X-ray powder diffraction (XRD), thermal gravimetric analysis (TGA), surface area measurements, and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy were used to examine the surface properties of organosilane-modified smectite-type aluminosilicate clays. Organic modified clays derived from the reactions of montmorillonite (containing 93–95% montmorillonite from a bentonite, <1% quartz, and 4–6% opal CT) with octadecyltrichlorosilane (C18H37SiCl3) and octadecyltrimethoxysilane [C18H37Si(OMe)3] are highly hydrophobic. Surface loadings of the modified clays depend on the organosilane and the solvent, and they range from 10 to 25 wt. %. The organic species are probably adsorbed to the outer surfaces and bound to the edges of the clay via condensation with edge-OH groups. Encapsulation of montmorillonite with C18H37SiCl3 and C18H37Si(OMe)3 resulted in a hydrophobic coating that acts like a “cage” around the clay particles to limit diffusion. Basal spacings of the organic modified clays remain at ∼15 Å upon heating to 400°C in N2, whereas those of unmodified clays collapse to ∼10 Å. A considerable reduction in surface area (by 75–90%) for organic modified clays is observed, which is consistent with the existence of a surface coating. The solvent used can affect the amount of organic silane coated on the clay particles, whereas the difference between the products prepared using C18H37SiCl3 and C18H37Si(OMe)3 in the same solvent is relatively small. The carbon and oxygen K-edge NEXAFS spectroscopy of the modified montmorillonite surfaces showed that surface coatings on the outside of the clay particles exist. The encapsulating system may allow for economical remediation and storage of hazardous materials.

Experimental data on structure formation in highly concentrated aqueous dispersions of kaolinite were analyzed using rheological models. The physicochemical properties of the clay mineral surface were studied during heating at a range of temperatures, and correlation of acid-base properties with physicomechanical characteristics of the spatial structures formed during heating was obtained. It was shown that interparticle interactions and plastic yield mechanisms under load are dependent upon interfacial phenomena. A method for estimating optimal structural parameters was developed for semidry dispersions, enabling regulation of physicochemical and mechanical properties of ceramic mixtures during processing.

The electrochemical properties of kaolinite before and after modification with chlorodimethyl-octadecylsilane have been studied by electrophoretic mobility, surface charge titration, and extrapolated yield stress measurements as a function of pH and ionic strength. A heteropolar model of kaolinite, which views the particles as having a pH-independent permanent negative charge on the basal planes and a pH-dependent charge on the edges, has been used to model the data. The zeta potential and surface charge titration experimental data have been used simultaneously to calculate acid and ion complexation equilibrium constants using a surface complex model of the oxide-solution interface. The experimental data were modeled following subtraction of the basal plane constant negative charge, describing only the edge electrical double layer properties. Extrapolated yield stress measurements along with the electrochemical data were used to determine the edge isoelectric points for both the unmodified and modified kaolinite and were found to occur at pH values of 5.25 and 6.75, respectively. Acidity and ion complexation constants were calculated for both sets of data before and after surface modification. The acidity constants, pKa1 = 5.0 and pKa2 = 6.0, calculated for unmodified kaolinite, correlate closely with acidity constants determined by oxide studies for acidic sites on alumina and silica, respectively, and were, therefore, assigned to pH-dependent specific chemical surface hydroxyl groups on the edges of kaolinite. The parameters calculated for the modified kaolinite indicate that the silane has reacted with these pH-dependent hydroxyl groups causing both a change in their acidity and a concomitant decrease in their ionization capacity. Infrared data show that the long chain hydrocarbon silane is held by strong bonding to the kaolinite surface as it remains attached after washing with cyclohexane, heating, and dispersion in an aqueous environment.

