CN107219105B - Method for observing AZ31 magnesium alloy internal shear band - Google Patents
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/00—Sampling; Preparing specimens for investigation
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
The invention discloses an observation method of an AZ31 magnesium alloy internal shear band, which comprises the following steps: firstly, adopting sliding friction to enable AZ31 magnesium alloy to generate plastic deformation; secondly, sampling the AZ31 magnesium alloy subjected to plastic deformation and annealing; grinding the annealed AZ31 magnesium alloy sample step by step to obtain an AZ31 magnesium alloy sample observation plane; fourthly, corroding the observation plane of the AZ31 magnesium alloy sample; and fifthly, observing the appearance of the internal shear band of the AZ31 magnesium alloy sample after corrosion by using an optical microscope. According to the invention, the contrast difference between the internal shear band region and the non-shear band region of the AZ31 magnesium alloy sample is improved through annealing treatment, the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample after deformation can be clearly observed, and the method has the advantages of simple process, low cost and easiness in popularization.
Description
Technical Field
The invention belongs to the technical field of metal material microstructure observation, and particularly relates to an observation method for an AZ31 magnesium alloy internal shear band.
Background
The magnesium alloy is a metal structure material with the minimum density, has higher specific strength and specific modulus, and has wide application prospect in the fields of electronics, communication, aerospace and the like. The magnesium alloy has a close-packed hexagonal crystal structure, and thus has little independent slip system and low plasticity at room temperature. According to different deformation conditions, the plastic deformation mechanism of magnesium alloy is mainly divided into three types: (1) dislocation glide under high temperature conditions; (2) twinning under low temperature conditions; (3) shear band at high strain rate. Under the first two mechanisms, magnesium alloys typically exhibit continuous plastic deformation that is slow and predictable. In the third shear band mechanism, the magnesium alloy may be suddenly broken, causing serious consequences, so the research on the shear band is particularly important. The AZ31 magnesium alloy is the most widely used magnesium alloy at present, and has better room temperature strength, good ductility and excellent corrosion resistance. Therefore, it is necessary to study the morphology and distribution of the internal shear band of the AZ31 magnesium alloy.
Shear bands are a deformed structure formed by plastic deformation concentrated in localized areas. The heat generated by plastic deformation causes a rapid increase in the temperature within the shear band, causing the material strength within the shear band to be significantly lower than the surrounding non-shear band regions, and this weakening of the strength causes the shear band regions to become initiation and rapid propagation zones for cracks. Therefore, the research on the spatial distribution mode of the shear band is the key to research on the plastic deformation and fracture mechanism of the AZ31 magnesium alloy under the condition of high strain rate. At present, the shear band is directly observed mainly through the contrast difference between a shear band region and a non-shear band region after the AZ31 magnesium alloy subjected to plastic deformation is corroded, but the contrast of the shear band region and the non-shear band region is relatively close to each other under the condition and is not easy to distinguish, so that the spatial distribution of the shear band is difficult to accurately reflect. The problems of small contrast difference and difficult determination of the shear band also exist when the scanning electron microscope is used for observing the shear band in the AZ31 magnesium alloy, and the observation range of the perspective electron microscope on the shear band is small, so that the accurate determination of the appearance and distribution of the shear band in a large range is difficult to realize.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for observing an AZ31 magnesium alloy internal shear band aiming at the defects of the prior art. According to the method, the AZ31 magnesium alloy sample which is plastically deformed by sliding friction is annealed, so that the shear band region of the AZ31 magnesium alloy sample is completely recrystallized, and obvious contrast difference is formed between the shear band region and the surrounding non-shear band region after the corrosive agent acts, and the appearance and distribution of the shear band are highlighted. The method has the advantages of simple process, low cost and easy popularization.
In order to solve the technical problem, the invention provides a method for observing an AZ31 magnesium alloy internal shear band, which is characterized by comprising the following steps:
step one, adopting sliding friction to enable the surface of AZ31 magnesium alloy to generate plastic deformation;
step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample;
step three, using 600 in sequence#、1000#、2000#、5000#The silicon carbide abrasive paper is used for gradually grinding the surface of the AZ31 magnesium alloy sample after annealing treatment in the step two to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
The method as described above, wherein the sliding friction in the first step has a strain rate of 102s-1～103s-1。
The method is characterized in that the annealing treatment temperature in the second step is 160-200 ℃, and the heat preservation time is 20 min.
