CN104677715B - A kind of method for being used for record in situ and observing magnesium alloy microstructures corrosion behavior - Google Patents
A kind of method for being used for record in situ and observing magnesium alloy microstructures corrosion behavior Download PDFInfo
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Abstract
The present invention relates to a kind of method for home position observation record magnesium alloy microstructures corrosion behavior, belong to material corrosion analysis field.Sample preparation first, one block of metallographic specimen is taken on magnesium alloy materials to be analyzed, it is stand-by after corase grind, fine grinding, polishing, corrosion；On metallographic microscope articles holding table, the good cover glass of a piece of translucency is placed, cover glass size covers microscope peep hole completely；The sample handled well is placed on the cover slip, adjustment camera lens obtains clearly metallographic structure；Dip corrosion salting liquid with cotton swab, gently wipe samples sightingpiston several times after, sample is placed on cover glass；The corrosion behavior of sample is observed and recorded by microscope, record in situ is carried out to crystal boundary, crystal grain, the second phase corrosion condition at interval of the equal time.Sample preparation of the present invention is simple, the cycle is short, analyze speed is fast, and the corrosion behavior of magnesium alloy microstructures is analyzed by paired observation, can accurately determine its preferential corrosion area, so as to judge the corrosion mechanism of material.
Description
Technical field
The present invention relates to a kind of method for home position observation record magnesium alloy microstructures corrosion behavior, belong to material corruption
Lose analysis technical field.
Technical background
Magnesium alloy has the advantages that high specific strength, high specific stiffness, good damping performance, easy to process, widely should
With fields such as Aero-Space, military project, automobile and electronic products.But because alloying element adds in magnesium alloy, magnesium it is strong just
Big influence electrically and to alloying element solubility is produced, magnesium has very strong chemical affinity with alloying element, promotes metal
Between compound formed.Because these intermetallic compounds have the electrode potential different from solid solution, micro cell is formed with solid solution,
So as to cause galvanic corrosion, therefore corrosion stability of magnesium alloy can be very undesirable.
In the magnesium alloy, generally 3 pairs of miniature corrosion cells be present, be respectively：Precipitated phase/α-Mg matrixes, side in crystal grain
Block phase/α-Mg, tiny precipitated phase and rare Zr addition/crystal boundary are without precipitation area.Study magnesium alloy substrate, precipitated phase, crystal boundary
Size, distribution and between interaction, disclose magnesium alloy in galvanic corrosion corrosion mechanism, for improve magnesium alloy sheet
Corrosion resistance is levied, developing new corrosion-resistant magnesium alloy has important scientific meaning.
At present, it is relatively simple for forming the means of micro cell reaction in home position observation magnesium alloy, such as stereomicroscope,
SEM observation etc..But stereomicroscope is generally limited by enlargement ratio, and utilize scanning electron microscopy
The operation of mirror home position observation is relative complex.Utilize the differentiation of metallographic microscope in-situ monitoring magnesium alloy microstructures corrosion behavior
Journey has unique advantage, such as simple to operate, image clearly.It can be used as to stereomicroscope, SEM etc.
The strong supplement of in-situ corrosion research, for macroscopical association Journal of Sex Research between microcosmic corrosion phenomenon, it may also be used for long-term rotten
Lose the timely monitoring of research.
The content of the invention
It is an object of the invention to provide it is a kind of for home position observation record magnesium alloy microstructures corrosion behavior method,
Corrosion in situ can be carried out using common cover glass and metallographic microscope to the corrosion behavior of magnesium alloy microstructures to observe
Record.
A kind of method for home position observation record magnesium alloy microstructures corrosion behavior, comprise the following steps：
(1) sample preparation：One block of metallographic specimen is taken on magnesium alloy materials to be analyzed, after corase grind, fine grinding, polishing, corrosion
It is stand-by；
(2) on metallographic microscope articles holding table, the good cover glass of a piece of translucency is placed, cover glass size covers completely
Microscope peep hole；By step（1）In the sample handled well place on the cover slip, adjustment camera lens obtains clearly metallographic group
Knit；
(3) dip corrosion salting liquid with cotton swab, gently wipe samples sightingpiston several times after, sample is placed in cover glass
On；
(4) corrosion behavior of sample is observed and recorded by microscope, at interval of the equal time to crystal boundary, crystal grain, second
Phase corrosion condition carries out record in situ.
