Spectroscopy and Diffraction
Molecular level solid-, liquid- and gas-interactions can be investigated through structural, chemical and compositional analysis with remarkable atomic scale spatial and high-energy resolution spectrometers and diffractometers for novel fundamental research. See a complete list of Spectroscopy and Diffraction instruments.
Resources and Techniques
- Electron spectroscopy
- Electron backscatter diffraction
- Atom probe tomography
- Ion/molecular beam spectroscopy
- 57Fe-Mössbauer spectroscopy
- Optical spectroscopy
- X-ray tomography and diffractometers
Additional Information:
Science Theme:
Molecular level solid-, liquid- and gas-interactions can be investigated through structural, chemical and compositional analysis with remarkable atomic scale spatial and high-energy resolution spectrometers and diffractometers for novel fundamental research. See a complete list of Spectroscopy and Diffraction instruments.
Resources and Techniques
- Electron spectroscopy
- Electron backscatter diffraction
- Atom probe tomography
- Ion/molecular beam spectroscopy
- 57Fe-Mössbauer spectroscopy
- Optical spectroscopy
- X-ray tomography and diffractometers
Additional Information:
Attachments:
Deadline approaching for EMSL’s Science Theme proposals
Detecting Technetium in Groundwater
EMSL opens the call for FY 2017 proposals
Design of Ternary Nanoalloy Catalysts: Effect of Nanoscale Alloying and Structural Perfection on Electrocatalytic Enhancement.
Abstract:
The ability to tune the atomic-scale structural and chemical ordering in nanoalloy catalysts is essential for achieving the ultimate goal of high activity and stability of catalyst by design. This article demonstrates this ability with a ternary nanoalloy of platinum with vanadium and cobalt for oxygen reduction reaction in fuel cells. The strategy is to enable nanoscale alloying and structural perfection through oxidative–reductive thermochemical treatments. The structural manipulation is shown to produce a significant enhancement in the electrocatalytic activity of the ternary nanoalloy catalysts for oxygen reduction reaction. Mass activities as high as 1 A/mg of Pt have been achieved by this strategy based on direct measurements of the kinetic currents from rotating disk electrode data. Using a synchrotron high-energy X-ray diffraction technique coupled with atomic pair function analysis and X-ray absorption fine structure spectroscopy as well as X-ray photoelectron spectroscopy, the atomic-scale structural and chemical ordering in nanoalloy catalysts prepared by the oxidative–reductive thermochemical treatments were examined. A phase transition has been observed, showing an fcc-type structure of the as-prepared and the lower-temperature-treated particles into an fct-type structure for the particles treated at the higher temperature. The results reveal a thermochemically driven evolution of the nanoalloys from a chemically disordered state into chemically ordered state with an enhanced degree of alloying. The increase in the chemical ordering and shrinking of interatomic distances as a result of thermochemical treatment at increased temperature is shown to increase the catalytic activity for oxygen reduction reaction, exhibiting an optimal activity at 600 °C. It is the alloying and structural perfection that allows the optimization of the catalytic performance in a controllable way, highlighting the significant role of atomic-scale structural and chemical ordering in the design of nanoalloy catalysts.
Citation:
Wanjala BN, B Fang, S Shan, V Petkov, P Zhu, R Loukrakpam, Y Chen, J Luo, J Yin, L Yang, M Shao, and CJ Zhong.2012."Design of Ternary Nanoalloy Catalysts: Effect of Nanoscale Alloying and Structural Perfection on Electrocatalytic Enhancement."Chemistry of Materials 24(22):42834293. doi:10.1021/cm301613j
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2012
Magnetic Separation Dynamics of Colloidal Magnetic Nanoparticles.
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Surface functionalized magnetic nanoparticles (MNPs) are appealing candidates for analytical separation of heavy metal ions from waste water and separation of actinides from spent nuclear fuel. This work studies the separation dynamics and investigates the appropriate magnetic-field gradients. A dynamic study of colloidal MNPs was performed for steady-state flow. Measurements were conducted to record the separation time of particles as a function of magnetic field gradient. The drag and magnetic forces play a significant role on the separation time. A drop in saturation magnetization and variation of particle size occurs after surface functionalization of the MNPs; these are the primary factors that affect the separation time and velocity of the MNPs. The experimental results are correlated to a theoretical one-dimensional model.
Citation:
Kaur M, H Zhang, and Y Qiang.2013."Magnetic Separation Dynamics of Colloidal Magnetic Nanoparticles."IEEE Magnetics Letters 4:4000204. doi:10.1109/LMAG.2013.2271744
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2013
Advanced Oxide Dispersion Strengthened and Nanostructured Ferritic Alloys .
