Preparation and characterization of (metal, nitrogen)-codoped TiO_2 by TiCl_4 sol-gel auto-igniting synthesis

The nitrogen-doped and （metal, nitrogen）-codoped TiO2 photocatalysts （metal = Ag, Ce, Fe, La） were synthesized by sol-gel auto-igniting synthesis （SAS） with the complex compound sol of TiCl4-NH4NO3-citri acid-metal nitrate- NH3.H20 as a precursor. The products were characterized by means of XRD, XPS, and UV-Vis diffuse reflectance spectra, and their photocatalytic activity was investigated under visible light. It was found that all the synthesized powders showed good absorption for visible light, and that the radius and alterable valence states of doping metallic cations played important roles on their photocatalytic activity. These results were discussed in detail.

Synthesis, Characterization and Optical Morphology of ZnO Nanoparticles

The ZnO molecule plays an important role in the industry due to it special features, anti-corrosion anti-bacterial properties, as well as due to its low electrical conductivity and heat resistance. In these experimental researches, the sol-gel method was chosen, which enables control of nucleation, aging and growth of particles in the solution. ZnO synthesis was prepared utilizing chemical method with Zinc acetate dyhidrate and NaOH with the appropriate methanol solvent and heating (60˚C). The methods used in identification and characterization are FTIR, UV/VIS, OPTICAL MICROSCOPY, SEM and XRD. The FTIR spectra of synthesized ZnO with corresponding ones show characteristic bands at the corresponding wavelengths, which confirm the presence of ZnO nanoparticles. SEM characterization of ZnO shows the morphology of needle-shaped nanoparticles. XRD spectar in this research by chemical method indicates the particle size of 17.76 nm.

Enhanced photocatalytic activity of (La, N) co-doped TiO_2 by TiCl_4 sol-gel autoigniting synthesis

（La, N） co-doped TiO2 photocatalysts were synthesized using TiC14 sol-gel autoignidng synthesis （SAS） starting from a complex compound system of TiCl4-La（NO3）3-citric acid-NH4NO3-NHyH2O, in which the （La, N） co-doped process was accompushed in the formation of TiO2 nanocrystals. The prepared samples were characterized by using X-ray diffraction （XRD）, X-ray photoemission spectroscopy （XPS） and UV-vis diffuse reflectance spectra. The results indicated that nitrogen and lanthanum were incorporated into the lattice and interstices of titania nanocrystals, which resulted in narrowing the band gap and promoting the separation of photoexcited hole-electron pairs, respectively, and showing expected red-shifts and enhanced photocatalytic activity under visible light. The mechanism on nitrogen doping and enhancement in photocatalyfic activity of （La, N） co-doped titania by SAS was discussed in detail.

Novel Synthesis of Sol-gel Derived Nanosized Mullite Powder

Using hydrous aluminum chloride （AlCl3·6H2O） and silicon ethoxide （Si （OC2H5）4） as raw materials, a kind of nano-sized mullite powder was synthesized with the sol-gel process at the medium calcination temperature. The microstructures of the alumina-silica binary aerogel and calcined nano-sized materials were investigated by means of thermogravimetry-differential thermal analysis （TG-DTA）, scanning electron microscopy （SEM） and X-ray diffractometer （XRD）. The results show that the mullitization of Al2O3-SiO2 in gel starts from about 1 000℃ and its formation ofmullite takes place in the range of 1 100℃-1 250 ℃. The size of the nano-sized mullite powder calcined at 1 250 ℃ is measured to be about 30 nm.

