Advanced MicroCT for Non-Destructive 3D Multiscale Analysis
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The document discusses the capabilities and applications of advanced microcomputed tomography (microCT) technology, highlighting its versatility across various sectors including consumer goods, life sciences, and additive manufacturing. It emphasizes how microCT enables non-destructive 3D imaging to analyze materials' structures and properties, making it a valuable tool for research and quality control. The presentation also invites collaboration and encourages researchers to explore how microCT can benefit their specific fields of study.
Advanced MicroCT for Non-Destructive 3D Multiscale Analysis
- 1. Advanced MicroCT for Non- destructive 3D Multiscale Analysis Robert E. A. Williams, PhD Assistant Director for Research and Development CEMAS Mark Riccio Product Marketing Manager for X-ray microCT Thermo Fisher Scientific
- 2. Advanced MicroCT for Non- destructive 3D Multiscale Analysis Experts showcase the depth of applications that are possible with advanced MicroCT.
- 3. Robert E. A. Williams, PhD Advanced MicroCT for Non- destructive 3D Multiscale Analysis Assistant Director for Research and Development Center of Electron Microscopy and Analysis (CEMAS) at The Ohio State University Proprietary & Confidential | 2021 3
- 4. CEMAS Center for Electron Microscopy and AnalysiS Robert E.A. Williams Assistant Director of Research and Development williams.2156@osu.edu David W. McComb Director, Center for Electron Microscopy and Analysis mccomb.29@osu.edu cemas.osu.edu Mark L. Riccio Product Marketing Manager, X-ray Imaging mark.riccio@thermofisher.com thermofisher.com
- 6. 6 CEMAS Instrumentation (Scanning) Transmission Electron Microscopy • Titan 60-300 Image Corrected • Themis Z Probe Corrected • Tecnai TF20 TEM • Tecnai T30 TEM • Glacios cryo-TEM • Titan Krios image corrected cryo-TEM Focused Ion Beam • Helios 600 Dual Beam • Nova 600 Dual Beam Scanning Electron Microscopy • Apreo FEG SEM (analytical) • Apreo FEG SEM (high resolution) • Quanta SEM • Quattro Environmental SEM Other Analytical Techniques • Heliscan X-ray MicroCT • XRD • Nanoindentation
- 7. Local Operating Environments Environmental Requirements • Temperature Stability • Power Quality and Availability • Electromagnetic Interference • Mechanical Vibration
- 9. Hamish L. Fraser Professor Michael J. Mills Professor David W. McComb Professor Jinwoo Hwang Assistant Professor David B. Williams Professor, Dean CoE CEMAS Faculty Vicky Doan-Nguyen Assistant Professor Frank J. Scheltens Associate Professor of Practice
- 10. CEMAS Staff Henk Colijn Assistant Director Res. Operations Binbin Deng, Ph.D. Cryo/Bio Daniel Huber, Ph.D. Assistant Director Infrastructure Robert Williams, Ph.D. Assistant Director Res. Develop Daniel Veghte, Ph.D. SEM Carley Goodwin X-ray MicroCT Yoshie Narui, Ph.D. Cryo/Bio
- 11. Outline • Introduce Micro CT and how the system fits in a multi scale characterization facility • Present MicroCT examples from: • Consumer goods and health care • Life Science application • 3D printing and Additive manufacturing • Cybersecurity, electronics and semiconductor sectors The goal of this talk is to introduce the versatility of the MicroCT across a variety of material systems and engineering sectors. While applications presented may not be on your specific area of interest, I encourage all listeners to imagine how a given example might work for your research. If you think CEMAS can assist, please do not hesitate to email: williams.2156@osu.edu
- 13. Probing Materials Structure / Property Relationships via Multi-scale Characterization Irradiation Pinned dislocations Point defects Materials structure properties Fatigue Creep Cracks/ Cavity coalescence Critical cavities GB sliding Cavity nucleation Point defects Long cracks Microstructural cracks Grain Boundary cleavage GB sinks Composites Damage Woven defects Delamination Fiber fracture GB segregation 1nm 1 µm <1nm Spatial resolution Region of Interest 10 µm 100 µm 1 mm 300 µm 1nm 500nm 3 mm 10 mm 500 µm DualBeam FIB/SEM TEM Characterization Techniques Micro CT Bridging Length Scales Macro CT • Recently developed “Monster” 9000kV CT system • Acknowledgements: Manchester University
- 14. Destructive Characterization of Apple Pencil https://www.cnet.com/tech/computing/apple-pencil-powered-by-amazingly-tiny-tech/ • Quality control • Forensic analysis • OEM vs Vendor components • Cybersecurity • Chip architecture
- 15. Destructive Characterization of Apple Pencil • Is this the optimal technique for characterization? https://www.cnet.com/tech/computing/apple-pencil-powered-by-amazingly-tiny-tech/
- 17. 3D Visualization of Entire Pencil • Only the Heliscan is capable of producing a full-field visualization of the entire pencil with 1 scan! (9 mm voxel size) • Ideal for feature identification and determination of volumes for higher resolutions imaging.
