CN107541768A - A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples - Google Patents
A kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples Download PDFInfo
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Abstract
The invention discloses a kind of electrolytic polishing liquid and electrolytic polishing method for being used to prepare magnesium alloy EBSD samples, belong to technical field of magnesium alloy surface treatment.Each component content is in every liter of the electrolytic polishing liquid：90~100ml of normal propyl alcohol, 10~15ml of perchloric acid, 15~20ml of deionized water, 8~12g of oxyquinoline, 60~70g of citric acid, 40~45g of sodium sulfocyanate, surplus are absolute ethyl alcohol.The electrolytic polishing liquid of the present invention, the stressor layers and oxide layer of Mg alloy surface can effectively be removed, after electrobrightening Mg alloy surface it is smooth and it is bright cleaning, without continuous corrosion cheat, compared with existing magnesium alloy electrolytic polishing liquid, have the advantages that material source is extensive, preparation is simple, cheap, demarcation rate is high；The relatively low and magnesium alloy EBSD sample electrolysis polishing methods of effect stability the invention also discloses a kind of easily operated, cost.
Description
Technical field
The invention belongs to technical field of magnesium alloy surface treatment, and in particular to a kind of to be used to prepare magnesium alloy EBSD samples
Electrolytic polishing liquid and electrolytic polishing method.
Background technology
Magnesium alloy has low density, specific strength and specific stiffness are high, modulus of elasticity is small, dimensional stability is high, thermal conductivity is good etc.
Advantage, it is widely used to the fields such as Aero-Space, automobile, telecommunications；Simultaneously because magnesium alloy has biology in human body
Degradability, it also has huge applications prospect as medical embedded material.Due to mechanical property of cast magnesium alloys and corrosion-resistant
Property is poor, thus magnesium alloy using will be extruded as previous, a series of manufacturing procedures such as drawing or rolling, and magnesium alloy
Texture can be formed in deformation process, preferred orientation occurs in crystal grain.In recent years be used for research material heterogeneous microstructure and its
The EBSD technologies of the problems such as change in orientation in deformation process are quickly grown, compared to transmission electron microscope analysis technology, EBSD samples
Prepare relatively easily, but because EBSD only occurs in tens nanometer ranges of specimen surface pole superficial layer
It is interior, so EBSD samples require the unstressed layer in surface, non-oxidation layer, without continuous corrosion hole, bright cleaning, it could so obtain matter
The higher diffraction pattern of amount.
Prepared by sample plays conclusive effect in EBSD experiments, and the quality of sample quality directly affects the height of demarcation rate
It is low.It is electrolytic polishing liquid to influence first factor prepared by EBSD samples, and second factor is that electrolytic polishing method is especially electric
The selection of current voltage.The price of the electrolytic polishing liquid of commercial AC -2 is up to 5000 yuan/liter, and has stopped production comprehensively, and the country does not have at present
There are similar production and sale.At present, studies in China personnel are mainly thrown using the electrolytic polishing liquid and electrolysis oneself prepared
Light method prepares magnesium alloy EBSD samples, but is in the stage of fumbling more, and bath composition ratio is uncertain, electrobrightening parameter
Uncertain, electrobrightening is ineffective.
The content of the invention
It is an object of the invention to provide a kind of electrolytic polishing liquid and electrobrightening for being used to prepare magnesium alloy EBSD samples
Method, improve quality and stability prepared by magnesium alloy EBSD samples.
The purpose of the present invention is achieved through the following technical solutions：
A kind of to be used to prepare the electrolytic polishing liquids of magnesium alloy EBSD samples, each component content is in every liter of electrolytic polishing liquid：
90~100ml of normal propyl alcohol, 10~15ml of perchloric acid, 15~20ml of deionized water, 8~12g of oxyquinoline, 60~70g of citric acid,
40~45g of sodium sulfocyanate, surplus are absolute ethyl alcohol.
