Characterization of stable hydrophobic carbon coating and its application in removing organic pollutants

Polydimethylsiloxane (PDMS) thin films were deposited on Ni particles with a mean size of ～1 μm using chemical vapor deposition method. The thin films consisting of these PDMS-covered Ni particles showed a water contact angle higher than 160°, corresponding to the superhydrophobicity. These superhydrophobic films were found to be resistant toward acidic and basic media. The PDMS-covered Ni particles showed high affinity toward non-polar organic solvent such as toluene. Together with an external magnetic field, the PDMS-covered Ni can be used for separating water and toluene from a water/toluene heterogeneous mixture.     

A study of phase transfer processes of Ag nanoparticles

With the protection of sodium oleate, Ag nanoparticles are produced through the reduction of AgNO₃ with NaBH₄ in an aqueous solution. The possible mechanism of phase transfer of the Ag nanoparticles was discussed. At a suitable concentration of sodium oleate, after adding NaH₂PO₄, the oleic acid molecule can change its position on the surface of Ag nanoparticles under the effects of water and toluene and become amphipathic. So most of the nanoparticles form a film between water/toluene. For the case of a higher concentration of sodium oleate, excess sodium oleate will form a closed monolayer film on the surface of the Ag nanoparticles. After adding NaH₂PO₄, the oleic acid molecule cannot move on the Ag nanoparticles surface, thus the colloid particles are hydrophobic but not amphipathic. So most of the particles transfer to the organic phase. UV–Vis spectra, TEM and conventional metallographic microscopy are used to characterize the Ag nanoparticles and nanoparticles films.     

Matrix-assisted pulsed laser evaporation of polyfluorene thin films

Poly(9,9-dioctylfluorene) (PF8) thin films have been deposited by matrix-assisted pulsed laser evaporation (MAPLE) using a KrF excimer laser. The influence of the laser fluence (50-500 mJ/cm²) and the nature of the solvent (chloroform, toluene, tetrahydrofuran) on the films properties have been studied. The chemical composition of the deposited films was investigated by Fourier transform infrared (FTIR) spectroscopy and compared with the one of spin coated films. To investigate the effect of the deposition parameters on the optical properties of the films, photoluminescence (PL) measurements were performed. Poor structural and optical properties were observed for films deposited starting from chloroform solutions. When using toluene as solvent, the spectra characteristics improved with increasing laser fluence, while wide PL spectra were observed. The characteristic emission bands of the PF8 polymer were nicely detected for films deposited starting from a tetrahydrofuran (THF) solution. Moreover, in this last case, the PF8 structure is preserved at high laser fluences, too.     

An XPS study on the attachment of triethoxsilylbutyraldehyde to two titanium surfaces as a way to bond chitosan

A bioactive coating has the ability to create a strong interface between bone tissue and implant. Chitosan, a biopolymer derived from the exoskeletons of shellfish, exhibits many bioactive properties that make it an ideal material for use as a coating such as antibacterial, biodegradable, non-toxic, and the ability to attract and promote bone cell growth and organized bone formation. A previous study reported on the bonding of chitosan to a titanium surface using a three-step process. In the current study, 86.4% de-acetylated chitosan coatings were bound to implant quality titanium in a two-step process that involved the deposition of triethoxsilylbutyraldehyde (TESBA) in toluene, followed by a reaction between the aldehyde of TESBA with chitosan. The chitosan coatings were examined on two different metal treatments to determine if any major differences in the ability of titanium to bind chitosan could be detected. The surface of the titanium metal and the individual reaction steps were examined using X-ray photoelectron spectroscopy (XPS). Following the deposition of TESBA, significant changes were seen in the amounts of oxygen, silicon, carbon, and titanium present on the titanium surface, which were consistent with the anticipated reaction steps. It was demonstrated that more TESBA was bound to the piranha-treated titanium surface as compared to the passivated titanium surface. The two different silane molecules, aminopropyltriethoxysilane (APTES) and TESBA, did not affect the chemistry of the resultant chitosan films. XPS showed that both the formation of unwanted polysiloxanes and the removal of the reactive terminal groups were prevented by using toluene as the carrier solvent to bond TESBA to the titanium surfaces, instead of an aqueous solvent. Qualitatively, the chitosan films demonstrated improved adhesion after using toluene, as the films remained attached to the titanium surface even when placed under the ultra-high vacuum necessary for XPS, unlike the chitosan films deposited using an aqueous solvent, which were removed when exposed to the ultra-high vacuum environment of XPS.     