Synthesis of NiMoO_4 nanoparticles by sol-gel method and their structural,morphological,optical,magnetic and photocatlytic properties

Nickel molybdate(NiMoO4)nanoparticles(NPs)were synthesized by sol-gel method.Utilizing water as solvent providescrystalline nanostructures.These nanocrystals were structurally characterized by X-ray diffraction,energy dispersive X-ray analysis(EDX),and Fourier transform infrared spectra.Compositional stoichiometry was confirmed by EDX technique.The size and shapewere observed by scanning electron microscopy(SEM)and transmission electron microscope(TEM).It was found that the obtainedNPs were pure and single phase crystalline with monoclinic structure.The optical properties were studied by ultraviolet-visiblediffuse reflectance spectroscopy(UV-Vis-DRS)and photoluminescence(PL)measurements at room temperature.The magneticproperties were studied by vibrating sample magnetometer(VSM)and results showed superparamagnetic behavior of the obtainednanoparticles.Photocatalytic activity of NiMoO4was studied.The photocatalytic activity of NiMoO4was enhanced with the additionof TiO2.The catalysts NiMoO4,TiO2and NiMoO4-TiO2nanocomposites(NC)were tested for photocatalytic degradation(PCD)of4-chlorophenol(4-CP).It was found that PCD efficiency of NiMoO4-TiO2NC was higher than that of pure NiMoO4and TiO2.

Synthesis and Structure Transformation of Orthorhombic LiMnO2 Cathode Materials by Sol-gel Method

Orthorhombic LiMnO2 cathode materials were synthesized successfully at lower temperature by sol-gel method. When LiMnO2 precursor prepared by sol-gel method was fired in air, the product was a mixture of spinel structure LiMn2O4 and rock-salt structure Li2MnO3, whereas in argon single-phase orthorhombic LiMnO2 could obtain at the range of 750℃ to 920℃. The substitution of Mn by Zn2+ or Co3+ in LiMnO2 led to the structure of LiMnO2 transiting to Qα-LiFeO2. The results of electrochemical cycles indicated that the discharged capacity of orthorhombic-LiMnO2 was smaller at the initial stages, then gradually increased with the increasing of cycle number, finally the capacity stabilized to certain value after about 10th cycles. This phenomenon reveals that there is an activation process for orthorhombic LiMnO2 cathode materials during electrochemical cycles, which is a phase transition process from orthorhombic LiMnO2 to tetragonal spinel Li2Mn2O4. The capacity of orthorhombic LiMnO2 synthesized at lower temperature is larger than that synthesized at high temperature.

Green Synthesis of Titanium Oxide Nanoparticles Using Natural Extracts

Green synthesis is an alternative method for obtaining nanoparticles for environmentally friendly purposes. The present work describes the synthesis and characterization of titanium oxide nanoparticles, starting from three natural sources: orange peel, hibiscus rosa sinensis and Aloe vera. Titanium (IV) tetrabutoxide in ethanol solution was used as precursor. The methodology used was based on the sol-gel technique, through which TiO2 nanoparticles were obtained in the anatase phase. The characterization of the nanoparticles was carried out by means of x-ray diffraction (XRD), scanning electron microscopy (SEM) and infrared spectrophotometry (FTIR), which allowed the identification of a good degree of purity and crystallinity of the samples obtained.

In-Situ Synthesis of Terbium Complex with Salicylic Acid in Silica Matrix by a Two-Step Sol-Gel Process

A process for in situ synthesis of terbium complex with salicylic acid by a two-step solgel method in silica matrix has been proposed. The luminescence properties of the silica gelscodoped with terbium and salicylic acid have also been discussed with respect to that of the geldoped with terbium and that of pure terbium complex with salicylic acid.

Synthesis and Luminescence Properties of Ternary Europium Complexes inTitania Matrix in the Presence of Dimethylformamide by a Sol-Gel Process

In-situ synthesis of ternary europium complex with thenoyltrifluoacetone (TTA) and 1,10-phenanthroline (phen) in titania matrix in the presence of dimethylformamide (DMF) by a sol-gel process was described, which was confirmed by the luminescence excitation spectra and infrared spectra. The titania gel that contains europium complex exhibits Eu3+ characteristic emission bands and presents a longer fluorescence lifetime than the pure complexes dissolved in ethanol solution. The concentration effect on the luminescence intensity was also investigated.

