Characterization of Minerals, Metals, and Materials: Method Development
Sponsored by: TMS Extraction and Processing Division, TMS: Materials Characterization Committee
Program Organizers: Shadia Ikhmayies, Al Isra University; Bowen Li, Michigan Technological University; John Carpenter, Los Alamos National Laboratory; Jian Li, CanmetMATERIALS; Jiann-Yang Hwang, Michigan Technological University; Sergio Monteiro, Military Institute of Engineering ; Firrao Donato, Collegio Universitario, Italy; Mingming Zhang, ArcelorMittal Global R&D; Zhiwei Peng, Central South University; Juan P. Escobedo-Diaz, UNSW Australia; Chenguang Bai, Chongqing University; Eren Kalay, METU; Ramasis Goswami, Naval Research Laboratory; Jeongguk Kim, Korea Railroad Research Institute

Thursday 8:30 AM
March 2, 2017
Room: 30D
Location: San Diego Convention Ctr

Session Chair: Jeongguk Kim, Korea Railroad Research Institute; Tomoko Sano, US Army Research Laboratory

8:30 AM  
Characterizing Ballistic Resistance: Legacy Methods Versus Novel Statistical Tools: Frederik Coghe1; 1Royal Military Academy (BE MoD)
    Since the industrial production of armour materials, test methods have been developed in order to assess their effective ballistic resistance. Two common test methods are using either a proof velocity (Vproof) or a statistical ballistic limit (V50), the latter assuming that a normal distribution describes the generalized complete perforation. Although this is correct for a given impact velocity, there is no theoretical or experimental background to support its extension to the full velocity field. This invalidates the use of a σ50 to estimate low probability values, like V01 or V99. Recently, statistical concepts from the world of fundamental physics (i.e. Brownian motion) have been introduced in other fields (e.g. finances, communications…) to tackle similar problems. Applying this new method for the V50 shows great promise to further enhance our understanding of the stochastic penetration process, and to have more reliable estimates in the (very) low and (very) high probability regions.

8:50 AM  
A Forward Modeling Approach to Defect Characterization in a Scanning Electron Microscope: Saransh Singh1; Marc De Graef1; 1Carnegie Mellon University
    Defects have traditionally been studied in a TEM using one of many techniques, including bright/dark field imaging, weak beam imaging etc. Recently, Electron Channeling Contrast imaging (ECCI) has been shown to be a viable alternative to the TEM based methods and offers some advantages in sample preparation and the study of bulk samples. In this contribution, we present a forward model approach to defect characterization in an SEM. A forward model for Electron Channeling Patterns (ECP) will be presented. The forward model is combined with the dictionary approach to index ECPs for quantitative studies, such as g.b analysis. Finally, the forward model is extended to simulate arbitrary defects using the ECCI modality. We will present some results of defect simulation in structural materials and semiconductors. We will also discuss the efficient implementation of these routines on the massively parallel GPU architecture as part of the open source EMsoft project.

9:10 AM  
In-Situ Femtosecond Laser Milling Technique for Microstructural Characterization: Tomoko Sano1; Jonathan Ligda1; 1US Army Research Laboratory
    The technique of using the femtosecond laser to mill away material for microstructural characterization has been developed. This rapid technique allows larger areas to be characterized in a much shorter time since the femtosecond laser milling rate is orders of magnitude faster than that of the ion beam. The femtosecond laser is introduced into the focused ion beam, through an objective lens connected to a micromanipulator. Scripts were written to automate the milling controls, image capture, and stage motion for secondary electron, electron backscattered diffraction, and energy dispersive spectroscopy characterization. With the femtosecond laser coupled to the focused ion beam, both 2D and serial sectioning for 3D volumetric characterization are possible. In this oral paper, this technique is described and the effect of the femtosecond laser parameters, including power, number of steps, and polarization is evaluated for both ceramics and lightweight alloys.

