Cu K-edge XANES: polymer, organic, inorganic spectra, and experimental considerations

Abstract

In pursuit of design and characterization of Cu adsorbing in thin films, we present data from a large variety of Cu-K edge X-ray Absorption Near Edge Spectroscopy spectra obtained from organic and inorganic standards. Additionally, we have explored the impact of beam damage inducing redox alterations. Polymer nanoparticles were tested against films to produce higher concentration samples while maintaining high surface area to bulk effects. Spectra from nanoparticles were highly comparable to thin films of ~8 nm thickness, implying comparable contributions by surface effects on copper association. Finally, we observed no impact on Cu XANES spectra from vitrification with DMSO to produce amorphous frozen, hydrated samples. The spectra should act as a valuable resource in assisting the design of experiments and identification of copper associations.

Spatio‐Chemical Heterogeneity of Defect‐Engineered Metal–Organic Framework Crystals Revealed by Full‐Field Tomographic X‐ray Absorption Spectroscopy

“…The spectra exhibits al ower edge energy than the MOF and features aless intense white line at 8997 eV with ashoulder at 8991 eV and an additional feature at 8996 eV.T he closest comparable spectra considered, is that of am etal-aquo complex [Cu(H 2 O) 6 ] 2+ . [41] We henceforth assigned this minor phase to be inorganic copper, and given its preferential location, possibly as ynthesis or surface recrystallization remnant. Thet hird component, the mid-density phase dispersed in clusters throughout the crystal and surround by the HKUST-1 lattice,i sb yp rocess of elimination the secondary and nanocrystalline/amorphous coordination polymer detected by PXRD (Figure 1d).…”

Interpreting the Operando XANES of Surface-Supported Subnanometer Clusters: When Fluxionality, Oxidation State, and Size Effect Fight

“…2 XANES has been used to extract relevant information such as oxidation state and geometry of inorganic metal complexes as well as metal and metal oxide surfaces. [4][5][6][7][8] XANES is sensitive to geometry and to the oxidation state of the metal center, which makes it an important tool to distinguish between different structures. [9][10][11][12] The pre-edge region can be used to estimate the ligand field, spin state, and centrosymmetry of the site.…”

Spatio‐Chemical Heterogeneity of Defect‐Engineered Metal–Organic Framework Crystals Revealed by Full‐Field Tomographic X‐ray Absorption Spectroscopy

“…The spectra exhibits al ower edge energy than the MOF and features aless intense white line at 8997 eV with ashoulder at 8991 eV and an additional feature at 8996 eV.T he closest comparable spectra considered, is that of am etal-aquo complex [Cu(H 2 O) 6 ] 2+ . [41] We henceforth assigned this minor phase to be inorganic copper, and given its preferential location, possibly as ynthesis or surface recrystallization remnant.…”