CN105388174A - Method for evaluating microcrack initiation of magnesium alloy - Google Patents
Method for evaluating microcrack initiation of magnesium alloy Download PDFInfo
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- CN105388174A CN105388174A CN201510725436.1A CN201510725436A CN105388174A CN 105388174 A CN105388174 A CN 105388174A CN 201510725436 A CN201510725436 A CN 201510725436A CN 105388174 A CN105388174 A CN 105388174A
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Abstract
The invention discloses a method for evaluating microcrack initiation of magnesium alloy. The method includes the following steps that an in-situ tension method is adopted for acquiring the data of an in-situ scanning electron microscope (SEM) and the data of in-situ electron back scattering diffraction (EBSD); according to the data of the in-situ SEM and the data of the in-situ EBSD, the eulerian angles representing grain orientation information are acquired; in accordance with the eulerian angles, the crack initiation parameter F1 is calculated, and the possible microcrack initiation position is predicted. According to the method for evaluating the microcrack initiation of the magnesium alloy, the in-situ EBSD method is adopted so that slipping and twinning information in grains and microcrack initiation in the uniaxial drawing process of the magnesium alloy can be observed dynamically; the correlation between microcrack initiation on the grain boundary and the orientation and stress direction of surrounding grains can be evaluated comprehensively through calculation of the crack initiation parameter F1; the nucleation and the happening position of microcracks can be accurately predicted through calculation of the F1 value, and it is of great significance to improve the plasticity of the magnesium alloy.
Description
Technical field
The present invention relates to technical field of measurement and test, particularly a kind of method of evaluating magnesium alloy microcrack initiation.
Background technology
At present, for main with fracture failure in all kinds of inefficacies of metal material, endanger maximum.And crackle is the prelude of fracture failure.So the germinating position of prediction micro-crack has great significance for the fracture failure caused because of crackle.
Existing research for fracture behaviour has two kinds of diverse ways.Be a method for fracturing mechanics, it is Elasticity according to metal and elastic plastic theory, and a kind of method studying fracture behaviour considered material internal to have defect and set up.Another is the method for metal physics, from the microstructure of material, microdefect, even studies the method for fracture behaviour from the yardstick of molecule and atom.The research method of fracturing mechanics compares and is applicable to there is obvious macroscopic cracking analysis.
The current generation for magnesium alloy materials micro-crack and the inefficacy caused thereof, existing research means has distorted area employing ion beam gridding (FIB), the impact of local train on micro-crack is analyzed by drawing strain cloud atlas to distortion of the mesh degree, but the size that the method discusses grain boundaries local train affects micro-crack, do not consider crystal boundary surrounding grains orientation, the impact of twin and slippage.
Summary of the invention
The present invention is directed to above-mentioned problems of the prior art, a kind of method of evaluating magnesium alloy microcrack initiation is proposed, can realize observing and quantitative evaluation from meso-scale (crystal grain in and intercrystalline) magnesium alloy microcrack initiation, the generation position of prediction crystal boundary micro-crack thus the Materials Fracture that prevention causes because of micro-crack extension lost efficacy.
For solving the problems of the technologies described above, the present invention is achieved through the following technical solutions:
The invention provides a kind of method of evaluating magnesium alloy microcrack initiation, it comprises the following steps:
S11: the method adopting original position stretching, obtains the data of in-situ scanning Electronic Speculum (SEM) and original position Electron Back-Scattered Diffraction (EBSD);
S12: according to the data of described in-situ scanning Electronic Speculum and original position Electron Back-Scattered Diffraction, obtains the Eulerian angle representing grain orientation information;
S13: according to described Eulerian angle, calculates crack initiation parameter F1, the position that prediction micro-crack may germinate.
