Interface wettability regulation and control method for inhibiting growth of silicon dendrites in CVD process of zone-melting-grade polycrystalline silicon

A polysilicon and inhibition zone technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems that the mechanical properties of products are difficult to meet the processing and production of molten grade polysilicon, and the growth of silicon dendrites.

Pending Publication Date: 2021-09-14
河南硅烷科技发展股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the deposition process of zone melting grade polysilicon, the growth of silicon dendrites is very easy to occur, which makes the mechanical properties of the product difficult to meet the further processing and production of zone melting grade polysilicon.

Method used

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  • Interface wettability regulation and control method for inhibiting growth of silicon dendrites in CVD process of zone-melting-grade polycrystalline silicon
  • Interface wettability regulation and control method for inhibiting growth of silicon dendrites in CVD process of zone-melting-grade polycrystalline silicon
  • Interface wettability regulation and control method for inhibiting growth of silicon dendrites in CVD process of zone-melting-grade polycrystalline silicon

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Experimental program
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Effect test

Embodiment 1

[0036] A method for inhibiting the growth of silicon dendrites and promoting uniform deposition in the process of preparing molten-grade polysilicon by silane method CVD, such as figure 1 As shown, including the steps of surface treatment of U-shaped silicon core to remove surface impurities, including: cleaning, wiping and drying; the treated U-shaped silicon core is placed inside the thermal cracking furnace reactor, and nitrogen is introduced to replace the air inside the reactor ; Introduce hydrogen to replace nitrogen in the reactor; continue to inject hydrogen, and apply current to the silicon core in the reactor for a certain period of time to reduce the oxide layer on the surface of the silicon core, regulate its wettability and build a "super-silicon-philic" Surface; adjust the current to control the silicon core to reach a suitable reaction temperature, and introduce a mixture of high-purity silane and high-purity hydrogen. layered growth”, resulting in dense polycry...

Embodiment 2

[0045] (1) The U silicon core was rinsed with ultrapure water (≥15MΩ*cm, 25°C) for 3 times, and then wiped with absolute ethanol and ethyl acetate for 3 times;

[0046] (2) The cleaned and wiped silicon cores are stored in a vacuum drying oven in a clean workshop (≥100,000 grades) for drying, and the temperature is set to 100°C;

[0047] (3) The silicon core is placed inside the reactor, and nitrogen (O 2 ≤0.001%) replace the air inside the reactor for 3 times;

[0048] (4) Use hydrogen (≥99.99%) to replace the nitrogen inside the reaction furnace for 3 times;

[0049] (5) Continue to feed hydrogen for 20m 3 / h, load current on the silicon core in the reactor, set the current to 80A, keep it for 2 hours, adjust its wettability and build a "super-siliconophilic" surface;

[0050] (6) Adjust the current and control the reaction temperature of the silicon core to be 900-950 ° C, the initial molar ratio of silane to hydrogen is 0.12, and the initial mixed gas flow rate is 600 m...

Embodiment 3

[0053] (1) The U silicon core is rinsed with ultrapure water (≥15MΩ*cm, 25°C) for 5 times, and then wiped with a mixed solution of absolute ethanol, ethyl acetate and acetone for 3 times;

[0054] (2) The cleaned and wiped silicon cores are stored in a vacuum drying oven in a clean workshop (≥100,000 grades) for drying, and the temperature is set to 80°C;

[0055] (3) The silicon core is placed inside the reactor, and nitrogen (O 2 ≤0.001%) replace the air inside the reactor for 5 times;

[0056] (4) Use hydrogen (≥99.99%) to replace the nitrogen inside the reaction furnace for 5 times;

[0057] (5) Continue to feed hydrogen for 30m 3 / h, load current on the silicon core in the reactor, set the current to 50A, keep it for 4 hours, adjust its wettability and build a "super-silicon-philic" surface;

[0058] (6) Adjust the current and control the reaction temperature of the silicon core to be 1000-1050°C, the initial molar ratio of silane to hydrogen is 0.08, and the initial m...

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Abstract

The invention discloses an interface wettability regulation and control method for inhibiting growth of silicon dendrites in a CVD process of zone-melting-grade polycrystalline silicon, and relates to the field of zone-melting-grade polycrystalline silicon. The method comprises the steps of removing surface impurities on the surface of a U-shaped silicon core; placing in a thermal cracking furnace reactor, and replacing air with nitrogen; replacing nitrogen with hydrogen; continuously introducing hydrogen, loading current to the silicon core in the reactor so as to enable an oxide layer on the surface of the silicon core to be reduced, regulating and controlling the wettability of the silicon core, and constructing a super-hydrophilic silicon surface; and regulating the current to control the silicon core to reach the reaction temperature, introducing mixed gas of high-purity silane and high-purity hydrogen, enabling the silane to be subjected to high-temperature cracking on the surface of the silicon core, enabling the product silicon to be subjected to uniform nucleation and layered growth on the surface of the super-hydrophilic silicon core, and finally obtaining a compact polycrystalline silicon rod . According to the method, the problems of 'island growth' and silicon dendrites in the silicon deposition process can be effectively inhibited by regulating and controlling the surface interface and reducing the nucleation barrier, so that the product meeting the mechanical property of the zone-melting-grade polycrystalline silicon is obtained, and the method is reasonable in design, convenient to operate and high in practicability.

Description

technical field [0001] The invention relates to the field of zone melting level polysilicon, in particular to an interface wettability control method for inhibiting the growth of silicon dendrites during the CVD process of zone melting level polysilicon. Background technique [0002] Polysilicon can be divided into solar grade and electronic grade. Solar grade polysilicon is the basic raw material of the solar energy industry chain, mainly used to produce solar panels, and mostly used in some large-scale environmental protection projects. Electronic grade polysilicon, as a key basic material for the preparation of integrated circuits, is a strategic raw material for the development of the national integrated circuit industry, mainly used in the production of electronic equipment and chips. District melting grade polysilicon is a high-end product of electronic grade polysilicon. District melting grade rod-shaped polysilicon refers to a rod-shaped crystalline silicon material ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/035
CPCC01B33/035
Inventor 梁正孟国均李建设吕永峰郭蕊钱光凝仪得志陈源茂刘纪江丁远清
Owner 河南硅烷科技发展股份有限公司
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