Operando Xps

Operando X-ray photoelectron spectroscopy (operando XPS) is a surface-analysis technique that measures elemental composition and chemical states while a material performs its function under realistic operating conditions. It irradiates the sample with X-rays and analyzes the kinetic energies of emitted photoelectrons, while controlled gases, liquids, temperature, or applied potentials reproduce the working environment. Time-resolved spectra can track oxidation-state changes, adsorbed intermediates, and surface reconstruction during catalysis, electrocatalysis, and battery operation. By linking surface chemistry to performance, operando XPS helps identify active sites, reaction pathways, degradation processes, and design principles for improved materials.

Operando Xps - Related Videos

Research

JoVE Journal - Chemistry
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Determining the Chemical Composition of Corrosion Inhibitor/Metal Interfaces with XPS: Minimizing Post Immersion Oxidation

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Cited by 20 •

2017

A protocol to avoid the oxidation of metallic substrates during sample transfer from an inhibited acidic solution to an X-ray photoelectron spectrometer is presented.

Research

JoVE Journal - Chemistry
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Preparation of Nanoparticles for ToF-SIMS and XPS Analysis

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Cited by 14 •

2020

A number of different procedures for preparing nanoparticles for surface analysis are presented (drop casting, spin coating, deposition from powders, and cryofixation). We discuss the challenges, opportunities, and possible applications of each method, particularly regarding the changes in the surface properties caused by the different preparation methods.

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JoVE Journal - Engineering
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Coin Cell Battery Chamber Design for Low-temperature Operando Experiments

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Cited by 1 •

2026

A design is presented to enable cost-effective low-temperature battery cycling for 2032 coin cells in a low-humidity environment. Cells are cycled at 0 °C inside a chamber cooled by thermoelectric modules. This simple design can be adapted for experiments that require similar thermal and humidity-controlled environments or different battery geometries.

Research

JoVE Journal - Chemistry
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Fluid-cell Raman Spectroscopy for operando Studies of Reaction and Transport Phenomena during Silicate Glass Corrosion

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Cited by 1 •

2025

Fluid-cell Raman Spectroscopy (FCRS) enables in operando observations of reaction and transport phenomena during the aqueous corrosion of silicate glasses at a microscopic level, at elevated temperatures, and in real-time. Without interrupting ongoing processes, FCRS provides information about reaction mechanisms, kinetics, and transport processes.

Research

JoVE Journal - Chemistry

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

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Cited by 2 •

2018

The incorporation of reference electrodes in a Li-ion battery provides valuable information to elucidate degradation mechanisms at high voltages. In this article, we present a cell design that accommodates multiple reference electrodes, along with the assembly steps to assure maximum accuracy of the data obtained in electrochemical measurements.

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