Step（1）In, described metallographic specimen passes through 240#, 800#, 2000#, and 5000# sand paper corase grind is thrown with after fine grinding
Light；Polished sightingpiston corrodes under corresponding metallographic etchant microstructure after, dried up with hair-dryer, it is stand-by；It is described
Metallographic etchant be 4%（Volume %）Nital etc..
Step（2）In, the thickness of described cover glass is 0.17 ± 0.02mm, and otherwise the permeability of light is bad, is influenceed
Observing effect.
Step（3）In, described corrosion salting liquid is NaCl solution, Na2SO4、(NH4)2SO4Solution etc., to observe magnesium conjunction
Corrosion behavior of the gold in different medium；Concentration of salt solution is 1 × 10-5~1 × 10-3Between mol/L, excessive concentration or too low
Sample etches speed can be influenceed, causes effectively to observe and record.
The number that corrosive liquid wipe samples surface is dipped with cotton swab is 3~16 times（Number is wiped depending on alloy is intrinsic resistance to
Corrosion）, sample is put on metallographic microscope rapidly after wiping and observed.
Step（4）In, the time interval for recording the corrosion behavior of sample is 0.5s~5s, to the record time of corrosion behavior
It is equally spaced, otherwise can not be effectively contrasted between the metallographic of record in situ.
After corrosion behavior observes and records 2~5min, sample surfaces corrosion gradually extends from preferential corrosion area, causes
The generation of large area corrosion, observing and recording, it is necessary to by sightingpiston again on 5000# sand paper for corrosion behavior should not be carried out again
Polished and polished, repeat step (2)~(4).
Advantages of the present invention：
（1）Sample preparation is simple, the cycle is short, analysis is easy to be reliable, and the corrosion of magnesium alloy microstructures is analyzed by paired observation
Behavior, corrosion area is accurately determined, quickly Corrosion Behaviors of Magnesium Alloys mechanism, corrosion type are judged.It can be used as to stereoscopic micro-
The strong supplement of the in-situ corrosions such as mirror, SEM research, for macroscopical relevance between microcosmic corrosion phenomenon
Research, it may also be used for the timely monitoring of long-term corrosion research.
（2）Mirror body is avoided to pollute：Because cover glass size is much larger than lens opening size, corrosive medium will not be straight with mirror body
Connect or mediate contact.The translucency of cover glass is good simultaneously, can meet enlargement ratio for 1000 × metallographic microscope it is in situ rotten
Erosion analysis uses.
Brief description of the drawings
Fig. 1 is metallographic microscope microcosmic corrosion analysis schematic diagram in situ.
Fig. 2 is 500 times of metallographs of 1~6s of EW75 magnesium alloy in-situ corrosion Continuous Observations after solution treatment.
Fig. 3 is 1~6s of WE93 magnesium alloy in-situ corrosion Continuous Observations of As-extruded 500 times of metallographs.
Fig. 4 is 2~12s of AZ80 magnesium alloy in-situ corrosion Continuous Observations of aging state 200 times of metallographs.
Fig. 5 is 0.5~3s of EW75 magnesium alloy in-situ corrosion Continuous Observations of As-extruded 500 times of metallographs.
Fig. 6 is 1~6s of EW75 magnesium alloy in-situ corrosion Continuous Observations of aging state 200 times of metallographs.
Embodiment
For further open technical scheme, elaborated with reference to Figure of description by embodiment：
As shown in figure 1, be metallographic microscope microcosmic corrosion analysis schematic diagram in situ, wherein, 1 is sample to be seen, and 2 be lid
Slide, 3 be metallographic microscope objective table, and 4 be metallography microscope lens head.
