Intercalation and grafting of benzene derivatives into zinc–aluminum and copper–chromium layered double hydroxide hosts: an XPS monitoring study

Abstract

We report an original strategy to describe, via X-ray photoelectron spectroscopy (XPS) measurements, the interactions between the organic and the mineral sub-systems within a multifunctional hybrid material. A tunable layered double hydroxide (LDH) host system, either a Zn(2)Al- or Cu(2)Cr-hydrotalcite like compound, is modified with the insertion of the organic guest entities, 4-phenol-sulfonate (HBS) or -carboxylate (HBC). The resulting interactions are studied at two levels: after the organic molecules' insertion in the host LDH (ionic exchange between the LDH counter-ions and the organic anions) and after the condensation (grafting) of the organic species onto the mineral layers when thermally treated. For the inserted material, the main XPS results show a stabilization of the organic molecules within the mineral sheets via H bonding as found elsewhere with FTIR study, the mineral matrix being unchanged. The XPS signal of the organic molecules slightly changes with a widening of core peaks, attesting to some local surrounding modifications. When heating up the Zn(2)Al hybrid material, stronger interactions between organic and inorganic systems appeared from around 80 °C with some obvious electronic changes as monitored with the XPS S2p signal of the HBS guest molecules. At the same time, the PXRD pattern clearly shows a decrease of the basal spacing according to a two step contraction process which could be interpreted as a progressive organic molecule condensation onto the inorganic layers via iono-covalent bonds. A copper-chromium LDH is also studied to probe the same kind of interactions with the HBS molecules. The ability of distortion of such mineral material involves a peculiar process of contraction from 40 °C with the immediate and effective anchorage of organic molecules.

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“…The C 1 s spectrum (Figure S5a in the Supporting Information) shows three peaks at 284.6, 286.6, and 288.1 eV, which are attributed to CC, CO, and CN/CO, respectively 19. The N 1 s spectrum (Figure S5b in the Supporting Information) shows two peaks at 397.5 and 399.5 eV, which can be attributed to NC, and NH, respectively 20. The O 1 s spectrum (Figure S5c in the Supporting Information) exhibits two peaks at 531.7 and 533.0 eV, which are assignable to CO and COH/C‐O‐C groups, respectively 21.…”

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“…The organic molecules should then have a direct impact in the final metal cation's composition of the host layers. 33 The O1s peak of the ZnAl-LDH film with NO 3 À is divided into three peaks, with binding energies of 532.3, 531.6, and 531.0 eV (Fig. 5c).…”

One-step, green, and economic synthesis of water-soluble photoluminescent carbon dots by hydrothermal treatment of wheat straw, and their bio-applications in labeling, imaging, and sensing

“…The C 1s spectrum ( Figure 4B) shows three peaks at 284.9, 286.0, and 288.9 eV, which are attributed to C-C, C-N, and C = N/C = O, respectively [36] . The N 1s spectrum ( Figure 4C) shows single peaks at 399.5 eV, which is attributed to the C-N-C band [37] . The O 1s spectrum ( Figure 4D) exhibits two peaks at 532.5 and 533.5 eV, which are attributed to C = O and C-OH/C-O-C groups, respectively [38] .…”