An electrolytic stripping device and method for carbon extraction replication of steel mounted samples

Abstract

The invention relates to an electrolytic membrane removal device and method for a steel mounting carbon extraction replica. The device comprises an electrolytic bath, a stainless steel cathode, a diaphragm, an anode module, a bracket, a height adjustment line, a conductor wire and a power supply. The electrolytic membrane removal method comprises the following technological steps: I. preparation of a special mounting; II. preparation of a carbon replica, namely grinding and polishing as well as conducting deep corrosion on a mounted sample and then spraying carbon; and III. electrolytic membrane removal, namely fixing the sample with a sprayed carbon membrane on the anode module, electrolyzing until the carbon membrane falls and freely falls into the diaphragm below, taking out and immersing the diaphragm into distilled water so as to spread the carbon membrane, and fishing out the membrane. According to the method, the mounting of the corrosion-resistant sheet or irregular sample can be subjected to fast membrane removal after carbon extraction replica is conducted, so that the defects that the samples are difficultly subjected to electrolytic membrane removal, and long in chemical membrane removal time to cause breakage of the carbon membrane or gathering of corrosive product residues, and the like can be successfully overcome. In addition, the device is practical and safe, convenient to assemble and disassemble, easy to operate and use, and applicable to conventional conductive samples and non-conductive samples.

Description

technical field [0001] The invention relates to an electrolytic stripping device and method for carbon extraction replicas of iron and steel mounted samples. The invention belongs to the technical field of iron and steel material precipitate analysis. Background technique [0002] With the in-depth study of precipitates in iron and steel materials, carbon extraction replica technology has become an important means to study the morphology, structure and distribution of precipitates in iron and steel materials. The method of removing the carbon membrane has a crucial impact on the success of the carbon extraction replica. Conventional stripping methods are divided into chemical corrosion method and electrolytic stripping method. Chemical corrosion method is widely used in the stripping of conventional corrosive materials, and the stripping can be done within 1-30 minutes. Electrolytic stripping is mainly used for corrosion-resistant samples, and the samples need to be conduc...

AI Technical Summary

Problems solved by technology

For thin sheet corrosion-resistant samples or samples with irregular shapes, the sample is usually not conductive due to the need for sample preparation after mounting, so the sample can only be removed by chemical corrosion. This process usually takes several hours or even tens of hours, and The carbon film produced by chemical corrosion is not only fragile, but also contains many corrosion products, which have a great impact on the later detection results; although electrolytic stripping can be used to inlay samples with conductive inserts, there are major problems in actual use

First, the conductive insert with excellent electrical conductivity is expensive, which is 6-8 times the price of conventional non-conductive inserts; second, the carbon film on the surface of the conductive insert may fall off when the film is peeled off, which will interfere with the choice of carbon film

At the same time, the currently commonly used film removal device needs to artificially predict the time when the carbon film will fall off. It is necessary to quickly take out the sample and move it to distilled water to make the carbon film fall off when the carbon film is about to fall off, which requires a high level of experience for the operator. And the control of the time node is difficult to grasp

Compared with the existing documents, patents and other technical materials, the present invention has the following improvements: the article "Cr-Mo Steel Carbon Film Extraction Best Specification", "30CrMnSiA Steel Deformation and Aging Microscopic Observation", "Ti-Nb Microalloy Steel Welding Coarse Grain Heat-Affected Zone Microstructure and Toughness" and patents "A Manufacturing Method of Transmission Electron Microscope Carbon Extraction Replica Sample (Application No.: CN201110008660.0)", "REPLICA FILMGENERATION METHOD OF VANADIUM ALLOY MATERIAL (Application No.: JP201272325A)" and "PREPARATION OF EXTRACTED REPLICA FILM OFALUMINUM ALLOY (application number: JP199324502A)" all mentioned the method of electrolytic film removal, but the method in the article is only suitable for large conductive samples, and it needs to be thin or irregular. Inlaid samples are not applicable, and the release time needs to be predicted, which requires high requirements for operators

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