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Plymouth Electron Microscopy CentreMulti-Scale Characterization for Multi-Scale Research

ZEISS Crossbeam

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Diverse Fields of Application…

Materials Research

• Task: Understand and tailor physical properties of materials. Develop new materials.

• Examples: Steels, Alloys, Polymers, Ceramics, Composites

• Image: Manganese sulfide inclusions in steel. Courtesy of Georgsmarienhütte GmbH, Germany

Earth & Planetary Sciences

• Task: find new profitable deposits of natural resources

• Examples: Oil&Gas (sedimentary rocks, shale), Mining

• Image: Pyrites and voids in shale rock. Courtesy of NanoFUN, Poland

Electronics / Semiconductors

• Task: Design better and more efficient electronic devices. Failure Analysis.

• Examples: Semiconductors, Polymer Electronics, Photonics

• Image: Cross-Section of IC with Intel 22nm-Tri-Gate-technology. Courtesy of UBM TechInsights, Canada

Advanced Manufacturing

• Task: quality control of material systems used in different industries (e.g. automotive)

• Examples: Coatings, Oxidation, Corrosion, Irradiation

• Image: Crack in steel sheet. Courtesy of AUDI AG, Germany

Materials Development

• Task: Design materials and functional nanostructureswith improved or new physical properties

• Examples: Metamaterials, MEMS, Biomaterials

• Image: Focused-Ion-Beam Nanofabrication of Near-Infrared Magnetic Metamaterials, Enkrich et al. Adv. Mater. 17 (2005)

Life Sciences

• Task: understand structure and function of biological material

• Examples: Cell biology, Neurobiology, Histology, Zoology, Botany

• Image: drosophila larval brain. Courtesy of C. Shan Xu, HHMI, USA

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ZEISS CrossbeamAn essential tool for materials science

Imaging &

Analytics

Tomography

Sample

Prep

Nanopatterning

Maximum useable SEM and FIB FOV

Ag / Ni / Cu sample

Sample courtesy of D. Willer, MPA StuttgartImaging with Quad mode

…more information in less time

InLens

EsB

SE2

InLens + SE2

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Live ImagingHigh throughput SEM imaging while milling

FIB patterning of a spiral in Si.

Spiral pitch and line width are

150 nm and 20 nm, respectively.

Frames of a movie, InLens signal Same structure, ETSE signal

Multi-Scale Characterization of LIB Cathode Imaging & Analysis in the FIB-SEM

2 µm

InLens SE

2 µm

InLens EsB

2 µm Mn La

EDS

FIB-SEM

Preparation and Analysis of STEM SamplesHigh Resolution STEM and EDS Study of Cr Depletion in Stainless Steel

(A) STEM image of a grain boundary (GB) of heat affected a X2CrNi18-10 steel sample showing corrosion

(B) Chromium carbides form at the GB and cause chromium depletion of the matrix

(C,D) EDS analysis (15 kV) shows high spatial resolution and allows to quantify the extent of chromium depletion

Cr Fe

Pillars for Compression Tests High entropy alloy

Array milling = 13.5 h

(~33 min per pillar)

• Preparation of pillars for compression testing experiments

• Lathe milling was used to obtain perfectly perpendicular pillar walls.

• The lathe milling step was automatized using the API of the Crossbeam instrument.

FIB Direct Patterning

Array of annular shapes

Each shape is 450 nm in

diameter with 1 μm spacing

(pitch) between shapes

Nano-channels

FOV = 59 µm

3D Milling

3D structure milled into silicon

using Atlas 5 Nanopatterning

3D-Profiler tool

FOV = 30 µm

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FIB Direct Patterning

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Tomography with ZEISS Crossbeam

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FIBMilling

SEMImaging

=+ Nanotomography

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Sample: Resin-Embedded B. subtilis bacteriaCourtesy of Kedar Narayan, Subramaniam Group, NIH NCI, USA

High Resolution in 3DApplication to Biological Sciences

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High Resolution in 3DApplication to Biological Sciences

Aluminum Alloy 7075-T651

SEM @ 1.5kV, 5nA

820 slices

Voxel size = (10 x 10 x 10) nm³

Sample courtesy of N. Chawla and S. Singh, Arizona State University

High Resolution in 3DApplication to Materials Science

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courtesy of M. Cantoni, EPFL Lausanne

High Resolution in 3Dwith combined Imaging & Chemical Analysis

1.8 kV, Inlens SE

Voxel = (10 x 10 x 10) nm³

6 kV, EDS

Voxel = (40 x 40 x 100) nm³

Ag

Cu

5 µm

Lead free solder contains Sn,

Ag, and Cu.

High Resolution in 3DApplication to Earth & Planetary Science

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High Resolution in 3Dwith combined imaging, EDS & Structural Analysis…