Corrosive agent and corrosion method for second phase of zirconium alloy

A kind of corrosive agent and zirconium alloy technology, which is applied in the field of corrosion analysis of zirconium alloy microstructure, to achieve the effect of simple and efficient research work

Inactive Publication Date: 2018-12-21
INST OF METAL RESEARCH - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention can well solve the problem that there is a vacancy in the existing research on the second phase of zirconium alloy, so that the research on the macroscopic distribution of the second phase of zirconium alloy, the statistics of particle size and the research on the relationship with the matrix become simple and efficient

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  • Corrosive agent and corrosion method for second phase of zirconium alloy
  • Corrosive agent and corrosion method for second phase of zirconium alloy
  • Corrosive agent and corrosion method for second phase of zirconium alloy

Examples

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Effect test

Embodiment 1

[0033] Zircaloy-4 alloy, its nominal composition is Zr-1.5Sn-0.2Fe-0.1Cr (wt.%). The alloy has excellent corrosion resistance and is widely used as cladding material for pressurized water reactors and heavy water reactors. This embodiment adopts the Zircaloy-4 alloy (hereinafter referred to as the annealed Zircaloy-4 alloy) of forging + annealing treatment, and its matrix structure is a typical equiaxed structure, the grain size is 5-16 μm, and the type of phase is HCP structure The α phase, the specific organization is as attached figure 2 shown. The second phase in the alloy was observed in STEM mode by transmission electron microscopy. as attached image 3 shown, with image 3 Round or oval grains with medium black contrast are the second phase in the alloy.

[0034] The second phase etchant of the annealed Zircaloy-4 alloy consists of hydrofluoric acid (HF), nitric acid (HNO 3 ) and water (H 2 O) composition, the volume proportion of its each component is: 20 μ l (...

Embodiment 2

[0046] For the annealed Zircaloy-4 alloy in Example 1, the volume of HF in the second-phase etchant must be controlled at about 20 μl (provided that the volumes of water and nitric acid are both 70ml), if the volume of HF is too small, you can use extended However, if the concentration of HF in the etchant is too high or the corrosion time is too long, the corrosion effect will be poor or even distorted. For example: using corrosive agent: 100μl hydrofluoric acid, 70ml nitric acid, 70ml H 2 O, corrosion time 0.5min. The corroded samples were observed under a scanning electron microscope, and the obtained morphology was as attached Figure 6 It can be seen that severe pitting corrosion has occurred on the polished surface of the alloy, and sharp corrosion holes will be left after the substrate is corroded (the corrosion holes of the second phase are rounder). These traces of local corrosion have covered up the second phase At this time, the specific information of the second ...

Embodiment 3

[0048] Zircaloy-2 is a commercial zirconium alloy widely used in nuclear reactor cladding materials. The organization of Zircaloy-2 in the as-cast state is attached Figure 7 As shown, the organization is a lamellar α-phase interlaced weaving. Observe the second phase in the alloy in STEM mode. as attached Figure 8 shown, with Figure 8 Round or oval grains with medium black contrast are the second phase in the alloy.

[0049] The second phase corrosion agent of as-cast Zircaloy-2 alloy consists of hydrofluoric acid (HF), nitric acid (HNO 3 ) and water (H 2 O) composition, the volume proportion of its each component is: 10 μ l (40wt.%) HF+60ml (65wt.%) HNO 3 +60ml H 2 O. The disposition method of this etchant is the same as embodiment 1.

[0050] The second phase corrosion method of as-cast Zircaloy-2 alloy comprises the steps:

[0051] ① Firstly, a block sample with a size of 10*10*10mm is intercepted by wire cutting method;

[0052] ② Grinding with 150#, 400#, 80...

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Abstract

The invention aims at providing a corrosive agent and corrosion method for a second phase of zirconium alloy. The corrosive agent is characterized by being prepared from hydrofluoric acid, nitric acidand water according to a certain proportion. By corroding the second phase in the zirconium alloy through the corrosive agent, the macroscopic distribution and the particle size of the second phase of the zirconium alloy can be clearly observed. According to the corrosive agent and corrosion method for the second phase of the zirconium alloy, the problem that a blank exists in research on the second phase of the zirconium alloy can be well solved, and work such as macroscopic distribution research and particle size statistics of the second phase of the zirconium alloy and research on the relation between the second phase of the zirconium alloy and a substrate become simple and efficient.

Description

technical field [0001] The invention relates to the technical field of microstructure corrosion analysis of zirconium alloys, and in particular provides a second-phase corrosion agent and corrosion method for zirconium alloys. Background technique [0002] Zirconium alloys are widely used in nuclear reactor cladding materials due to their small thermal neutron absorption cross section, excellent corrosion resistance and good mechanical properties. For example: Zircaloy-2 (Zr-1.5Sn-0.1Fe-0.1Cr-0.05Ni), Zircaloy-4 (Zr-1.5Sn-0.2Fe-0.1Cr), E635 (Zr-1.2Sn-1Nb-0.4Fe), ZIRLO (Zr-1.0Nb-1.0Sn-0.1Fe). At present, the content of alloy elements in the relatively mature zirconium alloys is relatively small (such as the zirconium alloys listed above), so the matrix structure of zirconium alloys at room temperature is mainly α-Zr (HCP structure). Many alloying elements (such as: Fe, Cr and Nb) have small solid solubility (<0.5wt.%) in the α-Zr matrix, so these alloying elements are ea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2202
CPCG01N23/2202
Inventor 李阁平袁福森袁改焕储林华李晓珊高博罗倩倩彭胜刘承泽韩福洲张英东顾恒飞
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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