Opportunities in 3D and 4D Imaging with X -ray Microscopy ... X-ray... · Opportunities in 3D and...

Opportunities in 3D and 4D Imaging with X-ray MicroscopyIn the materials and life sciences research laboratory

Nicolas GueninchaultProduct Application and Sales Specialist for XRM – EMEA/LATAM

[email protected]

2Carl Zeiss Microscopy

Carl Zeiss founded a workshop for precision mechanics and optical instruments in Jena in 1846. Ernst Abbe – a young science professor and collaborator with the company – joined and became a partner in 1876.

Optical technologies pave the way for many innovations. Zeiss and Abbe recognized this early on, and this led to the creation of innovative new products and business areas that enabled the company to meet its customers’ needs.

The Founder and his partner

A Strong Foundation for a Strong Future

Carl ZeissFounder

Ernst AbbePartner


Over 30 Nobel laureates worldwide use ZEISS instruments to achieve progress in science

1906 1911 1925 1952 1953 1967 1991 1995 1999 2001 20021905 20082006 20112010 2012 2013 2014

Robert KochPhysiology/Medicine

Allvar GullstrandPhysiology/Medicine

ManfredEigen Chemistry

Christiane Nüsslein-Volhard Physiology/Medicine

Sir Paul M. Nurse Leland H. HartwellTimothy Hunt Physiology/Medicine

Craig C. Mello Andrew Z. FirePhysiology/Medicine

Andre GeimKonstantin NovoselovPhysics

Eric BetzigStefan W. HellWilliam E. MoernerChemistry

Sir John B. GurdonShinya Yamanaka Physiology/Medicine

John O'Keefe May-Britt Moser Edvard I. MoserPhysiology/Medicine

Eric A. CornellPhysics

Richard Adolf Zsigmondy Chemistry

Bert Sakmann Erwin Neher Physiology/Medicine

Harald zur HausenPhysiology/Medicine

Osamu ShimomuraMartin ChalfieRoger TsienChemistry

Sidney Brenner H. Robert HorvitzJohn E. Sulston Physiology/Medicine

Dan ShechtmanChemistry

Santiago Ramón y Cajal Camillo GolgiPhysiology/Medicine

Frits ZernikePhysics

Günter Blobel Physiology/Medicine

Ahmed A. ZewailChemistry

In close collaboration with ZEISS staff






2018

Arthur AshkinGérard MourouDonna StricklandPhysics


Why Do We Use X-ray Microscopy?Materials characterization in 3D

Visualize, characterize, and quantify internal three dimensional structures of objects without physical cutting


Tomography in 3D X-ray MicroscopyHow it works

Projections

3D Reconstruction

Virtual slicesQuantitative

Analysis

ZEISS Xradia Versa

Source

Sample

Detector


3D X-ray Imaging for Research Applications

Xradia Versa Family Xradia Ultra FamilyXradia Context

X-ray microCT X-ray MicroscopySynchrotron technology extended to the lab

0.95 μm spatial resolution

0.5 μm spatial resolution, RaaD 50 nm spatial

resolution

Other Commercial Systems

Projection-based geometric magnification architecture Two-stage magnification with

scintillator-coupled optical objectivesTransmission XRM architecture with

X-ray focusing optics (condenser, zone plate)


ZEISS Xradia Ultra 3D X-ray nanotomography down to 50 nm resolution

• High brightness X-ray source• Xradia 810 Ultra: 5.4 keV• Xradia 800 Ultra: 8.0 keV

• 50 nm spatial (16 nm voxel) resolution • Advanced X-ray optics• Absorption and Zernike phase contrast

Mode Mag 2D Res Voxel Field of ViewLarge Field of View 200X 150 nm 64 nm 65 µm x 65 µmHigh Resolution 800X 50 nm 16 nm 16 µm x 16 µm

50 nm

The only non-destructive, laboratory based 3D imaging solution with resolution down to 50 nm: Ideal for 4D and in situ studies

X-ray source Condenser lens SampleObjective lens (Zone Plate)

