A kind of preparation method of nanoscale carbide transmission electron microscope extraction replica sample

A technique of transmission electron microscopy and extraction replica, which is applied in the preparation of test samples, scanning probe technology, instruments, etc. Improved success rate and good carbon film morphology

Active Publication Date: 2018-02-23
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing a replica sample extracted by transmission electron microscopy of nano-scale carbides, so as to solve the problems that it is difficult to extract small-sized nano-scale carbides and the success rate is low by traditional methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) The surface of the sample is repeatedly mechanically ground and polished until the surface is smooth and scratch-free.

[0028] (2) Immerse the sample in a methanol solution containing picric acid with a mass fraction of 0.5% and bromic acid with a volume fraction of 1%. After corroding for 6 minutes, soak it in absolute ethanol to clean the corrosion solution on the surface of the sample. , then remove to dry.

[0029] (3) Spray carbon film on the surface: spray a layer of carbon film on the surface of the sample by using a vacuum coating device.

[0030] (4) Electrolytic stripping: Use a blade to divide the carbon film on the surface of the sample into small squares of 3mm×3mm; take the sample as the anode and the stainless steel sheet as the cathode, and the surface of the sample is inclined to form an angle of 15° with the vertical direction; Electrolyze in an absolute ethanol solution containing 4% nitric acid by volume and 0.5% bromic acid by volume fraction,...

Embodiment 2

[0033] (1) The surface of the sample is repeatedly mechanically ground and polished until the surface is smooth and scratch-free.

[0034] (2) Immerse the sample in methanol solution containing picric acid with mass fraction of 0.2% and bromic acid with volume fraction of 1.5%. Remove to dry.

[0035] (3) Spray carbon film on the surface: spray a layer of carbon film on the surface of the sample by using a vacuum coating device.

[0036] (4) Electrolytic stripping: Use a blade to divide the carbon film on the surface of the sample into small squares of 3mm×3mm; take the sample as the anode and the stainless steel sheet as the cathode, and the surface of the sample is inclined to form an angle of 30° with the vertical direction; Electrolyze in absolute ethanol solution containing 5% nitric acid by volume fraction and 1% bromic acid by volume fraction, the electrolysis current is controlled at 0.3mA, and the electrolysis time is 3min.

[0037] (5) Film removal: After the carbo...

Embodiment 3

[0039] (1) The surface of the sample is repeatedly mechanically ground and polished until the surface is smooth and scratch-free.

[0040] (2) Immerse the sample in a methanol solution containing picric acid with a mass fraction of 0.8% and bromic acid with a volume fraction of 2%. After corroding for 4 minutes, put it into absolute ethanol and soak it to clean the corrosion solution on the surface of the sample, and then Remove to dry.

[0041] (3) Spray carbon film on the surface: spray a layer of carbon film on the surface of the sample by using a vacuum coating device.

[0042] (4) Electrolytic stripping: Use a blade to divide the carbon film on the surface of the sample into small squares of 3mm×3mm; take the sample as the anode and the stainless steel sheet as the cathode, and the surface of the sample is inclined to form an angle of 40° with the vertical direction; Electrolyze in an absolute ethanol solution containing 6% nitric acid by volume and 0.8% bromic acid by v...

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Abstract

The invention discloses a method for preparing a replica sample extracted by a nanoscale carbide transmission electron microscope. The steps are: mechanically grinding and polishing the sample until the surface is smooth and free of scratches; into alcohol for cleaning, and then take it out for drying; wherein, the corrosion solution is a mixed solution of picric acid, bromic acid and methanol; use a vacuum coating instrument to spray a layer of carbon film on the surface of the sample; the carbon film on the surface of the sample Divided into a grid shape, electrolyzed in the electrolyte, the surface of the sample is inclined, so that the carbon film is separated from the surface of the sample; wherein, the electrolyte is a mixed solution of nitric acid, bromic acid, and absolute ethanol; The membrane was removed from the electrolyte, rinsed in alcohol, and dried on filter paper or air-dried. The carbon extraction replica sample produced by the invention has good carbon film shape and high sample preparation success rate, and is suitable for observing very small nanoscale carbides with a transmission electron microscope.

Description

technical field [0001] The invention belongs to the field of material sample preparation, and in particular relates to a method for preparing a replica sample extracted by a nanoscale carbide transmission electron microscope. Background technique [0002] For iron and steel materials, the fine-sized carbides precipitated in steel have a strong strengthening effect and can significantly increase the strength of iron and steel materials. Studying the precipitation behavior of carbides is of great significance for the development of high-strength steel materials. [0003] Transmission electron microscopic analysis is a commonly used and effective method to study the precipitation behavior of carbides in steel. Steel samples usually used for transmission electron microscope analysis are metal flakes. The preparation method is: grind the sample into a disc sample with a thickness of 50 μm and a diameter of 3 mm, and then perforate the center of the sample by double-jet electroly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/32G01Q30/20
Inventor 周雪峰江红兵方峰蒋建清黄慧玲
Owner SOUTHEAST UNIV
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