Halloysite nanotubes (HNTs) have attracted much attention as delivery carriers for various drugs, but the loading of one such drug, quercetin, on HNTs has been investigated only rarely and usually involved cyclic vacuum pumping. The main objective of the present study was to develop a novel carrier system based on HNTs for quercetin delivery without a vacuum process and to investigate the effect of chemical modification of HNTs on the loading and release of quercetin. For this purpose, comparative studies of five chemical modification reagents (sodium lauroamphoacetate, cocoamidopropyl betaine, 1-hydroxyethyl 2-nonyl imidazoline betaine, triethanolamine, and dipicolinic acid) functionalized on HNTs were investigated for quercetin loading and in vitro release. Characterization of raw halloysite, modified halloysite, and quercetin-loaded halloysite were done by X-ray diffraction (XRD), Fourier-transform infrared spectrometry (FTIR), thermogravimetric analysis (TGA), and transmission electron microscopy (TEM). The results indicated that chemical modification could improve the interactions between HNTs and quercetin. After chemical modification, quercetin was anchored to both the inner and outer surfaces of HNTs by electrostatic attraction, hydrogen bonding, and van der Waals forces. Sodium lauroamphoacetate-modified HNTs were given the highest loading of 1.96 wt.% among the five reagents. Cocamidopropyl betaine-modified HNTs exhibited the best sustained-release profile with only 29.07% for initial burst release and 480 h of consecutive release. Carboxyl groups of the modification reagent improved the loading capacity of quercetin. Amide groups prolonged drug release due to the strong affinity between amine and phenolic hydroxyl groups of quercetin. The release of quercetin from the cocamidopropyl betaine-modified HNTs fitted a first-order kinetics model well. The present study suggested that cocamidopropyl betaine-modified HNTs offer promise as vehicles for delivery of quercetin and for extending the application of quercetin.

Lubricants are an essential component in high-performance mechanical equipment, but traditional lubricants are becoming inadequate for meeting the increasing demands for anti-friction and anti-wear properties and they discharge harmful chemicals to the environment. The purpose of the present study was to explore the use of sepiolite as a novel oil additive to extend the performance of lubricants. Sepiolite nanofibers were first treated by acid followed by a dry air flow, aimed at increasing the pore volume and decreasing the particle size. Then the nanofibers were further modified by an organosilane coupling agent to reduce the surface free energy and to improve the dispersion stability in lubricant. A significant improvement in the performance of the lubricant was achieved by using the modified sepiolite nanofibers as an additive. When the amount of modified sepiolite nanofibers added was 1.5 wt.%, the best performance was demonstrated by the lubricant, showing a viscosity increase at 40°C and 100°C, and an increase in resistance to oxidation. Moreover, the acid value and pour point decreased, and the copper sheet corrosion level dropped to its lowest value.

Modified sericite mica was prepared by combining the intercalation of cetyltrimethylammonium bromide (CTAB) through ion exchange and surface modification of 3-aminopropyltriethoxysilane (KH550) with the following steps: high-temperature activation of sericite mica, acid activation, sodium modification, LiNO3 treatment, the ion-exchange intercalation of the cetyltrimethylammonium cation (CTA+) and surface modification of KH550. High-temperature activation was the most critical step for the modified sericite mica, and the number of hydroxyl groups of mica under high temperature directly affected the surface modification of KH550. The effects of various activation temperatures on the surface modification of sericite mica were investigated. The structure of activated sericite mica was intact when activation temperature was 600°C or 700°C, and the surface modification of sericite mica was not affected. The structure of activated sericite mica was partially destroyed at 800°C. The optimal temperature for activating sericite mica was 700°C. The structure and morphology of modified sericite mica were characterized by Fourier-transform infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, Brunauer–Emmett–Teller (BET) analysis and loose bulk volume. The KH550 could not only chemically graft onto the surface of sericite mica, but also enter into the interlayer through electrostatic attraction after its end amino group was protonated. The interlayer spacing of modified sericite mica increased to 3.22 nm, indicating that it might be an excellent layered silicate for preparing clay–polymer nanocomposites.

In this study, we report a simple one-pot synthesis of iron oxide nanoparticles (IONPs) modified with thermoresponsive polymers potentially applicable for nucleic acid capture. Ferrous (Fe2+) and ferric (Fe3+) ions were coprecipitated to a dispersion of previously prepared poly(N-isopropylacrylamide-co-2-aminoethyl methacrylate) P(NIPAAm-co-AEM) for in situ synthesis of magnetite (Fe3O4) and concurrent surface modification of Fe3O4 with the polymer to obtain magnetic nanocomposites. Fourier-transform infrared (FTIR) spectroscopy analysis reveals the surface modification of Fe3O4 with P(NIPAAm-co-AEM) and P(NIPAAm) as functional and control polymers, respectively. Fe3O4@P(NIPAAm-co-AEM) and Fe3O4@P(NIPAAm) nanocomposites’ surfaces contain 7.5 and 2.3 wt% of immobilized polymers, respectively. Vibrating sample magnetometry (VSM) result indicates a high saturation of magnetization value, 75 emu/g, for Fe3O4@P(NIPAAm-co-AEM) nanocomposites. The hydrodynamic diameter of Fe3O4@P(NIPAAm-co-AEM) in water changes depending on pH and temperature. A study for deoxyribonucleic acid (DNA) capture ability of Fe3O4@P(NIPAAm-co-AEM) nanocomposites shows a maximum 18.5 mg/g of DNA can be adsorbed on Fe3O4@P(NIPAAm-co-AEM).

Some interesting properties such as superelasticity, shape memory effect, kink resistance, good biocompatibility, biomechanical properties, and corrosion resistance made nitinol a popular biomaterial as stent and orthopedic implants. But surface modification is needed to control nickel leaching from its surface, making safe for human body. The aim of this study was to modify the nitinol surface by the silanization technique and electrophoretically deposited hydroxyapatite coating, and to conduct a detailed in vitro and in vivo investigation. Detailed in vitro investigation involved MTT assay with the human osteoblastic cells (MG63 cell) over a period of 5 days and confocal image study. In case of in vivo study, histological study, fluorochrome labeling study, and Micro-Ct study were conducted. The overall in vitro and in vivo results indicate that silanized nitinol samples are showing slightly better level of performance, but both the surface-modified samples are suitable as the potential bio-implant for orthopedic purpose.

Fluorescent quantum dots (QDs) modified with polyethylene glycol (PEG) and albumin bovine serum (BSA) have profound application in the detection and treatment of hepatocellular carcinoma (HCC) cells. In the present study, the effects and mechanism of PEG and BSA modification on the cytotoxicity of QDs have been explored. It was found that the diameter of the as-prepared QDs, PEG@QDs, BSA@QDs is 3–5 nm, 4–5 nm, and 4–6 nm, respectively. With increase of the treatment time from 0 to 24 h, the HCC cell viability treated with QDs, PEG@QDs, and BSA@QDs obviously decreases, showing a certain time-dependent manner. When the concentration of several nanomaterials is increased from 10 to 90 nM, the cell viability decreases accordingly, exhibiting a certain concentration-dependent manner. Under the same concentration change conditions, the reactive oxygen species contents of cells treated by QDs, PEG@QDs, and BSA@QDs also rise from 7.9 × 103, 6.7 × 103, and 4.7 × 103 to 13.2 × 103, 14.3 × 103, and 12.3 × 103, respectively. In these processes, superoxide dismutase does not play a major role. This study provides strong foundation and useful guidance for QD applications in the diagnosis and treatment of HCC.

In order to improve the dispersibility of halloysite nanotubes (HNTs) in polytetrafluoroethylene (PTFE), the modification of HNT surfaces was studied with three types of modifiers (polymethyl methacrylate [PMMA], sodium dodecyl sulfate [SDS] and carboxylic acid). The modified HNTs were characterized by Fourier-transform infrared (FTIR) spectrometry, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and contact angle measurements. The HNTs were used to reinforce the mechanical properties of PTFE. The mechanical results indicated that the tensile strength of the modified HNT-filled PTFE nanocomposites (F-HNT/PTFE) improved to an acceptable degree and Young's modulus increased significantly. The tribological results showed that the wear rate of F-HNT/PTFE decreased by 21–82 and 9–40 times compared to pure PTFE and the pristine F-HNT/PTFE, respectively.