9:30 AM  
Development of A New Recycling Process of PGM from Metal-supported Catalyst Using Complex Oxide: Takashi Nagai1; Hiroki Kumakura1; Kenji Abe1; Rentaro Seki1; Daiki Noguchi1; 1Chiba Institute of Technology
    A large amount of platinum group metals (PGM) are used in automobile catalyst. It is important to recover the metals from wasted catalyst. PGM in the catalyst are supported by ceramics for four-wheel vehicle or metals such as stainless steel for two-wheel ones. The recycling process of PGM from the metal-supported catalyst has not developed, while the process for ceramic-supported catalyst was developed, such as Rose process. We designed a noble recycling process of PGM from metal-supported catalyst using complex oxides between PbO and PGM oxide. In this study, complex oxides, PbPt2O4, PbPdO2, PbRh2O4 and so on were synthesized at about 773 - 973 K. And the dissolution behavior of these compounds to hydrochloric acid was investigated. PbPt2O4 and PbPdO2 were dissolved to hydrochloric acid easily, but PbRh2O4 was not.

9:50 AM  
In Situ Mechanical and Thermal Damage Mechanisms Investigation in Asteoridal Rocks: Jefferson Cuadra1; Kavan Hazeli2; Harry Martz1; KT Ramesh3; 1Lawrence Livermore Nation Laboratory; 2University of Alabama in Huntsville; 3Johns Hopkins University
    Rock fracturing on the surface of planetary bodies has traditionally been attributed to the meteorite impacts. Note that the ejecta velocities for small kilometer-sized asteroids typically exceed the gravitational escape velocity, which limits the amount of retained ejecta following a high-velocity impact event. The objective of this study, therefore, is to identify and quantify the sensitivity of meteorite samples to crack initiation and propagation as a result of diurnal temperature variations. We use in situ X-ray computed tomography to obtain quantitative information of the damage process under thermal fatigue and mechanical loading. The presented results demonstrate that the dissimilarity in physical properties of the constituent phases results to a different damage pattern under thermal fatigue versus mechanical stress. The presented damages assessment methodology, which is capable of resolving 3D geometry, shows promise in differentiating of the dominant damage mechanisms activated under mechanical disruption against thermal disaggregation in heterogeneous materials.

10:10 AM Break

10:25 AM  
Nondestructive Characterization of Railway Materials and Components with Infrared Thermography Technique: Jeongguk Kim1; 1Korea Railroad Research Institute
    Infrared (IR) thermography is an advanced nondestructive evaluation technique based on the detection of infrared radiation. Especially, IR thermography provides a quick, full-field and real-time inspection as well as a non-contact mode. Using those advantages, it is possible to perform thermographic analysis of railway materials/components including brake disc, abnormal heating, mechanical testing monitoring, etc. In this investigation, current research activities in railway materials/components with IR thermography will be introduced. For example, the electrical units of diesel electric locomotives were characterized for deterioration evaluation using infrared thermography technique. The high-speed infrared camera was used to measure surface temperature changes during tensile testing of railway steels. The damage evolution due to generation of hot spots on railway brake shoe or disc was successfully monitored using a high-speed IR camera. In this paper, the useful applications of IR thermography in railway areas will be introduced and recent research results will be also presented.

10:45 AM  
Nondestructive Materials Characterization in 3D by Laboratory Diffraction Contrast Tomography: Erik Lauridsen1; Christian Holzner2; Florian Bachmann1; Allan Lyckegaard1; Hrishikesh Bale2; Leah Lavery2; 1Xnovo Technology ApS; 2Carl Zeiss X-ray Microscopy Inc.
    The majority of metallic and ceramic engineering materials of interest are polycrystalline. The ability to characterise this crystallographic microstructure, nondestructively and in three-dimensions, is thus a powerful tool for understanding many facets of materials performance. The introduction of diffraction contrast tomography as an additional imaging modality on the ZEISS Xradia Versa laboratory X-ray microscope has opened up a whole new range of possibilities for studies of the effect of 3D crystallography on materials performance. The nondestructive 3D crystallographic imaging capabilities of the laboratory diffraction contrast tomography technique (LabDCT), complements the structural data obtained by traditional absorption-based tomography and together they provide an unprecedented insight into materials structure. Here we will present a selection of results of LabDCT with particularly emphasis on its nondestructive operation. We will discuss the boundary conditions of the current implementation and point to the future of the technique.

