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Method for preparing colorless corundum monocrystal

A single crystal and corundum technology, applied in the field of crystal growth, can solve problems such as difficulty in meeting high-performance requirements, unstable crystal single crystal quality, and limited crystal size, so as to ensure crystal growth quality, shorten processing time, and reduce stress defects. effect of density

Active Publication Date: 2012-10-31
登封市蓝天石化光伏电力装备有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its advantage is that the equipment requirements are simple and the yield is high. The disadvantage is that the crystal size is limited, the crystal single crystal quality is unstable, and the dislocation density is high.
[0009] However, when these preparation methods are produced in industrialized batches, there is crystal impurity pollution, the crystal single crystal quality is unstable, and the crystal size is limited. It is difficult to meet the high-performance requirements of components such as military fields, optics, and semiconductors. long

Method used

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  • Method for preparing colorless corundum monocrystal
  • Method for preparing colorless corundum monocrystal

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Experimental program
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Effect test

Embodiment 1

[0034] The preparation method of the colorless corundum single crystal of this embodiment includes the following sequential steps:

[0035] 1) Raw material pretreatment: Place a cylindrical polycrystalline alumina block with a diameter of Φ180mm, a height of 240mm, and a weight of 30.2kg in the center of the crucible in the crystal growth furnace. The polycrystalline alumina block accounts for 95% of the total feeding. , and then 1.59kg of polycrystalline alumina pellets with a purity of Φ1mm greater than 99.996% were used to fill the gaps in the crucible, with a total weight of 31.79kg; -3 pa) at a rate of 600°C / h to 2150°C, the alumina reaches a molten state and remains in a vacuum environment;

[0036] 2) Cleaning and seed crystal: uniformly cool down at a rate of 20°C / h for 4 hours to cool the temperature of the alumina solution to 2070°C, and place the seed crystal (the diameter of the seed crystal is Φ10mm, the length is 120mm, and the crystal orientation is a direction ...

Embodiment 2

[0042] The preparation method of the colorless corundum single crystal of this embodiment includes the following sequential steps:

[0043] 1) Raw material pretreatment: Place a cylindrical polycrystalline alumina block with a diameter of Φ200mm, a height of 250mm, and a weight of 38.2kg in the center of the crucible in the crystal growth furnace. The polycrystalline alumina block accounts for 93% of the total feed. , and then 2.87kg of polycrystalline alumina particles with a purity of Φ2mm greater than 99.996% were evenly stirred, and the gaps in the crucible were filled, with a total weight of 41.07kg; -3 pa) at a rate of 800°C / h to 2150°C, the alumina reaches a molten state and remains in a vacuum environment;

[0044] 2) Cleaning and seeding: uniform cooling at a rate of 25°C / h for 3.1 hours to cool the temperature of the alumina solution to 2070°C, and the seed crystal (the diameter of the seed crystal is Φ12mm, the length is 130mm, and the crystal orientation is a direc...

Embodiment 3

[0050] The preparation method of the colorless corundum single crystal of this embodiment includes the following sequential steps:

[0051] 1) Raw material pretreatment: Place a cylindrical polycrystalline alumina block with a diameter of Φ250mm, a height of 340mm, and a weight of 59.2kg in the center of the crucible in the crystal growth furnace. The polycrystalline alumina block accounts for 92% of the total input , and then use 5.14kg of 5mm polycrystalline alumina pellets with a purity greater than 99.996% to fill the gap in the crucible, with a total weight of 64.34kg; -3 pa) at a rate of 500°C / h to 2150°C, the alumina reaches a molten state and remains in a vacuum environment;

[0052] 2) Cleaning and seeding: uniform cooling at a rate of 15°C / h for 5.1 hours to cool the temperature of the alumina solution to 2070°C, and the seed crystal (the diameter of the seed crystal is Φ16mm, the length is 140mm, and the crystal orientation is a direction ± 0.1°) to sink to 40mm be...

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Abstract

The invention discloses a method for preparing colorless corundum monocrystal and a special corundum crystal growth furnace structure. The preparation method comprises steps of preprocessing raw materials, cleaning, seeding crystal, enabling the crystal to grow through a Czochralski method, enabling the crystal to grow freely, performing in situ annealing and a cooling treatment and finally obtaining the colorless corundum monocrystal. By the aid of the method, the Czochralski method is combined with a Kyropoulos method in a creative way, a stable temperature gradient environment which meets crystal growth requirements is provided by a corundum crystal growth furnace, the quality of prepared crystal monocrystal is good, the success ratio of the crystal growth exceeds 90%, and the method is suitable to industrial production, convenient, energy-saving, safe and reliable.

Description

technical field [0001] The invention relates to a preparation method of a colorless corundum single crystal, in particular to a growth method of an industrial corundum single crystal, and belongs to the technical field of crystal growth. Background technique [0002] The main component of corundum is alumina (Al 2 o 3 ). It is a crystalline material whose hardness is second only to diamond in nature. The oxygen atoms in its structure are arranged in a manner close to HCP (hexagonal closed packed), and about 2 / 3 of the gaps between the octahedral coordination between the oxygen atoms are filled with aluminum atoms, which makes it have high strength and hardness (Mohs hardness 9), high temperature resistance (melting point up to 2050 ° C), strong abrasion resistance, corrosion resistance, stable chemical properties, generally insoluble in water, not subject to acid corrosion, only at high temperatures (above 3000 ° C) can be used for Hydrofluoric acid (HF), phosphoric acid...

Claims

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Application Information

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IPC IPC(8): C30B15/20C30B15/00C30B29/20
Inventor 张博赵东
Owner 登封市蓝天石化光伏电力装备有限公司
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