Scanning Transmission X-Ray Microscopy of Curative and Filler Migration of Inner Liner Compounds

2007 ◽  
Vol 80 (1) ◽  
pp. 14-23
Author(s):  
D. A. Winesett ◽  
A. H. Tsou

Abstract Materials of significance in the rubber industry generally consist of a complex blend of elastomers, fillers, curing agents and other additives. Elucidating the complex microstructure-to-property relationship of these materials is essential for optimal product development. This requires characterization techniques that are capable to differentiate, map, and quantify these similar materials with sufficiently high spatial resolution. A technique that can provide such chemical microspeciation is Scanning Transmission X-ray Microscopy (STXM). STXM is a beamline based microscopy that utilizes the chemical specificity of Near Edge X-ray Absorption Fine Structure (NEXAFS) combined with zone plate optics to achieve high spatial resolution (< 50 nm) and low beam damage to allow the successful characterization of multi-component materials that would be difficult or impossible with other techniques. A brief introduction to the technique will be presented along with example applications showing curative and filler distribution mapping in multi-component elastomeric systems.

2003 ◽  
Vol 76 (4) ◽  
pp. 803-811 ◽  
Author(s):  
D. A. Winesett ◽  
H. Ade ◽  
A. P. Smith ◽  
S. G. Urquhart ◽  
A. J. Dias ◽  
...  

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.


2005 ◽  
Vol 71 (3) ◽  
pp. 1300-1310 ◽  
Author(s):  
Brandy Toner ◽  
Sirine Fakra ◽  
Mario Villalobos ◽  
Tony Warwick ◽  
Garrison Sposito

ABSTRACT Pseudomonas putida strain MnB1, a biofilm-forming bacterial culture, was used as a model for the study of bacterial Mn oxidation in freshwater and soil environments. The oxidation of aqueous Mn+2 [Mn+2 (aq)] by P. putida was characterized by spatially and temporally resolving the oxidation state of Mn in the presence of a bacterial biofilm, using scanning transmission X-ray microscopy (STXM) combined with near-edge X-ray absorption fine structure (NEXAFS) spectroscopy at the Mn L2,3 absorption edges. Subsamples were collected from growth flasks containing 0.1 and 1 mM total Mn at 16, 24, 36, and 48 h after inoculation. Immediately after collection, the unprocessed hydrated subsamples were imaged at a 40-nm resolution. Manganese NEXAFS spectra were extracted from X-ray energy sequences of STXM images (stacks) and fit with linear combinations of well-characterized reference spectra to obtain quantitative relative abundances of Mn(II), Mn(III), and Mn(IV). Careful consideration was given to uncertainty in the normalization of the reference spectra, choice of reference compounds, and chemical changes due to radiation damage. The STXM results confirm that Mn+2 (aq) was removed from solution by P. putida and was concentrated as Mn(III) and Mn(IV) immediately adjacent to the bacterial cells. The Mn precipitates were completely enveloped by bacterial biofilm material. The distribution of Mn oxidation states was spatially heterogeneous within and between the clusters of bacterial cells. Scanning transmission X-ray microscopy is a promising tool for advancing the study of hydrated interfaces between minerals and bacteria, particularly in cases where the structure of bacterial biofilms needs to be maintained.


2015 ◽  
Vol 22 (5) ◽  
pp. 1306-1311 ◽  
Author(s):  
Nark-Eon Sung ◽  
Ik-Jae Lee ◽  
Kug-Seong Lee ◽  
Seong-Hun Jeong ◽  
Seen-Woong Kang ◽  
...  

A microprobe system has been installed on the nanoprobe/XAFS beamline (BL8C) at PLS-II, South Korea. Owing to the reproducible switch of the gap of the in-vacuum undulator (IVU), the intense and brilliant hard X-ray beam of an IVU can be used in X-ray fluorescence (XRF) and X-ray absorption fine-structure (XAFS) experiments. For high-spatial-resolution microprobe experiments a Kirkpatrick–Baez mirror system has been used to focus the millimeter-sized X-ray beam to a micrometer-sized beam. The performance of this system was examined by a combination of micro-XRF imaging and micro-XAFS of a beetle wing. These results indicate that the microprobe system of the BL8C can be used to obtain the distributions of trace elements and chemical and structural information of complex materials.


Author(s):  
Ernest L. Hall ◽  
John B. Vander Sande

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.


2019 ◽  
Vol 90 (6) ◽  
pp. 063702
Author(s):  
P. Mabey ◽  
B. Albertazzi ◽  
Th. Michel ◽  
G. Rigon ◽  
S. Makarov ◽  
...  

2012 ◽  
Vol 111 (8) ◽  
pp. 084904 ◽  
Author(s):  
Amrinder S. Gill ◽  
Zhong Zhou ◽  
Ulrich Lienert ◽  
Jonathan Almer ◽  
David F. Lahrman ◽  
...  

Nanoscale ◽  
2015 ◽  
Vol 7 (5) ◽  
pp. 1534-1548 ◽  
Author(s):  
Angela E. Goode ◽  
Alexandra E. Porter ◽  
Mary P. Ryan ◽  
David W. McComb

Benefits and challenges of correlative spectroscopy: electron energy-loss spectroscopy in the scanning transmission electron microscope (STEM-EELS) and X-ray absorption spectroscopy in the scanning transmission X-ray microscope (STXM-XAS).


2016 ◽  
Vol 43 (6Part1) ◽  
pp. 2731-2740 ◽  
Author(s):  
Jakob C. Larsson ◽  
Ulf Lundström ◽  
Hans M. Hertz

2011 ◽  
Vol 6 (12) ◽  
pp. C12013-C12013 ◽  
Author(s):  
H Kudrolli ◽  
H Bhandari ◽  
M Breen ◽  
V Gelfandbein ◽  
S R Miller ◽  
...  

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