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Electrochemical corrosion method for observing nano second phase in zirconium alloy

An electrochemical and zirconium alloy technology, applied in scientific instruments, measuring devices, instruments, etc., can solve problems such as observation limitations, complicated sample preparation, and difficult operation, and achieve a clear outline of the second phase, simple preparation methods, and convenient operation Effect

Inactive Publication Date: 2019-03-12
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method is simple to operate, can accurately, quickly and clearly display the morphology, size and distribution characteristics of the nano-sized second phase in zirconium alloys, and solves the problem of sample preparation in the study of zirconium alloy nano-sized second phases in existing TEM technology. Complex, operationally difficult, observational limitations

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  • Electrochemical corrosion method for observing nano second phase in zirconium alloy
  • Electrochemical corrosion method for observing nano second phase in zirconium alloy
  • Electrochemical corrosion method for observing nano second phase in zirconium alloy

Examples

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Embodiment 1

[0047] Zircaloy-4 alloy (Zr-1.5wt%Sn-0.2wt%Fe-0.1wt%Cr) is the most widely used zirconium-tin zirconium alloy in nuclear reactors, which has excellent corrosion performance and good mechanical properties . The matrix phase of Zircaloy-4 (hereinafter referred to as Zr-4) at room temperature is the α-Zr phase of the hexagonal close-packed structure, and the common second phase morphology in the alloy is mainly spherical or ellipsoidal, and the second phase size is about Around 100nm. What used in the present embodiment is the Zr-4 alloy of cold-rolled annealing state, and concrete implementation steps are as follows:

[0048] (1) Preparation of electrochemical corrosion agent: First, measure 450ml of alcohol with a graduated cylinder and place it in a glass beaker. Under a backlit environment at room temperature, measure 50ml of perchloric acid with a graduated cylinder, and slowly pour it into the above-mentioned beaker with a glass rod drainage In the process, the electroche...

Embodiment 2

[0054] What is used in this embodiment is forged Zircaloy-2 whose nominal composition is Zr-1.5Sn-0.1Fe-0.1Cr-0.05Ni (wt%). The alloy is a commercial zirconium alloy, which is mainly used in the field of nuclear reactor cladding. In the present embodiment, the electrochemical corrosion process steps of the second phase of the wrought Zircaloy-2 alloy are as follows:

[0055] (1) prepare electrochemical etchant: get the methanol solution of 50ml perchloric acid solution and 450ml, prepare electrochemical etchant according to description in the summary of the invention step (1);

[0056] (2) Sample preparation: After the wrought Zircaloy-2 alloy to be corroded is polished with 150#, 320#, 800#, 2000# water-grinding sandpaper in sequence, then nano-SiO 2 The suspension is mechanically polished until the polished surface shows a mirror effect, and then the sample is washed with water and alcohol in turn, and dried for use;

[0057] (3) Electrochemical corrosion process: pour the...

Embodiment 3

[0060] N18 (Zr-1Sn-0.3Nb-0.3Fe-0.1Cr) is a new type of zirconium alloy for stacking independently developed by my country. This embodiment is mainly for the corrosion of the second phase of the extruded N18 alloy, and the main steps are as follows:

[0061] (1) prepare electrochemical etchant: get 40ml perchloric acid solution, 400ml ethanol and 60ml methyl alcohol, prepare electrochemical etchant according to description in the step (1) of the summary of the invention;

[0062] (2) Sample preparation: After polishing the N18 zirconium alloy to be corroded through 150#, 320#, 800#, and 2000# water-grinding sandpaper in sequence, then use nano-SiO 2 The suspension is mechanically polished until the polished surface shows a mirror effect, and then the sample is washed with water and alcohol in turn, and dried for use;

[0063] (3) Electrochemical corrosion process: pour the electrochemical etchant prepared in step (1) into the beaker of the electrochemical corrosion device, the...

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Abstract

The invention aims to provide an electrochemical corrosion method capable of accurately and clearly displaying a nano second phase in a zirconium alloy, so as to achieve the purpose of observing and counting the second phase in the zirconium alloy under a scanning electron microscope. The method adopts a unique electrochemical corrosion reagent, takes a zirconium alloy sample as an anode, takes astainless steel plate as a cathode, and adopts liquid nitrogen to perform electrochemical corrosion after cooling; and the second phase can be finally observed under the scanning electron microscope.The method is simple in operation; morphology features, dimension sizes and distribution features of the nano-scale second phase in the zirconium alloy can be accurately, quickly and clearly displayed; and the problems of complex sample preparation, difficult operation and limited observation in research on the nano second phase in the zirconium alloy in an existing TEM (Transmission electron microscope) technology are solved.

Description

technical field [0001] The invention relates to the field of nanometer second phases of zirconium alloy materials and the field of metallographic electrochemical corrosion, and specifically provides an electrochemical corrosion method for observing the nanometer second phases in zirconium alloys. Background technique [0002] Zirconium alloy has a low thermal neutron absorption cross-section, which can ensure that there are enough thermal neutrons in the atomic energy reactor to maintain the normal operation of the reactor. In addition, zirconium alloy has good corrosion resistance and mechanical properties, as well as good reliability. Processability, so it is widely used in structural materials of nuclear reactors, such as cladding materials and end plugs of nuclear reactors. With the development of the economy, people have put forward higher and higher requirements for the safety and reliability of nuclear materials, so various countries have changed the microstructure of...

Claims

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Application Information

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IPC IPC(8): G01N23/2202G01N23/2251
CPCG01N23/2202G01N23/2251
Inventor 李阁平韩福洲刘承泽袁福森张英东郭文斌穆罕默德.阿里顾恒飞
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI