CN102383176A - Preparation method of magnesium-alloy electron backscatter diffraction sample (EBSD) and special electrolyte thereof - Google Patents

Preparation method of magnesium-alloy electron backscatter diffraction sample (EBSD) and special electrolyte thereof Download PDF

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Publication number
CN102383176A
CN102383176A CN2010102714474A CN201010271447A CN102383176A CN 102383176 A CN102383176 A CN 102383176A CN 2010102714474 A CN2010102714474 A CN 2010102714474A CN 201010271447 A CN201010271447 A CN 201010271447A CN 102383176 A CN102383176 A CN 102383176A
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sample
electrolysis
magnesium alloy
ebsd
electrolyte
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CN2010102714474A
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张士宏
宋广胜
严操
王忠堂
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Priority to CN2010102714474A priority Critical patent/CN102383176A/en
Publication of CN102383176A publication Critical patent/CN102383176A/en
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Abstract

The invention relates to a preparation method of a magnesium-alloy electron backscatter diffraction sample (EBSD) and special electrolyte thereof, which belongs to the field of magnesium-alloy electrolysis process and is mainly applied in preparing high-quality EBSD samples. The method comprises the following steps of: (1) preparation of the electrolyte: putting perchloric acid and alcohol into a beaker according to the volume ratio of 1:9, and stirring till the minimum volume of the electrolyte can meet the condition that an electrolytic sample can be wholly immersed; (2) sample coating: covering the parts of the sample without need of electrolysis by using coating liquid, and avoiding from covering the connecting part of the sample and an anode; (3) electrolysis: pouring liquid nitrogen into the beaker containing the electrolyte, and when the temperature of the electrolyte is between -20 DEG C and -50 DEG C, carrying out electrolysis; and (4) sample cleaning. By adoption of the invention, the problems such as high cost and the like in the prior art can be solved, the electrolyte can replace the commercial electrolyte of magnesium alloy with expensive price, the qualified magnesium-alloy EBSD sample is prepared, the cost is low and the implementation is easy.