- 18. 3D Visualization and Virtual Dissection • Subset of full-field visualization, collected with 1 scan, with 9 mm voxel size! • Ideal for feature identification and determination of volumes for higher resolutions imaging.
- 19. 2D virtual slice of Pencil Battery • Full-field Heliscan data is information rich, often this level of analysis is sufficient? (9 mm voxel size) • For some data sets, the full field data set is used to identify feature for higher
- 20. 500mm • Observed from ROI data set, 1mm voxel size 2D Virtual Slices to Image Battery Defects
- 21. 2D Virtual Slices to Image Battery Defects Higher Density Impurity/Inclusion Voids, delamination observed in cathode layer • Observed from full field data set, 1 mm voxel size • ROI scan performed in battery region for smaller voxel size and increased spatial resolution. • Sample can now be reduced in size, destructively, for even more spatial resolution. • Correlative analytical electron microscopy may be applied to remove regions for SEM
- 22. • We need to understand: – Macroscopic distribution of tubules – 3D structure of tubules – The composition of microtubule inner-surface Focussed Ion Beam (FIB) slice & view tomography MACRO MICRO NANO Multi-Scale Approach STEM-HAADF and XEDS Tomography X-ray Microtomography (XMT) Focussed Ion Beam (FIB) slice & view tomography STEM-HAADF and XEDS Tomography Imagine this analysis applied to a 3D printed component, for example? Could this analysis apply to your material system? Multiscale Correlative Analysis
- 26. Life Science Applications • Please note worm is hydrated in fluid. MicroCT can collect data from: • Animals (bone, heart, brain, skin) • Plants • Insects
- 27. 2D Virtual Slice Voxel size: 2 µm Full-Field MicroCT of Bee
- 28. 3D-Morphology of Honey-bee Mandibles Dr. Hongmei Li-Byarlay, Honeybee Research Lab, Central State University, Wilberforce, Ohio 0.2 mm 1 mm • Elegant imaging of the bee mandible is achievable and permits validation with manual bee dissection and traditional characterization methods. • Cross sections that are unachievable through dissection are virtually accessible from microCT data • From the MicroCT data, CAD models may be generated and used for 3D printing replicas from actual honey bee mandibles. Could this apply to your research as well?
- 29. Smith, J., et al (2021) ‘Morphological Changes in Mandible Accompany the Defensive Behavior of Indiana Mite Biting Honey Bees Against Varroa Destructor;, Front. Ecol. Evol., Quantification of Salient Features • One strength of MicroCT is the ability to extract quantatitive information from data sets. This creates a powerful characterization technique to develop accurate, quantitative measures that can act as inputs for models and statistical analysis.
- 30. MicroCT analysis of Powders for Additive Manufacturing Dr. Sriram Vijayan, Materials Science Engineering, The Ohio State University Applicable to : • 3D printing • Automotive • Aerospace • Pharmaceutical • Consumer Goods • Perhaps your material as well?
- 31. Dr. Sriram Vijayan, Materials Science Engineering, The Ohio State University Quantification and Statistical Significance The quantitative data that can be extracted from MicroCT datasets provides and opportunity to apply statistically relevant inputs into various types of predictive models.
