Near total reflection X-ray photoelectron spectroscopy: Quantifying chemistry at solid/liquid and solid/solid interfaces

TL;DR

This paper demonstrates the use of near total reflection X-ray photoelectron spectroscopy to precisely analyze chemical concentration gradients and buried interfaces at solid/liquid and solid/solid boundaries with nanometer depth resolution.

Contribution

It introduces practical methods for ambient pressure X-ray photoelectron spectroscopy using near total reflection, enabling high-resolution interface analysis without complex sample preparation.

Findings

Depth accuracy of ~1 nm achieved

Effective analysis of buried interfaces and concentration profiles

Simplified sample preparation compared to multilayer mirror techniques

Abstract

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.