Analysis of Slip Systems in Nickel

Superalloy by Micro Laue Diffraction

Project Advisor: Jennifer Carter | Author: Aaron Thompson
Case Western Reserve University
December 2015

Summary
The proposed project entails the analysis of slip systems in nickel superalloy via
analysis of the shape of Laue diffraction peaks. The objective is to develop a process to
measure the localization of deformation as well as the slip systems active.
It has been observed qualitatively that deformation is distributed according to the
nature of grain boundaries as well as distance from grain boundaries through in-situ
TEM analysis. Under elevated temperature creep conditions it was found that the areas
of most significant deformation accumulation experienced slip along multiple planes.
There were also grain boundaries that experienced grain boundary sliding (GBS) which
were found to only experience single slip [1]. With both dislocation motion and grain
boundary sliding contributing to creep in modern turbine disk alloys [2], a predictive
model of grain boundary orientation and morphology would allow the engineering of
grain boundaries to minimize creep.
Deformation and dislocation mechanisms will be determined from the shape and
orientation of the peaks in Laue diffraction patterns. A 3D tomography of these Laue
images will be obtained via a novel Micro Laue diffraction technique developed at
Argonne National Labs Advanced Photon Source [3]. Deformation is indicated as
elongated or split peaks in the diffraction patterns. This is caused by dislocations adding
a slight rotation to the lattice about the dislocation line. Additionally the direction in
which the peak is split or smeared can inform which slip planes are active [4].
The measurement of the deformation and slip systems will be conducted by
fitting an ellipse to each peak in order to determine peak aspect ratio and orientation.
The images will be filtered to reduce the impact of image noise. Ellipses will be fit to the
filtered peaks by a moment of inertia based algorithm instead of a perimeter based
algorithm in order to take pixel intensity into account. Once the aspect ratio and
orientation have been determined, the sensor geometry must be correlated to the
crystalline orientation to relate the ellipse rotation angle to obtain slip plane activation.
Once these parameters are measured for each peak, relations can be made given
distance from grain boundaries, twin boundaries, etc.
The measured relationships between deformation and distance to grain
boundaries is expected to validate what was observed with TEM analysis, as well as
providing rudimentary quantitative results for the purpose of building a predictive model.
A predictive model would allow grain boundary engineering to obtain optimized creep
properties.

Problem Statement
The goal of this investigation is to determine the distance at which deformation
within grains of polycrystalline nickel superalloy transitions from single slip system
deformation to complex slip regimes. In crystalline plasticity simulations, the current
assumption is that each grain only slips along one glide plane and in one direction.
While this assumption is relatively accurate for the center of large grains, it has been
previously observed via in-situ TEM analysis that slip systems become more complex at
grain boundaries. This knowledge will allow more accurate plasticity models to be
developed such that performance and lifetime of parts can be more accurately
predicted.

Technical Background
Nickel superalloys are extremely important to the aerospace industry, comprising
the components that must endure the hottest regions of turbine engines. Failure of
these parts occurs when they begin to deform appreciably, and it is of great importance
to be able to predict failure as engine failure is costly and potentially life threatening.
Previous work started with digital image correlation of a small region of a
superalloy tensile specimen as it was deformed in-situ within a scanning electron
microscope. By watching the motion of a random pattern of microscopic ceramic
markers that were deposited on the surface of the tensile bar as it deformed, the
localization of the deformation was determined (Figure 1)[5].

Figure 1 DIC strain map of nickel superalloy. Images were taken in-situ at regular time
intervals as sample was deformed at 700C. [5]

Attempts were made to correlate microstructural features to this deformation,

including orientation mapping using electron backscatter diffraction, and indexing of
grain boundary character (High angle vs. 3 vs. 4-29). These 2D techniques were
found to not give enough information to provide the underlying mechanisms for the
distribution of slip [6]. Given this, 3D analysis techniques were considered. One
potential solution is EBSD combined with serial sectioning, where the a thin layer is

sputtered away in between EBSD images [7]. Deformation information can be gleaned
from the shape of the diffraction maxima [4], and the 2D raster combined with the serial
sectioning gives a full 3D dataset. The benefit of this technique is that it has a relatively
high spatial resolution (on the order of 250nm), as some of the microstructural features
in this particular alloy are on the order of only several microns. The drawbacks,
however, include the fact that this is a destructive test, as material must be etched away
in-between every image taken. It is also incredibly time intensive both from a
preparation, acquisition, and an image analysis standpoint [6]. Due to these limitations,
another technique was explored, micro-Laue diffraction pioneered by the beamline
scientists at the Advanced Photon Source at Argonne National Lab [3].
The main concept of micro-Laue is very similar to traditional Laue diffraction,
where white (polychromatic) x-rays illuminate a sample, and the beam diffracts in
accordance with Braggs law to form patterns on an image sensor. The angles between
peaks are measured and used to determine what crystalline planes they were reflected
from. Knowing the plane indices, the rotational orientation of the lattice can then be
determined [8].
The micro-Laue technique involves using the high brilliance synchrotron x-ray
source in order to gather data up to roughly 100 microns deep into the sample. A pair of
elliptic KirkpatrickBaez mirrors focus the beam to a sub-micron diameter by
progressively reflecting the xray at incredibly shallow angles [9]. The sample is mounted
on a motorized platform capable of sub-micron stepping in the x, y, and z axes where
the z axis is parallel to the beam [10]. For each given X-Y position the image sensors
then receive diffraction information from every point along the line at once. A thin
platinum wire (referred to as a differential aperture) is used to block a small segment of
angles at a time and is then scanned in the z direction along the surface of the sample
in order to determine what diffraction peaks are being blocked at each depth of the wire
(Figure 2).
Using the geometry of the sensor and the position of the wire, the image values
of the pixels are subtracted from each other in order to extract images of only the
diffraction peaks from each depth. The resultant data is a set of images representing the
Laue diffraction patterns from each 3D position in the sample. From those patterns, the
crystalline orientations are determined exactly as with traditional Laue backscatter
diffraction [8], and also contain information about the residual strain and accumulated
deformation [12]. This technique has several major benefits over EBSD combined with
serial sectioning: micro-Laue imaging is non-destructive, involves much less sample
preparation, as well as being much faster than the serial sectioning technique for image
segmentation and alignment.
The strain data of interest is then contained within the shape of the peaks in the
Laue patterns. As the crystal deforms, added dislocation content create sub-grains with
slight rotations with respect to the average orientation of the whole grain. These slight
rotations cause the peaks to smear or split slightly in the direction of the slip [13]. The
direction and magnitude of this change of peak shape contains information regarding
the amount and direction of slip, and is the main focus of this study. For example, if a
material experiences single slip system activation, the peaks will elongate into ellipses
along the direction of the burgers vector of the slip system. If multiple slip systems are

activated the peak will first broaden more spherical in nature. When sub-grains are
formed these elongated or broaden peaks subsequently split into sub peaks.

Figure 2 Diagram of the working principle of scanning the Pt wire across the surface of the
sample in order to extract diffraction information from specific depths of the sample[11].

Technical Approach
The primary goal of this investigation is to measure the shape of the diffraction
peaks, and use the orientation data provided from Argonne National Lab to correlate
slip with grain boundaries and other meso-scale structures. Being a data-centric
problem, the research will be conducted by writing code and scripts in Python in order to
run computations on large amounts of data. Python was selected as a programming
language for its forgiving learning curve, strong scientific community support, and open
source licensing.
The data provided by Argonne comes in two primary forms that must be utilized
in conjunction with each other. The first dataset is the diffraction images as
reconstructed from each individual scan of the Pt wire. These images take the form of a
2D array of 16bit pixel intensity values representing the x-ray intensity at any given point
on the detector. These images were then run through a set of algorithms to find peaks,
as well as determine which planes of atoms those peaks were reflected from. Knowing
which peaks correlate to which planes allows the orientation of the crystal to be
determined within the lab space. These algorithms return data in the form of a large
XML file, which contains a hierarchical representation of every peak forming every
pattern for every image.
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Given these inputs, the project can be broken down into five main tasks:
Data munging: organizing the data so that it is possible to analyze peak
shape on a per diffraction pattern basis instead of organized on a perimage basis.
Image filtering: removing noise and irrelevant data
Peak shape analysis: ellipse fitting algorithm
Geometry correlation of slip systems: determine relation between ellipse
long-axis measurements in diffractor space with slip systems in crystal
space, and relate slip direction and magnitude to grain boundary proximity

