• Everett Rosa posted an update 2 months ago

    This study demonstrates a simple and multistep approach for a covalent functionalization of chemically-prepared graphene oxide (GO) using branched polyethylenimine (PEI) through nucleophilic addition reaction to prepare GO-PEI. Further layer-by-layer (LBL) assembly on functionalized GO-PEI with anionic polyelectrolyte, poly(acrylic acid sodium salt) (PAA) and poly(sodium 4-styrenesulfonate) (PSS) have been undertaken to fabricate polymer brushes (PB). The physicochemical structures of GO, GO-PEI and LBL assembled PB have been explored using standard spectral and morphological analysis. The macrotribological results demonstrated that GO-PEI-PAA/GO-PEI-PSS (0.5 wt%) as paraffin oil dispersible additives significantly decreased the coefficient of friction (COF) and wear at different contact pressures of steel-steel tribopairs. The influence of contact pressure and load-bearing ability of the polymer-grafted GO as nanolubricants have been examined carefully. The COF of PB particles provided a reduction of 85% (low pressure, ∼0.9 MPa) and 66.65% (high pressure, ∼1.35 GPa) compared to lube paraffin oil and exhibited a lower specific wear rate (2.26 × 10-8 mm3 N-1 m-1) at macrotribological pin/ball-on-disc trials, revealing superior lubricity. The PB containing nanolubricants also exhibited high load-bearing ability (till ∼1000 N load, Pm ∼6.1 GPa) with considerably lower COF and wear, which were investigated using a four-ball tribotester. Among the functionalized polymeric GO particles, PSS polyelectrolyte containing GO-PEI-PSS showed better COF and wear reduction ability with extremely high load-bearing capacity due to the strong interfacial adhesion properties of PSS to generate strong protective synergetic lubricating tribofilm into the rubbing interfaces, which is comprehensively investigated by post-tribological analysis.Granular hydrogels with high stability, strength, and toughness are laborious to develop. Post-curing is often employed to bind microgels chemically and enhance mechanical properties. Here a unique strategy was investigated to maintain microgels together with a novel self-reinforced silk granular hydrogel composed of 10 wt% 20 kDa poly(ethylene glycol) dimethacrylate microgels and regenerated silk fibroin fibers. The principle is to use the swelling of microgels to concentrate the surrounding solution and regenerate silk fibroin in situ. Self-reinforcement is subsequently one of the added functions. We showed that silk fibroin in most compositions was homogeneously distributed and had successfully regenerated in situ around microgels, holding them together in a network-like structure. FTIR analysis revealed the presence of amorphous and crystalline silk fibroin, where 50% of the secondary structures could be assigned to strong β-sheets. Swelling ratios, i.e. 10-45 vol%, increased proportionally with the microgel content, suggesting that mainly microgels governed swelling. In contrast, the elastic modulus, i.e. 58-296 kPa, increased almost linearly with silk fibroin content. Moreover, we showed that the precursor could be injected and cast into a given shape. Viscous precursors of various compositions were also placed side by side to create mechanical gradients. Finally, it was demonstrated that silk granular hydrogel could successfully be synthesized with other microgels like gelatin methacryloyl. Silk granular hydrogels represent, therefore, a novel class of self-reinforced hydrogel structures with tunable swelling and elastic properties.To explore whether chalcogen bonding was able to drive the formation of supramolecular helices, alanine-based azapeptides containing a β-turn structure, with a thiophene group, respectively, incorporated in the N- or C-terminus, were employed as helical building blocks. While the former derivative formed a supramolecular M-helix via intermolecular SS chalcogen bonding in crystals, the latter formed P-helix via intermolecular SO chalcogen bonding.We characterize temperature-dependent macroscopic and nanoscopic phase transitions and nanoscopic pre-transitions of water-soluble single chain nanoparticles (SCNPs). The studied SCNPs are based on polymers displaying lower-critical solution temperature (LCST) behavior and show nanoscale compartmentation. Calcium folinate chemical structure SCNPs are amenable to continuous wave electron paramagnetic resonance (CW EPR) spectroscopy to study how amphiphilic, non-covalently added nitroxide spin probes or covalently attached spin labels sample their environment concerning nanoscale structures (polarity, hydrophilicity/-phobicity) and dynamics. These SCNPs are formed through single-chain collapse and have been shown to have nanosized compartments that are rigidified during the crosslinking process. We analyze the temperature-dependent phase transitions of spin-labeled SCNPs by rigorous spectral simulations of a series of multicomponent EPR-spectra that derive from the nanoinhomogeneities (1) that are due to the single-chain compartmentation in SCNPs and (2) the transformation upon temperature change due to the LCST behavior. These transitions of the SCNPs and their respective polymer precursors can be monitored and understood on the nanoscale by following EPR-spectroscopic parameters like hyperfine couplings that depend on the surrounding solvent molecules or Heisenberg spin exchange between small molecule spin probes or covalently attached spin labels in the nanocompartments. In particular, for one SCNP, we find an interesting behavior that we ascribe to the properties of the nanosized inner core with continuous effects before and jump-like changes after the macroscopic thermal collapse, indicating highly efficient desolvation and compaction upon an increase in temperature and aggregation of individual nanoparticles above the collapse temperature.The homeostasis and imbalance of glutathione (GSH), an important antioxidant in organisms, are one of the key signals that reflect the health of organisms. In this paper, a novel SERS sensing platform based on Ag film@Si that self-assembled using silver nanospheres was proposed, which was used for the highly sensitive and selective detection of GSH. With the aid of an oil/water/oil three-phase system, the nano-silver film was self-assembled and finally deposited on silicon wafers. The heterobifunctional crosslinking agent N-succinimidyl-3-(2-pyridyldithio)propionate (SPDP), which contains pyridine rings and disulfide bonds, was involved in the exchange reaction between the sulfhydryl groups and disulfide bonds. With the addition of GSH, the breakage of disulfide bonds was promoted, thereby enhancing the SERS signal of SPDP. GSH can be detected sensitively by detecting the changes in the SPDP signal. The detection limit of GSH is 10 nM, and the method is still highly stable when the external environment is serum or other more complex environments.

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