The method as described above, wherein the etchant used in step four is prepared from oxalic acid, nitric acid and water in an amount of 5 g: 10 ml: 0.5ml, and the oxalic acid and the nitric acid are analytically pure reagents.
The method as described above, wherein the etching treatment time in the fourth step is 30 seconds.
The specific method for plastically deforming the AZ31 magnesium alloy by adopting a sliding friction manner in the first step is disclosed in the invention patent with the publication number CN102321791B of 'a method for realizing the nanocrystallization of the surface of a metal material by using sliding friction'.
The principle of the invention is as follows: after plastic deformation of the AZ31 magnesium alloy by sliding friction, the inside of the AZ31 magnesium alloy generates a shear band region having a defect density much higher than that of the surrounding non-shear band region, resulting in a shear band region having higher deformation energy storage, which leads to a shear band region having higher recrystallization ability under appropriate conditions. And (3) annealing the AZ31 magnesium alloy sample after plastic deformation, completely recrystallizing the shear belt region, and enabling the defect density in the shear belt region after complete recrystallization to be lower than that in the surrounding non-shear belt region, so that the shear belt region has high corrosion resistance. After the processing of the corrosive agent, the shear zone area and the surrounding non-shear zone area respectively show bright white and gray black, the contrast difference is obvious, and the appearance and the distribution of the shear zone are further highlighted.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the internal shear band region of the AZ31 magnesium alloy sample is completely recrystallized through the annealing process, so that the contrast difference between the internal shear band region and the non-shear band region of the AZ31 magnesium alloy sample is improved, the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample after plastic deformation are clearly shown, the process is simple, and the cost is low.
2. According to the invention, the optical microscope is adopted to directly observe the shear band in the AZ31 magnesium alloy sample, the distribution of the shear band can be accurately determined in a larger range, a scanning electron microscope and an electronic lens are not required, the equipment requirement is low, and the popularization is easy.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a graph showing the internal shear band of the AZ31 magnesium alloy sample in example 1 of the present invention.
FIG. 2 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of comparative example 1 according to the present invention.
FIG. 3 is a graph showing the internal shear band of the AZ31 magnesium alloy sample in example 2 of the present invention.
FIG. 4 is a graph showing the internal shear band of the AZ31 magnesium alloy sample in example 3 of the present invention.
FIG. 5 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of comparative example 2 according to the present invention.
FIG. 6 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of comparative example 3 according to the present invention.
Detailed Description
Example 1
Step one, adopting sliding friction to enable the surface of the AZ31 magnesium alloy to generate plastic deformation, and controlling the strain rate of the sliding friction of the surface of the AZ31 magnesium alloy to be 102s-1；
Step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample; the temperature of the annealing treatment is 180 ℃, and the heat preservation time is 20 min;
step three, using 600 in sequence#、1000#、2000#、5000#The silicon carbide abrasive paper is used for gradually grinding the surface of the AZ31 magnesium alloy sample after annealing treatment in the step two to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents; the time of the corrosion treatment is 30 s;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
FIG. 1 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of this example, wherein the arrows indicate the shear band. In FIG. 1, the internal sheared area of the AZ31 magnesium alloy sample is bright white, the non-sheared area is gray black, the contrast difference between the sheared area and the surrounding non-sheared area is very obvious, and the appearance and distribution of the sheared area are clear and easy to observe.
Comparative example 1
Step one, adopting sliding friction to enable the surface of the AZ31 magnesium alloy to generate plastic deformation, and controlling the strain rate of the sliding friction of the surface of the AZ31 magnesium alloy to be 102s-1；
Step two, using 600 in sequence#、1000#、2000#、5000#The silicon carbide abrasive paper grinds the surface of the AZ31 magnesium alloy sample subjected to plastic deformation in the step two step by step to obtain a flat and fine-scratched observation plane of the AZ31 magnesium alloy sample; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step three, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step two by using a corrosive agent, so that a shear band in the AZ31 magnesium alloy sample is shown; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents; the time of the corrosion treatment is 30 s;
and step four, observing the appearance and distribution of the shear band inside the AZ31 magnesium alloy sample shown in step three by using an optical microscope.