- 32. 3D-Printed Ti-scaffold 3D Visualization and Structure Analysis Voxel Size 313 nm
- 33. Quality Control for 3D Printed Components Can be used for: Validation of component geometry Quality Assurance/Control Quantitive Analysis of component to provide input into models and simulations • Provide insight into printed structure based on 3D printing parameters • Provide inputs for modelling such as FEM or AI/ML. CAD Model for 3D Printing Manufacturing defects: Internal porosity Material overhang regions Surface roughness Inhomogeneous due to sintered powder particles Dense inclusions 2D Virtual Slice
- 34. Intermediate Summary MicroCT has produced information-rich data sets across most material systems: • Consumer goods and health care • Life Science • 3D printing and Additive Manufacturing • Cybersecurity, electronics and semiconductor sectors • Pharmaceuticals • These information rich data sets can be interrogated for: • Imaging and visualization • Feature identification • Multiscale correlative characterization and analysis. While applications presented may not be on your specific area of interest, I encourage all listeners to imagine how a given example might work for your research. If you think CEMAS can assist, please do not hesitate to email: williams.2156@osu.edu or visit, cemas.osu.edu
- 35. Mark Riccio Advanced MicroCT for Non- destructive 3D Multiscale Analysis Product Marketing Manager for X-ray microCT Thermo Fisher Scientific Proprietary & Confidential | 2021 35
- 36. Outline Solutions and Application Spaces 2 1 3 HeliScan MicroCT Technology Highlights Extended Solutions (4D, in situ, macroscale to atomic) 4 Conclusions
- 37. HeliScan MicroCT: Enable Discoveries Now with 400nm resolution Capture Critical Context (e.g. Large Volumes) • Stitch-free Artifact-free scanning of large volumes Leverage High Resolution, Multiple X-ray Spectrums • Spatial Resolution • 800nm via Tungsten filament (standard) • 400nm via LaB𝟔 filament (optional) Acquire Regions of Interest (ROI) with High Resolution • Up to 4x zoom Regions of Interest (ROI) scans (Off-axis) Accommodate Large Samples, Metals • 200 mm maximum, 160 kV maximum energy Optimize Scans for Speed or Contrast or Phase • Flexible scanning trajectories • Double Helix (Helical) • Space Filing (Faster Helical) • Circular • Patented correction technology • Iterative & Phase reconstruction algorithms State-of-the-Art Scientific Discoveries • Thermo Multimodal Workflow (mesoscale to nanoscale) • Combine 3D-Xray, 3D FIB-SEM, EBSD, TEM, etc
- 38. HeliScan: Helical Scanning trajectory
- 39. 2D/3D/4D+ Acquisition and Analysis Ceramics, Glasses Metals, Alloys and Powders Composites, Polymers Biomaterials Batteries Additive Manufacturing Semiconductors Food and Agriculture HeliScan MicroCT Application Spaces
- 40. 3D Visualizations to Reveal Hidden/Internal Structures 3D Visualizations to Reveal Hidden/Internal Structures AVIZO Software Thermo Scientific Solution. Academic and Industrial 2D/3D/4D Data Understand Visualize Analyze Battery Cathode. Active material connectivity analysis. Data acquisition: Thermo Scientific Helios™ PFIB DualBeam™.
- 42. 3D Data Pores Dense Particles Pores and Substrate HeliScan: Sample example
- 44. Multiscale Approach MICRO Scale NANO Scale Correct result? MACRO Scale CIRCULAR Scanning ROI ROI Probability of acquiring representative region = ?
- 45. Helical vs Circular Scanning CIRCULAR HELISCAN MICRO-CT HELICAL Spatially Hetergeneous
- 46. What’s INSIDE My Sample? 101 Questions for MicroCT Can we IDENTIFY structures of interest? Can we TRUST the data? Large field of view for high quality STATISTICS? High enough RESOLUTION for structural analysis? Can we QUANTIFY via advanced algorithms (e.g. tortuosity)? Possible to leverage multiscale MULTIMODAL datasets? 2 mm Each Layer = Different Condition Cathode + binder Application: Batteries Collaboration with UCSD: Jonathan Scharf, Shirley Meng, et al., Submitted Bridging Nano and Micro-scale X-ray Tomography for Battery Research by Leveraging Artificial Intelligence. arXiv:2107.07459
- 47. HeliScan Keeps the Context 2 mm Large X-ray Detector Virtual slice #1000 (3000 total slices) Voxel = 1um Helical Scan Sample courtesy of S. Meng Lab @ UCSD
- 48. HeliScan: High Resolution (LaB𝟔) 90um Sample courtesy of S. Meng Lab @ UCSD HeliScan Voxel = 190nm Voxel = 1um 400um
- 49. >50 scans HeliScan One. Micro-CT Many. CIRCULAR: Micro-CT • Voxel = 200nm; bin 2 = 1024 x 1024 • Volume = 0.2 mm x 0.2 mm x 0.2 mm 1 scan 125 µm HELICAL: HeliScan • Voxel = 190nm, bin1 = 3050 x 3050 • Volume = .54mm x .54mm x 1.19mm 1 scan
- 50. HeliScan: Metal Samples (160kV) Titanium Airplane Component
- 51. Heliscan 3D Imaging: Titanium Sample Voxel size 17.8um Internal porosity Voxel size 6um ZOOM IN For Higher Resolution 3D Visualization 2D Virtual Slice Manufacturing defects: • Internal porosity • Material overhang regions • Surface roughness Inhomogeneous due to sintered powder particles • Dense Inclusions
- 52. Standard Phase Contrast Retrieval 100 µm 100 µm 100 µm Reconstruction method uses the phase contrast signal to enhance structural contrast for better segmentation HeliScan enables Phase Contrast Retrieval Reconstruction LaB𝟔 spectrum for highest sensitivity
- 53. Phase Contrast Retrieval: Accurate Fiber Segmentation
- 54. HeliScan with Deben In Situ Stage https://deben.co.uk/tensile- testing/%C2%B5xct/tensile-stages-for-x- ray-ct-tomography/ • Compression – Tensile – Temperature • Applications: • Additive manufacturing • Batteries • Fiber reinforced polymers • Geology • Electronics
- 55. HeliScan: In Situ Access Cross section canal: 80x80 mm Bending radius 200 mm Experiment can be built outside of cabinet!
