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Method for preparing substrate material with multilayer composite protective film

A base material, multi-layer composite technology, applied in metal material coating process, coating, gaseous chemical plating and other directions, can solve the problems of high temperature, inability to form a uniform film, lack of step coverage, etc., to achieve good oxidation resistance. Effect

Inactive Publication Date: 2011-02-16
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The above-mentioned technologies have a very wide range of applications, but for products, devices, and parts with particularly complex three-dimensional structures, PVD, CVD and other methods have serious limitations, lack of good step coverage, and cannot form uniform films on all surfaces
At the same time, for some electronic devices, the temperature required by the common CVD method is too high, which also limits its application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: Depositing a multilayer composite protective film on Cu, the steps are:

[0025] 1. Pretreat the Cu base material and put it into the reaction chamber, evacuate to an air pressure of 0.1~10 Torr, heat to 100 oC~500 oC, preferably between 200 oC~350 oC,

[0026] 2. Introduce the trimethylaluminum TMA precursor for a duration of 0.2s to 5s, preferably 0.5s to 3s, then inhale nitrogen for 2 to 4s, and then introduce ozone for a reaction time of 0.2s to 5s, preferably 0.5s to 3s, and finally blowing in nitrogen for 2 to 4s, repeating this more than 10 times, preferably 10 to 100 times, to form 2 to 50nm Al 2 o 3 Floor.

[0027] 3. Pass SiCl 4 For the precursor, the duration is 0.2s to 5s, preferably 2s to 4s, and then nitrogen is passed through for cleaning for 2 to 4s, and then ozone is passed through for a reaction time of 0.2s to 5s, preferably 1s to 3s, and finally nitrogen is passed through for cleaning. The time lasts for 2-4s, and this is repeated m...

Embodiment 2

[0029] Example 2: Repeat the above steps 2-3 for the composite protective film obtained in Example 1, so that the thickness of the composite layer reaches 10-50 nm. Experiments have shown that the thickness of the formed composite protective film is controllable, with good uniformity and compactness. When the thickness reaches 10nm or more, it has good protective performance, and the preferred thickness is between 10nm and 10nm. No discoloration occurred after 24 hours as checked by the thioacetamide corrosion test (TAA test).

Embodiment 3

[0030] Example 3: Depositing a multi-layer composite protective film on a 5252 aluminum-magnesium alloy substrate, the implementation steps are the same as in Example 2, and a protective film with good uniformity and compactness can also be obtained. No discoloration occurred after 30 hours by thioacetamide corrosion test (TAA test).

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PUM

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Abstract

The invention relates to a method for preparing a substrate material with a multilayer composite protective film, which comprises the following steps: putting the substrate material into a reaction chamber, and heating the substrate material until the temperature thereof is 100 to 500 DEG C; introducing trimethyl aluminum or Al (CH3) N (CH2) 5CH3 precursor into the reaction chamber within 0.2 to 0.5 seconds under the pressure of 0.1 to 10 Torr; introducing nitrogen or inert gas into the reaction chamber so as to remove the trimethyl aluminum or Al (CH3) N (CH2) 5CH3 residual gas which is not subjected to chemisorption by a substrate; under the pressure of 0.1 to 10 Torr, introducing ozone or vapor reactive gas into the reaction chamber within 0.2 to 0.5 seconds so as to deposit an alumina atom layer on the substrate, wherein the thickness of the alumina atom layer on the substrate is 2 to 100nm; and replacing the trimethyl aluminum or Al (CH3) N (CH2) 5CH3 precursor by using chlorosilane, hexachlorodisilane or tetraethyl orthosilicate as silicon source, then repeating the steps above, and covering a silicon dioxide layer on an alumina layer, wherein the thickness of the alumina layer is 2 to 100nm; and finally, obtaining the substrate material with a composite inorganic protective film in a Al2O3 / SiO2 double-layer structure, wherein the thickness of the substrate material is 5 to 120nm. The method can precisely control the thickness of the film, wherein the thickness of the film can directly and precisely be controlled within a range of 1 to 100nm, and the film has excellent oxidation resistance and gas permeation resistance, and can control the ratio of Al2O3 to SiO2.

Description

field of invention [0001] The invention relates to a preparation method of a base material with a multilayer composite inorganic protective film. Background technique [0002] There are many methods for protecting metal products, devices, and parts, such as surface modification, protective agent coating, surface coating and other technologies. Among them, a layer of aluminum oxide, silicon oxide, titanium nitride, silicon carbide, diamond-like film, etc. is formed on the metal surface by spraying, physical or chemical vapor deposition methods. The above materials have low gas permeability to oxygen-containing gases such as air or water vapor. Moreover, it has good hardness, which can not only improve its oxidation resistance and barrier properties, but also improve the substrate hardness and wear resistance. For example, the patent "Alumina coating, coated products and their manufacturing method" (application number: 200580007972.2) uses chemical vapor deposition technology...

Claims

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Application Information

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IPC IPC(8): C23C16/40
Inventor 尹桂林宋佳金彩虹何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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