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:

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

14YWT oxide dispersion strengthened (ODS) ferritic steel was irradiated with of 5 MeV Ni2+ ions, at 300 °C, 450 °C, and 600 °...
Melanoma is a malignant tumor of melanocytes. Although extensive investigations have been done to study metabolic changes in primary melanoma in...
Grain growth of nanocrystalline materials is generally thermally activated, but can also be driven by irradiation at much lower temperature. In...
Dual beam depth profiling strategy has been widely adopted in ToF-SIMS depth profiling, in which two basic operation modes, interlaced mode and non-...
The microstructure and chemistry of SmCo2Fe2B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron...

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Instruments

There are no related projects at this time.

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: 

1H NMR Metabolomics Study of Metastatic Melanoma in C57BL/6J Mouse Spleen.

Abstract: 

Melanoma is a malignant tumor of melanocytes. Although extensive investigations have been done to study metabolic changes in primary melanoma in vivo and in vitro, little effort has been devoted to metabolic profiling of metastatic tumors in organs other than lymph nodes. In this work, NMR-based metabolomics combined with multivariate data analysis is used to study metastatic B16-F10 melanoma in C57BL/6J mouse spleen. Principal Component Analysis (PCA), an unsupervised multivariate data analysis method, is used to detect possible outliers, while Orthogonal Projection to Latent Structure (OPLS), a supervised multivariate data analysis method, is employed to find important metabolites responsible for discriminating the control and the melanoma groups. Two different strategies, i.e., spectral binning and spectral deconvolution, are used to reduce the original spectral data before statistical analysis. Spectral deconvolution is found to be superior for identifying a set of discriminatory metabolites between the control and the melanoma groups, especially when the sample size is small. OPLS results show that the melanoma group can be well separated from its control group. It is found that taurine, glutamate, aspartate, O-Phosphoethanolamine, niacinamide ,ATP, lipids and glycerol derivatives are decreased statistically and significantly while alanine, malate, xanthine, histamine, dCTP, GTP, thymidine, 2'-Deoxyguanosine are statistically and significantly elevated. These significantly changed metabolites are associated with multiple biological pathways and may be potential biomarkers for metastatic melanoma in spleen.

Citation: 
Wang X, MY Hu, J Feng, M Liu, and JZ Hu.2014."1H NMR Metabolomics Study of Metastatic Melanoma in C57BL/6J Mouse Spleen."Metabolomics 10(6):1129-1144. doi:10.1007/s11306-014-0652-z
Authors: 
X Wang
MY Hu
J Feng
M Liu
JZ Hu
Volume: 
10
Issue: 
6
Pages: 
1129-1144
Publication year: 
2014

ToF-SIMS Depth Profiling Of Insulating Samples, Interlaced Mode Or Non-interlaced Mode?

Abstract: 

Dual beam depth profiling strategy has been widely adopted in ToF-SIMS depth profiling, in which two basic operation modes, interlaced mode and non-interlaced mode, are commonly used. Generally, interlaced mode is recommended for conductive or semi-conductive samples, whereas non-interlaced mode is recommended for insulating samples, where charge compensation can be an issue. Recent publications, however, show that the interlaced mode can be used effectively for glass depth profiling, despite the fact that glass is an insulator. In this study, we provide a simple guide for choosing between interlaced mode and non-interlaced mode for insulator depth profiling. Two representative cases are presented: (1) depth profiling of a leached glass sample, and (2) depth profiling of a single crystal MgO sample. In brief, the interlaced mode should be attempted first, because (1) it may provide reasonable-quality data, and (2) it is time-saving for most cases, and (3) it introduces low H/C/O background. If data quality is the top priority and measurement time is flexible, non-interlaced mode is recommended because interlaced mode may suffer from low signal intensity and poor mass resolution. A big challenge is tracking trace H/C/O in a highly insulating sample (e.g., MgO), because non-interlaced mode may introduce strong H/C/O background but interlaced mode may suffer from low signal intensity. Meanwhile, a C or Au coating is found to be very effective to improve the signal intensity. Surprisingly, the best analyzing location is not on the C or Au coating, but at the edge (outside) of the coating.