Multilayer Membranes Based on Ceramic Materials——Sol-gel Synthesis,Characterization and Membrane Performance

In nearly all chemical and petrochemical systems, separation of products generally accounts for more than 50% of the capital cost and the greatest part of the energy consumption. It is generally believed that membrane systems can offer benefits in both reducing the energy consumption of the separation stages and lowering the capital expenditure （CAPEX）. Microporous ceramic membranes have the potential to overcome the limitation in polymer membranes operation, which has been the subject of a large amount of research worldwide in the last two decades. And most of the research has aimed at the production of the asymmetric multilayered membrane based on amorphous oxides by sol-gel techniques. The paper is to give an overview of publications on ceramic membranes, including less common materials of titania, zirconia, which can be used for pervaporation in corrosive media. Commercially available microporous membranes based on these membrane materials and the membrane economics are also summarized.

Facile and Controlled Synthesis of Silica Sol Nanospheres Through a Modifi ed Sol-Gel Process

An effective and reproducible preparation of silica sol nanospheres via a modified sol-gel process has been described. Monodisperse and stable silica sol nanospheres with uniformsize were successfully obtained through the optimized synthesis in which the mixture of tetraethyl orthosilicate （TEOS） and ethanol was followed by the addition of water and ammonium hydroxide （NH3） separately, and the size of silica sol spheres was strictly controlled in the range of 25-119 nm with a narrow size distribution by fine adjustment of several reaction parameters. Results showed that in the presence of low concentration of TEOS, spheres size rose first and reached maximum when H2O concentration was up to 66 g/L. However, the diameter of silica sol spheres decreased above 66 g/L of H2O concentration. Furthermore, it was also found that the size and size distribution of silica sol nanospheres were affected by NH3 concentration. As NH3 concentration increased from 15 to 35 g/L, the diameter declined from 83 to 64 nm. Nevertheless, higher NH3 concentration would result in relatively broad size distribution, and gelation occurred when NH3 concentration reached 44 g/L. In addition, the effect of the different feed rates ofNH3 on the size growth of silica sol nanospheres was also discussed.

Preparation and densification of BaTiO_3 nanopowder by sol-gel autoigniting synthesis

Autoigniting synthesis of gel from Ba(NO_3)_2, TiO(NO_3)_2 and C_6H_8O_7centre dot H_2O aqueous solution was investigated at an initial temperature of 600 deg C andtetragonal BaTiO_3 nanopowder with particle size of 80nm was prepared. It is indicated that thespecific surface area of the combustion product before and after calcinations is 14.74 m^2/g and12.49 m^2/g, respectively. The combustion wave is composed of solid phase reaction zone and gaseousphase flame reaction zone. The combustion flame temperature is 1 123 K derived from thermocouplemeasurement. The characteristics and densification behavior of the sol-gel autoigniting synthesizedBaTiO_3 nanopowder were investigated.

SYNTHESIS OF MeO-SiO_2:Eu^(3+),Bi^(3+)LUMINOPUORS BY THE SOL-GEL METHOD AND A STUDY OF THEIR LUMINESCENCE SPECTRA

The luminophors MeO-SiO_2:Eu^(3+),Bi^(3+)and MeO-SiO_2Bi^(3+)(Me=Mg.Sr)were synthesized at relatively lower temperature by the sol-gel method using the silica sol as a source of silica.The optimum composition and synthesis conditions were obtained by studying the excitation and emission spectra and the effects of energy transfer from the Bi^(3+)ions to the Eu^(3+)ions.

Elaboration of an Easy Aqueous Sol-Gel Method for the Synthesis of Micro- and Mesoporous <i>γ</i>-Al₂O₃Supports

An aqueous sol-gel method for the synthesis of γ-Al2O3 supports has been developed for the use in tar reforming applications. It was determined the influences of two different aluminum precursors (aluminum sec-butoxide (Al[OCH(CH3)CH2CH3]3) and aluminum nitrate (Al(NO3)3)) on the textural and crystallographic properties of Al2O3 supports. Only the formation of γ-Al2O3 is aimed in order to use these alumina materials as catalytic supports, because it presents high specific surface area and pore volume values. Additionally, the synthesis of γ-Al2O3 was realized with the use of a functionalized silicon precursor, [3-(2-aminoethylamino)propyl]trimethoxysilane, called EDAS. By the presence of an ethylenediamine group in this molecule, it is possible to chelate metallic ions and to highly increase their dispersion at a molecular level during the synthesis of metallic catalysts supported on alumina, which is an asset for catalytic applications. So it was developed a synthesis sol-gel procedure for the cogelation between the functionalized silicon alkoxide EDAS and alumina precursor. The alumina supports synthesized with Al(NO3)3 as precursor presented higher porous values than the ones obtained with aluminium sec-butoxide precursor. Since nitrate salts are much easier to handle than alkoxides, these observations allowed validating Al(NO3)3 as aluminum source for the future synthesis procedures for metallic catalysts supported on alumina.

