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Register a new userUsing near-total-reflection hard X-ray photoelectron spectroscopy for high-resolution depth profiling
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By adjusting the incidence angle of incoming X-ray near the critical angle of X-ray total reflection, the photoelectron intensity is strongly modulated due to the variation of X-ray penetration depth. Photoemission spectroscopy (PES) combining with near total reflection (NTR) exhibit tunable surface sensitivity, providing depth-resolved information. In this work, the technique and some recent experimental works using NTR-PES are reviewed. The emphasis is on its applications to correlated oxide heterostructures, especially quantitative depth analyses of compositions and electronic states.
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We report the development of a laboratory-based Rowland-circle monochromator that incorporates a low poer x-ray (bremsstrahlung) tube source, a spherically-bent crystal analyzer (SBCA), and an energy-resolving solid-state detector. This relatively inexpensive, introductory level instrument achieves 1-eV energy resolution for photon energies of 5 keV to 10 keV while also dmeonstrating a net efficiency previously seen only in laboratory monochromators having much coarser energy resolution. Despite the use of only a compact, air-cooled 10 W x-ray tube, we find count rates for nonresonant x-ray emission spectroscopy (XES) comparable to those achived at monochromatized spectroscopy beamlines at synchrotron light sources. For x-ray absorption near edge structure (XANES), the monochromatized flux is small (due to the use of a low-powered x-ray generator) but still useful for routine transmission-mode studies of concentrated samples. These results indicate that upgrading to a standard commercial high-powered line-focused x-ray tube or rotating anode x-ray generator would result in monochromatized fluxes of order 10^6 to 10^7 photons/s with no loss in energy resolution. This work establishes core technical capabilities for a rejuvenation of laboratory-based x-ray spectroscopies that could have special relevance for contemporary research on catalytic or electrical energy storage systems using transition-metal, lanthanide, or noble-metal active species.
Near total reflection regime has been widely used in X-ray science, specifically in grazing incidence small angle X-ray scattering and in hard X-ray photoelectron spectroscopy. In this work, we introduce some practical aspects of using near total reflection in ambient pressure X-ray photoelectron spectroscopy and apply this technique to study chemical concentration gradients in a substrate/photoresist system. Experimental data are accompanied by X-ray optical and photoemission simulations to quantitatively probe the photoresist and the interface with the depth accuracy of ~1 nm. Together, our calculations and experiments confirm that near total reflection X-ray photoelectron spectroscopy is a suitable method to extract information from buried interfaces with highest depth-resolution, which can help address open research questions regarding our understanding of concentration profiles, electrical gradients, and charge transfer phenomena at such interfaces. The presented methodology is especially attractive for solid/liquid interface studies, since it provides all the strengths of a Bragg-reflection standing-wave spectroscopy without the need of an artificial multilayer mirror serving as a standing wave generator, thus dramatically simplifying the sample synthesis.
The conducting interface of LaAlO$_3$/SrTiO$_3$ heterostructures has been studied by hard X-ray photoelectron spectroscopy. From the Ti~2$p$ signal and its angle-dependence we derive that the thickness of the electron gas is much smaller than the probing depth of 4 nm and that the carrier densities vary with increasing number of LaAlO$_3$ overlayers. Our results point to an electronic reconstruction in the LaAlO$_3$ overlayer as the driving mechanism for the conducting interface and corroborate the recent interpretation of the superconducting ground state as being of the Berezinskii-Kosterlitz-Thouless type.
This work reports the measurement of magnetic dichroism in angular-resolved photoemission from in-plane magnetized buried thin films. The high bulk sensitivity of hard X-ray photoelectron spectroscopy (HAXPES) in combination with circularly polarized radiation enables the investigation of the magnetic properties of buried layers. HAXPES experiments with an excitation energy of 8 keV were performed on exchange-biased magnetic layers covered by thin oxide films. Two types of structures were investigated with the IrMn exchange-biasing layer either above or below the ferromagnetic layer: one with a CoFe layer on top and another with a Co$_2$FeAl layer buried beneath the IrMn layer. A pronounced magnetic dichroism is found in the Co and Fe $2p$ states of both materials. The localization of the magnetic moments at the Fe site conditioning the peculiar characteristics of the Co$_2$FeAl Heusler compound, predicted to be a half-metallic ferromagnet, is revealed from the magnetic dichroism detected in the Fe $2p$ states.
Magnetite (Fe3O4) thin films on GaAs have been studied with HArd X-ray PhotoElectron Spectroscopy (HAXPES) and low-energy electron diffraction. Films prepared under different growth conditions are compared with respect to stoichiometry, oxidation, and chemical nature. Employing the considerably enhanced probing depth of HAXPES as compared to conventional x-ray photoelectron spectroscopy (XPS) allows us to investigate the chemical state of the film-substrate interfaces. The degree of oxidation and intermixing at the interface are dependent on the applied growth conditions; in particular, we found that metallic Fe, As2O3, and Ga2O3 exist at the interface. These interface phases might be detrimental for spin injection from magnetite into GaAs.
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