scholarly journals Development of small particle speciation for nuclear forensics by soft X-ray scanning transmission spectromicroscopy

The Analyst ◽  
2018 ◽  
Vol 143 (6) ◽  
pp. 1349-1357 ◽  
Author(s):  
J. I. Pacold ◽  
A. B. Altman ◽  
K. B. Knight ◽  
K. S. Holliday ◽  
M. J. Kristo ◽  
...  
Keyword(s):  
Synchrotron Radiation ◽  
Spatial Resolution ◽  
Nuclear Forensics ◽  
Small Particle ◽  
Nuclear Materials ◽  
Chemical Sensitivity ◽  
X Ray ◽  
Scanning Transmission

Synchrotron radiation spectromicroscopy provides a combination of submicron spatial resolution and chemical sensitivity that is well-suited to analysis of heterogeneous nuclear materials.

X-ray Microscopy of Polymeric Materials

1994 ◽  
Vol 375 ◽  
Author(s):  
H. Adel ◽  
B. Hsiao ◽  
G. Mitchell ◽  
E. Rightor ◽  
A. P. Smith ◽  
...  
Keyword(s):  
Spatial Resolution ◽  
National Laboratory ◽  
Polymeric Materials ◽  
Brookhaven National Laboratory ◽  
Chemical Bonds ◽  
Chemical Sensitivity ◽  
Specific Chemical ◽  
X Ray ◽  
Oriented Samples ◽  
Scanning Transmission

AbstractWe describe how the scanning transmission x-ray microscope at Brookhaven National Laboratory can be used to investigate the bulk characteristics of polymeric materials with chemical sensitivity at a spatial resolution of about 50 nm. We present examples ranging from unoriented multiphase polymers to highly oriented Kevlar fibers. In the case of oriented samples, a dichroism technique is used to determine the orientation of specific chemical bonds. Extension of the technique to investigate surfaces of thick samples is discussed.

scholarly journals An ultrahigh-resolution soft x-ray microscope for quantitative analysis of chemically heterogeneous nanomaterials

2020 ◽  
Vol 6 (51) ◽  
pp. eabc4904
Author(s):  
David A. Shapiro ◽  
Sergey Babin ◽  
Richard S. Celestre ◽  
Weilun Chao ◽  
Raymond P. Conley ◽  
...  
Keyword(s):  
Spatial Resolution ◽  
High Performance ◽  
Ultrahigh Resolution ◽  
High Brightness ◽  
X Ray ◽  
Correlative Analysis ◽  
Scanning Transmission ◽  
Chemical States ◽  
Scanning Mechanism ◽  
Performance Computing

The analysis of chemical states and morphology in nanomaterials is central to many areas of science. We address this need with an ultrahigh-resolution scanning transmission soft x-ray microscope. Our instrument provides multiple analysis tools in a compact assembly and can achieve few-nanometer spatial resolution and high chemical sensitivity via x-ray ptychography and conventional scanning microscopy. A novel scanning mechanism, coupled to advanced x-ray detectors, a high-brightness x-ray source, and high-performance computing for analysis provide a revolutionary step forward in terms of imaging speed and resolution. We present x-ray microscopy with 8-nm full-period spatial resolution and use this capability in conjunction with operando sample environments and cryogenic imaging, which are now routinely available. Our multimodal approach will find wide use across many fields of science and facilitate correlative analysis of materials with other types of probes.

scholarly journals One-Step Synthesis of Copper and Cupric Oxide Particles from the Liquid Phase by X-Ray Radiolysis Using Synchrotron Radiation

2016 ◽  
Vol 2016 ◽  
pp. 1-16 ◽  
Author(s):  
Akinobu Yamaguchi ◽  
Ikuo Okada ◽  
Takao Fukuoka ◽  
Mari Ishihara ◽  
Ikuya Sakurai ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Synchrotron Radiation ◽  
Cupric Oxide ◽  
Oxide Particle ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
One Step ◽  
Oxide Particles

The deposition of copper (Cu) and cupric oxide (Cu4O3, Cu2O, and CuO) particles in an aqueous copper sulfate (CuSO4) solution with additive alcohol such as methanol, ethanol, 2-propanol, and ethylene glycol has been studied by X-ray exposure from synchrotron radiation. An attenuated X-ray radiation time of 5 min allows for the synthesis of Cu, Cu4O3, Cu2O, and CuO nano/microscale particles and their aggregation into clusters. The morphology and composition of the synthesized Cu/cupric oxide particle clusters were characterized by scanning electron microscopy, scanning transmission electron microscopy, and high-resolution transmission electron microscopy with energy dispersive X-ray spectroscopy. Micro-Raman spectroscopy revealed that the clusters comprised cupric oxide core particles covered with Cu particles. Neither Cu/cupric oxide particles nor their clusters were formed without any alcohol additives. The effect of alcohol additives is attributed to the following sequential steps: photochemical reaction due to X-ray irradiation induces nucleation of the particles accompanying redox reaction and forms a cluster or aggregates by LaMer process and DLVO interactions. The procedure offers a novel route to synthesize the Cu/cupric oxide particles and aggregates. It also provides a novel additive manufacturing process or lithography of composite materials such as metal, oxide, and resin.