Abstract:
Nanostructured ferritic alloy is a subcategory of oxide dispersion strengthened steels intended for advanced reactor applications. The complex ultrafine grained microstructure of an advanced nanostructured ferritic alloy, as determined by electron microscopy and atom probe tomography, is summarised. Three distinct populations of precipitates were observed: 20–50 nm Ti(N,O,C), 5–10 nm diameter Y2Ti2O7/Y2TiO5 and 1–4 nm diameter Ti,Y,O enriched nanoclusters. The first two populations were predominantly located along grain boundaries together with Cr, W and C segregation. A dense population of nanoclusters was observed both in the grain interior as well as on the grain boundaries. These nanoclusters are highly tolerant to high dose irradiation at elevated temperatures.
Citation:
Miller MK, CM Parish, and Q Li.2013."Advanced Oxide Dispersion Strengthened and Nanostructured Ferritic Alloys ."Materials Science and Technology 29(10):1174-1178. doi:10.1179/1743284713Y.0000000207
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29
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10
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1174-1178
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2013
Multi-Detector STEM-EDS Mapping of Ion-Irradiated Nanostructured Ferritic Alloys.
Abstract:
Materials used in advanced fission or fusion reactors must be able to withstand radiation damage doses of several hundred displacements per atom (dpa) under high temperature and elevated creep stresses, in corrosive environments.
Citation:
Parish CM, RM White, JM LeBeau, Y Zhang, and MK Miller.2013."Multi-Detector STEM-EDS Mapping of Ion-Irradiated Nanostructured Ferritic Alloys."Microscopy and Microanalysis 19(Supplement S2):1144-1145. doi:10.1017/S143192761300771X
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0
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1144-1145
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2013
Pollution changes clouds' ice crystal genesis
Microbial mineral colonization across a subsurface redox transition zone.
Abstract:
Thisstudyemployed16SrRNAgeneampliconpyrosequencingtoexaminethehypothesisthatchemolithotrophicFe(II)-oxidizing bacteria(FeOB)would preferentially colonizetheFe(II)-bearing mineral biotite compared to quartz sand whenthe minerals were incubated in situ within a subsurface redox transition zone(RTZ) at the Hanford 300 Area site in Richland, WA, USA.The work was motivated by the recently documented presence of neutral-pH chemolithotrophic FeOB capable of oxidizing structural Fe(II) in primary silicate and secondary phyllosilicate minerals in 300 Area sediment sand groundwater (Benzineetal.,2013). Sterilized portions of sand+biotite or sand alone were incubated in situ for 5 months within a multilevel sampling(MLS) apparatus thats pannedaca. 2-minterval across the RTZ in two separate groundwater wells.Parallel MLS measurements of aqueous geochemical species were performed prior to deployment of the minerals. Contrary to expectations, the 16S rRNA gene libraries showed no significant difference in microbial communities that colonized the sand+biotite vs. sand-only deployments.Both mineral-associated and groundwater communities were dominated by heterotrophictaxa, with organisms from the Pseudomonadaceae accountingforupto70% of all reads from the colonized minerals. These results are consistent with previous results indicating the capacity for heterotrophic metabolism(including anaerobic metabolism below the RTZ) as well as the predominance of heterotrophictaxa within 300 Area sediments and ground water.Although heterotrophic organisms clearly dominated the colonized minerals,several putativelithotrophic (NH4+,H2,Fe(II),andHS−oxidizing) taxa were detected in significant abundance above and within the RTZ. Such organisms may play a role in the coupling of anaerobic microbial metabolism to oxidative pathways with attendant impacts on elemental cycling and redox-sensitive contaminant behavior in the vicinity of the RTZ.
Citation:
Converse B, JP McKinley, CT Resch, and EE Roden.2015."Microbial mineral colonization across a subsurface redox transition zone."Frontiers in Microbiology 6:858. doi:10.3389/fmicb.2015.00858
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2015
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Description
Capability Details
- Electron spectrometers with high spatial and energy resolution in-situ and ex-situ x-ray photoelectron spectroscopy
- Secondary ion mass spectrometers with single and cluster ion sources, and time-of-flight and magnetic mass analyzers
- Electron microscopes with energy dispersive X-ray spectroscopy, electron energy loss spectroscopy and electron backscatter diffraction
- Local Electrode Atom Probe tomography system with 355 nm UV laser and reflectron flight path for high mass resolution
- Fourier transform infrared spectrometers with vacuum bench and variable temperature capability
- Confocal-Raman, cryogenic time-resolved fluorescence, circular dichroism, stopped-flow absorbance, laser-induced breakdown and sum frequency generation optical tools
- Variable temperature Mössbauer spectroscopy systems for bulk (transmission mode) and surface (emission) measures
- X-ray diffraction instruments with sealed tube or rotating anode for analysis of powder, thin film and single crystal samples; point, CCD and image plate detection. X-ray computed tomography with 225- and 320-kV fixed, and 225-kV rotating target options using a 2000x2000 pixel area detector and state-of-the-art processing and visualization software
Electron spectroscopy – Achieving nanoscale spatial resolution, users can study elemental composition, structural properties, and chemical states of materials with applications to thin films, nanomaterials, catalysis, biological and environmental sciences, corrosion, and atmospheric aerosols.
