Cold core shouldering micropulling proparation method of large size sapphire single crystal

A sapphire crystal and sapphire technology, which is applied in the self-melting liquid pulling method, single crystal growth, single crystal growth and other directions, can solve the difficulty in mass production of sapphire products at low cost and high quality, increase the dislocation density of single crystal, Defects and high stress values, to achieve obvious economic and social benefits, reduce defects, and low costs

Active Publication Date: 2007-06-27
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above method, the single crystal grown by the flame method has a large temperature gradient and high defects and stress values, so it is difficult to mass-produce sapphire products with low cost and high quality; although the pulling method can produce high-quality single crystal crystal material, but because the seed crystal requires a certain speed of rotation during the growth process, the diameter of the single crystal is small, and the crystallographic direction used by the single crystal has a certain angle with the pulling direction of the single crystal, so the utilization rate is very low ; Although the zone melting method can reduce the energy consumption of single crystal growth, it will greatly increase the dislocation density of the single crystal and reduce its use efficiency; The method of using the substrate substrate sapphire was not adopted because the defect density per unit area of ​​sapphire was too high; the common feature of the heat exchange method and the guided temperature gradient method is that it can grow a larger sapphire single crystal, and the crystal quality is very high. The utilization rate of the crucible is very low, making the cost of this method high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: The present invention adopts resistance heating, and 25.5 kg of pretreated aluminum oxide is packed into a crucible made of pure tungsten. Open the cooling water, the flow rate is 6m 3 / h; increase the power to 55kw at a rate of 2.5w per hour, during which the vacuum degree once dropped to 1.0×10 -2 pa, caused by the volatilization of organic matter in the furnace, returned to 6.0×10 after 40 minutes -3 Pa. When the target voltage is reached, observe the liquid surface and find a small amount of bubbles escaping from the liquid surface, judging that the temperature in the crucible is too high, and adjust the power at a speed of 250w per hour, so that the solid-liquid transformation image of orderly convection just appears on the liquid surface. After being stable under this condition for 4 hours, start seeding 8 times at the "cold core position", the seed rod pulling speed is 5mm / h, and the power drop adjustment rate is 2.5w / h. After the above-mentioned...

Embodiment 2

[0012] Embodiment 2: 27.5 kg of pretreated aluminum oxide is packed into a crucible made of pure tungsten. Open the cooling water, the flow rate is 6.2m 3 / h. Raise the voltage to 9700mV at a rate of 70mV per hour, during which the vacuum degree dropped once, and returned to 6.0×10 after 35 minutes -3 pa. When the target voltage is reached, observe the liquid surface and find that there are a large number of bubbles escaping from the liquid surface. It is judged that the temperature in the crucible is higher than the crystallization temperature, and the voltage is adjusted at a rate of 75mV / h, so that an orderly convective solid state just appears on the liquid surface. liquid conversion image. After stabilizing under this condition for 8 hours, start seeding at the "cold core position", the seed rod is pulled at a speed of 4.5mm / h, and the rate of voltage drop regulation is 7mV / h. After the above-mentioned process is completed, start shouldering, the pulling speed of the ...

Embodiment 3

[0013] Embodiment 3: 26 kg of pretreated aluminum oxide is packed into a crucible. Open the cooling water, the flow rate is 5m 3 / h. Raise the voltage to 9600mV at a rate of 100mV per hour. When reaching the target voltage, adjust the voltage at a rate of 75mV per hour, so that the solid-liquid transformation image of orderly convection just appears on the liquid surface. After 10 hours of stability under this condition, start to put shoulders at the "cold core" position, the pulling speed of the seed rod is 6mm / h, and the rate of voltage drop adjustment is 10mV / h; after the above process is completed, start to put the shoulders, the seed crystal The rod pulling speed is 4mm / h, the voltage drop rate is 8mV / h; the seed rod pulling speed is 5.5mm / h in the isodiametric stage, and the voltage drop adjustment rate is 8mV / h. After the crystallization process is completed, the voltage is adjusted to drop at a rate of 12mV / h for 12 hours, and then the voltage is lowered at a rate of...

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PUM

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Abstract

The invention relates to sapphire single crystal growth method. The feature is that: the temperature of cooling water output is stabilized at 15-35 degree centigrade and during the whole technology process the vacuum pressure is less than 6*0.001Pa. Using tungsten heating body and crucible, tungsten molybdenum separating shield and high temperature component, the sapphire crystal is made in the single crystal furnace. In the crystal seeding process, it includes slowly adjusting the seed crystal to make the bottom above the melt liquid surface 5-20mm, preheating and removing thermal stress; using the classic crystal pulling method technology, after 5-15 times crystal seeding along the cold core departure direction to transferring the crystallizing center to cold core, cooperating rotating controlling and the rotating speed is 2-16 round per minute.

Description

Technical field: [0001] The invention relates to a method for growing a sapphire single crystal, in particular to a method for preparing a large-size sapphire single crystal by cold-heart shoulder micro-pulling. Background technique: [0002] Sapphire (α-Al 2 o 3 ), also known as white gem, is a crystal material whose hardness is second only to diamond. It has high hardness (Mohs hardness 9), high temperature resistance (melting point up to 2050 ℃), strong abrasion resistance and corrosion resistance, stable chemical properties, generally insoluble in water, not subject to acid corrosion, light transmission performance, electrical insulation performance A series of excellent characteristics. Sapphire single crystal can be used in microwave tube media, ultrasonic transmission components, delay lines, waveguide laser cavities and precision instrument bearings, optical components such as balance knife edges, as well as infrared military devices, satellite space technology, w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B15/00C30B29/20
Inventor 韩杰才孟松鹤左洪波张明福
Owner HARBIN INST OF TECH
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