CN103529065A - Measurement method for effective grain size of structural steel with complex microstructure - Google Patents
Measurement method for effective grain size of structural steel with complex microstructure Download PDFInfo
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Abstract
The invention relates to a measurement method for the effective grain size of structural steel with a complex microstructure. The method comprises the following steps: acquiring a crystal diffraction pattern by using EBSD; measuring misorientation of crystal boundaries through the diffraction pattern and drafting a misorientation distribution curve chart; calculating threshold values of an effective grain size based on the misorientation distribution curve chart; and measuring transversal or longitudinal space between misorientation of the threshold values of the effective grain size and subjecting space data to statistical treatment so as to obtain average space between misorientation of average threshold values, wherein the average space is the effective grain size of a measured material. According to the invention, misorientation between crystal grains is used as a standard for measurement of the effective grain size, a prediction method for the threshold values of the effective grain size is brought forward, and it is convenient to formulate the threshold values of the effective grain size according to specific conditions of the material.
Description
Technical field
The present invention relates to crystallite dimension fields of measurement, be specifically related to a kind of method of measuring the effective particle size of complicated heterogeneous microstructure steel.
Background technology
In order to improve the obdurability of material, usually ferrous materials is designed to have multiple phase or the compound complicated heterogeneous microstructure of Various Tissues type.Soft phase and firmly guarantee respectively mutually plasticity and the intensity that material is good in material, soft or hard cooperatively interacts mutually, utilizes mobile dislocations a large amount of in organizing and full of twists and turns crystal boundary, makes material have good crack arrest characteristic.Because various organization feature in this class material is not obvious, grain shape very irregular, crystal boundary is unintelligible, and grain contours impalpable has brought very large difficulty to the tissue typing of this class material and the measurement of crystallite dimension.On the other hand, utilize the crystallite dimension of pattern unit definition and the relevance of performance bad, the crystallite dimension that classic method records can not characterize the tissue signature of this type of material.Just because of diversity and the complicacy of this class ferrous materials tissue, traditional quantitative technique can not meet its requirement.
Owing to thering is the good combination property of complicated heterogeneous microstructure steel, in recent years in transportation pipe lineman journey, construction(al)steel field, high-altitude and boats and ships are weather-proof has obtained increasing application with fields such as steel, tissue characterization's parameter of these class steel need to be proposed, particularly with its intensity, plasticity and toughness closely-related " effective particle size ", have research and development, quality testing evaluation and the quality control demand of complicated heterogeneous microstructure steel to meet.
Summary of the invention
In order to solve above technical matters, the invention provides a kind of method of measuring the effective particle size of complicated heterogeneous microstructure steel, the method has been filled up the blank to complicated heterogeneous microstructure steel effective particle size threshold values Forecasting Methodology in prior art, has solved complicated heterogeneous microstructure steel and has been difficult to the problem of measuring because of diversity and the effective particle size threshold values that causes of complicacy of tissue.
The method is achieved through the following technical solutions:
A method for the effective particle size of complicated heterogeneous microstructure steel, comprises the steps:
By EBSD, gather crystal diffraction style;
By described crystal diffraction style, measure grain boundary orientation, draw grain boundary orientation angular distribution curve map;
According to described grain boundary orientation angular distribution curve map, calculate effective particle size threshold values;
Measure transversal spacing and the vertical spacing of cutting between effective particle size threshold values, the spacing data of measuring is carried out to statistical treatment, the average headway obtaining between effective particle size threshold values misorientation is the effective particle size of measuring material.
