SOFT X-RAY MICROSCOPY OF SOFT MATTER — HARD INFORMATION FROM TWO SOFTS

2002 ◽  
Vol 09 (01) ◽  
pp. 193-201 ◽  
Author(s):  
A. P. HITCHCOCK ◽  
C. MORIN ◽  
T. TYLISZCZAK ◽  
I. N. KOPRINAROV ◽  
H. IKEURA-SEKIGUCHI ◽  
...  
Keyword(s):  
Soft Matter ◽  
Phase Segregation ◽  
Soft Materials ◽  
Quantitative Information ◽  
Quantitative Chemical Analysis ◽  
X Rays ◽  
X Ray ◽  
Hard Information ◽  
Scanning Transmission ◽  
X Ray Absorption

Scanning transmission X-ray microscopy (STXM) and X-ray photoelectron emission microscopy (X-PEEM) provide quantitative chemical analysis at a spatial resolution well below 100 nm. Soft X-ray absorption or near edge X-ray absorption (NEXAFS) contrast provides sensitive differentiation of species which have similar elemental composition but are chemically distinct. Due to the ability of soft X-rays at wavelengths below the O K-edge to penetrate water, and on account of lower radiation damage, soft X-ray microscopy is an ideal tool for providing quantitative information about soft matter in the context of biological, polymer and environmental studies. Examples are given from recent studies of: phase segregation in polyurethanes and polymer blends, protein adsorption on polymers relating to biomaterial optimization, and metal mapping in biofilms. These examples show that it is indeed possible to get quantitative (hard) information by combining soft X-rays and soft materials.

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.

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.

scholarly journals Imaging local electric fields produced upon synchrotron X-ray exposure

2014 ◽  
Vol 112 (3) ◽  
pp. 696-701 ◽  
Author(s):  
Christopher M. Dettmar ◽  
Justin A. Newman ◽  
Scott J. Toth ◽  
Michael Becker ◽  
Robert F. Fischetti ◽  
...  
Keyword(s):  
Electric Fields ◽  
Second Harmonic ◽  
Soft Materials ◽  
Local Fields ◽  
X Rays ◽  
Electron Hole ◽  
X Ray ◽  
X Ray Absorption ◽  
Static Electric Fields ◽  
Cryogenic Conditions

Electron–hole separation following hard X-ray absorption during diffraction analysis of soft materials under cryogenic conditions produces substantial local electric fields visualizable by second harmonic generation (SHG) microscopy. Monte Carlo simulations of X-ray photoelectron trajectories suggest the formation of substantial local electric fields in the regions adjacent to those exposed to X-rays, indicating a possible electric-field–induced SHG (EFISH) mechanism for generating the observed signal. In studies of amorphous vitreous solvents, analysis of the SHG spatial profiles following X-ray microbeam exposure was consistent with an EFISH mechanism. Within protein crystals, exposure to 12-keV (1.033-Å) X-rays resulted in increased SHG in the region extending ∼3 μm beyond the borders of the X-ray beam. Moderate X-ray exposures typical of those used for crystal centering by raster scanning through an X-ray beam were sufficient to produce static electric fields easily detectable by SHG. The X-ray–induced SHG activity was observed with no measurable loss for longer than 2 wk while maintained under cryogenic conditions, but disappeared if annealed to room temperature for a few seconds. These results provide direct experimental observables capable of validating simulations of X-ray–induced damage within soft materials. In addition, X-ray–induced local fields may potentially impact diffraction resolution through localized piezoelectric distortions of the lattice.

Studies of metaphase chromosomes in the scanning transmission x-ray microscope: Image fidelity, radiation damage and specimen preparation

1992 ◽  
Vol 50 (2) ◽  
pp. 1038-1039
Author(s):  
Shawn Williams ◽  
Xiaodong Zhang ◽  
Susan Lamm ◽  
Jack Van’t Hof
Keyword(s):  
Visible Light ◽  
Radiation Damage ◽  
Cross Section ◽  
Imaging Techniques ◽  
Dose Range ◽  
Specimen Preparation ◽  
X Rays ◽  
Metaphase Chromosomes ◽  
X Ray ◽  
Scanning Transmission

