We report that transparent mesostructured silica/gold nanocomposite materials with an interpore distance of 4.1 nm, as-synthesized from a templated sol–gel synthesis method using discotic trinuclear gold(I) pyrazolate complex, were successfully utilized for the fabrication of thin film mesoporous silica nanocomposites containing gold nanoparticles. The material exhibited a highly ordered hexagonal structure when subjected to a thermal hydrogen reduction treatment at 210 °C. In contrast, when the material was subjected to calcination as a heat treatment from 190 to 450 °C, the thin film nanocomposites showed an intense d 100 X-ray diffraction peak. Moreover, gold nanoparticles inside the thin film nanocomposites were confirmed by the presence of the d 111 diffraction peak at 2θ = 38.2°, a surface plasmon resonance peak between 500–580 nm, and the spherical shape observed in the transmission electron microscope images, as well as the visual change in color from pink to purple. Interestingly, by simply dipping the material into a reaction solution of 4-nitrophenol at room temperature, the highly ordered structure of the as-fabricated silica/gold nanoparticle thin film composite after thermal hydrogen reduction at 210 °C resulted in an improved catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol compared to the material calcined at 250 °C. Such catalytic activity is due to the presence of gold nanoparticles of smaller size in the silicate channels of the highly ordered mesoporous film nanocomposites.
Gold nanoparticles (AuNPs) with small particle size have been difficult to be synthesized due to their strong agglomeration. Herein we report that the nanochannels of mesoporous silica synthesized from template sol-gel synthesis were utilized to prepare AuNPs by employing thermal hydrogen reduction. Mesoporous silica composite with an interpore distance of 4.1 nm was successfully fabricated as a thin film by an amphiphilic trinuclear gold(I) pyrazolate complex ([Au3Pz3]C10TEG) as a template. In contrast to calcination method of this composite and the bulk [Au3Pz3]C10TEG complex at 450ºC for 3 h, thermal hydrogen reduction at 250ºC for 2 h showed transmission electron microscope (TEM) images and diffraction pattern with smaller particle size (14.5 nm) and more homogenous distribution of AuNPs with up to 44% of the particle size in the range of 10 to 20 nm. The decreasing of average particle size in this new strategy indicated by the red-shifting of the surface plasmon resonance (SPR) band from 518 (AuNPs from the bulk [Au3Pz3]C10TEG complex) and 544 (calcination) to 558 nm.
Gold nanoparticles (AuNPs) having particle size less than 10 nm can exhibit enhancement of surface area to give high activity such as in catalytic reaction. However, it is hard to synthesize AuNPs with small particle size due to the strong agglomeration. Herein we report that channels of mesoporous silica synthesized via the template sol-gel synthesis can be used to prepare AuNPs by calcination method. Mesoporous silica with an interpore distance of 4.1 nm was successfully fabricated as transparent thin film by using an amphiphilic trinuclear gold (I) pyrazolate complex as a template for the sol-gel synthesis. Upon calcination at 450 °C for 3 h, silica film nanocomposites showed red-shifting of surface plasmon resonance (SPR) bands from 518 (AuNPs from the bulk) to 544 nm owing to decreasing of the average particle size. The formation of AuNPs was also supported by the appearance of diffraction peaks of d111 at 2θ = 38.20° having a cubic phase. Moreover, transmission electron microscope (TEM) images and X-ray diffraction (XRD) peaks also showed smaller and more homogenous distribution of AuNPs.
Column gravity chromatography suffered from several drawbacks such as time-consuming and need a large amount of eluents. Herein we reported an efficient technique for effective separation of amphiphilic trinuclear gold(I) pyrazolate complex ([Au3Pz3]C10TEG) with high polarity based on size-exclusion principle of chromatographic technique. Based on the size-exclusion limit, [Au3Pz3]C10TEG having a larger size with molecular weight of 4011.39 Da (4030.40 Da when added Na+) was successfully eluted and collected firstly from its impurities after being recycled for 2 times. In the chromatogram for first cycle, an intense peak upon excitation at 220 nm for [Au3Pz3]C10TEG was observed at retention time of 58 mins, while small peaks due to the presence of impurities was observed in the range between 73 to 85 mins. In the second cycle, the impurities were flushed away before [Au3Pz3]C10TEG was successfully collected at retention time of 170 mins in the third cycle. The columns were a set of polystyrene/divinylbenzene (PS/DVB) JAIGEL-1H and -2.5H connected in series having exclusion limit of 1 X 103 and 2 X 104 in which chloroform was used as the eluent at flow rate of 3.5 mL min-1. As a result, the visual appearance of dark-yellowish [Au3Pz3]C10TEG was successfully purified to give pale-yellowish product. Moreover, differential scanning calorimetry thermogram showed that extra shoulder from impurities at 6.13 °C in the first endothermic peak of [Au3Pz3]C10TEG at 0.76 °C was completely removed. Hence, it can be concluded that size-exclusion chromatography can be used as an effective purification method with much more convenience and small consumption of solvents.
