Synthesis and characterization of cellulose acetate–calcium carbonate hybrid nanocomposite

A hybrid nanocomposite composed of calcium carbonate (CaCO₃) and cellulose acetate (CA) was fabricated by bubbling CO₂ gas into the mixture of CA and Ca(OH)₂ solution. Cellulose acetate–calcium carbonate (CA–CC) nanocomposite was characterized by spectral, thermal and optical methods. FTIR and XRD analysis confirmed the formation of the hybrid nanocomposite and XRD confirmed the formation of CaCO₃ with calcite polymorph. Thermal analysis showed CA–CC nanocomposite has better thermal stability than pristine CA. The CaCO₃ nanoparticles were in sphere shape with 100–1000 nm diameter.     

Synthesis and characterization of hollow glass–ceramics microspheres

Hollow glass–ceramics microspheres (HGCMs), with the diameter from 10 to 60 μm and the shell thickness less than 2 μm, were successfully fabricated by a simple technique using polyacrylamide microspheres (PAMs) as template. The corresponding HGCM were obtained after a thermal treatment of the core–shell microspheres, which were synthesized with organic template method. The size, morphology and phase composition of synthesized products were determined via XRD, SEM, TGA. The effects of the amount of glass powder, the Hydrophile–Lipophile Balance (HLB) value, the sintering temperature, and the ratio of pre-adsorbed water to the water in the slurry on the morphologies of HGCM have been investigated. The results showed that the agglomeration of HGCM can be reduced by adjusting the HLB value. In addition, the amount of solid beads decreases obviously by reducing ratios and adjusting the HLB value. As the sintering temperature increases, the surface of the HGCM becomes smooth and compact. Meanwhile, computational investigations are carried out to better understand the strengthen effect of taking glass–ceramics materials in the system MgO–Al₂O₃–SiO₂ (MAS) as shell materials.     

Synthesis and characterization of chitosan–carbon nanotube composites

Acid functionalized single walled carbon nanotubes were covalently grafted to chitosan by first reacting the oxidized carbon nanotubes with thionyl chloride to form acyl-chlorinated carbon nanotubes which are subsequently dispersed in chitosan and covalently grated to form composite material, CNT–chitosan, 1, which was washed several times to remove un-reacted materials. This composite has been characterized by FTIR, 13C NMR, TGA, SEM and TEM and has been shown to exhibit enhanced thermal stability. The reaction of 1, with poly lactic acid has also been accomplished to yield CNTchitosan–g-poly(LA), 2 and fully characterized by the above techniques. Results showed covalent attachment of chitosan and chitosan–poly lactic acid to the carbon nanotubes.     

Synthesis and characterization of gold–polypyrrole film composite

Polypyrrole (PPy) coatings have potential applications in batteries, fuel cells, sensors, anti-corrosion coatings, and drug delivery systems. In this article, PPy film coating on the electrode of quartz crystal microbalance (QCM) was exposed to acidic aqueous HAuCl₄ solution. The reduction for gold ions took place and gold particles were produced at the film surface. The gold content at the PPy film was monitored by using QCM. The concentration of gold uptake increases as the original concentration of HAuCl₄ solution increases. The morphology of the film before and after the deposition of the gold particles was studied by the scanning electron microscopy coupled with energy dispersive X-ray spectrometry. The gold particles are of undefined shape and have diameters around 200–600 nm. However, the image of the composite powder shows that gold particles of sizes 100–120 nm are distributed over the surface of the polymer particles with some aggregation. Infrared spectroscopy and X-ray diffraction were used to characterize the composite.     

Synthesis and characterization of barium ferrite–silica nanocomposites

In this work, we prepared barium ferrite-silica (BaM-SiO₂) nanocomposites of different molar ratios by high-energy ball milling, followed by heat-treatment at different temperatures. The microstructure, morphology and magnetic properties were characterized for different synthesis conditions by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometry (VSM). The results indicate that 15 h of milling was enough to avoid the generation of hematite phase and to get a good dispersion of barium ferrite particles in the ceramic matrix. For milling periods beyond 15 h and heat treatment above 900 °C, the XRD patterns showed the presence of hematite phase caused by the decomposition of BaM. The agglomerate size observed through SEM analysis was around 150 nm with a good BaM dispersion into the SiO₂ matrix. The highest saturation magnetization (Ms) value obtained was 43 emu/g and the corresponding coercivity (Hc) value of 3.4 kOe for the composition 60BaM-40SiO₂ milled for 15 h and heat treated at 900 °C. This coercivity value is acceptable for the application in magnetic recording media.     

