Digital imaging analysis of microstructures as a tool to identify local plastic deformation

Marjan Suban, Robert Cvelbar, Borut Bundara Institute of metal constructions, Mencingerjeva 7, 1001 Ljubljana, Slovenia

Abstract: This paper presents a methodology to detect plastic deformation on micro level. The analysis based on statistical data describing the morphological and crystallographic textures of a sample microstructure, obtained from an optical microscopy using digital imaging analysis. Important parameters necessary to describe a microstructure were identified as grain size and grain orientation distributions. Change in weighted product of these two parameters, grain size as area of grain and grain orientation as moment of inertia of grain can represent a measure to identify plastic deformation on small area. Demonstration of applicability was performed on a real object as part of failure analysis of ruptured pipe in thermal power plant boiler. Presented analysis leads to the fast identification of the local plastic deformation and in a case of periodical analysis of the same sample can even be used as a measure to identify creeping. Keywords: digital imaging analysis, plastic deformation, grain orientation, local deformation analysis

1 INTRODUCTION The quantification of materials microstructure is important for the evaluation of materials state and some of its properties. The size and the shape of the grains strongly influence many properties of the material. Observations of changes in geometric features of grains may be quantified by image analysis. Microscopy is powerful non-invasive tool for studying materials microstructure, especially if complemented with image analysis. The paper presents the possibilities of evaluation of elastic/plastic deformation based on microstructural grain layouts. Contrary to other researchers work our methodology of grain shape and orientation evaluation is based on moments of inertia of individual grains. When a load is applied to a material, it will cause the material to change shape. Observing effects of the process of deformation on materials microstructure using optical microscopy can be evidently seen on Fig. 1. Changes in microstructure can be easily described on grain level by using three parameters: change in grain area, shape (elongation) and orientation. New proposed methodology to evaluate these three parameters is presented below. 1.1 Digital imaging There are many imaging techniques available for viewing microstructure in 2D and thus useful in collecting images on each cross section. These imaging methods include techniques like secondary electron (SE), back-scattered electron (BSE), ion-induced secondary electron (ISE) and electron back-scatter diffraction (EBSD) (see Fig. 2). While each method generates an image in 2D, there are significant issues with some of the techniques [2]. Many laboratories are unfortunately limited to use optical microscopy as essential and only available method for microstructures evaluation. If grain boundaries are very clearly defined, computer programs could be written to take higher dimensional measurements (area and shape measurements) on digital images, but often many grain boundaries are hard to distinguish. Current state of optical recognition software offers many tools to improve image resolutions, so that grain boundaries can be easily recognized.

Figure 1:

Microstructures of the C-Mn steel (a) initial microstructure before deformation; (b) microstructures after deformation [1]

Figure 2:

Analysis of microstructure (a) optical microscopy, (b) secondary electron microscopy image, (c) EBSD [3]

1.2 Quantitative Characterization Quantitative characterization is an obvious tool for researchers to use when attempting to develop a relationship between microstructure and properties. As a result of many studies numerous different methods, philosophies, and rules have been developed. In reality the application of the characterization greatly dictates the nature of the measurement technique chosen. Often measurements are performed only in 2D using optical microscopy and digital imaging. Microstructural quantification should be designed effectively to maximize the value of the data. Almost infinite number of parameters and correlations can be used to describe microstructure, but just some of these parameters are actually important. Measurement of grain size has received the most effort of all quantifiable microstructural parameters. It is known that the grain size of a polycrystalline material is extremely important in determining its properties. Various properties exhibit correlation with grain size, such as: yield stress, ductility, and hardness [4]. Generally grain size is measured as an average scalar value such as intercept length, grain area or grain volume [5]. 1.3 Grain shape and principle axis orientation The shape of grains is likely to be of importance in a number of applications, but irregular geometries of grains in a polycrystalline microstructure make grain shape a difficult parameter to quantify. The difficulty lies in the need for data to measure the true grain shape. Usually a number of simplifying assumptions were made. Similar to the calculation of grain size, the determination of grain shape has been greatly aided by EBSD maps. The boundaries of each grain can clearly be found and measured by identifying local changes in orientation. One difference between quantifying grain shape and grain size is the inability to clearly describe shape. Grain area is a relatively straightforward measurement yielding a scalar value, while shape really needs to be described by local curvatures, which becomes more complicated and requires higher order mathematical descriptors. It is most common in everyday work to use prototypical objects to describe shape such as ellipse.

Quantification of grain shape is that done by calculation of the length of equivalent ellipse major Emax and minor axis Emin, where the area of grain is equivalent to the area of approximated ellipse. Ratio of minor axis of the equivalent ellipse to its major axis represents measure of grain roundness. Roundness is a measurement of the length width relationship, with a value in the range 0 to 1. A perfect round grain has roundness 1, while a very narrow elongated grain has roundness close to 0. In addition, many shape descriptors involve combining groups of size parameters to generate a dimensionless value like length/width (aspect ratio), area/convex area (solidity) and length/fiber length (curl) [6], which can be sometimes ambiguous. Some scalar parameters, such as moments of inertia, can do an adequate or better job of expressing grain shape and orientation. The principal axes orientation quantifies the orientation of the grains principal axes relative to the global coordinate system of cross section. It is important to distinguish between the principal axes orientation, which is the orientation referring to the principal axes and the crystal lattice (crystallographic) orientation, which is usually determined by EBSD. In a case of ellipse shown on Fig. 3 orientation is presented as angle measured counterclockwise from the horizontal axis x to the axis of lowest moment of inertia x1.

