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Preparation method of high-quality self-support diamond thick film

A diamond thick film and diamond film technology, which is applied in metal material coating process, gaseous chemical plating, coating, etc., can solve the problems of difficult diamond thick film, easy local cracks, and increased phase content, so as to avoid Partial or penetrating cracks, good quality consistency

Active Publication Date: 2016-04-20
山西新碳超硬材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the difference in expansion coefficient between the diamond film and the base material, when the diamond film is larger than a certain thickness (generally > 1mm), this difference will cause a large thermal stress inside the film, which will cause the film to be completely in contact with the substrate. or partial peeling, while localized cracks or penetrating cracks are prone to occur in the film
In addition, studies have shown that during the CVD process, as the deposition time increases and the film thickness increases, the grain and grain boundary sizes of the diamond film will gradually increase, and the deposition rate will continue to increase. At the same time, the SP in the film 2 The phase content will increase, which will cause the mechanical properties and quality of the diamond film to decrease with the increase of thickness
The reason for this phenomenon is that during the deposition of the diamond film, as the thickness increases, the position of the film surface in the plasma changes, which leads to a change in the concentration ratio of hydrogen atoms and active groups on the film surface. , that is, the concentration of carbon groups on the surface of the film gradually increases, causing the film deposition rate to increase and the quality to decrease
Therefore, it is difficult to prepare a complete diamond thick film with high mechanical strength and uniform quality by MPCVD, which limits the application of this material to a certain extent.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0035] A high-quality diamond thick film with a diameter of 50 mm and a thickness of 2 mm was prepared using MPCVD equipment with a frequency of 2.45 GHz.

[0036] 1) Prepare a high-quality diamond film with a diameter of 50 mm and a thickness of 0.5 mm: use a Si disc with a thickness of 2 mm and a diameter of 50 mm as the substrate for preparing the diamond film, and grind the Si disc with diamond powder with a particle size of 0.2 μm to make it The surface is uniformly roughened to increase the diamond nucleation density, then ultrasonically cleaned in acetone solution, and dried with hot air. Open the reaction chamber of the MPCVD equipment, place the cleaned Si wafer at the center of the substrate table in the reaction chamber, close the reaction chamber and turn on the vacuum system, and wait until the vacuum degree of the chamber reaches 1×10 -2 When it is below Pa, feed hydrogen with a purity of 99.9999%, and its flow rate is 300 sccm, adjust the pressure of the reactio...

Embodiment 2

[0040] A high-quality diamond thick film with a diameter of 70 mm and a thickness of 3 mm was prepared using an MPCVD equipment with a frequency of 2.45 GHz.

[0041] 1) Preparation of a high-quality diamond film with a diameter of 70 mm and a thickness of 0.6 mm: use a Si disc with a thickness of 3 mm and a diameter of 70 mm as the substrate for preparing the diamond film, and grind the Si disc with diamond powder with a particle size of 0.2 μm to make it The surface is uniformly roughened to increase the diamond nucleation density, then ultrasonically cleaned in acetone solution, and dried with hot air. Open the reaction chamber of the MPCVD equipment, place the cleaned Si wafer at the center of the substrate table in the reaction chamber, close the reaction chamber and turn on the vacuum system, and wait until the vacuum degree of the chamber reaches 1×10 -2 When it is below Pa, feed hydrogen with a purity of 99.999%, and its flow rate is 700 sccm, adjust the pressure of th...

Embodiment 3

[0045] A high-quality diamond thick film with a diameter of 150 mm and a thickness of 3.5 mm was prepared using MPCVD equipment with a frequency of 915 MHz.

[0046] 1) Preparation of a high-quality diamond film with a diameter of 150 mm and a thickness of 0.7 mm: use a Si disc with a thickness of 5 mm and a diameter of 150 mm as the substrate for preparing the diamond film, and grind the Si disc with diamond powder with a particle size of 0.5 μm to make it The surface is uniformly roughened to increase the diamond nucleation density, then ultrasonically cleaned in acetone solution, and dried with hot air. Open the reaction chamber of the MPCVD equipment, place the cleaned Si wafer at the center of the substrate table in the reaction chamber, close the reaction chamber and turn on the vacuum system, and wait until the vacuum degree of the chamber reaches 1×10 -2 When it is below Pa, feed hydrogen gas with a purity of 99.99999%, and its flow rate is 2000 sccm, adjust the pressu...

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Abstract

The invention discloses a preparation method of a high-quality self-support diamond thick film. The preparation method comprises the following steps: preparing a high-quality self-support diamond film which is 0.5 to 0.7 mm thick according to a chemical vapor deposition method; conducing grinding and polishing on a nucleation surface of the high-quality self-support diamond film, removing residual carbonide, and preparing a high-quality diamond film which is 1 to 3 mm thick on the treated nucleation surface by taking the treated nucleation surface as a base body, wherein during the two preparation processes, once the thickness of the diamond film is increased by 50 to 100 [mu]m, the methane flow rate is reduced by 0.5 to 1 percent of an initial methane flow rate. The high-quality self-support diamond thick film prepared according to the preparation method is high in quality uniformity, has no crack, and is high in mechanical strength.

Description

technical field [0001] The invention relates to a method for preparing a high-quality self-supporting diamond thick film, belonging to the technical field of superhard material preparation. Background technique [0002] The self-supporting diamond film prepared by chemical vapor deposition (CVD) can be divided into tool grade, heat sink grade, optical grade and electronic grade (or detector grade) according to the quality, among which the tool grade diamond film requires relatively high mechanical strength. Performance, its interior contains a large number of various defects, so it appears gray and black in appearance. The heat sink grade diamond film needs to have relatively high thermal conductivity, and the density of various defects contained in it is lower than that of the tool grade diamond film. Optical-grade diamond film needs to have relatively high optical transmittance, which requires fewer defects in it to ensure its excellent optical transparency in appearance ...

Claims

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Application Information

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IPC IPC(8): C23C16/27C23C16/511C23C16/52
CPCC23C16/274C23C16/52
Inventor 于盛旺王荣高洁黑鸿君张阿莉刘小萍贺志勇
Owner 山西新碳超硬材料科技有限公司
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