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EBSD presentation

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7 views34 pages

EBSD presentation

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PranjalGupta
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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INDIAN INSTITUTE OF TECHNOLOGY ROORKEE

Electron Backscatter Diffraction (EBSD): Fundamentals,


sample preparation, and applications

Pranjal Gupta

supervised by
Prof. Apurbba Kumar Sharma
Prof. Inderdeep Singh
Mechanical and Industrial Engineering Department
IIT Roorkee

July 2024
EBSD fundamentals

Scanning electron microscopy (SEM)

[Source: edax.com] 2
EBSD fundamentals

Backscattered electrons
• High-energy electrons produced by elastic scattering of the primary beam electrons with atom nuclei.
• Incident (primary) electrons interact with the nuclei of the atoms and their trajectories are deviated and emerge
on the surface of the sample.
• Typically, heavier elements, because of their bigger nuclei, can deflect incident electrons more strongly than
lighter elements.

Figure. Schematic of the incident electron being backscattered by the interaction with
the atom nuclei [Source: nanoscience.com]
3
EBSD fundamentals

BSE imaging

Figure. Comparison of a secondary electron image (left) and a backscattered electron image (right) of the letter part of a carbon-
coated name card (seen at the centre of both images), taken at an accelerating voltage of 15 kV. [Soure:jeol.com]

Figure. An example involving observations of a ruptured ceramic surface. [Source:hitachihitech.com]


5
EBSD fundamentals

BSE imaging

Figure. a) SEM image of an Al/Cu sample, b), c) Simplified illustration of the


interaction between electron beam with aluminium and copper. Copper atoms
(higher Z) scatter more electrons back towards the detector than the lighter
aluminium atoms and therefore appear brighter in the SEM image. Figure. BSE images of a tin ball sample with carbon dirt flakes taken with
[Source: azom.com] 5kV and 15kV beam acceleration voltages. Since the dirt flakes are very
shallow, they become less visible when a 15kV acceleration voltage is used.
[Source: thermofisher.com]

6
EBSD fundamentals

BSE imaging

Figure. (a) SEM micrograph showing distinct characteristics at the interface of resolidified layer and the parent material, (b)
EBSD IPF of (i) as-received parent material, and (ii) interface of parent material and resolidified layer, (c) EDS spectra of
parent material and resolidified layer, and (e) corresponding elemental mapping showcasing segregated niobium,
molybdenum and titanium elements.
7
EBSD fundamentals

Electron backscattered diffraction

[Source: edax.com] 8
EBSD fundamentals

EBSD detectors

[Source: oxfordinstruments.com] 9
EBSD fundamentals

Bragg’s law of diffraction


• Governs the interaction of radiation with planes of atoms
within the crystal lattice.

• EBSD patterns are formed by a 2-step diffraction process:


1. Convergent beams enter the sample and forms a “virtual
point source” from which electrons are scattered
inelastically in all the directions.
This forms typical interaction volume.
2. Electrons from the virtual point source travel toward the
tilted sample surface and scatter elastically on the way out if
they meet Bragg 's condition.
3. As the diffracted electrons reach the detector EBSD
patterns are formed.

[Source: edax.com] 10
EBSD fundamentals

Electron backscattered diffraction

Figure. Schematic of the diffracting cones with respect to the reflecting plane, the specimen,
Figure. Backscatter Kikuchi pattern from cadmium at 20 keV,
and the phosphor screen
acquired with an analog video camera

[Reference: Schwartz, A., Kumar, M., Adams, B., Field, D. (eds) Electron Backscatter Diffraction in Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-88136-2_18] 11
EBSD fundamentals

Kossel cones

12
EBSD fundamentals

• An orientation map is generated by shading


each point in the scan according to some
parameter reflecting the orientation at each
point
• A grain boundary map can be generated by
comparing the orientation between each pair
of neighbouring points in the scan. A line is
drawn separating a pair of points if the
difference in orientation between the points is
between a specified range.

13
EBSD fundamentals

Texture
Texture is a measurement of the similarity in orientation of the crystal lattice within the constituent grains of a
polycrystal. A single crystal would have the maximum texture, and a material where all the grains have
different orientations would have a random texture. Most materials fall somewhere in between these two
extremes depending on how the material was processed.

14
EBSD fundamentals

Texture

15
EBSD fundamentals

Stereographic projection

17
EBSD fundamentals

Pole figures

[Reference: Schwartz, A., Kumar, M., Adams, B., Field, D. (eds) Electron Backscatter Diffraction in Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-88136-2_18] 19
EBSD fundamentals

Texture

Cube texture Copper texture Brass texture


Recrystallized Plastically Rolled FCC
FCC materials. deformed FCC material, eg Brass
Eg. Cu, Al material, eg Cu

Figure. Pole figure of TiN coatings on a WC+Co substrate. (a) is the 001 pole figures
of the coatings produced by two different companies. The wear resistance of coating
(b) was almost ten times that of (c).
[Reference: Schwartz, A., Kumar, M., Adams, B., Field, D. (eds) Electron Backscatter Diffraction in Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-88136-2_18] 20
EBSD fundamentals

