Two-step preparation method of large Al2O3-based crystal

A large-scale, two-step technology, applied in crystal growth, chemical instruments and methods, single crystal growth, etc., can solve the problems that the two-step growth process has not been reported, and achieve short preparation cycle, short time-consuming, instrument simple effect

Inactive Publication Date: 2013-01-16
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In contrast, other gem crystals such as Ni:Al 2 o 3 Crystal, Fe:Al 2 o 3 There are few reports on crystals, and there are few reports on its synthesis process, doping ratio, and performance applications, and its two-step growth process has not been reported.

Method used

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  • Two-step preparation method of large Al2O3-based crystal
  • Two-step preparation method of large Al2O3-based crystal
  • Two-step preparation method of large Al2O3-based crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: The crystal growth furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optical floating zone method crystal growth furnace produced by Crystal Systems Corporation of Japan, and what grows is Ni:Al doped with 1wt% NiO 2 o 3 crystals.

[0033] (1) Al 2 o 3 The powder and NiO powder are mixed according to the mass ratio of 99.0:1.0, placed in a ball mill tank for ball milling, dried and sieved.

[0034] (2) Put the powder obtained in (1) into a long rubber balloon for compaction, and place the rubber ball filled with the powder under isostatic pressure to make a green bar.

[0035] (3) Fix the biscuit rod obtained in (2) on the seed rod of the single crystal furnace (called the seed rod), and adjust the position of the seed rod so that the top of the seed rod is on the same horizontal line as the halogen lamp .

[0036] (4) In an air atmosphere, the halogen lamp of the single crystal furnace outputs a power of 2720W / h, the seed rod rotates ...

Embodiment 2

[0040] Embodiment 2: The crystal growth furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optical floating zone method crystal growth furnace produced by Crystal Systems Corporation of Japan, and what grows is Ni:Al doped with 1.5wt% NiO 2 o 3 crystals.

[0041] (1) Al 2 o 3 The powder and NiO powder are mixed according to the mass ratio of 98.5:1.5, placed in a ball mill tank for ball milling, dried, and sieved.

[0042] (2) Put the powder obtained in (1) into a long rubber balloon with a diameter of 10 and compact it, and place the rubber ball filled with the powder under isostatic pressure to make a green bar.

[0043] (3) Fix the biscuit rod obtained in (2) on the seed rod of the single crystal furnace (called the seed rod), and adjust the position of the seed rod so that the top of the seed rod is on the same horizontal line as the halogen lamp .

[0044] (4) In an air atmosphere, the halogen lamp of the single crystal furnace outputs a power of 2750W...

Embodiment 3

[0048] Embodiment 3: The crystal growth furnace used in the present invention is the FZ-T-10000-VI-VPO-PC optical floating zone method crystal growth furnace produced by Crystal Systems Corporation of Japan, and what grows is Ni:Al doped with 2wt% NiO 2 o 3 crystals.

[0049] (1) Al 2 o 3 The powder and NiO powder are mixed according to the mass ratio of 98.0:2.0, placed in a ball mill tank for ball milling, dried and sieved.

[0050] (2) Put the powder obtained in (1) into a long rubber balloon for compaction, and place the rubber ball filled with the powder under isostatic pressure to make a green bar.

[0051] (3) Fix the biscuit rod obtained in (2) on the raw material rod of the single crystal furnace (called a material rod), and adjust the position of the material rod so that the end of the material rod is on the same horizontal line as the halogen lamp.

[0052] (4) In the air atmosphere, the halogen lamp of the single crystal furnace outputs a power of 2750W / h, the ...

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Abstract

The invention discloses a two-step preparation method of a large Al2O3-based crystal, comprising the following steps of: preparing Al2O3 powder and doped powder into a biscuit bar as a seed crystal bar or charge bar and enabling the top end of the seed crystal bar or the tail end of the charge bar to be on the same horizontal line with a halogen lamp; outputting the power of 2720-3060W / h by the halogen lamp in an air atmosphere, scanning and heating the biscuit bar in a reciprocating way till the biscuit bar is melted and crystallized to obtain polycrystal charge bars; with one of the polycrystal charge bars as a seed crystal and another one as a raw material bar, enabling the tail end of the raw material bar to be in contact with the top end of the seed crystal bar, wherein the contact part is on the same horizontal line with the halogen lamp; outputting the power of 3200-3400W / h by the halogen lamp in an air atmosphere; and reversely rotating the seed crystal and the raw material bar, downwards and upwards moving the raw material bar and the seed crystal bar respectively to pass through a melting zone for crystal growth. Crystals obtained with the method provided by the invention contains no impurities, has fewer small-angled crystal boundaries and shows favorable crystal quality.

Description

technical field [0001] The invention belongs to the field of crystal growth, in particular to Al 2 o 3 A two-step method for the preparation of base crystals. Background technique [0002] Corundum is widely used due to its physical properties such as high strength, high melting point, chemical inertness and various optical properties. Undoped α-Al 2 o 3 It is called white gemstone, doped with Cr 2 o 3 Al 2 o 3 The crystal is red and is usually called ruby. Corundum of other colors than ruby ​​is called (color) sapphire, such as colorless sapphire, blue sapphire, yellow sapphire, pink sapphire, green sapphire, orange sapphire, purple sapphire. Al doped with different elements 2 o 3 Crystals exhibit different colors and play an increasingly important role in the fields of industry, decoration, medical devices, optics, etc. due to their unique physical and chemical properties. As a decorative gemstone, mixed with different elements, it can be made into imitations of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/20C30B13/00
Inventor 王越范修军徐宏蒋毅坚
Owner BEIJING UNIV OF TECH
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