X-Ray Microscopy Of Multiphase Polymeric Materials

1996 ◽  
Vol 437 ◽  
Author(s):  
H. Ade ◽  
A. P. Smith ◽  
G. R. Zhuang ◽  
B. Wood ◽  
I. Plotzker ◽  
...  
Keyword(s):  
Liquid Crystalline ◽  
National Laboratory ◽  
Polymeric Materials ◽  
High Energy ◽  
Brookhaven National Laboratory ◽  
Energy Calibration ◽  
High Energy Resolution ◽  
X Ray ◽  
Scanning Transmission ◽  
Spectral Fidelity

AbstractWe have utilized the scanning transmission x-ray microscope at Brookhaven National Laboratory to acquire high energy resolution spectra of various polymers and to investigate the bulk characteristics of multiphasic polymeric materials with chemical sensitivity at a spatial resolution of about 50 nm. We present studies ranging from phase separated liquid crystalline polyesters and polyurethanes to various polymer blends. Improvements in the NEXAFS imaging and spectral acquisition protocol in the recent past provide much improved spectral fidelity and include in situ energy calibration with CO2.

Mapping DNA and protein in biological samples using the scanning transmission x-ray microscope

1994 ◽  
Vol 52 ◽  
pp. 50-51
Author(s):  
X. Zhang ◽  
R. Balhorn ◽  
C. Jacobsen ◽  
J. Kirz ◽  
S. Williams
Keyword(s):  
Biological Samples ◽  
National Laboratory ◽  
Local Environment ◽  
High Energy ◽  
Brookhaven National Laboratory ◽  
High Energy Resolution ◽  
X Rays ◽  
X Ray ◽  
Scanning Transmission ◽  
Absorption Edges

The Scanning Transmission soft X-ray Microscope (STXM) at the XIA beamline at the National Synchrotron Light Source, Brookhaven National Laboratory, has achieved 50 nm Rayleigh resolution and has been used to image wet biological samples using the natural absorption differences between carbon and water in the water window (between carbon and oxygen K-absorption edges). The step-like jumps in the absorption of soft x-rays by materials as a function of energy have been used for elemental mapping. Examination of these absorption "edges" with high energy resolution resolves fine absorption structures. These fine structures are strongly affected by the atom's local environment, such that they carry detailed information about the atom's chemical state. We have used this chemical sensitivity to distinguish between materials which have similar elemental composition but are chemically different. Images with 50 nm resolution and spectra from a spot size less than (0.2 (μm)2 can be acquired routinely.Figure 1 shows the x-ray absorption fine structure spectra at the carbon absorption edge from DNA and bovine serum albumin (BSA, a typical protein) taken using the STXM.

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.

Chemical and orientational imaging of polymeric samples

1994 ◽  
Vol 52 ◽  
pp. 68-69
Author(s):  
H. Ade ◽  
B. Hsiao ◽  
G. Mitchell ◽  
E. Rightor ◽  
A. P. Smith ◽  
...  
Keyword(s):  
Ethylene Terephthalate ◽  
National Laboratory ◽  
Brookhaven National Laboratory ◽  
Carbonyl Groups ◽  
Aromatic Rings ◽  
Edge Structure ◽  
X Ray ◽  
Scanning Transmission ◽  
Polymeric Samples ◽  
X Ray Absorption

We have used the Scanning Transmission X-ray Microscope at beamline X1A (X1-STXM) at Brookhaven National Laboratory (BNL) to acquire high resolution, chemical and orientation sensitive images of polymeric samples as well as point spectra from 0.1 μm areas. This sensitivity is achieved by exploiting the X-ray Absorption Near Edge Structure (XANES) of the carbon K edge. One of the most illustrative example of the chemical sensitivity achievable is provided by images of a polycarbonate/pol(ethylene terephthalate) (70/30 PC/PET) blend. Contrast reversal at high overall contrast is observed between images acquired at 285.36 and 285.69 eV (Fig. 1). Contrast in these images is achieved by exploring subtle differences between resonances associated with the π bonds (sp hybridization) of the aromatic groups of each polymer. PET has a split peak associated with these aromatic groups, due to the proximity of its carbonyl groups to its aromatic rings, whereas PC has only a single peak.

