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2021-04-07 - Analysis of Complex Geological Materials With FeaturePhase in AZtecFeature

This document discusses analyzing complex geological materials using automated feature analysis and phase identification. It provides two examples: (1) analyzing a sample containing ilmenite and magnetite grains that are difficult to distinguish in BSE images due to cracks and similar brightness; and (2) analyzing exsolution lamellae in pyroxenes. EDS mapping is used to identify phases by composition rather than BSE contrast. The combined mapping and feature analysis approach, called FeaturePhase, allows accurate analysis of challenging samples by identifying phases and extracting morphological and compositional data on individual features. This provides valuable information for understanding geological structures and processes.

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Luis Cañari
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0% found this document useful (0 votes)
31 views

2021-04-07 - Analysis of Complex Geological Materials With FeaturePhase in AZtecFeature

This document discusses analyzing complex geological materials using automated feature analysis and phase identification. It provides two examples: (1) analyzing a sample containing ilmenite and magnetite grains that are difficult to distinguish in BSE images due to cracks and similar brightness; and (2) analyzing exsolution lamellae in pyroxenes. EDS mapping is used to identify phases by composition rather than BSE contrast. The combined mapping and feature analysis approach, called FeaturePhase, allows accurate analysis of challenging samples by identifying phases and extracting morphological and compositional data on individual features. This provides valuable information for understanding geological structures and processes.

Uploaded by

Luis Cañari
Copyright
© © All Rights Reserved
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Download as PDF, TXT or read online on Scribd
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Analysing Complex Geological Materials with Application Note

AZtecFeature & FeaturePhase

Geological structures are present on a variety of


scales from kilometres to <1μm. These structures
are produced by geological processes such as
tectonic movement, volcanism and cooling. As
a melt cools and solidifies, crystals sequentially
exsolve from it into distinct mineral phases
with different elements migrating to different
phases, accommodated by differing crystal
structures. This can cause a range of different
characteristics within a rock, depending on the
relationship between the minerals formed. There
is a significant value in being able to measure,
interrogate and understand these relationships as
they provide a wealth of information on the rock
in which they are found.
Geological samples can be challenging to
analyse en-masse by automated approaches
in the SEM. This can be for reasons related
to the formation of the rock itself – such as
mineral grains having very similar brightness,
when imaged in the SEM, to neighbouring
grains despite significant compositional
differences. Here we discuss how automated
analysis of challenging geological samples
can be performed using a combined mapping
and Feature analysis approach known as
FeaturePhase.
Automated Feature analysis often uses
backscattered electron (BSE) images for the
identification and detection of grains from
one another. This is because images of this
type have a contrast that relates to the mean
atomic number of the material under the beam
– meaning that they can display compositional
variation. Grey level thresholds are applied
to these images to identify grain locations
for subsequent analysis. This process can be
hindered by various factors such as low BSE
contrast between mineral phases and physical
surface features such as cleavages, cracks and
scratches. Such surface characteristics are
clearly visible in BSE images and therefore have
the potential to impact thresholding.
Example 1: A Single Grain

In the example below (Fig. 1A), two relatively bright grains can be seen to be next to each other in the centre of
the image. The minerals forming the grains (Ilmenite (FeTiO3) and Magnetite (Fe3O4)) have similar mean atomic
numbers and therefore have similar grey levels in the BSE image. Many cracks that may have an effect on
grey level thresholding are also present within both grains. Cracks often appear as darker than the host grain
meaning that it may be treated as a grain boundary and multiple analyses may be performed instead of the
real single grain being analysed. This is a common problem as it is often not desirable to make thresholds large
enough to include cracks as darker thresholds are needed to detect other, real phases in the sample. However,
the problem can be overcome by using EDS elemental mapping to detect the features by their composition
instead of from the BSE image – effectively seeing through the cracks. In addition, the low contrast between
the grains becomes irrelevant, allowing accurate analyses of the grains of interest to be performed. By utilising
large area Ultim® Max detectors working at high count rates for this mapping, short live times per pixel can be
used to ensure that throughput is maintained.

Fig. 1 - Electron images and EDS maps of magnetite and ilmenite. A. The different phases can be seen in the BSE image but
grey level thresholding is made difficult by the low contrast between them and pervasive cracks. B-H: EDS maps of oxygen,
silicon, titanium, aluminium, calcium, magnesium and iron. EDS mapping is not affected by the cracks or low image contrast
in the same way as the BSE image.

