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Making method of three-dimensional atom probe sample

A technology of atom probe and sample, which is applied in the field of preparation of three-dimensional atom probe samples, can solve the problems of easy breakage of samples, Pt desoldering, etc., and achieve the effects of high repeatability, improved accuracy, and simple operation

Active Publication Date: 2016-08-17
INST OF RES OF IRON & STEEL JIANGSU PROVINCE
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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing a three-dimensional atomic probe sample, which is used to solve technical problems such as easy Pt desoldering when using a focused ion beam to prepare a three-dimensional atomic probe sample, and the sample is easily broken during the test process.

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Embodiment Construction

[0020] The technical solutions of the present invention will be further described below in conjunction with preferred embodiments.

[0021] The region of interest in this embodiment comes from the vicinity of a steel sample crack;

[0022] (1) Spray the Pt protective layer 4 on the area of ​​interest, and use the focused ion beam to cooperate with the manipulator 3 to extract the area of ​​interest 5. The specific steps are as follows:

[0023] 1) The sample stage is tilted at 52 degrees, and the area of ​​interest is selected with electron beam 2, and Pt is sprayed on the area of ​​interest with ion beam 1: a Pt layer of 4 μm in length × 2 μm in width × 2 μm in thickness, and then the area of ​​interest is concaved up and down with the ion beam pit;

[0024] 2) Turn the sample stage to 0 degrees, use the ion beam to cut off the right side and bottom side of the sample, cut off the bottom left side, leave the upper left cantilever, weld Pt on the top of the manipulator and th...

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Abstract

The invention relates to a making method of a three-dimensional atom probe sample. The method comprises the following steps: 1, spraying Pt on a region-of-interest, and extracting the region-of-interest through cooperating a focused ion beam with a manipulator; 2, finishing a three-dimensional atom probe to form a required shape; 3, welding the extracted region-of-interest to the tip of the finished probe through using Pt; and 4, processing the region-of-interest by using the focused ion beam to obtain dimensions required by the three-dimensional atom probe. The three-dimensional atom probe sample of the region-of-interest can be rapidly, accurately and visually made through the method, so the disadvantage of unable positioning of the region-of-interest of traditional electrolytic polishing making methods is solved, and the problem of easy breaking of three-dimensional atom probe samples made by using the focused ion beam in the test process is also solved; and the making method in the invention, adopting the probe as a support, has the advantages of low cost and convenient operation.

Description

technical field [0001] The invention belongs to the technical field of material test sample preparation, and relates to a method for preparing a three-dimensional atom probe sample. Background technique [0002] The three-dimensional atom probe has a remarkable effect on the analysis of element segregation, dislocation distribution and disperse phase precipitation process in materials. At present, the most commonly used method for preparing three-dimensional atom probe samples is electrolytic polishing. The circular or square filaments with a diameter or side length less than 0.5 mm are electrolytically separated from the middle part through the electrolyte to form two needle-shaped samples. In order to make the tip part meet the requirements of instrument testing, the needle is usually further trimmed by micro-electropolishing technology. This method can realize the sample preparation of conventional steel test samples, and for samples with a relatively uniform distributio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
CPCG01N1/286
Inventor 金传伟张珂吴园园洪慧敏
Owner INST OF RES OF IRON & STEEL JIANGSU PROVINCE
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