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A kind of preparation method of transmission electron microscope metal sample

A technology for metal samples and transmission electron microscopy, which is applied in the preparation of test samples, etc., can solve the problems of long preparation period and high cost of transmission electron microscopy samples, and achieve the effects of shortening the sample preparation period, high success rate and low pollution

Inactive Publication Date: 2017-02-15
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing a transmission electron microscope sample with a simple preparation process, low cost and high success rate in view of the problems of long preparation period and high cost of the existing transmission electron microscope sample

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: prepare the sample of lens electron microscope metal Fe, its preparation process is as follows:

[0025] Step 1. Wire-cut metal Fe into 0.3mm thick Fe flakes. Grind the Fe flakes to a thickness of 80 μm with an automatic metallographic sample grinder. During the grinding process, use water cooling to cool down the Fe flakes during the entire grinding process. The temperature is lower than 100°C to ensure that the structure of the Fe sample does not change; the above-mentioned pre-ground Fe sheet is cut into a disc with a diameter of 3mm by a punch;

[0026] Step 2. Use a nanosecond laser with an energy of 300mJ and a frequency of 1Hz. The laser wavelength is 532nm. Focus through a lens so that the laser beam forms an angle of 30 degrees with the surface of the Fe sheet as the target, and the laser radiation acts for 2 minutes, thereby Make oblique holes on the Fe sheet;

[0027] Step 3. Pickling-cleaning the Fe sheet with oblique holes:

[0028] Prepare ...

Embodiment 2

[0031] Embodiment 2: prepare the sample of lens electron microscope metal Mg, its preparation process is as follows:

[0032] Step 1. Cut the metal Mg wire into 0.3mm thick Mg sheets, manually grind the Mg sheets to 60 μm, and cut the pre-ground Mg sheets into discs with a diameter of 3mm;

[0033] Step 2. Use a picosecond laser. The energy of the laser is 100μJ, the frequency is 1KHz, and the laser wavelength is 800nm. Focus through the lens so that the laser beam and the surface of the Mg sheet form an angle of 50 degrees. The laser radiation acts on 1-3 femtosecond pulses at Oblique holes are opened on the Mg sheet;

[0034] Step 3: slowly pour 2mL of perchloric acid into 50mL of absolute ethanol and stir to prepare an acidic solution for pickling, absorb the acidic solution with a needle, pickle the laser hole on the Mg sheet, and use it immediately after pickling Clean the place with ion water, repeat the pickling-cleaning process three times, so far the metal Mg sample ...

Embodiment 3

[0035] Embodiment 3: prepare the sample of lens electron microscope metal Ti, its preparation process is as follows:

[0036] Step 1. Cut the metal Ti wire into 0.3mm thick Ti slices, thin the Ti slices to 60 μm by manual grinding, and cut the pre-grinded Ti slices into discs with a diameter of 3mm with a punch;

[0037] Step 2. Use a nanosecond laser. The energy of the laser is 450mJ, the frequency is 2Hz, and the laser wavelength is 266nm. Focus through the lens so that the laser beam forms an angle of 60 degrees with the target Ti sheet, and the laser radiation acts on the Ti sheet for 1 minute. oblique hole;

[0038] Step 3: Mix 6mL of hydrofluoric acid and 25mL of absolute ethanol to prepare an acidic solution, absorb the acidic solution with a needle, pickle the laser opening on the Ti sheet, and then clean the place with acetone to prepare a lens electron microscope A sample of metal Ti is used; the obtained sample is stored in absolute ethanol for observation by trans...

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Abstract

The invention discloses a preparation method of a transmission electron microscope metal sample. The method comprises the steps of machining, punching an inclined hole by laser and acid-washing and cleaning an area around the inclined hole; the method is mainly suitable for conventional metals such as Fe, Mg and Ti. Particularly, the method comprises the steps of processing a metal sheet in a manner of cutting, grinding and the like through a machining method to enable the thickness of the metal sample to preliminarily reach 50-100 microns; after that, punching the inclined hole in the metal sheet at the inclination angle of 30-60 degrees by short or ultra-short pulse laser with the wavelength being less than 1064nm; and aiming at different metals, carrying out acid washing or alkaline washing on the area of the hole, punched by the laser, of the metal sheet with a proper acid or alkaline solution, immediately cleaning with a conventional organic solvent, and repeating the process of acid washing and cleaning or alkaline washing and cleaning for 1-3 times. Compared with a method for preparing a transmission electron microscope sample by ion thinning, the method has the advantages that the period is shortened, the after-treatment of the sample is simpler, and the cost is lowered.

Description

technical field [0001] The invention belongs to the technical field of electron microscope sample preparation, in particular to a method for preparing a transmission electron microscope metal sample. Background technique [0002] The transmission electron microscope is one of the important instruments for studying the microstructure of materials, but the premise of being able to observe on the transmission electron microscope is that the electron beam of the transmission electron microscope can penetrate the sample, and the quality of the image observed by the transmission electron microscope is strongly dependent on the thickness of the sample. Therefore the part of the sample to be observed must be very thin. The ability of an electron beam to penetrate a solid sample depends primarily on the accelerating voltage and the atomic number of the sample composition. Generally speaking, the higher the accelerating voltage, the smaller the atomic number of the sample, and the gr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N1/32
Inventor 魏强李薇许伟泽刘浩锐
Owner TIANJIN UNIV
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