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Method for preparing diamond film through multiple-doped hot filament chemical vapor deposition

A technology of diamond thin film and hot wire chemistry, which is applied in the direction of gaseous chemical plating, metal material coating process, coating, etc., can solve the problems of processing accuracy and surface finish, difficulty in grinding and polishing, and decrease in tool durability. Achieve the effect of improving insulation performance and smoothness, and facilitating adhesion

Active Publication Date: 2012-07-18
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the other hand, due to the crystallization habit of diamond, the surface of the conventional thin film coating is uneven, and the hardness of diamond is extremely high, so it is very difficult to grind and polish. Therefore, in the application of coating molds and wear-resistant devices, grinding and polishing Heavy workload
The Chinese invention patent (ZL01113027.X) adopts conventional and nano-diamond coating composite technology to reduce the polishing workload of diamond film, but due to the large internal stress of the nano-diamond coating, the nano-coating will partially peel off during polishing. In the application of diamond-coated tools, the rough surface of the film increases the cutting resistance, the coating is easy to peel off, the durability of the tool is significantly reduced, and it also has an adverse effect on the machining accuracy and surface finish.
In addition, in the field of thin film microfabrication, the surface of diamond thin film is uneven, which makes it difficult to improve its lithographic resolution, and has always hindered the application of diamond thin film in the field of microelectromechanical systems.

Method used

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  • Method for preparing diamond film through multiple-doped hot filament chemical vapor deposition
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  • Method for preparing diamond film through multiple-doped hot filament chemical vapor deposition

Examples

Experimental program
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Effect test

Embodiment 1

[0037] The substrate is a polished high-resistance silicon wafer at 3 o'clock. The pretreatment uses W1 diamond micropowder to grind the polished surface for 15 minutes. After washing with pure water, it is dried and placed on a rotating platform in the reaction chamber to start the deposition of CVD diamond film. There are six Φ6 parallel straight-drawn tantalum wires (hot wires) above the rotating platform, and the distance between the tantalum wires and the silicon wafer is 10 mm. The deposition process conditions of the diamond film are: the carbon source is acetone, tetraethoxysilane is dissolved in the acetone, wherein the Si / C atomic ratio is 1: 100, the reaction chamber pressure is 4.5KPa, and the total gas flow weighs 700 ml / min. The volume ratio of acetone / hydrogen is 1-2:100, and the temperature of the tantalum wire is about 2100°C. After 8 hours of deposition, an intrinsic diamond film with a thickness of 16 microns and an area of ​​3 o'clock is obtained. Compared ...

Embodiment 2

[0040] Take 10 Φ5mm cemented carbide (YG6) milling cutters, place the blades of the milling cutters in Murakami agent for ultrasonic corrosion, and the formula (weight ratio) of the corrosion solution is potassium ferricyanide: potassium hydroxide: water is 1: 1:10, the time is about 20 minutes, take it out and wash it with water, then put it in hydrochloric acid hydrogen peroxide solution (volume ratio 1:4) to corrode for 20-30 seconds, wash it with water, then put it in diamond micropowder (particle size 20 microns) ethanol Ultrasonic oscillation treatment in the suspension for 20 minutes, then wash and dry, insert 10 milling cutters evenly into the cooling socket and place them in the CVD reaction chamber to start the deposition of the CVD diamond film coating. The process parameters are: carbon source is acetone Mainly, tetraethoxysilane and trimethyl borate are dissolved at the same time, wherein the Si / C atomic ratio is 3:100, the B / C atomic ratio is 1:100, the reaction c...

Embodiment 3

[0043] Take 5 Φ15mm cemented carbide (YG6) milling cutters, place the blades of the milling cutters in Murakami agent for ultrasonic corrosion, and the formula (weight ratio) of the corrosion solution is potassium ferricyanide: potassium hydroxide: water is 1: 1:10, the time is about 20 minutes, take it out and wash it with water, then put it in sulfuric acid hydrogen peroxide solution (volume ratio 1:10) to corrode for 20-30 seconds, wash it with water, then put it in diamond micropowder (particle size 20 microns) ethanol Ultrasonic oscillation treatment in the suspension for 20 minutes, then wash and dry, insert 5 milling cutters evenly into the cooling socket and place them in the CVD reaction chamber to start the deposition of the CVD diamond film coating. The process parameters are: carbon source is acetone Mainly, dimethyldiethoxysilane, trimethyl borate and urea are dissolved at the same time, wherein the atomic ratio of Si / C is 0.1:100, the atomic ratio of B / C is 0.1:10...

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Abstract

The invention discloses a method for preparing a diamond film through multiple-doped hot filament chemical vapor deposition and a reaction gas conveying device for the method. The method uses silicon, silicon carbide or silicon nitride ceramics, hard alloy and high-melting-point metal materials (including tungsten, tantalum, molybdenum, titanium and the like) as a substrate and adopts a chemical vapor deposition (CVD) method as the deposition means, an organic compound containing Si, an organic compound containing Si and N, an organic compound containing Si and B or an organic compound containing Si, N and B are simultaneously added into reaction gas hydrogen and acetone (or acetone and carbinol) steam to form a multiple-doped system. a submicron or nanoscale diamond film coating is obtained through the reaction, and the coating thickness can be adjusted in a range of 10-50 mum. The diamond film has the characteristics of abrasion resistance, corrosion resistance, high insulation resistance (in a boron-free occasion), smooth surface, small friction coefficient, easy grinding and polishing and the like, namely has the double advantages of a micro-diamond coating and a nano-diamond coating.

Description

technical field [0001] The invention relates to a preparation method in the field of thin film technology, in particular to a method for preparing a diamond thin film by multi-component doped hot wire chemical vapor deposition and a reaction gas delivery device. Background technique [0002] Chemical vapor deposition (referred to as CVD method, Chemical Vapor Deposition) diamond film has various excellent physical and chemical properties, its hardness is extremely high, and the friction coefficient between metal and ceramics is small, it has excellent thermal conductivity and Excellent chemical stability. Intrinsic diamond film is a good insulator, and it is an excellent semiconductor material after doping. In addition, the optical transmittance of diamond film coating is also very good. At present, CVD diamond technology has been practically applied, such as coating molds, cutting tools and wear-resistant devices in the field of tools, electrochemical corrosion-resistant a...

Claims

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Application Information

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IPC IPC(8): C23C16/455C23C16/46C23C16/30
Inventor 孙方宏张文骅张志明郭松寿沈荷生
Owner SHANGHAI JIAO TONG UNIV
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