Preparation of Nano-Ceramics via Aqueous Sol-Gel Method Modified with Surfactants: An Overview

2010 ◽  
Vol 644 ◽  
pp. 79-84
Author(s):  
Yibran Perera

The present paper shows an overview related to the preparation and characterization of different nano-materials such as: silica, alumina, di- and tri-calcium silicates and a composite in the ternary CaO-SiO2-Al2O3 system. These nano-materials are related to the construction area so some basic tests are carried out to evaluate their cementitious and/or pozzolanic behavior. The nano-ceramics have been synthesized via hydrolysis and condensation of aqueous sol-gel method modified with surfactants using different precursors such as: tetraethyl orthosilicate (TEOS), calcium nitrate tetrahydrate (Ca(NO3)2.4H2O), sodium silicate (Na2O.SiO2), aluminum nitrate nonahydrate (Al(NO3)3•9H2O) and an industrial aluminum hydroxide (gibbsite). The synthesis parameters such as: pH, temperature, kind of surfactants, etc., are reported. To characterize the structural, chemical composition, particle size and morphology of the nanoparticles, different techniques such as: Fourier transform infrared (FTIR), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), field emission electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM) are used.

2010 ◽  
Vol 13 (1-2) ◽  
pp. 85 ◽  
Author(s):  
S. Manocha ◽  
Parth Joshi ◽  
Bhavini Patel ◽  
L.M. Manocha

<p>Hydroxyapatite (HAp) is a unique material having high adsorption capacity of heavy metals, high ion exchange capacity, high biological compatibility, low water solubility, high stability under reducing and oxidizing conditions, availability and low cost. Hydroxyapatite nanoparticles have been synthesized by Sol-gel method using Calcium nitrate tetrahydrate [Ca(NO<sub>3</sub>)<sub>2</sub>•4H<sub>2</sub>O] and Phosphorus pentaoxide (P<sub>2</sub>O<sub>5</sub>) as starting reactants. The addition of Phosphorus pentaoxide to Calcium nitrate tetrahydrate was carried out slowly with simultaneous stirring. After addition, solution was aged for 10 minutes for maturation. The precipitate was dried at 80 °C overnight and further heat treated at 550 °C for 2 hours. The dried and calcined particles were characterized by X-ray diffractometry, Fourier transform infra-red spectroscopy and Thermo gravimetric analysis. The particle size and morphology were studied using transmission electron microscopy. TEM examination of the treated powders displayed particles of polygon morphology with dimensions 20-50 nm in length. The FT-IR spectra for sample confirmed the formation of hydroxyapatite.</p>


2018 ◽  
Vol 24 (8) ◽  
pp. 5523-5526 ◽  
Author(s):  
B Shalini ◽  
A. Ruban Kumar ◽  
A. Mary Saral

Hydroxyapatite (HAp) is the most widely accepted biomaterial for the repair and reconstruction of bone tissue defects. The current study is based on HAp was synthesized using sol–gel method. The drug was loaded in presence and absence of gelatin with pure HAp. Precursors like calcium nitrate tetrahydrate and diammonium hydrogen orthophosphate were used and ammonia solution was added to maintain the pH value at 10.5 throughout the reaction. The synthesized HAp, drug loaded HAp and drug loaded HAp with gelatin were characterized using PXRD, FTIR, SEM, Drug loading, drug release studies. Results shows that the average crystallite size of the prepared HAp and drug loaded HAp with gelatin are 30 to 60 nm and 100 to 300 nm respectively was calculated using PXRD and morphology of pure HAp and drug loaded HAp with polymer was found using SEM. Drug loading and release percentage was calculated.