Synthesis of soluble polyimide/silica–titania core–shell nanoparticle hybrid thin films for anti-reflective coatings

In this study, researchers prepared polyimide/silica–titania core–shell nanoparticle hybrid thin films (PI/SiO₂–TiO₂) from soluble fluorine-containing polyimide, colloidal silica, and titanium butoxide. The soluble polyimide with carboxylic acid end groups (6FDA–6FpDA–4ABA–COOH) could condense with titanium butoxide to provide organic–inorganic bonding, and thus prevent macrophase separation. TGA and DSC analysis showed that the decomposition temperature of hybrid materials increased with an increase in the content of silica–titania nanoparticles within the hybrid films. FTIR spectra indicated that the imidization was complete and the cross-linking Ti–O–Ti network formed. HRTEM and HRSEM images showed that the size of the core–shell nanoparticles were 18–20 nm. The thickness of titania shell on the silica is about 2.5 nm. The n&k and UV–Vis analysis showed that the prepared hybrid films had good optical properties and a high refractive index of 1.735. Researchers applied the prepared PI/SiO₂–TiO₂ hybrid thin films to develop a three layer antireflective (AR) coating on the glass and PMMA substrate. Results showed that the reflectance of the AR coating on the glass and PMMA substrate at 550 nm was 0.356 and 0.495%, respectively. The transparency was greater than 90% for both AR coatings on the glass and PMMA substrates.     

Synthesis and characterization of PVAm/SBA-15 as a novel organic–inorganic hybrid basic catalyst

Composite polyvinyl amine/SBA-15 (PVAm/SBA-15) in various amounts of SBA-15 were prepared and characterized. The physical and chemical properties of PVAm/SBA-15 were investigated using FT-IR, XRD, BET, SEM and TGA techniques. The catalytic performance of each material was determined for the Knoevenagel condensation reaction between carbonyl compounds and ethyl cyanoacetate in the presence of ethanol as solvent. The effects of reaction temperature, solvent and the amounts of catalyst as well as recyclability of the catalyst were investigated. The catalyst used for this synthetically useful transformation showed a considerable degree of reusability besides being very active.     

Synthesis and characterization of photoconductive C60–N-vinylcarbazole copolymers

Soluble C60–N-vinylcarbazole copolymers with different C60 contents were synthesized in lithium naphthalene-initiated anionic polymerization reactions. 13C nuclear magnetic resonance (NMR) results provided strong evidence for the covalent attachment of poly(N-vinylcarbazole; PVK) units to the C60 cores. The chemical shifts located at 142.16, 143.21, 144.70, 145.61, 146.65, 147.09, 149.08 and 170.28 p.p.m. in the 13C NMR spectrum of the copolymer are assigned to the unsaturated carbon signals of the substituted C60 cage. Its ultraviolet–visible absorption spectrum tends to move to the longer wavelength compared with those of the N-vinylcarbazole (NVC) monomer and PVK, and the peak range also extended from about 350 to 640 nm due to charge-transfer interaction between C60 and N-ethylcarbazole units. X-ray diffraction evidence suggests that the structure of the resultant copolymer might be a layered structure. Like the C60 chemically modified PVK, this material also exhibits good photoconductivity and temperature sensitivity. An unusual temperature dependence of the ESR spectrum is observed. In addition, it is also found that both [60] fullerene polyanion salts [(Cn-60) M+n, M=Li, Na, K] and fullerene itself are unable to initiate the polymerization of such monomers as N-vinylcarbazole, styrene and acrylonitrile, etc. © 1998 Kluwer Academic Publishers     

Synthesis and electrical properties of graphene–manganese oxide hybrid nanostructures

Journal of Materials Science: Materials in Electronics - In the present contribution, grapheme–manganese oxide hybrid nanostructures (G/MnO2) were synthesized via rapid and facile microwave...     

Fabrication and characterization of microcapsules with polyamide–polyurea as hybrid shell

Well-defined microcapsules with polyamide–polyurea as a hybrid shell have been described for biomedical applications. Interfacial polymerization method with surfactant and cosurfactant was developed for the preparation of the hybrid microcapsules. After reaction, centrifugation, and freeze drying processes, the polyamide–polyurea hybrid microcapsules with porous membranes were successfully fabricated. Compared with previous researches of the single polyamide or polyurea microcapsules, experimental data showed that the hybrid microcapsules have a thicker shell and excellent mechanical property. Various diameters and morphologies for the hybrid microcapsules can be obtained by changing the stirring rate, drying method, and surfactant content.     