For the germinating of micro-crack and the observation of expansion and research, need to adopt and can be out of shape while the means of home position observation material microscopic appearance, and original position SEM and original position EBSD can follow the tracks of the deformational behavior of tens to one hundred crystal grain from meso-scale (crystal grain interior and intercrystalline).Original position SEM can capture the generation of micro-crack and the situation of expansion, and the observation of original position EBSD can provide the information of grain orientation and twin, and the convenient crystal grain environment analyzed around crackle affects it.The calculating of crack initiation parameter F1 can quantitative analysis crack initiation and surrounding grains orientation, and the relation in twin reciprocation and applied stress direction, plays an important role to the prediction of microcrack initiation position.
The people such as Bieler define crack initiation parameter (fip), and find that crack initiation parameter F1 value can assess TiAl alloy crack initiation situation well; The people such as Fallahi, A, Kumar, D have added up the F1 value of TiAl alloy great number of grains group, found that the F1 value of the crystal grain of crackle that has of 98% is greater than full die, and will test the crystal grain group of Ti alloy further.
At present, crack initiation parameter F1 value is adopted also not to be used to the method that grain boundaries crackle is predicted same with slippage and the twin Mg alloy for main deformation mechanism, therefore the inventive method has used for reference the research method of other metal materials to crackle, in conjunction with the deformation characteristics of magnesium alloy, propose a kind of computing method of brand-new evaluating magnesium alloy microcrack initiation.
Preferably, described step S11 specifically comprises the following steps:
S111: prepare original position stretching sample;
S112: surface treatment is carried out to original position stretching sample;
S113: carry out original position stretching experiment, obtains scanning electron microscopy picture and the Electron Back-Scattered Diffraction image of distorted area under same deflection.
Preferably, described step S111 is specially: carry out Linear cut to magnesium alloy, is processed into the drawing sheet of sheet.
Preferably, described step S112 is specially: original position stretching sample is polished, polishing, corrosion and oven dry.
Preferably, the polishing in described step S112 is specially: adopt 800,1200, No. 4000 silicon carbide papers to polish to described original position stretching sample successively, and the time of each step is 1min.
Preferably, polishing in described step S112 is specially: employing granularity is the oil base diamond suspension of 6 μm, 3 μm, 1 μm successively, then adopt granularity to be that the silica gel solution of 0.05 μm carries out polishing to described original position stretching sample, the time is followed successively by 12min, 5min, 5min, 8min.
Preferably, the ratio of the corrosive liquid that the corrosion in described step S112 adopts is: 5ml nitric acid, 15ml acetic acid, 60ml alcohol and 20ml water, and etching time is 1 ~ 2s.
Preferably, described step S113 is specially: described step S113 is specially: be arranged on the fixture of drawing stand by described original position stretching sample, make the cushion block inclination predetermined angle below described fixture, when keeping carrying out unilateral stretching when not unloading, obtain the scanning electron microscope image of distorted area under same deflection and electron backscattered image K-M simultaneously.
Preferably, described step S13 is specially: the computing formula of microcrack initiation parameter is:
Wherein: m
slip/twrepresent the maximum schimidfactor of twin or slip band in this group crystal grain,
represent m
slip/twcorresponding unit Bai Shi vector,
represent drawing stress direction,
represent the unit Bai Shi vector of two neighboring die residue dislocations.
Compared to prior art, the present invention has the following advantages:
(1) method of evaluating magnesium alloy microcrack initiation provided by the invention, in conjunction with original position stretching method and crack initiation parameter, original position stretching method dynamically can to observe in magnesium alloy original position stretching process slippage and twin information and microcrack initiation in crystal grain, the microcrack initiation parameter comprehensive evaluation correlativity of the germinating of grain boundaries micro-crack and the orientation of surrounding grains and stress direction, F1 value supplements the Nucleation Mechanism of crackle, can predict the forming core of micro-crack and the position of generation;
(2) the present invention can evaluate from meso-scale magnesium alloy microcrack initiation, crack initiation parameter comprises three partial geometry parameters, discuss the schimidfactor corresponding to grain orientation fully, in the residue dislocation of neighboring die and crystal grain, slippage and twin reciprocation and stress direction are on the impact of microcrack initiation, and energy quantitative description, the generation position of crackle can be predicted as more accurately, most important to the moulding raising of magnesium alloy.
