Preparation and characterization of nano-porous silica aerogel from rice husk ash by drying at atmospheric pressure

Silica aerogel, a mesoporous material, was prepared from rice husk ash by sol–gel method and dried under atmospheric pressure. In this method, rice husk ash, which is rich in silica, was extracted with sodium hydroxide solution to produce a sodium silicate solution. This solution was neutralized with acid to form a silica hydrosol, and a small amount of tetraethyl silicate (TEOS) to form a gel. The aged gel was washed carefully by distilled water and ethanol and finally dried under atmospheric air. The prepared silica aerogels were characterized by XRF, FT-IR, TG, DTA, DTG, XRD, BET and SEM measurements. The synthesized TEOS-doped silica aerogel was a light solid with specific surface area of 315 m²/g, pore volume 0.78 cm³/g, average pore size 9.8 nm, bulk density 0.32 g/cm³ and porosity 85%.     

Enhanced photoactivity and anatase thermal stability of silica–alumina mixed oxide additives on sol–gel nanocrystalline titania

Nanocrystalline titania with silica and silica–alumina mixed oxide as additives has been prepared through a sequential approach sol–gel method starting from titanyl sulphate in aqueous medium. The mixed oxide added titania shows increased anatase phase stability and high surface area. The complete transformation of anatase to rutile in the mixed oxide added titania occurs only above 1100 °C. The silica and silica–alumina added titania precursor even after calcination at 800 °C show specific surface area of 53 m² g^− 1 and 63 m² g^− 1 respectively. Further, the mixed oxide added titania sample shows excellent photoactivity compared to the commercially available Hombikat UV 100 titania, with respect to degradation of methylene blue. The addition of mixed oxide has resulted in better properties with respect to specific surface area, increased anatase to rutile phase transformation and photocatalytic activity of titania.     

Nanoporous carbon synthesized from sol–gel template for adsorbing gibberellic acid in aqueous solution

A novel method, based on dynamic carbonization and silica template formed by sol–gel, was developed to prepare nanoporous carbon materials with tailored pore structures. The effects of the sol–gel reaction and carbonization process on the final nanoporous carbon product were investigated by pore features such as specific surface area, the total pore volume, and pore size distribution, which were systemically characterized by iodine index, transmission electron microscopy, and nitrogen adsorption. The experimental results indicate that the pore structures of the prepared nanoporous carbon are tunable on the nano-scale by controlling the preparation process in the proposed method. The nanoporous carbon prepared under the optimal conditions has a high total pore volume of 1.26 cm³/g, a large specific surface area of 1744 m²/g, and a maximal adsorption capacity of 9.2 mg/g to gibberellic acid in aqueous solution, which is nearly 6 times that of commercial activated carbon.     

Preparation of poly(vinyl alcohol)/tin glycolate composite fibers by combined sol–gel/electrospinning techniques and their conversion to ultrafine tin oxide fibers

Ultrafine composite fibers made from poly(vinyl alcohol) (PVA)/tin glycolate — a moisture-stable tin oxide containing compound — were prepared by a combined sol–gel processing and electrospinning technique. These fibers were subsequently converted to ultrafine tin oxide fibers by calcination treatment, with the aim of producing tin oxide fiber with a high surface area-to-mass ratio and a high specific conductivity value. The acidity of spinning solution plays an important role to the morphology and size of the obtained fibers. The average diameters of the obtained composite fibers were in the range of 87–166 nm. It was found that the ultrafine tin oxide fiber showed the high conductivity value of 1.59 × 10³ S cm^?1 at calcinations temperature of 600 °C, and the BET surface area was in a range of 71 and 275 m² g^?1. Moreover, the effect of calcinations temperature on the phase and the size of the tin oxide fibers were investigated in this study.     

Morphology of ferromagnetic sol–gel submicron silica powders doped with iron and nickel particles

The sol–gel submicron spherical silica particles were obtained with the modified Stöber method using methanol. Iron and nickel dopants produced by the exploding wire method were introduced to the SiO₂ powders during the sol–gel process. The electron microscopy and laser diffraction particle size analyzer studies showed that the hybrid powders agglomerated easily in ethanol. The difference of ζ-potential in pure water between the pure silica (− 46.8 mV), the Fe-doped (− 39.7 mV) and the Ni-doped silica (− 41.5 mV) proved that doping changes the surface properties. The SEM studies confirmed that the Ni-particles could attach to the surface of the silica shells. With TEM it has been found that the differently sized Ni-particles may be encapsulated in silica shells, form clusters within silica or they may remain separate if they were larger than the silica particles. The saturation magnetization of the ferromagnetic hybrid powders was 0.81 emu/g (Fe-doped) and 0.51 emu/g (Ni-doped), while the hysteresis of magnetization revealed that the magnetic particles may have close to a single domain structure. The magnetization values and the X-ray studies confirmed that some Fe-oxides of the initial doping powder remained in the hybrid powder, while the Ni applied was nearly totally metallic.     

