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 Content

Expanding Possibilities with Next-Generation

Engineering and Structural Materials 6

Developing Green Energy Devices for Mobility

and Sustainability 9

Powering Miniaturization Technologies with

Functional and Nanomaterials 14
Nano Forsterite: Identification of fragile microscopic structures
during mineral transformations in wet supercritical CO2. Biomaterials: Connecting with and Learning
Images acquired with ZEISS ORION NanoFab, the unique
Helium-Neon ion microscope (HIM) from ZEISS. from the Natural World 17
Kindly provided by Bruce W. Arey and Andrew R. Felmy,
Pacific Northwest National Laboratory, Richland, USA. 2 µm

2 3
 Building the Future.
Meet the challenges of materials research with
state of the art microscopy solutions from ZEISS

Designing the materials for tomorrow’s engineering innovations

will require an ever-better understanding of the complex
connections between processing, properties and the underlying
structures that, collectively, influence how a material performs
and why it might fail.

Today, ZEISS is working in a variety

of application fields with scientists at
ZEISS is the only manufacturer of
multiple technologies covering a range “often
…at an engineering level,
the behavior of a
the forefront of materials research. of scales, modalities and dimensions:
material and the lifetime of
Take, for example, the development of that’s why researchers value ZEISS
a material are determined
additive manufacturing processes for microscopes as a critical piece of their
the design and production of complex characterization suites. We invite you to
by how defects nucleate and
parts. Or the push for advancements in explore a few examples of how these grow.
lithium ion batteries and other energy complementary technologies are being
storage and conversion devices that will used to help overcome some of today’s And so if we can under-
change the way we power our lives on most pressing research challenges. stand how defects grow,
the go. ZEISS is also collaborating with Together, we are building the future starting with a small
researchers to understand and exploit of materials science and engineering.
nucleus and moving from
unique material properties at the
a propagation phase to
nanoscale for the rapid miniaturization
of functional devices.
ultimate failure, then we can
engineer those materials
to slow down the rate of the
nucleation of the defects or
even remove the defects in
structure the first place by improving
manufacturing.

characterization We can then move to

much safer and higher
performing materials with
longer lifetimes…
properties

processing ZEISS offered us this

opportunity to work hand
in glove to see things
that just couldn’t be seen
Light Microscopic Analysis of Nd2Fe14B: The demand of raw materials leads to a search for new magnetically hard
phases. Magnets from rare earth metals and transition metals, such as Nd2Fe14B, are currently investigated in this context.
performance before. ”
The magnetic domains are visualized using the magneto-optic Kerr effect. The polished surface of a magnetic specimen is
illuminated with linear polarized light. The goal is to develop a method which can be used to directly calculate the intrinsic,
Tomorrows materials demand to be lighter, faster, stronger, smarter, and more durable. Characteri- Prof. Phil Withers
zation techniques represent a key link that tie together the cornerstones of the materials design paradigm. Regius Professor of Materials in the
hard-magnetic properties from the domain structure using a classic compound microscope and digital image analysis.
Solving the challenge of connecting processing and structure with properties and performance.
Shown here is a Kerr image of an Nd2Fe14B smelting sample at 200× magnification in a compound microscope with typical School of Materials, University of
and in some cases complex domain patterns (closure domains: turquoise; stripe domains: dark blue).
50 µm Manchester, UK.

4 5
Expanding Possibilities with Next-Generation
Engineering and Structural Materials

The demands for materials to meet a variety of structural needs

has spawned advancements in an assortment of fields including:
advanced alloys resistant to heat or fatigue, high strength-to-
weight ratio composite structures, environmentally-durable and
self-healing concrete, and reliable, robust protective coatings.