Description

A kind of magnesium alloy electronic back scattering diffraction preparation method of sample and special electrolysis liquid thereof
Technical field
The present invention relates to a kind of magnesium alloy electronic back scattering diffraction (EBSD) preparation method of sample and special electrolysis liquid thereof, belong to the electrolysis process field of magnesiumalloy, be mainly used in the high-quality EBSD sample of preparation.
Background technology
Along with science and technology development, EBSD (EBSD) technology that is used to measure crystallographic features and the distribution thereof at material crystals orientation, research microcosmic texture, interface has obtained developing rapidly and is perfect.Its principal feature is the diffraction (providing the data of crystallography) that when keeping the conventional characteristics of sem, carries out the spatial resolution submicron order.Crystalline orientation according to collecting in the sample is classified, and is oriented to reference with a certain, and other orientation compares with it respectively, and the zone that will have an a certain same orientation difference reconstructs multicrystal orientation maps with color or gray scale at random.Because EBSD (EBSD) only occurs in the extremely shallow top layer of specimen surface (depth rangees of tens nanometers), so the preparation of EBSD sample is higher than the requirement of general metallographic specimen.The EBSD sample requires the unstressed layer in surface, no successive corrosion pit, and the non-oxidation layer, fluctuating can not excessive and bright cleaning.
Preparing qualified EBSD sample is the work that the AZ31 magnesiumalloy carries out EBSD experiment most critical, and the sample quality quality is that can experimentation accomplish the most critical factor, and wherein, the link of decision sample quality most critical is the electrolytic process of sample.
At present, the EBSD sample demarcation rate of the traditional electrolytic solution of domestic employing preparation is too low, though and adopt the EBSD sample demarcation rate of AC-2 electrolytic solution preparation of import very high, cost is too high.
Summary of the invention
The object of the invention is to provide a kind of magnesium alloy electronic back scattering diffraction preparation method of sample and special electrolysis liquid thereof; Solve the problems such as cost height that exist in the prior art; This electrolytic solution substitutes the commercial electrolytic solution of expensive magnesiumalloy; Prepare qualified magnesiumalloy EBSD sample, it is with low cost and be easy to realize.
Technical scheme of the present invention:
A kind of magnesium alloy electronic back scattering diffraction preparation method of sample comprises the steps:
(1) electrolyte quota
Perchloric acid and alcohol are put into beaker by 1: 9 volume ratio and stirred, and the electrolytic solution minimum volume can satisfy the electrolysis sample and can all immerse and get final product;
(2) sample applies
Do not need electrolytic position to cover with coating liquid on sample, the position that sample is connected with anode will cover scarcely;
The effect of coating liquid is to prevent the magnesium alloy sample electrolysis, and coating liquid can be selected nail varnish, pyroxylin (e) cement, silica gel or double faced adhesive tape etc. for use.
(3) electrolysis
Liquid nitrogen is poured in the beaker that fills electrolytic solution, is-20 ℃ to-50 ℃ up to the temperature of electrolytic solution, and magnesium alloy sample is suspended to anode; Stainless steel plate is suspended to negative electrode; After direct supply voltage transferred to 15V~20V, again sample is immersed electrolytic solution and carry out electrolysis, and pick up counting; Will guarantee current value during electrolysis in 0.1A~0.5A scope, electrolysis time was controlled at 120~200 seconds;
Among the present invention, adopt liquid nitrogen electrolyte temperature to be reduced to below-20 ℃, its effect is the perchloric acid generation chemical reaction that prevents in sample and the electrolytic solution, influences amount of electrolyte.
(4) sample cleans
When electrolysis finishes; The electrolytic sample of institute is taken out in electrolytic solution; And successively sample is put into 3 beakers that fill acetone and clean; Scavenging period in each beaker is 30 seconds~2 minutes, and carrying out ultrasonic cleaning then is 1~3 minute, sample is taken out again and dries up with blower cold wind.
When adopting technology of the present invention to carry out electrolysis, the raw material perchloric acid and the alcohol purity of preparing electrolyte are high more, and electrolysis effectiveness is good more, if adopt not high perchloric acid and the alcohol of purity can't reach required electrolysis effectiveness, and then can't carry out the EBSD experiment.Among the present invention, the purity of perchloric acid is 70.0~72.0%wt, and the purity of alcohol is >=99.7%wt.
