Investigation of microstructural changes in impacted polyurea coatings using small angle X-ray scattering (SAXS)

2011 ◽  
Vol 26 (2) ◽  
pp. 149-154 ◽  
Author(s):  
Edward Balizer ◽  
Jeffry Fedderly ◽  
Gilbert Lee ◽  
Susan Bartyczak ◽  
Willis Mock

Three polyureas with decreasing soft segment molecular weights of 1000, 650, and a 250/1000 blend were molded onto circular steel plates and then impacted with a high speed (275 m/s) conical-shaped steel cylinder. The polyurea layer of the post mortem bilayers was characterized on a molecular level by small angle synchrotron X-ray scattering (SAXS) at the Advanced Photon Source at the Argonne National Laboratory. Analysis revealed that the hard domains of the polyureas with lower molecular weight soft segments reformed and oriented over a greater area of the coating, thus increasing the polymer strain hardening and resulting in visibly less out of plane bilayer deformation. This agrees with the hypothesis that polymer strain hardening is a mechanism that retards necking failure of the metal plate.

2018 ◽  
Vol 51 (3) ◽  
pp. 867-882 ◽  
Author(s):  
Jan Ilavsky ◽  
Fan Zhang ◽  
Ross N. Andrews ◽  
Ivan Kuzmenko ◽  
Pete R. Jemian ◽  
...  

Following many years of evolutionary development, first at the National Synchrotron Light Source, Brookhaven National Laboratory, and then at the Advanced Photon Source (APS), Argonne National Laboratory, the APS ultra-small-angle X-ray scattering (USAXS) facility has been transformed by several new developments. These comprise a conversion to higher-order crystal optics and higher X-ray energies as the standard operating mode, rapid fly scan measurements also as a standard operational mode, automated contiguous pinhole small-angle X-ray scattering (SAXS) measurements at intermediate scattering vectors, and associated rapid wide-angle X-ray scattering (WAXS) measurements for X-ray diffraction without disturbing the sample geometry. With each mode using the USAXS incident beam optics upstream of the sample, USAXS/SAXS/WAXS measurements can now be made within 5 min, allowingin situandoperandomeasurement capabilities with great flexibility under a wide range of sample conditions. These developments are described, together with examples of their application to investigate materials phenomena of technological importance. Developments of two novel USAXS applications, USAXS-based X-ray photon correlation spectroscopy and USAXS imaging, are also briefly reviewed.


2009 ◽  
Vol 42 (3) ◽  
pp. 469-479 ◽  
Author(s):  
Jan Ilavsky ◽  
Pete R. Jemian ◽  
Andrew J. Allen ◽  
Fan Zhang ◽  
Lyle E. Levine ◽  
...  

The design and operation of a versatile ultra-small-angle X-ray scattering (USAXS) instrument at the Advanced Photon Source (APS) at Argonne National Laboratory are presented. The instrument is optimized for the high brilliance and low emittance of an APS undulator source. It has angular and energy resolutions of the order of 10−4, accurate and repeatable X-ray energy tunability over its operational energy range from 8 to 18 keV, and a dynamic intensity range of 108to 109, depending on the configuration. It further offers quantitative primary calibration of X-ray scattering cross sections, a scattering vector range from 0.0001 to 1 Å−1, and stability and reliability over extended running periods. Its operational configurations include one-dimensional collimated (slit-smeared) USAXS, two-dimensional collimated USAXS and USAXS imaging. A robust data reduction and data analysis package, which was developed in parallel with the instrument, is available and supported at the APS.


2013 ◽  
Vol 46 (1) ◽  
pp. 1-13 ◽  
Author(s):  
Scott Classen ◽  
Greg L. Hura ◽  
James M. Holton ◽  
Robert P. Rambo ◽  
Ivan Rodic ◽  
...  

The SIBYLS beamline (12.3.1) of the Advanced Light Source at Lawrence Berkeley National Laboratory, supported by the US Department of Energy and the National Institutes of Health, is optimized for both small-angle X-ray scattering (SAXS) and macromolecular crystallography (MX), making it unique among the world's mostly SAXS or MX dedicated beamlines. Since SIBYLS was commissioned, assessments of the limitations and advantages of a combined SAXS and MX beamline have suggested new strategies for integration and optimal data collection methods and have led to additional hardware and software enhancements. Features described include a dual mode monochromator [containing both Si(111) crystals and Mo/B4C multilayer elements], rapid beamline optics conversion between SAXS and MX modes, active beam stabilization, sample-loading robotics, and mail-in and remote data collection. These features allow users to gain valuable insights from both dynamic solution scattering and high-resolution atomic diffraction experiments performed at a single synchrotron beamline. Key practical issues considered for data collection and analysis include radiation damage, structural ensembles, alternative conformers and flexibility. SIBYLS develops and applies efficient combined MX and SAXS methods that deliver high-impact results by providing robust cost-effective routes to connect structures to biology and by performing experiments that aid beamline designs for next generation light sources.