The Scanning Transmission X-ray Microscope (STXM) is well suited for investigating metaphase chromosome structure. The absorption cross-section of soft x-rays having energies between the carbon and oxygen K edges (284 - 531 eV) is 6 - 9.5 times greater for organic specimens than for water, which permits one to examine unstained, wet biological specimens with resolution superior to that attainable using visible light. The attenuation length of the x-rays is suitable for imaging micron thick specimens without sectioning. This large difference in cross-section yields good specimen contrast, so that fewer soft x-rays than electrons are required to image wet biological specimens at a given resolution. But most imaging techniques delivering better resolution than visible light produce radiation damage. Soft x-rays are known to be very effective in damaging biological specimens. The STXM is constructed to minimize specimen dose, but it is important to measure the actual damage induced as a function of dose in order to determine the dose range within which radiation damage does not compromise image quality.

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.

X-Ray absorption edge elemental imaging of B. thuringienis

1989 ◽  
Vol 47 ◽  
pp. 212-213
Author(s):  
R. L. Stears
Keyword(s):  
Absorption Edge ◽  
Elemental Distribution ◽  
X Rays ◽  
Differential Absorption ◽  
Synchrotron Source ◽  
High Brightness ◽  
X Ray ◽  
Elemental Imaging ◽  
Cellular Integrity ◽  
X Ray Absorption

Because of the nature of the bacterial endospore, little work has been done on analyzing their elemental distribution and composition in the intact, living, hydrated state. The majority of the qualitative analysis entailed intensive disruption and processing of the endospores, which effects their cellular integrity and composition.Absorption edge imaging permits elemental analysis of hydrated, unstained specimens at high resolution. By taking advantage of differential absorption of x-ray photons in regions of varying elemental composition, and using a high brightness, tuneable synchrotron source to obtain monochromatic x-rays, contact x-ray micrographs can be made of unfixed, intact endospores that reveal sites of elemental localization. This study presents new data demonstrating the application of x-ray absorption edge imaging to produce elemental information about nitrogen (N) and calcium (Ca) localization using Bacillus thuringiensis as the test specimen.

scholarly journals Al-driven peculiarities of local coordination and magnetic properties in single-phase Alx-CrFeCoNi high-entropy alloys

Nano Research ◽  
2021 ◽  
Author(s):  
Alevtina Smekhova ◽  
Alexei Kuzmin ◽  
Konrad Siemensmeyer ◽  
Chen Luo ◽  
Kai Chen ◽  
...  
Keyword(s):  
Magnetic Properties ◽  
Single Phase ◽  
Magnetic Circular Dichroism ◽  
Surface Region ◽  
Face Centered Cubic ◽  
X Rays ◽  
X Ray ◽  
High Entropy ◽  
X Ray Absorption ◽  
Absorption Edges

AbstractModern design of superior multi-functional alloys composed of several principal components requires in-depth studies of their local structure for developing desired macroscopic properties. Herein, peculiarities of atomic arrangements on the local scale and electronic states of constituent elements in the single-phase face-centered cubic (fcc)- and body-centered cubic (bcc)-structured high-entropy Alx-CrFeCoNi alloys (x = 0.3 and 3, respectively) are explored by element-specific X-ray absorption spectroscopy in hard and soft X-ray energy ranges. Simulations based on the reverse Monte Carlo approach allow to perform a simultaneous fit of extended X-ray absorption fine structure spectra recorded at K absorption edges of each 3d constituent and to reconstruct the local environment within the first coordination shells of absorbers with high precision. The revealed unimodal and bimodal distributions of all five elements are in agreement with structure-dependent magnetic properties of studied alloys probed by magnetometry. A degree of surface atoms oxidation uncovered by soft X-rays suggests different kinetics of oxide formation for each type of constituents and has to be taken into account. X-ray magnetic circular dichroism technique employed at L2.3 absorption edges of transition metals demonstrates reduced magnetic moments of 3d metal constituents in the sub-surface region of in situ cleaned fcc-structured Al0.3-CrFeCoNi compared to their bulk values. Extended to nanostructured versions of multicomponent alloys, such studies would bring new insights related to effects of high entropy mixing on low dimensions.

