Method for preparing nano crystal cubic boronnitride film

A technology of cubic boron nitride and nanocrystals, applied in chemical instruments and methods, nitrogen compounds, inorganic chemistry, etc., can solve problems such as environmental pollution, and achieve the effects of easy-to-obtain raw materials, simple equipment, and novel processes

Inactive Publication Date: 2006-10-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the third method improves the cubic phase purity of the film and reduces the residual compressive stress of the film, it pollutes the environment due to the use of fluorine.

Method used

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  • Method for preparing nano crystal cubic boronnitride film

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Comparison scheme
Effect test

Embodiment 1

[0020] The preparation of nanocrystalline cubic boron nitride film comprises the following steps:

[0021] 1) Clean the surface of the substrate (silicon single crystal in this example) and place it on the substrate table and fix it with clamps. Use a vacuum pump to evacuate the reaction chamber to 10 -3 Pa;

[0022] 2) Input protective gas hydrogen and argon into the reaction chamber, heat the substrate and control its temperature at 600°C, adjust the pressure of the reaction chamber to 0.2Pa, and generate plasma in the reaction chamber;

[0023] 3) Adjust the substrate bias to -80V, and then input nitrogen, chlorine and BCl into the reaction chamber in sequence 3 , to carry out thin film growth, control the flow rate of nitrogen gas to 2 sccm, the flow rate of chlorine gas to 1 sccm, BCl 3 The flow rate is 3sccm. After 30 minutes of deposition, a cubic boron nitride film with a grain size of 5-30 nanometers is obtained on the silicon substrate.

Embodiment 2

[0025] The preparation of nanocrystalline cubic boron nitride film comprises the following steps:

[0026] 1) Clean the surface of the substrate (glass in this example) and place it on the substrate table and fix it with clamps; evacuate the reaction chamber to 10°C with a vacuum pump. -3 After Pa;

[0027] 2) Input protective gas hydrogen and neon into the reaction chamber, heat the substrate and control its temperature at 500°C, adjust the pressure of the reaction chamber to 2Pa, and generate plasma in the reaction chamber;

[0028] 3) Adjust the substrate bias to -20V, and then input nitrogen, ammonia and BCl into the reaction chamber in sequence 3 , to carry out thin film growth, control the flow rate of nitrogen gas to 2 sccm, the flow rate of ammonia gas to 2 sccm, BCl 3 The flow is at 2sccm. After 20 minutes of deposition, a cubic boron nitride film with a grain size of 5-20 nanometers is obtained on the silicon substrate.

Embodiment 3

[0030] The preparation of nanocrystalline cubic boron nitride film comprises the following steps:

[0031] 1) Clean the surface of the substrate (silicon single crystal in this example) first, place it on the substrate table and fix it with clamps; use a vacuum pump to vacuum the reaction chamber to 10 -3 Pa;

[0032] 2) Input protective gases hydrogen, neon and argon into the reaction chamber, heat the substrate and control its temperature at 900°C, adjust the pressure of the reaction chamber to 5Pa, and generate plasma in the reaction chamber;

[0033] 3) Adjust the substrate bias to -200V, and then input BH to the reaction chamber in sequence 3 ·NH 3 and hydrogen chloride for thin film growth and control of BH 3 ·NH 3 The flow rate is 5 sccm, the hydrogen chloride flow rate is 3 sccm, and after 60 minutes of deposition, a cubic boron nitride film with a grain size of 20-50 nanometers is obtained on the silicon substrate.

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Abstract

The invention discloses a method for preparing a nano crystal cubic boron nitride film, comprising the steps of: 1) cleaning the surface of a substrate and placing the substrate in the reaction chamber of a gas phase growing device, where vacuum degree in the reaction chamber is at least ten to the power -1 Pa; 2) charging protective gas into the reaction chamber, heating the substrate and controlling at 300-1100 deg.C, regulating pressure strength in the reaction chamber to 0.1-10 Pa and generating plasma in the reaction chamber; 3) controlling bias voltage on the substrate at 0-250 V, then in turn charging nitrogen source, chlorine source and boron source into the reaction chamber and making film growth. The invention has characters of simple process and equipment, easy to obtain raw materials, and the prepared film has high purity and low residual stress, size of crystal grains less than 50 nm, low surface roughness, and high hardness.

Description

technical field [0001] The invention relates to a preparation method of a nanocrystalline cubic boron nitride film. Background technique [0002] The Vickers hardness of cubic boron nitride film reaches 5000-6000kg / mm 2 , the hardness in nature is second only to diamond, because the cubic boron nitride film does not react with iron-based alloys and oxygen in the air even at a high temperature of 1100 ° C, it is expected to become an ideal tool material for processing steel products (diamond at temperature When it reaches 700°C, it begins to chemically react with iron and oxygen, which is not suitable for processing steel materials). In addition, the cubic boron nitride film is transparent in the infrared and visible regions, has a band gap of 6.4eV, is easy to do p-type and n-type doping, and has high thermal conductivity. It can also be widely used in the protective film of optical components, the automatic control of ultra-high-power machines in harsh environments, as we...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/064
Inventor 杨杭生
Owner ZHEJIANG UNIV
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