In technique scheme, the described step according to described grain boundary orientation angular distribution curve map calculating effective particle size threshold values is as follows:
When grain boundary orientation distribution curve meets orientation stochastic distribution curve, the threshold values that 15 ° of grain boundary orientation angle critical values are effective particle size;
When grain boundary orientation distribution curve departs from stochastic distribution curve and occurred the peak of misorientation angular distribution before 15 °, the frequency occurring according to misorientation distribution peak, choose the misorientation angle under respective frequencies, be the concentrated value of misorientation that texture causes, then according to the concentrated value of this misorientation, select the threshold values of effective particle size;
When grain boundary orientation distribution curve departs from stochastic distribution curve and occurred the peak of misorientation angular distribution and when 20～45 ° of misorientation angular distribution are lower, determine effective particle size threshold values according to the crystal boundary value that occurs turning point on Fracture Profile in Metallic Materials cleavage plane unit and On Crack Propagation path before 15 °;
In technique scheme, according to the crystal boundary value that occurs turning point on Fracture Profile in Metallic Materials cleavage plane unit and On Crack Propagation path, determine that the step of effective particle size threshold values is as follows:
Step 1: analytic target material is carried out to low temperature Charpy-type test, obtain the fracture of material fragility fracture;
Step 2: adopt EBSD to analyze the Crack Extension path of fracture, it is poor that acquisition is distributed in the grain orientation of crackle both sides, and set up crackle both sides grain orientation declinate degree distribution table;
Step 3: according to corresponding different grain orientation declinate degree in the grain-oriented crystal boundary contrast contrast figure of fracture and misorientation angular distribution table, analyze the impact of crackle both sides crystal grain On Crack Propagation;
During crackle generation deviation, the minimum value of corresponding grain orientation declinate degree is the threshold values of effective particle size evaluation.
In technique scheme, described low temperature Charpy-type test, at-160～-200 ℃ of temperature, is carried out according to GB/T229-20074 standard.
In technique scheme, the transversal spacing between described measurement effective particle size threshold values and the vertical transversal number of times that cuts spacing are got minimum transversal number of times.
In technique scheme, described minimum transversal number of times is to meet the transversal number of times that the smallest grain size of effective particle size threshold values requirement obtains as transversal spacing.
A device for the effective particle size of complicated heterogeneous microstructure steel, comprising:
Acquisition module, gathers crystal diffraction style by EBSD;
Drafting module, measures grain boundary orientation by described crystal diffraction style, draws grain boundary orientation angular distribution curve map;
Computing module, calculates effective particle size threshold values according to described grain boundary orientation angular distribution curve map;
Measurement module, measures transversal spacing and the vertical spacing of cutting between effective particle size threshold values;
Statistical module, carries out statistical treatment to the spacing data of measuring, and the average headway obtaining between effective particle size threshold values misorientation is the effective particle size of measuring material.
The invention solves complicated heterogeneous microstructure structure of steel complexity various, crystal grain is difficult to the difficulty of distinguishing and measuring.By EBSD, gather crystal diffraction style and measure grain boundary orientation angle, solved the measurement problem of complicated crystalline granular texture, according to measurement result, draw misorientation angular distribution curve map, the grain boundary orientation angular distribution curve map of summing up in conjunction with the present invention according to the concrete condition of material misorientation angular distribution curve again calculates effective particle size threshold values, makes the measurement intuitive and convenient of the effective particle size of complicated heterogeneous microstructure steel.
Accompanying drawing explanation
Sample surfaces after the steel sample electropolishing that Fig. 1 provides for the embodiment of the present invention.
Crystal boundary contrast (Band Contrast) the contrast figure (black line represents wide-angle misorientation crystal boundary, and white wire represents low-angle misorientation crystal boundary) on orientation mapping figure sample crystal diffraction surface before noise reduction that Fig. 2 provides for the embodiment of the present invention.
Sample surfaces crystal boundary contrast (Band Contrast) contrast figure (only showing wide-angle misorientation crystal boundary) after the orientation mapping figure noise that Fig. 3 provides for the embodiment of the present invention drops to zero.
The grain boundary orientation angular distribution figure of the steel sample that Fig. 4 a provides for the embodiment of the present invention.
Spacing between 16 ° of misorientations of the steel sample that Fig. 4 b provides for the embodiment of the present invention.
