Poly(o-toluidine dihydrochloride): Spectral Characterization and Synthesis of Eskolite Nanoparticles

Poly(o-toluidine?·?2HCl) and its doped polymers with Mn and Cr ions have been synthesized and characterized by FT-IR, UV–Vis. and thermogravimetrical analyses. Potassium dichromate has been used as an initiator and a dopant of chromium in CrPOT preparation. The effect of doping on thermal and optical properties of Poly(o-toluidine dihydrochloride) has been discussed.

CrPOT has been used as a precursor of Cr₂O₃ nanoparticles through thermal decomposition rout. The obtained nanoparticles have been characterized by X-ray diffraction and high resolution transmission electron microscope. The results indicated that Cr₂O₃ exists in hexagonal structure as mesoporous Eskolit with average particle size of 48?nm. Optical band gap measurements indicated that Eskolite nanoparticles have wider band gap than the bulk.     

Surface modification of Cr2O3 nanoparticles with 3-amino propyl trimethoxy silane (APTMS). Part 1: Studying the mechanical properties of polyurethane/Cr2O3 nanocomposites

The surface of Cr₂O₃ nanoparticles was modified with various amounts of 3-amino propyl trimethoxy silane (APTMS). Thermal gravimetric analysis (TGA), turbidimeter and Fourier transform infrared (FTIR) spectroscopy were utilized in order to investigate APTMS grafting on the nanoparticles. Then, polyurethane nanocomposites were prepared using various loadings of silane modified Cr₂O₃ nanoparticles. The nanoparticles dispersion in the coating matrix was studied by a field emission scanning electron microscopy (FESEM). Dynamic mechanical thermal analysis (DMTA) and tensile test were utilized in order to investigate the mechanical properties of the nanocomposites. Results obtained from FTIR, TGA and turbidimeter measurements revealed that the organic functional groups of the silane were successfully grafted on the surface of the nanoparticles. The mechanical properties of the polyurethane were significantly enhanced using 2 wt% Cr₂O₃ nanoparticles modified with 0.43 g silane/5 g pigment compared with other samples.     

Amorphous Ru1−yCryO2 loaded on TiO2 nanotubes for electrochemical capacitors

Amorphous Ru_1−yCr_yO₂/TiO₂ nanotube composites were synthesized by loading different amount of Ru_1−yCr_yO₂ on TiO₂ nanotubes via a reduction reaction of K₂Cr₂O₇ with RuCl₃·nH₂O at pH 8, followed by drying in air at 150 °C. Cyclic voltammetry and galvanostatic charge/discharge tests were applied to investigate the performance of the Ru_1−yCr_yO₂/TiO₂ nanotube composite electrodes. For comparison, the performance of amorphous Ru_1−yCr_yO₂ was also studied. The results demonstrated that the three dimensional nanotube network of TiO₂ offered a solid support structure for active materials Ru_1−yCr_yO₂, allowed the active material to be readily available for electrochemical reactions, and increased the utilization of active materials. A maximum specific capacitance 1272.5 F/g was obtained with the proper amount of Ru_1−yCr_yO₂ loaded on the TiO₂ nanotubes.     

Synthesis of Fe2O3 nanoparticles for nitrogen dioxide gas sensing applications

Iron (III) oxide, Fe₂O₃, nanoparticles of approximately 40 nm diameter were synthesized by sol–gel method and their nitrogen dioxide adsorption and desorption kinetics were investigated by custom fabricated gas sensor unit. The morphology and crystal structure of Fe₂O₃ nanoparticles were studied by scanning electron microscopy (SEM), field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD) respectively. The roughness of film surface was investigated by atomic force microscopy (AFM). Relative sensitivity of Fe₂O₃ nanoparticles for NO₂ sensor was determined by electrical resistance measurements. Our reproducible experimental results show that Fe₂O₃ nanoparticles have a great potential for nitrogen dioxide sensing applications operating at a temperature of 200 °C.     

