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Growth method of calcium fluoride single crystal and used device

A growth method, calcium fluoride technology, applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems of small single crystal rate of stress birefringence, low single crystal yield, high crystal structure requirements, etc., to achieve Improved yield and crystal quality, low stress birefringence, and high single crystal transmittance

Pending Publication Date: 2020-06-12
秦皇岛本征晶体科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, calcium fluoride can be grown by the crucible drop method or the pulling method. During the growth process of the crucible drop method, the melt contacts the inner wall of the crucible. Since the calcium fluoride single crystal belongs to the cubic crystal system, it is very easy to crystallize. On the surface, it is easy to generate multiple crystal nuclei, and the yield of single crystal is low; during the growth process of the pulling method, the crystal and the crucible wall do not contact, and the seed crystal with good structure can be used for directional growth. The crystal grown by this method has small stress birefringence, single High crystal rate and other advantages, but the growth method with a single heater is commonly used in the pulling method. The temperature gradient in the crystal furnace is uncontrollable, and it is difficult to obtain an ideal temperature range. At the same time, the crystallization rate and crystal orientation of each crystal nucleus are different in the growth process of a single heater Defects such as polycrystals or dislocations
Calcium fluoride windows for excimer lasers have high requirements on the crystal structure, and crystals with structural defects usually have poor performance and cannot be used

Method used

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  • Growth method of calcium fluoride single crystal and used device
  • Growth method of calcium fluoride single crystal and used device
  • Growth method of calcium fluoride single crystal and used device

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A method for growing a calcium fluoride single crystal, using calcium fluoride as a raw material, and using a crucible pulling method to grow a calcium fluoride single crystal, wherein the device used in the crucible pulling method is provided with a side heater on the side of the crucible, There is a bottom heater at the bottom. The raw material calcium fluoride is ultraviolet grade, and the purity is 99.99%.

[0035] The growth method includes the following steps:

[0036] S1 Load the raw materials into the graphite crucible, and evacuate until the vacuum degree reaches (or higher than) 10 -2 Pa;

[0037] The S2 side heater and the bottom heater are both heated at 50°C / h at the same time, and the temperature of the side heater and the bottom heater are both raised to 150°C, and the temperature is kept constant for 48 hours (the process of heating and constant temperature also plays a role in removing the heat in the device. the action of water vapor), until the int...

Embodiment 2

[0046] Example 2 is basically the same as Example 1 above, except that in step S4 of the calcium fluoride single crystal growth method, the side heater is heated to 1400°C and then kept at a constant temperature, the bottom heater is heated to 1250°C and kept at a constant temperature, the side heater and After the temperature of the bottom heater is stabilized, the temperature is kept at a constant temperature for more than 5 hours, until the raw material is melted and the melt temperature in the crucible reaches equilibrium, and the seed crystals are fused; the heating rates of the side heater and the bottom heater are 50°C / h and 30°C / h respectively; The orientation of the seed crystal is .

[0047] The device used for the growth of calcium fluoride single crystal is basically the same as that in Example 1, the difference is that a circle of side soaking rings 7 (such as figure 2 shown).

Embodiment 3

[0049] Example 3 is basically the same as Example 1 above, except that in step S4 of the calcium fluoride single crystal growth method, the side heater is heated to 1390°C and then kept at a constant temperature, the bottom heater is heated to 1230°C and kept at a constant temperature, the side heater and After the temperature of the bottom heater is stabilized, the temperature is kept at a constant temperature for more than 5 hours, until the raw material is melted and the melt temperature in the crucible reaches equilibrium, and the seed crystals are fused; the heating rates of the side heater and the bottom heater are 50°C / h and 30°C / h respectively; The orientation of the seed crystal is ;

[0050] The device used for the growth of calcium fluoride single crystal is basically the same as that in Example 1, the difference is that a side heating ring 7 is arranged between the side heater 3 and the crucible 2, and a bottom heating ring is arranged between the bottom heater 4 an...

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Abstract

The invention provides a growth method of a calcium fluoride single crystal and a used device, and belongs to the technical field of new material preparation. The method comprises the following steps:using calcium fluoride as a raw material and adopting a crucible pulling method to obtain a calcium fluoride single crystal, jointly adjusting the temperature of the calcium fluoride single crystal by a side heater arranged on the side surface of the crucible and a bottom heater arranged at the bottom of the crucible in the growth process, and controlling seed crystal fusion and the change of theheating or cooling rate in the crystal growth process. According to the single crystal growth device, the temperature near the seed crystal can be accurately controlled so that the seed crystal welding is controlled; the whole process of the calcium fluoride single crystal growth method is free of lead, zinc and other deoxidants so as to ensure that the prepared calcium fluoride single crystal has no ultraviolet region absorption, the single crystal transmittance is high, the stress birefringence is low, and compared with a single heater growth mode, the yield and the crystal quality of the calcium fluoride single crystal can be effectively improved and thus the crystal is more suitable for being used as an excimer laser window material.

Description

technical field [0001] The invention relates to a growth method and a growth device of a calcium fluoride single crystal, and belongs to the technical field of new material preparation. Background technique [0002] Calcium fluoride, chemical formula CaF 2 , colorless crystal or white powder; insoluble in water, slightly soluble in inorganic acid; react with hot concentrated sulfuric acid to generate hydrofluoric acid. The crystal structure of calcium fluoride belongs to the equiaxed crystal system, which is cubic, octahedral or dodecahedral. Colorless crystal or white powder, natural ore contains impurities, slightly green or purple, glows when heated, density 3.18 g / cm 3 , melting point 1402 ℃, boiling point 2497 ℃, refractive index 1.434, low toxicity. Calcium fluoride has a wide range of uses, and with the advancement of science and technology, the application prospects are becoming more and more broad. At present, it is mainly used in three major industries of metal...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B15/10C30B15/14C30B15/20C30B15/36
CPCC30B29/12C30B15/10C30B15/14C30B15/20C30B15/36
Inventor 彭明林徐悟生张可生周方杨春晖
Owner 秦皇岛本征晶体科技有限公司
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