Opportunities in 3D and 4D Imaging with X-ray Microscopy In the materials and life sciences research laboratory
Nicolas Gueninchault Product Application and Sales Specialist for XRM – EMEA/LATAM [email protected] A Strong Foundation for a Strong Future
The Founder and his partner
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 Carl Zeiss Ernst Abbe new products and business areas that enabled Founder Partner the company to meet its customers’ needs.
Carl Zeiss Microscopy 2 Over 30 Nobel laureates worldwide use ZEISS instruments to achieve progress in science
Sir Paul M. Nurse Leland H. Hartwell Eric Betzig Timothy Hunt Stefan W. Hell Physiology/Medicine William E. Craig C. Mello Moerner Andrew Z. Fire Chemistry Robert Koch Allvar Gullstrand Manfred Christiane Physiology/Medicine In close collaboration with ZEISS staff Physiology/Medicine Physiology/Medicine Eigen Nüsslein- In close collaboration Chemistry Volhard with ZEISS staff John O'Keefe Physiology/Medicine Eric A. Andre Geim May-Britt Cornell Konstantin Physics Novoselov Moser Edvard In close Physics I. Moser collaboration Physiology/Medicine with ZEISS staff
1905 1906 1911 1925 1952 1953 1967 1991 1995 1999 2001 2002 2006 2008 2010 2011 2012 2013 2014 2018
Sidney Brenner Sir John B. Gurdon Richard Adolf Bert Sakmann Zsigmondy H. Robert Shinya Yamanaka Arthur Ashkin Erwin Neher Physiology/Medicine Chemistry Physiology/Medicine Horvitz Gérard Mourou In close collaboration John E. Sulston Dan Shechtman Donna Strickland with ZEISS staff Physiology/Medicine Chemistry Physics Günter Blobel Physiology/Medicine Harald zur Hausen Santiago Ramón y Frits Zernike Physiology/Medicine Cajal Camillo Golgi Physics Physiology/Medicine In close collaboration Osamu Shimomura with ZEISS staff Ahmed A. Zewail Chemistry Martin Chalfie Roger Tsien Chemistry
In close collaboration with ZEISS staff
Carl Zeiss Microscopy 3 Why Do We Use X-ray Microscopy? Materials characterization in 3D
Visualize, characterize, and quantify internal three dimensional structures of objects without physical cutting
Carl Zeiss Microscopy 4 Tomography in 3D X-ray Microscopy How it works
ZEISS Xradia Versa Detector
Projections Sample
Source
3D Reconstruction
Quantitative Analysis Virtual slices
Carl Zeiss Microscopy 5 3D X-ray Imaging for Research Applications
X-ray microCT X-ray Microscopy Synchrotron technology extended to the lab
Projection-based geometric Transmission XRM architecture with Two-stage magnification with magnification architecture X-ray focusing optics (condenser, scintillator-coupled optical objectives zone plate) Xradia Context Xradia Versa Family Xradia Ultra Family
Other Commercial Systems
0.95 μm spatial resolution
0.5 μm spatial resolution, RaaD 50 nm spatial resolution
Carl Zeiss Microscopy 6 ZEISS Xradia Ultra 3D X-ray nanotomography down to 50 nm resolution
The only non-destructive, laboratory based 3D imaging solution with resolution down to 50 nm: Ideal for 4D and in situ studies
• High brightness X-ray source 50 nm • 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 View Large Field of View 200X 150 nm 64 nm 65 µm x 65 µm High Resolution 800X 50 nm 16 nm 16 µm x 16 µm
Objective lens X-ray source Phase ring X-ray camera Condenser lens Sample (Zone Plate)
Carl Zeiss Microscopy 7 ZEISS A complete 3D microscopy portfolio
Metrotom 1 X-ray CT
10-1
10-2 Xradia Versa Sub-micron 3D X-ray Microscope Xradia Context 10-3 mm microCT
10-4 samplesize [m]
10-5 Xradia Ultra Nanoscale 3D X-ray Microscope Crossbeam -6 micron 10 FIB-SEM ORION Nanofab HIM micron nanometer 10-7 10-3 10-4 10-5 10-6 10-7 10-8 10-9 3D Voxel Dimension [m]
Carl Zeiss Microscopy 8 Analysis and Measurements
Local Cathode Thickness (μm) Local Size 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 Measurements ORS Dragonfly Pro used to measure the local variation in feature sizes of the LSM network
LSM Anode Triple Phase Boundary Visualization Generated by a series of dilations on the NiO, YSZ, and pore phases, shows the locations of electrochemical reaction sites
Voids in YSZ Electrolyte
YSZ
NiO TPB
5 μm
Carl Zeiss Microscopy 9 3D nano-XRM of human hair Effects of treatments on the internal structure
Natural Treated
Pores Hair Pin Epoxy
Pores Melanosomes Melanosomes
Carl Zeiss Microscopy 10 ZEISS A complete 3D microscopy portfolio
Metrotom 1 X-ray CT
10-1
10-2 Xradia Versa Sub-micron Xradia Context 3D X-ray Microscope 10-3 mm microCT
10-4 samplesize [m]
10-5 Xradia Ultra Nanoscale 3D X-ray Microscope Crossbeam -6 micron 10 FIB-SEM ORION Nanofab HIM micron nanometer 10-7 10-3 10-4 10-5 10-6 10-7 10-8 10-9 3D Voxel Dimension [m]
Carl Zeiss Microscopy 11 Limitations of microCT Geometric Magnification “You can only get so close”
With microCT architecture…
…you can image the whole object… …and then you can zoom in a little. But if you want to see the small things (seed), you need to cut it open
Carl Zeiss Microscopy 12 Chopping Up Samples for Higher Resolution When 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 There are frequent cases to cut? where working with larger or …you are working inside an in situ chamber or rig? intact samples is beneficial Carl Zeiss Microscopy 13 X-ray Microscopy with Two-Stage Magnification Geometric + optical magnification
ZEISS Xradia Versa - Multiple scintillator-coupled optics for different magnification
Scintillators
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 Optical Magnification (not visible)
Carl Zeiss Microscopy 14 What Can We Do with RaaD? Not just for apples
Analysis of lithium ion batteries is challenging – many critical quality and safety effects only become apparent with aging.
