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Preparation method of seed crystal-free fine monocrystal diamond micro-powder

A diamond and diamond single crystal technology, which is applied in metal material coating process, gaseous chemical plating, coating, etc., can solve the problems of ignoring the influence of growth and lattice distortion of single crystal particles, and achieve concentrated size distribution and high Impact resistance, the effect of eliminating the particle size screening process

Inactive Publication Date: 2014-11-26
SHANGHAI JIAO TONG UNIV +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] After searching the literature of the prior art, it is found that Taiwan KINIK Company has recorded a method of synthesizing seedless diamond single crystals using HFCVD diamond equipment in the literature "The CVD growth of micro crystals of diamond" published in the journal "Diamond and Related Materials". Crystal particle method, this method uses oxygen-free copper as the substrate, and under the condition of no diamond crystal seed, by controlling the distance between the hot wire and the substrate, the preparation of ultra-fine diamond with good crystal shape of 6-7μm is realized. However, it ignores the influence of carbon source concentration, reaction pressure, and bias current intensity on the growth of CVD seedless diamond single crystal particles, which makes the synthesized single crystal particles have crystal shape quality problems such as lattice distortion, and how to achieve seedless diamond with different particle sizes The preparation of crystalline diamond single crystal micropowder and how to collect the particles non-destructively failed to propose an effective solution

Method used

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Effect test

Embodiment 1

[0030] The preparation of M0 / 0.5 particle size CVD high-grade fine diamond single crystal micropowder is carried out on the mirror polished single crystal silicon substrate.

[0031] First, the surface of the silicon-based substrate was uniformly mechanically ground for 0.5 min with 0.5 μm diamond micropowder, and then the mechanically ground silicon-based substrate was ultrasonically cleaned in deionized water and acetone solution for 3 min.

[0032] Next, put the pretreated silicon-based substrate into the reaction chamber of the hot-wire CVD device for deposition. The hot-wire adopts a twisted-pair tantalum wire with a diameter of Φ0.4mm, and arranges the hot-wire in parallel on the silicon-based substrate. Above, and use high temperature resistant springs to keep the hot wire in a straight and horizontal state during the deposition process. After the reaction chamber is evacuated, the reaction gas (hydrogen and acetone) is introduced, and after adjusting the pressure of th...

Embodiment 2

[0036] The preparation of CVD high-grade fine diamond single crystal powder with M0 / 1 particle size is carried out on the mirror polished single crystal silicon wafer as the substrate.

[0037] First, the silicon-based substrate surface was uniformly mechanically ground for 1 min with 2.0 μm diamond micropowder, and then the mechanically ground silicon-based substrate was ultrasonically cleaned in deionized water and acetone solution for 5 min, respectively.

[0038] Next, put the pretreated silicon-based substrate into the reaction chamber of the hot-wire CVD device for deposition. The hot-wire adopts a twisted-pair tantalum wire with a diameter of Φ0.4mm, and arranges the hot-wire in parallel on the silicon-based substrate. Above, and use high temperature resistant springs to keep the hot wire in a straight and horizontal state during the deposition process. After the reaction chamber is evacuated, the reaction gas (hydrogen and acetone) is introduced, and after adjusting th...

Embodiment 3

[0042] The preparation of M0.5 / 1 particle size CVD high-grade fine diamond single crystal micropowder is carried out on the mirror polished single crystal silicon substrate.

[0043] First, the silicon-based substrate surface was uniformly mechanically ground for 0.7 min with 2.0 μm diamond micropowder, and then the mechanically ground silicon-based substrate was ultrasonically cleaned in deionized water and acetone solution for 4 min, respectively.

[0044] Next, put the pretreated silicon-based substrate into the reaction chamber of the hot-wire CVD device for deposition. The hot-wire adopts a twisted-pair tantalum wire with a diameter of Φ0.4mm, and arranges the hot-wire in parallel on the silicon-based substrate. Above, and use high temperature resistant springs to keep the hot wire in a straight and horizontal state during the deposition process. After the reaction chamber is evacuated, the reaction gas (hydrogen and acetone) is introduced, and after adjusting the pressur...

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Abstract

The invention discloses a preparation method for seed crystal-free fine monocrystal diamond micro-powder. The preparation method comprises the following steps of: uniformly and independently dispersing nuclear bodies on a silicon-based substrate by adopting a matrix self-nucleation substrate pre-treatment method; depositing the pre-treated silicon-based substrate by using a hot filament chemical vapour deposition method which comprise two phases, namely diamond nucleation and diamond grain growth, so as to obtain diamond monocrystal grains with regular crystalline forms; and treating the obtained diamond monocrystal grains by combining the process of chemical corrosion to the silicon-based substrate and a high-speed grain centrifugal sedimentation process so as to obtain the fine monocrystal diamond micro-powder. The proportion of crystals of high-grade hexahedral to octahedral poly-crystal shapes or icosahedral poly-crystal shape in the fine monocrystal diamond micro-powder obtained by the preparation method disclosed by the invention is high; the fine micro-powder obtained by the method is preponderant in terms of crystalline form and surface quality; and moreover, the process flow is simple, the obtained micro-powder has intensive size distribution, and a granularity screening process for the micro-powder can be omitted.

Description

technical field [0001] The invention relates to the technical field of diamond manufacturing, in particular to a method for preparing seed-free fine diamond single crystal powder. Background technique [0002] Diamond powder usually refers to diamond particles with a particle size between 0.1 μm and 54 μm, and those smaller than 5 μm are also called fine powder. Diamond micropowder is mainly used in the ultra-precision finishing of the surface of the workpiece - grinding and polishing processes. With the development of electronic technology, there is an increasing demand for polishing precision devices such as various optoelectronic crystals, computer hard disk substrates, optical components and semiconductor integrated circuit silicon wafers. In order to meet the processing requirements of these precision devices, the fine diamond powder The demand is increasing, and at the same time, higher requirements are put forward for the crystal shape, uniformity and mechanical prop...

Claims

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Application Information

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IPC IPC(8): C23C16/27C23C16/56C01B31/06
Inventor 张韬孙方宏张文骅沈彬郭睿张志明郭松寿
Owner SHANGHAI JIAO TONG UNIV
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