Structure,morphology and opto-magnetic properties of Bi_2MoO_6 nano-photocatalyst synthesized by sol-gel method

Bismuth molybdate （Bi2MoO6） nano-particles （NPs） were synthesized using bismuth nitrate, ammonium molybdate, citric acid and ethyl cellulose by a simple sol-gel method. The structure, morphology, opto-magnetic and photocatalytic properties of the obtained powder were characterized by X-ray diffraction （XRD）, Fourier transform infrared （FT-IR） spectra, high resolution scanning electron microscopy （HRSEM）, energy dispersive X-ray （EDX）, ultraviolet-visible diffuse reflectance spectra （DRS）, photoluminescence （PL） spectra and vibrating sample magnetometer （VSM） techniques. The XRD, FT-IR and EDX results indicate that the resultant powder is pure and single phase crystalline Bi2MoO6 with orthorhombic structure. The HRSEM image shows that the morphology of obtained powder consists with well defined nano-particles structure. The VSM results show superparamagnetic behavior of the obtained nano-particles. The photocatalytic activity of Bi2MoO6 nano-particles was performed. The addition of TiO2 catalyst enhances the photocatalytic activity of Bi2MoO6 nano-particles. The catalysts Bi2MoO6, TiO2 and mixed oxide catalyst Bi2MoO6-TiO2 nano-composites （NCs） were tested for the photocatalytic degradation （PCD） of 4-chlorophenol （4-CP）. It is found that the PCD efficiency of Bi2MoO6-TiO2 NCs is higher than that of pure Bi2MoO6 and TiO2 catalysts.

Synthesis and characterization of multiwall carbon nanotubes/alumina nanohybrid-supported cobalt catalyst in Fischer-Tropsch synthesis

Multiwall carbon nanotubes （MWNTs） and alumina are combined to give a new type of nanohybrid for Fisher-Tropsch synthesis （FTS） catalyst support. Alumina nano-particles （10 wt%） were introduced directly on functionalized MWNTs by a modified sol-gel method. Microstructure observations show that alumina particles were homogeneously dispersed on the inside and outside of modified MWNTs surfaces. 15 wt% cobalt loading catalysts were prepared with this nanohybrid and γ-alumina as a reference, using a sol-gel technique and wet impregnation method respectively. These catalysts were characterized by TEM, XRD, N2-adsorption, H2 chemisorption and TPR. The deposition of cobalt nanoparticles synthesized by sol-gel technique on the MWNTs nanohybrid shift the reduction peaks to a low temperature, indicating higher reducibility for uniform cobalt particles. Nanohybrid also aided in high dispersion of metal clusters and high stability and performance of catalyst. The proposed MWNTs nanohybrid-supported cobalt catalysts showed the improved FTS rate （gHc/（gcat.min））, CO conversion （%）, and water gas shift rate （WGS）（gcoz/（gcat.h）） of 0.012, 52, and 30E-3, respectively, as compared to those of 0.007, 25, and 18E-3, respectively, on the γ-alumina-supported cobalt catalysts with the same Co loading.

Synthesis and structural characterization of macroporous bioactive glass

Porous sol-gel glass of CaO-SiO2-P2O5 system with macropores larger than 100 μm was prepared by adding stearic acid as pore former when the sintering was carried out at 700 ℃ for 3h.The sol-gel porous glass shows an amorphous structure. The diameter of the pore created by pore former varies from 100 to 300 μm, and macroporous glass has a narrow and small pore size distribution in mesoporous scale. The porosity and pore size of macroporous bioactive glass can be controlled.