11:05 AM  
Five Dimensional Microanalysis of In-situ Reactions in Solution: Tyler Ley1; Qinang Hu1; Mohammed Aboustait1; Masoud Moradian1; Taehwan Kim; Taehwan Kim2; Jay Hanan1; Jeff Bullard3; George Scherer4; Robert Winarski5; Volker Rose5; Jeff Gelb6; 1Oklahoma State University; 2University of New South Wales; 3NIST; 4Princeton; 5Argonne National Laboratory; 6Zeiss Xradia Inc
    Progress has been halted in a number of critical fields because it is challenging to make quantitative in-situ measurements at the nanoscale. Recent advances in synchrotron based nano scale X-ray imaging have made it possible to map in-situ structure and chemistry of fluid based reactions. This work will present methodologies to combine nano computed tomography and fluorescence mapping to produce 5D data sets at a ~50 nm resolution. The results give quantitative measurements of 3D structure, chemistry and mass density of the changes that occur over time. Next, data from a specialized flow through cell will be presented that allows time resolved, in-situ chemical mapping of changes in the material surface and the surrounding solution. A case study will be presented for calcium silicate reactions in different solutions; however, these methods can be applied to many different materials to allow improved understanding of nanoscale phenomenon.

11:25 AM  
Improvements in High Speed Simultaneous EDS-EBSD Mapping: Matt Nowell1; 1EDAX-TSL
    Through simultaneous collection of Energy Dispersive Spectroscopy (EDS) and Electron Backscattered Diffraction (EBSD) information, it is possible to improve the phase differentiation capability beyond that which is possible compared with either technique used individually. Advanced in EBSD detector technology allow for faster collection speeds while improvements in EDS detectors allow for higher throughput of detected X-ray events with maintaining resolution stability. However, the excitation volume from these techniques do not match exactly, which can have implications when the sampling step size approaches the EDS interaction volume size of (≈ 1Ám). Two approaches will be described to address this issue to better align the EDS information with the EBSD information. To demonstrate the effects of data collection speed on the usability of simultaneous EDS and EBSD information, data from a thermal barrier coating on a nickel superalloy turbine blade will be presented.

11:45 AM  
Measuring Bauschinger Effects in Rolled Sheet Metal: Christopher Calhoun1; Evan Rust1; Dilip Banerjee1; Tim Foecke1; 1NIST
    Predicting deformation during metal stamping processes remains illusive to engineers and scientists. Experimentally, capturing complex loading conditions in a controlled laboratory setting on the desired material presents key challenges. Here, we seek to quantify the effect of load reversal (i.e. tension to compression) during in-plane uni-axial loading on sheet metal. Researchers have observed a drop in flow stress upon load reversal, termed the Bauschinger effect, in bulk metal. In sheet metal, preventing buckling poses the primary challenge to measuring the stress-strain response during compression. This presentation will include the development of a technique for tension and compression testing sheet metal during load reversal. The technique employs the use of anti-buckling guides, Digital Image Correlation (DIC), and additional load cells on a conventional uni-axial testing machine. Validation of the method serves as the primary focus of the talk, but it also includes measured stress-strain response for potential automotive alloys.

12:05 PM  
Micromanipulation Techniques for Site Specific Materials Characterization: Lucille Giannuzzi1; 1EXpressLO LLC
    The ex situ lift out (EXLO) method for micromanipulation of site specific focused ion beam (FIB) specimens has been extended to the micromanipulation of ceramic fibers, particulates, carbon nanotubes, graphene, and glassy stand-alone thin films. Micromanipulation is performed using direct Van der Waals forces and/or facilitated with adhesive. Once manipulated to newly designed grid carriers, samples may be directly analyzed by transmission electron microscopy (TEM) or FIB milled to create suitable surfaces for surface analysis, electron microscopy, and associated analytical methods. EXLO techniques for FIB prepared specimens micromanipulated to new grid carriers will be reviewed, and examples of similar methods applied to the micromanipulation and materials characterization of non-FIB-type samples will be shown.