scholarly journals Physicochemical Characterization and Drug Release Properties of Methyl-Substituted Silica Xerogels Made Using Sol–Gel Process

2021 ◽  
Vol 22 (17) ◽  
pp. 9197
Author(s):  
Adél Len ◽  
Giuseppe Paladini ◽  
Loránd Románszki ◽  
Ana-Maria Putz ◽  
László Almásy ◽  
...  

In this work, a multi-analytical approach involving nitrogen porosimetry, small angle neutron and X-ray scattering, Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopies, X-ray diffraction, thermal analysis and electron microscopy was applied to organically modified silica-based xerogels obtained through the sol–gel process. Starting from a tetraethoxysilane (TEOS) precursor, methyltriethoxysilane (MTES) was added to the reaction mixture at two different pH values (2.0 and 4.5) producing hybrid xerogels with different TEOS/MTES molar ratios. Significant differences in the structure were revealed in terms of the chemical composition of the silica network, hydrophilic/hydrophobic profile, particle dimension, pore shape/size and surface characteristics. The combined use of structural characterization methods allowed us to reveal a relation between the cavity dimensions, the synthesis pH value and the grade of methyl substitution. The effect of the structural properties on the controlled Captopril release efficiency has also been tested. This knowledge facilitates tailoring the pore network for specific usage in biological/medical applications. Knowledge on structural aspects, as reported in this work, represents a key starting point for the production of high-performance silica-based hybrid materials showing enhanced efficacy compared to bare silica prepared using only TEOS.

Materials ◽  
2020 ◽  
Vol 13 (1) ◽  
pp. 227 ◽  
Author(s):  
Zrinka Švagelj ◽  
Vilko Mandić ◽  
Lidija Ćurković ◽  
Martina Biošić ◽  
Irena Žmak ◽  
...  

In the present work, alumina (Al2O3) foam was prepared by the replica method where a polyurethane (PU) foam (30 pores per inch (ppi)) template was impregnated with a 60 wt.% Al2O3 suspension. Sintered Al2O3 foam was used as substrate for the deposition of sol-gel derived titania (TiO2) film using dip coating. For the preparation of TiO2 sol, titanium(IV) isopropoxide (Ti-iPrOH) was used as the precursor. The common problem of qualification and quantification of a crystalline coating on a highly porous 3D substrate with an uneven surface was addressed using a combination of different structural characterization methods. Using Powder X-ray Diffraction (PXRD) and synchrotron Grazing Incidence X-ray Diffraction (GIXRD) on bulk and powdered Al2O3 foam and TiO2-coated Al2O3 foam samples, it was determined Al2O3 foam crystallizes to corundum and coating to anatase, which was also confirmed by Fourier Transformed Infrared Spectroscopy (FTIR). Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM/EDS) revealed the structural and microstructural properties of the substrate and coating. Differential Thermal Analysis (DTA) and Thermogravimetric Analysis (TGA) were used to clarify the evolution of the porous microstructure. The Al2O3-TiO2 composite was evaluated as a photocatalyst candidate for the degradation of the micropollutant medication memantine. The degradation rate was monitored using a light-emitting diode (LED) lamp operating at electromagnetic (EM) wavelength of 365 nm. The photocatalytic activity of sol-gel-derived TiO2 film immobilized on the Al2O3 foam was compared with commercially available TiO2 nanoparticles, P25-Degussa, in the form of a suspension. The levels of memantine were monitored by High-Performance Liquid Chromatography–Tandem Mass Spectrometry (HPLC–MS/MS). The efficiency and rate of the memantine photodegradation by suspended TiO2 nanoparticles is higher than the TiO2-coated Al2O3 foam. But, from the practical point of view, TiO2-coated Al2O3 foam is more appropriate as a valuable photocatalytic composite material.