5 µm 500 µm 250 µm 100 µm

Developing and improving these
types of engineering materials takes
a detailed understanding of the
connections between processing,
structure, performance and properties
Figure 2: When higher resolution is needed,
field emission scanning electron microscopy
manufacturing become increasingly (FE-SEM) offers a flexible platform along with the
prolific and more complex. Microscopy opportunity to incorporate analytical techniques
such as EDS, EBSD or Raman in addition to in situ
characterization techniques are central
devices. This image reveals electron channeling
to this paradigm, enabling you to study contrast in steel.
features of interest such as grain structure
Figures 3: While 2D approaches provide meaningful insights, the recent emergence of more complex
3D material structures, partially driven by additive manufacturing techniques, has provided motivation
for characterizing materials in their native 3D state. X-ray microscopes help us understand the effects
of geometric complexity or anisotropy of microstructural features. Left: This image shows voids in an
additive manufactured Inconel lattice, courtesy of Kavan Hazeli, Mechanical and Aerospace Engineering
at the University of Alabama, Huntsville. The extension of 3D X-ray tomography to incorporate diffraction
information enables non-destructive 3D grain mapping of bulk polycrystalline samples, complementing
existing 2D techniques such as polarized light microscopy or ESBD. Right: This image of 3D grain structure

throughout the material’s life cycle. and sizes, texture, phases and phase tran- in a titanium alloy was acquired by diffraction contrast tomography (LabDCT).

This is even more important as ad- sitions, volume fractions, inclusion and
vanced technologies such as additive impurity distributions, and surface finish.

s
Precipitate
Corrosion
Pits Phases
s efects
Inclusion Lattice D
and Grain s
e
Boundari
Surface
ss
Roughne
Texture
Grain
Cracks Orientati
on

Voids

Figure 1: Microstructural features critical to the properties and performance of

engineering materials.

200 µm

Figure 4: Light microscopy technologies such as stereo, zoom and confocal laser scanning microscopes can be used for a range of contrast modalities to
enable fast and easy surface imaging. This image depicts additive manufactured AlSi10Mg alloy in cross-section, imaged with digital light microscopy.

6 7
Technology Highlight: Engineering
Understanding Material Transformations with in situ Microscopy
Observing materials in a static state
can reveal useful insights into their
microstructure, but there’s much more
to be learned from observing them
in situ under real service conditions.
Such techniques can teach us how
materials respond to changes in
imposed stimulus, behavior under
variable or extreme loads, initiation
and propagation of failure, or long-
term structural evolution.
ZEISS FE-SEMs use a field-free lens
design and a large distortion-free
field of view to ensure detection and
visualization of critical changes or
events in the sample.
600 N
1 mm
Figures 6: Here we see the evolution of 3D structures studied non-destructively using X-ray microscopy with 4D or ‘time-lapse’ imaging. A ceramic matrix
composite (CMC) was mounted within an in situ tensile rig to perform sequential steps of imaging and increasing load. These virtual cross-sections show crack
initiation and propagation through the structure. Ultimately, failure can be characterized in 3D at the micrometer scale.
8 9
Different stage options support pheno-
mena such as heating, mechanical load
requirements or integrated atomic force
microscopy (AFM).
Non-destructive 3D data obtained
with X-ray microscopy opens the
door to repetitive ‘4D’ in situ imaging.
Using optical architectures that
are unique compared to microCT,
these microscopes maintain very
high 3D spatial resolution, even for
samples mounted within in situ rigs
or chambers. Different load rigs can
be integrated to study such aspects
as heating, cooling and mechanical
loading.
Figure 5: 3D rendering of absorption contrast
tomography data of the CMC sample overlaid
with the strain fields (shown in color) computed
using Digital Volume Correlation (DVC).
750 N
1 mm
Developing Green Energy Devices
for Mobility and Sustainability
As natural resources become increasingly scarce and the
demand grows for more portable, reliable, safe and sustainable
forms of energy, scientists face new challenges in materials
research and engineering.
200 µm 1 µm 1 5 µm
Figure 7: This 3D X-ray tomography scan of an extracted cathode layer from a lithium ion battery has Figure 8: A portion of a solid oxide fuel cell is
undergone extensive cycling (left). An individual cathode particle is imaged with high resolution electron imaged with nanometer scaled X-ray microscopy.
1m
m microscopy, with contrast providing insight into local electrical behavior (right). Sample courtesy of: D. U. 3D data reveals local pore size measurements in
Sauer and E. Figgemeier, ISEA, RWTH Aachen University, DE. the cathode (top), porosity and cracking in the
electrolyte (center) and triple phase boundary
sites in the anode (bottom).
1050 N
Devices ranging from solar to fuel cells
and batteries—and the often highly
heterogeneous materials they contain—
offer the possibility of renewable and
clean energy conversion and storage.
Today’s researchers are focusing on the
fundamental mechanisms that dictate
50 µm
the performance of such devices in
order to extend the lifetime of current Figure 9: This image of a magnet used in Figure 10: Solar cell imaged with ZEISS LSM
1 mm
technologies, improve the efficiency e-motors, produced with Kerr microscopy, (confocal Laser Scanning Microscope). Typical
shows the stripe and closure domains in which application for research on solar cells in order
of future designs and ensure their safe
the magnitization is longitudinal or orthogonal to find suitable parameters for a laser scribe
operation. to the image plane. (blue conductive pass, green absorbing materials).
Image visualizes the quality and cleanliness of the
laser scribe pass.
In these investigations, microscope
technologies in multi-scale and multi-
modal approaches are essential to
understanding the links between
structure, chemistry and performance
in structural degradation, packaging
defects, 3D transport and diffusion,
local chemical effects, and electro-
chemical reactions and charge trans-
port.
Technology Highlight: Green Energy
Multi-scale and Correlative Workflows

