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CVD (Chemical Vapor Deposition) system for preparing refractory high-entropy alloy target material and control method thereof

A high-entropy alloy, refractory technology, applied in metal material coating process, vacuum evaporation plating, coating and other directions, can solve the problems of refractory high-entropy alloy target, low target quality, segregation, etc. The effect of the purification effect

Pending Publication Date: 2022-04-29
亚芯半导体材料(江苏)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The current preparation method of refractory high-entropy alloy target mainly relies on the traditional melting method. During the preparation process of the melting method, the difference in the melting point of the elements is likely to lead to material waste and component segregation, resulting in low quality target and complicated production process. control
[0003] At present, there is no CVD (Chemical Vapor Deposition) equipment specially used for refractory high-entropy alloy targets on the market. In order to meet higher R&D and production requirements, a new CVD system is urgently needed to prepare high-quality refractory high-entropy alloys. Alloy target

Method used

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  • CVD (Chemical Vapor Deposition) system for preparing refractory high-entropy alloy target material and control method thereof
  • CVD (Chemical Vapor Deposition) system for preparing refractory high-entropy alloy target material and control method thereof
  • CVD (Chemical Vapor Deposition) system for preparing refractory high-entropy alloy target material and control method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 1. Open the nitrogen cylinder purge pipeline;

[0041] 2. Pour the purified fluoride liquid (99.9999%) raw materials (the fluoride liquids of W, Mo, Ta, Nb, and V respectively) into the container in the evaporation area, and use water bath heating. The liquid level of the raw material should be When it is lower than the liquid level heated by the water bath, turn on the power supply to start heating, open the air inlet valve, and observe the flow of the five gases at any time. If it meets the requirements, immediately close the air pipe valve and take out the water bath beaker with tweezers;

[0042] 3. Turn on the vacuum pump, close the valve of the mixed gas zone into the vacuum chamber, and evacuate until the vacuum degree of the deposition chamber is 1.3-13Pa.

[0043] 4. Introduce hydrogen to the mixed gas area. When the flow rate reaches the standard, close all the valves of the evaporation area entering the mixed gas area, open the hydrogen analyzer, and conduct ...

Embodiment 2

[0051] The only difference between this embodiment and embodiment 1 is that the high-purity solid raw material is put into the evaporation area.

[0052] The prepared refractory high-entropy alloy target is tested. The main content of the test includes density, grain size, crystal structure analysis, etc. The test methods are Archimedes drainage method, metallographic microscope observation intercept method, XRD, ICP spectrometer etc.

[0053] Test results: XRD results show that it is a single BCC phase with a density greater than 99.6%, a purity greater than 99.9999%, and an oxygen content of less than 100ppm. Read-only spectroscopy proves that it is a high-entropy alloy with a grain size of about 25μm.

Embodiment 3

[0055] The only difference between this embodiment and embodiment 1 and embodiment 2 is that the high-purity raw material gas is put into the evaporation area.

[0056] The prepared refractory high-entropy alloy target is tested. The main content of the test includes density, grain size, crystal structure analysis, etc. The test methods are Archimedes drainage method, metallographic microscope observation intercept method, XRD, ICP spectrometer etc.

[0057] Test results: XRD results show that it is a single BCC phase with a density greater than 99.9%, a purity greater than 99.9999%, and an oxygen content of less than 100ppm. Read-only spectroscopy proves that it is a high-entropy alloy with a grain size of about 33μm.

[0058] It can be seen that the preparation of fluoride liquid can obtain refractory high-entropy alloy targets with smaller grain size and low oxygen content on the basis of meeting the maximum density and purity.

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Abstract

The invention belongs to the technical field of chemical vapor deposition, and particularly relates to a CVD system for preparing a refractory high-entropy alloy target material and a control method thereof.The CVD system comprises an evaporation area used for evaporating a fluoride liquid raw material to obtain a fluoride gasified raw material; the gas mixing area is used for being connected with the evaporation area to receive the fluoride gasification raw material and mixing the fluoride gasification raw material with hydrogen to obtain mixed gas; the deposition area is used for being connected with the gas mixing area so as to receive the mixed gas, and deposition is carried out to prepare the refractory high-entropy alloy target material; the tail gas treatment area is used for connecting the gas mixing area with the deposition area and treating gas and by-products which are not completely reacted; according to the method, most associated impurities in fluoride liquid are removed by evaporating the fluoride liquid by utilizing the characteristic of low boiling point of fluoride, and meanwhile, a better purification effect is achieved by utilizing the characteristic of low hydrogen reduction temperature and cooperating with a fluoride gasification raw material; and under the action of thermodynamic driving force, crystals can be formed at a higher deposition rate to obtain the refractory high-entropy alloy target material.

Description

technical field [0001] The invention belongs to the technical field of chemical vapor deposition, and in particular relates to a CVD system for preparing a refractory high-entropy alloy target and a control method thereof. Background technique [0002] At present, the research on high-entropy alloys has attracted more and more attention, and high-entropy thin films have shown better performance than bulk materials, especially in terms of hardness, wear resistance, corrosion resistance, and oxidation resistance. The refractory high-entropy alloy film has excellent high-temperature stability, and is expected to be used in high-end manufacturing industries such as aerospace to replace high-temperature alloys, especially the use of alloy films to modify the surface of structural parts to replace GH4169 and other grades currently used in advanced aircraft aero-engines . The current preparation method of refractory high-entropy alloy target mainly relies on the traditional meltin...

Claims

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Application Information

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IPC IPC(8): C23C16/08C23C16/448C23C16/455C23C14/34
CPCC23C16/08C23C16/4481C23C16/45512C23C14/3414
Inventor 徐从康贺涛马赛王江涌陈箫箫
Owner 亚芯半导体材料(江苏)有限公司
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