ISM2019 (Microscopy)

BRINGING SYNCHROTRON BEAMLINE X-RAY MICROANALYSIS (µXRF, XAS AND NANO-XRM) TECHNIQUES TO THE LABORATORY


Synchrotron beamline X-ray techniques have several inherent advantages over their laboratory equivalent in terms of their massive increase in flux, energy coherence, tuneability and sub-micron resolution capabilities. Synchrotron x-ray microanalysis techniques such as microXRF (microXRF), XAS (X-ray absorption Spectroscopy/ XANES & EXAFS) and nano XRM ( X-ray Microscopy) are becoming increasingly central to advanced research in alternative energy, catalysts, medicine, semiconductor materials to geology. This has led to oversubscription and immense competition in acquiring beamtime. In spite of the growth of these techniques at synchrotron facilities, efforts toward developing higher sensitivity and smaller X-ray spot size laboratory X-ray capabilities have progressed relatively slowly. This is due, in part, to bottlenecks in regards to both X-ray optics and low brightness laboratory X-ray sources. Conventional X-ray source designs rely on target materials deposited on a metal substrate, and are fundamentally limited in flux by the power loadings afforded by the metals.

We have developed a breakthrough patented laboratory microfocus X-ray source with user selectable or tunable energy which has significantly higher brightness/flux than conventional micro focus &/or rotating anode sources. Coupling this source with our novel double-paraboloidal X-ray mirror lenses, we envision developing a suite of laboratory X-ray instrumentation with performances close to their synchrotron equivalent. In this paper we are pleased to announce three of these integrated products, namely, micro X-ray fluorescence (microXRF), X-ray absorption spectroscopy (XAS), and nano X-ray microscopy (nano-XRM) instrumentation.


Rapid non destructive trace level elemental compositional mapping at ambient by the Attomaptm (µXRF) will be illustrated with biological tissue, nanoparticles in drug delivery, geology and material science. The metrology of thin film thickness and dopants from atomic layer deposition (ALD) at sub A thickness sensitivity in semiconductor wafers will also be shown. The detection sensitivity of the Attomaptm is the the sub ppm level which is comparable to TOF-SIMS.

The Lab Quantum Leaptm XAS system has sub-eV energy resolution for chemical state analysis (for valence or oxidization states using XANES) and bond length or neighboring atoms analysis with EXAFS techniques. Scan times are in minutes to hours. This technique is crucial for our understanding of charge-discharge cycle of batteries; the aging of catalysts and processes in a variety of novel advanced materials. Results obtained are comparable to synchrotron XAS. The Trilambdatm nano-XRM is a tomography system for 3D volumetric representations of material microstructures with spatial resolutions down to 40 nm with a choice of three X-ray energies to analyze soft to hard materials.

All these novel X-ray techniques are complementary. They form part of the essential components in the emerging field of correlative and functional microscopy, tying structural information from optical and electron microscopy with elemental, chemical states and 3D volumetric data in applied research.