The effect of magnetic field on the plasma parameters and surface modification of Cu-alloy has been investigated. For this purpose, we have employed Nd: YAG laser at various irradiances ranging from 1.9 to 5 GW/cm2 to irradiate Cu-alloy under 5 torr pressure of argon, neon, and helium. The evaluated values of excitation temperature (Texc) and electron number density (ne) of Cu-alloy plasma explored by laser-induced breakdown spectroscopy technique are higher in the presence of 1.1 Tesla magnetic field as compared with field-free case. It is true at all irradiances as well as under all environmental conditions. It is also found that trends of both Texc and ne are increasing with increasing laser irradiance from 1.9 to 4.4 GW/cm2. For the highest used irradiance 5 GW/cm2, the decrease in both parameters is observed. The analytically calculated values of thermal beta, directional beta, confinement radius, and diffusion time for laser-irradiated Cu-alloy plasma confirm the validity of magnetic confinement. Scanning electron microscope analysis is utilized to study the surface modifications of laser-irradiated Cu samples and reveals the formation of islands, craters, cones, and droplets. The finer-scale surface structures are grown in case of magnetic. It is also revealed Texc and ne play a substantial part in the growth of surface structures on Cu-alloy.

The objective of the study was to modify the external surface of commercially produced polyethylene (PE) tubes made by Balton, Poland, to improve their hydrophilic properties. The process was conducted in a new dielectric barrier discharge reactor. The carrier gases were argon and air, whereas carbon dioxide and hydrogen were the doping gases. The influence of the gas composition in the plasma chamber on the surface free energy (SFE) of PE tubes was investigated. For the gas composition 50 vol% of Ar + 50 vol% of CO2, the highest value of the SFE (53.4 mJ/m2) was obtained. It means an increase in SFE approx. 17% as compared to the unmodified sample (46.0 mJ/m2). Fourier-transform infrared spectroscopy with attenuated total reflectance (FTIR-ATR) results indicates that on the surface of the tubes, carboxyl, carbonyl, and hydroxyl groups were formed. Those oxygen-containing groups could be responsible for the increase of the hydrophilic effect. The O/C ratio on the surface, measured by the X-ray photoelectron spectroscopy method, was three times higher in the case of the modified samples than in those which were not subjected to plasma treatment.

Characterization of the topmost surface of biomaterials is crucial to understanding their properties and interactions with the local environment. In this study, the oxide layer microstructure of plasma-modified 316L stainless steel (SS316L) samples was analyzed by a combination of electron backscatter diffraction and electron channeling contrast imaging using low-energy incident electrons. Both techniques allowed clear identification of a nano-thick amorphous oxide layer, on top of the polycrystalline substrate, for the plasma-modified samples. A methodology was developed using Monte Carlo simulations combined with the experimental results to estimate thickness of the amorphous layer for different surface conditions. X-ray photoelectron spectroscopy depth profiles were used to validate these estimations.

Irradiation damage, caused by the use of beams in electron and ion microscopes, leads to undesired physical/chemical material property changes or uncontrollable modification of structures. Particularly, soft matter such as polymers or biological materials is highly susceptible and very much prone to react on electron/ion beam irradiation. Nevertheless, it is possible to turn degradation-dependent physical/chemical changes from negative to positive use when materials are intentionally exposed to beams. Especially, controllable surface modification allows tuning of surface properties for targeted purposes and thus provides the use of ultimate materials and their systems at the micro/nanoscale for creating functional surfaces. In this work, XeF2 and I2 gases were used in the focused ion beam scanning electron microscope instrument in combination with gallium ion etching of high-density polyethylene surfaces with different beam currents and accordingly different gas exposure times resulting at the same ion dose to optimize and develop new polymer surface properties and to create functional polymer surfaces. Alterations in the surface morphologies and surface chemistry due to gas-assisted etching-based nanostructuring with various processing parameters were tracked using high-resolution SEM imaging, complementary energy-dispersive spectroscopic analyses, and atomic force microscopic investigations.