A number of microscopic methods have evolved to investigate today’s varied and complex
material microstructures. These specialize in capturing a relatively specific window of scales,
modalities or dimensions of information.

200 µm 5 µm 5 µm

Figure 11: A high resolution, large-area image of a Li-ion battery electrode was produced with ZEISS MultiSEM, the unique multi-beam scanning electron
microscope from ZEISS. Acquisition time for the entire area of around 1 mm² was less than 7 minutes. For comparison: a state-of-the-art single beam SEM using
the same imaging parameters needs almost 3 hours to acquire the same area. The image reveals the heterogeneity and multi-scale nature of such structures,
with substantial morphology variations from the millimeter to micrometer scale. Correlative approaches can complement this type of analysis with additional
modalities or targeted imaging at particular length scales or locations.
Figure 12: ZEISS ZEN Connect, a software, has a graphical user interface tailored for correlative experiments, the so-called correlative workspace. It shows
information from various modalities: light microscopy and electron microscopy as well as EDX and Raman. This workspace enables easy navigation and overlay
It has become increasingly clear Correlative microscopy solutions of images while maintaining orientation and context of the sample across multiple scales and contrast mechanisms.
that understanding the diversity of empower researchers to move samples
microstructural features within a easily between instruments, relocating
given system—along with the physical targeted regions of interest and
a) c)
mechanisms they control—often collecting complementary information
requires studying a broad range of across different length scales and
information, well beyond the scope of modalities. These workflows enable
any individual technique. As a result, robust analysis for multi-scale or
there is a need for coordinated and multi-modal problems and also ease
efficient systems to navigate between, the complications associated with
and correlate data from, multiple identifying and navigating to specific
instrument platforms. or sparse locations when transferring
between low and high resolution
500 µm 2 µm
systems.
b) Figure 13: 3D correlation is used to identify and interrogate
subsurface regions of interest. Anomalous particles inside
a battery electrode were identified by X-ray microscopy (a),
which was used as a navigational aid to directly guide FIB-SEM
milling and imaging (b) along with EDX analysis (c) to specific
subsurface volumes.

100 µm 10 µm

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Microscopy Lab
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This illustration of a virtual core facility provides an ideal environment

to investigate or design new materials.

Discover your possibilities:

• understanding materials properties with light microscopy
• imaging and analyzing samples with SEMs
• perform 3D analysis with FIB-SEMs
• explore matter in 3D and 4D with XRMs
• revolutionize the speed of electron microscopy with MultiSEM
• leverage digital solutions to maximize the information you extract from
your specimens
• reach new levels of nanofabrication and nanoscale imaging with HIM

12 13
Powering Miniaturization Technology Highlight: Nanomaterials
Technologies with Functional and Nanopatterning and Nanofabrication
Nanomaterials

