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Preparation method of bismuth copper iodide crystal

A technology of copper crystal and crystal furnace, which is applied in the field of preparation of iodine-bismuth-copper crystals, can solve problems such as explosions and a large number of exothermic crucibles, and achieve the effects of overcoming technical bottlenecks, reducing component segregation, and avoiding errors

Active Publication Date: 2020-08-11
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the first step, the iodine-bismuth-copper polycrystalline material is synthesized by segmental heating in a swing furnace, which solves the problem of a large amount of exothermic heat in the traditional solution preparation process of the polycrystalline material and the problem that the crucible is likely to explode due to too large a vapor pressure. The second step uses the original Bit solidification growth technology successfully grows high-quality iodine-bismuth-copper crystals without taking out the crucible, breaking through the technical barriers in the growth process of iodine-bismuth-copper crystals

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  • Preparation method of bismuth copper iodide crystal

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Embodiment 1

[0031] A preparation method of iodine bismuth copper crystal, comprising the steps of:

[0032] 1) Preparation of iodine bismuth copper polycrystalline material; the preparation process includes the following steps:

[0033] ①Weigh copper powder, bismuth powder and iodine particles with a purity greater than or equal to 99.99% in a dark room according to the molar ratio Cu:Bi:I=1:1:4.

[0034] ②In the darkroom, mix 5.7019g copper powder and 18.7516g bismuth powder evenly, put 45.5465g iodine particles into the mortar for grinding, then put the copper-bismuth mixture into the bottom of the quartz crucible, put the ground iodine particles into The upper layer of the quartz crucible; wrap the outside of the quartz crucible with tin foil to avoid light, and then vacuumize and seal the quartz crucible with the raw materials, so that the vacuum degree in the quartz crucible is 1×10 -1 Pa. The quartz crucible used has a wall thickness of 1 mm and a tip with an angle of 30° at the b...

Embodiment 2

[0041] A preparation method of iodine bismuth copper crystal, comprising the steps of:

[0042] 1) Preparation of iodine bismuth copper polycrystalline material; the preparation process includes the following steps:

[0043] ①Weigh copper powder, bismuth powder and iodine particles with a purity greater than or equal to 99.99% in a dark room according to the molar ratio Cu:Bi:I=1:1:4. The raw materials are cuprous iodide and bismuth iodide. A quartz crucible with a wall thickness of 1.2 mm is prepared, and a tip with an angle of 40° is provided at the bottom thereof, and a seed well for placing a seed crystal is also provided at the bottom of the quartz crucible. The iodine-bismuth-copper crystal that spontaneously nucleates and grows is ground into a cylinder with a length of 60 mm and a diameter of 2 mm in the direction of as a seed crystal, and the seed crystal is placed in the seed well of a quartz crucible in advance.

[0044] ②In the darkroom, mix 5.7019g copper powde...

Embodiment 3

[0051] A preparation method of iodine bismuth copper crystal, comprising the steps of:

[0052] 1) Preparation of iodine bismuth copper polycrystalline material; the preparation process includes the following steps:

[0053] ① Weigh cuprous iodide and bismuth iodide with a purity greater than or equal to 99.99% at a molar ratio of Cu:Bi=1:1 in a dark room. Prepare a quartz crucible with a wall thickness of 1.5 mm, and a tip with an angle of 45° is provided at the bottom of the quartz crucible, and a seed well for placing a seed crystal is also provided at the bottom of the quartz crucible. The iodine-bismuth-copper crystal that spontaneously nucleates and grows is ground into a cylinder with a length of 60 mm and a diameter of 2 mm in the direction of as a seed crystal, and the seed crystal is placed in the seed well of a quartz crucible in advance.

[0054] ②In the darkroom, put the weighed cuprous iodide under the quartz crucible, put the weighed bismuth iodide into the up...

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Abstract

The invention discloses a preparation method of a bismuth copper iodide crystal. The preparation method comprises the steps of preparation of a bismuth copper iodide polycrystalline material and growth of the bismuth copper iodide crystal. The preparation method comprises the following steps: weighing raw materials according to a stoichiometric ratio, putting the raw materials into a quartz crucible, vacuumizing and sealing the quartz crucible, and setionally heating the quartz crucible in a rocking furnace to obtain the bismuth copper iodide polycrystalline material; and then putting the quartz crucible filled with the polycrystalline material into a crystal furnace for crystal growth to finally obtain the bismuth copper iodide crystal. The bismuth copper iodide crystal is successfully grown by adopting the two-step method using the rocking furnace and the crystal furnace, the size of the obtained bismuth copper iodide crystal is 17 * 80 mm, the technical bottleneck of existing bismuth copper iodide crystal growth is overcome, the technical problem that the bismuth copper iodide crystal cannot successfully grow is solved, and a new thought is provided for the growth of the bismuthcopper iodide crystal.

Description

technical field [0001] The invention relates to the technical field of crystal growth, in particular to a preparation method of iodine bismuth copper crystal. Background technique [0002] Perovskite materials are a class of calcium titanate (CaTiO 3 ) A series of compound materials with the same crystal structure, because of their excellent photoelectric properties such as large light absorption coefficient, high carrier mobility, long diffusion length, low exciton binding energy, photoluminescence, electroluminescence, etc. performance and better thermoelectric performance has become a popular research material. And because of its simple preparation, low production cost and other characteristics, it is widely used in various devices. At this stage, more and more attention is paid to the problem of energy shortage. Because perovskite materials can be widely used in solar cell devices, they have become an indispensable basic material for obtaining green and renewable energ...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B11/02
CPCC30B11/002C30B11/02C30B29/12
Inventor 孙瑞徐家跃申慧
Owner SHANGHAI INSTITUTE OF TECHNOLOGY
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