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Protective film for corrosion resistance of metal niobium at high temperature and preparation method of protective film

A technology of protective film and metal niobium, which is applied in the direction of metal material coating technology, climate sustainability, and reduction of greenhouse gases, and can solve problems such as corrosion of refractory metal niobium

Active Publication Date: 2021-11-30
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a protective film based on the corrosion resistance of niobium metal at high temperature and its preparation method in order to solve the problem of serious corrosion of niobium refractory metal at high temperature in view of the above-mentioned deficiencies in the prior art. Provides an effective protection approach and lays a theoretical foundation for the engineering application of refractory metal niobium in structural materials in the nuclear industry

Method used

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  • Protective film for corrosion resistance of metal niobium at high temperature and preparation method of protective film
  • Protective film for corrosion resistance of metal niobium at high temperature and preparation method of protective film
  • Protective film for corrosion resistance of metal niobium at high temperature and preparation method of protective film

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preparation example Construction

[0056] The present invention is a method for preparing a protective film based on the corrosion resistance of metal niobium at high temperature. The refractory metal niobium is placed in liquid lead-bismuth to form a protective film in situ, and the specific steps are as follows:

[0057] S1. Obtain dense niobium rods through vacuum smelting, rolling, and annealing, and then cut the niobium rods into several experimental samples of 50x6x3mm; grind the experimental samples with a grinder and ultrasonic cleaning with alcohol to remove the wire cutting marks of the samples and oil pollution;

[0058] S2. Put 500g of lead-bismuth alloy (Pb44.5%, Bi55.5%) for nuclear use into a 50ml alumina crucible, and put them together into a high-temperature energy-saving atmosphere furnace; set the program to raise the temperature in the furnace to 125-200°C , keep warm for 30-60 minutes to completely melt the lead-bismuth alloy;

[0059] The so-called mass process of the lead-bismuth alloy i...

Embodiment 1

[0086] Experimental preparation process of refractory metal Nb in situ forming protective film in liquid lead bismuth:

[0087]The production process of the refractory metal niobium used in this example: aluminothermic reduction of Nb 2 o 5 → Crude niobium → Purification by electron beam melting → Rolling → Annealing.

[0088] Among them, the thermite reduction of Nb 2 o 5 The flow chart is as figure 1 , the reaction formula is:

[0089] 3Nb 2 o 5 +10Al→6Nb+5Al 2 o 3

[0090] The impurity concentration of the finally prepared Nb is shown in Table 1. The lead-bismuth alloy used in the experiment was provided by Henan Huapu Alloy Materials Co., Ltd., China, and the impurity concentration was detected by SEM-EDS, as shown in Table 2.

[0091] 1) The diameter is obtained by smelting, rolling, heat treatment, etc. It is a 20mm dense niobium bar, and the bar is cut into 50x6x3mm experimental samples, lightly polished with 1000#, 1200#, 1500# SiC water sandpaper, and pol...

Embodiment 2

[0095] According to the aforementioned plan, the sample is taken out within the interval of 20-40h, and the cross-section of the sample in the interval of 20-40h is obtained by preparing the cross-sectional sample, such as Figure 4 As shown, the in situ generated NbO / NbO can be observed 2 The thickness of the protective film is 4-5 μm.

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Abstract

The invention discloses a protective film for corrosion resistance of metal niobium at a high temperature and a preparation method of the protective film. The preparation method comprises the following steps of sequentially carrying out vacuum melting, rolling and annealing treatment on a niobium bar, and then cutting the niobium bar into an experimental sample; melting a lead-bismuth alloy to obtain liquid lead bismuth; putting the treated experimental sample into the liquid lead bismuth, fixing the sample, and carrying out interface reaction and diffusion reaction on Nb in the experimental sample and oxygen dissolved in the liquid lead bismuth to generate a layer of NbO surface film at first; the NbO surface film further reacts with oxygen dissolved in the liquid lead bismuth to generate a layer of NbO2 protective film; and the experimental sample is taken out and placed on a stainless steel sheet, and metal niobium with the protective film is obtained after the experimental sample is cooled. The protective film lays a foundation for expanding the application of the refractory metal in the industry.

Description

technical field [0001] The invention belongs to the field of corrosion science and protection technology, and specifically relates to a protective film based on the corrosion resistance of metal niobium at high temperature and a preparation method thereof. Background technique [0002] With the rapid development of aviation, aerospace, energy, petrochemical and other industries, the requirements for the service performance of metal materials are getting higher and higher, requiring them to work under higher temperatures and harsher environments. For example, when the steam engine began to develop, the steam temperature was only 300°C, but today its operating temperature has reached 630-650°C, and the operating temperature of modern aircraft engines exceeds 1000°C. The corrosion resistance of materials at high temperatures has become one of the key factors affecting the development of the above industries, and it is imminent to adopt more perfect protection methods. [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C8/42C22C12/00
CPCC23C8/42C22C12/00Y02E30/30
Inventor 马胜强付沙沙邢建东郭鹏佳吕萍
Owner XI AN JIAOTONG UNIV
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