Showing 14 results for Sol-Gel
A. Najafi, F. Golestani-Fard, H. R. Rezaie, N. Ehsani,
Volume 8, Issue 2 (6-2011)
Abstract
Abstract: SiC nano particles with mono dispersed distribution were synthesized by using of silicon alkoxides and phenolic resin as starting materials. After synthesis of sample, characterizations of the obtained powder were investigated via Fourier Transform Infrared Spectroscopy (FTIR) with 400-4000 cm-1, X-ray Diffractometry (XRD), Laser Particle Size Analyzing (LPSA), Si29 NMR analysis, Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). FTIR and Si29 NMR results of the gel powder indicated that Si-O-C bonds were formed due to hydrolysis and condensation reactions . FTIR results showed a very strong peak for heat treated powder at 1500°C after carbon removal which is corresponded to Si-C bond. Obtained pattern from X-ray diffractometry showed that the final products contain -SiC phase with poly crystalline planes and little amounts of residual carbon. PSA results showed that the average particles size were 50.6 nm with monosized distribution. Also microstructural studies showed that the SiC nano powders have semi spherical morphology with mean particles size of 30-50 nm and also there are some agglomerates with irregular shape.
Simin Janitabar-Darzi, Alireza Mahjoub,
Volume 9, Issue 3 (9-2012)
Abstract
Yellow-colored nitrogen doped TiO2 photocatalyst and a pure TiO2 powder were synthesized via sol-gel method using TiCl4 and urea as raw materials. However, the synthesis procedure for nitrogen doped TiO2 was catalyzed by acid that dialed with controlled precipitation and slow nucleation. According to XRD analysis, the nitrogen doped TiO2 consisted of anatase phase of titania which was a significant achievement regarding its possible photocatalytic applications. The band gaps of nitrogen doped TiO2 and pure TiO2 were estimated from UV-Vis spectroscopy data to be 2.8 and 3.3 ev, respectively. Photocatalytic properties of the nitrogen doped TiO2 nanocatalyst and pure TiO2 were compared for degradation of crystal violet dye in visible light irradiation. In comparison to pure TiO2, nitrogen doped TiO2 showed superior photocatalytic efficiency towards the dye.
J. Jac Faripour Maybody, A. Nemati, E. Salahi,
Volume 10, Issue 2 (6-2013)
Abstract
In the present study, bioceramic composites based hydroxyapatite (HAp) reinforced with carbon nanotubes (CNTs) was synthesized via sol-gel technique. The dried gels were individually heated at a rate of 5°C/min up to 600°C for 2 h in a muffle furnace in order to obtain HAp-MWCNTs mixed powder. Composites were characterized by XRD, FT-IR, SEM, TEM/SAED/EDX and Raman spectroscopy techniques. Results showed the synthesis of HAp particles in the MWCNTs sol which was prepared in advance, leads to an excellent dispersion of MWCNTs in HAp matrix. Apparent average size of crystallites increased by increasing the percentage of MWCNTs. The average crystallite size of samples (at 600°C), estimated by Scherrer’s equation was found to be ~50-60 nm and was confirmed by TEM. MWCNTs kept their cylindrical graphitic structure in composites and pinned and fastened HAp by the formation of hooks and bridges.
A. Najafi, F. Golestani-Fard, H. R. Rezaie,
Volume 11, Issue 1 (3-2014)
Abstract
Mono dispersed nano SiC particles with spherical morphology were synthesized in this project by hydrolysis and condensation mechanism during sol gel processing. pH, temperature and precursor’s ratio considered as the main parameters which could influence particles size. According to DLS test results, the smallest size of particles in the sol (<5nm) was obtained at pH<4. It can be observed from rheology test results optimum temperature for achieving nanometeric gel is about 60 ˚C. The optimum pH values for sol stabilization was (2-5) determined by zeta potentiometery. Si 29NMR analysis was used in order to get more details on final structure of gel powders resulted from initial sol. X-ray diffraction studies showed sythesized powder consists of β-SiC phase. Scanning electron microscopy indicated agglomerates size in β-SiC synthesis is less than 100 nm. Finally, TEM studies revealed morphology of β-SiC particles treated in 1500˚C and after 1hr aging is spherical with (20-30) nm size
Z. Ghiami, S. M. Mirkazemi, S. Alamolhoda,
Volume 12, Issue 2 (6-2015)
Abstract
trontium hexaferrite (SrFe
12
O
19
) nanosized powders were synthesized by sol-gel auto-combustion method
with and without cetyltrimethylammonium boromide (CTAB) addition in the sol with Fe/Sr ratio of 11 (using additional
Sr). The resultant powders were investigated by X-ray Diffraction (XRD), Transmission Electron Microscope (TEM),
Field Emission Scanning Electron Microscope (FESEM) and Vibration Sample Magnetometer (VSM) techniques.