A kind of electrolytic polishing method for being used to prepare magnesium alloy EBSD samples, comprises the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, will
Beaker is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 20~25V, electrobrightening is then begun to, magnesium is closed
The golden polished face of sample is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and size of current is by magnesium alloy
The distance between the polished face of sample and stainless steel substrates determine that control is in 0.1~0.5A, electrobrightening during electrobrightening
Between control in 30~60s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Compared with prior art, the present invention has the advantage that and had the beneficial effect that：
The electrolytic polishing liquid of the present invention, can effectively remove the stressor layers and oxide layer of Mg alloy surface, and surface of polished is put down
Whole and bright cleaning, cheat without continuous corrosion, have the advantages that material source is extensive, preparation is simple, cheap, demarcation rate is high,
Available for the replacement electrolytic polishing liquid of commercial AC -2；Electrolytic polishing method of the invention is easily operated, cost is relatively low and effect stability,
The hardware requirement of magnesium alloy EBSD samples preparation can be effectively reduced, is easy to be widely popularized.
Brief description of the drawings
Fig. 1 is the Kikuchi band contrast figure of ZK30 extruded Magnesium Alloys in embodiment 1；
Fig. 2 is the orientation mapping figure that ZK21 extrudes aging state magnesium alloy in embodiment 5；
Fig. 3 is the orientation mapping figure of ZK60 extruded Magnesium Alloys in embodiment 6；
Fig. 4 is the pole figure of ZK20-Nd extruded Magnesium Alloys in embodiment 7：(a) 0001 crystal face pole figure；(b) 10-10 crystal faces
Pole figure；(c) 2-1-10 crystal faces pole figure.
Embodiment
The present invention is further illustrated below by embodiment, but is confined to following examples, other application field is equal
Technical scheme fall within scope of the invention, scope of patent protection of the invention should be limited by every claim.
Embodiment 1：
Electrobrightening processing is carried out with ZK30 extruded Magnesium Alloys in the present embodiment, each component contains in every liter of electrolytic polishing liquid
Measure and be：Normal propyl alcohol 100ml, perchloric acid 10ml, deionized water 15ml, oxyquinoline 8g, citric acid 70g, sodium sulfocyanate 40g, it is remaining
Measure as absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 25V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.3A, the electrobrightening time is 40s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Fig. 1 is the Kikuchi band contrast figure of ZK30 extruded Magnesium Alloys in embodiment 1, image clearly, it is preferable to characterize effect.
Embodiment 2：
Electrobrightening processing is carried out with AZ31 extruded Magnesium Alloys in the present embodiment, each component contains in every liter of electrolytic polishing liquid
Measure and be：Normal propyl alcohol 95ml, perchloric acid 12ml, deionized water 16ml, oxyquinoline 9g, citric acid 65g, sodium sulfocyanate 41g, surplus
For absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 20V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.5A, the electrobrightening time is 60s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Embodiment 3：
Electrobrightening processing is carried out with ZK30-Nd extruding aging state magnesium alloys in the present embodiment, in every liter of electrolytic polishing liquid
Each component content is：Normal propyl alcohol 100ml, perchloric acid 10ml, deionized water 15ml, oxyquinoline 8g, citric acid 70g, thiocyanic acid
Sodium 40g, surplus are absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 24V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.4A, the electrobrightening time is 35s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Embodiment 4：
Electrobrightening processing is carried out with ZK60 extruding aging state magnesium alloys in the present embodiment, each group in every liter of electrolytic polishing liquid
Point content is：Normal propyl alcohol 90ml, perchloric acid 11ml, deionized water 18ml, oxyquinoline 12g, citric acid 70g, sodium sulfocyanate
45g, surplus are absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 25V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.4A, the electrobrightening time is 30s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Embodiment 5：
Electrobrightening processing is carried out with ZK21 extruding aging state magnesium alloys in the present embodiment, each group in every liter of electrolytic polishing liquid
Point content is：Normal propyl alcohol 100ml, perchloric acid 10ml, deionized water 15ml, oxyquinoline 8g, citric acid 70g, sodium sulfocyanate
40g, surplus are absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 22V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.3A, the electrobrightening time is 45s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Fig. 2 is the orientation mapping figure that ZK21 extrudes aging state magnesium alloy in embodiment 5, the contrast between different orientation crystal grain
Substantially, and in image contain less noise, work well.
Embodiment 6：
Electrobrightening processing is carried out with ZK60 extruded Magnesium Alloys in the present embodiment, each component contains in every liter of electrolytic polishing liquid
Measure and be：Normal propyl alcohol 90ml, perchloric acid 11ml, deionized water 18ml, oxyquinoline 12g, citric acid 70g, sodium sulfocyanate 45g, it is remaining
Measure as absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 25V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.5A, the electrobrightening time is 35s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Fig. 3 is the orientation mapping figure of ZK60 extruded Magnesium Alloys in embodiment 6, and the contrast between different orientation crystal grain is bright
It is aobvious, and contain less noise in image, work well.