Task 1: Data Munging

The first challenge is to take the data collected about the peaks and diffraction
patterns provided in the XML and sort it into a native python object on a per-diffraction
pattern basis rather than a per-image basis. It is not uncommon for a given image to
contain an incomplete pattern that could not be fully indexed, in which case no
orientation data can be obtained. These images are therefore not useful to the project,
as correlations to orientation cannot be made. These images are therefore excluded
from analysis. It is also common for images to contain multiple patterns, as with
instances where a given measurement volume lies across a grain boundary, and the
diffraction image is sampling multiple grains at the same time. In this case it is beneficial
to the analysis of the data to treat the peaks on each of the patterns as unique, and as
such the peaks are sorted on a per-pattern basis.
The XML file is first converted into a searchable python object called an element
tree in order to facilitate the organization of the data [14]. When a pattern is found for a
given image the hkl indices of the fitted peaks are rotated by the same rotation as the
reciprocal lattice, and compared to the listed q-vectors of all the points found. This
serves to extract the peaks from only that pattern in the event there are multiple
patterns present in the same image, or there were peaks located but not attributed to a
pattern.

Task 2: Image Filtering

Once the peaks for each pattern are identified for analysis, a series of image
filtering stages will be employed to ensure the accuracy of the ellipse fitting to follow. A
simple blurring filter will be used to reduce low amplitude background noise by taking
the median value of the 9 adjacent pixels [15]. A threshold is then applied to the image
to select the bright peak from the dark background [16]. Successive minimum and
maximum filters are applied in a similar way to the median filter, and have the effect of
first reducing the radius of all peaks present, eliminating small peaks remaining from
background noise, then increasing the radius of the desired peak back to its original
size [17]. Finally unique indices are given to all connected regions and only the peak in
center of the region of interest is selected Figure 3[18]. This accounts for the possibility
of having two distinct peaks within close proximity to each other, by removing nonconnected peaks from the region of interest.

Figure 3

Task 3: Peak Shape Analysis

After the peaks are sorted, their shape must be determined in order to analyze
the direction and magnitude of the deformation. An ellipse was chosen as a target
shape to fit to each peak, as with the magnitude of the major axis, the minor axis, and
the angle of inclination, many important features of the peak can be described. Many
ellipse fitting algorithms rely on finding the shape of the perimeter of an object via a
least-squares regression [19], however, this approach would not take into account the
pixel values. Instead a moment of inertia based approach fits an ellipse to each peak
based on the pixel intensity values [20]. Imagining the pixel values represent masses on
a flat sheet, the first order moments are used to determine the center of mass and the
second order moments are used to determine aspect ratio and angle of orientation. One
small benefit of this approach is that the calculations involved are deterministic, and
execute particularly fast; an important consideration when working with large datasets.

Task 4: Geometry Correlation of slip systems

Once peak shapes have been determined, the crystalline orientation must be
related to the direction of peak elongation. This relation will be created by computing the
sensor geometry in relation to the sample geometry all with respect to the lab
coordinate system. From there the vectors must be normalized into crystalline direction
components to account for the possibility of complicated slip systems [4], [13].
Additionally, sample points must be sorted by crystalline orientation and position to
group data points into discreet grains. Once discreet grains are formed, grain
boundaries can be defined and distance from any given point to a grain boundary can
be calculated. This data will then be compared to the qualitative results found by Carter
et al [1].

Risk Assessment and Mitigation

See Appendix Figure

Unsupervised Computation(Figure 4 a)
Much of the processing of the data is done with no visual output, as there are
tens of thousands of images to be considered with up to twenty or so peaks on some
images. Manually looking over the results to confirm the validity of the computation is
infeasible, however it is possible that the data will cause incorrect fitting of ellipses in
some cases. In these cases data will still be recorded, and no errors will be thrown. One
potential way to mitigate this risk is to determine analytical methods to identify poor

ellipse fitting and generate visual representations of only those with poor fits. Given the
visual representations decisions can be made on either how to re-fit the images or to
exclude certain outliers in the data.

Code Incompatibility(Figure 4 b)
Python was selected as a language among other things for its portability and
cross platform compatibility. The code may however depend on platform specific
libraries that may not work on all machines. Mitigations for this include creating a virtual
environment running Linux specifically for the computation of this data, as well as
striving to preemptively code for multiple operating systems.

