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Method for preparing magnesium alloy transmission electron microscope sample

A technology for transmission electron microscope samples and magnesium alloys, which is applied in the field of preparing metal transmission electron microscope thin film samples, to achieve high thinning rate, avoid excessive acidity, and large thin area

Active Publication Date: 2011-06-15
GUIZHOU BRANCH CHINA ALUMINUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the active nature of magnesium alloys, the samples are very easy to corrode and oxidize, and the surface is not bright during the electrolytic double-spray sample preparation. It is difficult to obtain high-quality samples, so it is difficult to obtain real and clear microscopic information of the samples. Appropriate electrolytic double jet sample preparation method is necessary

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment (1

[0015] The composition of the electrolytic double spray solution (volume measurement) is:

[0016] Methanol: 120ml (63.2%); Nitric acid: 20ml (11.6%); Glycerol: 50ml (30.3%).

[0017] For magnesium alloys, electrolytic double-spraying is used as the final thinning method, that is, the sample is sawed at a low speed, the thickness is reduced to 100um by double-sided grinding and polishing, and the double-sided polishing is free of scratches, and the surface of the sample is cleaned with acetone or alcohol. Puncher Acquisition The 3mm sample is placed on the sample holder of the electrolytic double jet instrument.

[0018] The electrolyte temperature is -25°C and the voltage is 20V for electrolytic double-jet thinning, and the sample is taken out when the optical fiber sensor alarms, that is, the sample is perforated and light-transmitting. After the sample is taken out, it is quickly and fully rinsed with alcohol to remove the residual electrolyte on the surface of the sampl...

Embodiment (2

[0020] The composition of the electrolytic double spray solution (volume measurement) is:

[0021] Methanol: 115ml (58.1%); Nitric acid: 23ml (11.6%); Glycerol: 60ml (30.3%)

[0022] For magnesium alloys, electrolytic double-spraying is used as the final thinning method, that is, the sample is sawed at a low speed, and the thickness is reduced to about 100um by double-sided grinding and polishing. Hole meter acquisition The 3mm sample is placed on the sample holder of the electrolytic double jet instrument.

[0023] The electrolyte temperature is -22°C and the voltage is 20V for electrolytic double-jet thinning, and the sample is taken out when the optical fiber sensor alarms, that is, the sample is perforated and light-transmitting. After the sample is taken out, it is quickly and fully rinsed with alcohol to remove the residual electrolyte on the surface of the sample.

Embodiment (3

[0025] The composition of the electrolytic double spray solution (volume measurement) is:

[0026] Methanol: 125ml (61.6%); Nitric acid: 18ml (8.9%); Glycerol: 60ml (29.5%)

[0027] For extruded magnesium rare earth alloys, electrolytic double spraying is used as the final thinning method, that is, the sample is sawed at a low speed, and the thickness is reduced to about 100um by double-sided grinding and polishing. Both sides are bright without scratches, and cleaned with acetone or alcohol. surface, the puncher acquires 3mm sample, put it on the sample holder of the electrolytic double jet instrument.

[0028] The electrolyte temperature is -20°C and the voltage is 18V for electrolytic double-jet thinning, and the sample is taken out when the optical fiber sensor alarms, that is, the sample is perforated and light-transmitting. After the sample is taken out, it is quickly and fully rinsed with alcohol to remove the residual electrolyte on the surface of the sample.

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Abstract

A method for preparing a magnesium alloy transmission electron microscope sample relates to a method for preparing a metal transmission electron microscope film sample. The invention is characterized in that the preparation process uses the electrolyte containing the components with volume proportions as follows: 8-12% of nitric acid, 55-65% of methanol or ethanol, and 25-35% of propanetriol, propanediol or glycol, and the sample is thinned by using an electrolyte double spraying method; electrolysis double spraying is carried out at a voltage of 15-25V and the temperature is controlled between -35 DEG C and -20 DEG C. By adding the propanetriol and electrolyzing at a low temperature, the sample surface oxidation by strong electrolyte acid can be effectively avoided. The method has the advantages of no stress in thinning process, high thinning speed, no erosion and large thinning area of the sample surface, and the like; and the method is applicable to quick and large preparation of high quality magnesium alloy film samples.

Description

technical field [0001] A method for preparing a magnesium alloy transmission electron microscope sample relates to a method for preparing a metal transmission electron microscope thin film sample. Background technique [0002] Because magnesium alloy has light specific gravity, high strength (the specific strength of magnesium alloy is higher than that of aluminum alloy and steel, slightly lower than that of fiber-reinforced plastic with the highest specific strength), good rigidity (specific stiffness is equivalent to that of aluminum alloy and steel, much higher than that of fiber Reinforced plastics), good die-casting performance, good thermal and electrical conductivity, noise reduction, electromagnetic shielding and shock absorption, and recyclable properties, are widely used in aerospace industry, military industry, transportation, 3C digital products and other fields . With the decline of application costs and the continuous expansion of application fields, countrie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/32G01N23/225
Inventor 黄霞韩冬赵春芳
Owner GUIZHOU BRANCH CHINA ALUMINUM IND
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