Annealing treatment method of crystal in neutral and inert atmosphere

A technology of annealing treatment and inert atmosphere, which is applied in the field of crystal annealing method and heat treatment, can solve the problems of unsatisfactory transparency, ion valence state change, and affecting crystal performance, so as to improve crystal integrity and optical uniformity, with good effect and Good recrystallization effect

Pending Publication Date: 2006-03-08
周永宗
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  • Application Information

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Problems solved by technology

[0003] The crystal is annealed at high temperature in an oxidizing atmosphere (atmosphere). Although it can achieve decarburization and decolorization and eliminate the color centers formed by point defects such as oxygen vacancies in the crystal, due to the diffusion and back diffusion of dust in the atmosphere, the annealed crystal will be Impurities in the air are polluted again (resulting in secondary pollution). Therefore, the brightness and transparency of crystals annealed in an oxidizing atmosphere are always unsatisfactory (high-temperature annealing in an oxidizing atmosphere: generally suitable for crystals that need to be annealed in an oxidizing atmosphere first) Crystal), and high-temperature annealing in reducing atmosphere (hydrogen), although the brightness and transparency of the crystal are much better than the results of annealing in oxidizing atmosphere, due to the reduction effect of strong reducing atmosphere in hydrogen, the oxidized crystals grown by various methods In the physical crystal, the color centers formed by point defects such as oxygen vacancies (oxygen vacancies) are not only difficult to eliminate or even deepen, but the crystal varieties that can adapt to annealing in hydrogen are highly targeted, even for the same sapphire crystal. It is also very different (it is only suitable for crystals that really need to be annealed in a reducing atmosphere, such as titanium-doped sapphire), and more importantly, annealing in an oxidizing atmosphere or annealing in a reducing atmosphere is likely to cause changes in the valence state of ions in the crystal lattice. Affect crystal properties

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  • Annealing treatment method of crystal in neutral and inert atmosphere
  • Annealing treatment method of crystal in neutral and inert atmosphere
  • Annealing treatment method of crystal in neutral and inert atmosphere

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Experimental program
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Effect test

Embodiment 1

[0015] Embodiment 1: Three pieces of sapphire crystal blanks grown by guided temperature gradient method are placed in the heat treatment chamber of the "crystal annealing device". After the annealing device is sealed, the gas in the annealing device (annealing furnace) is exhausted to a vacuum degree higher than 3×10 -3 Pa, filled with high-purity argon, decarburized and decolorized, recrystallized and annealed at high temperature in an inert atmosphere. The annealing program is heating rate: 90°C / hour-110°C / hour; constant temperature at 1830°C for 96 hours; cooling rate: 90°C / hour-110°C / hour.

[0016] Evaluation of crystal detection level before annealing: the first crystal has a slight filamentous optical path and internal filaments (B501 grade); the second crystal has obvious filamentous optical paths and internal white filaments (B901 grade); the third There are obvious filamentary light paths and filaments (B912 grade) inside the fast crystal (the whole).

[0017] Afte...

Embodiment 2

[0018] Embodiment 2: five pieces of sapphire crystal blanks grown by guided temperature gradient method are placed in the heat treatment chamber of the "crystal annealing device". After the annealing device is sealed, the gas in the annealing device (annealing furnace) is exhausted until the vacuum degree is higher than 3×10 -3 Pa, filled with high-purity hydrogen, decarburized and decolorized, recrystallized and annealed at high temperature in a reducing atmosphere. The annealing procedure is the same as that of Example 1: heating rate: 90°C / hour-110°C / hour; constant temperature at 1830°C for 96 hours; cooling rate: 90°C / hour-110°C / hour.

[0019] Evaluation of crystal detection grade before annealing: the first crystal is B661 grade; the second fast crystal is B900 grade; the third fast crystal is B012 grade; the fourth fast crystal is B810 grade; the fifth fast crystal is B431 grade.

[0020] After high-temperature annealing in a reducing atmosphere (hydrogen), the inspecti...

Embodiment 3

[0027] Embodiment 3: the decarburization and decolorization of 2 inch cylinders in diameter, the annealing of color center, the sapphire crystal blank that guides temperature gradient method growth, is processed into 2 inch cylinders in diameter ( figure 2 ), placed in the heat treatment chamber of the "crystal annealing device", after the annealing device is sealed, exhaust the gas in the annealing device (annealing furnace) to a vacuum degree higher than 3×10 -3 Pa, fill high-purity nitrogen into the furnace to make the pressure in the furnace greater than the atmospheric pressure, start to heat up, when the furnace temperature rises to about 900°C, start to deflate, and maintain the pressure in the furnace at 0.03-0.05MPa. The annealing program is heating rate: 215°C / hour-310°C / hour; constant temperature at 1740°C for 5 hours; cooling rate: 215°C / hour-305°C / hour. After being annealed in a neutral atmosphere (nitrogen), the sapphire cylinder becomes a crystal clear colorles...

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Abstract

This invention relates to an annealing process method for crystals in neutral and inert atmosphere, which puts crystals to be annealed and processed in a crystal anneal device to charge neutral, or inert or mixed gas to carry out annealing of the crystals and realize carbon, color center elimination, pollution elimination and eliminating the inner stress of the crystals to each their recrystalization. The annealing at high temperature in the neutral or inert gas will not generate new lattice defect and variance of ionic valence by the strong adsorption of inert gas under high temperature.

Description

technical field [0001] The invention belongs to the field of heat treatment of crystals, and relates to high-temperature annealing and heat treatment of crystals, in particular to an annealing method and a heat treatment method of crystals in a neutral atmosphere, an inert atmosphere and a mixed atmosphere of the two. Background technique [0002] Today, the techniques for growing crystals include the induction heating pulling method (ie, the upward method), the Kyroplasty method, the resistance heating pulling method, the oriented temperature gradient method (ie, the oriented temperature gradient method, referred to as the temperature gradient method), and the heat exchange method. Crystal growth is a crystallization process in which the temperature difference at the solid-liquid interface promotes the formation of crystal planes, which is prone to lattice point defects and the introduction of ambient atmosphere pollution, seriously affecting crystal performance. Therefore,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B33/02
Inventor 周永宗
Owner 周永宗
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