Sample preparation first：One block of metallographic specimen is taken on the material to be analyzed, is treated after corase grind, fine grinding, polishing, corrosion
With；On metallographic microscope articles holding table, the good cover glass of a piece of translucency is placed（Thickness is 0.17mm ± 0.02mm）, size
Microscope peep hole is covered completely, the sample handled well is placed on the cover slip, and adjustment camera lens obtains clearly metallographic group
Knit；Concentration is dipped as 1 × 10 with cotton swab-5~1 × 10-3Mol/L NaCl solution（Observe corruption of the magnesium alloy in different medium
Erosion behavior, different salting liquids is chosen, such as select Na2SO4、(NH4)2SO4Solution etc.）, gently wipe samples sightingpiston 3~16 times
Afterwards, sample is placed on cover glass rapidly；The corrosion behavior of sample is observed and recorded by microscope, at interval of the x seconds（0.5s≤x
≤5s）Record in situ is carried out to crystal boundary, crystal grain, the second phase corrosion condition.Because cover glass and sightingpiston directly contact, make alloy
Gas caused by corrosion cannot discharge in time, bubble can be formed around corrosion area, bubble area is preferential corrosion area
Area；The microstructure etch state of comparative analysis alloy, analyzes its corrosion mechanism.
Embodiment 1
Microstructure corrosion behavior of the EW75 magnesium alloys in NaCl solution after home position observation record solution treatment：
(1) sample preparation：One block of metallographic specimen is taken on EW75 magnesium alloy materials, by 240#, 800#, 2000#, 5000# sand
Paper is roughly ground with after fine grinding, is polished；Polished sightingpiston is 4%（Volume %）Corrode under nital after microstructure,
Dried up with hair-dryer, it is stand-by.
(2) on metallographic microscope articles holding table, the good cover glass of a piece of translucency is placed, cover glass size covers completely
Microscope peep hole；By step（1）In the sample handled well place on the cover slip, adjustment camera lens obtains clearly metallographic group
Knit；The thickness of cover glass is 0.17 ± 0.02mm, and otherwise the permeability of light is bad, influences observing effect.
(3) 1 × 10 is dipped with cotton swab-4Mol/L NaCl corrosive liquids, gently after wipe samples sightingpiston 6 times, sample is put
In on cover glass；
(4) corrosion behavior of sample is observed and recorded by microscope, shape is corroded to crystal boundary, crystal grain, the second phase at interval of 1s
Condition carries out record in situ.
Fig. 2 is 500 times of metallographs of 1~6s of EW75 magnesium alloy in-situ corrosion Continuous Observations after solution treatment, and it is seen
The condition of examining is：Corrosive liquid 1 × 10-4Mol/L NaCl, it is 6 times that sightingpiston, which wipes number, time interval x=1s.
From figure 2 it can be seen that after EW75 magnesium alloy solution treatment, the domain of the existence for not having the second phase around crystal grain is not sent out
Raw corrosion；But in the second phase and the crystal boundary intersection of incomplete back dissolving, due to the potential difference effect between the second phase and matrix,
Galvanic corrosion occurs on matrix and the second boundary, reaction equation is:Mg+2H2O→Mg(OH)2+H2↑, produce H2Formed
Bubble, because cover glass and sightingpiston directly contact, gas caused by alloy corrosion is set to discharge in time, can be in corrosion region
Bubble is formed around domain, bubble area is the area of preferential corrosion area；With the continuous progress of corrosion, corrosion area area is not
It is disconnected to expand, form obvious contrast with the region that surrounding is not corroded.
Embodiment 2
The WE93 magnesium alloys of home position observation record As-extruded are in NaHSO3Microstructure corrosion behavior in solution, it is observed
Condition is：Corrosive liquid 1 × 10-4mol/L NaHSO3, it is 8 times, time interval x=1s that sightingpiston, which wipes number, and other steps are the same as real
Apply example 1.
Fig. 3 is 1~6s of WE93 magnesium alloy in-situ corrosion Continuous Observations of As-extruded 500 times of metallographs.Can from Fig. 3
To find out, obvious in the larger zonal corrosion of the second phase size, the size of the second phase is bigger, the matrix potential difference alternate with second
Effect is more obvious, and bigger in the trend of matrix and generation galvanic corrosion on the second boundary, alloy corrosion produces H2Form gas
Bubble, because cover glass and sightingpiston directly contact, makes gas caused by alloy corrosion to discharge in time, can be in corrosion area
Surrounding forms bubble, and bubble area is the area of preferential corrosion area.WE93 As-extruded alloy corrosion resistances are preferable, corrosion rate compared with
Low, bubble is smaller produced by corrosion.
