Method for preparing alpha-phase molybdenum carbide crystals through microwave plasma enhanced chemical vapor deposition

A technology of chemical vapor deposition and microwave plasma, which is applied in the direction of gaseous chemical plating, metal material coating process, coating, etc., can solve the problems of different research results, affecting the performance and content of molybdenum carbide, and achieve energy density Large, deposition-promoting, easily dissociated effects

Inactive Publication Date: 2016-10-12
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It is reported that molybdenum carbide crystals will undergo superconducting transition at a temperature of 10K. However, the related research results are not the same. The main reason is that there are certain defects in the preparation method of molybdenum carbide crystals.
Most of the traditional molybdenum carbide crystal preparation methods use a mixed gas of methane and hydrogen to reduce molybdenum oxide, and the product is a powdery molybdenum carbide crystal. Due to the difficulty in controlling the reactio...

Method used

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  • Method for preparing alpha-phase molybdenum carbide crystals through microwave plasma enhanced chemical vapor deposition
  • Method for preparing alpha-phase molybdenum carbide crystals through microwave plasma enhanced chemical vapor deposition
  • Method for preparing alpha-phase molybdenum carbide crystals through microwave plasma enhanced chemical vapor deposition

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Using ethanol and acetone solutions in sequence to ultrasonically clean the silicon substrate to remove surface impurities. Subsequently, the silicon wafer is placed in the center above the substrate stage, the metal flange is sealed, and the cavity is evacuated.

[0025] (2) Pass hydrogen into the chamber, adjust the microwave power, hydrogen flow and pressure, and the gas absorbs microwave energy to excite plasma. The process parameters used are: hydrogen flow 200 sccm, working pressure 10kPa, microwave power 800W.

[0026] (3) Adjust the height of the substrate stage so that the plasma wraps the silicon wafer and heats the silicon substrate (the temperature is 600°C-800°C, and the temperature is determined by the heat generated by microwave energy). Adjust the vacuum trimmer valve to keep the air pressure in the chamber at about 11kPa.

[0027] (4) When the plasma state is stable, feed methane and molybdenum hexafluoride successively to adjust the gas flow and r...

Embodiment 2

[0031] (1) Using ethanol and acetone solutions in sequence to ultrasonically clean the silicon substrate to remove surface impurities. Subsequently, the silicon wafer is placed in the center above the substrate stage, the metal flange is sealed, and the cavity is evacuated.

[0032] (2) Pass hydrogen into the cavity, adjust the microwave power, hydrogen flow and air pressure, and the gas absorbs microwave energy to excite and generate plasma. The process parameters used are: hydrogen flow 300 sccm, working pressure 10kPa, microwave power 1000W.

[0033] (3) Adjust the height of the substrate table so that the plasma wraps the silicon wafer and heats the silicon substrate (the temperature is 600°C-800°C). Adjust the vacuum trimmer valve to keep the air pressure in the chamber at about 15kPa.

[0034] (4) When the plasma state is stable, feed methane and molybdenum hexafluoride successively to adjust the gas flow and ratio (the volume ratio of methane and molybdenum hexafluorid...

Embodiment 3

[0037] (1) Using ethanol and acetone solutions in sequence to ultrasonically clean the silicon substrate to remove surface impurities. Subsequently, the silicon wafer is placed in the center above the substrate stage, the metal flange is sealed, and the cavity is evacuated.

[0038] (2) Pass hydrogen into the cavity, adjust the microwave power, hydrogen flow and pressure, and the gas absorbs microwave energy to excite plasma. The process parameters used are: hydrogen flow 300sccm, working pressure 10kPa, microwave power 1200W.

[0039] (3) Adjust the height of the substrate table so that the plasma wraps the silicon wafer and heats the silicon substrate (the temperature is 600°C-800°C). Adjust the vacuum trimmer valve to keep the air pressure in the chamber at about 20kPa.

[0040] (4) When the plasma state is stable, feed methane and molybdenum hexafluoride successively to adjust the gas flow and ratio (the volume ratio of methane and molybdenum hexafluoride is CH 4 :MoF 6...

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Abstract

The invention belongs to the field of two-dimensional crystal preparation and discloses a method for preparing alpha-phase molybdenum carbide crystals through microwave plasma enhanced chemical vapor deposition. The method is characterized by comprising the steps of 1, placing cleaned silicon wafers into a cavity of a device for preparing the molybdenum carbide crystals and vacuumizing the cavity; 2, guiding hydrogen gas into the cavity, adjusting the microwave power, the hydrogen flow and the air pressure and stimulating generation of plasmas after gas inside the cavity absorbs the microwave energy; 3, covering the silicon wafers with the plasmas, heating the silicon wafers, adjusting a vacuum micrometering valve and enabling the air pressure inside the cavity to be kept within a certain range; and 4, sequentially guiding methane and molybdenum hexafluoride into the cavity after the state of the plasmas becomes stable, adjusting the gas flow and the proportion, turning off a microwave source after reaction is completed, taking out samples after the cavity is cooled and finally obtaining the alpha-phase molybdenum carbide crystals. The purity of the molybdenum carbide crystals prepared through the method is high, research on the characteristics such as the electric property and the superconductivity of the molybdenum carbide crystals is convenient, and the obtained samples have low-temperature superconductivity.

Description

technical field [0001] The invention belongs to the field of two-dimensional crystal preparation, and in particular relates to a method for preparing α-phase molybdenum carbide crystals by a microwave plasma chemical vapor deposition device. Background technique [0002] With the discovery of graphene and graphene-like two-dimensional materials, two-dimensional materials have attracted much attention due to their unique structure and composite form, and exhibit excellent properties. When the material is thinned to a certain thickness, the electronic structure will appear. The change of the energy band gap leads to the improvement of the electronic transition mode. Two-dimensional materials have a wide range of applications in electro-optical devices, catalysis, electrochemistry, photodetection, etc. Transition metal carbides (TMCs), such as molybdenum carbide (Mo 2 C) is a class of materials with special properties and applications. In the crystal structure, the combinatio...

Claims

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Application Information

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IPC IPC(8): C23C16/32C23C16/511
CPCC23C16/32C23C16/511
Inventor 赵洪阳马志斌蔡康高攀
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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