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PBN crucible oxidation pretreatment device and method and application thereof

A pretreatment device and pretreatment technology, applied in chemical instruments and methods, self-solidification method, single crystal growth, etc., can solve problems such as crystal side wall pits and cracks, quartz ampoule expansion, affecting crystal quality, etc., to prevent Effects of heating device and PBN crucible damage, reduction of heterogeneous nucleation phenomenon, and easy industrial application

Pending Publication Date: 2021-08-06
广东先导微电子科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if it is not handled properly, it will lead to the formation of oxide layers on both sides of the PBN crucible. Since boron oxide is extremely easy to absorb water and form boric acid, the existence of a large thin layer of boron oxide makes it easy for the PBN crucible to absorb a large amount of water when it is exposed to air.
Therefore, the water vapor formed by the excess water remaining in boron oxide during the high-temperature crystal growth process can easily increase the internal pressure of the quartz ampoule and cause the quartz ampoule to expand, eventually causing damage to the heater and even causing the quartz ampoule to explode.
In addition, excessive moisture in the crystal growth process makes it easy to form bubbles between the gallium arsenide melt and the crucible wall, causing macroscopic defects such as pits and cracks on the crystal side wall, which seriously affects the quality of the crystal

Method used

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  • PBN crucible oxidation pretreatment device and method and application thereof
  • PBN crucible oxidation pretreatment device and method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] This embodiment provides a PBN crucible oxidation pretreatment device.

[0041] Such as figure 1 As shown, the device includes: a quartz ampoule 4 containing a PBN crucible 3 , the PBN crucible 3 is placed in the quartz ampoule 4 , and the outer wall of the PBN crucible 3 is bonded to the inner wall of the quartz ampoule 4 . The top opening of the quartz ampoule 4 is provided with a suitable quartz sealing cover 2 at the top opening. The quartz sealing cover 2 is detachable, and the quartz sealing cover 2 is provided with an air inlet. The bottom of the ampoule 4 is provided with an air outlet, the bottom of the PBN crucible 3 is a seed crystal end, and the seed crystal end is open, and the opening of the seed crystal end communicates with the air outlet at the bottom of the quartz ampoule 4, and the quartz ampoule 4 and Oxygen in the PBN crucible 3 can be discharged from the air outlet. The air inlet and the air outlet are connected to the air inlet pipe 5 and the ai...

Embodiment 2

[0043] This embodiment provides a PBN crucible oxidation pretreatment method, the treatment method is as follows:

[0044] (1) Provide a PBN crucible oxidation pretreatment device described in Example 1;

[0045](2) First, put the PBN crucible 3 in an acid solution for ultrasonic cleaning for 2 hours. In the acid solution, HF acid: deionized water = 2:1, then use deionized water to rinse the acid solution on the surface of the PBN crucible 3, and finally The washed PBN crucible 3 is soaked in ethanol for 10 minutes and then dehydrated, and the cleaned PBN crucible 3 is placed on a clean workbench to naturally dry the ethanol and water on its surface. Put the PBN crucible 3 whose surface has been dried in the quartz ampoule 4, control the heating device 1, heat up to 200°C and bake for 1 hour, and dry the moisture on the surface of the crucible;

[0046] (3) Use the quartz sealing cap 2 to seal the opening of the quartz ampoule 4, close the air inlet pipe 5 and the air outlet ...

Embodiment 3

[0050] This embodiment provides a method of using embodiment 2 to process the obtained PBN crucible 3 in gallium arsenide single crystal

[0051] For the application of the growth process, in this embodiment, bulk gallium arsenide polycrystalline material is used to fill the PBN crucible 3 to produce 10 kg of gallium arsenide single crystal material with a diameter of 4 inches, and the total length of the equal diameter part is 200 mm.

[0052] The single crystal growth process of this embodiment is as follows: use the PBN crucible 3 pretreated in this embodiment to charge, and hold 10Kg of gallium arsenide polycrystalline material in total, place the PBN crucible 3 containing the polycrystalline material in a quartz ampoule 4, pump Vacuum treatment until the pressure in the quartz ampoule 4 is lower than 10 -2 After Pa, the quartz tube is welded and sealed with an oxyhydrogen flame. Put the sealed quartz ampoule 4 containing the PBN crucible 4 and the polycrystalline materia...

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Abstract

The invention belongs to the technical field of semiconductor material preparation, and particularly discloses a PBN crucible oxidation pretreatment device and method and application thereof. The pretreatment device comprises a quartz ampoule containing a PBN crucible, wherein an opening is formed in the top of the quartz ampoule, a matched sealing cover is arranged at the top opening, an air inlet is formed in the sealing cover, an air outlet is formed in the quartz ampoule, and the air inlet and the air outlet are respectively communicated with an air inlet pipe and an air outlet pipe; a vacuumizing device, which is connected with the quartz ampoule; a heating device, which is arranged to be used for heating the quartz ampoule and the air inlet pipe; and an air supply device, which is connected with the air inlet pipe. In the growth process of the gallium arsenide single crystal, the oxidation layer is only formed on the inner wall of the PBN crucible treated by the method disclosed by the invention, the moisture in the air absorbed by the oxidation layer in the contact process with the air can be effectively reduced in the charging process, and the damage of a heating device and the PBN crucible in the crystal growth stage caused by the expansion of the quartz ampoule in the crystal growth process is effectively prevented.

Description

technical field [0001] The invention belongs to the technical field of semiconductor material preparation, and more specifically relates to a PBN crucible oxidation pretreatment device, method and application thereof. Background technique [0002] At present, large-scale commercial production of gallium arsenide single crystal basically adopts VGF / VB method. PBN crucible has the characteristics of not reacting with gallium arsenide and high temperature resistance, so it is used as a container for gallium arsenide growth. [0003] The VGF / VB method is a directional solidification single crystal growth technology. The liquid-solid phase transition will inevitably occur during the crystal growth process. To grow high-quality gallium arsenide single crystals, it is necessary to suppress the occurrence of heterogeneous nucleation during the phase transition process. In this way, the occurrence of defects such as dendrites and twins can be avoided, and the purpose of improving the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B41/87C30B11/00C30B29/42
CPCC04B41/87C04B41/009C04B41/5006C30B11/002C30B29/42
Inventor 吕新杨易明辉刘建忠吴晓波周铁军
Owner 广东先导微电子科技有限公司
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