CN104677715A - Method for recording and observing corrosion behavior of magnesium alloy microstructure in situ - Google Patents
Method for recording and observing corrosion behavior of magnesium alloy microstructure in situ Download PDFInfo
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- CN104677715A CN104677715A CN201310641922.6A CN201310641922A CN104677715A CN 104677715 A CN104677715 A CN 104677715A CN 201310641922 A CN201310641922 A CN 201310641922A CN 104677715 A CN104677715 A CN 104677715A
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- corrosion
- magnesium alloy
- corrosion behavior
- cover glass
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Abstract
The invention relates to a method for recording and observing the corrosion behavior of a magnesium alloy microstructure in situ, and belongs to the field of material corrosion analysis. The method comprises the following steps: firstly, sampling, taking a metallographic specimen from a to-be-analyzed magnesium alloy material, carrying out rough grinding, fine grinding, polishing and corroding for later use; putting a cover glass with good light transparency on a shelving unit of a metallographic microscope, wherein the cover glass can completely cover a microscope observation hole; putting a processed sample on the cover glass, and adjusting a lens so as to obtain a clear metallographic structure; dipping a cotton swab in a corrosion salt solution, wiping the observation surface of the specimen lightly for multiple times, and putting the specimen on the cover glass; observing and recording the corrosion behavior of the specimen by the microscope, and recording the crystal boundary, the crystal grain and the second phase corrosion status at each time interval by observing and recording the corrosion behavior of the specimen by the microscope. According to the invention, the sampling is simple, the cycle is short, and the analysis speed is high; the priority corrosion region can be determined accurately by comparing, observing and analyzing the corrosion behavior of the magnesium alloy microstructure, so that the corrosion mechanism of the material can be judged.
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 corrosion analysis technical field.
Technical background
Magnesium alloy has high specific strength, high specific stiffness, good damping performance, is easy to the advantages such as processing, is widely used the fields such as Aero-Space, military project, automobile and electronic product.But because alloying element adds in magnesium alloy, the strong electropositivity of magnesium and alloy element solid solution degree produces large impact, magnesium and alloying element have very strong chemical affinity, impel intermetallic compound to be formed.Because these intermetallic compounds have the electrode potential being different from solid solution, form micro cell, thus cause bimetallic corrosion with solid solution, therefore corrosion stability of magnesium alloy can be very undesirable.
In the magnesium alloy, usually have 3 to miniature corrosion cell, respectively: in crystal grain, precipitated phase/α-Mg matrix, square phase/α-Mg, tiny precipitated phase and rare Zr addition/crystal boundary are without precipitation district.Research magnesium alloy substrate, precipitated phase, the size of crystal boundary, distribution and between interaction, disclose the corrosion mechanism of bimetallic corrosion in magnesium alloy, for the intrinsic corrosion stability improving magnesium alloy, the corrosion-resistant magnesium alloy of development of new has important scientific meaning.
At present, more single for the means forming micro cell reaction in home position observation magnesium alloy, such as stereomicroscope, sem observation etc.But stereomicroscope is subject to the restriction of enlargement ratio usually, and utilizes the operation relative complex of scanning electron microscope home position observation.The evolution process of metaloscope in-situ monitoring magnesium alloy microstructures corrosion behavior is utilized to have unique advantage, as simple to operate, clear picture etc.Can be strong supplementary as what study the in-situ corrosion such as stereomicroscope, scanning electron microscope, for the relevance research between Macrocosm and microcosm corrosion phenomenon, also can be used for the timely monitoring of long-term corrosion research.
Summary of the invention
The object of the present invention is to provide a kind of method for home position observation record magnesium alloy microstructures corrosion behavior, utilize common cover glass and metaloscope can carry out the corrosion observed and recorded of original position to the corrosion behavior of magnesium alloy microstructures.