Citation: 
Wang Z, K Jin, Y Zhang, F Wang, and Z Zhu.2014."ToF-SIMS Depth Profiling Of Insulating Samples, Interlaced Mode Or Non-interlaced Mode?"Surface and Interface Analysis 46(S1):257-260. doi:10.1002/sia.5419
Authors: 
Z Wang
K Jin
Y Zhang
F Wang
Z Zhu
Volume: 
46
Issue: 
0
Pages: 
257-260
Publication year: 
2014

Microstructure of Multistage Annealed Nanocrystalline SmCo2Fe2B Alloy with Enhanced Magnetic Properties.

Abstract: 

The microstructure and chemistry of SmCo2Fe2B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe)4B (1:4:1) and Sm2(Co,Fe)17Bx (2:17:x) magnetic phases were confirmed using both techniques. Fe2B at a scale of ∼5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

Citation: 
Jiang X, A Devaraj, B Balamurugan, J Cui, and JE Shield.2014."Microstructure of Multistage Annealed Nanocrystalline SmCo2Fe2B Alloy with Enhanced Magnetic Properties."Journal of Applied Physics 115(6):Article No. 063902. doi:10.1063/1.4865298
Authors: 
X Jiang
A Devaraj
B Balamurugan
J Cui
JE Shield
Volume: 
0
Issue: 
0
Pages: 
0
Publication year: 
2014

Stability Of Nanoclusters In 14YWT Oxide Dispersion Strengthened Steel Under Heavy Ion-irradiation By Atom Probe Tomography.

Abstract: 

14YWT oxide dispersion strengthened (ODS) ferritic steel was irradiated with of 5 MeV Ni2+ ions, at 300 °C, 450 °C, and 600 °C to a damage level of 100 dpa. The stability of Ti–Y–O nanoclusters was investigated by applying atom probe tomography (APT) in voltage mode, of the samples before and after irradiations. The average size and number density of the nanoclusters was determined using the maximum separation method. These techniques allowed for the imaging of nanoclusters to sizes well below the resolution limit of conventional transmission electron microscopy techniques. The most significant changes were observed for samples irradiated at 300 °C where the size (average Guinier radius) and number density of nanoclusters were observed to decrease from 1.1 nm to 0.8 nm and 12 × 1023 to 3.6 × 1023, respectively. In this study, the nanoclusters are more stable at higher temperature.

Citation: 
He J, F Wan, K Sridharan, TR Allen, AG Certain, V Shutthanandan, and Y Wu.2014."Stability Of Nanoclusters In 14YWT Oxide Dispersion Strengthened Steel Under Heavy Ion-irradiation By Atom Probe Tomography."Journal of Nuclear Materials 455(1-3):41-45. doi:10.1016/j.jnucmat.2014.03.024
Authors: 
He J
F Wan
K Sridharan
TR Allen
AG Certain
V Shutthanan
Y Wu
Facility: 
Instruments: 
Volume: 
455
Issue: 
0
Pages: 
41-45
Publication year: 
2014

The Effect of Eectronic Energy Loss on Irradiation-Induced Grain Growth in Nanocrystalline Oxides.

Abstract: 

Grain growth of nanocrystalline materials is generally thermally activated, but can also be driven by irradiation at much lower temperature. In nanocrystalline ceria and zirconia, contributions from both displacement damage and ionization to the grain growth are identified. Our atomistic simulations have revealed fast grain boundary (GB) movements due to the high density of disorder near GBs. Our experimental results have shown that irradiation-induced grain growth is a function of total energy deposited, where the excitation of target electrons and displacement of lattice atoms both contribute to the overall disorder and both play important roles in grain growth. The coupling of energy deposition to the electronic and lattice structures should both be taken into consideration when engineering nanostructural materials.

Citation: 
Zhang Y, DS Aidhy, T Varga, S Moll, PD Edmondson, F Namavar, K Jin, CN Ostrouchov, and WJ Weber.2014."The Effect of Eectronic Energy Loss on Irradiation-Induced Grain Growth in Nanocrystalline Oxides."Physical Chemistry Chemical Physics. PCCP 16(17):8051-8059. doi:10.1039/c4cp00392f
Authors: 
Y Zhang
DS Aidhy
T Varga
S Moll
PD Edmondson
F Namavar
K Jin
CN Ostrouchov
WJ Weber
Facility: 
Volume: 
16
Issue: 
17
Pages: 
8051-8059
Publication year: 
2014

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Dr. Bowden joined EMSL in 2009 and currently 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...