A facile method for the production of high-surface-area mesoporous silica gels from geothermal sludge

Mesoporous silica gels were successfully produced from geothermal sludge by alkali extraction followed by acidification. The silica in the geothermal sludge was dissolved by NaOH solution to produce a sodium silicate solution, which was then reacted with HCl or tartaric acid to produce silica gels. The effects of silica concentration and pH on the silica gel properties were investigated. In addition, an improved method was proposed by incorporating two-step aging. The first aging step, which was conducted at pH 10, was used to induce Ostwald ripening to increase the size of the primary particles, and the second step was used to strengthen the gel network. Decreasing the silica concentration by diluting the as-prepared sodium silicate solution tended to increase the surface area and pore volume of the prepared silica gels. The silica gels produced by tartaric acid possessed higher surface area and pore volume than those by HCl. The surface area and pore volume reached approximately 450 m² g⁻¹ and 0.8 cm³ g⁻¹, respectively. When the gelation pH was decreased to 6, the surface area exceeded 600 m² g⁻¹. The first aging process increased the size and uniformity of the primary particles, which in turn increased the surface area of the particles. The pore diameter for all cases was greater than 5 nm, indicating that the silica gels were mesoporous.     

In situ synthesis and luminescence characteristics of complexes of europium(III) with 4,6-diacetylresorcinol

The complexes of europium(III) with 4,6-diacetylresorcinol (H₂DAR) and a co-ligand (phen, bpy or 2,2′-bipyridine N,N′-dioxide (2,2′-bpyO₂)) were in situ synthesized in silica matrix via a two-step gel process. The formation of complexes in silica gel was confirmed by the luminescence excitation spectra. The silica gels that contain in situ synthesized europium complexes exhibit the characteristic emission bands of the Eu(III). The results show that there are two ways to enhance the emission intensity of the Eu(III): (i) synthesize the complex in silica matrix and (ii) synthesize the complex with a co-ligand, which coordinates with Eu(III) in the composite system and can efficiently transfer the energy from 4,6-diacetylresorcinol to the Eu(III). The order of the luminescence intensities of the complexes is: Eu₂(DAR)₃(phen)₂-(sol–gel) > Eu₂(DAR)₃(2,2′-bpyO₂)₂-(sol–gel) > Eu₂(DAR)₃ (bpy)₂-(sol–gel) > Eu₂(DAR)₃-(sol–gel) > pure Eu₂(DAR)₃·4H₂O.     

A facile method for production of high-purity silica xerogels from bagasse ash

In this paper, we systematically report the synthesis of mesoporous silica xerogels in high purity from bagasse ash. The bagasse ash was chosen as the raw material due to its availability and low-price, and environmental considerations also were important. Silica was extracted as sodium silicate from bagasse ash using NaOH solution. The sodium silicate was then reacted with HCl to produce silica gel. To produce high-purity silica xerogels, three different purification methods were investigated, i.e., acid treatment, ion exchange treatment, and washing with de-mineralized water. We were able to produce high-purity silica (>99 wt.%) by washing the produced gels with either de-mineralized water or with ion exchange resin. The specific surface area of the prepared silica xerogels ranged from 69 to 152 m² g^?1 and the pore volume ranged from 0.059 to 0.137 cm³ g^?1. The pore radii were 3.2–3.4 nm, which indicated that the silica xerogels was mesoporous. From the adsorption characterization, it was obvious that adsorptive capacity was better for high-purity silica xerogels compared with low-purity. The maximum adsorption capacity by high-purity silica xerogel was 0.18 g-H₂O/g-SiO₂. Finally, we demonstrate the potential of bagasse ash for mesoporous silica production with its excellent adsorptive capacity that makes it beneficial as an environmental solution.     