Quantitative Chemical Analysis of Sub-Micron Phase Segregation In Polyurethane Polymers by Soft X-Ray Spectromicroscopy

1997 ◽  
Vol 3 (S2) ◽  
pp. 909-910
Author(s):  
A.P. Hitchcock ◽  
S.G. Urquhart ◽  
E.G. Rightor ◽  
W. Lidy ◽  
H. Ade ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Spatial Resolution ◽  
Chemical Properties ◽  
Phase Segregation ◽  
Quantitative Chemical Analysis ◽  
X Ray ◽  
Scanning Transmission ◽  
Complex Polymers ◽  
Physical And Chemical ◽  
Quantitative Chemical

Phase segregation is important in determining the physical and chemical properties of many complex polymers, including polyurethanes. Achieving a better understanding of the connections between formulation chemistry, the chemical nature of segregated phases, and the physical properties of the resulting polymer, has the potential to greatly advance the development of improved polyurethane materials. However, the sub-micron size of segregated features precludes their chemical analysis by most existing methods. Near edge X-ray absorption spectroscopy carried out with sub micron spatial resolution provides one of the few suitable means for quantitative chemical analysis (speciation) of individual segregated phases. We have used the NSLS and ALS scanning transmission x-ray microscopes (STXM) to record images and spectra of both model and real polyurethane polymers. Relative to energy loss spectroscopy in a transmission electron microscope, STXM has remarkable advantages with regard to a much lower radiation damage rates and much higher spectral resolution (∼0.1 eV at the C ls edge), with a spatial resolution (∼0.1 μm) adequate for many real world problems in polymer analysis.

scholarly journals Application of Scanning Transmission X-Ray Microscopy to the Rubber Industry

2003 ◽  
Vol 76 (4) ◽  
pp. 803-811 ◽  
Author(s):  
D. A. Winesett ◽  
H. Ade ◽  
A. P. Smith ◽  
S. G. Urquhart ◽  
A. J. Dias ◽  
...  
Keyword(s):  
High Spatial Resolution ◽  
Chemical Sensitivity ◽  
Rubber Industry ◽  
X Ray ◽  
Complex Morphology ◽  
Component Systems ◽  
Scanning Transmission ◽  
X Ray Absorption ◽  
Beam Damage

Abstract Materials of commercial significance in the rubber industry are usually multi-component systems composed of several elastomers and various fillers. Elucidating the complex morphology that can arise from blending and understanding how this affects the various properties are essential. A technique advantageous to the study of multi-component elastomeric systems is Scanning Transmission X-ray Microscopy (STXM). STXM utilizes the chemical sensitivity of Near Edge X-ray Absorption Fine Structure (NEXAFS) and combines with relatively high spatial resolution and low beam damage to allow the successful characterization of multi-component materials that may be difficult or impossible with other techniques. An overview of the technique and example applications for the rubber industry is presented.

Digital x-ray mapping of catalyst particles

1984 ◽  
Vol 42 ◽  
pp. 654-655
Author(s):  
C. E. Lyman
Keyword(s):  
Spatial Resolution ◽  
Energy Dispersive Spectrometer ◽  
Scanning Transmission Electron Microscope ◽  
Polished Section ◽  
Early Application ◽  
X Ray ◽  
Electron Probe Microanalyzer ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Early Maps

Formation of 2-dimensional dot maps of x-ray intensity from various elements in a flat polished section was an early application of the scanning beam electron probe microanalyzer. The spatial resolution of those early maps was the same as the microprobe itself, about lpm. These maps were usually scanned in an analogue fashion, and there was generally enough x-ray signal to produce maps with good peak-to-background ratios. For analysis of individual catalyst particles, a scanning transmission electron microscope (STEM) must be used to obtain the required spatial resolution. However, the x-ray signal level is usually low and is collected with an energy-dispersive spectrometer which has a lower peak-to-background ratio than the wavelength-dispersive spectrometer used in the microprobe. To produce suitable high magnification x-ray maps of catalyst particles digital beam techniques were employed.