In the rapidly-evolving digital world, devices that are Microscope systems leveraging charged particle beams (electron and ion) open up exciting
simultaneously smaller, faster, and more efficient are being opportunities in the fields of nanopatterning and nanofabrication.
developed, largely by studying materials at length scales well
into the nanometer range, and sometimes even into the class
of 2D materials.
Moving well beyond the common use
of microscopes as imaging and analysis
possible by the superb low-voltage
FIB performance. Combining this with
“ofWe demonstrate the use
helium ion milling for the
tools, focused ion beams (FIBs) can be gas injection systems enables complex
controllable fabrication of
At these small length scales, unique electrical, magnetic, thermal and used to both image and modify samples processes such as etching and material
nanostructures in few-layer
properties emerge that are distinctly chemical properties. To understand and simultaneously, producing a variety deposition. In addition, ion systems can
different than they are at the bulk level, manipulate these properties, different of structures. These include photonic leverage unique gas field ion source
hexagonal boron nitride
leading to the concept of functional microscope technologies offer the arrays, nanoscale and semiconductor technology to generate He and Ne ion (h-BN).
materials with tailored properties. ability to observe, analyze and even devices, antenna structures and sensors, beams, making them ideal for the finest
Variations can be found and exploited modify the underlying structure and and micromechanical test specimens milling tasks and creating very high … This ability to pattern
in mechanical properties (strength), composition at the nanoscale. as well as damage-free samples for aspect ratio structures and lithography h-BN sheets with high-
but also optical (photonics), acoustic, other techniques such as transmission patterning, free from proximity effects. throughput and sub-10 nm
electron microscopy (TEM)—all made
precision paves the way
for future studies that make
use of atomically-thin,
nanostructured insulators
such as those needed for
2 µm 2 µm nanopore sequencing and
patterned van der Waals

2 µm 2 µm 1 µm
heterostructures.
”
Figures 15: Preparation of samples for TEM or other techniques can require a high level of milling
precision. Left: Excellent low voltage performance is mandatory for final milling and polishing of
S.M. Gilbert, University of
damage-free samples. Right: TEM image of resulting lamella. California, Berkeley
from: Gilbert et al.,
MRS Advances, 3, Issue 6-7, 2018,
pp. 327-331. DOI: 10.1557/adv.2018.117

1 µm

Figure 14: Helium ion beam imaging offers the high resolution and surface sensitivity required to image 5 µm
challenging samples such as this freestanding graphene sheet grown on GaN pillars.
Figure 16: Patterning of elaborate designs or structures are performed with high resolution ion beam
milling. Left: A meandering nanofluidic channel with tapered inlets was produced for DNA sequencing
studies. Right: patterning of a Fresnel zone plate optical structure.

14 15
Technology Highlight: Nanomaterials
More Diverse Information from Multi-modal and Analytical
Microscopy
Microscope technologies provide the ideal platform for analysis
of a material’s elemental, chemical and crystallographic
structure.
Building on the familiar energy dis-
persive spectroscopy (EDS or EDX)
technique for SEM, field emission (FE)
SEM systems have leveraged the latest
advances in EDS detector technology to
push spatial mapping resolution down
to tens of nanometer—with sensitivity
for elements as light as lithium. For
chemical mapping of binding states,
RISE (Raman Imaging and Scanning
Electron) microscopy integrates
correlative electron and confocal
Raman mapping without breaking
the chamber vacuum.
When more sensitive analysis is
required, secondary ion mass spectros-
copy (SIMS) is performed using ion
beam systems. Pushing resolution into
the nanometer scale with extreme
sensitivity achieves the ultimate in
16
6 µm
Figure 17: Raman imaging of MoS 2, overlaid on the SEM view, was performed on an SEM system with
integrated Raman spectroscopy. CVD-grown MoS 2 2D crystals on Si/SiO2 substrate, crystals (green),
multilayers (blue) and single layers (red).
surface analysis of functional materials.
In the field of crystallographic imaging,
the diffractive power of X-rays is
used to perform diffraction contrast
tomography (LabDCT) in a lab-based
X-ray microscope. LabDCT complements
the traditional 3D X-ray absorption
contrast imaging (which provides
density information) by capturing
diffraction patterns originating
from polycrystalline samples. Such
patterns can then be computationally
reconstructed to provide an internal
3D map of the position, shape and
orientation of the various grains within
the sample (compare Fig. 3).
Biomaterials:
Connecting with and Learning from the Natural
World
Scientists come up against a unique set of challenges
when developing materials that are compatible with
the biological world. Not only the chemistry, but the
structure, geometry and properties of devices must be
carefully designed for compatibility and effectiveness
with the host. This includes pharmaceutical tablets and
drug delivery systems, soft tissue scaffolds, biological
implants and topical gels. Validating and improving
these designs requires microscopic characterization,
often on sensitive and complex material structures.
Figure 19: This height map shows
the surface topography of a portion
of a biomedical implant, acquired
with a confocal laser scanning
microscope. The texture of the
surface has a substantial influence
on the osseointegration of the
implant with the host tissue.
Figure 20: Imaging sensitive or fragile materials
in their native states can prove difficult. Cryogenic
freezing, such as performed here on skin cream
500 nm
emulsion, can be used to stabilize structures
during imaging and thereby reduce the chances
Figure 18: SIMS on CIGS (copper indium
gallium selenide) solar cell was produced with a
of damage or modification under even minor
heating or charged particle radiation. In this
helium/neon ion system. Green and red indicate
image the structure was examined by cryo field
higher concentration of Na and K at the grain 200 nm
emission scanning electron microscopy.
boundaries.
17
 Technology Highlight: Biomaterials
Entering a New Dimension with 3D Characterization