Synthesis of electrically active biopolymer–SiO2 nanocomposite aerogel

Silica nanoparticles encapsulated acacia gum–silica (AgSiO₂) composites were synthesized through sol–gel method using tetraethyl orthosilicate (TEOS) as silica precursor in basic condition. The nanocomposite gels were dried at different temperatures to form aerogels. The incorporation of nanostructured silica will influence the electronic behavior of composite. The composition of silica with acacia gum was tailored to optimize the material having good electronic properties. The resulting material was characterized by FTIR, XRD and AFM. The control curing of the composite resulted to mesoporous material with nanosize silica. At optimum composition, electrical conductivity and ion transference number of hybrid material are found to be 18.3 × 10^− 2 Scm^− 1 and 4.26 × 10² cm² V^− 1 s^− 1 respectively. The electrical conductivity of biopolymeric hybrid is comparable to that of commercially used synthetic conducting polymers. The ion transfer number of AgSiO₂ nanocomposites attributes the superionic character for electrical conduction.     

Application feasibility of Pb(Zr,Ti)O3 ceramics fabricated from sol–gel derived powders using titanium and zirconium alkoxides

It is believed that what may be termed the ‘Nanoscaled Century’ will lead to a new industrial revolution, particularly in terms of sol–gel methods of assembly for nanostructure devices. A propyl alcohol (1-Pro) based sol–gel chemical has been developed to replace 2-methoxyethanol (MOE), 1,1,1-tris(hydroxymethyl)ethane (THOME) for the fabrication of PbZr_0.53Ti_0.47O₃ (PZT) piezoelectric ceramics. This chemical is prepared from sol–gel derived powders that are near to the morphotropic phase boundary (MPB). The pyrochlore phase was still apparent when calcining at 900 °C with a shorter calcining time, such as 30 min. However, it disappeared for longer calcining times, for example 3 h or more. From the results of the analysis, PZT ceramics calcinations at 900 °C for 4 h, and sintering at 1100 °C for 2 h could reach a pyrochlore-free crystal phase with relative density of approximately 7.9 g/cm³—close to 98% of the theoretical value. The P–E hysteresis loop, measured by the Sawyer–Tower circuit, revealed that the remanent polarization (P_r) and coercive field (E_c) were 8.54 μC/cm² and 15.6 kV/cm, respectively. The vibration modes of the PZT ceramics were between 150 and 1.5 MHz. Morevoer, under such processing conditions the PZT piezoceramics had uniform grain size distribution less than 1 μm and zero temperature coefficient of resonant frequency (TCF). In summary, the PZT ceramics derived from the sol–gel method were confirmed to possess excellent piezoelectric properties. Furthermore, the processing temperatures were scaled down by 100–200 °C, compared to conventional oxide reaction. Finally, from an energy-saving viewpoint, this experiment can potentially make a very positive contribution.     

Rapid synthesis of ordered hexagonal mesoporous silica and their incorporation with Ag nanoparticles by solution plasma

Rapid synthesis of silica with ordered hexagonal mesopore arrangement was obtained using solution plasma process (SPP) by discharging the mixture of P123 triblock copolymer/TEOS in acid solution. SPP, moreover, was utilized for Ag nanoparticles (AgNPs) incorporation in silica framework as one-batch process using silver nitrate (AgNO₃) solution as precursor. The turbid silicate gel was clearly observed after discharge for 1 min and the white precipitate formed at 3 min. The mesopore with hexagonal arrangement and AgNPs were observed in mesoporous silica. Two regions of X-ray diffraction patterns (2θ < 2° and 2θ = 35–90°) corresponded to the mesoporous silica and Ag nanocrystal characteristics. Comparing with mesoporous silica prepared by a conventional sol–gel route, surface area and pore diameter of mesoporous silica prepared by solution plasma were observed to be larger. In addition, the increase in Ag loading resulted in the decrease in surface area with insignificant variation in the pore diameter of mesoporous silica. SPP could be successfully utilized not only to enhance gelation time but also to increase surface area and pore diameter of mesoporous silica.     

Effect of processing methods on physicochemical properties of titania nanoparticles produced from natural rutile sand

Titania (TiO₂) nanoparticles were produced from natural rutile sand using different approaches such as sol–gel, sonication and spray pyrolysis. The inexpensive titanium sulphate precursor was extracted from rutile sand by employing simple chemical method and used for the production of TiO₂ nanoparticles. Particle size, crystalline structure, surface area, morphology and band gap of the produced nanoparticles are discussed and compared with the different production methods such as sol–gel, sonication and spray pyrolysis. Mean size distribution (d₅₀) of obtained particles is 76 ± 3, 68 ± 3 and 38 ± 3 nm, respectively, for sol–gel, sonication and spray pyrolysis techniques. The band gap (3.168 < 3.215 < 3.240 eV) and surface area (36 < 60 < 103 m² g^?1) of particles are increased with decreasing particle size (76 > 68 > 38 nm), when the process methodology is changed from sol–gel to sonication and sonication to the spray pyrolysis. Among the three methods, spray pyrolysis yields high-surface particles with active semiconductor bandgap energy. The effects of concentration of the precursor, pressure and working temperature are less significant for large-scale production of TiO₂ nanoparticles from natural minerals.     

