Visual directional growth device and growth method for large-size bromine-lead-cesium single crystal

A technology of crystal growth and directional growth, which is applied in the directions of single crystal growth, single crystal growth, and crystal growth. Quality and optical transmittance, easy to observe the crystal growth status, good effect of crystal transparency

Active Publication Date: 2019-09-10
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the melt-grown CsPbBr 3 There are still some problems that cannot be ignored in single crystal: (1) CsPbBr 3 Single crystal growth cannot be observed in real time, and parameter adjustments cannot be made according to the real-time growth status. Only after the crystal growth is completed and the temperature is lowered to take out the crystal can it be known whether it has grown into a single crystal; (2) The current melt method grows CsPbBr 3 For spontaneous nucleation, it is easy to generate polycrystalline, which affects the quality of single crystal growth; (3) CsPbBr 3 The crystal has two phase transition points at 89°C and 130°C, and the crystal grown by the melt method will undergo a phase transition during the cooling process, which will easily lead to cracks in the crystal, and the transparency of the grown crystal is poor
Therefore, CsPbBr 3 Single crystal growth still faces many difficulties and challenges, such as the growth process cannot be observed, the crystal size is small, the crystal is easy to crack, the crystal transparency is poor, and the crystal is difficult to grow directional.
[0006] In addition, there is currently no dedicated large-scale CsPbBr 3 Report on Visual Growth Device of Single Crystal

Method used

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  • Visual directional growth device and growth method for large-size bromine-lead-cesium single crystal
  • Visual directional growth device and growth method for large-size bromine-lead-cesium single crystal
  • Visual directional growth device and growth method for large-size bromine-lead-cesium single crystal

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Experimental program
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Effect test

Embodiment 1

[0050] One for large size CsPbBr 3 A device for visual directional growth of single crystals, with a structure such as figure 1 As shown, it includes a body of furnace and a rotary descending system. The body of furnace includes a quartz furnace tube 4 and a heating device. The cavity in the quartz furnace tube is a crystal growth chamber, and the heating device is arranged outside the quartz furnace tube 4. The outer jacket of the heating device is provided with an insulating sleeve 6, the insulating sleeve 6 is a transparent quartz tube, the inner wall of the transparent quartz tube is coated with a gold layer, and the insulating sleeve is close to the heating device; the wall thickness of the transparent quartz tube is 2 mm to 5 mm; The translucent insulation sleeve is convenient for observing the growth status in the furnace during the crystal growth process; at the same time, the gold layer can reflect the heat generated by the heater to the center of the furnace body to ...

Embodiment 2

[0054] One for large size CsPbBr 3 The visual directional growth device of a single crystal is the same as that in Example 1, except that the length of the seed crystal bag is 20mm and the inner diameter is 6mm; the angle of the funnel-shaped shoulder area is 60°; the inner diameter of the equal-diameter area determines the growth of the crystal. outside diameter.

Embodiment 3

[0056] A kind of utilizing the device of embodiment 1 to grow large size CsPbBr 3 The method for a single crystal comprises the following steps:

[0057] Step 1: Cleaning the Crystal Growth Crucible

[0058] (a) Preliminary rinsing of the quartz crucible is carried out with deionized water;

[0059] (b) immerse the rinsed quartz crucible in a hydrofluoric acid solution with a concentration of 10% for 1 hour, and then rinse the quartz crucible soaked in hydrofluoric acid with deionized water;

[0060] (c) Soak the washed quartz crucible with absolute ethanol and ultrasonically for 2 hours, then rinse it with deionized water;

[0061] (d) drying the quartz crucible in a vacuum oven for crystal growth;

[0062] Step 2: The a-direction CsPbBr for orientation processing 3 The seed crystal is placed in the seed crystal bag at the bottom of the crystal growth crucible, and then 220g CsPbBr 3 The polycrystalline material is placed in the crystal growth crucible, and the vacuum is...

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Abstract

The invention relates to a visual directional growth device and a growth method for a large-size bromine-lead-cesium single crystal. The device comprises a furnace body and a rotary descending system,wherein the furnace body comprises a quartz furnace tube and a heating device, a cavity in the quartz furnace tube is a crystal growth cavity, the heating device is arranged outside the quartz furnace tube, a heat insulation sleeve is sleeved outside the heating device of the quartz furnace tube, a crystal growth crucible is arranged in the crystal growth cavity, the bottom of the crystal growthcrucible is a seed crystal bag, and CsPbBr3 seed crystals are arranged in the seed crystal bag; and the rotary descending system comprises a long crystal rod and a driving device for driving the longcrystal rod to rotate and descend, and the seed crystal bag is fixed on the long crystal rod. The CsPbBr3 single crystal obtained by the visual directional growth device is large in size and good in crystal transparency, and the device is beneficial to discharging of impurities in the crystal growth process, and adopts a slow cooling rate to prevent the crystal from cracking.

Description

technical field [0001] The invention relates to a visual directional growth device and a growth method for large-size bromine-lead-cesium single crystals, belonging to the technical field of crystal growth. Background technique [0002] In recent years, halogen perovskite materials have shown broad application prospects in the fields of solar cells, light-emitting diodes, photoelectric detection, and nuclear radiation detection. Compared with organic-inorganic composite halogen perovskite materials, the all-inorganic halide perovskite crystal bromide lead cesium (molecular formula: CsPbBr 3 ) has excellent characteristics of insensitivity to temperature, light and moisture in the air, and the stability of materials and devices is better. [0003] Cesium lead bromide (CsPbBr 3 ) single crystal has the following advantages as a room temperature nuclear radiation detector material: CsPbBr 3 The crystal has a large atomic number (Pb: 82, Cs: 55, Br: 35), and a moderate band g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/12C30B11/00C30B11/06
CPCC30B11/00C30B11/002C30B11/06C30B29/12
Inventor 张国栋张鹏李想陶绪堂
Owner SHANDONG UNIV
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