Synthesis of LiNiPO4 via citrate sol–gel route

Journal of Sol-Gel Science and Technology - In this paper, LiNiPO4 powders were prepared by sol gel method using citric acid as chelating agent. The article investigated the effect of annealing...     

Synthesis and sol–gel assembly of nanophosphors

Some recent works made in our group on inorganic nanophosphors are briefly reviewed in this paper. We first present the synthesis of highly concentrated semiconductor quantum dot colloids allowing the extension of the well-known oxide sol–gel process to chalcogenide compounds. Secondly, we show the synthesis and the chemical functionalization of lanthanide-doped insulator nanoparticles. In particular, the annealing process of these particles at high temperature leads to highly bright nanocrystals, which can be used as biological luminescent labels or for integration in transparent luminescent coatings. Finally, we consider luminescent transition metal clusters, which combine the inorganic structure of nanoparticles with the monodispersity and the easy functionalization of the organic molecules. Emphasis is put on the original thermochromic luminescence properties of copper iodide clusters trapped in siloxane-based films.     

Synthesis and characterization of silica xerogels obtained via fast sol–gel process

The synthesis and physical properties of high surface area silica xerogels obtained by a two-step sol–gel process in the absence of supercritical conditions are reported. The hydrolysis and condensation reactions were followed by infrared spectroscopy. The increment in the bands corresponding to silanol and hydroxyl groups suggests that the hydrolysis reaction was complete during the first 30 min. The effect on surface area and global reaction time under various reaction conditions, such as type of alkaline catalyst and solvents, water–monomer and solvent–monomer molar ratios, was also studied. The obtained results suggest that surface area was increased using 3-aminopropyltriethoxysilane as catalyst. The use of isopropyl alcohol as solvent promotes the reduction of the capillary stress, giving a well-structured xerogel. As a conclusion, with H₂O/i-PrOH/TEOS in a molar ratio of 10:4:1, it was possible to obtain silica xerogels with surface areas about 1,240 m²/g. Such surface areas are comparable with those obtained under supercritical conditions (aerogels), and higher than those xerogels conventionally obtained under normal condition (500–800 m²/g).     

Synthesis of MCM-48 from silatrane via sol–gel process

High-quality cubic MCM-48 is successfully synthesized using a new silica source known as silatrane and cetyltrimethylammonium bromide (CTAB) as the structure-directing agent via sol–gel process. The effects of synthesis parameters, viz. crystallization temperature, crystallization time, surfactant concentration, quantity of NaOH, and silica source, on the product structure are investigated. The synthesized samples are characterized using X-ray diffractometer (XRD), N₂ adsorption–desorption isotherms, and electron microscopy. Optimally, this product is synthesized from samples crystallized at 140°C for 16 h with a CTAB/SiO₂ ratio of 0.3 and NaOH/SiO₂ ratio of 0.5. The XRD result exhibits a well-resolved pattern, corresponding to the Ia3d space group of MCM-48. The BET surface area of this product is as high as 1,300 m²/g with a narrow pore-size distribution of 2.86 nm. The scanning electron microscopic (SEM) images also show the truncated octahedral shape and well-ordered pore system of MCM-48 particles.     

Synthesis and characterization of sol–gel alumina nanofibers

Abstract Alumina nanofibers of high aspect ratio with surface area of >300 m² g⁻¹ has been prepared successfully in bulk quantities by the sol–gel method. The synthesis parameters including the binary water–alcohol solvent system to aluminium isopropoxide ratio, pH, type of solvent and aging temperature affect the uniformity and formation of nanofibers. It is proposed that alumina nanofibers were formed by the curling of the nanosheets upon condensation after the hydrolysis. The phase evolution of alumina nanofibers from pseudoboehmite to α phase has been shown by XRD and FTIR. ²⁷Al NMR investigations show that the Al atoms are six and four coordinated. The morphology of the alumina nanofibers does not change much as the calcination temperature was increased. In addition, the average pore size increases and the BET surface area decreases as a function of calcination temperature. The thermal behavior of alumina nanofibers was investigated by TGA. Graphical Abstract      

Synthesis of nanostructural Yttrium fluorosilicate glass ceramic via sol–gel method

Journal of Sol-Gel Science and Technology - The yttrium fluorosilicate glass ceramic pieces were prepared by sol–gel method starting from yttrium acetate, trifluoroacetic acid, and...     

Optical spectroscopy methods for the characterization of sol–gel materials

Journal of Sol-Gel Science and Technology - In this paper, structural, optical, and electrical features of undoped and copper-incorporated nickel oxide (Cu/NiO) films with different mole ratios...     

Synthesis of a dysprosium aluminum garnet nanopowder via sol–gel method

A dysprosium aluminum garnet (DAG) nanopowder was synthesized by aqueous sol–gel method using Al powder, HCl and Dy(CH₃COO)₃·4H₂O as raw materials. The dried amorphous gel was heat treated in the range of 800–1,200 °C. The influence of heat treatment on crystallization and phase transformation of the dried gel was investigated using X-ray diffractometery, scanning electron microscopy, thermogravimetry and differential thermal analysis and Fourier transform infrared spectroscopy. It was shown that the gel calcined from 900 to 1,200 °C resulted in the formation of a crystalline DAG nanopowder with particle size distribution ranges from 26 to 98 nm.     

Synthesis of ultrafine MgFe2O4 nanofibers via electrospining using sol–gel precursor

In the present study, MgFe₂O₄ nanofibers with smaller diameter have been successfully fabricated via electrospinning utilizing sol–gel precursor. The single phase of spinel ferrite was obtained at 700 °C. Different PVP concentrations were used and the results show that PVP concentration had played important role in the formation, uniformity, homogeneity and particularly in the reduction of nanofibers diameter. The average diameter of the nanofibers prepared with PVP concentration (6.3, 7.6, and 8.9 wt%) and calcined at 700 °C were 70 ± 7.6, 86 ± 11 and 113 ± 13 nm respectively.     