聚乙二醇/聚乙烯吡咯烷酮修饰的纳米Fe3O4粒子的制备与表征

为了获得能够在水中稳定分散,具有广泛应用前景的磁性纳米粒子,以不同分子量的聚乙烯吡咯烷酮(PVP)作为修饰剂,在聚乙二醇(PEG)中高温热分解乙酰丙酮铁(Fe(acac)₃)制备了纳米Fe₃O₄粒子。采用X射线粉末衍射仪(XRD)、透射电镜(TEM)、高分辨透射电镜(HRTEM)、超导量子干涉仪(SQUID)、热重分析仪(TGA)、傅里叶变换红外光谱仪(FT-IR)、纳米粒度与zeta电位分析仪对样品进行了表征,并对样品在生理盐水和生理缓冲液中的稳定性进行了研究,结果表明:制备的纳米Fe₃O₄粒子具有高的结晶度以及单分散性,在300 K下,具有超顺磁性和较高的饱和磁化强度;PEG和PVP共同修饰于纳米Fe₃O₄粒子表面,为纳米Fe₃O₄粒子提供了良好的水分散性;制备的纳米Fe₃O₄粒子在生理盐水和多种生理缓冲液中能够高度溶解并稳定地分散。水中的纳米Fe₃O₄粒子表面呈电中性,表面修饰层的空间位阻效应是所制备的纳米粒子在水溶液中高分散的原因。     

Using a β-Cyclodextrin-functional Fe3O4 as a Reinforcement of PLA: Synthesis,Thermal, and Combustion Properties

In this work, Fe₃O₄ nanoparticles were chemically grafted with β-cyclodextrin (β-CD@Fe₃O₄). Fe₃O₄ nanoparticles were modified using N,N-dimethylformamide as a solvent, β-cyclodextrin as a modifier, and 3-glycidoxypropyltrimethoxysilane as a coupling agent at room temperature. The obtained modified Fe₃O₄ were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, and thermogravimetric analysis techniques. β-CD@Fe₃O₄ was incorporated into a poly(lactic acid) matrix to prepare new green nanocomposites with modified properties. β-CD@Fe₃O₄ showed good dispersion in the poly(lactic acid) matrix and thermal and combustion properties of the nanocomposites were improved.     

Role of Ni2+ substituent on the structural,optical and magnetic properties of chromium oxide (Cr2-xNixO3) nanoparticles

Pristine chromium oxide (Cr₂O₃) and nickel ions (Ni²⁺) substituted Cr₂O₃ nanoparticles were synthesized using a simple co-precipitation technique. The main objective of this work is to investigate Ni²⁺ substituent's role at different concentrations on the structural, morphological, optical, and magnetic properties of Cr₂O₃ nanoparticles. Structural analyses based on X-ray diffraction (XRD), Raman and Fourier transform infra-red (FTIR) data confirmed the successful incorporation of Ni²⁺ into Cr₂O₃ nanoparticles up to x = 0.05 of Ni²⁺ content, without affecting the rhombohedral crystal structure of Cr₂O₃ nanoparticles. Rietveld refinement results showed the variation in lattice parameters and cell volumes alongwith the substitution of Ni²⁺ into Cr₂O₃ nanoparticles. Raman and FTIR spectra also depicted a considerable shift in the characteristic vibration modes of Cr₂O₃ nanoparticles due to strain-induced by Ni²⁺ substitution. Beyond x = 0.05, the structural transformation took place from rhombohedral to cubic crystal structure. Subsequently, new peaks (apart from Cr₂O₃ phase modes) have been observed at x = 0.1 of Ni²⁺ content due to the formation of secondary phase i.e., nickel chromate (NiCr₂O₄). Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) illustrated the changes in the morphology of Cr₂O₃ nanoparticles with Ni²⁺ substitution. UV–Vis analysis revealed a narrowing of optical band energy (E_g) of Ni²⁺ substituted Cr₂O₃ nanoparticles from 3 to 1.85 eV as Ni²⁺ content varies from x = 0 to 0.2, respectively. Afterward, there is an increase in optical band gap energy (E_g) when Ni²⁺ content increased from x = 0.3 to 0.5, as NiCr₂O₄ started dominating the Cr₂O₃ phase. Single-phase Ni²⁺ substituted Cr₂O₃ nanoparticles exhibited a superparamagnetic behavior, whereas the multi-phase compound ascribed to both superparamagnetic and paramagnetic. These changes in optical and magnetic properties can lead to novel strategies to render applications in the field of optoelectronics and optomagnetic devices.     

ZnO/Cr2O3 catalyst for reverse-water-gas-shift reaction of CAMERE process

The stability and the activity of Fe₂O₃/Cr₂O₃ and ZnO/Cr₂O₃ catalysts were examined for a reverse-watergas-shift reaction (RWReaction). The initial activities of those catalysts were quite high so that the conversion reached close to equilibrium. The activity of Fe₂O₃/Cr₂O₃ catalyst decreased from 33.5 to 29.8% during the RWReaction for 75 h at 873 K with GHSV (ml/gcat · h) of 100,000. Moreover, the coke formation on the Fe₂O₃/Cr₂O₃ catalyst caused clogging in the RWReactor of the CAMERE process. On the other hand, the ZnO/Cr₂O₃ catalyst showed no coke formation and no deactivation for the RWReaction at 873 K with GHSV (ml/gcat · h) of 150,000. The ZnO/Cr₂O₃ was a good catalyst for the RWReaction of the CAMERE process.     

