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Method for growing GZO(ZnO: Ga) crystals

A crystal and crystal material technology, applied in the field of crystal growth, can solve the problems of small crystal size, uneven composition, stress generation, etc., and achieve the effect of fast growth and high efficiency

Active Publication Date: 2015-01-28
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, the size of the crystals is small and the composition is not uniform
Second, it is easy to bring flux impurities into the crystal during the growth process, resulting in stress
This is disadvantageous for applications in electronic materials where impurity levels and stoichiometric ratios must be well controlled
Third, ZnO is volatile, which is also a challenge for this method
[0005] At present, the flux used to grow pure zinc oxide is PbF 2 , P 2 o 5 +V 2 o 5 , V 2 o 5 +B 2 o 3 ,V 2 o 5 +MoO 3 , there is no report about the growth of GZO crystals by flux method

Method used

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  • Method for growing GZO(ZnO: Ga) crystals
  • Method for growing GZO(ZnO: Ga) crystals
  • Method for growing GZO(ZnO: Ga) crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Put ZnO (99.99%) powder in the ZrO 2 In the nylon tank of the grinding medium, use absolute ethanol as the dispersant for ball milling, drying, and 200-mesh sieving to obtain ZnO powder with uniform particle size.

[0037] (2) Put the powder obtained in step (1) into a long rubber balloon, compact and seal, vacuumize, and make a biscuit rod with uniform thickness and density under 70MPa isostatic pressure.

[0038] (3) The material rod prepared in step (2) was placed in a vertical pulling rotary furnace and sintered at 1250°C for 24 hours to obtain a dense and uniform polycrystalline material rod.

[0039] (4) Cut a section of the polycrystalline rod prepared in (3) instead of the seed crystal and tie it to the bracket of the lower rotating rod, so that the cut surface is horizontally centered, and the wafer containing the flux is placed on it, and the remaining polycrystalline The material rod is suspended under the upper rotating rod, adjusted to the center, the ...

Embodiment 2

[0043] (1) The powder ZnO (99.99%), Ga 2 o 3 (99.99%) by ZnO:0.05wt%Ga 2 o 3 (referred to as GZO-0.05wt%) stoichiometric ratio for weighing, placed in a ZrO 2 GZO‐0.05wt% powder with uniform particle size was obtained after ball milling and drying with absolute ethanol as the dispersant in the nylon tank of the grinding medium, and sieved through 200 mesh.

[0044] (2) The details of the intermediate experiment process are the same as in Example 1.

[0045] (3) Set them to rotate in reverse, the upper rotation speed is 250rpm, the lower rotation speed is 250rpm, the crystal growth rate is 0.3mm / h to start growing, and the output power of the halogen lamp in the floating zone furnace is 1100-1134W / h. The size of the grown crystal is Φ12mm×92mm, and the growth time is 309h.

[0046] (4) Set the cooling time to 6 hours, and cool the grown crystals to room temperature.

Embodiment 3

[0048] (1) The powder ZnO (99.99%), Ga 2 o 3 (99.99%) by ZnO:0.1wt%Ga 2 o 3 (referred to as GZO-0.1wt%) stoichiometric ratio was weighed, placed in a ZrO 2 GZO‐0.1wt% powder with uniform particle size was obtained after ball milling and drying with absolute ethanol as the dispersant in the nylon tank of the grinding medium, and 200 mesh sieve.

[0049] (2) The details of the intermediate experiment process are the same as in Example 1.

[0050] (3) Set them to rotate in reverse, the upper rotation speed is 350rpm, the lower rotation speed is 350rpm, the crystal growth rate is 0.4mm / h to start growing, and the output power of the halogen lamp in the floating zone furnace is 1100-1140W / h. The size of the grown crystal is Φ12.5mm×93mm, and the growth time is 235h.

[0051] (4) Set the cooling time to 5 hours, and cool the grown crystals to room temperature.

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Abstract

The invention provides a method for growing GZO(ZnO: Ga) crystals and belongs to the technical field of crystal growth. The method comprises the following steps: firstly, preparing a compact and uniform single-phase good-quality charge bar; secondly, optimizing the components and the proportions of the components of a fluxing agent; finally, obtaining the optimal process parameters, such as the growing power, the growing speed and the rotating speed of the charge bar and the seed crystal for growing the series of single crystals, of a mobile-fluxing agent optical float-zone method. The crystals obtained by use of the method for growing the GZO(ZnO: Ga) crystals are high in crystallization quality, fixed in growth direction and excellent in electrical properties.

Description

technical field [0001] The invention relates to a method for growing GZO (ZnO:Ga) crystals, in particular to growing centimeter-level GZO crystals with different Ga-doped concentrations by using a moving flux floating zone method, and belongs to the technical field of crystal growth. Background technique [0002] GZO crystal is a kind of multifunctional, direct bandgap and wide bandgap semiconductor material which integrates various excellent properties such as transparent conduction, ultrafast attenuation scintillation, and ultraviolet laser emission. [0003] At present, the growth methods of zinc oxide single crystal mainly include hydrothermal method, flux method, gas phase method and so on. Specific to GZO crystal materials, there are only reports of hydrothermal growth at present, and there are two limitations: 1, the amount of gallium doped is too small, not more than 0.1wt%; 2, the size is small, the maximum size is 30.44mm×24.84mm×5.40mm . Crystal growth is limite...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/22C30B9/12
CPCC30B9/12C30B29/22C30B29/16C30B13/24C04B35/453C04B2235/3251C04B2235/3256C04B2235/3284C04B2235/3286C04B2235/3409C04B2235/6567C04B2235/94C30B13/02C30B13/00C30B19/02C30B13/22C30B13/34
Inventor 蒋毅坚马云峰王越梅晓平张春萍王强徐仰立
Owner BEIJING UNIV OF TECH