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Preparation method of zinc selenide polycrystalline material for single crystal growth

A polycrystalline material, zinc selenide technology, applied in the direction of single crystal growth, single crystal growth, polycrystalline material growth, etc., can solve the problems of long preparation time and high cost, and achieve short holding time, low cost and simple process Effect

Inactive Publication Date: 2010-03-10
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the shortcomings of long preparation time and high cost in the prior art, the present invention proposes a method for preparing zinc oxide polycrystalline material used for single crystal growth

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In this example, a high-purity zinc selenide polycrystalline powder material is prepared in one step.

[0019] The raw material of this embodiment adopts 99.999% high-purity block zinc and block selenium, selects a tubular electronic-grade high-purity quartz ampoule with an inner diameter of Φ20mm, and places the quartz ampoule horizontally in a tube furnace to complete the preparation of zinc selenide powder . Its preparation process comprises the following steps:

[0020] Step one, clean the ampoule:

[0021] Cleaning the ampoules is done in 3 small steps:

[0022] 1. First soak the ampoule with aqua regia for 11 hours, then rinse it with tap water until neutral, then soak it with acetone for 11 hours, then rinse it with ultra-pure deionized water with a resistivity higher than 15MΩ·cm for 5 times to remove the ampoule. Organic pollution and inorganic impurities.

[0023] 2. Place the cleaned ampoule in a vacuum oven with the temperature controlled at 130°C for 3 ...

Embodiment 2

[0033] In this example, a high-purity zinc selenide polycrystalline powder material is prepared in one step.

[0034] In this embodiment, high-purity block zinc and block selenium with a purity of 99.999% are used as raw materials, and a tubular electronic-grade high-purity quartz ampoule with an inner diameter of Φ16 mm is selected, and the quartz ampoule is horizontally placed in a tube furnace. The preparation process Include the following steps:

[0035] Step one, clean the ampoule.

[0036] Cleaning the ampoules is done in 3 small steps:

[0037] 1. Soak in aqua regia for 12 hours, then rinse with tap water until neutral, then soak in acetone for 12 hours, then rinse with ultra-pure deionized water with a resistivity higher than 15MΩ·cm for 4 times to remove organic matter in the ampoule Pollution and inorganic impurities.

[0038] 2. Place the cleaned ampoule in a vacuum oven with the temperature controlled at 120°C for 5 hours to remove the water vapor in the ampoule...

Embodiment 3

[0048] In this example, a high-purity zinc selenide polycrystalline powder material is prepared in one step.

[0049]In this embodiment, high-purity block zinc and block selenium with a purity of 99.999% are used as raw materials, and a tubular electronic-grade high-purity quartz ampoule with an inner diameter of Φ16 mm is selected, and the quartz ampoule is horizontally placed in a tube furnace. The preparation process Include the following steps:

[0050] Step one, clean the ampoule.

[0051] Cleaning the ampoules is done in 3 small steps:

[0052] 1. Soak in aqua regia for 12 hours, then rinse with tap water until neutral, then soak in acetone for 12 hours, then rinse with ultra-pure deionized water with a resistivity higher than 15MΩ·cm for 3 times to remove organic matter in the ampoule Pollution and inorganic impurities.

[0053] 2. Place the cleaned ampoule in a vacuum oven with the temperature controlled at 125°C for 5 hours to remove the water vapor in the ampoule,...

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Abstract

The invention discloses a preparation method of a zinc selenide polycrystalline material for single crystal growth. The zinc selenide polycrystalline material is prepared from blocky zinc and blocky selenium of which the purities are over 99.999 percent as raw materials in an electronic-grade quartz ampoule. The preparation method comprises the following steps: removing impurities on the inner wall of the ampoule; feeding the zinc and the selenium in a molar ratio of (1.0-1.05):1.0 into the ampoule; feeding a reaction promoter of which the volume concentration is 3-12mg.cm<-3> into the ampoule; evacuating the ampoule, sealing the ampoule, horizontally standing the ampoule in a tube furnace, and quickly raising the temperature to between 94 and 1,000 DEG C; and after maintaining the temperature, cooling the ampoule to a room temperature to generate a large amount of high-purity zinc selenide polycrystalline powder. The zinc selenide polycrystalline powdery material prepared by the invention has the components of Zn and Se, with high purity of over 99.999 percent, in a ratio of 1.0:(1.0-1.03), and can be directly used as a growing raw material of a zinc selenide single crystal. The preparation method has the advantages of simple process, low cost and wide application range.

Description

1. Technical field [0001] The invention belongs to the field of photoelectric materials, in particular to a method for preparing a zinc selenide polycrystalline material used for single crystal growth. 2. Background technology [0002] Zinc selenide (ZnSe) crystal is a II-VI wide bandgap compound semiconductor material. Due to its excellent physical and chemical properties, it is widely used in blue light semiconductor light-emitting devices, nonlinear optoelectronic devices, nuclear radiation detection devices and near-ultraviolet-visible light detection devices. Devices have important application prospects. Since the growth of zinc selenide single crystal is very sensitive to impurities, the commonly used preparation methods of zinc selenide single crystal include melt method, high temperature solution method, solid phase recrystallization method and vapor phase growth method, all of which require a purity of up to 99.999%. The above zinc selenide polycrystalline raw mate...

Claims

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Application Information

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IPC IPC(8): C01B19/04C01G9/00C30B29/48
Inventor 李焕勇介万奇
Owner NORTHWESTERN POLYTECHNICAL UNIV
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