Embodiment 3
Microstructure corrosion behavior of the AZ80 magnesium alloys of home position observation record aging state in NaCl solution, it observes bar
Part is：Corrosive liquid 1 × 10-5Mol/L NaCl, it is 3 times, time interval x=2s that sightingpiston, which wipes number, the same embodiment of other steps
1。
Fig. 4 is 2~12s of AZ80 magnesium alloy in-situ corrosion Continuous Observations of aging state 200 times of metallographs.From Fig. 4
As can be seen that the second phase of AZ80 magnesium alloys Mg of aging state17Al12It is thicker, and connection reticulates to a certain extent.Due to
Galvanic corrosion occurs for matrix and the second alternate potential difference effect, alloy.Sparse place is compared second, alloy is preferentially sent out
Raw corrosion, and as the gradual progress of corrosion, corrosion area expand to gradual around.This be primarily due to second be connected be connected into
It is netted, corrosion barrier is effectively forms, inhibition is served to corrosion.Alloy corrosion produces H2Bubble is formed, due to lid
Slide and sightingpiston directly contact, and gas caused by alloy corrosion is discharged in time, can be formed around corrosion area
Bubble, bubble gradually spread from the second mutually sparse region to close quarters.
Embodiment 4
Microstructure corrosion behavior of the EW75 magnesium alloys of home position observation record As-extruded in NaCl solution, it observes bar
Part is：Corrosive liquid 5 × 10-4Mol/L NaCl, it is 5 times, time interval x=0.5s that sightingpiston, which wipes number, and other steps are the same as implementation
Example 1.
Fig. 5 is 0.5~3s of magnesium alloy in-situ corrosion Continuous Observation of As-extruded 500 times of metallographs.Can be with from Fig. 5
Find out, the zonal corrosion on extruding streamline is obvious, the second phase dense distribution on extruding streamline, the matrix electricity alternate with second
Potential difference effect is more obvious, and bigger in the trend of matrix and generation galvanic corrosion on the second boundary, alloy corrosion produces H2Shape
Into bubble, because cover glass and sightingpiston directly contact, gas caused by alloy corrosion is discharged in time, can corrode
Bubble is formed around region, bubble area is the area of preferential corrosion area.
Embodiment 5
Microstructure corrosion behavior of the EW75 magnesium alloys of home position observation record aging state in NaCl solution, it observes bar
Part is：Corrosive liquid 1 × 10-4Mol/L NaCl, it is 4 times, time interval x=1s that sightingpiston, which wipes number, the same embodiment of other steps
1。
Fig. 6 is 1~6s of EW75 magnesium alloy in-situ corrosion Continuous Observations of aging state 200 times of metallographs.Can from Fig. 6
To find out, for the corrosion distribution of EW75 aging states than more uniform, this is due to that the second distributed mutually of the EW75 alloys of aging state is uniform, brilliant
The size of grain is basically identical, and in galvanic corrosion generating process, general corrosion occurs in alloy surface.It is gradual with corrosion
Carry out, bubble caused by total corrosion gradually expands, and will eventually join together, and the corrosion type of EW75 alloys belongs to face corruption
Erosion.
After corrosion behavior observes and records 2~5min, sample surfaces corrosion gradually extends from preferential corrosion area, causes
The generation of large area corrosion, observing and recording, it is necessary to by sightingpiston again on 5000# sand paper for corrosion behavior should not be carried out again
Polished and polished, repeat step (2)~(4).
In the present invention, because cover glass and sightingpiston directly contact, gas caused by alloy corrosion is set to release in time
Put, bubble can be formed around corrosion area, bubble area is the area of preferential corrosion area；Microcosmic group of comparative analysis alloy
Etch state is knitted, analyzes its corrosion mechanism.By above example, it can be seen that, sample preparation of the present invention is simple, the cycle is short, analysis is fast
Degree is fast, and the corrosion behavior of magnesium alloy microstructures is analyzed by paired observation, can accurately determine its preferential corrosion area, so as to
The corrosion mechanism of material is judged.