In addition, carry out smoothly in order to guarantee the EBSD experiment after the electrolysis, mechanical polishing to certain smooth finish need be carried out in the electrolysis position of sample before electrolysis, and the smooth finish scope is >=11 grades.Current value and electrolysis time may have certain variation because of the size of sample.
Among the present invention, the material of magnesium alloy sample can be magnesium-aluminum-zinc-manganese series deformation magnesium alloys such as AZ31, AZ61 or AZ80.
Advantage of the present invention and beneficial effect are:
1, magnesium alloy electronic back scattering diffraction of the present invention (EBSD) preparation method of sample is compared with traditional method for making sample, when carrying out the EBSD analysis; Kikuchi band sharpness is high; Orientation demarcation rate can arrive more than 95%, and adopts traditional method for making sample, and its orientation demarcation rate is 85%.
2, EBSD preparation method of sample of the present invention has practicality and the low advantage of expense, and cost can reduce by 100 times.
Description of drawings
Fig. 1 makes AZ31 magnesium alloy sample EBSD experimental result for the present invention, and the Kikuchi band is high-visible.
Fig. 2 makes the grain orientation figure result that AZ31 magnesium alloy sample EBSD tests for the inventive method, and orientation demarcation rate reaches 95%.
Fig. 3 makes AZ61 magnesium alloy sample EBSD experimental result for the present invention, and the Kikuchi band is high-visible.
Fig. 4 makes AZ80 magnesium alloy sample EBSD experimental result for the present invention, and the Kikuchi band is high-visible.
Embodiment
Embodiment 1
Magnesium alloy electronic back scattering diffraction preparation method of sample of the present invention comprises the steps:
(1) electrolyte quota is put into perchloric acid and alcohol beaker by 1: 9 volume ratio and is stirred, and the electrolytic solution minimum volume can satisfy the electrolysis sample and can all immerse and get final product;
In the present embodiment, the purity of perchloric acid is 70.0~72.0%wt, and the purity of alcohol is >=99.7%wt.
(2) sample applies, and does not need electrolytic position with nail varnish (conventional nail enamel all can, acting effective constituent is toluene, butylacetate, formaldehyde resin and ETHYLE ACETATE etc.) covering on sample, and the position that sample is connected with anode will cover scarcely;
(3) electrolysis is poured liquid nitrogen in the beaker that fills electrolytic solution into, up to the temperature of electrolytic solution to being lower than-20 ℃; The AZ31 magnesium alloy sample is suspended to anode, and stainless steel plate is suspended to negative electrode, direct supply voltage is transferred to 15V~20V after; Again sample is immersed electrolytic solution and carry out electrolysis; And pick up counting, to guarantee current value during electrolysis in 0.1A~0.5A scope, electrolysis time is controlled between 120~200s;
(4) sample cleans; When electrolysis finishes; Rapidly the electrolytic sample of institute is taken out in electrolytic solution, and successively sample is put into 3 beakers that fill acetone and clean, the scavenging period in each beaker is about 1 minute; And carried out ultrasonic cleaning about two minutes, then sample is taken out and dry up with blower cold wind.
In addition, carry out smoothly in order to guarantee the EBSD experiment after the electrolysis, mechanical polishing to certain smooth finish need be carried out in the electrolysis position of sample before electrolysis, and smooth finish is >=11 grades.
Adopt method of the present invention, prepared AZ31 magnesium alloy electronic back scattering diffraction (EBSD) sample.Fig. 1 makes AZ31 magnesium alloy sample EBSD experimental result for the inventive method, and the Kikuchi band is high-visible.Fig. 2 makes the grain orientation figure result that AZ31 magnesium alloy sample EBSD tests for the inventive method, and orientation demarcation rate reaches 95%.
Embodiment 2
Adopt with embodiment 1 in identical step and technical requirements, prepared AZ61 magnesium alloy electronic back scattering diffraction (EBSD) sample, Fig. 3 is the EBSD sample Kikuchi band figure of prepared AZ61, the Kikuchi band among the figure is high-visible, reaches the EBSD experimental requirements.
Embodiment 3
Adopt with embodiment 1 in identical step and technical requirements, prepared AZ80 magnesium alloy electronic back scattering diffraction (EBSD) sample, Fig. 4 is the EBSD sample Kikuchi band figure of prepared AZ80, the Kikuchi band among the figure is more clear, reaches the EBSD experimental requirements.