2006 ◽  
Vol 309-311 ◽  
pp. 317-320 ◽  
Author(s):  
Ill Yong Kim ◽  
Chikara Ohtsuki ◽  
Masanobu Kamitakahara ◽  
Masao Tanihara ◽  
S.B. Cho

CaO-SiO2 gels for bioactive organic-inorganic composites were prepared from tetraethoxysilane (TEOS) and calcium nitrate tetrahydrate (Ca(NO3)2⋅4H2O) by a sol-gel method with the addition of polyethylene glycol (PEG) and methacryloxypropyltrimethoxysilane (MPS). The effects of PEG and MPS on morphology and bioactivity of the gel were investigated. The samples with the nominal compositions of Ca(NO3)2:TEOS:MPS = 30:70:0 and 30:63:7 (in molar ratio) were prepared with or without coexistence of PEG at a molar ratio of (TEOS+MPS):PEG = 70:0.16. Spherical powders were obtained regardless of the addition of MPS after removal of PEG by washing, whereas the samples prepared without PEG gave crack-free bulk bodies. Incorporation of MPS was confirmed form the results of Fourier transform infrared spectroscopy (FT-IR). All the samples, regardless of addition of PEG and MPS, formed apatite on their surfaces in simulated body fluid (SBF), when washing time was 3 h during the preparation. These results show that the bioactive spherical powder of CaO-SiO2 gel modified with MPS can be obtained by the present method. It is expected to induce the increase of the chemical bonding with surrounding organic matrix when it was used as fillers for composite materials.


2011 ◽  
Vol 80-81 ◽  
pp. 426-430 ◽  
Author(s):  
Dai Hua He ◽  
Qian Zhao ◽  
Chang Bao Wang ◽  
Hao Zhang ◽  
Xiao Run Zhang ◽  
...  

The bioceramic hydroxyapaptie (HA) is frequently used as coat in titanium medical implants improving bone fixation and thus increasing a lifetime of the implant. However, its joining to the titanium alloy is not satisfactorily good. The aim of this work is to produce TiO2and HA gradient coatings on Ti6Al4V alloy to improve the interface joining. Compared the microstructures of cross section of Ti6Al4V-HA coating and Ti6Al4V-TiO2/HA gradient coatings. HA coatings were obtained by sol-gel method with sol solutions prepared from calcium nitrate tetrahydrate and triethyl phosphate as the calcium and phosphorous sources. And TiO2 coatings were obtained from Tetra Butyl Titanate and absolute ethyl alcohol as the sources by sol-gel method too. The configuration and structure were investigated with scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. The results demonstrated that the TiO2/HA gradient coatings have a homogeneous microstructure. The TiO2coating made the HA coating adhere to the Ti-6Al-4V substrate well.


2011 ◽  
Vol 694 ◽  
pp. 128-132 ◽  
Author(s):  
Erlani Pusparini ◽  
Iis Sopyan ◽  
Mohd. Hamdi ◽  
Singh Ramesh

The nanocrystalline HA powders were produced through sol-gel method which employed calcium nitrate tetrahydrate [Ca(NO3)2.4H2O] and diammonium hydrogen phosphate [(NH4)2HPO4] as calcium and phosphorous precursors. Sodium ion (Na+) is one of the trace elements found in biological apatite and believed to have important effect in its performance. The concentrations of sodium dopant were varied from 0 mol% until 15 mol% by using sodium nitrate (NaNO3) as the source of dopant. Characterization of nanopowders was investigated by using X-ray diffraction (XRD), Fourier transform infra red (FTIR) and Transmission Electron Microscope (TEM). XRD analysis revealed that there are no other phases exist in the synthesized powder, evinced single phase of HA and a trend shows an increase of cristallinity with increase of sodium dopant concentration. While the TEM images showed evidence that the particle sizes were bigger with the increasing sodium concentration, showing the effect of sodium dopant on the densification of the powder.


Author(s):  
Perica Paunović ◽  
Anita Grozdanov ◽  
Andrej Češnovar ◽  
Petre Makreski ◽  
Gennaro Gentile ◽  
...  

This work is concerned with development of sol–gel method for preparation of nanoscaled TiO2 using organometallic precursor—titanium tetraisopropoxide (TTIP) and determination of the present crystalline phases depending on the temperature of further thermal treatment. The characteristic processes and transformations during the thermal treatment were determined by means of thermal gravimetric analysis and/or differential thermal analysis (TGA/DTA) method. The crystalline structure and size of the TiO2 crystallites were analyzed by means of Raman spectroscopy and X-ray powder diffraction (XRPD) method. At 250 °C, cryptocrystalline structure was detected, where amorphous TiO2 is accompanied with crystalline anatase. The anatase crystallite phase is stable up to 650 °C, whereas at higher temperature rutile transformation begins. It was observed that at 800 °C, almost the whole TiO2 is transformed to rutile phase. According to XRPD analysis, the increase of the temperature influences on the increase of the size of the crystalline particles ranging from 6 nm at 250 °C to less than 100 nm at 800 °C. The size and shape of the TiO2 crystalline particles were observed by transmission electron microscopy (TEM). The shape of the studied samples changes from nanospheres (250, 380, and 550 °C) to nanorods (650 and 800 °C). Morphology of the formed TiO2 aggregates was observed by scanning electron microscopy (SEM).


