CN107219105A - A kind of observational technique to AZ31 magnesium alloy internal shear bands - Google Patents
A kind of observational technique to AZ31 magnesium alloy internal shear bands Download PDFInfo
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Abstract
The invention discloses a kind of observational technique to AZ31 magnesium alloy internal shear bands, comprise the following steps：First, it is plastically deformed AZ31 magnesium alloys using sliding friction；2nd, the AZ31 magnesium alloys sampling after plastic deformation is made annealing treatment；3rd, the AZ31 magnesium alloys sample after annealing is ground step by step, obtains AZ31 magnesium alloy sample observation planes；4th, AZ31 magnesium alloy sample observation planes are corroded；5th, the pattern of the AZ31 magnesium alloy sample interior shear bands after being corroded using observation by light microscope.The present invention improves the contrast difference that AZ31 magnesium alloys sample interior shears region and non-shear region by annealing, can clear view to deformation after AZ31 magnesium alloy sample interior shear bands pattern and distribution, and technique is simple, and cost is relatively low, it is easy to promote.
Description
Technical field
The invention belongs to metal material microstructure observation technology field, and in particular to a kind of to being cut inside AZ31 magnesium alloys
Cut the observational technique of band.
Background technology
Magnesium alloy is the minimum structural metallic materials of existing density, with higher specific strength and specific modulus, in electronics, is led to
The fields such as news, Aero-Space have broad application prospects.Magnesium alloy has Patterns for Close-Packed Hexagonal Crystal structure, thus in room temperature condition
Lower independent slip system is few and plasticity is low.According to the difference of deformation condition, the Plastic Deformation Mechanism of magnesium alloy is broadly divided into three kinds：
(1) dislocation movement by slip under hot conditions；(2) twin under cryogenic conditions；(3) shear band under high strain rate.In first two
Mechanism under, magnesium alloy typically exhibits out continuous plastic deformation, and this plastic deformation is slow, predictable.The 3rd
Kind shear band mechanism under, magnesium alloy can then produce unexpected fracture, cause serious consequence, therefore to the research of shear band particularly
It is important.AZ31 magnesium alloys are a kind of magnesium alloys being most widely used at present, with preferable room temperature strength, good ductility
And excellent resistance to corrosion.Therefore, the pattern of research AZ31 magnesium alloy internal shear bands and distribution are necessary.
Shear band is concentration of plastic deformation in a kind of distressed structure formed by regional area.It is plastically deformed the thermal conductivity produced
Shear band internal temperature is caused to raise rapidly, so that shear band internal material intensity is substantially less than surrounding non-shear region, this
The reduction for planting intensity causes shearing region to become the germinating area and fast spreading area of crackle.So the space of research shear band
Distribution mode is the plastic deformation and the key of fracture mechanism of AZ31 magnesium alloys under the conditions of research high strain rate.At present, to cutting
Cut the contrast of the main shearing region and non-shear region by after the AZ31 Corrosion Behaviors of Magnesium Alloys of plastic deformation of research of band
Difference is directly observed, but shearing region is compared close with the contrast of non-shear region under the conditions of this, is not easily distinguishable, this
It is difficult to accurately reflect the spatial distribution of shear band.Using the shear band in scanning electron microscopic observation AZ31 magnesium alloys it is same there is also
The problem of contrast difference is smaller, shear band is difficult to determine, and the range of observation for having an X-rayed Electronic Speculum to shear band is smaller, it is difficult to realize compared with
The accurate pattern for determining shear band and distribution in a wide range of.
The content of the invention
The technical problems to be solved by the invention are to close AZ31 magnesium there is provided a kind of for above-mentioned the deficiencies in the prior art
The observational technique of golden internal shear band.This method is carried out at annealing to the AZ31 magnesium alloys sample being plastically deformed by sliding friction
Reason, make the shearing region perfect recrystallization of AZ31 magnesium alloy samples, corrosive agent effect after with around non-shear region shape
Into obvious contrast difference, so as to highlight pattern and the distribution of shear band.This method technique is simple, and cost is relatively low, it is easy to promote.
