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Preparation method of bromine-lead-cesium monocrystal by horizontal moving zone melting

A technology of horizontal movement, bromine lead cesium, which is applied in the field of melting preparation of horizontal movement zone of bromine lead cesium single crystal, can solve the problems of large phase transformation stress and easy cracking, and achieves low thermal stress, small mechanical vibration, and few cracks. Effect

Active Publication Date: 2018-06-22
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] 1) Solve CsPbBr 3 The problem of large phase transition stress and easy cracking during crystal growth

Method used

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  • Preparation method of bromine-lead-cesium monocrystal by horizontal moving zone melting
  • Preparation method of bromine-lead-cesium monocrystal by horizontal moving zone melting
  • Preparation method of bromine-lead-cesium monocrystal by horizontal moving zone melting

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Ampoule preparation

[0034] Ampoule wash.

[0035] (a) Soak in concentrated nitric acid with a mass fraction of 68wt% for 48h, then clean the soaked ampoule with deionized water above 10MΩ;

[0036] (b) Soak in acetone solution for 48h, then clean the soaked ampoule with deionized water above 10MΩ;

[0037] (c) Clean the ampoule ultrasonically with deionized water above 10 MΩ.

[0038] Ampoule coated with carbon. The ampoule after cleaning is dried, and a layer of carbon film is coated on the inner wall. Its carbon plating process adopts nitrogen gas with a purity of 99.999% at a rate of 110mL / s at 1150°C as a carrier gas, and then maintains the original speed to continue to feed the carrier gas at a speed of 60mL / s with a purity of 99.999% after stabilization. The methane continued for 20 minutes, and then the temperature of the carbon coating device was lowered to room temperature to obtain a carbon coated ampoule. After the carbon plating is completed, take...

Embodiment 2

[0044] (1) Ampoule preparation

[0045] Ampoule wash.

[0046] (a) Soak in concentrated nitric acid with a mass fraction of 68wt% for 48h, then clean the soaked ampoule with deionized water above 10MΩ;

[0047] (b) Soak in acetone solution for 48h, then clean the soaked ampoule with deionized water above 10MΩ;

[0048] (c) Clean the ampoule ultrasonically with deionized water above 10 MΩ.

[0049] Ampoule coated with carbon. The ampoule after cleaning is dried, and a layer of carbon film is coated on the inner wall. Its carbon plating process adopts nitrogen gas with a purity of 99.999% at a rate of 110mL / s at 1150°C as a carrier gas, and then maintains the original speed to continue to feed the carrier gas at a speed of 60mL / s with a purity of 99.999% after stabilization. The methane continued for 20 minutes, and then the temperature of the carbon coating device was lowered to room temperature to obtain a carbon coated ampoule. After the carbon plating is completed, take...

Embodiment 3

[0055] (1) Ampoule preparation

[0056] Ampoule wash.

[0057] (a) Soak in concentrated nitric acid with a mass fraction of 68wt% for 48h, then clean the soaked ampoule with deionized water above 10MΩ;

[0058] (b) Soak in acetone solution for 48h, then clean the soaked ampoule with deionized water above 10MΩ;

[0059] (c) Clean the ampoule ultrasonically with deionized water above 10 MΩ.

[0060] Ampoule coated with carbon. The ampoule after cleaning is dried, and a layer of carbon film is coated on the inner wall. Its carbon plating process adopts nitrogen gas with a purity of 99.999% at a rate of 80mL / s at 1150°C as a carrier gas. After stabilization, the original speed is maintained to continue to feed the carrier gas, and the purity is 99.999% at a rate of 40mL / s. The methane continued for 20 minutes, and then the temperature of the carbon coating device was lowered to room temperature to obtain a carbon coated ampoule. After the carbon plating is completed, take out...

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Abstract

The invention discloses a preparation method of a bromine-lead-cesium monocrystal by horizontal moving zone melting. The preparation method specifically comprises the following steps: (1) placing a quartz ampoule in a reaction furnace chamber, and introducing methane to carry out carbon film plating treatment to obtain a carbon-plated ampoule; (2) loading bromine-lead-cesium powder into the carbon-plated ampoule, carrying out vacuumizing and sealing, and placing the ampoule in a heat treatment furnace to melt the bromine-lead-cesium powder first, and then cooling and solidifying the product toform a polycrystalline material rod; and (3) placing the sealed ampoule containing the polycrystalline material rod in a horizontal moving zone melting furnace, heating a heater to 620-650 DEG C, andmoving the heater from the tip of the sealed ampoule to the tail end of the sealed ampoule, thereby completing the growth of a bromine-lead-cesium crystal and obtaining the bromine-lead-cesium crystal. The preparation method provided by the invention can effectively solve the problems of large mechanical vibration, high thermal stress in the crystal, difficulty in growing a large-size bromine-lead-cesium monocrystal and the like in a crystal growth process compared with the prior art by improving the key integral flow process design, and reaction conditions and parameters of each step.

Description

technical field [0001] The invention belongs to the field of crystal growth, more specifically, relates to a cesium lead bromide (CsPbBr 3 ) single crystal by horizontal moving zone melting preparation method, the prepared bromine lead cesium single crystal can be widely used in high-energy ray sensing, energy, LED display and other fields. Background technique [0002] High-energy nuclear radiation detector materials and their detection technologies have been widely used in many fields, such as astrophysics, security, military, medical, nuclear industry and environmental monitoring. With the continuous improvement of detection accuracy and sensitivity requirements in application scenarios, higher requirements are also put forward for materials used in nuclear radiation detectors. [0003] The materials used in the preparation of high-energy nuclear radiation detectors generally have the following characteristics: large band gap, high atomic number, high density, and high c...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B28/06C30B13/14C30B13/28
CPCC30B13/14C30B13/28C30B28/06C30B29/12
Inventor 郑志平傅邱云周东祥罗为陈成张明智张森
Owner HUAZHONG UNIV OF SCI & TECH
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