Synthesis and characterization of polymetalate based photochromic inorganic–organic nanocomposites

A novel reversible photochromic nanocomposite film based on a hybrid inorganic–organic matrix in which heteropolyacid H₃PW₁₂O₄₀ (PWA) was entrapped was prepared. The structure, photochromic behaviors and mechanism of the film were investigated by means of infrared (IR) spectroscopy, UV-Vis absorption spectra and electron spin resonance (ESR). The results showed that heteropolyanion, i.e. PW₁₂O₄₀³⁻ (PW₁₂), maintained a Keggin structure in the film and there was a strong interaction between anion PW₁₂ and cation R–NH₃⁺ (R=link of hybrid composite). The photochromic properties of the composite film originated from the reversible charge transfer between the anions and cations. Under ultraviolet (UV) irradiation, the anion would be reduced via one-electron step with simultaneous oxidation of the cation, accompanied by a color change from colorless to blue. Then the bleaching could occur when the film was in contact with ambient air or O₂ in the dark.     

Synthesis and characterization of phenol–formaldehyde microcapsules for self-healing coatings

Phenol–formaldehyde microcapsules containing solvent and epoxy resin are successfully prepared via in situ polymerization. Resin–solvent capsules are produced in high yield (up to 82.33%) and high core content (up to 86.3%), of which the diameter distribution ranges between 51 and 323 μm depending on the agitation rate varying from 400 to 1200 rpm. Chemical structure of the capsules is studied by FTIR, and surface morphology is further characterized by optical and electron microscopes. It is found that the capsules possess a rough and compact shell. Meanwhile, encapsulated core materials still keep sufficiently high chemical reactivity, and healing efficiencies effectively exceed 100% with the addition of 20 wt% microcapsules in the host polymer matrix.     

Synthesis and characterization of biocomposites with different hydroxyapatite–collagen ratios

Hydroxyapatite (HA)-type I collagen (Col) composite is a tissue-engineered bone graft which can act as a carrier or a template structure for cells or any other agents. In this paper, the effect of Col ratio on the scaffold structure and composition was analyzed. Scaffolds composed by HA/Col with different weight ratios (80:20; 50:50; 20:80, and 10:90) were produced by the precipitation method at pH 8–9, 37°C and 6 h of ripening. Using X-ray diffraction data, the Rietveld structure refinement showed that the size of HA crystals along the c-axis direction (002) decreases significantly in the presence of Col. Thus, the HA crystal shape turned from needle-like in pure HA, into spherical, in the 10:90 composite due to Col fibrillogenesis. The homogeneity of the composite was significantly dependent on the amount of Col in it. HA/Col 20/80 composite presented HA particles in a more homogenous way. Such a biocomposite was successfully produced in a rapid way and it is potentially useful for both small tissue repairs and engineering.     

Synthesis and characterization of NiO nanoparticles by sol–gel method

Nickel oxide nanoparticles have been synthesized in the presence of agarose polysaccharide by sol–gel method. The structure, morphology, optical and magnetic properties of the product was examined by X-ray diffraction, transmission electron microscopy, UV–visible spectrophotometer and superconducting quantum interference device magnetometer. The result of thermogravimetric analysis of the precursor product showed that the proper calcination temperature was 400 °C. X-ray diffraction result revealed that the obtained product was nickel oxide with face-centered cubic structure. TEM image demonstrated that the nickel oxide nanoparticles have spherical shape with size around 3 nm. Analysis of FTIR spectra confirmed the composition of product. The optical absorption band gap of the NiO nanoparticles was estimated to be 3.51 eV. Magnetic measurement showed that the nickel oxide nanoparticles exhibit superparamagnetic behavior at 300 K. Moreover, the nanoparticles show ferromagnetic interactions at 4.2 K owing to the existence of uncompensated moments on the surface of the nanoparticles.     

Preparation and characterization of hybrid antimicrobial materials based on Zn–Lu composites

The development of advanced functional materials, capable of providing effective antimicrobial activity, has a big demand from the contemporary society. Advanced functional antimicrobial amorphous silica composites (ASC) are prepared by using sol–gel process and modified by Zn ions and rare-earth element Lu. The preparation conditions are optimized by single-factor analysis, and as-prepared functional hybrids are characterized by scanning electron microscopy (SEM), X-ray diffraction analysis, X-ray photoelectron spectroscopy (XPS), atomic adsorption spectrometry and inductively coupled plasma analyses. The presence of homogeneously mixed Zn and Lu, in the form of ZnO and Lu₂O₃, and dense micropores is confirmed by SEM and XPS. The amorphous structure and large surface area are beneficial for better antimicrobial performance. The as-prepared Zn–Lu ASC exhibited excellent antimicrobial properties against Escherichia coli and Staphylococcus aureus. We demonstrate that the addition of rare-earth element, Lu, has rendered synergistic effect on antimicrobial properties by increasing the release of Zn ions and generating excess reactive oxygen species. The present study provides a mechanistic insight and novel approach to fabricate functional antimicrobial materials for a wide range of applications.     