2013 ◽  
Vol 2013 ◽  
pp. 1-8
Author(s):  
Krit Koyvanich ◽  
Chitnarong Sirisathitkul ◽  
Supagorn Rugmai

The segmentation between rigid and rubbery chains in polyurethanes (PUs) influences polymeric properties and implementations. Several models have successfully been proposed to visualize the configuration between the hard segment (HS) and soft segment (SS). For particulate PU composites, the arrangement of HS and SS is more complicated because the fillers tend to disrupt the chain formation and segmentation. In this work, the effect of ferromagnetic cobalt (Co) powders (average diameter 2 μm) on PU synthesized from a reaction between polyether polyol (soft segment) and diphenylmethane-4,4′-diisocyanate (hard segment) was studied with varying loadings (0, 20, 40, and 60 wt.%). The 300 μm thick PU/Co samples were tape-casted and then received heat treatment at 80°C for 180 min. From synchrotron small angle X-ray scattering (SAXS), the plot of the X-ray scattering intensity (I) against the scattering vector (q) exhibited a typical single peak of PU whose intensity was reduced by the increase in the Co loading. Characteristic SAXS peaks in the case of 0-20 wt.% Co agreed well with the scattering by globular hard segment domains according to Zernike-Prins and Percus-Yevick models. The higher Co loadings led to larger deviations from all theoretical models.


1992 ◽  
Vol 63 (1) ◽  
pp. 1065-1067 ◽  
Author(s):  
L. A. Bernardes ◽  
H. Tolentino ◽  
A. R. D. Rodrigues ◽  
A. Craievich ◽  
I. Torriani

1981 ◽  
Vol 54 (5) ◽  
pp. 963-975 ◽  
Author(s):  
J. W. C. Van Bogart ◽  
P. E. Gibson ◽  
S. L. Cooper

Abstract The technique of small-angle x-ray scattering (SAXS) was used to investigate the morphology of three heat set (200–400% strain at 110–125°C) segmented elastomer samples—two polyester-polyurethanes and one polyether-polyester. The degree of hard-segment ordering in the samples varied from amorphous to slightly crystalline to highly crystalline. The results showed that the hard-segment domains in the semicrystalline materials developed axial ratios of about 2:1 for the axes parallel and perpendicular to the direction of stretch, while the sample with amorphous hard-segment domains showed no similar distortion in hard-segment domain shape and no anisotropy in the thickness of the interface between hard- and soft-segment domains.


2010 ◽  
Vol 57 (3) ◽  
pp. 1706-1715 ◽  
Author(s):  
Patrick M De Lurgio ◽  
Gary R Drake ◽  
Andrew S Kreps ◽  
Guy Jennings ◽  
John T Weizeorick ◽  
...  

Nanomaterials ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 860
Author(s):  
Alessio De Francesco ◽  
Luisa Scaccia ◽  
Ferdinando Formisano ◽  
Eleonora Guarini ◽  
Ubaldo Bafile ◽  
...  

We used the high-resolution Inelastic X-ray Scattering beamline of the Advanced Photon Source at Argonne National Laboratory to measure the terahertz spectrum of pure water and a dilute aqueous suspension of 15 nm diameter spherical Au nanoparticles (Au-NPs). We observe that, despite their sparse volume concentration of about 0.5%, the immersed NPs strongly influence the collective molecular dynamics of the hosting liquid. We investigate this effect through a Bayesian inference analysis of the spectral lineshape, which elucidates how terahertz transport properties of water change upon Au-NP immersion. In particular, we observe a nearly complete disappearance of the longitudinal acoustic mode and a mildly decreased ability to support shear wave propagation.


1981 ◽  
Vol 13 (5) ◽  
pp. 501-516 ◽  
Author(s):  
Takeji Hashimoto ◽  
Shoji Suehiro ◽  
Mitsuhiro Shibayama ◽  
Kenji Sauo ◽  
Hiromichi Kawai

2015 ◽  
Vol 22 (3) ◽  
pp. 760-765 ◽  
Author(s):  
Wenli Bi ◽  
Jiyong Zhao ◽  
Jung-Fu Lin ◽  
Quanjie Jia ◽  
Michael Y. Hu ◽  
...  

A new synchrotron radiation experimental capability of coupling nuclear resonant inelastic X-ray scattering with the cryogenically cooled high-pressure diamond anvil cell technique is presented. The new technique permits measurements of phonon density of states at low temperature and high pressure simultaneously, and can be applied to studies of phonon contribution to pressure- and temperature-induced magnetic, superconducting and metal–insulator transitions in resonant isotope-bearing materials. In this report, a pnictide sample, EuFe2As2, is used as an example to demonstrate this new capability at beamline 3-ID of the Advanced Photon Source, Argonne National Laboratory. A detailed description of the technical development is given. The Fe-specific phonon density of states and magnetism from the Fe sublattice in Eu57Fe2As2at high pressure and low temperature were derived by using this new capability.


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