In order to solve the above technical problems, the invention provides a kind of observational technique to AZ31 magnesium alloy internal shear bands,
Characterized in that, this method comprises the following steps：
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then
AZ31 magnesium alloy samples are made annealing treatment；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 4: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；
Step 5: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4
And distribution.
Above-mentioned method, it is characterised in that the strain rate of sliding friction described in step one is 102s-1~103s-1。
Above-mentioned method, it is characterised in that the temperature made annealing treatment described in step 2 is 160 DEG C~200 DEG C, during insulation
Between be 20min.
Above-mentioned method, it is characterised in that corrosive agent described in step 4 is by oxalic acid, nitric acid and water according to 5g：10ml：
0.5ml ratio is mixed, and the oxalic acid and nitric acid are AR.
Above-mentioned method, it is characterised in that the time of corrosion treatment described in step 4 is 30s.
Sliding friction mode is used to make the specific method that AZ31 magnesium alloys are plastically deformed for Granted publication in step one
Number draped over one's shoulders for the CN102321791B patent of invention of " a kind of method that making Nano surface of metal material is realized in utilization sliding friction "
The method of dew.
The present invention principle be：Made using sliding friction after AZ31 magnesium alloys are plastically deformed, AZ31 magnesium alloys it is interior
The defect concentration that portion is generated in shearing region, the region is far above surrounding non-shear region, causes shearing region tool
There is higher deformation energy, this causes shearing region to have higher recrystallization ability under suitable condition.Plasticity is become
AZ31 magnesium alloy samples after shape are made annealing treatment, and perfect recrystallization, the shearing after perfect recrystallization occur for shearing region
Defect concentration in region is less than the non-shear region of surrounding, so that shearing region has higher corrosion resistance
Energy.After caustic treatment, brilliant white and grey black, contrast difference is presented with surrounding non-shear region in shearing region respectively
Substantially, and then pattern and the distribution of shear band are highlighted.
The present invention has advantages below compared with prior art：
1st, the present invention makes AZ31 magnesium alloys sample interior shear region and occurs perfect recrystallization by annealing process, from
And the contrast difference of AZ31 magnesium alloys sample interior shearing region and non-shear region is improved, clearly displaying is plastically deformed
The pattern of AZ31 magnesium alloys sample interior shear band and distribution afterwards, technique is simple, and cost is relatively low.
2nd, the present invention directly observes AZ31 magnesium alloy sample interior shear bands using light microscope, can be in a big way
The interior accurate distribution for determining shear band, without using ESEM and electron lens, equipment requirement is low, it is easy to promote.
Technical scheme is described in further detail below by drawings and examples.
Brief description of the drawings
Fig. 1 is the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the embodiment of the present invention 1.
Fig. 2 is the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in comparative example 1 of the present invention.
Fig. 3 is the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the embodiment of the present invention 2.
Fig. 4 is the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the embodiment of the present invention 3.
Fig. 5 is the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in comparative example 2 of the present invention.
Fig. 6 is the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in comparative example 3 of the present invention.
Embodiment
Embodiment 1
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed, AZ31 Mg alloy surfaces are controlled
The strain rate of sliding friction is 102s-1；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then
AZ31 magnesium alloy samples are made annealing treatment；The temperature of the annealing is 180 DEG C, and soaking time is 20min；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 4: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；The corrosive agent is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml's
Ratio is mixed, and the oxalic acid and nitric acid are AR；The time of the corrosion treatment is 30s；
Step 5: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4
And distribution.
Fig. 1 is that arrow show shear band in the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the present embodiment, figure.
AZ31 magnesium alloys sample interior shear band is brilliant white in Fig. 1, and non-shear region is grey black, and shearing region and surrounding are non-
Clearly, the pattern of shear band and distribution are clear, it is easy to observe for the contrast difference of shearing region.
Comparative example 1
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed, AZ31 Mg alloy surfaces are controlled
The strain rate of sliding friction is 102s-1；
Step 2: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 be plastically deformed after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 3: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 2 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；The corrosive agent is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml's
Ratio is mixed, and the oxalic acid and nitric acid are AR；The time of the corrosion treatment is 30s；
Step 4: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 3
And distribution.