FIG. 2 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of this example, wherein the arrows indicate the shear band. In the AZ31 magnesium alloy sample which is not annealed in FIG. 2, the internal sheared strip is gray black, the non-sheared strip area is gray, the contrast between the sheared strip area and the surrounding non-sheared strip area is not obvious, the appearance and distribution of the sheared strip are fuzzy, and the observation is difficult.
Comparing example 1 with comparative example 1, it can be seen that the contrast difference between the internal shear band region and the surrounding non-shear band region of the annealed AZ31 magnesium alloy sample is more obvious than that of the non-annealed AZ31 magnesium alloy, the appearance and distribution of the shear band are more clearly visible, and the observation is easier, which shows that the annealing treatment is helpful for the observation of the internal shear band of the AZ31 magnesium alloy. The method of the invention can be used for conveniently observing the appearance and distribution of the shear band in the AZ31 magnesium alloy sample in a larger range.
Example 2
Step one, adopting sliding friction to enable the surface of the AZ31 magnesium alloy to generate plastic deformation, and controlling the strain rate of the sliding friction of the surface of the AZ31 magnesium alloy to be 5.5 multiplied by 102s-1；
Step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample; the temperature of the annealing treatment is 160 ℃, and the heat preservation time is 20 min;
step three, using 600 in sequence#、1000#、2000#、5000#The silicon carbide abrasive paper is used for gradually grinding the surface of the AZ31 magnesium alloy sample after annealing treatment in the step two to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents; the time of the corrosion treatment is 30 s;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
FIG. 3 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of this example, wherein the arrows indicate the shear band. In FIG. 3, the internal sheared area of the AZ31 magnesium alloy sample is bright white, the non-sheared area is gray black, the contrast difference between the sheared area and the surrounding non-sheared area is obvious, the appearance and distribution of the sheared area are clear, and the observation is easy.
Example 3
Step one, adopting sliding friction to enable the surface of the AZ31 magnesium alloy to generate plastic deformation, and controlling the strain rate of the sliding friction of the surface of the AZ31 magnesium alloy to be 103s-1；
Step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample; the temperature of the annealing treatment is 200 ℃, and the heat preservation time is 20 min;
step (ii) ofThirdly, use 600 in turn#、1000#、2000#、5000#The silicon carbide abrasive paper is used for gradually grinding the surface of the AZ31 magnesium alloy sample after annealing treatment in the step two to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents; the time of the corrosion treatment is 30 s;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
FIG. 4 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of this example, wherein the arrows indicate the shear band. In FIG. 4, the internal sheared area of the AZ31 magnesium alloy sample is bright white, the non-sheared area is gray black, the contrast difference between the sheared area and the surrounding non-sheared area is obvious, the appearance and distribution of the sheared area are clear, and the observation is easy.
The contrast difference between the internal shear zone area and the surrounding non-shear zone area of the AZ31 magnesium alloy samples subjected to annealing treatment in example 1, example 2 and example 3 is obvious, and the appearance and distribution of the shear zone are clear; after the annealing temperature was increased from 160 ℃ to 200 ℃, there was no significant change in the shear band density, indicating that all shear band regions had completely recrystallized after the annealing process.
Comparative example 2
Step one, adopting sliding friction to enable the surface of the AZ31 magnesium alloy to generate plastic deformation, and controlling the strain rate of the sliding friction of the surface of the AZ31 magnesium alloy to be 103s-1；
Step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample; the temperature of the annealing treatment is 120 ℃, and the heat preservation time is 20 min;
step three, using 600 in sequence#、1000#、2000#、5000#The silicon carbide abrasive paper is used for gradually grinding the surface of the AZ31 magnesium alloy sample after annealing treatment in the step two to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents; the time of the corrosion treatment is 30 s;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
FIG. 5 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of this example, wherein the arrows indicate the shear band. In FIG. 5, the AZ31 magnesium alloy sample has white internal sheared area, gray non-sheared area, unobvious contrast between sheared area and surrounding non-sheared area, unclear appearance and distribution of sheared area, and difficult observation.
