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
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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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