Synthesis and Characterization of Nanoscale Mullite Powder

Nanoscale mullite powder were synthesized via Sol-gel-SCFD and middle temperature treatment by using AIP( aluminum-isopropoxde) and TEOS ( tetraethyl orthosili-cate) as starting materials. Both of the binary aerogel of alumina-silica and calcined nanoscale materials were investigated by using TG-DSC ( thermogravimetry-differentialscanning calorimeter) , TEM( transmission electron microscope) , XRD(X-Ray diffractometer ) and specific surfacearea and porosimetry. TG-DSC indicated the removal of most of the volatiles, i.e. 15.98% up to about 700℃ ,and in the DSC curve , existence of two exothermic peak atabout 445℃ and 1015℃ may be due to the crystallizationof Si-O-Al-O in diphasic gels and mullitization and a small endothermic peak at about 805℃ indicated the decomposition of structural water molecules . On the colligation of the results of TG-DSC, XRD and TEM, the beginning temperature of mullitization in Al2O3-SiO2 aerogel system can be confirmed at about 1015℃. XRD results also showed the formation of mullite at the range 1100-1200℃. TEM and surface area and porosimetry results showed that the nanosized mullite were calcinated at 1100and 1200℃ exhibited size 30 nm and 50 nm, specific surface area 138.91 m2/g and 95.81 m2/g.

Effect of Mn Promoter on Structure and Performance of K-Co-Mo Catalyst for Synthesis of Higher Alcohols from CO Hydrogenation

A series of Mn-doped K-Co-Mo catalysts were prepared by a sol-gel method. The catalyst structure was well characterized by X-ray diffraction, N2 physisorption, NH3 temperature- programmed adsorption, in situ diffuse reflectance infrared Fourier transform spectroscopy, and X-ray absorption fine structure spectroscopy. The catalytic performance for higher alcohol synthesis from syngas was measured. It was found that the Mn-doped catalysts ex- hibited a much higher activity as compared to the unpromoted catalyst, and in particular the C2＋ alcohol selectivity increased significantly. The distribution of alcohol products de- viated from the Anderson-Schulz-Flory law. The portion of methanol in total alcohol was suppressed remarkably and the ethanol became the predominant product. Characterization results indicated that the incorporation of Mn enhanced the interaction of Co and Mo and thus led to the formation of Co-Mo-O species, which was regarded as the active site for the alcohol synthesis. Secondly, the presence of Mn reduced the amount of strong acid sites significantly and meanwhile promoted the formation of weak acid sites, which had a positive effect on the synthesis of alcohol. Furthermore, it was found that the incorporation of Mn can enhance the adsorption of linear- and bridge-type CO significantly, which contributed to the formation of alcohol and growth of carbon chain and thus increased the selectivity to C2＋OH.

Synthesis of Tenoltrifluoroacetone Composite Doped with Terbium, Dysprosium and Europium Encapsulated in Silica Oxide Matrix

The synthesis of the thenoyltrifluoroacetone compound doped with terbium, dysprosium and europium encapsulated in a silica matrix (TTA:Tb:Dy:Eu@SiO2) were performed by the sol-gel method. The precursors to obtain the vitreous phase (SiO2) were: Tetraethylorthosilicate (TEOS, C8H2O4Si, 98%, Aldrich), and ethyl alcohol (CH3CH2OH, 99.5%, Meyer), distilled water and 0.05 ml of hydrochloric acid (HCl, Meyer). The sample with molar ratio 20:80 TTA:Tb:Dy:Eu@SiO2 has the best emission intensity. Thermogravimetric analysis (TGA) shown that silica encapsulated samples decompose at lower temperatures than pure TTA:Tb:Dy:Eu luminescent material. Fourier Transform Infrared (IR-TF) shown the characteristic Si-O-Si bands that are presented at a wavelength of 1049, 853 and 440 cm-1 confirming that the luminescent material is encapsulated in a silica matrix, finally X-ray diffraction (XRD) shown that TTA:Tb:Dy:Eu@SiO2 composite is amorphous.