Electron backscatter diffraction – Samples of microstructures in environmental and material science can be examined with three dimensional reconstruction and characterization using focused ion beam-electron backscatter diffraction analysis.
Atom probe tomography – Atom Probe Tomography (APT) provides comprehensive and accurate three dimensional chemical imaging for characterization of both metallic materials and low electrical conductivity materials, such as semiconductors, oxides, carbides, nitrides and composites.
Ion/molecular beam spectroscopy – Secondary ions and scattered ions from various materials are analyzed in straight, magnetic or time-of-flight mass spectrometers to investigate elemental, isotopic and molecular compositions through surface spectra, one dimensional depth profiling and two dimensional and three dimensional chemical imaging.
57Fe-Mössbauer spectroscopy – Using 57Fe (a versatile, highly sensitive, and stable isotope with natural abundance of 2.2%), users can obtain information about the valence state, coordination number and magnetic ordering temperatures for a wide range of Fe-containing samples; (e.g., Fe-organic matter complexes, sediments, catalysts, glass materials).
Optical spectroscopy – Fluorimetry, stopped-flow absorbance, FTIR and confocal-Raman tools enable analysis for biology, radiochemistry, and catalysis. Sum frequency generation-vibrational spectroscopy and second harmonic generation are available to study liquid, liquid and solid, and liquid interfaces.
X-ray tomography and diffractometers – X-ray computed tomography delivers images of microstructures (components, pore structure and connectivity) in biological and geological samples at tens of microns spatial resolution. General purpose and specialized x-ray diffraction systems, including single-crystal, microbeam and variable temperature powder capabilities, empower phase analysis of polycrystalline, epitaxial thin films, protein structure determination, and studies of problematic small inorganic molecules.
Instruments
The atmospheric pressure reactor system is designed for testing the efficiency of various catalysts for the treatment of gas-phase pollutants. EMSL...
Custodian(s): Russell Tonkyn
The LEAP® 4000 XHR local electrode atom probe tomography instrument enabled the first-ever comprehensive and accurate 3-D chemical imaging studies...
Custodian(s): Arun Devaraj, Daniel Perea
This unique instrument is capable of measuring gas/solid reaction rates under realistic, high-pressure (∼1 atm) conditions using model, low-surface...
Custodian(s): Janos Szanyi
EMSL's non-thermal interfacial reactions instrumentation is available for use in research directed toward understanding non-thermal interfacial...
Custodian(s): Greg Kimmel
The SMSAS is a multi-technique surface analysis instrument based on elemental mapping using either scanning small spot X-rays or the electronics in...
Custodian(s): Shuttha Shutthanandan
Publications
The activities of CeO2, Mn2O3-CeO2 and ZrO2-CeO2 were measured for acetic acid ketonization under reaction conditions relevant to pyrolysis vapor...
The ability to tune the atomic-scale structural and chemical ordering in nanoalloy catalysts is essential for achieving the ultimate goal of high...
Surface functionalized magnetic nanoparticles (MNPs) are appealing candidates for analytical separation of heavy metal ions from waste water and...
Nanostructured ferritic alloy is a subcategory of oxide dispersion strengthened steels intended for advanced reactor applications. The complex...
Materials used in advanced fission or fusion reactors must be able to withstand radiation damage doses of several hundred displacements per atom (dpa...
Science Highlights
Posted: November 28, 2016
Catalysts known as zeolites are vital to fuel production and other processes. Coke deposits in zeolites are a costly problem in petroleum refinement...
Posted: October 21, 2016
The Science
Aerosols play an important role in climate, air quality, and health. A recent study provides new molecular-level insights into how a...
Posted: September 15, 2016
Scientists from the University of Minnesota and Pacific Northwest National Laboratory used capabilities at EMSL and other facilities to make...
Posted: September 13, 2016
The Science
Sodium-ion batteries are an attractive alternative to lithium-ion batteries due to their high efficiency and low cost, but development...
Posted: September 12, 2016
Manganese, unlike other elements, can lose up to seven electrons or take as many as three electrons from its surroundings, which has implications...
Instruments
The aim of this proposal is to build upon our initial success in the exploration of the 3-D location and distribution of the Al and Si atoms in...
Biological particles may be an important source of ice nucleating particles (INPs) at modestly supercooled cloud temperatures. These particles can...
Quantum information science is an up and coming area of research aimed to transform computing capabilities in the future. The use of quantum bits, or...
A critical challenge for high temperature electrochemistry is metallic catalyst stability. Rapid migration of nickel features is a key limitation to...
The Nuclear Process Science Initiative (NPSI) is an internal, Laboratory Directed Research and Development (LDRD) program investment in support of...
Leads
(509) 371-7816
Dr. Bowden manages EMSL's optical spectroscopy and diffraction, subsurface flow and transport, and microfabrication and deposition capabilities. He is responsible for the X-ray diffraction facility and assists or conducts measurement and...