- 56. HeliScan: Compaction 4D Experiment FEM Modeling Courtesy: Dr. Mohammad Saadatfar, ANU, Australia
- 57. Easy Cross-Platform Workflows Maps microCT DualBeam TEM SEM 3D Data Support Make finding your way easier on every tool A single project, multiple scales Maps Software is compatible with the full line of Thermo Scientific microscopes Keep the data at the center of your research to drive your investigation
- 58. HeliScan MicroCT: Common Holder for Correlative Workflow microCT 3D data PFIB 3D data
- 59. MAPS Software Correlative Multiscale Microscopy Understanding material performance is multi-scale in nature X-ray and electron-microscopy Optical Crystallography Spectroscopy Any relevant imagery microCT SEM/DualBeam TEM Import 2D and 3D images from ANY source Correlate image layers easily and accurately Explore and interpret all your data efficiently and with context MAPS (Ma): workflows for systematic materials characterization Easy to capture, correlate and investigate multi-scale, multi-modal datasets
- 60. Conclusions Hardware, Software and Collaboratory Solutions • Flexibility and large volumes • Materials Science • Geology • Engineering • Life Science • High Resolution, Multiple X-ray spectrum • 800nm with Tungsten (standard) • 400nm with LaB6 (optional) • Phase Contrast Retrieval • ThermoFisher Scientific Workflow • Macroscale to nanoscale • Stitch-free scanning of larger volumes • ROI ZOOM • High resolution Regions of Interest (ROI) • Spatial Resolution • 800nm with Tungsten (standard) • 400nm with LaB6 (optional) • Sample sizes • 200 mm maximum • Flexible scanning trajectories • Helical • Circular • Space Filing (Faster) • Highest image fidelity • Iterative reconstruction algorithm • Patented correction software • Phase contrast retrieval • ThermoFisher Scientific Workflow • Mesoscale to nanoscale QA/QC Failure Analysis Reverse Engineering Process Optimization Digital Rock Pharma Materials Science Engineering Life Science Electronics Geology Paleontology
- 61. AZO Darius Soo Lum & Colleagues CEMAS David McComb, Robert Williams, Carley Goodwin, Daniel Huber & Colleagues ThermoFisher Scientific David Wall, Dirk Laeveren, Frantisek Zelenka, Raphaela Scharfschwerdt & Colleagues Thank You
- 62. Thank you for participating! Robert E. A. Williams, PhD Assistant Director for Research and Development CEMAS Mark Riccio Product Marketing Manager for X-ray microCT Thermo Fisher Scientific CLICK HERE to learn more and watch the webinar
Editor's Notes
- #5: We are here to give you data and information that you have not been able to acquire before, so that you, as the leading experts in Steel, may be able to make the most informed and educated decisions.