Fig. 2 is that arrow show shear band in the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the present embodiment, figure.
The AZ31 magnesium alloy sample interiors shear band without annealing is grey black in Fig. 2, and non-shear region is grey, shear band
The contrast difference in region and surrounding non-shear region is not obvious, and the pattern of shear band and distribution are fuzzy, and observation is difficult.
Embodiment 1 is compared with comparative example 1 it is known that by the AZ31 magnesium alloy sample interior shear bands of annealing
The contrast difference of region and surrounding non-shear region without the AZ31 magnesium alloys of annealing than becoming apparent, the shape of shear band
Looks and distribution are apparent visible, and it is also more easy to observe, and illustrates that annealing contributes to AZ31 magnesium alloy internal shear bands
Observation.AZ31 magnesium alloy sample interior shear bands can be observed with very convenient interior in a big way by using the method for the present invention
Pattern and distribution.
Embodiment 2
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed, AZ31 Mg alloy surfaces are controlled
The strain rate of sliding friction is 5.5 × 102s-1；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then
AZ31 magnesium alloy samples are made annealing treatment；The temperature of the annealing is 160 DEG C, and soaking time is 20min；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 4: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；The corrosive agent is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml's
Ratio is mixed, and the oxalic acid and nitric acid are AR；The time of the corrosion treatment is 30s；
Step 5: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4
And distribution.
Fig. 3 is that arrow show shear band in the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the present embodiment, figure.
AZ31 magnesium alloys sample interior shear band is brilliant white in Fig. 3, and non-shear region is grey black, and shearing region and surrounding are non-
The contrast difference for shearing region is obvious, and the pattern of shear band and distribution are clear, it is easy to observe.
Embodiment 3
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed, AZ31 Mg alloy surfaces are controlled
The strain rate of sliding friction is 103s-1；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then
AZ31 magnesium alloy samples are made annealing treatment；The temperature of the annealing is 200 DEG C, and soaking time is 20min；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 4: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；The corrosive agent is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml's
Ratio is mixed, and the oxalic acid and nitric acid are AR；The time of the corrosion treatment is 30s；
Step 5: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4
And distribution.
Fig. 4 is that arrow show shear band in the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the present embodiment, figure.
AZ31 magnesium alloys sample interior shear band is brilliant white in Fig. 4, and non-shear region is grey black, and shearing region and surrounding are non-
The contrast difference for shearing region is obvious, and the pattern of shear band and distribution are more clear, it is easy to observe.
AZ31 magnesium alloys sample interior shearing region in embodiment 1, embodiment 2 and embodiment 3 by annealing
Contrast difference with non-shear region around is it is obvious that the pattern of shear band and distribution will be apparent that；Annealing temperature is from 160 DEG C
It is increased to after 200 DEG C, significant change does not occur for the density of shear band, illustrates that all shearing regions are all sent out after the annealing process
Perfect recrystallization is given birth to.
Comparative example 2
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed, AZ31 Mg alloy surfaces are controlled
The strain rate of sliding friction is 103s-1；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then
AZ31 magnesium alloy samples are made annealing treatment；The temperature of the annealing is 120 DEG C, and soaking time is 20min；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 4: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；The corrosive agent is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml's
Ratio is mixed, and the oxalic acid and nitric acid are AR；The time of the corrosion treatment is 30s；
Step 5: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4
And distribution.
Fig. 5 is that arrow show shear band in the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the present embodiment, figure.
AZ31 magnesium alloys sample interior shear band is white in Fig. 5, and non-shear region is grey, shearing region and surrounding non-shear
The contrast difference of region is not obvious enough, and the pattern of shear band and distribution are not clear enough, and observation is more difficult.
Comparative example 3
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed, AZ31 Mg alloy surfaces are controlled
The strain rate of sliding friction is 103s-1；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then
AZ31 magnesium alloy samples are made annealing treatment；The temperature of the annealing is 150 DEG C, and soaking time is 20min；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after
The surfaces of AZ31 magnesium alloy samples ground step by step, obtain the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；
Change every time after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until upper one
The cut of secondary grinding is ground off；
Step 4: corrosion treatment is carried out to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent,
Show the shear band of AZ31 magnesium alloy sample interiors；The corrosive agent is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml's
Ratio is mixed, and the oxalic acid and nitric acid are AR；The time of the corrosion treatment is 30s；
Step 5: using the pattern of the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4
And distribution.