In this work we reported low and high repetition frequency femtosecond laser-induced modifications of tungsten-based thin film. The tungsten-titanium (WTi) thin film, thickness of 190 nm, was deposited by sputtering on single crystal Si (100) wafer. Irradiations were performed in air by linearly polarized and focused femtosecond laser beams with following parameters: (1) pulse duration 160 fs, wavelength 800 nm, laser repetition frequency (LRF) 75 MHz — high LRF, and (2) duration 40 fs, wavelength 800 nm, LRF of 1 kHz — low LRF. The results of femtosecond lasers processing of the WTi thin film revealed laser induced periodical surface structures (LIPSS) in the case of low LRF regime. LIPSSs were formed with different periodicity and different orientation to the laser polarization at the surface: micro-scale LIPSSs with orientation perpendicular to the laser polarization and nano-scale LIPSSs parallel and perpendicular to the laser polarization. After processing of the WTi/Si system in high LRF regime ablation and nano-particles formation were registered.

Calcium hydroxyl and fluoroapatite (CaHAp and CaFAp) were prepared in the presence of the 2-carboxyletylphosphonic acid (2-CEPA), by hydrothermal method. The incorporation of phosphonic acid within the apatite structure was confirmed by powder XRD, IR and MAS-NMR spectroscopies and SSA. The X-ray powder analysis showed that the cristallinity was not affected by the presence of organic moieties. IR spectroscopy showed new vibration modes related to phosphonate groups. 31P MAS-NMR spectra exhibit new signals, assigned to the presence of organic phosphorus. Specific surface area (SSA) increases with increasing of phosphonate amount, especially for CaHAp. According to these results, a mechanism is proposed for the formation of two types of ionic interaction (-C-O-Ca) and (Ca-O-Porg).

Laser surface melting is one of the most important processes in laser material processing. Selective vaporization of alloying elements in laser melting offers fundamental understanding of laser processing on metallic alloys. This work provides linkage between laser melting and material properties using secondary ion mass spectrometry (SIMS) for tiny vaporized species in laser-generated plume and energy dispersive spectroscopy (EDS) for solid solution range in molten pool, both qualitatively and quantitatively (up to hundreds of micron). Silicon wafer was used to collect the generated plume. Chemical analysis was carried out on top surface and sub-surface of the deposited plume. Transport behavior as well as distribution of the vaporized species inside the plume was further proposed.

The response of titanium surface irradiated with high intensity (1013 – 1015 W/cm2) Ti:sapphire laser was studied in vacuum. Most of the reported investigations were conducted with nano- to femtosecond lasers in gas atmospheres while the studies of titanium surface interacting with femtosecond laser in vacuum are scarce. The laser employed in our experiment was operating at 800 nm wavelength and pulse duration of 60 fs in single pulse regime. The observed surface changes and phenomena are (1) creation of craters, (2) formation of periodic surface structures at the reduced intensity, and (3) occurrence of plasma in front the target. Since microstructuring of titanium is very interesting in many areas (industry, medicine), it can be concluded from this study that the reported laser intensities can effectively be applied for micromachining of the titanium surface (increasing the roughness, formation of parallel periodic surface structures etc.).

The microstructure of a 55 μm diameter, cold-worked Ni-Ti microwire is investigated by different transmission electron microscopy techniques. The surface consists of a few hundred nanometer thick oxide layer composed of TiO and TiO2 with a small fraction of inhomogeneously distributed Ni. The interior of the wire has a core-shell structure with primarily B2 grains in the 1 μm thick shell, and heavily twinned B19′ martensite in the core. This core-shell structure can be explained by a concentration gradient of the alloying elements resulting in a structure separation due to the strong temperature dependence of the martensitic start temperature. Moreover, in between the B2 part of the metallic core-shell and the oxide layer, a Ni3Ti interfacial layer is detected.

A versatile and non destructive technique for a chemical modification by grafting N-vinylcaprolactam (VCL) monomer on the polylactic (PLA) film surface is described. The film substrate is treated with a VCL solution, hexane and benzophenone (BP), the latest promotes the photo initiation. Grafting percentage is derived by a gravimetric method and the success in grafting is evaluated by contact angle technique, UV and ATR-FTIR analysis. The influence of the photoinitiator concentration is evaluated by the polymerization rate (Cp), grafting percentage (Cg) and grafting efficiency (Eg). The modified surface shows higher level of humectation or hydrophilicity, confirming successful surface functionalization of the polylactic acid film.