For a method for home position observation record magnesium alloy microstructures corrosion behavior, comprise the following steps:
(1) sample preparation: get one block of metallographic specimen on magnesium alloy materials to be analyzed, stand-by after corase grind, fine grinding, polishing, corrosion;
(2) on metaloscope articles holding table, place the cover glass that a slice light transmission is good, cover glass size covers microscopic examination hole completely; Placed on the cover slip by the sample handled well in step (1), adjustment camera lens obtains metallographic structure clearly;
(3) dip corrosive salt solution with cotton swab, gently after wipe samples sightingpiston several times, sample is placed on cover glass;
(4) by the corrosion behavior of microscopic examination record sample, at interval of the equal time, original position record is carried out to crystal boundary, crystal grain, second-phase corrosion condition.
In step (1), described metallographic specimen through 240#, 800#, 2000#, 5000# sand paper corase grind and fine grinding after, polishing; Polished sightingpiston dries up with hair-dryer erode away microstructure under corresponding metallographic etchant after, stand-by; Described metallographic etchant is 4%(volume %) nital etc.
In step (2), the thickness of described cover glass is 0.17 ± 0.02mm, otherwise the permeability of light is bad, affects observing effect.
In step (3), described corrosive salt solution is NaCl solution, Na
2sO
4, (NH
4)
2sO
4solution etc., to observe the corrosion behavior of magnesium alloy in different medium; Concentration of salt solution is 1 × 10
-5~ 1 × 10
-3between mol/L, excessive concentration or too lowly all can affect sample etches speed, causing can not effective observed and recorded.
The number of times dipping corrosive liquid wipe samples surface with cotton swab is 3 ~ 16 times (wiping number of times depends on alloy intrinsic corrosion stability), is put on metaloscope by sample rapidly and observes after wiping.
In step (4), the time interval of the corrosion behavior of record sample is 0.5s ~ 5s, is equally spaced, otherwise can not effectively contrasts between the metallographic of original position record the writing time of corrosion behavior.
After corrosion behavior observed and recorded 2 ~ 5min, sample surfaces corrosion is expanded gradually from preferential corrosion area, cause the generation that large area is corroded, the observed and recorded of corrosion behavior should not be carried out again, need sightingpiston to be carried out again on the sand paper of 5000# polishing and polishing, repeat step (2) ~ (4).
Advantage of the present invention:
(1) sample preparation is simple, the cycle is short, it is reliably easy to analyze, and is analyzed the corrosion behavior of magnesium alloy microstructures, accurately determine corrosion area, judge fast to Corrosion Behaviors of Magnesium Alloys mechanism, corrosion type by paired observation.Can be used as and the strong of the in-situ corrosion such as stereomicroscope, scanning electron microscope research is supplemented, for the relevance research between Macrocosm and microcosm corrosion phenomenon, also can be used for the timely monitoring of long-term corrosion research.
(2) avoid mirror body pollution: because cover glass size is much larger than lens opening size, corrosive medium directly or indirectly can not contact with mirror body.Simultaneously the light transmission of cover glass is good, to meet enlargement ratio be 1000 × the analysis of metaloscope in-situ corrosion use.
Accompanying drawing explanation
Fig. 1 is metaloscope original position microcosmic corrosion analysis schematic diagram.
Fig. 2 is 500 times of metallographs of the EW75 magnesium alloy in-situ corrosion Continuous Observation 1 ~ 6s after solution treatment.
Fig. 3 is 500 times of metallographs of the WE93 magnesium alloy in-situ corrosion Continuous Observation 1 ~ 6s of As-extruded.
Fig. 4 is 200 times of metallographs of the AZ80 magnesium alloy in-situ corrosion Continuous Observation 2 ~ 12s of aging state.
Fig. 5 is 500 times of metallographs of the EW75 magnesium alloy in-situ corrosion Continuous Observation 0.5 ~ 3s of As-extruded.
Fig. 6 is 200 times of metallographs of the EW75 magnesium alloy in-situ corrosion Continuous Observation 1 ~ 6s of aging state.
