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