The photochemical synthesis of two-dimensional (2D) nanostructured from semiconductor materials is unique and challenging. We report, for the first time, the photochemical synthesis of 2D tin di/sulfide (PS-SnS2-x, x = 0 or 1) from thioacetamide (TAA) and tin (IV) chloride in an aqueous system. The synthesized PS-SnS2-x were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), a particle size distribution analyzer, X-ray photoelectron spectroscopy (XPS), Fourier-transform infrared spectroscopy (FTIR), thermal analysis, UV–Vis diffuse reflectance spectroscopy (DR UV–Vis), and photoluminescence (PL) spectroscopy. In this study, the PS-SnS2-x showed hexagonally closed-packed crystals having nanosheets morphology with the average size of 870 nm. Furthermore, the nanosheets PS-SnS2-x demonstrated reusable photo-degradation of methylene blue (MB) dye as a water pollutant, owing to the stable electronic conducting properties with estimated bandgap (Eg) at ~2.5 eV. Importantly, the study provides a green protocol by using photochemical synthesis to produce 2D nanosheets of semiconductor materials showing photo-degradation activity under sunlight response.
Gold(I) pyrazolate complex ([Au3Pz3]C10TEG) has been widely studied due to its interesting liquid crystalline properties by exhibiting the discotic hexagonal columnar arrangement. Generally, the liquid crystalline properties of the gold complex were confirmed based on their differential scanning calorimetry thermogram and polarized optical microscopy (POM) images. However, there is still no in-depth study on the phase transition in liquid crystals of [Au3Pz3]C10TEG especially on its structural change at variable temperature. In this study, the resulting liquid crystalline properties of [Au3Pz3]C10TEG upon being heated and cooled was extensively demonstrated via variable-temperature POM (VT-POM) and small angle X-ray scattering (VT-SAXS). Based on the VT-POM images, it was indicated that [Au3Pz3]C10TEG displayed a fan-shaped texture for typical arrangements of discotic hexagonal columnar of liquid crystals. Moreover, VT-SAXS results was in good agreement with the VT-POM images as it showed that [Au3Pz3]C10TEG might consist of two types of stacking system, which are ordered and disordered hexagonal discotic arrangements. Likewise, VT-SAXS analysis also demonstrated that hexagonal columnar mesophase of [Au3Pz3]C10TEG could be recovered even after the heating and cooling for two cycles.
Recent advances in the field of biomedical have been remarkably achieved in the last few years, especially in the fabrication of nanomaterials that have various applications. Carbon nanotubes (CNTs) are carbon-based materials with cylindrical shapes that have an average diameter of less than 2 nanometre (nm) for single-walled CNTs (SWCNTs) and multi-walled CNTs (MWCNTs) with average diameters up to 100 nm. CNTs demonstrate various outstanding and excellent mechanical, electrical, conductivity, thermal properties, high surface area, and high biocompatibility. These remarkable properties have led to the development of CNTs-based materials in the biomedical field. For the past decades, the functionalization of CNTs has been actively researched in order to increase their biocompatibility for application in antibacterial materials, dentistry, drug delivery, and biosensing. The surface functionalization enhances the capabilities, features, and properties by modifying the surface chemistry of CNTs to improve their biocompatibility. The functionalization of CNTs will enable the biomolecule loading on the surface of CNTs, and thus can be used for drug delivery for targeted cells or immobilization support. In this review, we discuss the related literatures on biomedical applications of CNTs such as antibacterial, dental materials, cancer therapy and biosensors from 2007 – 2022. We also review the antibacterial properties between SWCNTs and MWCNTs, functionalized CNTs-reinforced nanocomposite for dental applications, and the ability of CNTs to work as nanocarriers to deliver drugs directly to cancer cells. Moreover, the applications of CNTs-based biosensors in detecting biological and biomedical compounds are also discussed.
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