Method for growing large-size fluoride crystals through top seed crystal kyropoulos method

A technology of fluoride and foaming method, applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., can solve the problems of invisible growth process, slow crystal growth, long growth cycle, etc., to achieve visible and controllable growth process, The effect of high crystal quality and short growth cycle

Inactive Publication Date: 2013-07-24
江苏国晶光电科技有限公司
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Problems solved by technology

However, this method cannot observe seed crystal inoculation and the entire growth process, and cannot be adjusted in real time during the growth process, and the growth cycle is long (in 2003, Schott Lithotec, Germany, successfully grew Φ350mm×100mm CaF2 crystals by using the improved crucible drop method. , the growth period is 2 months);
[0006] The temperature gradient method can avoid the complex convection and temperature fluctuation of the solid-liquid interface caused by the interference of the irregular mechanical vibration source, so the quality of the grown crystal and the s

Method used

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Embodiment Construction

[0030] The present invention will be further described below. The following examples are only used to illustrate the technical solution of the present invention more clearly, but not to limit the protection scope of the present invention.

[0031] In this example, to grow CaF 2 (calcium fluoride) crystal as an example, the method for growing large-size fluoride crystals by the top seed crystal kyroplasty method is illustrated, and the rest of the fluoride crystals are the same as this process. The method includes the following steps:

[0032] 1. Pretreatment of raw materials

[0033] The raw material preparation process is as follows: use high-precision electronic balance to accurately weigh high-purity (5N) CaF 2 and PbF 2 (Oxygen scavenger) powder, generally PbF 2 The amount of CaF 2 1-2wt% of the total amount, if growing doped calcium fluoride crystals, add the corresponding doped ion fluoride raw material according to the designed doping amount, weigh and mix in the m...

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Abstract

The invention discloses a method for growing large-size fluoride crystals through a top seed crystal kyropoulos method. The method comprises the following steps: weighing and mixing fluoride crystals and deoxidant powder, and pressing a mixture to form a block; drying the pressed block; putting the block into a crucible, sequentially installing thermal field components and installing seed crystals; vacuumizing, and heating to smelt the material until observing that the block is molten; descending the seed crystals to contact with a melting liquid level so as to slightly melt the seed crystals, pulling seed crystal rods and growing the block on the seed crystals in a condensation manner; after finishing crystal seeding, entering a shouldering period at power reduction, maintaining the crystals rotating and keeping the crystal pulling speed in the period, gradually increasing the diameters of the crystals in an upward pulling process, and entering an isometrical growth period until the crystal growth is finished; and cooling and annealing after the crystal weight reaches the feed weight. The method is low in growth cost and short in growth period; the method is suitable for large-size fluoride crystals, and the fluoride crystals grow in a vacuum condition without oxygen impurities; and the growth process is visible and controllable, so that the crystal quality is improved.

Description

technical field [0001] The invention relates to a method for growing large-sized fluoride crystals by the top seed crystal kyrophoroplasty method. Background technique [0002] Alkaline-earth fluoride crystal is a traditional crystal material. Because of its excellent optical and physical and chemical properties, as well as unique structural characteristics, it has always played a very important role in both industrial applications and scientific research. And with the development of human science and technology, new application prospects are constantly emerging. In terms of industrial applications, alkaline earth fluoride crystals have a wide range of transmission wavelengths and are used as window materials in the vacuum ultraviolet to infrared bands. At the same time, the low refractive index and low dispersion characteristics make alkaline earth fluoride crystals become excellent achromatic and apochromatic lens materials, and are widely used in ultraviolet lithography,...

Claims

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Application Information

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IPC IPC(8): C30B17/00C30B29/12
Inventor 王庆国钱兵朱烨汪红卫鞠星李倩
Owner 江苏国晶光电科技有限公司
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