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Preparation method for boron-doped diamond (BDD) powder

A boron-doped diamond and diamond thin film technology, applied in the field of new material synthesis, can solve the problems of poor control of boron-doped amount, etc., and achieve the effect of controllable boron-doped amount

Inactive Publication Date: 2016-11-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There will also be B 2 o 3 After being dissolved in an organic solvent, the boron-containing organic solvent is passed into the reaction chamber with a carrier gas, but the amount of boron doping is not easy to control in this method

Method used

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  • Preparation method for boron-doped diamond (BDD) powder
  • Preparation method for boron-doped diamond (BDD) powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Use acetone, ethanol and deionized water to ultrasonically clean the titanium sheet carrier for 15 minutes, and dry it;

[0023] (2) Put an ethanol solution with a concentration of 5 mg / mL boron powder into a beaker, oscillate ultrasonically for 30 minutes to form a dispersion, drop it on a titanium sheet, and dry it to obtain a substrate;

[0024] (3) Put the dried substrate on the sample stage in the reaction chamber, and pump the background vacuum to 1×10 -3 Above Pa. Introduce hydrogen, and adjust the pumping speed of the vacuum pump to maintain the air pressure in the reaction chamber at 30Torr;

[0025] (4) The filament material is selected as tantalum wire, heated to 2000-2200°C, the substrate temperature is 650-950°C, and the substrate surface is etched with hydrogen for 40 minutes;

[0026] (5) Keep the filament temperature and the substrate temperature constant, feed methane, the percentage of hydrogen is 1%, the flow rate is 1.5 / 100sccm, and the deposit...

Embodiment 2

[0030] (1) Use acetone, alcohol and deionized water to ultrasonically clean the titanium sheet carrier for 15 minutes, and dry it;

[0031] (2) Put an ethanol solution with a concentration of 12 mg / mL titanium diboride into a beaker, oscillate ultrasonically for 30 minutes to form a dispersion, drop it on a titanium sheet, and dry it to obtain a substrate;

[0032] (3) Put the dried substrate on the sample stage in the reaction chamber, and pump the background vacuum to 1×10 -3 Above Pa. Introduce hydrogen, and adjust the pumping speed of the vacuum pump, so that the pressure in the reaction chamber is maintained at 50 Torr;

[0033] (4) The filament material is tungsten wire, heated to 2000-2200°C, the substrate temperature is 650-950°C, and the substrate surface is etched with hydrogen for 30 minutes;

[0034] (5) Keep the filament temperature and the substrate temperature constant, feed methane, the percentage of hydrogen is 1.5%, the flow rate is 1.5 / 100sccm, and the dep...

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Abstract

The invention belongs to the field of new material synthesis and provides a preparation method for a boron-doped diamond powder. An ethanol solution of a boron source is subjected to ultrasonic oscillation to form a dispersion that is then dripped onto a carrier, and the carrier is dried to obtain a substrate. A diamond film is prepared by use of a hot filament chemical vapor deposition (HFCVD) method; fine cleaning and activation treatment are performed on the substrate in the environment of 100% hydrogen, and the activation treatment lasts for 20-40 min. During the activation treatment and the deposition of the diamond film, the temperature is maintained within a range of 2000 to 2200 DEG C; the temperature of the substrate ranges from 650 to 950 DEG C; the total pressure in a reaction chamber ranges from 20 to 70 Torr. During the deposition of the diamond film, the concentration of methane ranges from 0.5% to 2%, and the deposition lasts for 1 to 6 h; the diamond film is placed in a tubular furnace; a protective gas is fed into the tubular furnace after the furnace is vacuumized, followed by diffusion annealing treatment. The method has the advantages of simplicity, convenience, safety, controllable boron doping quantity and the like. The method is especially suitable for preparing BDD electrodes acting as cathode catalysts for fuel cells.

Description

technical field [0001] The invention belongs to the field of new material synthesis, and relates to the synthesis of electrochemical catalysis or active electrode materials, in particular to boron-doped nanometer, submicron or micron diamond, to obtain boron doped diamond (BDD) with conductive properties, so as to effectively Applied in various fields of electrochemistry. Background technique [0002] BDD is a widely studied electrode catalytic material with good physical and chemical properties, such as high mechanical strength, high hardness, electrical resistivity and thermal conductivity, good light transmittance, biocompatibility, chemical inertness and good Conductivity; electrochemically, it has a wide potential window, low double-layer capacitance, adsorption and background current, and has extremely high corrosion resistance in different solutions. As a catalyst material, it is widely used in the fields of electroanalysis, electrosynthesis, sewage treatment, fuel c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/27C23C16/56C23C16/02C01B31/06
CPCC01P2002/82C23C16/02C23C16/271C23C16/56
Inventor 张贵峰索妮王蕾黄昊
Owner DALIAN UNIV OF TECH