Figure 3:

Schematic representation of the grains approximation by their equivalent ellipse

2 METHODOLOGY Generally, the microstructure images suffer from defects of improper illumination, artifacts that are developed at the time of sample preparation and noise. First stage is important to achieve good segmentation classification and quantification. RGB microstructure image was then processed using tools of digital imaging with final goal to achieve image without noise, with set of individual grains, excluding border grains. For digital imaging and calculation which description follows, application called Particle analysis or Blob analysis in National Instruments IMAQ Vision software was used. Blob analysis is the process of detecting and analyzing distinct two-dimensional shapes within a region of the image. It can provide information about number, location, shape, area, perimeter, and orientation of grains. As one of main result from analyzing software is moment of inertia or second moment of area, which is a property of a cross section that can be used to predict the resistance of cross section areas to bending and deflection, around an axis that lies in the cross-sectional plane. The moments of inertia for any cross section defined as a simple polygon on x-y plane can be computed in a generic way by summing contributions from each segment of a polygon. For each segment defined by two consecutive points of the polygon, consider a triangle with two corners at these points and third corner at the origin of the coordinates. Integration by the area of that triangle and summing by the polygon segments yields: = 12
1 1 2 =1 ( 2 + +1 + +1 )

(1)

 = 12 =

1 2 =1 ( + 1 1 ( +1 24 =1

2 +1 + +1 )

(2) (3)

+ 2 + 2+1 +1 + +1 )

From this values which represents moment of inertia for x-y axis, moments of inertia for principle axis x1-y1 can be calculated (for axis presentation see Fig. 3). 1,1 =
+ 2

2 2

2 +

(4)

In this case Ix1 represent the minimum eigenvalue of moment of inertia while Iy1 maximum value. The roundness of the grain can be than calculated using ratio of these two values and it ranges from 0 (extremely elongated grain) to 1 (round grain). = 1

(5)

In equations above represents the angle of rotation of coordinate system around the grain center of mass and can be calculated using Eq. 6. It is also used as a parameter to quantify orientation of the individual grain. Correction of angle is needed to transform angles range from 0 180o to 0 90o (e.g. grain orientation for angle 1o is almost equal as for 179o).

= 2 atan

(6)

3 EXPERIMENTAL RESULTS AND DISCUSSION For the experimentation we have used many microstructure images of low carbon and austenitic stainless steel of various resolutions (i.e. magnifications) & grain shapes. These images are obtained from optical microscopy. Sample of microstructure image (magnification 500x) of austenitic stainless steel and steps of digital imaging are shown in Fig. 4.

Figure 4:

Schematic representation of steps of digital imaging and obtained calculated result for marked grain

From the Fig. 5-left present comparison of roundness calculated using ratio of equivalent ellipse axis and ratio of moment of inertia for principle axis. It is observed that second mentioned roundness is much more sensitive to grain shape then the first one. The range of calculated results is also much wider. On the right side of Fig. 5 results for examined sample on Fig. 4 are shown. From the group of diagrams it can be concluded that roundness of the grains in microstructure is around 0,46 and that median of the grains orientation angle is approximately 15o, while average value is 21o. In short it can be said, grains are elongated in direction close to horizontal axis.

1 0,9 0,8 0,7

90 80 70 60

R (ratio Ix1/Iy1)

0,6 0,5 0,4

corr.
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1

50 40 30 20 10 0 0 0,2 0,4 0,6 0,8 1

0,3
0,2 0,1

R (eq. ellipse)

Figure 5:

Correlation between calculated roundness (left) and correlation between roundness and orientation angle (right)

4 CASE STUDY Samples taken from ruptured steam pipe was marked as No. 2 and No. 4 (magnification 200x) were analyzed using above described methodology. Average value calculated roundness using Eq. 5 for sample No. 4 is 0,4, while for sample No. 2 is 0,36. As it can be seen from Fig. 6, grains in a case of sample No. 4 are more elongated then in case of sample No. 2. Similar difference can also be found when observing grain orientation angle. Grain orientation angle distribution for sample No. 4 is almost flat and median is 45o, which means that grains how no tendency in orientation. In second case median of grain orientation angle is 64o and average value 59o. This can also be observed from grains in microstructure on Fig. 6 right. 5 CONCLUSIONS In this paper, a semi-automatic digital microstructure image analysis system to qualify and quantify the microstructure mainly for steels is developed. As input into analysis process, image obtained from optical microscopy was used. In a calculation part of investigation a moment of inertia was introduced as a major parameter to quantify grain shape and orientation. The results obtained by proposed method are reproducible and repeatable. The method is robust and computationally inexpensive. It demonstrates its accuracy and its usefulness by comparing the computed values with other methods. When the proposed method will be fully developed and automated it will allow fast processing of given sample within few seconds. Presented case study on sample of ruptured steam pipe demonstrates its laboratory and industrial applications in the field of material investigations.

No.4

No. 2

90 80 70 60

90 80 70

60

corr.

corr.

50 40 30

50 40

30
20 10

20
10 0 0 0,2 0,4 0,6 0,8 1

0 0 0,2 0,4 0,6 0,8 1

Figure 6:

Position of samples No. 4 (left) and 2 (right) on ruptured steam pipe and corresponding microstructures

6 1.

2. 3.

4. 5. 6.

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