Comparative example 3
Step one, adopting sliding friction to enable the surface of the AZ31 magnesium alloy to generate plastic deformation, and controlling the strain rate of the sliding friction of the surface of the AZ31 magnesium alloy to be 103s-1；
Step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample; the temperature of the annealing treatment is 150 ℃, and the heat preservation time is 20 min;
step three, using 600 in sequence#、1000#、2000#、5000#The silicon carbide sand paper is annealed in the second stepGrinding the surface of the treated AZ31 magnesium alloy sample step by step to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents; the time of the corrosion treatment is 30 s;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
FIG. 6 is a graph showing the internal shear band of the AZ31 magnesium alloy sample of this example, with the shear band indicated by the arrow. In FIG. 6, the AZ31 magnesium alloy sample has bright white internal shear zone, gray non-shear zone area, slightly obvious contrast difference between shear zone area and surrounding non-shear zone area, and clear appearance and distribution of shear zone.
Comparing example 2, example 3, comparative example 2 and comparative example 3, it can be known that when the annealing temperature is less than 160 ℃, the contrast of the internal shear zone area and the surrounding non-shear zone area of the AZ31 magnesium alloy sample is not obvious enough, and the appearance and distribution of the shear zone are not clear enough; when the annealing temperature is 200 ℃, a small part of the shear band in the AZ31 magnesium alloy sample becomes wide and the brightness increases, and if the annealing temperature exceeds 200 ℃, more shear bands become wide and even are connected into one piece, so that the appearance and distribution of the shear band are not easy to see. Therefore, the temperature of the annealing treatment is selected to be 160-200 ℃.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (3)
1. A method of viewing internal shear bands in AZ31 magnesium alloy, the method comprising the steps of:
step one, adopting sliding friction to enable the surface of AZ31 magnesium alloy to generate plastic deformation;
step two, sampling the AZ31 magnesium alloy subjected to plastic deformation in the step one to obtain an AZ31 magnesium alloy sample, and then annealing the AZ31 magnesium alloy sample; the temperature of the annealing treatment is more than 160 ℃ and less than 200 ℃, and the heat preservation time is 20 min;
step three, using 600 in sequence#、1000#、2000#、5000#The silicon carbide abrasive paper is used for gradually grinding the surface of the AZ31 magnesium alloy sample after annealing treatment in the step two to obtain a flat and fine-scratched AZ31 magnesium alloy sample observation plane; after replacing the silicon carbide abrasive paper each time, horizontally rotating the observation plane of the AZ31 magnesium alloy sample by 90 degrees, and then grinding until the scratches of the previous grinding are ground off;
step four, carrying out corrosion treatment on the observation plane of the AZ31 magnesium alloy sample obtained in the step three by using a corrosive agent to show a shear band in the AZ31 magnesium alloy sample; the corrosive agent is prepared from oxalic acid, nitric acid and water according to the weight ratio of 5 g: 10 ml: 0.5ml of oxalic acid and nitric acid are both analytically pure reagents;
and step five, observing the appearance and distribution of the internal shear band of the AZ31 magnesium alloy sample shown in the step four by using an optical microscope.
2. The method for observing an AZ31 magnesium alloy internal shear band according to claim 1, wherein the sliding friction strain rate in step one is 102s-1～103s-1。
3. An observation method of an AZ31 magnesium alloy internal shear band as claimed in claim 1, wherein the time of said corrosion treatment in the fourth step is 30 s.
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| CN103983499A (en) * | 2014-05-12 | 2014-08-13 | 太原科技大学 | Method for observing inner shearing zone of zirconium base amorphous alloy |
| CN107976443A (en) * | 2017-11-24 | 2018-05-01 | 西北有色金属研究院 | A kind of observational technique of pure magnesium metallographic structure |
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| CN103983499A (en) * | 2014-05-12 | 2014-08-13 | 太原科技大学 | Method for observing inner shearing zone of zirconium base amorphous alloy |
| CN107976443A (en) * | 2017-11-24 | 2018-05-01 | 西北有色金属研究院 | A kind of observational technique of pure magnesium metallographic structure |
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| 不同轧制工艺对AZ31镁合金板材组织与性能的影响;黄鑫;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20130315;摘要、论文第2、3章 * |
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