Preparation of carbon aerogel microspheres by a simple-injection emulsification method

Carbon aerogel microspheres were successfully prepared using a simple-injection emulsification method, employing sol–gel polycondensation of a resorcinol–formaldehyde solution containing sodium carbonate as a catalyst. This process was followed by solvent exchange using acetone, supercritical drying with carbon dioxide and carbonization in a nitrogen atmosphere. The effect of curing time before starting injection, injection rate and agitation rate of continuous phase on the particle size and the porous properties of the carbon aerogel microspheres was investigated. Adsorption of phenol by using the prepared carbon aerogel microspheres was also examined. The diameter of carbon aerogel microspheres was controlled in the range of 20–55 μm by varying injection rate and agitation rate. The mean diameter of carbon aerogel microspheres decreased with increasing the injection rate and the agitation rate, whereas their mean diameter was independent of the curing time. The BET surface area and total pore volume of carbon aerogel microspheres increased with increasing the curing time. In contrast, their BET surface area and total pore volume decreased with increasing the injection rate and the agitation rate. The BET surface area, total pore volume, mesopore volume and micropore volume of the carbon aerogel microspheres with a mean diameter of 45 μm were 903 m²/g, 0.60 cm³/g, 0.31 cm³/g and 0.27 cm³/g, respectively. The phenol-adsorption capacity of these carbon aerogel microspheres was 29.3 mg phenol/g adsorbent.     

A simple process for magnetic nanocrystalline porous Co–Fe alloy hollow microfibers

A simple process has been developed to fabricate the magnetic nanocrystalline porous Co–Fe alloy microfibers with a hollow structure by the sol–gel and phase transformation at a low temperature. The alloy microfibers consisting of nanoparticles about 30 nm are characterized with a fiber diameter around 0.5 μm, a ratio of the hollow diameter to the fiber diameter about 1/2 and pore sizes of 50 to 300 nm. These nanocrystalline porous Co–Fe alloy hollow microfibers have a good magnetic property, with the specific saturation magnetization of 212.8 A m² kg^?1and coercivity of 15.6 kA m^?1 at room temperature.     

Spectroscopic properties of Tm3+/Al3+ co-doped sol–gel silica glass

Tm³⁺/Al³⁺ co-doped silica glass was prepared by sol–gel method combined with high temperature sintering. Glasses with compositions of xTm₂O₃–15xAl₂O₃–(100 − 16x) SiO₂ (in mol%, x = 0.1, 0.3, 0.5, 0.8 and 1.0) were prepared. The high thulium doped silica glass was realized. Their spectroscopic parameters were calculated and analyzed by Judd–Ofelt theory. Large absorption cross section (4.65 × 10⁻²¹ cm² at 1668 nm) and stimulated emission cross section (6.00 × 10⁻²¹ cm² at 1812 nm), as well as low hydroxyl content (0.180 cm⁻¹), long fluorescence lifetime (834 μs at 1800 nm), large σ_em × τ_rad (30.05 × 10⁻²¹ cm² ms) and large relative intensity ratio of the 1.8 μm (³F₄ → ³H₆) to 1.46 (³H₄ → ³F₄) emissions (90.33) are achieved in this Tm³⁺/Al³⁺ co-doped silica glasses. According to emission characteristics, the optimum thulium doping concentration is around 0.8 mol%. The cross relaxation (CR) between ground and excited states of Tm³⁺ ions was used to explain the optimum thulium doping concentration. These results suggest that the sol–gel method is an effective way to prepare Tm³⁺ doped silica glass with high Tm³⁺ doping and prospective spectroscopic properties.     

Synthesis of hydroxyapatite nanotubes for biomedical applications

Single phase, stoichiometrically pure, hollow nanotubes of hydroxyapatite have been synthesized and single-particle analysis has been performed to successfully prove the sole formation of Ca₁₀(PO₄)₆(OH)₂ phase. The facile synthesis involves a sol–gel process under neutral conditions in the presence of a sacrifical anodic alumina template. The structures formed are hollow nanotubes that have been characterized by XRD, SEM, TEM, SAED, EELS, EDS and BET measurements. The diameter of the resulting tubes is in the range of 140–350 nm, length is on the order of a few microns and the wall thickness of the tubes was found to be ca. 30 nm. Moreover these tubes had a large BET surface area of 115 m²/g and were found to be biocompatible. They displayed inertness in the presence of NIH 3T3 mouse fibroblast cells as dictated by an MTT assay.     