Applications of high spatial resolution hicroanalysis to materials problems using dedicated STEM

1978 ◽  
Vol 36 (1) ◽  
pp. 418-419
Author(s):  
Ernest L. Hall ◽  
John B. Vander Sande
Keyword(s):  
Spatial Resolution ◽  
High Spatial Resolution ◽  
Profile Analysis ◽  
Scanning Transmission Electron Microscope ◽  
Dramatic Improvement ◽  
X Ray ◽  
Transmission Electron ◽  
Probe Size ◽  
Scanning Transmission ◽  
Compositional Variations

The scanning transmission electron microscope has afforded a dramatic improvement in the spatial resolution of X-ray microanalysis of thin specimens, allowing the investigation of extremely localized compositional variations in materials systems. In this paper, the results of high resolution composition profile analysis in several materials are presented. The materials were analyzed in a 100 kV field emission STEM manufactured by VG Microscopes, Ltd., and fitted with an energy dispersive X-ray spectrometer. The specimens were held in a double-tilt graphite cartridge which allowed X-ray detection in the tilt range 0°-20° about each axis. The vacuum in the specimen chamber was ∿ 2 x 10-9 torr during analysis. Electron probe spot sizes of 5-10 Å were used, corresponding to probe currents in the range of 10-10-10-9 amps.For a given specimen composition, the spatial resolution of X-ray microanalysis in thin specimens is a function of probe size, accelerating voltage, specimen atomic number, and thickness.

scholarly journals Chemically Sensitive Tomography at 50 nm Spatial Resolution using a Soft X-ray Scanning Transmission X-Ray Microscope

2006 ◽  
Vol 12 (S02) ◽  
pp. 1412-1413 ◽  
Author(s):  
GA Johansson ◽  
JJ Dynes ◽  
AP Hitchcock ◽  
T Tyliszczak ◽  
GD Swerhone ◽  
...  
Keyword(s):  
Spatial Resolution ◽  
X Ray ◽  
Scanning Transmission

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

In situ Analysis of the Fate and behavior of Inorganic Nanomaterials in Biological System by Synchrotron Radiation X-ray Probe Techniques

2021 ◽  
Vol 17 ◽  
Author(s):  
Shuang Zhu ◽  
Yaling Wang ◽  
Chunying Chen
Keyword(s):  
Synchrotron Radiation ◽  
Biological Systems ◽  
Analytical Techniques ◽  
High Sensitivity ◽  
Electronic Configuration ◽  
X Ray ◽  
Scanning Transmission ◽  
Inorganic Nanomaterials ◽  
And Behavior ◽  
Fate And Behavior

Background: The comprehensive understanding of nanomaterial behavior in biological systems is essential in accurately modeling and predicting nanomaterial fate and toxicity. Synchrotron radiation (SR) X-ray techniques, based on their ability to study electronic configuration, coordination geometry, or oxidative state of nanomaterials with high sensitivity and spatial resolution, have been introduced to analyze the transformation behavior of nanomaterials in biological systems. Methods: Previous research in this field are classified and summarized. Results: To start with, a brief introduction of a few widely used SR-based analytical techniques including X-ray absorption spectroscopy, X-ray fluorescence microprobe, scanning transmission X-ray microscopy and circular dichroism spectroscopy is provided. Then, the recent advances of their applications in the analysis of nanomaterial behaviors are elaborated based on different nanomaterial transformation forms such as biodistribution, biomolecule interaction, decomposition, redox reaction, and recrystallization/agglomeration. Finally, a few challenges faced in this field are proposed. Conclusion: This review summarizes the application of SR X-ray techniques in analyzing the fate of inorganic nanomaterials in biological systems. We hope it can help the readers to have a general understanding of the applications of SR-based techniques in studying nanomaterial biotransformation and to stimulate more insightful researches in relevant fields.

Quantitative Chemical Speciation of Multi-Phase Polymers Using Zone Plate x-ray Microscopy

1998 ◽  
Vol 4 (S2) ◽  
pp. 808-809
Author(s):  
A.P. Hitchcock ◽  
S.G. Urquhart ◽  
H. Ade ◽  
E.G. Rightor ◽  
W. Lidy
Keyword(s):  
Chemical Analysis ◽  
Spatial Resolution ◽  
Phase Segregation ◽  
Zone Plate ◽  
Quantitative Chemical Analysis ◽  
X Ray ◽  
Scanning Transmission ◽  
Complex Polymers ◽  
Multi Phase ◽  
Quantitative Chemical

Phase segregation is important in determining the properties of many complex polymers, including polyurethanes. Achieving a better understanding of the links between formulation, chemical nature of segregated phases, and physical properties, has the potential to aid development of improved polymers. However, the sub-micron size of segregated features precludes detailed chemical analysis by most existing methods. Zone-plate based, scanning transmission X-ray microscopes (STXM) at NSLS and ALS provide quantitative chemical analysis (speciation) of segregated polymer phases at ∼50 nm spatial resolution. Image sequences acquire much more data with less radiation damage, than spot spectra. After alignment, they provide high quality near edge spectra, and thus quantitative analysis, at full spatial resolution.Fig. 1 shows an image and spectra acquired with the NSLS STXM of a macro-phase segregated TDI polyurethane. Spectral decomposition using model polymer spectra is used to measure the local urea, urethane and polyether content.

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