2020 ◽  
Vol 3 (3) ◽  
Author(s):  
Jothi M ◽  
Sowmiya K

Nickel Oxide (NiO) is an important transition metal oxide with cubic lattice structure. NiO is thermally stable that is suitable for tremendous applications in the field of optic, ceramic,glass, electro-chromic coatings, plastics, textiles, nanowires, nanofibers, electronics,energy technology, bio-medicine, magnetism and so on. In this present study, NiO nanoparticles were successfully synthesized by sol-gel technique. Nano-sols were prepared by dissolving Nickel-Chloride [NiCl2.6H2O] in NaOH solvent and were converted into nano structured gel on precipitation. A systematic change in preparation parameters like calcination temperature, time, pH value has been noticed in order to predict the influence on crystallite size. Then the prepared samples were characterized by the X-ray Diffraction Spectroscopic (XRD), UV-VIS Spectroscopy, Fourier Transform Infra-Red Spectroscopy (FTIR), Energy Dispersive X-ray Spectroscopy (EDX), Scanning Electron Microscopy (SEM) and Particle Size Analyzer (PSA). From XRD, the average crystalline-size has been calculated by Debye-Scherrer Equation and it was found to be 12.17 nm and the band gap energy of Nickel oxide (NiO) from UV studies reveals around 3.85 eV. Further, EDX and FTIR studies, confirm the presences of NiO nanoparticles. The SEM study exhibits the spherical like morphology of Nickel oxide (NiO). Further from PSA, the mean value of NiO nanoparticles has been determined.


2012 ◽  
Vol 501 ◽  
pp. 236-241 ◽  
Author(s):  
Ftema W. Aldbea ◽  
Noor Bahyah Ibrahim ◽  
Mustafa Hj. Abdullah ◽  
Ramadan E. Shaiboub

Thin films nanoparticles TbxY3-xFe5O12 (x=0.0, 1.0, 2.0) were prepared by the sol-gel process followed by annealing process at various annealing temperatures of 700° C, 800° C and 900° C in air for 2 h. The results obtained from X-ray diffractometer (XRD) show that the films annealed below 900°C exhibit peaks of garnet mixed with small amounts of YFeO3 and Fe2O3. Pure garnet phase has been detected in the films annealed at 900°C. Before annealing the films show amorphous structures. The particles sizes measurement using the field emission scanning electron microscope (FE-SEM) showed that the particles sizes increased as the annealing temperature increased. The magnetic properties were measured at room temperature using the vibrating sample magnetometer (VSM). The saturation magnetization (Ms) of the films also increased with the annealing temperature. However, different behavior of coercivity (Hc) has been observed as the annealing temperature was increased.


2020 ◽  
Vol 10 (7) ◽  
pp. 2595 ◽  
Author(s):  
Chih-Ling Huang ◽  
Wei Fang ◽  
Bo-Rui Huang ◽  
Yan-Hsiung Wang ◽  
Guo-Chung Dong ◽  
...  

Bioactive glass (BG) was made by the sol–gel method and doped with boron (B) to increase its bioactivity. Microstructures of BG and B-doped BG were observed by scanning electron microscopy, and phase identification was performed using an X-ray diffraction diffractometer. The ion concentrations released after soaking in simulated body fluid (SBF) for 1, 4, and 7 days were measured by inductively coupled plasma mass spectrometry, and the pH value of the SBF was measured after soaking samples to determine the variation in the environment. Brunauer–Emmett–Teller (BET) analysis was performed to further verify the characteristics of mesoporous structures. High performance liquid chromatography was used to evaluate the drug delivery ability of teicoplanin. Results demonstrated that B-doped BG performed significantly better than BG in parameters assessed by the BET analysis. B-doped BG has nanopores and more rough structures, which is advantageous for drug delivery as there are more porous structures available for drug adsorption. Moreover, B-doped BG was shown to be effective for keeping pH values stable and releasing B ions during soaking in SBF. The cumulative release of teicoplanin from BG and B-doped BG reached 20.09% and 3.17% on the first day, respectively. The drug release gradually slowed, reaching 29.43% and 4.83% after 7 days, respectively. The results demonstrate that the proposed bioactive glass has potential as a drug delivery system.


2012 ◽  
Vol 217-219 ◽  
pp. 733-736
Author(s):  
Xiu Mei Han ◽  
Shu Ai Hao ◽  
Ying Ling Wang ◽  
Gui Fang Sun ◽  
Xi Wei Qi

Zn2SiO4:Eu3+, Dy3+ phosphors have been prepared through the sol-gel process. X-ray diffraction (XRD), thermogravimetric and ddifferential thermal analysis (TG-DTA), FT-IR spectra and photoluminescence spectra were used to characterize the resulting phosphors. The results of XRD indicated that the phosphors crystallized completely at 1000oC. In Zn2SiO4:Eu3+,Dy3+ phosphors, the Eu3+ and Dy3+ show their characteristic red(613nm, 5D0-7F2), blue (481nm, 4F9/2–6H15/2) and yellow (577nm, 4F9/2–6H13/2) emissions.