Electron-energy loss spectroscopy and Raman studies of nanosized chromium carbide synthesized during carbothermal reduction process from precursor Cr(CO)6

Nanosized chromium carbide has been prepared by metal-organic chemical vapour deposition (MOCVD) method in a fluidized bed and carburized in the mixture of CH₄/H₂ atmosphere in temperature range 700-850 °C. The carburization process involves carbon deposition on the outer surface of the Cr₂O₃ powder, followed by carbon diffusion into the powder, leading to formation of metastable Cr₃C_2−x phase and stable Cr₃C₂. The phase transformation from Cr₂O₃ to Cr₃C₂ via an intermediate state Cr₃C_2−x has been identified using electron-energy loss spectroscopy (EELS) and micro-Raman spectroscopy. We could hypothesize that the formation of carbon nanofilms surrounding the carbide crystallites provides the stress and assist the phase transformation from metastable Cr₃C_2−x to stable Cr₃C₂.     

Efficient solar photocatalyst based on cobalt oxide/iron oxide composite nanofibers for the detoxification of organic pollutants

A Co₃O₄/Fe₂O₃ composite nanofiber-based solar photocatalyst has been prepared, and its catalytic performance was evaluated by degrading acridine orange (AO) and brilliant cresyl blue (BCB) beneath solar light. The morphological and physiochemical structure of the synthesized solar photocatalyst was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FTIR). FESEM indicates that the Co₃O₄/Fe₂O₃ composite has fiber-like nanostructures with an average diameter of approximately 20 nm. These nanofibers are made of aggregated nanoparticles having approximately 8.0 nm of average diameter. The optical properties were examined by UV-visible spectrophotometry, and the band gap of the solar photocatalyst was found to be 2.12 eV. The as-grown solar photocatalyst exhibited high catalytic degradation in a short time by applying to degrade AO and BCB. The pH had an effect on the catalytic performance of the as-grown solar photocatalyst, and it was found that the synthesized solar photocatalyst is more efficient at high pH. The kinetics study of both AO and BCB degradation indicates that the as-grown nanocatalyst would be a talented and efficient solar photocatalyst for the removal of hazardous and toxic organic materials.     

Dynamic corrosion of Al2O3-ZrO2-SiO2 and Cr2O3-containing refractories by molten frits. Part II: Microstructural study

In this work results on dynamic corrosion studies of fused cast Al₂O₃-SiO₂-ZrO₂ and isostatically pressed and sintered Cr₂O₃-based refractories by two crystalline (transparent) frits are described. Experiments have been performed using the “Merry Go Round” test at ≅1500 °C.Microstructural and mineralogical analyses of selected areas from the corroded regions of the studied refractories were performed by reflected light optical microscopy and scanning electron microscopy with analysis by X-ray dispersive energy.Significant differences between the corrosion mechanisms acting in the two types of materials were found. In the fused cast Al₂O₃-SiO₂-ZrO₂ specimens corrosion took place by the dissolution of alumina and zirconia in the frit and in the glass formed by the reaction between the frit and the refractory. In the Cr₂O₃-based materials the corrosion process was controlled by the capillar penetration of the molten frit through the open pores. The reaction between the ZnO from the frits and Cr₂O₃ led to the formation of spinel (ZnCr₂O₄), a high-melting point bonding phase that retarded the frit penetration. Results are discussed using the relevant phase equilibrium diagrams.     

The effect of nano-Cr2O3 on solid-solution assisted sintering of MgO refractories

The effect of Cr₂O₃ particle size on the densification of magnesia refractories was investigated. Magnesia grains (<45 μm) were mixed with 2 wt% of micro-Cr₂O₃ (2 μm) and nano-Cr₂O₃ particles (10–20 nm) and sintered at 850–1450 °C, for 5 h in air. The progress of the densification and phase evolution of samples was studied with the support of X-ray diffraction phase analysis (XRD), Fourier transformer infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). It was shown that the densification of magnesia was enhanced by reducing the particle size of the added chromia to the range of 20 nm. According to the phase analysis results, the higher dissolution rate of Cr₂O₃ in MgO in the MgO–Cr₂O₃ system was responsible for the faster densification of nano-Cr₂O₃ containing mixes.     

