A preparation method of iron and steel samples for transmission electron microscope observation
An electron microscope and sample technology, applied in the preparation of test samples, etc., can solve the problems of contaminated samples, slow speed, electrolyte residue, etc.
Active Publication Date: 2016-01-27
SHANXI TAIGANG STAINLESS STEEL CO LTD
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Problems solved by technology
[0005] The above two final thinning methods have their own advantages and disadvantages. The electrolytic double spraying speed is fast (1-5 minutes), but it is only suitable for conductive samples, and it is easy to have electrolyte residue, which will pollute the sample; ion thinning can be applied to any sample , but it needs to be pitted in advance, the speed is slow, and the efficiency is low. It takes about 8 hours or even longer to prepare a steel sample.
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Embodiment
[0033] This embodiment is the following sequential steps:
[0034] (1) Mechanical thinning
[0035] Cut the sample line to 0.5mm, both sides of the sample are ground and polished to the level of the metallographic polishing surface, each side has to go through four processes, the process is: rough grinding, fine grinding, rough polishing and fine polishing, and finally double-sided Grinding and polishing to 50-80μm and all have a mirror level. Use a manual punching machine to punch out Ф3mm discs for final thinning.
[0036] (2) Electrolytic double spray
[0037] The material of this embodiment is a 316LN steel sample, and the Tenupol-5 type electrolytic double spraying instrument produced by Struers Company is used to carry out electrolytic double spraying. The process parameters are: polishing liquid, 6% perchloric acid alcohol solution; voltage, 21V; stop light receiving The light intensity received by the device is 33; the pump speed is 19 (the gear of the liquid pump);...
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The present invention relates to a kind of preparation method of iron and steel sample for transmission electron microscope observation, and it comprises following steps in sequence: Ⅰ Mechanical thinning, mechanically thinned steel samples to 50-80 μm, punched out Ф3mm discs by manual punching machine; Ⅱ Electrolytic double spray, the technical parameters are voltage: 21±0.5V; polishing liquid: 6±1% perchloric acid alcohol solution; temperature: -15°C to -30°C; pump speed: 13~29°C; When the received light intensity reaches 32-80, it will stop automatically; Ⅲ Ion thinning, cleaning in the ion thinning instrument, the parameters are: the angle between the ion gun and the sample surface: 4~5°, in which, the left gun and the right gun are respectively incident from the upper surface and the lower surface of the sample; voltage: 4~ 5kv; time: 20±6 minutes. The steel sample preparation method for transmission electron microscope observation processes the steel sample, which has high speed, high efficiency and reliable quality.
Description
technical field [0001] The invention relates to a method for preparing a steel sample for transmission electron microscope observation. Background technique [0002] Transmission electron microscope sample requirements are: Ф3mm disc or a rectangle with a diagonal of no more than 3mm and a long side of 2.5mm, generally perforated in the middle, and the area with a thickness of the hole edge within 100nm must meet the observation needs, double-sided polishing, and the sample preparation process cannot bring about stress effects. The thickness of the sample received by the transmission electron microscope sample preparation room is generally 0.5mm, which needs to be mechanically thinned and finally thinned in the sample preparation room. During mechanical thinning, the two surfaces of the sample generally have to go through four or five processes, namely: coarse grinding, fine grinding, rough polishing and fine polishing. If necessary, an intermediate process can be added bet...
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IPC IPC(8): G01N1/28
Inventor 裴海祥赵振铎范光伟
Owner SHANXI TAIGANG STAINLESS STEEL CO LTD