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.

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.

scholarly journals Use of the Disk-of-least-confusion in X-ray Microanalysis

1998 ◽  
Vol 4 (S2) ◽  
pp. 274-275
Author(s):  
E. A. Kenik ◽  
S. X. Ren
Keyword(s):  
Spatial Resolution ◽  
Electron Scattering ◽  
Electron Probe ◽  
X Rays ◽  
High Brightness ◽  
X Ray ◽  
Electron Sources ◽  
Probe Diameter ◽  
Electron Probe Microanalyzer ◽  
Subsequent Emission

Whereas the spatial resolution for standard secondary electron (SEI) imaging in a scanning electron microscope or electron probe microanalyzer is related to the incident probe diameter, the spatial resolution for x-ray microanalysis is related to the convolution of the probe diameter with the spatial extent of the analyzed volume for a point probe. The latter is determined by electron scattering in the specimen and the subsequent emission of excited x-rays from the specimen. As such, it is possible that “What you see is not what you get”. This is especially true for instruments with high brightness electron sources (field emission). This problem is compounded by probe aberrations which at Gaussian image focus can produce significant electron tails extending tens of microns from the center of the probe.

Digital x-ray mapping of catalyst particles

1984 ◽  
Vol 42 ◽  
pp. 654-655
Author(s):  
C. E. Lyman
Keyword(s):  
Spatial Resolution ◽  
Energy Dispersive Spectrometer ◽  
Scanning Transmission Electron Microscope ◽  
Polished Section ◽  
Early Application ◽  
X Ray ◽  
Electron Probe Microanalyzer ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Early Maps

Formation of 2-dimensional dot maps of x-ray intensity from various elements in a flat polished section was an early application of the scanning beam electron probe microanalyzer. The spatial resolution of those early maps was the same as the microprobe itself, about lpm. These maps were usually scanned in an analogue fashion, and there was generally enough x-ray signal to produce maps with good peak-to-background ratios. For analysis of individual catalyst particles, a scanning transmission electron microscope (STEM) must be used to obtain the required spatial resolution. However, the x-ray signal level is usually low and is collected with an energy-dispersive spectrometer which has a lower peak-to-background ratio than the wavelength-dispersive spectrometer used in the microprobe. To produce suitable high magnification x-ray maps of catalyst particles digital beam techniques were employed.

Applications of high spatial resolution hicroanalysis to materials problems using dedicated STEM

1978 ◽  
Vol 36 (1) ◽  
pp. 418-419
Author(s):  
Ernest L. Hall ◽  
John B. Vander Sande
Keyword(s):  
Spatial Resolution ◽  
High Spatial Resolution ◽  
Profile Analysis ◽  
Scanning Transmission Electron Microscope ◽  
Dramatic Improvement ◽  
X Ray ◽  
Transmission Electron ◽  
Probe Size ◽  
Scanning Transmission ◽  
Compositional Variations

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.

scholarly journals Chemically Sensitive Tomography at 50 nm Spatial Resolution using a Soft X-ray Scanning Transmission X-Ray Microscope

2006 ◽  
Vol 12 (S02) ◽  
pp. 1412-1413 ◽  
Author(s):  
GA Johansson ◽  
JJ Dynes ◽  
AP Hitchcock ◽  
T Tyliszczak ◽  
GD Swerhone ◽  
...  
Keyword(s):  
Spatial Resolution ◽  
X Ray ◽  
Scanning Transmission

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

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.

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
Keyword(s):  
Spatial Resolution ◽  
High Spatial Resolution ◽  
X Ray ◽  
Scanning Transmission ◽  
Distribution Mapping ◽  
Similar Materials ◽  
Relationship Of ◽  
X Ray Absorption ◽  
Beam Damage

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.

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