Data Loss (Figure 4 c)

The raw data takes up a large amount of storage, and is most efficiently stored
on physical hard drives. Physical hard drives have mechanical elements that can fail,
and when that happens the data stored on the drive can sometimes become
unrecoverable. This would have catastrophic consequences, as the data would be very
difficult to re-collect. This risk can be mitigated by keeping redundant backups of the
data in multiple locations.

Time Management (Figure 4 d)

As an undergraduate, I have a relatively busy schedule, and can fall prey to not
managing my time efficiently. This can progressively delay the progress of the project
as I have to dedicate more time catching up with other work. I will attempt to mitigate
this risk by keeping a daily planner of assignments and updating my calendar regularly
to help myself stay on schedule.

Results and Discussion

The desired result of this investigation is to build data relating deformation
accumulation and slip system activity to proximity and type of grain boundaries. A data
model that retains information at multiple levels of complexity will be required to
structure the results according to any desired parameters to facilitate the making of
these relationships. Provided the results reinforce what was found with TEM analysis
[1], quantitative results such as distributions of deformation can be correlated to
parameters such as distance from grain boundaries. Models can be generated either
manually based on measured values and prior knowledge of physical laws, or by data
learning algorithms [21].

Conclusions/Summary
Polycrystalline nickel superalloys are critical to the performance of turbine disks,
and are subject to creep as they are under load at high temperature for prolonged
periods of time. Dislocation movement as well as grain boundary sliding have been
found to both contribute to creep, and be related to different dislocation mechanisms [1],
7

[2]. With a better understanding of these mechanisms, and how they impact
deformation, the models can be used to optimize the creep properties by engineering
the grain boundaries to distribute deformation more evenly and reduce grain boundary
sliding [22].

References
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Wang, H. l. Fraser, M. d. Uchic, and M. j. Mills, Characterization of Strain
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[2] A. Soula, Y. Renollet, D. Boivin, J.-L. Pouchou, D. Locq, P. Caron, Breacute, and Y.
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[3] B. C. Larson, W. Yang, G. E. Ice, J. D. Budai, and J. Z. Tischler, Three-dimensional
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[7] M. A. Groeber, B. K. Haley, M. D. Uchic, D. M. Dimiduk, and S. Ghosh, 3D
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symmetry. New York: Cambridge University Press, 2012.
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T. Sato, T. Tanaka, T. Kimura, H. Yokoyama, J. Kim, Y. Sano, Y. Hachisu, M.
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[10] United States D.O.E., Experimental Setup: Sample Coordinates, X-ray Laue
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[11] Image Reconstruction, Argonne National Laboratory. [Online]. Available:
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[14] XML tree, Wikipedia, the free encyclopedia. 29-Jun-2015.
[15] Median filter, Wikipedia, the free encyclopedia. 21-Apr-2015.
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Appendices
Risk Assessment

b)
.

d)
.

a)
.

c)
.

Figure 4

a)
b)
c)
d)

Unsupervised computations could potentially return incorrect results silently

Code may be incompatible on non Unix based computers
Hard disk drives may fail mechanically and incur data loss
Poor time management may lead to project delays

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Budget
SALARY:

Senior Project
4,800

Faculty
Undergraduate Student
SUB-TOTAL

1,440
6,240

FRINGE BENEFITS
27.00%
SALARY & FRINGE BENEFITS TOTAL

1,296
7,536

Consumables
Internal Services

500
1,000

NON-SALARY:

SUB-TOTAL
Total Direct Costs
Indirect Costs
Total

58.50%

1,500
9,036
5,286
14,322

Budget Justification
Faculty salary is billed at $50 per hour for a total of 96 hours over the course of a
year, totaling $4,800. Student salary is billed at $10 per hour for a total of 144 hours
over the course of a year, totaling $1,440. Accommodation for benefits brings the salary
sub total to $7,536. An allotment for $400 in additional hard drives (for data storage) is
made along with an allotment of $100 for shipping costs for a total of $500 in the
consumables category. The indirect costs of $1,000 account for charges associated
with network and technological resources such as network storage and server usage.
The total direct costs amount to $9,036 with an additional 58.5% in indirect costs,
bringing the total project budget to a total of $14,32200.

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