Chromium Oxide Supported on Mesoporous SBA-15 as Propane Dehydrogenation and Oxidative Dehydrogenation Catalysts

The catalytic activity and selectivity of Cr₂O₃ supported on mesoporous SBA-15 for non-oxidative and oxidative dehydrogenation of propane by O₂ and CO₂ have been studied and compared with those of Cr₂O₃/ZrO₂ and Cr₂O₃/-Al₂O₃ catalysts. Cr₂O₃/SBA-15 and Cr₂O₃/ZrO₂/SBA-15 are more selective to propene and more resistant to coking in comparison with Cr₂O₃/ZrO₂ and Cr₂O₃/-Al₂O₃ for non-oxidative dehydrogenation of propane. In oxidative dehydrogenation of propane by O₂ and CO₂, Cr₂O₃/SBA-15 also displays better activity, selectivity and stability than the other two supported catalysts. The propane conversion and propene yield on Cr₂O₃/SBA-15 catalyst for oxidative dehydrogenation of propane by CO₂ at 823 K reach 24.2 and 20.3%, respectively. XPS and TG/DTA have been used to characterize the catalysts before and after reaction. The differences in catalytic behavior of various supported Cr₂O₃ catalysts in the reactions have been discussed on the basis of the characterization results.     

Functionalized magnetic core-shell Fe3O4@SiO2 nanoparticles as selectivity-enhanced chemosensor for Hg(II)

A colorimetric and ‘‘turn-on” fluorescent chemosensor Rho-Fe₃O₄@SiO₂ for Hg²⁺ in which N-(rhodamine-6G)lactam-ethylenediamine (Rho-en) is conjugated with the magnetic core-shell Fe₃O₄@SiO₂ NPs has been strategically designed and synthesized. The final product was characterized by X-ray power diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectra (FTIR) and UV-visible absorption and fluorescence emission. Fluorescence and UV-visible spectra results showed that the resultant multifunctional nanoparticles Rho-Fe₃O₄@SiO₂ exhibited selective ‘turn-on’ type fluorescent enhancements and distinct color changes with Hg²⁺. The selectivity of the Rho-Fe₃O₄@SiO₂ for Hg(II) ion is better than that of the Rho-en in the same conditions. In addition, the presence of magnetic Fe₃O₄ nanoparticles in the sensor Rho-Fe₃O₄@SiO₂ NPs would also facilitate the magnetic separation of the Hg(II)-Rho-Fe₃O₄@SiO₂ from the solution.     

Magnetic and sterilizing properties of Ag(II)O–Fe3O4 hybrids synthesized via mechano-chemistry

Ag(II)O–Fe₃O₄ hybrids with good magnetic and bactericidal activity were synthesized via mechano-chemistry. The resulted products were characterized by transmission electronic microscope, X-ray diffraction, X-ray photoelectron and Fourier transform infrared spectroscopy, atomic absorption spectrophotometer, vibrating sample magnetometry and the shake-flask method. The results indicated that magnetite nanoparticles were effectively grafted onto the surface of Ag(II)O submicron particles. The functionalized particles remained dispersed and superparamagnetic. The saturation magnetization increased with the amount of magnetite in the hybrids. Element Ag was released from Ag(II)O–Fe₃O₄ hybrids with a slow dissolution speed. Ag(II)O–Fe₃O₄ hybrids had strong antibacterial properties. When the concentrations of the two hybrids with the mass ratio of Ag(II)O to Fe₃O₄ of 1:2 and 2:1 were 10 mg/L, more than 99.9% of the Staphylococcus aureus or Escherichia coli bacteria were killed.     

Electrochemical performance of LiV3−xNixO8 cathode materials synthesized by a novel low-temperature solid-state method

A series of cathode materials for lithium ion batteries with the formula LiV_3−xNi_xO₈ (x = 0.000, 0.025, 0.050 and 0.100) have been synthesized by a novel low-temperature solid-state method. The synthesized cathode materials have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), discharge-charge test, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). These results indicate that LiV_2.95Ni_0.050O₈ shows much better electrochemical performances than LiV₃O₈. This is due to better electrochemical reversibility and lower particle-to-particle resistance after Ni²⁺ doping.     