Micro-X-Ray Fluorescence Analysis on a Synchrotron Radiation Wiggler Beam Line

1991 ◽  
Vol 35 (B) ◽  
pp. 995-1000
Author(s):  
J.V. Gilfrich ◽  
E.F. Skelton ◽  
S.B. Qadri ◽  
N.E. Moulton ◽  
D.J. Nagel ◽  
...  
Keyword(s):  
Synchrotron Radiation ◽  
National Laboratory ◽  
Incident Beam ◽  
Fluorescence Analysis ◽  
High Energy ◽  
Brookhaven National Laboratory ◽  
Beam Line ◽  
X Rays ◽  
X Ray ◽  
Electron Orbit

AbstractIt has been well established over recent years that synchrotron radiation possesses some unique features as a source of primary x-rays for x-ray fluorescence analysis. Advantage has been taken of the high intensity emanating from the bending magnets of storage rings to develop x-ray microprobes utilizing apertures or focussing optics, or both, to provide a beam spot at the specimen of the order of micrometers. The use of insertion devices wigglers and undulatora, can further increase the available intensity, especially for the high energy photons. Beam Line X-17C at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory, accepts the unmodified continuum radiation from a superconducting wiggler in the storage ring. Some initial XRF measurements have been made on this beam line using apertures in the 10 to 100 micrometer range. The fluorescent radiation was measured by an intrinsic Ge detector having an energy resolution of 300 eV at 15 kev, and located at 90° to the incident beam in the plane of the electron orbit. In samples containing many elements, detection limits of a few ppm were achieved with 100 μm beams.

Imaging, Spectroscopy and Tomography of Frozen Hydrated Specimens With the Cryo Scanning Transmission X-Ray Microscope at The NSLS

1998 ◽  
Vol 4 (S2) ◽  
pp. 354-355
Author(s):  
J. Maser ◽  
C. Jacobsen ◽  
Y. Wang ◽  
A. Osanna ◽  
B. Winn ◽  
...  
Keyword(s):  
National Laboratory ◽  
Imaging Spectroscopy ◽  
Optical Resolution ◽  
Brookhaven National Laboratory ◽  
X Rays ◽  
X Ray ◽  
Measuring Techniques ◽  
Steady Improvement ◽  
Scanning Transmission ◽  
Synchrotron Light

With the steady improvement of x-ray optics with high resolution and efficiency, and continued development or adaptation of different imaging and measuring techniques, soft x-ray microscopy has emerged as a powerful method to image and analyze fully hydrated specimens of several micrometer thickness at sub-optical resolution (for a recent overview, see ref. 1). We report on experiments performed with the cryo scanning transmission x-ray microscope (cryo-STXM), which has recently come into operation at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory.Cryo-STXM uses x-rays with energies between the absorption edge of Carbon (E = 284 eV) and Oxygen (E = 543 eV) from the soft x-ray undulator at the NSLS. Fully hydrated specimens such as eucaryotic cells in water or ice layers of up to 10 micrometer thickness can be imaged without any additional need for contrast enhancing techniques.

In Situ Monitoring of the Electrochemical Absorption of Deuterium into Palladium by X-Ray Diffraction using Synchrotron-Wiggler Radiation

1998 ◽  
Vol 524 ◽  
Author(s):  
D. D. Dominguez ◽  
P. L. Hagans ◽  
E. F. Skelton ◽  
S. B. Qadri ◽  
D. J. Nagel
Keyword(s):  
Structural Changes ◽  
National Laboratory ◽  
High Energy ◽  
Brookhaven National Laboratory ◽  
In Situ Monitoring ◽  
X Rays ◽  
X Ray ◽  
Β Phase ◽  
Metallic Sample

ABSTRACTWith low energy x-rays, such as those from a Cu x-ray tube, only the outer few microns of a metallic sample can be probed. This low penetrating power prohibits structural studies from being carried out on the interior of an electrode in an electrochemical cell because of absorption by the cell material, electrodes and the electrolyte. The work described in this paper circumvents this problem by utilizing high energy, high brightness x-rays produced on the superconducting wiggler beam line, X-17C, at the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory. The penetrating power of the higher energy x-rays allowed Pd diffraction spectra to be obtained in-situ on a 1 mm diameter Pd wire cathode during electrolysis of heavy water. Moreover, the beam (28 × 28 μm in cross-section) allowed diffraction spectra to be acquired as a function of distance across the sample. Spectra were recorded in 50 μm steps from the edge of the Pd wire to its core. This was done at 2 minute intervals as a function of electrolysis time. The α-β phase transition induced in the Pd while deuterium was electrochemically absorbed was observed by monitoring the Pd-(422) diffraction peaks. Results allowed the diffusion rate and the diffusivity of deuterium atoms in the Pd wire to be determined. Other features of the structural changes associated with the absorption of deuterium into Pd are reported.