The acquired maps are then processed by our phase idetification algorithm, AutoPhaseMap, which compares
the individual element maps to determine what phases are present. Once identified, groups of neighbouring
pixels of the same phase are combined to form features. These features are measured for morphology in the
same way as “normal” features acquired on the basis of BSE image detection, and compositional information is
extracted from the maps of the features. Classifications are applied to these phase-acquired features, as they
are for “normal” features. An example of this is shown in Figure 2.
Fig. 2 - (Top Left) Automated EDS mapping, phase and feature extraction with AZtecFeature using FeaturePhase. The
classification scheme (Top right) shows the number of features detected for each phase. (Bottom) Example of the combined
morphology and compositional information recorded for the Ilmenite grain.

Example 2: Exsolution Lamellae in Pyroxenes

The analysis shown in case study 1 was a relatively simple case – working with a single field looking at one
grain. In practice, we often require far more extensive analysis – looking at potentially thousands of grains over
potentially hundreds of fields of view. The workflow that we just looked at can be extended to more complex
scenarios. Here we consider exsolution lamellae of orthopyroxene (OPX) in clinopyroxene (CPX) as shown in
Figs. 3 and 4. In this case, the OPX has exsolved from CPX (forming exsolution lamellae within the OPX grain)
after their mutual crystallisation from an initial melt.
Whilst, in this region, scratches/surface damage are not a major issue, the grey levels of the different phases
in the BSE image are very close, making FeaturePhase’s mapping based approach particularly valuable. Fig. 3
shows an example of a single field BSE image and the associated EDS element maps. It is clear that although
the BSE image gives some information, the EDS maps are far clearer in showing the distribution of the lamellae.
In this case, the whole field of view has been mapped: However, it is also possible to perform a standard grey
level thresholding of the sample and assign only certain thresholds to be mapped. This typically has the effect
of greatly reducing the area to be mapped and therefore increasing throughput and is particularly useful where
only certain phases within certain thresholds are hard to differentiate with the BSE image.
Fig. 3 - Single-field EDS map of fine OPX lamellae occurring in CPX. (A): The density variation is low, which is reflected on the
BSE image. (B-D): EDS maps of oxygen, calcium and iron.

When a larger area consisting of multiple fields of view is mapped and montaged (Fig. 4), the extensive nature of
the lamellae are shown and it is clear that large scale, automated analysis of this texture would give very useful
information on the sample.

Fig. 4 - Multiple-field EDS map. This map is an extended area acquisition of the single field map of Fig. 3. A. The larger area
covered shows additional phases are present and regions where surface damage is more of an issue.

These maps were acquired automatically as part of a large area AZtecFeature run. Immediately after being
acquired, they were processed with AZtec’s FeaturePhase algorithm to identify phases and then recorded
as features. This was repeated over the entire large area to form the image shown in Fig. 5. AZtecFeature’s
reconstruction algorithm was also applied to the dataset to reconstruct the larger features which were broken
by field boundaries. With the grains all detected, it was then possible to interpret the data – an example of this is
shown in Fig. 6 where the histogram shows the orientations of the long axes of the OPX grains – it is possible to
see two dominant peaks – one for each of the major cleavage directions and the angle between them.

Fig. 5 - Large area AZtecFeature


run with features coloured by class.
The combination of automated
feature analysis and phase analysis
has produced a clear identification
of both the host phase and the
lamellae, as well as identifying
additional minor phases.
Fig. 6 - Histogram showing the orientation of the
long axes of the exsolution lamellae features. The
two major peaks correspond to the two major
cleavage planes present in the mapped area.

Conclusion

• The use of EDS mapping data for feature detection enables grains
to be identified in geological samples where otherwise it would be
difficult or impossible to do so.
• Once phases are identified, groups of pixels of the same phase are
grouped to define Features. These are then treated in the same way
as those acquired via the standard grey-level thresholding method.
• Sample preparation damage, cracks, topography etc. can effectively
be “seen through” to get a true measurement of features of interest.
• The approach can be automatically applied to large areas and
provides a wealth of information for understanding the rocks being
studied.

nano.oxinst.com/AZtecFeature

The materials presented here are summary in nature, subject to change, and intended for
general information only. Performances are configuration dependent. Additional details are
available. Oxford Instruments NanoAnalysis is certified to ISO9001, ISO14001 and OHSAS
18001. AZtecFeature and Ultim Max are Registered Trademarks of Oxford Instruments plc,
all other trademarks acknowledged. © Oxford Instruments plc, 2020.
All rights reserved. LITR511912-01

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