Steel sample and sample coordinate system location diagram that Fig. 5 provides for the embodiment of the present invention.
The orientation stochastic distribution curve map that Fig. 6 provides for the embodiment of the present invention.
Each interregional misorientation distribution plan of Crack Extension edge one side that Fig. 7 provides for the embodiment of the present invention.
The effective particle size that Fig. 8 provides for the embodiment of the present invention and the graph of a relation of yield strength.
Embodiment
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in detail.
Embodiment is used material for X80 level large deformation straight-line joint submerged arc welding tube line steel pipe.
Sample intercepting: intercepting 10 * 5 * 3 (mm apart from 90 ° of body central cores of welded tube welding seam with wire cutting method
3) sample of size, when measuring, the long limit of 10mm is parallel to sample coordinate system RD direction, and the minor face of 5mm is parallel to sample coordinate system TD direction, and the minor face of 3mm is parallel to sample coordinate system ND direction (referring to accompanying drawing 5).Measurement face is selected the face vertical with TD direction, is called TD face, and measurement face is of a size of 10 * 3 (mm
2).
With No. 600 waterproof abrasive papers, each cross section of sample is polished, with No. 600, No. 800, No. 1000, No. 1200, No. 1500, No. 2000 waterproof abrasive papers will be measured face and polish step by step, when the left corase grind trace of front one sand paper does not observe completely, change a thin sand paper, the direction of flour milling grinding is should be with last sand paper mark direction in 90 ° or 45 °.Because pipe line steel be take ferrite as subject organization, more easily carry out electropolishing, adopt YJ63 DC current regulator power supply (Shanghai Hu Guang instrument plant) face to be measured to be carried out to electropolishing, polishing fluid: 5%HClO
4+ 95% alcohol, polishing electric current: 0.8mA, polishing voltage: 20～30V, polishing time: 40s, cleaning fluid: methyl alcohol, wash number: 3 times, drying mode: cold wind dries up, storing mode: monox exsiccator, storage time: be less than 24h.Sample surfaces state as shown in Figure 1.
Utilize the HKL Channel5 software of the hot field emission scanning electron microscope of ZEISS SUPER55 type and Oxford company to carry out orientation mapping analysis to measurement face.Enlargement factor: 500 times, measure area: 965 * 724 (μ m
2), scanning stride: 0.24 μ m, number of scan points: 698660 points, demarcation mode: bandwidth is demarcated, demarcates band number: 4～8 bands, resolution factor: 83.91.Contrast figure as shown in Figure 2 in crystal boundary contrast (Band Contrast).
Utilize HKL Channel5 software to carry out noise reduction process to MAP figure, contrast figure as shown in Figure 3 for the crystal boundary contrast (Band Contrast) after noise reduction.
Misorientation angular distribution figure is as shown in accompanying drawing 4a, obvious offset alignment stochastic distribution curve, known untextured orientation stochastic distribution curve (seeing accompanying drawing 6), and before 15 °, occur the peak of misorientation angular distribution and 20～45 ° of misorientation angular distribution lower, so determine effective particle size threshold values according to the crystal boundary value that occurs turning point on Fracture Profile in Metallic Materials cleavage plane unit and On Crack Propagation path.
Material is carried out to Charpy-type test according to GB/T229-20074 standard at-196 ℃, obtain the fracture of material fragility fracture;
In the Crack Extension district of Materials Fracture, carry out EBSD test and obtain the poor misorientation table (in Table 1) of listing of crackle both sides grain orientation, determine that effective particle size threshold values is 16 °.Analysis result is as follows: the orientation contrast analysis result at Crack Extension edge and Crack Extension through the misorientation between region as shown in Fig. 7 and table 1, when the misorientation in two regions surpasses 16 °, Crack Extension path deflects, broken line advances, when misorientation is less than 16 °, the expansion of the direct straight line of crackle is by this region, and the misorientation that shows crystal grain can effectively hinder Crack Extension while surpassing 16 °, therefore using 16 ° of angle threshold values as Effective grain size misorientation.