Embodiment
For disclosing technical scheme of the present invention further, elaborated by embodiment below in conjunction with Figure of description:
As shown in Figure 1, be metaloscope original position microcosmic corrosion analysis schematic diagram, wherein, 1 is sample to be seen, and 2 is cover glasses, and 3 is metaloscope objective tables, and 4 is metallography microscope lens heads.
First sample preparation: get one block of metallographic specimen on the material that will analyze, stand-by after corase grind, fine grinding, polishing, corrosion; On metaloscope articles holding table, place the cover glass (thickness is 0.17mm ± 0.02mm) that a slice light transmission is good, size will cover microscopic examination hole completely, is placed on the cover slip by the sample handled well, and adjustment camera lens obtains metallographic structure clearly; Dipping concentration with cotton swab is 1 × 10
-5~ 1 × 10
-3the NaCl solution of mol/L (being observed the corrosion behavior of magnesium alloy in different medium, being chosen different salt solusions, as selected Na
2sO
4, (NH
4)
2sO
4solution etc.), gently after wipe samples sightingpiston 3 ~ 16 times, rapidly sample is placed on cover glass; By the corrosion behavior of microscopic examination record sample, at interval of x second (0.5s≤x≤5s), original position record is carried out to crystal boundary, crystal grain, second-phase corrosion condition.Because cover glass directly contacts with sightingpiston, the gas that alloy corrosion is produced can not get timely release, can form bubble, the area of bubble area and preferential corrosion area around corrosion area; The microstructure etch state of comparative analysis alloy, analyzes its corrosion mechanism.
Embodiment 1
The microstructure corrosion behavior of EW75 magnesium alloy after the solution treatment of home position observation record in NaCl solution:
(1) sample preparation: get one block of metallographic specimen on EW75 magnesium alloy materials, after 240#, 800#, 2000#, 5000# sand paper corase grind and fine grinding, polishing; Polished sightingpiston is at 4%(volume %) erode away microstructure under nital after, dry up with hair-dryer, stand-by.
(2) on metaloscope articles holding table, place the cover glass that a slice light transmission is good, cover glass size covers microscopic examination hole completely; Placed on the cover slip by the sample handled well in step (1), adjustment camera lens obtains metallographic structure clearly; The thickness of cover glass is 0.17 ± 0.02mm, otherwise the permeability of light is bad, affects observing effect.
(3) 1 × 10 is dipped with cotton swab
-4mol/L NaCl corrosive liquid, gently after wipe samples sightingpiston 6 times, is placed in sample on cover glass;
(4) by the corrosion behavior of microscopic examination record sample, at interval of 1s, original position record is carried out to crystal boundary, crystal grain, second-phase corrosion condition.
Fig. 2 is 500 times of metallographs of the EW75 magnesium alloy in-situ corrosion Continuous Observation 1 ~ 6s after solution treatment, and its observation condition is: corrosive liquid 1 × 10
-4mol/L NaCl, sightingpiston wiping number of times is 6 times, time interval x=1s.
As can be seen from Figure 2, after the solution treatment of EW75 magnesium alloy, the domain of the existence of second-phase around crystal grain, is not had to corrode; But at second-phase and the crystal boundary intersection of incomplete back dissolving, due to the potential difference (PD) effect between second-phase and matrix, bimetallic corrosion occurs for matrix and second-phase interface, and reaction equation is: Mg+2H
2o → Mg (OH)
2+ H
2↑, produce H
2form bubble, because cover glass directly contacts with sightingpiston, the gas that alloy corrosion is produced can not get timely release, can form bubble, the area of bubble area and preferential corrosion area around corrosion area; Along with constantly carrying out of corrosion, corrosion area area constantly expands, and the region not occurring to corrode with surrounding forms obvious contrast.
Embodiment 2
The WE93 magnesium alloy of home position observation record As-extruded is at NaHSO
3microstructure corrosion behavior in solution, its observation condition is: corrosive liquid 1 × 10
-4mol/L NaHSO
3, sightingpiston wiping number of times is 8 times, time interval x=1s, and other steps are with embodiment 1.