Full-field of view 0.4x 4x 20x
. 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
Carl Zeiss Microscopy 15 X-ray Microscopy with RaaD Advantage over microCT
Traditional X-ray microCT ZEISS Xradia Versa
Carl Zeiss Microscopy 16 XRM Maintains High Resolution at Large Working Distances
XRM 2-stage magnification architecture
Traditional microCT architecture
Carl Zeiss Microscopy 17 Diversity of Applications in Academia Both the appeal and the challenge
Mouse knee
8” concrete Indented rat ulna Plant root
3D printed Al
Solderball interconnects
Geological 18650 Li-ion battery core sample
Carl Zeiss Microscopy 18 Materials Science Applications for X-ray microscopy
Polymers & Biomaterials Energy Materials Ceramics Composites
Metals Coatings Glass Concrete
Carl Zeiss Microscopy 19 Beyond Absorption (Density) Contrast
Advanced absorption with Propagation phase contrast for edge optimized scintillator optics enhancement & low density phases Dual scan contrast visualizer (DSCoVer) for differentiating similar-Z phases
Mobile phone camera lens assembly Vasculature in wood
Diffraction contrast tomography (LabDCT) to map polycrystalline materials Al-Si composite Ti alloy
Carl Zeiss Microscopy 20 Propagation Phase Contrast – insect in amber
Propagation phase contrast signal removed Absorption contrast removed
Carl Zeiss Microscopy 21 LabDCT with GrainMapper3D provides Comprehensive 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 3D grain map of an Armco iron sample. crystal reference system. Half the sample volume is removed to reveal inner grain (clusters). Courtesy of Prof. Burton R. GB processed with Dream3D Patterson, University of Florida, United States.
Carl Zeiss Microscopy 22 Some examples Combining ACT and DCT, Various applications
Grain structure in geological materials Pankhurst et al. 2019
Partial recrystallization in AlSi Courtesy of Prof. Dorte Juul Jensen, DTU 200 μm
Al-%4Cu alloy – inclusions and grain microstructure Courtesy of Prof. Masakazu Kobayashi, Toyohashi University of Technology 300 μm
Carl Zeiss Microscopy 23 LabDCT Grain growth kinetics in Armco Iron
Normal Grain Growth Abnormal Grain Growth
Large grain growth is typically unwanted as it can lead to failure
Carl Zeiss Microscopy 24 Applications in Material Sciences PUTTING XRM TO WORK
Carl Zeiss Microscopy 25 18650 Li-ion Battery High resolution interior tomography
High res interior tomography
• Intact 18650 Li ion battery Full field of view, entire object scan
Carl Zeiss Microscopy 26 Carl Zeiss Microscopy 27 18650 Li-ion Battery High resolution interior tomography
Legend Cathode Anode Al current collector Cu current collector
Carl Zeiss Microscopy 28 Additive Manufacturing Characterization of feedstock powder
Broad range of particle size
Non-spherical morphology
Likely satellite particles
Internal porosity Large 3D statistics using XRM
Carl Zeiss Microscopy 29 Additive Manufacturing Inconel 3D printed lattice structure
8 um/voxel • Structural integrity • Internal defects (porosity, impurities) 3.5 um/voxel Sample courtesy of Kavan Hazeli, Mechanical and Aerospace • Surface roughness Engineering, The University of Alabama, Huntsville
Carl Zeiss Microscopy 30 Additive Manufacturing Inconel 3D printed lattice structure
8 um/voxel • Structural integrity 3.5 um/voxel • Internal defects (porosity, impurities) Sample courtesy of Kavan Hazeli, Mechanical and Aerospace • Surface roughness Engineering, The University of Alabama, Huntsville
Carl Zeiss Microscopy 31 Building Materials Analysis of phases in concrete
• Interior tomography to target large particle • Strong absorption contrast reveals numerous solid phases • Aggregate particles segmented and can be quantified by size, shape, etc.
High Res
FFOV
Carl Zeiss Microscopy 32 ZEISS Microscopy Portfolio Multi-scale characterization for multi-scale research
An extensive microscopy portfolio…
Stereo microCT Sub-micron Widefield Polarized Confocal Nanoscale Helium Ion MultiSEM C-SEM FE-SEM FIB-SEM LM XRM LM LM LM XRM Microscope
1 μm < 1 μm 500 nm 250 nm 200 nm 200 nm < 50 nm < 4 nm < 2 nm < 1 nm < 1 nm < 0.5 nm
…to address multi-scale research challenges.
Carl Zeiss Microscopy 33 Richer datasets with analytical features of SEMs AA7075 – Linking XRM with FIB-SEM
XRM Data used to identify a representative volume element (RVE) Adding Imaging modalities Decreasing length scale
TOF-SIMS
Digging Deeper L S T
X-ray microscopy FIB tomography
• Grain size & shape • High-resolution localization • Inclusion distribution • Nano-scale precipitates • ROI / RVE identification • Grain contrast S. Singh et al., Materials Characterization 118 (2016). Femtosecond Laser
Carl Zeiss Microscopy 07.10.2020 34 [email protected]
Carl Zeiss Microscopy 07.10.2020 35