Each interregional misorientation table of table 1 Crack Extension edge
Utilize HKL Channel5 software to measure 16 ° of misorientation spacing (seeing accompanying drawing 4b) to misorientation angular distribution figure, transversal direction is parallel to RD direction, transversal number is 200 (transversal direction and number are set in software), 8853 16 ° of misorientation spacing data are derived, these data are averaged, and the effective particle size that can obtain this material is 4.8615 μ m.
Adopt the definite effective particle size assessment method of this patent, the Effective grain size of X80 pipe line steel is evaluated, the relation of the effective particle size of setting up and material yield intensity meets Hall-Petch relation, meets σ
y=σ
0+ k
yd
-1/2.The value drawing according to this assessment method is drawn the graph of a relation of effective particle size and yield strength, obtains linear relationship chart σ
y=726+29.11*D
-1/2, σ wherein
0≈ 726MPa, k
y≈ 29.11Nmm-3/2, σ
yfor the yield strength (can measure) of material, D is the effective particle size of measuring according to the described method of invention, as shown in Figure 8.The definite effective particle size assessment method of visible this patent is the reliable and effective method that meets Hall-Petch relation.
It should be noted last that, above embodiment is only in order to implementer's case of this material to be described and unrestricted, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (7)
1. a method of measuring the effective particle size of complicated heterogeneous microstructure steel, is characterized in that: comprise the steps:
By EBSD, gather crystal diffraction style;
By described crystal diffraction style, measure grain boundary orientation, draw grain boundary orientation angular distribution curve map;
According to described grain boundary orientation angular distribution curve map, calculate effective particle size threshold values;
Measure transversal spacing and the vertical spacing of cutting between effective particle size threshold values, the spacing data of measuring is carried out to statistical treatment, the average headway obtaining between effective particle size threshold values misorientation is the effective particle size of measuring material.
2. the method for the effective particle size of the complicated heterogeneous microstructure steel of measurement as claimed in claim 1, is characterized in that: described according to described grain boundary orientation angular distribution curve map, to calculate the step of effective particle size threshold values as follows:
When grain boundary orientation distribution curve meets orientation stochastic distribution curve, the threshold values that 15 ° of grain boundary orientation angle critical values are effective particle size;
When grain boundary orientation distribution curve departs from stochastic distribution curve and occurred the peak of misorientation angular distribution before 15 °, the frequency occurring according to misorientation distribution peak, choose the misorientation angle under respective frequencies, be the concentrated value of misorientation that texture causes, then according to the concentrated value of this misorientation, select the threshold values of effective particle size;
When grain boundary orientation distribution curve departs from stochastic distribution curve and occurred the peak of misorientation angular distribution and when 20～45 ° of misorientation angular distribution are lower, determine effective particle size threshold values according to the crystal boundary value that occurs turning point on Fracture Profile in Metallic Materials cleavage plane unit and On Crack Propagation path before 15 °.
3. the method for the effective particle size of the complicated heterogeneous microstructure steel of measurement as claimed in claim 1, is characterized in that: according to the crystal boundary value that occurs turning point on Fracture Profile in Metallic Materials cleavage plane unit and On Crack Propagation path, determine that the step of effective particle size threshold values is as follows:
Step 1: analytic target material is carried out to low temperature Charpy-type test, obtain the fracture of material fragility fracture;
Step 2: adopt EBSD to analyze the Crack Extension path of fracture, it is poor that acquisition is distributed in the grain orientation of crackle both sides, and set up crackle both sides grain orientation declinate degree distribution table;
Step 3: according to corresponding different grain orientation declinate degree in the grain-oriented crystal boundary contrast contrast figure of fracture and misorientation angular distribution table, analyze the impact of crackle both sides crystal grain On Crack Propagation;
During crackle generation deviation, the minimum value of corresponding grain orientation declinate degree is the threshold values of effective particle size evaluation.