1991 ◽  
Vol 30 (Part 2, No. 6A) ◽  
pp. L1052-L1055 ◽  
Author(s):  
Kumi Okuwada ◽  
Shin-ichi Nakamura ◽  
Motomasa Imai ◽  
Keiichi Kakuno

2018 ◽  
Vol 41 (3-4) ◽  
pp. 53-62 ◽  
Author(s):  
Behnaz Lahijani ◽  
Kambiz Hedayati ◽  
Mojtaba Goodarzi

Abstract In this work, the PbFe12O19 nanoparticles were prepared by the simple and optimized precipitation method with different organic surfactants and capping agents. In the next step, the TiO2 nanoparticles were synthesized using the sol-gel method. At the final step, the PbFe12O19-TiO2 nanocomposites were prepared via the sol-gel method. The effect of the precipitating agent on the morphology and particle size of the products was investigated. The prepared products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transform infrared spectroscopy. The results obtained by the vibrating sample magnetometer show the magnetic properties of the ferrite nanostructures. The photocatalytic effect of the PbFe12O19-TiO2 nanocomposite on the elimination of the azo dyes (acid black, acid violet and acid blue) under ultraviolet light irradiation was evaluated. The results indicate that the prepared nanocomposites have acceptable magnetic and photocatalytic performance.


2016 ◽  
Vol 20 (3) ◽  
pp. 863-866 ◽  
Author(s):  
Jia-Li Gu ◽  
Qiang-Hua Zhang ◽  
Yun-Bo Chen ◽  
Guo-Qiang Chen ◽  
Tie-Ling Xing

Cotton fabrics were treated by one-step sol-gel method. The pure silica hydrosol and phosphorus-doped hydrosol were prepared with the addition of a hydrophobic hexadecyltrimethoxysilane to decrease the surface energy of cotton fabric. The thermal properties and water repellency of treated cotton fabric were characterized by thermo-gravimetric analysis, micro combustion, limiting oxygen index, and contact angle measurement. The results showed that cotton fabric treated by phosphorus-doped silica hydrosol had excellent flame retardance, and the water repellence was apparently improved with the addition of hexadecyltrimethoxysilane.


2021 ◽  
Author(s):  
José de Jesus Serralta-Macías1 ◽  
Francisco de Paula Calderón-Piñar ◽  
Osmany García Zaldivar ◽  
Daniel Olguin ◽  
jose martin yañez limon

Abstract In this work, the ferroelectric, pyroelectric and dielectric properties of La-doped bismuth sodium titanate ceramics (BNLT) using amounts from 0 to 6.7 at.% La were studied. The precursor powders used to make dense BNLT ceramics were obtained by the sol-gel method using the acetic acid route. All samples were calcined at 700°C for 1hr and sintered at 1150°C for 30 min in an encapsulated crucible to avoid Na and Bi volatilization, obtaining relative densities equal or higher than 94%. The obtained X-ray diffraction patterns typical of the perovskite structure, confirm the incorporation of lanthanum into the lattice, evolving from rhombohedral phase to a mixture of rhombohedral and cubic structure for higher concentrations. Thermogravimetry (TG) and Differential Scanning Calorimetry (DSC) results indicate that the crystallization of precursors powders of BNT takes place between 500 and 700°C. Additionally, the Scanning Electron Microscopy (SEM) micrographs reveal a decrement of grain size from 4.5 to 0.5 μm with increasing La content. The ferroelectric hysteresis curves show that the best ferroelectric properties were obtained for BNT 1.3% La, where the obtained values of remnant polarization and coercive field were Pr=29 μC/cm2 and Ec=39 kV/cm respectively. Also, at this concentration, the pyroelectric response shows the higher value, 4 times the pyroelectric signal of the pure BNT.


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