Solvent-related effects in MAPLE mechanism

To study the role of the solvent and of the laser fluence in the matrix-assisted pulsed laser evaporation (MAPLE) process, we used a soft polymer (polydimethylsiloxane—PDMS) as “sensing surface” and toluene as solvent. Thin films of the PDMS polymer were placed in the position of the growing film, while a frozen toluene target was irradiated with an ArF laser at the conventional fluences used in MAPLE depositions (60–250 mJ/cm²). Apart the absence of solute, the MAPLE typical experimental conditions for the deposition of thin organic layers were tested. The effects on the PDMS films of the toluene target ablation, at different fluences, were studied using atomic force microscopy and contact angles measurements. The results were compared with the effects produced on similar PDMS films by four different treatments (exposure to a drop of the solvent, to saturated toluene vapors and to plasma sources of two different powers). From this comparative study, it appears that depending on the MAPLE experimental conditions: (1) the MAPLE process may be “semidry” rather than purely dry (namely the solvent is likely to be present in the deposition environment near the growing film), (2) the solvent, if sufficiently volatile, is in form of vapor molecules (neutral, ionized and probably dissociated) rather than in liquid phase near the substrate and (3) at relatively high laser fluences (>150 mJ/cm²), the formation of an intense plasma plume results which can damage/affect a soft substrate as well as a growing polymer film.     

Thin films of polyaniline deposited by MAPLE technique

Polyaniline (PAni) has important electro-conductive properties, high absorbance in microwave range and it is also frequently used in gas sensors because of its capability to convert chemical interactions into electrical signals. The methods of obtaining polyaniline in the form of thin films and/or nanostructures are complicated and request special physical and chemical treatments, both on the substrate surface and for the polymer itself.In this paper we applied matrix assisted pulsed lased evaporation (MAPLE) for obtaining thin films and nanostructures of polyaniline. In MAPLE, the target consisting of the material (usually 0.2-3 wt%) dissolved in a solvent is frozen and it is evaporated using a laser. In our case polyaniline-emeraldine salt (PAni-ES) was dissolved in xylene or toluene, frozen in liquid nitrogen and was used as target. The third and the fourth harmonics of a Nd-YAG laser (λ = 355 nm and 266 nm) were used as laser sources. The obtained films have been characterized by atomic force microscopy, dielectric spectroscopy and Fourier transform infrared spectroscopy. The influence of the solvent type and of the laser parameters (wavelengths and fluence) on the polyaniline structures composition and properties has been investigated.     

An infrared spectroscopic investigation of thin alumina films: measurement of acid sites and surface reactivity

The surface chemical activity of an alumina films grown on Mo(100) by oxidation of aluminum evaporated onto the surface and oxidized using water is examined using Auger, X-ray photoelectron and reflection/absorption infrared spectroscopies. The formation of alumina is confirmed using Auger and X-ray photoelectron spectroscopy from the positions and intensities of the aluminum features and using reflection-absorption infrared spectroscopy from the longitudinal optical modes of the Al–O bonds measured at 935 cm⁻¹. The presence of surface hydroxyls is monitored by forming films using D₂O which are evidenced by a feature at 2700 cm⁻¹. Ammonia adsorption on a dehydroxylated surface yields a single peak at 1260 cm⁻¹ due to ammonia adsorbed at a surface Lewis site where the principle symmetry axis of ammonia is oriented perpendicularly to the surface plane. Ammonia also appears to adsorb at Lewis sites on a hydroxylated surface with a slightly different adsorption geometry from that on a dehydroxylated surface. Finally, the chemistry of trimethyl aluminum adsorbed on the planar hydroxylated alumina surface is compared with that found on high-surface-area γ-alumina where the spectra and the chemistry found in both régimes is exactly identical except that the low-frequency methyl bending modes (at 769 and 718 cm⁻¹) are not obscured on the thin film by the intense substrate whereas they are on the high-surface-area support.     