Synthesis and characterization of γ-zirconium arsenate

The hydrothermal synthesis of a novel layered zirconium arsenate, Zr( AsO₄) (H₂AsO₄) · 2H₂O, with γ-type structure and preliminary data on its characterization by chemical and thermal analysis, X-ray diffraction (XRD) and ion exchange are reported. This XRD powder pattern is indexed on a monoclinic cell: a = 5.5699(2) Å, b = 6.8175(4) Å, c= 12.1203(6) Å and β= 103.15(1)°.     

Synthesis and characterization of Co–Fe nanoparticles supported on mesoporous silicas

Co–Fe bimetallic samples containing 25 wt% total of metal content were prepared by incipient wetness impregnation of cobalt nitrate and iron nitrate salts over hexagonal mesoporous silica (HMS) and SBA-15 supports. Changes in the textural properties and reduction behavior were compared with monometallic cobalt/iron-based samples. The samples were characterized by N₂ physisorption, X-ray diffraction (XRD), H₂-temperature programmed reduction (TPR), transmission electron microscopy (TEM) and H₂ chemisorption. The amount of incorporated metal was estimated by atomic absorption spectroscopy (AAS). Morphological properties revealed that after introduction of the metal to the SBA-15 support, the specific area, pore volume and pore diameter decreased to a lesser extent for bimetallic samples. XRD measurements detected the formation of Co₃O₄ and CoFe₂O₄ phases for both bimetallic samples. TPR profiles indicated similar behavior for both the bimetallic and monometallic samples. Higher temperatures were observed for the reducibility of Co–Fe/HMS as compared to Co–Fe/SBA-15. Dispersion values of the bimetallic samples were higher than Fe monometallic samples and lower than Co monometallic samples according to hydrogen chemisorption. The particle size distribution of the bimetallic samples estimated by TEM microphotographs showed a smaller fraction of larger size particles for Co–Fe/SBA-15.     

Synthesis and in vitro characterization of a novel PAA–ATP conjugate

The objective of this study was to improve the multifunctional properties of poly(acrylic acid) (PAA) by covalent attachment of 4-aminothiophenol (ATP) to its backbone. The permeation enhancing effect of PAA–ATP together with glutathione was evaluated in Ussing-type chambers using fluorescein isothiocyanate dextran as model compound. The mucoadhesive properties were evaluated in vitro on freshly excised porcine intestinal mucosa through the rotating cylinder method. The resulting conjugates PAA–ATP1 and PAA–ATP2 displayed 168 ± 35 and 426 ± 55 μmol immobilized free thiol groups per gram polymer, respectively. In addition, 279 ± 28 and 139 ± 22 μmol disulfide bonds per gram polymer, respectively, were identified on PAA–ATP1 and PAA–ATP2. Within disintegration studies in aqueous buffer solution, the modified polymers showed improved cohesive properties. Because of the immobilization of ATP, the swelling of PAA–ATP1 and PAA–ATP2 improved 12.0- and 17.8-fold, respectively. The adhesion times of the conjugates PAA–ATP1 and PAA–ATP2 were more than 20- and 30-fold increased in comparison to unmodified PAA. Furthermore, conjugates PAA–ATP1 and PAA–ATP2 exhibited a 1.86- and 2.07-fold higher permeation enhancing effect, respectively, over unmodified PAA. According to these results, PAA–ATP conjugates represent a very promising novel type of thiomer for the development of various mucoadhesive drug delivery systems.     

Synthesis and characterization of novel γ-induced porous PHEMA–IL composites

A novel porous polymer-ionic liquid composite with poly(2-hydroxyethyl methacrylate) (PHEMA) and 1-butyl-3-methylimidazolium hexafluorophosphate (BMIPF₆) has been synthesized by γ-irradiation without heat or chemical initiators. The products can be reversibly converted into organogels. The composites are potential candidates for electrochemical applications. The use of γ-radiation can be a simple and versatile alternative way to obtain these materials.     

Synthesis and characterization of nanocrystalline Ni–YSZ cermet anode for SOFC

Ni–YSZ cermet anode has been synthesized in one step using a simple and cost effective combustion synthesis process. The processed powder of NiO–YSZ is found to be nanocrystalline with crystallite sizes of 29 and 22 nm for NiO and YSZ respectively by X-ray diffraction and transmission electron microscopy analysis. X-ray diffraction analysis also shows that the precursor salts are converted to highly crystalline phases of NiO and YSZ (8 mol% Y₂O₃) without any intermediate calcination step and no undesirable phases are present. Comparison with the X-ray diffraction pattern of a commercial YSZ sample shows that the process is also effective in maintaining a close compositional control. The microstructure of the sintered and reduced sample shows a well defined network of pores which is necessary for the effective functioning of the anode. The electrical conductivity as a function of temperature shows metallic behavior.