scholarly journals Synchrotron X-ray induced acoustic imaging

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Seongwook Choi ◽  
Eun-Yeong Park ◽  
Sinyoung Park ◽  
Jong Hyun Kim ◽  
Chulhong Kim
Keyword(s):  
Acoustic Imaging ◽  
Signal Frequency ◽  
X Rays ◽  
Repetition Period ◽  
Linear Accelerators ◽  
X Ray ◽  
X Ray Computed ◽  
Medical Linear Accelerators ◽  
Ionizing Radiation Exposure ◽  
X Ray Absorption

AbstractX-ray induced acoustic imaging (XAI) is an emerging biomedical imaging technique that can visualize X-ray absorption contrast at ultrasound resolution with less ionizing radiation exposure than conventional X-ray computed tomography. So far, medical linear accelerators or industrial portable X-ray tubes have been explored as X-ray excitation sources for XAI. Here, we demonstrate the first feasible synchrotron XAI (sXAI). The synchrotron generates X-rays, with a dominant energy of 4 to 30 keV, a pulse-width of 30 ps, a pulse-repetition period of 2 ns, and a bunch-repetition period of 940 ns. The X-ray induced acoustic (XA) signals are processed in the Fourier domain by matching the signal frequency with the bunch-repetition frequency. We successfully obtained two-dimensional XA images of various lead targets. This novel sXAI tool could complement conventional synchrotron applications.

Dark-Field X-Ray Microscopy of Immunogold-Labeled Cells

1996 ◽  
Vol 2 (2) ◽  
pp. 53-62 ◽  
Author(s):  
Henry N. Chapman ◽  
Jenny Fu ◽  
Chris Jacobsen ◽  
Shawn Williams
Keyword(s):  
Colloidal Gold ◽  
Dark Field Image ◽  
Dark Field ◽  
X Rays ◽  
X Ray ◽  
Scanning Transmission ◽  
A Cell ◽  
Specific Antigens ◽  
Genetic Sequences ◽  
Novel Method

The methods of immunolabeling make visible the presence of specific antigens, proteins, genetic sequences, or functions of a cell. In this paper we present examples of imaging immunolabels in a scanning transmission x-ray microscope using the novel method of dark-field contrast. Colloidal gold, or silver-enhanced colloidal gold, is used as a label, which strongly scatters x-rays. This leads to a high-contrast dark-field image of the label and reduced radiation dose to the specimen. The x-ray images are compared with electron micrographs of the same labeled, unsectioned, whole cell. It is verified that the dark-field x-ray signal is primarily due to the label and the bright-field x-ray signal, showing absorption due to carbon, is largely unaffected by the label. The label can be well visualized even when it is embedded in or laying behind dense material, such as the cell nucleus. The resolution of the images is measured to be 60 nm, without the need for computer processing. This figure includes the x-ray microscope resolution and the accuracy of the label positioning. The technique should be particularly useful for the study of relatively thick (up to 10 μm), wet, or frozen hydrated specimens.

scholarly journals Semi-automated protein crystal mounting device for the sulfur single-wavelength anomalous diffraction method

2010 ◽  
Vol 43 (2) ◽  
pp. 341-346 ◽  
Author(s):  
Yu Kitago ◽  
Nobuhisa Watanabe ◽  
Isao Tanaka
Keyword(s):  
Diffraction Method ◽  
Systematic Errors ◽  
Protein Crystal ◽  
X Rays ◽  
Anomalous Diffraction ◽  
X Ray ◽  
Frozen Solution ◽  
Custom Made ◽  
Protein Molecules ◽  
X Ray Absorption

Use of longer-wavelength X-rays has advantages for the detection of small anomalous signals from light atoms, such as sulfur, in protein molecules. However, the accuracy of the measured diffraction data decreases at longer wavelengths because of the greater X-ray absorption. The capillary-top mounting method (formerly the loopless mounting method) makes it possible to eliminate frozen solution around the protein crystal and reduces systematic errors in the evaluation of small anomalous differences. However, use of this method requires custom-made tools and a large amount of skill. Here, the development of a device that can freeze the protein crystal semi-automatically using the capillary-top mounting method is described. This device can pick up the protein crystal from the crystallization drop using a micro-manipulator, and further procedures, such as withdrawal of the solution around the crystal by suction and subsequent flash freezing of the protein crystal, are carried out automatically. This device makes it easy for structural biologists to use the capillary-top mounting method for sulfur single-wavelength anomalous diffraction phasing using longer-wavelength X-rays.

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