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Preparation method of bromine-lead-cesium single crystals

A bromine-lead-cesium single crystal technology is applied in the field of preparation of bromine-lead-cesium single crystals for room temperature nuclear radiation detectors. The effect of single crystal cracking

Active Publication Date: 2016-04-13
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the above defects or improvement needs of the prior art, the present invention provides a method for preparing a bromine-lead-cesium single crystal, the purpose of which is to solve the problems of easy adhesion and cracking in the preparation of bromine-lead-cesium cesium

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  • Preparation method of bromine-lead-cesium single crystals
  • Preparation method of bromine-lead-cesium single crystals
  • Preparation method of bromine-lead-cesium single crystals

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Embodiment 1

[0060] Embodiment 1 is 8mm with diameter, and the preparation of the bromine-lead-cesium single crystal that length is 50mm is an example illustration;

[0061] In embodiment 1, adopt internal diameter to be the cylindrical quartz ampoule of 8mm, one end is the conical shape that cone angle is 20 °; The preparation process of bromine lead cesium single crystal among the embodiment 1 is set forth in detail below;

[0062] Step 1: Clean the quartz ampoule as follows:

[0063] (1.1) Soak the quartz ampoule with aqua regia (concentrated hydrochloric acid:concentrated nitric acid=3:1) for 24 hours, and rinse the soaked ampoule with deionized water above 10MΩ;

[0064] (1.2) Soak the washed quartz ampoule with 5% dilute hydrofluoric acid for 24 hours; and rinse the soaked ampoule with deionized water above 10 MΩ;

[0065] (1.3) Soak the quartz ampoule treated in step (1.2) with acetone for 24 hours; and ultrasonically clean the quartz ampoule after soaking in acetone for 3 hours (r...

Embodiment 2

[0074] Embodiment 2 is 12mm with diameter, and the preparation of the bromine-lead-cesium single crystal that length is 50mm is illustrated as an example;

[0075] In embodiment 2, adopt internal diameter to be the cylindrical quartz ampoule of 12mm, and one end thereof is the conical shape that taper angle is 20 °; The preparation process of bromine lead cesium single crystal among the embodiment 2 is set forth in detail below;

[0076] In embodiment 2, the cleaning of the quartz ampoule in step 1 and the process of coating the inner wall of the quartz ampoule in step 2 are the same as in embodiment 1;

[0077] Step 3: Add 15.7gCsPbBr 3 Put the powder into a quartz ampoule, and vacuumize the quartz ampoule to 10 -3 pa and seal; the quartz ampoule is naturally vertically suspended in a dual temperature zone vertical tube furnace with a high temperature resistant wire, the conical tip of the quartz ampoule points to the bottom of the furnace, the conical tip of the ampoule is 20...

Embodiment 3

[0084] Embodiment 3 is illustrated with the preparation of the bromine-lead-cesium single crystal that is 15mm in length and 50mm in length;

[0085] In embodiment 3, adopt internal diameter to be the cylindrical quartz ampoule of 15mm, and one end thereof is the conical shape that taper angle is 20 °; The preparation process of bromine lead cesium single crystal among the embodiment 2 is set forth in detail below;

[0086] In embodiment 3, step 1 is the same as embodiment 1 to the clear and step 2 process of coating the inner wall of quartz ampoule to quartz ampoule;

[0087] Step 3: Add 30.0 g of CsPbBr 3 Put the powder into a quartz ampoule, and vacuumize the quartz ampoule to 10 -3 pa and seal; the quartz ampoule is naturally vertically suspended in a dual temperature zone vertical tube furnace with a high temperature resistant wire, the conical tip of the quartz ampoule points to the bottom of the furnace, the conical tip of the ampoule is 200mm from the bottom of the fu...

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Abstract

The invention discloses a preparation method of bromine-lead-cesium single crystals. An ampoule which is plated with a carbon film and comprises a conical tip carries bromine-lead-cesium powder. The method specifically includes the following steps of vacuumizing and sealing the ampoule; heating the ampoule in a gradient mode in the direction from the conical tip to the top end of bromine-lead-cesium powder so that bromine-lead-cesium powder placed in the ampoule can be sufficiently molten; cooling the ampoule at a low speed till the temperature of the top end of bromine-lead-cesium powder is 0-5 DEG C lower than the solidifying point of bromine-lead-cesium, conducting heat preservation, and completing growth of bromine-lead-cesium single crystals; cooling bromine-lead-cesium single crystals in a staged mode, wherein bromine-lead-cesium single crystals are rapidly cooled through the first stage of rapid cooling, and bromine-lead-cesium single crystal phase change conversion is achieved through the second stage of slow cooling. According to the preparation method of bromine-lead-cesium single crystals, different cooling speeds are adopted in single crystal growth and single crystal cooling, the staged cooling method is adopted, the growth quality and the growth cycle of crystals are considered at the same time, and the problem that in the prior art, because of internal stress, bromine-lead-cesium single crystals crack in the single crystal preparation process is effectively solved.

Description

technical field [0001] The invention belongs to the technical field of single crystal growth, and more specifically relates to a method for preparing a bromine-lead-cesium single crystal for a room-temperature nuclear radiation detector. Background technique [0002] Since the successful nuclear test in the last century, the application of nuclear technology has expanded from military use to civilian use, involving various fields of scientific research, national economy and social life, and nuclear detection technology is also developing rapidly. Cesium lead bromide (CsPbBr 3 ) single crystal has the following advantages as a room temperature nuclear radiation detector material: [0003] (1) It has a wide band gap (2.25eV), ensuring that CsPbBr 3 Single crystal has high resistivity and low leakage current, and the detector can be used normally at or above room temperature; [0004] (2) Electrons and holes have high carrier mobility lifetime products of the same order of m...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B11/02
CPCC30B11/02C30B29/12
Inventor 郑志平傅邱云周东祥胡云香罗为张明智何健乐
Owner HUAZHONG UNIV OF SCI & TECH
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