite compound, in particular a method for preparing tin cesium trihalide is disclosed. Background technique [0002] The earliest discovered perovskite is a kind of ceramic oxide, its general molecular formula is ABO3, and it is in the shape of cube or octahedron. Such oxides are present in the calcium titanate CaTiO3 compound in perovskite, hence the name. Due to the many characteristics of the structure of this kind of compound, it is widely used and studied in condensed matter physics. [0003] Cesium trihalide tin cesium is a kind of perovskite inorganic compound, it is the collective name of cesium triiodide tin cesium (CsSnI3) and its analogues, the analogues of triiodide tin cesium CsSnI3 are mainly tribromotin iodide CsSnBr3, trichlortin Iodine CsSnCl3 and mixed trihalide tin iodide (CsSnBr2I, CsSnBr2Cl, CsSnI2Br, etc.)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/04
Inventor 黄福新
Owner SHANGHAI ZAOFU NEW MATERIAL TECH CO LTD
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