Certainly, implement arbitrary product of the present invention might not need to reach above-described all advantages simultaneously.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, embodiments of the present invention are described further:
Fig. 1 is the process flow diagram of the method for evaluating magnesium alloy microcrack initiation of the present invention;
Fig. 2 is the force-displacement curve in original position stretching process of the present invention;
Fig. 3 of the present inventionly to interact the grain-boundary crack schematic diagram germinated due to twin or slippage.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Composition graphs 1-Fig. 3, be described in detail the method for evaluating magnesium alloy microcrack initiation of the present invention, be illustrated in figure 1 its process flow diagram, it comprises the following steps:
S11: the method adopting original position stretching, obtains the data of in-situ scanning Electronic Speculum (SEM) and original position Electron Back-Scattered Diffraction (EBSD);
S12: by OIM software, according to the data of in-situ scanning Electronic Speculum (SEM) and original position Electron Back-Scattered Diffraction (EBSD), obtains the Eulerian angle representing grain orientation information;
S13: according to Eulerian angle, is calculated three partial geometry parameters of composition F1 value, thus calculates crack initiation parameter (fip) F1 by mathematical relation, the position that prediction micro-crack may germinate.
Wherein: step S11 specifically comprises the following steps:
S111: by the drawing sheet of magnesium alloy plate Linear cut slabbing, as original position stretching sample;
S112: original position stretching sample is processed;
Drawing sheet is pasted onto corase grind and fine grinding on automatic polishing machine on rosette, the grinding turn of employing is 80,1200, No. 4000 silicon carbide papers, and the time controling of each step is at 1min;
Automatic polishing machine adopts polishing cloth mechanical buffing, polishing order for granularity be the oil base diamond suspension of 6 μm, 3 μm and 1 μm, then employing granularity is the silica gel solution of 0.05 μm, and polishing time is followed successively by 12min, 5min, 5min and 8min;
Fast erosion in corrosive liquid, corrosive liquid is the mixed liquor of 5ml nitric acid, 15ml acetic acid, 60ml alcohol and 20ml water, and etching time is 1 ~ 2s, dries up after corrosion, is then placed in dry container.
S113: carry out original position stretching experiment, obtains the SEM information and EBSD information of agreeing to distorted area under deflection;
The original position stretching sample of above-mentioned process is arranged on above the fixture of drawing stand, guarantees the cushion block pre-tilt predetermined angle below fixture, EBSD image can be obtained while obtaining SEM image; Start extensometer, needing the deformation displacement point observed to press time-out, the force-displacement curve in original position deformation process and the position of intermediate suspension as shown in Figure 1, can obtain SEM information and the EBSD information of crystal grain simultaneously when keeping not unloading force.
Step S13 is specially: adopt OIM software to obtain the EBSD image corresponding to the SEM image of the germinating grain-boundary crack obtained in step S12 and represent grain-oriented three Eulerian angle; The computing formula of microcrack initiation parameter is:
Wherein: m
slip/twrepresent the maximum schimidfactor of twin or slip band in this group crystal grain,
represent m
slip/twcorresponding unit Bai Shi vector,
represent drawing stress direction,
represent the unit Bai Shi vector of adjacent two crystal grain residue dislocation.As Fig. 3 to interact the grain-boundary crack schematic diagram germinated due to twin or slippage, wherein: F1 is the product of three parts, Part I is m
slip/tw, this part defines the twin or the slippage that cause grain boundaries to produce maximum discontinuous detrusion; Part II is m
slip/twcorresponding unit Bai Shi vector
with drawing stress direction
dot product, this part define twin or slippage interact near grain-boundary strength; Part III is m
slip/twcorresponding unit Bai Shi vector
with the unit Bai Shi vector of the residue dislocation of adjacent two crystal grain
dot product sum, this part defines the degree that detrusion that is twin or slippage can coordinate dislocation motion around.F1 value is larger, represents that the possibility of the grain boundaries crack initiation that this crystal grain is right is larger.By F1 achieve quantitative evaluation magnesium alloy in position in deformation process intercrystalline be slippage or twin, the residue dislocation of neighboring die and the relation in applied stress direction in the germinating of crackle and crystal grain, from meso-scale, magnesium alloy microcrack initiation is evaluated, can be used for predicting the Materials Fracture inefficacy that the generation position thus prevent of crystal boundary micro-crack causes because of Crack Extension.