Phase ring X-ray camera


ZEISSA complete 3D microscopy portfolio

3D Voxel Dimension [m]10-3 10-4 10-5 10-6 10-7 10-8

sam

ple

size

[m]

1

10-1

10-2

10-3

10-4

10-5

10-6

Xradia UltraNanoscale3D X-ray Microscope

FIB-SEM

10-9

10-7HIM

Crossbeam

ORION Nanofab

micron nanometer

micron

mm

MetrotomX-ray CT

Xradia VersaSub-micron 3D X-ray Microscope

Xradia ContextmicroCT


Analysis and Measurements

0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Local Cathode Thickness (μm)

Voids in YSZElectrolyte

YSZ

NiO

LSM

5 μm

Local Size Measurements ORS Dragonfly Pro used to measure the local variation in feature sizes of the LSM network

Anode Triple Phase Boundary VisualizationGenerated by a series of dilations on the NiO, YSZ, and pore phases, shows the locations of electrochemical reaction sites

TPB


3D nano-XRM of human hairEffects of treatments on the internal structure

Natural Treated

Hair

EpoxyPin

Pores

Melanosomes

Pores

Melanosomes


ZEISSA complete 3D microscopy portfolio

3D Voxel Dimension [m]10-3 10-4 10-5 10-6 10-7 10-8

sam

ple

size

[m]

1

10-1

10-2

10-3

10-4

10-5

10-6

Xradia UltraNanoscale3D X-ray Microscope

FIB-SEM

10-9

10-7HIM

Crossbeam

ORION Nanofab

micron nanometer

micron

mm

MetrotomX-ray CT

Xradia ContextmicroCT

Xradia VersaSub-micron 3D X-ray Microscope


Limitations of microCT Geometric Magnification“You can only get so close”

…you can image the whole object… …and then you can zoom in a little.

With microCT architecture…

But if you want to see the small things (seed), you

need to cut it open


Chopping Up Samples for Higher ResolutionWhen all you have is microCT geometric magnification

Cutting an apple might be OK, but what if……it is a precious sample you can’t destroy?

…it is an intact device (battery, electronics component)?…cutting your sample risks damaging the structure?…you need to preserve your sample for future studies?…you have sparse features and don’t know where to cut?…you are working inside an in situ chamber or rig?

There are frequent cases where working with larger or intact samples is beneficial


X-ray Microscopy with Two-Stage MagnificationGeometric + optical magnification

Optical Magnification

Scintillators

ZEISS Xradia Versa -Multiple scintillator-coupled

optics for different magnification

Only an X-ray microscope can scan an apple seed at high resolution without cutting the apple open (RaaD = Resolution at a Distance) CCD Detector

(not visible)


What Can We Do with RaaD?Not just for apples

0.4x 4x 20xFull-field of view

X-ray microscopes (XRM) scan the intact battery to identify areas of interest and zoom-in for high resolution imaging With traditional X-ray microCT to scan at this resolution requires complete disassembly of the battery - requiring

glovebox and solvents, skill and time

Analysis of lithium ion batteries is challenging – many critical quality and safety effects only become apparent with aging.