Comparative study of the thermal behavior of Sr–Cu–O gels obtained by sol–gel and microwave-assisted sol–gel method

Journal of Thermal Analysis and Calorimetry - In the literature data, several papers reported the synthesis by various chemical or physical methods of the SrCu2O2 (SCO) having possible applications...     

Synthesis of MgB4O7 and Li2B4O7 crystals by proteic sol–gel and Pechini methods

Journal of Sol-Gel Science and Technology - Magnesium-tetraborates and lithium-tetraborates are excellent detectors for ionizing radiation. However, manufacturing these crystalline structures is...     

Synthesis of titanium dioxide nano-powder via sol–gel method at ambient temperature

Titanium dioxide is a semiconductor with excellent photo catalytic properties and an important material with high regarded in nanotechnology. In this study, titanium dioxide nanoparticles was successfully synthesized via sol–gel method using tetra-n-butyl orthotitanate, hydrochloric acid and ammonia. Tetra-n-butyl orthotitanate was used as precursor. The ingredients were mixed at ambient temperature for 9 h on a magnetic stirring, sol was formed and converted to gel by adding ammonia. X-ray diffraction analysis clearly showed anatase and rutile phases so that, with increasing calcination temperature anatase converts to the rutile. Scanning electron microscopy was used for agglomerate observations. Energy-dispersive detector analysis was carried out and confirmed the formation of titanium dioxide. The influences of calcination temperature and pH value on particles size were studied. The results indicate that synthesis at room temperature reduced the particle size to 15 nm.     

Synthesis and characterization of titania/MQ silicone resin hybrid nanocomposite via sol–gel process

Inorganic–organic hybrid materials were prepared via an aqueous sol–gel technique from tetra-n-butyl titanate as the precursor of titania, in the presence of MQ silicone resin. The samples were characterized by FT–IR, UV–Vis, DSC, TGA, SEM and XRD. It was illustrated that the Ti–O–Si covalent bonds had formed in the hybrid nanocomposite which were highly transparent in visible light region, and yet had high absorption in UV light range. The thermal stability of the hybrid materials was gradually improved with the increase of titania content. It was concluded that the hybrid material which particle size was around 50 nm were amorphous when the crystallization of titania was retarded by MQ silicone resin.     

Synthesis and characterization of an aliphatic monoimide-bridged polysilsesquioxane by the sol–gel route

Based on differential scanning calorimetry data, it was shown that the reaction of (3-triethoxysilylpropyl)succinic anhydride and (3-amino)propyltriethoxysilane at 110 °C resulted in the formation of polyamic acid, whereas the thermal treatment at 220 °C led to the generation of an aliphatic monoimide-bridged polysilsesquioxane as proved by FT-IR. X-ray powder diffraction studies showed a prominent reflection at 2θ = 6.66° (d = 1.32 nm) revealing that a crystalline area is formed. ²⁹Si CP-MAS-NMR and ¹³C CP-TOSS-MAS-NMR measurements proved that no cleavage of the Si–C bond occurred, and a highly condensed material was obtained.     

Synthesis and characterization of SiO2–CrO3, SiO2–MoO3, and SiO2–WO3 mixed oxides produced using the non-hydrolytic sol–gel process

Silica-based mixed oxide xerogels, namely SiO₂–CrO₃, SiO₂–MoO₃, and SiO₂–WO₃, were prepared using the non-hydrolytic sol–gel process. The materials were synthesized using metal chloride:tetraethoxysilane (TEOS) molar ratios of 0.1:2; 0.2:2 and 0.4:2 for each metal chloride and 1:2 SiCl₄:TEOS molar ratio. All of the xerogels containing Cr, Mo or W had considerably greater surface areas than that of SiO₂. The small angle X-ray scattering experiments suggest that the surface roughness of the aggregates in SiO₂–CrO₃ is less than that of SiO₂–MoO₃ and SiO₂–WO₃. The morphological characteristics of the silica-based mixed oxide xerogels were not affected by the nature and amount of metal chloride employed in the synthesis. An irregular morphology was observed for SiO₂–CrO₃, SiO₂–MoO₃ and SiO₂–WO₃, but a lamellar structure was observed for SiO₂. X-ray photoelectron spectroscopy analysis suggests that tungsten species were preferentially distributed on the outmost part of the grain. The resulting particle diameter was shown to be lower for the mixed oxides compared to that of bare silica. Furthermore, the presence of metals (Cr, Mo and W) on silica caused a decrease in the size of the particles as the atomic radii of these metals increased. According to the Fourier transform infrared spectroscopy and Raman, Cr, Mo and W were incorporated within the silica framework.     

Synthesis and characterization of lead oxide nano-powders by sol–gel method

Our goal in this research was to obtain lead oxide nano-powders by sol–gel method. In this method, lead oxide nano-powders were synthesized through the reaction of citric acid (C₆H₇O₈·H₂O) solution and lead acetate [Pb(C₂H₃O₂)₂] solution as stabilizer and precursor, respectively. The effect of different parameters including calcination temperature, (molar ratio of citric acid to lead acetate) and drying conditions were investigated. The prepared lead oxide nano-powders were characterized by FT-IR spectroscopy, X-ray diffraction, thermogravimetric analysis and scanning electron microscopy. The prepared PbO samples consist of the particles in the range of 50–120 nm or the thick plate like structures with thickness of 53 nm depending on the drying conditions.