Novel conductive magnetic nanocomposite based on poly (indole-co-thiophene) as a hemoglobin diagnostic biosensor: Synthesis,characterization and physical properties

The novel conductive nanocomposite has been successfully prepared by emulsion polymerization. First, magnetite nanoparticles were synthesized via coprecipitation reaction. Then, poly (indole-co-thiophene)@Fe₃O₄ nanocomposite was prepared via emulsion copolymerization of indole and thiophene monomers using sodium dodecyl sulfate as an emulsifier and ammonium persulfate as an oxidant in the presence of Fe₃O₄ nanoparticles. Characterization of the synthesized copolymer, Poly (In-co-T), and its magnetic nanocomposite were studied by Fourier transform infrared spectra, X-ray diffraction, scanning electron microscopy, thermal gravimetric analysis, differential scanning calorimetric, UV-vis spectrophotometer, and vibrating sample magnetometer. Also, the electrical conductivity of copolymer and nanocomposite were determined by four-probe instrument. Results showed a synergic effect in thermal stability by good interaction between polymer chain and magnetic nanoparticles. The conductivity of the nanocomposite was higher than bare copolymer, and increase of nanoparticles content caused an increment in the conductivity of the nanocomposites. The applicable properties of proposed conductive nanocomposite as a base at electrochemical biosensing have been investigated.     

Synthesis of LiNi0.9Co0.1O2 from Li2CO3, NiO or NiCO3, and CoCO3 or Co3O4 and their electrochemical properties

Cathode active materials with a composition of LiNi_0.9Co_0.1O₂ were synthesized by a solid-state reaction method at 850 °C using Li₂CO₃, NiO or NiCO₃, and CoCO₃ or Co₃O₄, as the sources of Li, Ni, and Co, respectively. Electrochemical properties, structure, and microstructure of the synthesized LiNi_0.9Co_0.1O₂ samples were analyzed. The curves of voltage vs. x in Li_xNi_0.9Co_0.1O₂ for the first charge–discharge and the intercalated and deintercalated Li quantity Δx were studied. The destruction of unstable 3b sites and phase transitions were discussed from the first and second charge–discharge curves of voltage vs. x in Li_xNi_0.9Co_0.1O₂. The LiNi_0.9Co_0.1O₂ sample synthesized from Li₂CO₃, NiO, and Co₃O₄ had the largest first discharge capacity (151 mA h/g), with a discharge capacity deterioration rate of −0.8 mA h/g/cycle (that is, a discharge capacity increasing 0.8 mA h/g per cycle).     

Thermo-mechanical behaviors of epoxy resins reinforced with silane-epoxide functionalized α-Fe2O3 nanoparticles

In this work, α-Fe₂O₃ nanoparticles was synthesized, terminal-epoxide functionalized by using 3-glycidoxypropyltrimethoxysilane (GPS) coupling agent, characterized by FT-IR, X-ray diffraction, TGA and particle size analyzer and used in preparation of nanocomposites with epoxy resin (DGEBA) using different weight fractions (2–11 wt%). TEM and SEM were used to observe particle dispersion in the resin matrix and to investigate the fractured surface of nanocomposites for evidence of extrinsic toughening mechanism. The mechanical and thermo-mechanical properties of nanocomposites prepared from DGEBA and modified epoxide-terminated α-Fe₂O₃ were compared with the properties of untreated α-Fe₂O₃/DGEBA nanocomposites and neat DGEBA. The modified α-Fe₂O₃/DGEBA nanocomposites showed improvement in properties such as glass transition temperature (T_g) and tensile, flexural and impact strength. These improvements are due to better dispersion of epoxide-terminated α-Fe₂O₃ particles in the resin matrix and enhanced interfacial adhesion between DGEBA and α-Fe₂O₃ phases.     

Oxidative dehydrogenation of ethane by carbon dioxide over sulfate‐modified Cr2O3/SiO2 catalysts

The oxidative dehydrogenation of ethane into ethylene by carbon dioxide over unsupported Cr₂O₃, Cr₂O₃/SiO₂ and a series of Cr₂O₃/SiO₂ catalysts modified by sulfate was investigated. The results show that Cr₂O₃/SiO₂ is an effective catalyst for dehydrogenation of ethane and CO₂ in the feed promotes the catalytic activity. Sulfation of silica will influence the catalytic behavior of Cr₂O₃/SiO₂ in dehydrogenation of ethane with carbon dioxide depending on the amount of sulfate. Cr₂O₃/6 wt% SO ₄ ^2- –SiO₂ catalysts exhibit an excellent performance for this reaction, giving an ethylene yield of 55% at 67% ethane conversion at 650°C. Characterizations indicate that addition of sulfate changes the bulk and surface properties of Cr₂O₃/SiO₂, promoting the reduction of Cr⁶⁺ to Cr³⁺ and favoring the catalytic conversion. This revised version was published online in July 2006 with corrections to the Cover Date.