Etchant for observation and energy spectrum analysis of sigma phase through scanning electron microscope and using method thereof

An electron microscope and energy spectrum analysis technology, which is applied in the field of etchant, can solve the problems of inability to detect and analyze the σ phase composition and affect the work of failure analysis, and achieve the effect of pollution-free erosion, simple composition and convenient use

Active Publication Date: 2019-08-16
DONGFANG BOILER GROUP OF DONGFANG ELECTRIC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the formation of corrosion pits, the energy spectrometer cannot be used to accurately detect and analyze the composition of the σ phase observed by the scanning electron microscope, which seriously affects the failure analysis work, such as Figure 1-2 shown

Method used

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  • Etchant for observation and energy spectrum analysis of sigma phase through scanning electron microscope and using method thereof
  • Etchant for observation and energy spectrum analysis of sigma phase through scanning electron microscope and using method thereof
  • Etchant for observation and energy spectrum analysis of sigma phase through scanning electron microscope and using method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 2g of copper sulfate pentahydrate as raw materials, 8g of sodium chloride, 20g of phosphoric acid, 1g of absolute ethanol, and 20g of distilled water. The purity grades of the copper sulfate pentahydrate, sodium chloride, phosphoric acid and absolute ethanol are analytically pure.

[0037] (1) Preparation of etchant: Put copper sulfate pentahydrate and sodium chloride in the container, then add distilled water and stir for 10 minutes, then add phosphoric acid and absolute ethanol, continue to stir for 20 minutes, and then let stand for 20 minutes to obtain the etching agent. etchant;

[0038] (2) Etching: Take the aging and invalid S31008 stainless steel as a sample, grind and polish the sample to be etched, and then immerse it in the etchant. During the etching process, use cotton to wipe the polished surface of the sample for 5 seconds. Take it out after light gray, rinse with water and then with absolute ethanol, and then dry it with hot air or dry it, then use...

Embodiment 2

[0043] Take 5 g of copper sulfate pentahydrate as raw materials, 12 g of sodium chloride, 30 g of phosphoric acid, 2 g of absolute ethanol, and 50 g of distilled water. The purity grades of the copper sulfate pentahydrate, sodium chloride, phosphoric acid and absolute ethanol are analytically pure.

[0044] (1) Preparation of etchant: Put copper sulfate pentahydrate and sodium chloride in the container, then add distilled water and stir for 10 minutes, then add phosphoric acid and absolute ethanol, continue to stir for 20 minutes, and then let stand for 20 minutes to obtain the etching agent. etchant;

[0045] (2) Etching: Take the aging and invalid 06Cr19Ni10 stainless steel as a sample, grind and polish the sample to be etched, and then immerse it in the etchant. During the etching process, use cotton to wipe the polished surface of the sample for 15 seconds. Take it out after light gray, rinse with water and then with absolute ethanol, and then dry it with hot air or dry i...

Embodiment 3

[0050] Take 10 g of copper sulfate pentahydrate as raw materials, 18 g of sodium chloride, 40 g of phosphoric acid, 4 g of absolute ethanol, and 70 g of distilled water. The purity grades of the copper sulfate pentahydrate, sodium chloride, phosphoric acid and absolute ethanol are analytically pure.

[0051] (1) Preparation of etchant: Put copper sulfate pentahydrate and sodium chloride in the container, then add distilled water and stir for 10 minutes, then add phosphoric acid and absolute ethanol, continue to stir for 20 minutes, and then let stand for 20 minutes to obtain the etching agent. etchant;

[0052] (2) Etching: Take aging and invalid TP347HFG stainless steel as a sample, grind and polish the sample to be etched, and then immerse it in the etchant. During the etching process, use cotton to wipe the polished surface of the sample for 20 seconds. Take it out after light gray, rinse with water and then with absolute ethanol, and then dry it with hot air or dry it, th...

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PUM

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Abstract

The invention discloses an etchant for observation and energy spectrum analysis of the sigma phase through a scanning electron microscope. The etchant is formed through mixing the following raw materials in percentage by mass: 1-12% of copper(II) sulfate pentahydrate, 8-21% of sodium chloride, 18-41% of phosphoric acid, 0.1-7.5% of absolute ethyl alcohol and 19-72% of distilled water; during the etching process of austenite heat-resistance stainless steel, the etchant composed of copper(II) sulfate pentahydrate, sodium chloride, phosphoric acid, absolute ethyl alcohol and distilled water can effectively restrain an etch pit formed through excessive corrosion, dissolving and falling; the scanning electron microscope can observe that the morphology of the sigma phase in the austenite heat-resistance stainless steel is complete and clear, the situation that an energy spectrometer can be adopted to carry out precise composition detection and analysis on the sigma phase is ensured, and a significance is played in analyzing and determining the failure cause of the austenite heat-resistance stainless steel material; and the etchant is simple in composition, stable in etching effect, and high in reproducibility, can be stored and used for a long time, and is an ideal etchant for observation and energy spectrum analysis of the sigma phase through the scanning electron microscope.

Description

technical field [0001] The invention relates to the technical field of etchant, in particular to an etchant for scanning electron microscope observation and energy spectrum analysis of σ phase. Background technique [0002] The sigma phase is an iron-chromium intermetallic compound (FeCr) with a body-centered tetragonal crystal structure, which is hard and brittle. For austenitic heat-resistant stainless steel used in power plant boilers, the σ phase will precipitate after long-term operation failure, and the precipitation and growth of the σ phase will significantly reduce the plasticity and toughness of the material, leading to early failure of the material. It is important to determine the cause of material failure. [0003] At present, the etchants commonly used in the metallographic examination of the σ phase include existing chemical etchants such as ferric chloride-hydrochloric acid aqueous solution, picric acid-hydrochloric acid-alcohol solution, etc. Normal etching...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23F1/28G01N23/2202
CPCC23F1/28G01N23/2202
Inventor 江平董猛曾辉谢逍原刘盛波高淼淼陈莉君
Owner DONGFANG BOILER GROUP OF DONGFANG ELECTRIC CORP
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