- #7: Two Titans Three other TEMs, Two Dual Beams Three SEMs
- #8: - Collaborative environment: VPN; IP phone/intercom; shared screens; swap control; just siting next to someone in the microscope control room at CEMAS
- #9: In -situ
- #10: Two Titans Three other TEMs, Two Dual Beams Three SEMs
- #11: Two Titans Three other TEMs, Two Dual Beams Three SEMs
- #23: This is a multi-scale problem, Needs correlative SuperX XEDS – 4 detectors, enables us to get high signal to noise in a relatively short time. Relevant to beam-sensitive materials http://www.listerineprofessional.co.uk/why-recommend-listerine/listerine-products/professional-advanced-defence/sensitivity-therapy https://www.dentalaegis.com/id/2011/09/dentin-hypersensitivity
- #30: From paper: “To compare the morphology of mandibles between commercial colonies and mite-biter colonies, we measured six different parameters from the microCT data: the length, width, height, long edge, short edge, and span of the spine area (Figure 4). The ANOVA between these two groups showed that the long edge of mandibles in the mite-biter colonies were significantly shorter than those in commercial colonies, F = 5.78, p = 0.03 (Figure 7). We found no significant difference between the two groups in the other five parameters (Figure 7), but in the length, height, short edge, and span of the spine area, we noticed a consistent trend of smaller values in the mite-biter colonies.” ORIGINAL RESEARCH article Front. Ecol. Evol., 27 April 2021 | https://doi.org/10.3389/fevo.2021.638308 Morphological Changes in the Mandibles Accompany the Defensive Behavior of Indiana Mite Biting Honey Bees Against Varroa Destructor Jada Smith1, Xaryn L. Cleare1, Krispn Given2 and Hongmei Li-Byarlay1,3* 1Department of Agricultural and Life Sciences, Central State University, Wilberforce, OH, United States 2Department of Entomology, Purdue University, West Lafayette, IN, United States 3Agricultural Research and Development Program, Central State University, Wilberforce, OH, United States
- #33: Movie of ROI A. Note that the spheres are non-melded particles.
- #34: Cut through central plane
- #38: This is similar to the last slide of the TECHNOLOGY PPT. The bullets are repeated in the samples we use for this messaging – TEXT in RED
- #41: Talking Points: For a complete Hardware and Software Solution we offer Avizo and Maps software. During our discussions today, our 3D visualizations and analysis are powered by our software, Avizo 2D/3DVisualizations Measurements Segmentation Advanced Calculations Correlative Analysis And it can be used in both academic and industrial settings. Avizo Software for Materials Research: Ceramics, glasses and porous media Metals, alloys and powders Composites, polymers and fibrous materials Biomaterials Batteries Additive manufacturing Semiconductors Food and agriculture Paleontology Archaeology Anthropology Geology Physics Chemistry Additive Manufacturing Aerospace Automotive Casting
- #44: If you wanted to charactertize porosity, Grains, inclusions you can do some at the Marco scale. You also want to find a location for the HeliScan to ZOOM in for higher resolution. Data here looks great. If you remember the images from the competitors, you’ll remember we didn’t even pick a Region of interest that was representative of the structures we wanted to study. We also couldn’t calculate statistically relevant data in the MACRO or Micro or Nano scale data.
- #45: Now let's expand the results by picking a region of interest and zooming in. That gives us multiscale results and the goal here is to pick a region where we want to zoom in to capture finer details for analysis and understanding. We can see some particles in the 3D data so we’ll pick an ROI there and can analyze the structures. Some of our competitors even have Resolution at a distance for zooming in at different scales. We end up at the submicron nano scale. But I'm curious. How do we know we have the CORRECT RESULT? Let’s REMEMBER THESE IMAGES
- #46: Picture speaks 1000 words. Remember this image. By the way, if the competition acquire same volume, they will pay the price in TIME (it can take 3-8x as long depending on how tall the sample is) and they also have to contend with stitching artifacts when they try to combine the individual volumes AND they can also have high cone angle artifact if they try to go faster. In other words, for the competition, it can take a lot longer and erode the quality of data.
- #47: Second story. Batteries. This sample from close collaborator Shirley Meng and her team at UCSD. Cathode + binder coating on Al foil as current collector Interested in looking at porosity and tortuosity Note: this is a Sweet spot for High Resolution
- #48: Now here's the HeliScan data with same voxel size and a LARGER field of view which allows analysis of all 4 layers with ONE scan, saving time and the potential of introducing artifact which would degrade their analysis, results and conclusions.
- #51: This a bigger Titanium 3D-printed part. It is a support used in a wing-flap of an airplane. A functional part of the plane. Size is ~130x60x15 mm
- #52: Cut of different planes
- #53: TIME for each method
- #54: Not JUST visualization. ANALYSIS as well
- #59: Showing that WE HAVE HW THAT SUPPORTS correlation!!!!!
- #62: Please attend our HeliScan deep dives into the technology and competition that we'll have for sales teams starting in March/April timeframe.