Comfortable sample double spray electrolytically thinning instrument for transmission electronic microscopy

Abstract

An electrolytic thickness reducer is composed of DC power, electrolytic device of magnetic agitation and double spray and illumination device. It is featured as using 0-36 V span for DC power, placing a p-m pole in double spray component set in outer organic box with electrolyte, using stainless steel sheet as negative pole, placing positive sample in between two nozzles, having electron microscopic sample conducted with phi 0.3 mm Pt wire and stainless steel bar and having parallel light conducted out by all reflecting cable.

Description

technical field [0001] The invention belongs to the technical field of sample preparation equipment manufacturing, and in particular provides a convenient and practical double-spray electrolytic thinning instrument for transmission electron microscope samples, which is a new complete set of equipment suitable for manufacturing transmission electron microscope experiment materials. Background technique: [0002] At present, in most colleges and research institutes in my country, most of the electrolytic double-spray instruments used to make TEM samples are domestically produced, and the main one is the MTP-1 electrolytic double-spray sample preparation instrument of Shanghai Jiaotong University, such as figure 1 As shown, there are the following disadvantages: (1) Compared with foreign countries, the electrolytic polishing current range is narrower (0-15mA range), and the corresponding parameters of foreign equipment are generally an order of magnitude higher (0-400mA range). ...

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Problems solved by technology

[0002] At present, in most colleges and research institutes in my country, most of the electrolytic double-spray instruments used to make TEM samples are domestically produced, and the main one is the MTP-1 electrolytic double-spray sample preparation instrument of Shanghai Jiaotong University, such as figure 1 As shown, there are the following disadvantages: (1) Compared with foreign countries, the electrolytic polishing current range is narrower (0-15mA range), and the corresponding parameters of foreign equipment are generally an order of magnitude higher (0-400mA range). When the double-jet instrument is used to make thin film samples for transmission electron microscopy, the range of electrolytic current at room temperature is strictly limited. Domestic colleges and research institutes mainly reduce the temperature of the electrolyte (-15°C to -5°C) to achieve The purpose of reducing the electrolysis current of the electrolyte is to obtain a satisfactory metal thin film sample, but the experimental temperature control process is cumbersome, and the low temperature condition is very unfavorable to the service life of the electrolytic double jet instrument, especially the damage to the instrument caused by liquid nitrogen quenching , mixing liquid nitrogen into the electrolyte has a significant cooling effect, but changes the effective concentration of the electrolyte; (2) Due to the rapid flow of the electrolyte, it is difficult for the double-jet electrolytic polishing to appear the limiting current plateau area pointed out by the theory, and its I-V curve is almost in a straight line, such as figure 2 As shown, the shape of the polished sample is different in each area of ​​the curve: corrosion occurs in the low-voltage area; the voltage is too high and the edge of the sample is perforated, and the film quality is not good; only the thinning at B is the best, and a large flat film can be obtained. But it is not easy to explore; (3) The material of the sample itself and its physical state, the composition of the electrolyte, the relationship between temperature and voltage and current values, the size of the instrument nozzle, the distance between electrodes, the shape of the sample holder and the flow rate of the electrolyte are all important factors for sample preparation. There are different degrees of influence, and the product design is difficult to meet or take into account. According to user reports, the nozzle of the instrument mad

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