X-ray Microscopy with RaaDAdvantage over microCT

Traditional X-ray microCT ZEISS Xradia Versa


XRM Maintains High Resolution at Large Working Distances

Traditional microCT architecture

XRM 2-stage magnification architecture


Diversity of Applications in AcademiaBoth the appeal and the challenge

8” concrete

18650 Li-ion battery

3D printed Al

Indented rat ulna

Mouse knee

Plant root

Geological core sample

Solderball interconnects


Materials ScienceApplications for X-ray microscopy

Polymers & Biomaterials Energy Materials Ceramics Composites

Metals Coatings Glass Concrete


Beyond Absorption (Density) Contrast

Advanced absorption with optimized scintillator optics

Mobile phone camera lens

assembly

Propagation phase contrast for edge enhancement & low density phases

Vasculature in wood

Dual scan contrast visualizer (DSCoVer)for differentiating similar-Z phases

Al-Si composite

Diffraction contrast tomography (LabDCT) to

map polycrystalline materialsTi alloy


Propagation Phase Contrast – insect in amber

Propagation phase contrast signal removed Absorption contrast removed


LabDCT with GrainMapper3D providesComprehensive Information on Grain Structure

GrainMapper3D offers: Grain Centroid Position

Grain Size

Grain Orientation

Grain Shape

Grain Boundary Information

Left-right: Faces of a selected grain color coded in random color, by IPF color, misorientation to neighboring grains, grain boundary curvature and grain boundary normal direction in crystal reference system.

3D grain map of an Armco iron sample.Half the sample volume is removed to reveal inner grain (clusters). Courtesy of Prof. Burton R. Patterson, University of Florida, United States.GB processed with Dream3D


Some examplesCombining ACT and DCT, Various applications

Al-%4Cu alloy –inclusions and grain microstructureCourtesy of Prof. Masakazu Kobayashi, Toyohashi University of Technology

Partial recrystallization in AlSiCourtesy of Prof. Dorte Juul Jensen, DTU

Grain structure in geological materials

300 μm

200 μm

Pankhurst et al. 2019


LabDCTGrain growth kinetics in Armco Iron

Normal Grain Growth Abnormal Grain Growth

Large grain growth is typically unwanted as it can lead to failure


PUTTING XRM TO WORKApplications in Material Sciences


18650 Li-ion BatteryHigh resolution interior tomography

• Intact 18650 Li ion battery

Full field of view, entire object scan

High res interior tomography


18650 Li-ion BatteryHigh resolution interior tomography

LegendCathodeAnodeAl current collectorCu current collector


Additive ManufacturingCharacterization of feedstock powder

Broad range of particle size

Non-spherical morphology

Internal porosity

Likely satellite particles

Large 3D statistics using XRM


Additive ManufacturingInconel 3D printed lattice structure

8 um/voxel3.5 um/voxel

• Structural integrity• Internal defects (porosity, impurities)• Surface roughness

Sample courtesy of Kavan Hazeli, Mechanical and Aerospace Engineering, The University of Alabama, Huntsville


Additive ManufacturingInconel 3D printed lattice structure

8 um/voxel3.5 um/voxel • Structural integrity

• Internal defects (porosity, impurities)• Surface roughness

Sample courtesy of Kavan Hazeli, Mechanical and Aerospace Engineering, The University of Alabama, Huntsville


Building MaterialsAnalysis of phases in concrete

FFOV

High Res

• Interior tomography to target large particle • Strong absorption contrast reveals numerous

solid phases• Aggregate particles segmented and can be

quantified by size, shape, etc.


ZEISS Microscopy PortfolioMulti-scale characterization for multi-scale research

An extensive microscopy portfolio…

…to address multi-scale research challenges.

Stereo LM

Sub-micron XRM

WidefieldLM

PolarizedLM

Confocal LM

NanoscaleXRM C-SEM FE-SEM FIB-SEM Helium Ion

Microscope

1 μm 500 nm 250 nm 200 nm 200 nm < 50 nm < 2 nm < 1 nm < 1 nm < 0.5 nm

MultiSEM

< 4 nm

microCT

< 1 μm

3407.10.2020Carl Zeiss Microscopy

Richer datasets with analytical features of SEMsAA7075 – Linking XRM with FIB-SEM

L

ST

Decreasing length scale

X-ray microscopy FIB tomography

• Grain size & shape• Inclusion distribution• ROI / RVE identification

• High-resolution localization• Nano-scale precipitates• Grain contrast

XRM Data used to identify a representative volume element (RVE)

S. Singh et al., Materials Characterization 118 (2016).

Adding Imaging modalities

TOF-SIMS

Digging Deeper

Femtosecond Laser

3507.10.2020Carl Zeiss Microscopy

[email protected]

Opportunities in 3D and 4D Imaging with X -ray Microscopy ... X-ray... · Opportunities in 3D and...

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