Fig. 3 is 500 times of metallographs of the WE93 magnesium alloy in-situ corrosion Continuous Observation 1 ~ 6s of As-extruded.As can be seen from Figure 3, obvious at the larger-size zonal corrosion of second-phase, the size of second-phase is larger, and the potential difference (PD) effect between matrix and second-phase is more obvious, and the trend that matrix and second-phase interface occur bimetallic corrosion is larger, and alloy corrosion produces H
2form bubble, because cover glass directly contacts with sightingpiston, the gas that alloy corrosion is produced can not get timely release, can form bubble, the area of bubble area and preferential corrosion area around corrosion area.WE93 As-extruded alloy corrosion resistance is better, and corrosion rate is lower, corrosion to produce bubble less.
Embodiment 3
The microstructure corrosion behavior of AZ80 magnesium alloy in NaCl solution of home position observation record aging state, its observation condition is: corrosive liquid 1 × 10
-5mol/L NaCl, sightingpiston wiping number of times is 3 times, time interval x=2s, and other steps are with embodiment 1.
Fig. 4 is 200 times of metallographs of the AZ80 magnesium alloy in-situ corrosion Continuous Observation 2 ~ 12s of aging state.As can be seen from Figure 4, the AZ80 magnesium alloy second-phase Mg of aging state
17al
12thicker, and connect into netted to a certain extent.Due to the potential difference (PD) effect between matrix and second-phase, alloy generation bimetallic corrosion.In the place that second-phase is more sparse, alloy preferentially corrodes, and carrying out gradually along with corrosion, corrosion area expands towards periphery gradually.This mainly because second-phase connects into netted, effectively forms corrosion barrier, serves inhibition to corrosion.Alloy corrosion produces H
2form bubble, because cover glass directly contacts with sightingpiston, the gas that alloy corrosion is produced can not get timely release, and can form bubble around corrosion area, bubble spreads from the region that second-phase is sparse gradually to close quarters.
Embodiment 4
The microstructure corrosion behavior of EW75 magnesium alloy in NaCl solution of home position observation record As-extruded, its observation condition is: corrosive liquid 5 × 10
-4mol/L NaCl, sightingpiston wiping number of times is 5 times, time interval x=0.5s, and other steps are with embodiment 1.
Fig. 5 is 500 times of metallographs of the magnesium alloy in-situ corrosion Continuous Observation 0.5 ~ 3s of As-extruded.As can be seen from Figure 5, zonal corrosion on extruding streamline is obvious, second-phase dense distribution on extruding streamline, and the potential difference (PD) effect between matrix and second-phase is more obvious, the trend that matrix and second-phase interface occur bimetallic corrosion is larger, and alloy corrosion produces H
2form bubble, because cover glass directly contacts with sightingpiston, the gas that alloy corrosion is produced can not get timely release, can form bubble, the area of bubble area and preferential corrosion area around corrosion area.
Embodiment 5
The microstructure corrosion behavior of EW75 magnesium alloy in NaCl solution of home position observation record aging state, its observation condition is: corrosive liquid 1 × 10
-4mol/L NaCl, sightingpiston wiping number of times is 4 times, time interval x=1s, and other steps are with embodiment 1.
Fig. 6 is 200 times of metallographs of the EW75 magnesium alloy in-situ corrosion Continuous Observation 1 ~ 6s of aging state.As can be seen from Figure 6, EW75 aging state corrosion distribution is relatively more even, and this is that the size of crystal grain is basically identical because the second-phase of the EW75 alloy of aging state is evenly distributed, in bimetallic corrosion generating process, in alloy surface generation general corrosion.Along with carrying out gradually of corrosion, the bubble adding up to corrosion to produce expands gradually, finally will join together, and the corrosion type of EW75 alloy belongs to face corrosion.