Fig. 6 is that arrow show shear band in the shape appearance figure of AZ31 magnesium alloy sample interior shear bands in the present embodiment, figure.
AZ31 magnesium alloys sample interior shear band is brilliant white in Fig. 6, and non-shear region is canescence, and shearing region and surrounding are non-
The contrast difference for shearing region is slightly obvious, and the pattern of shear band and distribution can see clearly.
Embodiment 2, embodiment 3, comparative example 2 and comparative example 3 are compared it is known that when the temperature of annealing is less than
At 160 DEG C, the contrast difference of the shearing of AZ31 magnesium alloys sample interior region and surrounding non-shear region is not obvious enough, shear band
Pattern and be distributed it is also not clear enough；When the temperature of annealing is 200 DEG C, the fraction of AZ31 magnesium alloy sample interiors is cut
Cut band to broaden and brightness increase, if the temperature of annealing is more than 200 DEG C, more shear bands broaden, or even join together,
The pattern and distribution that shear band will be made are difficult to see clearly.Therefore, the temperature for choosing annealing is 160 DEG C~200 DEG C.
It is described above, only it is presently preferred embodiments of the present invention, any limitation is not done to the present invention, it is every according to invention skill
Any simple modification, change and equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (5)
1. a kind of observational technique to AZ31 magnesium alloy internal shear bands, it is characterised in that this method comprises the following steps：
Step 1: the surface for making AZ31 magnesium alloys using sliding friction is plastically deformed；
Step 2: being sampled to the AZ31 magnesium alloys after being plastically deformed in step one, AZ31 magnesium alloy samples are obtained, then it is right
AZ31 magnesium alloy samples are made annealing treatment；
Step 3: using 600 successively#、1000#、2000#、5000#Carborundum paper in step 2 make annealing treatment after AZ31
The surface of magnesium alloy sample is ground step by step, obtains the fine and closely woven AZ31 magnesium alloy sample observation planes of smooth, cut；Every time more
Change after carborundum paper, AZ31 magnesium alloy sample observation planar horizontals are rotated by 90 ° and are ground again, until last time grinding
Cut grind off；
Step 4: carrying out corrosion treatment to the AZ31 magnesium alloy sample observations plane obtained in step 3 using corrosive agent, make
The shear band of AZ31 magnesium alloy sample interiors shows；
Step 5: using the AZ31 magnesium alloy sample interior shear bands shown in observation by light microscope step 4 pattern and point
Cloth.
2. a kind of observational technique to AZ31 magnesium alloy internal shear bands according to claim 1, it is characterised in that step
Sliding friction strain rate described in one is 102s-1~103s-1。
3. a kind of observational technique to AZ31 magnesium alloy internal shear bands according to claim 1, it is characterised in that step
The temperature made annealing treatment described in two is 160 DEG C~200 DEG C, and soaking time is 20min.
4. a kind of observational technique to AZ31 magnesium alloy internal shear bands according to claim 1, it is characterised in that step
Corrosive agent described in four is by oxalic acid, nitric acid and water according to 5g：10ml：0.5ml ratio is mixed, and the oxalic acid and nitric acid are equal
For AR.
5. a kind of observational technique to AZ31 magnesium alloy internal shear bands according to claim 1, it is characterised in that step
The time of corrosion treatment described in four is 30s.
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| CN108588721A (en) * | 2018-05-19 | 2018-09-28 | 湖南工学院 | A kind of wrought magnesium alloy corrosive agent and the preparation method and application thereof |
| CN113802075A (en) * | 2021-10-27 | 2021-12-17 | 成都大学 | Preparation method of AZ31 magnesium alloy with high strength and ductility |
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| CN113802075A (en) * | 2021-10-27 | 2021-12-17 | 成都大学 | Preparation method of AZ31 magnesium alloy with high strength and ductility |
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| CN107219105B (en) | 2020-02-07 |
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