The calculating of crack initiation parameter F1 can, by writing matlab program, only need input to represent grain-oriented Eulerian angle information, by mathematical relation, obtains the three partial geometry parameters forming F1 value, then obtains the result of calculation of F1, more easily realize.
Disclosed herein is only the preferred embodiments of the present invention, and this instructions is chosen and specifically described these embodiments, and being to explain principle of the present invention and practical application better, is not limitation of the invention.The modifications and variations that any those skilled in the art do within the scope of instructions, all should drop in scope that the present invention protects.
Claims (9)
1. a method for evaluating magnesium alloy microcrack initiation, is characterized in that, comprises the following steps:
S11: the method adopting original position stretching, obtains the data of in-situ scanning Electronic Speculum and original position Electron Back-Scattered Diffraction;
S12: according to the data of described in-situ scanning Electronic Speculum and original position Electron Back-Scattered Diffraction, obtains the Eulerian angle representing grain orientation information;
S13: according to described Eulerian angle, calculates crack initiation parameter F1, the position that prediction micro-crack may germinate.
2. the method for evaluating magnesium alloy microcrack initiation according to claim 1, it is characterized in that, described step S11 specifically comprises the following steps:
S111: prepare original position stretching sample;
S112: surface treatment is carried out to original position stretching sample;
S113: carry out original position stretching experiment, obtains scanning electron microscopy picture and the Electron Back-Scattered Diffraction image of distorted area under same deflection.
3. the method for evaluating magnesium alloy microcrack initiation according to claim 2, it is characterized in that, described step S111 is specially: carry out Linear cut to magnesium alloy, is processed into the drawing sheet of sheet.
4. the method for evaluating magnesium alloy microcrack initiation according to claim 3, it is characterized in that, described step S112 is specially: original position stretching sample is polished, polishing, corrosion and oven dry.
5. the method for evaluating magnesium alloy microcrack initiation according to claim 4, it is characterized in that, polishing in described step S112 is specially: adopt 800,1200, No. 4000 silicon carbide papers to polish to described original position stretching sample successively, and the time of each step is 1min.
6. the method for evaluating magnesium alloy microcrack initiation according to claim 4, it is characterized in that, polishing in described step S112 is specially: employing granularity is the oil base diamond suspension of 6 μm, 3 μm, 1 μm successively, then adopt granularity to be that the silica gel solution of 0.05 μm carries out polishing to described original position stretching sample, the time is followed successively by 12min, 5min, 5min, 8min.
7. the method for evaluating magnesium alloy microcrack initiation according to claim 4, is characterized in that, the ratio of the corrosive liquid that the corrosion in described step S112 adopts is: 5ml nitric acid, 15ml acetic acid, 60ml alcohol and 20ml water, and etching time is 1 ~ 2s.
8. the method for evaluating magnesium alloy microcrack initiation according to claim 2, it is characterized in that, described step S113 is specially: be arranged on the fixture of drawing stand by described original position stretching sample, make the cushion block inclination predetermined angle below described fixture, when keeping carrying out unilateral stretching when not unloading, obtain the scanning electron microscope image of distorted area under same deflection and electron backscattered image K-M simultaneously.