After corrosion behavior observed and recorded 2 ~ 5min, sample surfaces corrosion is expanded gradually from preferential corrosion area, cause the generation that large area is corroded, the observed and recorded of corrosion behavior should not be carried out again, need sightingpiston to be carried out again on the sand paper of 5000# polishing and polishing, repeat step (2) ~ (4).
In the present invention, because cover glass directly contacts with sightingpiston, the gas that alloy corrosion is produced can not get timely release, can form bubble, the area of bubble area and preferential corrosion area around corrosion area; The microstructure etch state of comparative analysis alloy, analyzes its corrosion mechanism.Can be seen by above embodiment, sample preparation of the present invention is simple, the cycle is short, analysis speed is fast, be analyzed the corrosion behavior of magnesium alloy microstructures by paired observation, accurately can determine its preferential corrosion area, thus the corrosion mechanism of material is judged.
Claims (8)
1., for a method for home position observation record magnesium alloy microstructures corrosion behavior, comprise the following steps:
(1) sample preparation: get one block of metallographic specimen on magnesium alloy materials to be analyzed, stand-by after corase grind, fine grinding, polishing, corrosion;
(2) on metaloscope articles holding table, place the cover glass that a slice light transmission is good, cover glass size covers microscopic examination hole completely; Placed on the cover slip by the sample handled well in step (1), adjustment camera lens obtains metallographic structure clearly;
(3) dip corrosive salt solution with cotton swab, gently after wipe samples sightingpiston several times, sample is placed on cover glass;
(4) by the corrosion behavior of microscopic examination record sample, at interval of the equal time, original position record is carried out to crystal boundary, crystal grain, second-phase corrosion condition.
2. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 1, is characterized in that: described metallographic specimen through 240#, 800#, 2000#, 5000# sand paper corase grind and fine grinding after, polishing; Polished sightingpiston dries up with hair-dryer erode away microstructure under metallographic etchant after, stand-by.
3. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 2, is characterized in that: described metallographic etchant is 4 volume % nitals.
4. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 1, is characterized in that: the thickness of described cover glass is 0.17 ± 0.02mm.
5. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 1, is characterized in that: described corrosive salt solution is NaCl solution, Na
2sO
4or (NH
4)
2sO
4solution, concentration is 1 × 10
-5~ 1 × 10
-3mol/L.
6. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 1, is characterized in that: the number of times dipping corrosive liquid wipe samples surface with cotton swab is 3 ~ 16 times.
7. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 1, is characterized in that: the time interval of the corrosion behavior of record sample is 0.5s ~ 5s.
8. the method for home position observation record magnesium alloy microstructures corrosion behavior according to claim 1, it is characterized in that: after corrosion behavior observed and recorded 2 ~ 5min, sightingpiston is carried out again on the sand paper of 5000# polishing and polishing, repeat step (2) ~ (4).
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| CN106289962A (en) * | 2016-10-12 | 2017-01-04 | 中国科学院金属研究所 | Can high low power online observation sample marking distance section deformation and the in-situ test system of damage |
| CN109540774A (en) * | 2018-11-01 | 2019-03-29 | 暨南大学 | Detection coating deforms the device and method of its corrosion resistance differentiation with magnesium substrates |
| CN109556939A (en) * | 2018-12-03 | 2019-04-02 | 中国科学院青藏高原研究所 | Sample nuclear track in-situ etch observation method and equipment |
| CN110887566A (en) * | 2018-09-07 | 2020-03-17 | 关西涂料株式会社 | Color measuring method for coated board and color mixing method using the same |
| 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 |
| 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 |
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| CN110887566A (en) * | 2018-09-07 | 2020-03-17 | 关西涂料株式会社 | Color measuring method for coated board and color mixing method using the same |
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| 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 |
| CN114252391A (en) * | 2020-09-21 | 2022-03-29 | 宝山钢铁股份有限公司 | Method for evaluating industrial atmospheric corrosion resistance of steel welding joint |
| 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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