At the same time, the natural world presents an abundance of inspiration for engineering design
based on the mimicry of organisms and structures that have benefited from millions of years of
evolutionary refinement. By observing and understanding some of the unique mechanisms that
exist in the biological world, we can gain insights into how to improve the properties of our own
range of synthetically engineered materials. Opportunities to understand and apply such micro-
scale knowledge abound in functional materials (photonics), specialized surfaces (engineered
adhesion or hydrophobicity) or incredibly high strength-to-weight ratio microstructures.
In materials science, two-dimensional microscopy and the analysis of the sample surface is
often not sufficient for the full characterization of the microstructure. Precise measurement of
particle or phase sizes, shapes and distributions, the extent of defects, inclusions, voids or cracks,
porosity, pore connectivity and tortuosity, etc. all call for 3D studies. Furthermore, validating and
guiding the development of models for materials also benefits from 3D characterization.

“usUnderstanding of a biomaterial at the microscale helps

understand form and function of that organism in its
Addressing these challenges requires a
comprehensive portfolio for 3D imaging
across multiple length scales, from
environment, and we can learn from that and bring that back
macro to nano. Confocal laser scanning
to inform engineering and design developments…It’s really
microscopes (LSMs) provide optical
important that we have cutting edge microscopy equipment surface topography and roughness
to allow us to characterize materials at varying length scales measurements. For internal structures,
and varying modalities – they could be manufactured, human- FIB-SEM tomography pushes nanoscale
made materials or biological materials. ” SEM imaging into the third dimension
with precise control of sequential
Prof. Richard Johnston milling and imaging tasks to provide
Swansea University, Co-Director of Advanced Imaging of Materials Facility exceptional isotropic resolution for
400 µm
imaging/analytics. Complementing
5 µm
FIB-SEM, researchers have increasingly Figure 22: 3D view and virtual cross-section of a cuttlefish bone acquired by X-ray microscopy. The

exploited the non-destructive nature cuttlefish bone displays a very anisotropic columnar structure, contributing to the organism’s unique
mechanical and biological properties (scale bar valid for both images).
Figure 21: 3D microscope technology provides of X-rays to observe internal features
the resolution and contrast needed to interrogate in 3D as well as 4D (3D plus time
and learn from complex natural structures. The
or stimulus) with different contrast
photonic crystals of a butterfly wing, shown here
in three dimensions after imaging on a nanoscale methods, including absorption, phase
X-ray microscope, provide its colorful appea- and diffraction contrast tomography.
rance. It is possible to observe discrete faceted
crystallites that help scientists better understand
the formation and function of this biological
nanostructured material.

1 mm

Figure 23: In situ three-dimensional imaging (‘4D imaging’) of a pharmaceutical tablet by X-ray
microscopy is used to provide direct visual insight into the dissolution and diffusion processes in drug
delivery. Orange shading represents the tablet, green is an osmogen to induce water uptake and blue
is the drug-saturated fluid as it emerges from a pre-drilled laser hole at the bottom of the tablet.

18 19
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EN_42_010_296 | Version 1.0 | CZ 08-2019 | Design, scope of delivery and technical progress subject to change without notice. | © Carl Zeiss Microscopy GmbH