Method for growing large size Ta2O5 single crystal by using floating zone method

A large-scale, floating zone technology, applied in the direction of single crystal growth, crystal growth, single crystal growth, etc., to achieve the effect of simple operation, no macroscopic defects, and good crystal growth quality

Active Publication Date: 2013-08-07
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, no large-size Ta has been grown by the floating zone method. 2 o 5 single crystal report

Method used

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  • Method for growing large size Ta2O5 single crystal by using floating zone method
  • Method for growing large size Ta2O5 single crystal by using floating zone method
  • Method for growing large size Ta2O5 single crystal by using floating zone method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Powder preparation: mix Ta 2 o 5 The powder was ball milled for 12 hours and dried at 80°C for 8 hours.

[0036] (2) Rod preparation: Ta after ball milling 2 o 5 Put the powder into a rubber tube and seal it, then use a vacuum pump to evacuate for 10 minutes, and then put it into a bar-shaped green bar under isostatic pressure at a pressure of 70Mpa;

[0037] (3) Seed crystal preparation: put the obtained green billet into a high-temperature sintering furnace, and obtain a polycrystalline rod after the sintering temperature is 1450° C. and the sintering time is 12 hours;

[0038] (4) Material rod and seed crystal installation: fix the pressed biscuit rod on the material rod of the single crystal furnace as the material rod, put the polycrystalline rod into the floating zone furnace as the seed crystal, seed crystal and material rod in a straight line in the vertical direction. Adjust the position of the rod and seed so that it touches and is at the same level a...

Embodiment 2

[0042] (1) Powder preparation: mix Ta 2 o 5 The powder was ball milled for 12 hours and dried at 80°C for 8 hours.

[0043] (2) Rod preparation: Ta after ball milling 2 o 5 Put the powder into a rubber tube and seal it, then use a vacuum pump to evacuate for 5 minutes, and then put it into a bar-shaped green bar under isostatic pressure at a pressure of 60Mpa;

[0044] (3) Seed crystal preparation: put the prepared green billet into a high-temperature sintering furnace, and obtain a polycrystalline rod after the sintering temperature is 1550° C. and the sintering time is 24 hours;

[0045] (4) Material rod and seed crystal installation: fix the sintered polycrystalline rod on the material rod of the single crystal furnace as the material rod, put the polycrystalline rod into the floating zone furnace as the seed crystal, the seed crystal and the material rod are vertically in a straight line. Adjust the position of the rod and seed so that it touches and is at the same le...

Embodiment 3

[0049] (1) Powder preparation: mix Ta 2 o 5 The powder was ball milled for 12 hours and dried at 80°C for 6 hours.

[0050] (2) Rod preparation: Ta after ball milling 2 o 5 Put the powder into a rubber tube and seal it, then evacuate it with a vacuum pump for 8 minutes, and then put it into a bar-shaped green bar under isostatic pressure at a pressure of 65Mpa;

[0051] (3) Seed crystal preparation: put the obtained green billet into a high-temperature sintering furnace, and obtain a polycrystalline rod after the sintering temperature is 1600° C. and the sintering time is 12 hours;

[0052] (4) Material rod and seed crystal installation: After sintering, the polycrystalline rod is fixed on the material rod of the single crystal furnace as a material rod, and the grown Ta 2 o 5 The single crystal is put into the floating zone furnace as the seed crystal, and the seed crystal and the material rod form a straight line in the vertical direction. Adjust the position of the ro...

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Abstract

The invention relates to a method for growing a large size Ta2O5 single crystal by using a floating zone method, and belongs to the field of crystal growth. The method comprises the following steps: carrying out ball milling and drying for a Ta2O5 powder material; placing the treated Ta2O5 powder material in a rubber tube, and carrying out isostatic pressing for the material to prepare a biscuit rod; carrying out sintering for the biscuit rod to obtain a polycrystalline rod; adopting the biscuit rod or the polycrystalline rod as the material rod, and adopting the polycrystalline or the Ta2O5 single crystal as the seed crystal, wherein the seed crystal and the material rod form a straight line in a vertical direction, and the contact point and a halogen lamp are at the same horizontal line; heating the material rod and the seed crystal until the material rod and the seed crystal are molten, wherein the heating rate is 30-60 DEG C per minute; adjusting the rotation speeds and the rotation directions of the material rod and the seed crystal, then carrying out inoculation; adopting the movement of a focusing lens or the up and down movement of the rod to enable the molten zone to be far away from the focusing point, enable the temperature of the molten zone to be decreased to realize the crystallization, wherein the crystal growth rate is 10-60 mm / h; cooling the grown crystal to the room temperature. With the method provided by the present invention, the growth period is short; the preparation efficiency is high; the Ta2O5 single crystal can be rapidly grown, wherein the grownTa2O5 single crystal has characteristics of size in centimeter magnitude, no macroscopic defect and high quality.

Description

technical field [0001] The invention belongs to the field of crystal growth, and relates to the growth of Ta 2 o 5 single crystal method. technical background [0002] The floating zone method does not require a crucible, is pollution-free, and has a fast growth rate, and is suitable for growing crystals with high melting points. Able to provide high-quality, small-sized crystals for easy component control. It has a wide range of applications and can be used for many types of materials such as oxides, semiconductors, and intermetallic compounds, especially crystals with strong melt reactions. The main advantage of this method is that no crucible is required, and the grown single crystal has high purity and uniform doping. Also because the heating is not limited by the melting point of the crucible, it has unique advantages in growing high melting point materials. The floating zone method provides a new research method and approach for the study of multi-system, high mel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/16C30B13/00
Inventor 蒋毅坚徐宏范修军王越
Owner BEIJING UNIV OF TECH
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