Stearic acid sol–gel synthesis of ultrafine-layered K2Nd2Ti3O10 at low temperature and its acid-exchanging property

A rapid and simple method was developed to prepare ultrafine K₂Nd₂Ti₃O₁₀ powders by combustion of stearic acid precursors. The acid-exchanging properties of obtained product were also studied. Results showed that by using stearic acid sol–gel method (SAM) the fabricating temperature was lowered (from 1100 to 800 °C) and the reacting time was shortened (from at least 11 to 2 h). Comparing with the product by traditional solid-state reaction (SSR), the particle size of the K₂Nd₂Ti₃O₁₀ synthesized by SAM is smaller, BET surface area is higher (more than 16.97 m²/g), and has different acid-exchanging properties. It can be easily exfoliated in 2 mol L^− 1 HNO₃ solution and the exfoliated monodisperse sheets scrolled to 20 × 100 nm nanotubes automatically.     

Preparation of YAG gel coated ZrB2–SiC composite prepared by gelcasting and pressureless sintering

In this paper, gelcasting and pressureless sintering of YAG gel coated ZrB₂–SiC (YZS) composite were conducted. YAG gel coated ZrB₂–SiC (YZS) suspension was firstly prepared through sol–gel route. Poly (acrylic acid) was used as dispersant. YZS suspension had the lowest viscosity when using 0.6 wt.% PAA as dispersant. Gelcasting was conducted based on AM–MBAM system. The gelcast YZS sample was then pressureless sintered to about 97% density. During sintering, YAG promoted the densification process from solid state sintering to liquid phase sintering. The average grain sizes of ZrB₂ and SiC in the YZS composite were 3.8 and 1.3 μm, respectively. The flexural strength, fracture toughness and microhardness were 375 ± 37 MPa, 4.13 ± 0.45 MPa m^1/2 and 14.1 ± 0.5 GPa, respectively.     

Comparison of electrochemical performances of LiFePO4/C composite materials by two preparation routes

This study reports on the preparation of LiFePO₄/C composite materials prepared by the hydrothermal and sol–gel processes for comparison. The synthesis condition on the hydrothermal process was performed at 170 °C for 19 h. The polystyrene (PS) polymer was used as a carbon source; the PS was added at a range of 0–5 wt.%. The temperature of the post-thermal process was set at 750–850 °C. The citric acid (denoted as CA) was used as the reducing agent and the carbon source in the sol–gel process. The temperatures of the sintering process were set at a range of 650–850 °C. The optimal sintering temperature was at 850 °C for 12 h in the hydrothermal process; the optimal carbon residue content was approximately 3.20 wt.%. It was revealed that the highest discharge capacity of LiFePO₄/C composites by the hydrothermal process at 0.1 C is 163 mAh g^?1. The optimal sintering temperature was found to be at 750 °C for the sol–gel process. The highest carbon content was approximately 11.94 wt.% as the molar ratio of CA is 1.0. The highest discharge capacity of LiFePO₄/C composites by the sol–gel process at 0.1 C was approximately 130.35 mAh g^?1.     

Potentiometric urea biosensor based on multi-walled carbon nanotubes (MWCNTs)/silica composite material

A novel potentiometric urea biosensor has been fabricated with urease (Urs) immobilized multi-walled carbon nanotubes (MWCNTs) embedded in silica matrix deposited on the surface of indium tin oxide (ITO) coated glass plate. The enzyme Urs was covalently linked with the exposed free –COOH groups of functionalized MWCNTs (F-MWCNTs), which are subsequently incorporated within the silica matrix by sol–gel method. The Urs/MWCNTs/SiO₂/ITO composite modified electrode was characterized by Fourier transform infrared (FTIR) spectroscopy, thermal gravimetric analysis (TGA) and UV–visible spectroscopy. The morphologies and electrochemical performance of the modified Urs/MWCNTs/SiO₂/ITO electrode have been investigated by scanning electron microscopy (SEM) and potentiometric method, respectively. The synergistic effect of silica matrix, F-MWCNTs and biocompatibility of Urs/MWCNTs/SiO₂ made the biosensor to have the excellent electro catalytic activity and high stability. The resulting biosensor exhibits a good response performance to urea detection with a wide linear range from 2.18 × 10^? 5 to 1.07 × 10^? 3 M urea. The biosensor shows a short response time of 10–25 s and a high sensitivity of 23 mV/decade/cm².