水性涂料施工过程中微观结构的FTIR研究

以市售立邦水性涂料作为研究对象,溶剂水作为变量因子。配制不同水料比的涂料系列样品,分别用FTIR/ATR、FTIR/漫反射光谱表征湿料、涂膜的微观结构特征,湿料抽滤得到的固型物用FTIR/漫反射光谱表征。分析其官能团变化情况,研究施工过程,溶剂对涂膜的影响。结果显示：随着加水量的增加,湿料的FTIR/ATR光谱中,1 727 cm-1对应的羰基吸收峰,逐渐转为肩峰,871 cm-1吸收峰发生蓝移,峰强度逐渐减弱;涂膜的漫反射红外图谱,3 400 cm-1的—OH吸收峰、3 030 cm-1不饱和—CH吸收峰强度逐渐变弱,2 962和2871 cm-1的甲基和亚甲基的吸收峰强度逐渐增强,2 516 cm-1吸收峰位移至2 603 cm-1形成肩峰,1 647 cm-1吸收峰逐渐位移至1 455 cm-1,1 107 cm-1对应的C—O伸缩振动吸收峰发生红移。在水性涂料施工过程中,溶剂水与涂料分子间存在相互作用,对涂层分子中电子云的密度分布有显著的影响,此结果对涂料的生产及施工有参考意义。     

Engineering and characterization of mesoporous silica-coated magnetic particles for mercury removal from industrial effluents

Mesoporous silica coatings were synthesized on dense liquid silica-coated magnetite particles using cetyl-trimethyl-ammonium chloride (CTAC) as molecular templates, followed by sol-gel process. A specific surface area of the synthesized particles as high as 150 m²/g was obtained. After functionalization with mercapto-propyl-trimethoxy-silane (MPTS) through silanation reaction, the particles exhibited high affinity of mercury in aqueous solutions. Atomic force microscopy (AFM), zeta potential measurement, thermal gravimetric analysis (TGA), analytical transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and atomic absorption spectroscopy (AAS) were used to characterize the synthesis processes, surface functionalization, and mercury adsorption on the synthesized magnetite particles. The loading capacity of the particles for mercury was determined to be as high as 14 mg/g at pH 2. A unique feature of strong magnetism of the synthesized nanocomposite particles makes the subsequent separation of the magnetic sorbents from complex multiphase suspensions convenient and effective.     

Experimental investigation of C60/NMP/toluene solutions by UV-Vis spectroscopy and small-angle neutron scattering

The transformation of the C₆₀ fullerene cluster state into C₆₀/N-methylpyrrolidone (NMP) solution after the addition of a nonpolar solvent (toluene, electric permittivity ?= 2.4) is studied. The results of ultraviolet-visible spectroscopy and small-angle neutron scattering measurements are used for comparison of the C₆₀/NMP/toluene system with C₆₀/NMP mixtures with a high-polar solvent (water, ? = 80). As to the observed reorganization of the cluster state, the C₆₀/NMP/toluene system is similar to the C₆₀/NMP/water system. This effect is explained by the formation of charge-transfer complexes in the initial C₆₀/NMP solution. These complexes are thought to be soluble in both binary mixtures. The connection between the cluster-reorganization effect and solvatochromism is discussed.