HIPPIE: a new platform for ambient-pressure X-ray photoelectron spectroscopy at the MAX IV Laboratory

Abstract

HIPPIE is a soft X-ray beamline on the 3 GeV electron storage ring of the MAX IV Laboratory, equipped with a novel ambient-pressure X-ray photoelectron spectroscopy (APXPS) instrument. The endstation is dedicated to performing in situ and operando X-ray photoelectron spectroscopy experiments in the presence of a controlled gaseous atmosphere at pressures up to 30 mbar [1 mbar = 100 Pa] as well as under ultra-high-vacuum conditions. The photon energy range is 250 to 2200 eV in planar polarization and with photon fluxes >1012 photons s−1 (500 mA ring current) at a resolving power of greater than 10000 and up to a maximum of 32000. The endstation currently provides two sample environments: a catalysis cell and an electrochemical/liquid cell. The former allows APXPS measurements of solid samples in the presence of a gaseous atmosphere (with a mixture of up to eight gases and a vapour of a liquid) and simultaneous analysis of the inlet/outlet gas composition by online mass spectrometry. The latter is a more versatile setup primarily designed for APXPS at the solid–liquid (dip-and-pull setup) or liquid–gas (liquid microjet) interfaces under full electrochemical control, and it can also be used as an open port for ad hoc-designed non-standard APXPS experiments with different sample environments. The catalysis cell can be further equipped with an IR reflection–absorption spectrometer, allowing for simultaneous APXPS and IR spectroscopy of the samples. The endstation is set up to easily accommodate further sample environments.

Stroboscopic operando spectroscopy of the dynamics in heterogeneous catalysis by event-averaging

“…Event-averaging by image recognition: 3.2 mbar CO oxidation. In the first set of experiments performed at the HIPPIE beamline 22 at the MAX IV Laboratory we exposed a Pd(100) surface, located in a cell volume of ∼ 1 l to 58 alternating pulses of CO-rich and O 2 -rich gas mixtures with CO:O 2 mixing ratios of 2.7:1 and 1:2.7, respectively. The total pressure and total flow were kept constant at 3.2 mbar and 9.6 sccm, respectively, while the sample temperature only was semi-constant at 550 ± 10 K, due to the exothermic heat and the reaction that turned on and off.…”

“…1, in Supplementary Figs. 4-7 and Supplementary Movies 1, 2, 4, 5, and 6 were all collected at the HIPPIE APXPS beamline during one single beamtime 22 . For these measurements, the Pd(100) single crystal was mounted on a transferrable 304 L stainless steel sample plate.…”

Probing Electrochemical Potential Differences over the Solid/Liquid Interface in Li-Ion Battery Model Systems

“…APPES measurements were performed at the HIPPIE beamline at the MAX IV synchrotron facility, Lund, Sweden. 28 All measurements were performed at a set photon energy of 1800 eV. The beam size was approximately 25 × 50 μm (vertical × horizontal), with an incident angle of 55°, with respect to the sample normal.…”

NanoMAX: the hard X-ray nanoprobe beamline at the MAX IV Laboratory

“…The realized beamline is the result of a number of design criteria established early in the project phase, through input from various stakeholders as well as through practical constraints as follows: the beamline was built simultaneously with six other beamlines (Klementiev et al, 2016;Enquist et al, 2018;Ursby et al, 2020;Zhu et al, 2021) and the two storage rings, meaning technical design resources were limited and commercial vendors preferred. The optics scheme should only be horizontally deflecting, beneficial for beam stability and have few optical elements to preserve the brilliance.…”

“…The realized beamline is the result of a number of design criteria established early in the project phase, through input from various stakeholders as well as through practical constraints as follows: the beamline was built simultaneously with six other beamlines (Klementiev et al, 2016;Enquist et al, 2018;Ursby et al, 2020;Zhu et al, 2021) energy range should span a large range to allow excitation of elements, for example, used in nano-technology or found in environmental science. The diverse experimental demands warranted two endstations, where the KB-focusing enables a large energy range and free working distance, while the Fresnel zone plates can provide higher resolution, but over a more limited photon energy range and with limited space around the sample.…”