4. the method for the effective particle size of the complicated heterogeneous microstructure steel of measurement as claimed in claim 3, is characterized in that: described low temperature Charpy-type test, at-160～-200 ℃ of temperature, is carried out according to GB/T229-20074 standard.
5. the method for the effective particle size of the complicated heterogeneous microstructure steel of measurement as claimed in claim 1, is characterized in that: the transversal spacing between described measurement effective particle size threshold values and the vertical transversal number of times that cuts spacing are got minimum transversal number of times.
6. the method for the effective particle size of the complicated heterogeneous microstructure steel of measurement as claimed in claim 5, is characterized in that: described minimum transversal number of times is to meet the transversal number of times that the smallest grain size of effective particle size threshold values requirement obtains as transversal spacing.
7. a device of measuring the effective particle size of complicated heterogeneous microstructure steel, is characterized in that, comprising:
Acquisition module, gathers crystal diffraction style by EBSD;
Drafting module, measures grain boundary orientation by described crystal diffraction style, draws grain boundary orientation angular distribution curve map;
Computing module, calculates effective particle size threshold values according to described grain boundary orientation angular distribution curve map;
Measurement module, measures transversal spacing and the vertical spacing of cutting between effective particle size threshold values;
Statistical module, carries out statistical treatment to the spacing data of measuring, and the average headway obtaining between effective particle size threshold values misorientation is the effective particle size of measuring material.
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| CN108181170A (en) * | 2017-12-27 | 2018-06-19 | 北京北冶功能材料有限公司 | Steel material crackle forms the stretching fracture determination method of period |
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| CN111537319A (en) * | 2020-06-15 | 2020-08-14 | 马鞍山钢铁股份有限公司 | Method for measuring pearlite steel ball size |
| CN113884521A (en) * | 2021-08-24 | 2022-01-04 | 中国科学院金属研究所 | Method for predicting selection difficulty of phase transition body at grain boundary of titanium alloy |
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| CN104111261A (en) * | 2014-06-30 | 2014-10-22 | 中国石油天然气集团公司 | Measuring method and apparatus for effective grain size of ultrafine lath structure low alloy steel |
| CN105181536A (en) * | 2015-09-25 | 2015-12-23 | 武汉钢铁(集团)公司 | Pearlite steel wire rod austenitic grain size measuring method |
| CN107358005A (en) * | 2017-07-24 | 2017-11-17 | 哈尔滨工业大学 | FEM model modeling method based on true heterogeneous microstructure SEM EBSD images |
| CN107677232A (en) * | 2017-09-21 | 2018-02-09 | 京东方科技集团股份有限公司 | A kind of crystallite dimension measuring method and device, the production method of polysilicon membrane |
| US10605596B2 (en) | 2017-09-21 | 2020-03-31 | Boe Technology Group Co., Ltd. | Method and apparatus for measuring a size of a crystal grain, and method for fabricating a poly-silicon thin film |
| CN107677232B (en) * | 2017-09-21 | 2020-03-31 | 京东方科技集团股份有限公司 | Method and device for measuring grain size and method for producing polycrystalline silicon film |
| CN108181170A (en) * | 2017-12-27 | 2018-06-19 | 北京北冶功能材料有限公司 | Steel material crackle forms the stretching fracture determination method of period |
| CN108181170B (en) * | 2017-12-27 | 2020-01-24 | 北京北冶功能材料有限公司 | Tensile fracture judgment method for steel material in crack formation period |
| CN109283103A (en) * | 2018-10-31 | 2019-01-29 | 首钢集团有限公司 | A kind of display methods of mild steel quenching state original austenite crystal prevention |
| CN111537319A (en) * | 2020-06-15 | 2020-08-14 | 马鞍山钢铁股份有限公司 | Method for measuring pearlite steel ball size |
| CN113884521A (en) * | 2021-08-24 | 2022-01-04 | 中国科学院金属研究所 | Method for predicting selection difficulty of phase transition body at grain boundary of titanium alloy |
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