Open Physics ◽  
2006 ◽  
Vol 4 (3) ◽  
Author(s):  
Abbas Al-Wattar ◽  
Baha Chiad ◽  
Wesam Twej ◽  
Sarmed Al-Awadi

AbstractThe solid host of a laser dye modifies its spectroscopic properties with respect to its liquid host. During the Sol-Gel process the dye molecules suffer from changing their environment. Two parameters affect this matter, the change in the concentration due to the evaporation of the solvent (drying) and the caging of dye molecules inside the pores or attachment to the silica network. Rhodamine 6G absorption and fluorescence spectra with different concentrations, during Sol-Gel time processing, have been studied. Both, absorption and fluorescence spectra of the dye in the solid host, for different concentrations, show a blue-shift relative to its liquid phase.


2002 ◽  
Vol 737 ◽  
Author(s):  
R.E. Melgarejo ◽  
M.S. Tomar ◽  
A. Hidalgo ◽  
R.S. Katiyar

ABSTRACTNd substituted bismuth titanate Bi4-xNdxTi3O12 were synthesized by sol-gel process and thin films were deposited on Pt substrate (Pt/TiO2/SiO2/Si) by spin coating. Thin films, characterized by X-ray diffraction and Raman spectroscopy, shows complete solid solution up to the composition x < 1. Initial results indicate that the ferroelectric polarization increases with increasing Nd content in the film with 2Pr = 50μC/cm2 for x = 0.46, which may have application in non-volatile ferroelectric memory devices.


Author(s):  
amal aboelnaga ◽  
talaat Meaz ◽  
amany M elnahrawy

Abstract The aim of this study is to investigate the effect of different doses of Velosef in magnesium silica/chitosan nanocomposite in terms of structural, morphology, optical properties, and bioactivity. Loading Velosef in fine-sized magnesium silica/chitosan is an efficient engineering approach for drug delivery. The sol-gel process was used to prepare magnesium silica fine-sized before being blended into chitosan matrix, which acts as a potential morphogenetic biomaterial. The Velosef/magnesium silica/chitosan nanocomposites were characterized by XRD, TEM, SEM, FTIR, UV-absorption, and antimicrobial studies. The XRD was characteristic of the crystallinity degree of the MgO-SiO2/chitosan/Velosef nanocomposites with three maximum peaks at 26.37°, 33.34o, 36.9°. FTIR results indicated the structural change occurred with the Velosef sol-gel polymerization process. UV-absorbance reveals that the MgO-SiO2/chitosan nanocomposite appeared a high performance for loading Velosef at two absorption bands at 253 and 347 nm. The MgO-SiO2/Chitosan/Velosef nanocomposites showed considerable antimicrobial activity in opposition to the tested representative microorganisms. The maximum antimicrobial activity was obtained with MgO-SiO2/Chitosan against both Escherichia coli and Candida albicans (37 mm), while the minimum antimicrobial activity (30 mm) was recorded against B. mycoides and E. coli with control.


2012 ◽  
Vol 476-478 ◽  
pp. 2059-2062
Author(s):  
Chen Wang ◽  
Ya Dong Li ◽  
Gu Qiao Ding

Tributyl borate was first adopted for the introduction of boron in the preparation of bioactive borosilicate xerogel by sol-gel method. The xerogel reacted continuously in 0.25M K2HPO4 solution with a starting pH value of 7.0 at 37 °C for 1day. The structural, morphologies and compositional changes resulting from the conversion were characterized using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. The results indicated that speed of formation of HA was cut way back on the time with the addition of boron and the induction period for the HA nucleation on the surface of the borosilicate xerogel was short than 1 days. The conversion mechanism of the borosilicate xerogels to hydroxyapaptite was also discussed.


2010 ◽  
Vol 93-94 ◽  
pp. 231-234
Author(s):  
B. Hongthong ◽  
Satreerat K. Hodak ◽  
Sukkaneste Tungasmita

Strontium substituted hydroxyapatite(SrHAp) were fabricated both in the form of powder as reference and thin film by using inorganic precursor reaction. The sol-gel process has been used for the deposition of SrHAp layer on stainless steal 316L substrate by spin coating technique, after that the films were annealed in air at various temperatures. The chemical composition of SrHAp is represented (SrxCa1-x)5(PO4)3OH, where x is equal to 0, 0.5 and 1.0. Investigations of the phase structure of SrHAp were carried out by using X-ray diffraction technique (XRD). The results showed that strontium is incorporated into hydroxyapatite where its substitution for calcium increases in the lattice parameters, and Sr3(PO4)2 can be detected at 900°C. The SEM micrographs showed that SrHAp films exhibited porous structure before develop to a cross-linking structure.


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