Claims (6)

1. the special electrolysis liquid of a magnesium alloy electronic back scattering diffraction specimen preparation is characterized in that, by volume, and perchloric acid: alcohol=1: 9.
2. a magnesium alloy electronic back scattering diffraction preparation method of sample is characterized in that, comprises the steps:
(1) electrolyte quota
Perchloric acid and alcohol are put into beaker by 1: 9 volume ratio and stirred, and the electrolytic solution minimum volume can satisfy the electrolysis sample and can all immerse and get final product;
(2) sample applies
Do not need electrolytic position to cover with coating liquid on sample, the position that sample is connected with anode is avoided covering;
(3) electrolysis
Liquid nitrogen is poured in the beaker that fills electrolytic solution, is-20 ℃ to-50 ℃ up to the temperature of electrolytic solution, and magnesium alloy sample is suspended to anode; Stainless steel plate is suspended to negative electrode; After direct supply voltage transferred to 15V~20V, again sample is immersed electrolytic solution and carry out electrolysis, and pick up counting; Will guarantee current value during electrolysis in 0.1A~0.5A scope, electrolysis time was controlled at 120~200 seconds;
(4) sample cleans
When electrolysis finishes, the electrolytic sample of institute is taken out in electrolytic solution, use acetone, obtain magnesium alloy electronic back scattering diffraction sample.
3. according to the described magnesium alloy electronic back scattering diffraction of claim 2 preparation method of sample, it is characterized in that in the said step (1), the purity of perchloric acid is 70.0~72.0%wt, the purity of alcohol is >=99.7%wt.
4. according to the described magnesium alloy electronic back scattering diffraction of claim 2 preparation method of sample, it is characterized in that in the said step (2), coating liquid is selected nail varnish, pyroxylin (e) cement, silica gel or double faced adhesive tape for use.
5. according to the described magnesium alloy electronic back scattering diffraction of claim 2 preparation method of sample, it is characterized in that in the said step (3), the material of magnesium alloy sample is AZ31, AZ61 or AZ80.
6. according to the described magnesium alloy electronic back scattering diffraction of claim 2 preparation method of sample; It is characterized in that, in the said step (4), when using acetone; Successively sample being put into 3 beakers that fill acetone cleans; Scavenging period in each beaker is 30 seconds~2 minutes, and carrying out ultrasonic cleaning then is 1~3 minute, sample is taken out again and dries up with blower cold wind.
CN2010102714474A 2010-09-03 2010-09-03 Preparation method of magnesium-alloy electron backscatter diffraction sample (EBSD) and special electrolyte thereof Pending CN102383176A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102827383A (en) * 2012-09-04 2012-12-19 浙江大学 Modification method for regioselectivity nanostructure on surfaces of polydimethylsiloxane
CN103868780A (en) * 2014-04-04 2014-06-18 重庆大学 Preparation method of colored metallographic specimens of aluminum alloys of Al-Mg and Al-Mg-Si series
CN106868578A (en) * 2017-01-25 2017-06-20 西北稀有金属材料研究院 A kind of beryllium material electrobrightening and the integral method of corrosion for EBSD tests
CN107541768A (en) * 2017-08-30 2018-01-05 北京科技大学 A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples
CN109900727A (en) * 2019-03-18 2019-06-18 中国科学院金属研究所 A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods
CN110618149A (en) * 2019-10-17 2019-12-27 江苏理工学院 Preparation method of magnesium alloy EBSD sample
CN111735836A (en) * 2020-06-29 2020-10-02 中国科学院金属研究所 Preparation method of ultra-pure high-chromium ferrite stainless steel EBSD sample

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN101591799A (en) * 2008-05-30 2009-12-02 比亚迪股份有限公司 A kind of electrolytic polishing liquid of magnesium alloy and surface finish treatment process thereof

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CN101591799A (en) * 2008-05-30 2009-12-02 比亚迪股份有限公司 A kind of electrolytic polishing liquid of magnesium alloy and surface finish treatment process thereof

Non-Patent Citations (1)

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Title
曾柯等: "EBSD技术在稀土变形镁合金微观表征中的应用", 《电子显微学报》, vol. 29, no. 1, 28 February 2010 (2010-02-28), pages 720 - 723 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102827383A (en) * 2012-09-04 2012-12-19 浙江大学 Modification method for regioselectivity nanostructure on surfaces of polydimethylsiloxane
CN103868780A (en) * 2014-04-04 2014-06-18 重庆大学 Preparation method of colored metallographic specimens of aluminum alloys of Al-Mg and Al-Mg-Si series
CN106868578A (en) * 2017-01-25 2017-06-20 西北稀有金属材料研究院 A kind of beryllium material electrobrightening and the integral method of corrosion for EBSD tests
CN106868578B (en) * 2017-01-25 2019-09-03 西北稀有金属材料研究院宁夏有限公司 A kind of integral method of the beryllium material electrobrightening tested for EBSD and corrosion
CN107541768A (en) * 2017-08-30 2018-01-05 北京科技大学 A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples
CN107541768B (en) * 2017-08-30 2020-01-10 北京科技大学 Electrolytic polishing solution and electrolytic polishing method for preparing magnesium alloy EBSD sample
CN109900727A (en) * 2019-03-18 2019-06-18 中国科学院金属研究所 A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods
WO2020186892A1 (en) * 2019-03-18 2020-09-24 中国科学院金属研究所 Method for preparing ultra-low-temperature weak current control metal material ebsd sample
CN110618149A (en) * 2019-10-17 2019-12-27 江苏理工学院 Preparation method of magnesium alloy EBSD sample
CN111735836A (en) * 2020-06-29 2020-10-02 中国科学院金属研究所 Preparation method of ultra-pure high-chromium ferrite stainless steel EBSD sample

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