Texture Fiber texture

Random texture

Cube texture

Rolled texture

Figure. Pole figures for the (a) random, (b) cube, and (c) rolled texture

Aaditya Lakshmanan, Mohammadreza Yaghoobi, Krzysztof S. Stopka, Veera Sundararaghavan, Crystal plasticity finite element modeling of grain size and morphology effects on yield strength and extreme
value fatigue response, Journal of Materials Research and Technology, Volume 19, 2022, Pages 3337-3354, ISSN 2238-7854,
21
EBSD sample preparation (for metals)

Cutting
Sample preparation techniques
1. Cutting
2. Mounting
3. Grinding (Manual/automatic)
4. Cloth polishing (optional)
5. Final surface preparation
• Electropolishing
• Polishing using colloidal silica
• Ion milling

Mounting Grinding Cloth polishing

[Source: struers.com] 22
EBSD sample preparation (for metals)

Electropolishing
Electrolytic polishing involves the removal of material (anodic
dissolution) of the specimen surface in an electrolytic cell, the
specimen being the anode.

Factors controlling polishing characteristics include:


• Electrolyte composition
• Electrolyte temperature
• Electrolyte stirring
• Area to be polished
• Voltage

Figure. A basic electrolytic cell

Figure. Current vs voltage plot


[Source: ebsd.com] 23
EBSD sample preparation (for metals)

Common electrolytes

ASTM standards

[Source: Standard Guide for Electrolytic Polishing of Metallographic Specimens-ASTM International] 24


EBSD sample preparation (for metals)

Electropolishing

[Source: ebsd.com] 25
EBSD sample preparation (for metals)

Automatic electropolishing machine

Make: Struers
Model: LectroPol-5

[Source: struers.com] 26
EBSD data analysis

Analysis software
• MATLAB
• EDAX OIM analysis
• AZtec Crystal
• HKL Channel 5
• Bruker Esprit
• Tango
• MTEX
• Dream 3D
• ASTAR
• EBSD Image

27
EBSD capabilities

• Orientation mapping
• Grain size and grain boundary analysis
• Orientation relationships between phases
• Texture measurements
• Phase identification
• Strain analysis

28
EBSD applications

Typical applications
• Metals
– Metal production i.e. sheet metal, castings, forgings - automotive, aerospace, power generation and
distribution, petrochemical and chemical plant, nuclear i.e. extreme duty materials - high strength, high
temperature and corrosive environments. Electronics.
– Phase identification and discrimination
– Texture analysis, grain boundary characterisation
– Deformation

• Geological
– Phase identification and discrimination
– Orientation & texture analysis

• Ceramics
– Phase identification and discrimination
– Orientation & texture analysis

29
EBSD applications in materials processing

Orientation mapping

• Tensile bar of pure, polycrystalline nickel was elongated to 1%,


5%, and 10% strain.
• Formation of deformation bands within the grains as the strain
increases.
• An increased density of LAGBs as the strain level increases

Figure. Different mapping algorithms applied to a data set from an interrupted tensile test on polycrystalline nickel. Scale bar on all
figures is 50 m. (a) Orientation: inverse pole figure with respect to x-axis (loading axis). (b) Grain boundary map: black lines are high-
angle (>10◦) boundaries, red lines are lowangle (1◦<<10◦) boundaries. (d) Average kernel misorientation map: 0–1.5◦, blue-red, cluster
(3×3 pixels) misorientation. (f) Integrated misorientation map (rainbow scale in degrees)

[Reference: Schwartz, A., Kumar, M., Adams, B., Field, D. (eds) Electron Backscatter Diffraction in Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-88136-2_18] 30
EBSD applications in materials processing

Orientation mapping

[Reference: Schwartz, A., Kumar, M., Adams, B., Field, D. (eds) Electron Backscatter Diffraction in Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-88136-2_18] 31
EBSD applications in materials processing

Grain boundaries mapping

[Reference: Schwartz, A., Kumar, M., Adams, B., Field, D. (eds) Electron Backscatter Diffraction in Materials Science. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-88136-2_18] 32
EBSD applications in materials processing

Phase identification

Figure. Backscattered electron image of the region of interest

Figure. EBSD patterns of four apparent phases in Fig. 6.2: (a) matrix grain, (b) dark, blocky phase, (c) small,
elongated phase, (d) bright, globular phase

33
EBSD applications in materials processing

Strain analysis Figure. (a) EBSD and EDS


maps of the region of interest
illustrating the initial resultant
phase map,as well as the
EDS signal from the Ni Ka,
Nb La, and Ti Ka peaks; and
(b) the phase map obtained
after incorporating the
EDS information shown in
Fig. 6.4(a). Assigned phases
are corroborated by the colors
observed in the optical
microscope image

34
EBSD research trend

35
Further reading

• Adam J. Schwartz · Mukul Kumar · Brent L. Adams · David P. Field Electron Backscatter
Diffraction in Materials Science.
• H Bunge (1982). Texture Analysis in Materials Science. Butterworths: London.
• Valerie Randle (2000). Introduction to texture analysis – Macrotexture, Microtexture and Orientation
Mapping.
• U. F. Kocks - Texture and Anisotropy

36
Thank you

37

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