Claims (8)
1. a kind of method for home position observation record magnesium alloy microstructures corrosion behavior, comprise the following steps：
(1) sample preparation：One block of metallographic specimen is taken on magnesium alloy materials to be analyzed, it is stand-by after corase grind, fine grinding, polishing, corrosion；
(2) on metallographic microscope articles holding table, the good cover glass of a piece of translucency is placed, cover glass size covers micro- completely
Sem observation hole；The sample handled well in step (1) is placed on the cover slip, adjustment camera lens obtains clearly metallographic structure；
(3) dip corrosion salting liquid with cotton swab, gently wipe samples sightingpiston several times after, sample is placed on cover glass；
(4) cover glass and sightingpiston directly contact, and gas caused by alloy corrosion is discharged in time, can be in corrosion area
Surrounding forms bubble, and bubble area is the area of preferential corrosion area；As the continuous progress of corrosion, corrosion area area are continuous
Expand, obvious contrast is formed with the region that surrounding is not corroded；The corrosion behavior of sample is observed and recorded by microscope, often
The equal time is spaced to crystal boundary, crystal grain, the second phase corrosion condition progress record in situ.
2. the method according to claim 1 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：Described metallographic specimen passes through 240#, 800#, 2000#, and 5000# sand paper corase grind polishes with after fine grinding；Polished sight
Examine after face corrodes under metallographic etchant and microstructure, dried up with hair-dryer, it is stand-by.
3. the method according to claim 2 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：Described metallographic etchant is the nital that percentage by volume is 4%.
4. the method according to claim 1 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：The thickness of described cover glass is 0.17 ± 0.02mm.
5. the method according to claim 1 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：Described corrosion salting liquid is NaCl solution, Na2SO4Or (NH4)2SO4Solution, concentration are 1 × 10-5~1 × 10-3mol/
L。
6. the method according to claim 1 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：The number that corrosive liquid wipe samples surface is dipped with cotton swab is 3~16 times.
7. the method according to claim 1 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：The time interval for recording the corrosion behavior of sample is 0.5s~5s.
8. the method according to claim 1 for home position observation record magnesium alloy microstructures corrosion behavior, its feature
It is：After corrosion behavior observes and records 2~5min, sightingpiston is polished and polished on 5000# sand paper again,
Repeat step (2)~(4).
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| CN105784579B (en) * | 2016-04-08 | 2018-05-01 | 四川理工学院 | A kind of system and method for being used to simulate dinosaur fossil acid rain corrosion process |
| CN106289962B (en) * | 2016-10-12 | 2024-03-22 | 中国科学院金属研究所 | In-situ test system capable of observing deformation and damage of sample gauge length section in high-low power on-line manner |
| JP6503134B1 (en) * | 2018-09-07 | 2019-04-17 | 関西ペイント株式会社 | Method of measuring color of coated plate, and method of toning using the method |
| CN109540774B (en) * | 2018-11-01 | 2021-06-11 | 暨南大学 | Device and method for detecting corrosion resistance evolution of coating along with magnesium substrate deformation |
| CN109556939B (en) * | 2018-12-03 | 2021-05-11 | 中国科学院青藏高原研究所 | Method and equipment for observing fission track of sample by in-situ etching |
| CN112129686A (en) * | 2019-06-24 | 2020-12-25 | 国标（北京）检验认证有限公司 | Positioning tracking characterization method for corrosion research |
| CN111999323A (en) * | 2020-08-13 | 2020-11-27 | 中国科学院金属研究所 | In-situ EBSD observation method for microscopic orientation evolution of magnesium alloy recrystallized grains |
| CN114252391B (en) * | 2020-09-21 | 2023-11-14 | 宝山钢铁股份有限公司 | Method for evaluating industrial atmospheric corrosion resistance of steel welded joint |
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| CN101581639B (en) * | 2009-06-26 | 2011-05-25 | 西北有色金属研究院 | Method for metallographic corrosion of welding surface of titanium steel plate welded by silver based solder |
| CN102383130B (en) * | 2010-08-27 | 2014-07-02 | 比亚迪股份有限公司 | Observation method for metallographic structures of amorphous alloys |
| CN102888606B (en) * | 2012-09-28 | 2014-12-03 | 东莞市凯昶德电子科技股份有限公司 | Chemical corrosive liquid for magnesium alloy microsection and application of chemical corrosive liquid |
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