Design of a Cryogenic Air-Free Sample Transfer System to Enable Volatile Materials Analysis with X-ray Photoelectron Spectroscopy

Abstract

Without an expensive near-ambient pressure XPS instrument, it is a great challenge to realize surface analysis of volatile samples using a traditional X-ray photoelectron spectrometer, especially for liquid samples. By developing the cryogenic air-free XPS sample transfer device with a liquid nitrogen freezing unit and gas exhausting/filling sealing unit, we have achieved the sample freezing under the protection of an ambient inert atmosphere in the ultrahigh vacuum (UHV) environment of the preparation chamber and the following quasi-in situ sample transfer for frozen samples into an X-ray photoelectron spectrometer. This work shows that the cryogenic air-free sample transfer system developed by us is effective for XPS measurement of volatile solid samples and even liquid-phase materials, as demonstrated by the XPS data of the following samples. For a volatile organic small molecule composite (1,3,5-trifluoro-2,4,6-triiodobenzene@2-(2-hydroxybenzylamino)-5-methoxypyridine), the XPS data consistent with its molecular structure were effectively obtained. For air-sensitive liquid-phase polysulfide (Li2S6), the Li 1s line at 55.89 eV from Li+ and S 2p peaks from the terminal S2– (at 162.21 eV) and the bridging Sn (at 163.82 eV) were clearly observed, indicating that the accurate chemical composition and structure of volatile samples can be analyzed by using our system.

Improving Hybrid Tin Halide Films by Tin Trifluoromethanesulfonate for Lead-Free Perovskite Solar Cells

“…The Sn-PVK film with Sn(OTF) 2 additives has a clear peak at 163.8 eV, indicating the existence of Sn(OTF) 2 on the surface of Sn-PVK films. 41 The XPS spectra of F elements are also analyzed in Figure 1g for the Sn-PVK films without and with different additives. The peak at 688.6 eV is obtained for the Sn-PVK film with Sn(OTF) 2 additives, while no XPS signal of F elements can be observed for the Sn-PVK film with SnF 2 additives.…”

“…Figure f shows the XPS spectra of the 2p states for S elements. The Sn-PVK film with Sn­(OTF) 2 additives has a clear peak at 163.8 eV, indicating the existence of Sn­(OTF) 2 on the surface of Sn-PVK films . The XPS spectra of F elements are also analyzed in Figure g for the Sn-PVK films without and with different additives.…”

Ionic Covalent Organosilicon Polymer Nanosheet for Selective and Sensitive Detection of Dopamine

“…The XPS spectra of HHTP-Si ICOP (Figure S7) agreed well with the ones observed for its corresponding model compound (Figure S8). Their energy survey spectra both showed the only existence of C, O, Si and minimal N. The low content of N could be ascribed to the instability of the counterion “NHEt 3 + ” which decomposed to NEt 3 gas in the ultrahigh vacuum chamber of the XPS instrument. , The high-resolution XPS scan of C (Figure S7b) and O (Figure S7c) showed deconvoluted Gauss peaks at 285.4 eV (referred as C -O), and 532.8 eV (referred as C- O ), which unitedly indicated the presence of only catecholate state in this hydroxyl linker-based polymer, suggesting the wide existence of SiPhO 4 units in HHTP-Si ICOP. As shown in Figure d, the binding energy at 102.5 eV (Si 2p) could be ascribed to the Si-PhO 4 unit, further indicating that the Si element only existed in pentacoordination state.…”

Recent Methods & Protocols from Chemistry of Materials: Promoting High-Quality Research and Transparency

“…Methods & Protocols are important manuscript types for Chemistry of Materials and the broader materials chemistry community as they outline best practices in the field, can define the frontiers of research through new methods for understanding materials, and promote open science with accessible guidance for those entering fields. Tables – summarize recent Methods & Protocols published in the journal according to theme. − Table provides reports on structural characterization methods by X-ray, neutron, and electron scattering/diffraction, which can be critical to achieving structure–property correlations of materials. − Table provides reports on property characterization or tools that enable property measurements, including best practices for magnetic measurements and Mössbauer spectroscopy and several methods specific to metal organic frameworks (MOFs). − Table reports methods for device fabrication as well as property measurements of materials for specific applications, e.g., batteries. − Table gives “how to” guides for material syntheses and fabrication, − but the table also includes papers on the application of X-ray techniques to identify reaction intermediates and advance mechanistic insights into material syntheses. , Table outlines computational and data science approaches for materials, including tutorial-style insights to demystify such approaches for experimentalists. − …”