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.

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.

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.

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.

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.

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.

Determination of the degree of radial order in Kevlar fibers using x-ray linear dichroism microscopy

1995 ◽  
Vol 53 ◽  
pp. 492-493
Author(s):  
A. P. Smith ◽  
H. Ade ◽  
B. Hsiao ◽  
S. Subramoney
Keyword(s):  
Spatial Resolution ◽  
National Laboratory ◽  
Linear Dichroism ◽  
Fiber Axis ◽  
X Rays ◽  
Specific Chemical ◽  
Edge Structure ◽  
Thin Sections ◽  
X Ray ◽  
X Ray Absorption

The Scanning Transmission X-ray Microscope (STXM) located at beamline X1A at the National Synchrotron Light Source at Brookhaven National Laboratory can be used to acquires high resolution, chemically and orientationally sensitive images with 50 nm spatial resolution, as well as point spectra from 0.1 μm2 areas. Chemical (valence) sensitivity can be achieved via the X-ray Absorption Near Edge Structure (XANES) at the carbon K edge. In addition, linear dichroism microscopy exploits the dependence of x-ray absorption resonances on the bond orientation relative to the linearly polarized x rays. Previous x-ray linear dichroism microscopy work has demonstrated the ability to determine the orientation of specific chemical groups within polymeric systems at high spatial resolution. Here, we have extended this technique to quantitatively determine the degree of radial order in various grades of poly(p-phenylene terephthalamide) (Kevlar™) fibers.The orientational dependence of the absorption cross-section yields “butterfly” patterns when thin sections of certain grades of Kevlar fibers cut at 45° with respect to the fiber axis are imaged at specific photon energies.

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.

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.

Determination of the Cation Distribution in NiFe2(PO4)2 using Resonant X-ray and Neutron Powder Diffraction

1995 ◽  
Vol 28 (5) ◽  
pp. 494-502 ◽  
Author(s):  
J. K. Warner ◽  
A. K. Cheetham ◽  
D. E. Cox
Keyword(s):  
Powder Diffraction ◽  
National Laboratory ◽  
Time Of Flight ◽  
Brookhaven National Laboratory ◽  
Neutron Powder Diffraction ◽  
Anomalous Scattering ◽  
Edge Structure ◽  
X Ray ◽  
Scattering Correction

The distribution of divalent iron and nickel over two metal sites of differing coordination geometry in NiFe2(PO4)2, sarcopside, has been investigated by resonant X-ray and time-of-flight neutron powder diffraction. To assess the reproducibility of the X-ray technique, data have been collected from instruments X7A at Brookhaven National Laboratory and 8.3 at the Synchrotron Radiation Source, Daresbury Laboratory, England, using wavelengths λ X1 = 1.7437 (3) Å and λ X2 = 1.7434 (1) Å, respectively, close to the Fe2+ K edge determined by X-ray absorption near-edge structure. The real part of the anomalous-scattering correction for iron at each energy, f′(Fe) X1 = −7.81 (9) and f′(Fe) X2 = −10.16 (6), was determined experimentally by diffraction from Fe3(PO4)2 under identical conditions. Occupancies obtained for iron at the M(1) site were found to be M(1) X1 = 0.366 (6) and M(1) X2 = 0.376 (3), compared with M(1) N = 0.26 (15) from time-of-flight neutron powder diffraction.

SPECTROMICROSCOPY OF BIOLOGICAL AND ENVIRONMENTAL SYSTEMS AT STONY BROOK: INSTRUMENTATION AND ANALYSIS

2002 ◽  
Vol 09 (01) ◽  
pp. 185-191 ◽  
Author(s):  
C. JACOBSEN ◽  
T. BEETZ ◽  
M. FESER ◽  
A. OSANNA ◽  
A. STEIN ◽  
...  
Keyword(s):  
Principal Component Analysis ◽  
Data Analysis ◽  
Environmental Science ◽  
National Laboratory ◽  
Principal Component ◽  
Brookhaven National Laboratory ◽  
National Synchrotron Light Source ◽  
X Ray ◽  
Synchrotron Light ◽  
Data Analysis Methods

Soft X-ray microscopy allows one to study nanoscale heterogeneities in dry and wet environmental science, biological, polymer, and geochemical specimens. Recent advances in instrumentation at the X-1A beamline at the National Synchrotron Light Source at Brookhaven National Laboratory are described. Spectromicroscopy data analysis methods including component mapping and principal component analysis (PCA) are then discussed.

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