Embodiment 7：
Electrobrightening processing is carried out with ZK20-Nd extruded Magnesium Alloys in the present embodiment, each group in every liter of electrolytic polishing liquid
Point content is：Normal propyl alcohol 100ml, perchloric acid 10ml, deionized water 15ml, oxyquinoline 8g, citric acid 70g, sodium sulfocyanate
40g, surplus are absolute ethyl alcohol.Comprise the following steps：
(1) electrolytic polishing liquid is poured into beaker, the volume of electrolytic polishing liquid meets that sample is completely immersed in, by beaker
It is put into the tank for filling mixture of ice and water；
(2) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immerses the burning for filling electrolytic polishing liquid
Bottom of a cup portion, using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole；
(3) before electrobrightening, the voltage of constant current regulated power supply is adjusted to 20V, then begins to electrobrightening, by magnesium alloy sample
The polished face of product is immersed in electrolytic polishing liquid parallel to stainless steel substrates, and carries out mechanical agitation, and adjustment magnesium alloy sample is polished
The distance between face and stainless steel substrates, by current control in 0.2A, the electrobrightening time is 50s；
(4) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave
Cleaning, finally dried up and preserved with hair-dryer cold wind.
Fig. 4 is the pole figure of ZK20-Nd extruded Magnesium Alloys in embodiment 7, and Fig. 4 a are 0001 crystal face pole figure, and Fig. 4 b are 10-
10 crystal face pole figures, Fig. 4 c are 2-1-10 crystal face pole figures, by analyzing different crystal face pole figures, can study magnesium alloy and become
Caused texture during shape.
Claims (5)
1. a kind of electrolytic polishing liquid for being used to prepare magnesium alloy EBSD samples, it is characterised in that in every liter of the electrolytic polishing liquid
Each component content is：90~100ml of normal propyl alcohol, 10~15ml of perchloric acid, 15~20ml of deionized water, 8~12g of oxyquinoline,
60~70g of citric acid, 40~45g of sodium sulfocyanate, surplus are absolute ethyl alcohol.
2. a kind of electrolytic polishing method for being used to prepare magnesium alloy EBSD samples using electrolytic polishing liquid described in claim 1, its
It is characterised by, comprises the following steps：
(1) using stainless steel substrates as negative electrode, it is connected with the negative pole of constant current regulated power supply, and immersion fills the electricity described in claim 1
In the beaker for solving polishing fluid；
(2) using magnesium alloy sample as anode, it is connected with constant current regulated power supply positive pole, is thrown filling the electrolysis described in claim 1
Electrobrightening is carried out in the beaker of light liquid；
(3) after electrobrightening terminates, magnesium alloy sample is taken out, rinsed with absolute ethyl alcohol, is carried out followed by ultrasonic wave clear
Wash, finally dried up and preserved with hair-dryer cold wind.
3. the electrolytic polishing method according to claim 2 for being used to prepare magnesium alloy EBSD samples, it is characterised in that electrolysis
The time of polishing, polishing voltage was 20~25V in 30~60s, and polishing electric current is 0.1~0.5A.
4. the electrolytic polishing method according to claim 2 for being used to prepare magnesium alloy EBSD samples, it is characterised in that use
For mixture of ice and water as water bath with thermostatic control, electrobrightening temperature is 0 DEG C.
5. the electrolytic polishing method according to claim 2 for being used to prepare magnesium alloy EBSD samples, it is characterised in that electrolysis
Polishing is carried out under mechanical agitation.
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Cited By (5)
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| CN110455840A (en) * | 2019-07-23 | 2019-11-15 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD |
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| CN110618149A (en) * | 2019-10-17 | 2019-12-27 | 江苏理工学院 | Preparation method of magnesium alloy EBSD sample |
| CN112748138A (en) * | 2020-11-26 | 2021-05-04 | 西北工业大学 | Method for preparing pure titanium EBSD sample with high oxygen content |
| CN115112697A (en) * | 2022-05-11 | 2022-09-27 | 重庆大学 | Magnesium alloy microstrain characterization method |
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