9. the method for evaluating magnesium alloy microcrack initiation according to claim 1, it is characterized in that, described step S13 is specially: the computing formula of microcrack initiation parameter is:
Wherein, Part I: m
slip/twrepresent the maximum schimidfactor of twin or slip band in this group crystal grain, this part defines the twin or the slippage that cause grain boundaries to produce maximum discontinuous detrusion; Part II:
represent m
slip/twcorresponding unit Bai Shi vector,
represent drawing stress direction, this part defines the grain-boundary strength near twin or slippage interaction; Part III:
represent the unit Bai Shi vector of adjacent two crystal grain residue dislocation.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106198226A (en) * | 2016-09-19 | 2016-12-07 | 中国科学院地质与地球物理研究所 | In conjunction with the method that EBSD technology characterizes crystal grain strain in situ |
| CN106289975A (en) * | 2016-08-12 | 2017-01-04 | 上海电气电站设备有限公司 | The test method of material domain fracture toughness |
| CN108857132A (en) * | 2018-07-24 | 2018-11-23 | 哈尔滨工业大学（深圳） | A kind of assessment Lead-Free Solder Joint reliability method |
| CN109596657A (en) * | 2018-11-29 | 2019-04-09 | 石家庄铁道大学 | High-speed EMUs EEF bogie moving component early defect extensive diagnostic method |
| CN110702497A (en) * | 2019-09-09 | 2020-01-17 | 中国航发北京航空材料研究院 | Method for predicting crack initiation position or propagation direction of metal surface |
| CN113358678A (en) * | 2021-05-11 | 2021-09-07 | 哈尔滨工业大学（深圳） | Semi-quantitative prediction and visualization method for mesoscopic stress and texture in alpha titanium deformation process |
| CN113504127A (en) * | 2021-07-09 | 2021-10-15 | 浙江省特种设备科学研究院 | In-situ stretching method for evaluating crack propagation of high-temperature nickel-based alloy with prefabricated notch |
| CN115372135A (en) * | 2022-08-10 | 2022-11-22 | 国标（北京）检验认证有限公司 | Method for measuring rotation angle of high-temperature alloy crystal grain |
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| CN106289975A (en) * | 2016-08-12 | 2017-01-04 | 上海电气电站设备有限公司 | The test method of material domain fracture toughness |
| CN106289975B (en) * | 2016-08-12 | 2020-01-21 | 上海电气电站设备有限公司 | Method for testing fracture toughness of material micro-area |
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| CN108857132A (en) * | 2018-07-24 | 2018-11-23 | 哈尔滨工业大学（深圳） | A kind of assessment Lead-Free Solder Joint reliability method |
| CN109596657A (en) * | 2018-11-29 | 2019-04-09 | 石家庄铁道大学 | High-speed EMUs EEF bogie moving component early defect extensive diagnostic method |
| CN110702497A (en) * | 2019-09-09 | 2020-01-17 | 中国航发北京航空材料研究院 | Method for predicting crack initiation position or propagation direction of metal surface |
| CN110702497B (en) * | 2019-09-09 | 2022-04-19 | 中国航发北京航空材料研究院 | Method for predicting crack initiation position or propagation direction of metal surface |
| CN113358678A (en) * | 2021-05-11 | 2021-09-07 | 哈尔滨工业大学（深圳） | Semi-quantitative prediction and visualization method for mesoscopic stress and texture in alpha titanium deformation process |
| CN113504127A (en) * | 2021-07-09 | 2021-10-15 | 浙江省特种设备科学研究院 | In-situ stretching method for evaluating crack propagation of high-temperature nickel-based alloy with prefabricated notch |
| CN115372135A (en) * | 2022-08-10 | 2022-11-22 | 国标（北京）检验认证有限公司 | Method for measuring rotation angle of high-temperature alloy crystal grain |
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