X-Ray Microscopy Analysis of the Morphology of Poly(Ethylene Terephthalate)/Vectra Blends Produced by Mechanical Alloying

1998 ◽  
Vol 4 (S2) ◽  
pp. 144-145
Author(s):  
A. P. Smith ◽  
C. Bai ◽  
H. Ade ◽  
R. J. Spontak ◽  
C. M. Balik ◽  
...  
Keyword(s):  
Mechanical Alloying ◽  
Ethylene Terephthalate ◽  
Polymeric Materials ◽  
High Energy ◽  
Polymer Science ◽  
X Rays ◽  
X Ray ◽  
Poly Ethylene Terephthalate ◽  
Scanning Transmission ◽  
Poly Ethylene

The intimate blending of two incompatible polymeric materials constitutes one of the most important fields of study in polymer science. A vast arsenal of techniques, ranging from copolymerization to melt-blending, has been assembled to mix intrinsically immiscible polymers and optimize the physical properties of the resultant system. For some systems, however, even established techniques cannot produce useable blends. To overcome this limitation, non-equilibrium mechanical alloying (high-energy ball milling of two or more dissimilar powders) has been employed to produce blends of poly(ethylene terephthalate) (PET) and Vectra (73/27 oxybenzoate/oxynaphthoate). Characterization of these blends by TEM is confounded by the absence of a preferential staining agent, in which case Scanning Transmission X-ray Microscopy (STXM) provides a valuable alternative in examining the morphology and chemistry of these blends.The x-ray microscope utilizes a diffraction element called a zone plate to focus soft x-rays into a microprobe. A thin section of sample is placed in this microprobe, and the transmitted photon intensity measured.

scholarly journals High-Energy-Resolution Fluorescence-Detected X-ray Absorption of the Q Intermediate of Soluble Methane Monooxygenase

2017 ◽  
Vol 139 (49) ◽  
pp. 18024-18033 ◽  
Author(s):  
Rebeca G. Castillo ◽  
Rahul Banerjee ◽  
Caleb J. Allpress ◽  
Gregory T. Rohde ◽  
Eckhard Bill ◽  
...  
Keyword(s):  
Energy Resolution ◽  
Methane Monooxygenase ◽  
High Energy ◽  
High Energy Resolution ◽  
X Ray ◽  
Soluble Methane Monooxygenase ◽  
X Ray Absorption

scholarly journals High-energy resolution X-ray absorption and emission spectroscopy reveals insight into unique selectivity of La-based nanoparticles for CO2

2015 ◽  
Vol 112 (52) ◽  
pp. 15803-15808 ◽  
Author(s):  
Ofer Hirsch ◽  
Kristina O. Kvashnina ◽  
Li Luo ◽  
Martin J. Süess ◽  
Pieter Glatzel ◽  
...  
Keyword(s):  
Energy Resolution ◽  
Emission Spectroscopy ◽  
High Energy ◽  
Unit Cell ◽  
High Energy Resolution ◽  
Electron Configuration ◽  
Edge Structure ◽  
X Ray ◽  
X Ray Absorption

The lanthanum-based materials, due to their layered structure and f-electron configuration, are relevant for electrochemical application. Particularly, La2O2CO3 shows a prominent chemoresistive response to CO2. However, surprisingly less is known about its atomic and electronic structure and electrochemically significant sites and therefore, its structure–functions relationships have yet to be established. Here we determine the position of the different constituents within the unit cell of monoclinic La2O2CO3 and use this information to interpret in situ high-energy resolution fluorescence-detected (HERFD) X-ray absorption near-edge structure (XANES) and valence-to-core X-ray emission spectroscopy (vtc XES). Compared with La(OH)3 or previously known hexagonal La2O2CO3 structures, La in the monoclinic unit cell has a much lower number of neighboring oxygen atoms, which is manifested in the whiteline broadening in XANES spectra. Such a superior sensitivity to subtle changes is given by HERFD method, which is essential for in situ studying of the interaction with CO2. Here, we study La2O2CO3-based sensors in real operando conditions at 250 °C in the presence of oxygen and water vapors. We identify that the distribution of unoccupied La d-states and occupied O p- and La d-states changes during CO2 chemoresistive sensing of La2O2CO3. The correlation between these spectroscopic findings with electrical resistance measurements leads to a more comprehensive understanding of the selective adsorption at La site and may enable the design of new materials for CO2 electrochemical applications.

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