Phase constituents of the synthesized samples which were heat treated at temperatures in the range of 700- 900 ◦C
were studied. XRD results revealed that CTAB addition facilitates the formation of single phase strontium hexaferrite
at 800 ◦C. Microstructural evaluations with FESEM represented that CTAB addition causes formation of larger
particles with a narrower size distribution. VSM results represented that the highest amount of intrinsic coercivity force
(
i
H
C
) was obtained in the sample without CTAB addition and with additional Sr, calcined at 800 ◦C for 1 h which was
equal to 5749.21 Oe, while the value of
i
H
C
was equal to 4950.89 Oe without additional Sr. The amount of maximum
magnetization (M
max
) was raised from 48.41 emu/g to 62.60 emu/g using CTAB and additional Sr. The microstructure
and magnetic properties of the samples have been explained
M. Khosravi Saghezchi, R. Ajami, M. Biazar Markie, H. Sarpoolaky,
Volume 12, Issue 4 (12-2015)
Abstract
A comparing study on formation and microstructure features of aluminum titanate is investigated through both solid-state and sol-gel processes. Aluminum titanate formed by firing at 1350ºC and 1450ºC for 4h in solid-state process. In the sol-gel process formation of submicron sized particles is followed by addition of sucrose into the transparent sol. XRD analysis was confirmed the formation of aluminum titanate at 1400ºC in lower duration of calcination (3h) without any additives in the sol-gel process. In this work 2wt% MgO is added to the samples as the additive for forming acceleration of aluminum titanate. The influence of MgO addition and heat treatment are studied on phase formation and microstructure development of aluminum titanate in both procedures. Additive optimizes aluminum titanate formation at lower temperatures (1300-1350ºC). Phase and microstructure studies of Mg containing samples optimally show significance in aluminum titanate formation.
S. Alamolhoda, S. M. Mirkazemi, T. Shahjooyi, N. Benvidi,
Volume 13, Issue 1 (3-2016)
Abstract
Nano-sized NiFe2O4 powders were synthesized by sol–gel auto-combustion method using pH values from 7 to 9 in the sol. The effect of pH variations on complexing behavior of the species in the sol has been explained. Changes in phase constituents, microstructure and magnetic properties by changes in pH values were evaluated by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and vibration sample magnetometer (VSM) techniques. Changes in pH value from 7 to 9 changes the amounts of NiFe2O4, FeNi3 and α-Fe2O3 phases. Calculated mean crystallite sizes are in the range of 44 to 51nm. FESEM micrographs revealed that increasing the pH value to 9 causes formation of coarse particles with higher crystallinity. Saturation magnetization was increased from 36.96emu/g to 39.35emu/g by increasing pH value from 7 to 8 which is the result of increased FeNi3 content. Using higher pH values in the sol reduces the Ms value.
F. Salehtash, H. Banna Motejadded Emrooz, M. Jalaly,
Volume 15, Issue 2 (6-2018)
Abstract
Mesoporous SiO2 nanopowder was synthesized under an acidic condition by a sol-gel method using various amounts of cetyltrimethyl ammonium bromide (CTAB) as structure directing agent. The samples were investigated with XRD, SEM, FTIR, TEM and N2 absorption-desorption analysis. Also, the incremental effect of surfactant were examined. The results obtained from the analysis suggested that an increase in the amount of surfactant resulted in increasing specific surface area, pore size and pore volume, of the synthesized particles up to 549 m2.g-1, 17.3 nm, and 2 cm3.g-1, respectively. Absorption behavior of the mesoporous silica was investigated for degradation of methylene blue pigments (MB) in aqueous solutions. The samples SC0, SC0.5 and SC1 showed the maximum absorption capacities of 333, 454 and 526 mg/g, respectively
M. Karimi Sahnesarayi, H. Sarpoolaky, S. Rastegari,
Volume 16, Issue 2 (6-2019)
Abstract
In this study nanosized TiO2coatings on the 316L stainless steel substrate were prepared by means of dip-coating technique in which thickness of the coating layer increased byrepeating the coating cycles in two different routes: (I) dipping and drying,respectively, were repeated one, three and five times and finally the dried coated sample was heat treated (single); (II) multiple heat treatment performed after each dipping and drying cycle, respectively.The structural, morphological and optical characterizations of coatings as well as thickness of coatings were systematically studied.The photocatalytic activity of the various TiO2 coatings was investigated based on the degradation of an aqueous solution of Methyl orange.Moreover, thecorrosion protective properties of coatings were evaluated in both dark and UV illumination conditions based on the obtained polarization curves. The results indicated 1.75 times improvement in photocatalytic reaction rate constant, a two orders of magnitude decrease in corrosion current density in dark condition and about 140 mV electrode potential reduction under UV illumination with optimum coating preparation procedure, repeating the cycle from dipping to heat treatment three times, than the sample prepared with one time coating and heat treatment since this procedure provided not only high thickness and defect-free coating but also transparent one.
Sara Ahmadi, Bijan Eftekhari Yekta, Hossein Sarpoolaky, Alireza Aghaei,
Volume 18, Issue 4 (12-2021)
Abstract
In the present work, monolithic gels were prepared through different drying procedures including
super critical, infrared wavelengths and traditional drying methods. Dense and transparent glasses
were obtained after controlled heat treatment of the dried porous xerogels in air atmosphere.
The chemical bonding as well as different properties of the prepared gels and the relevant glasses
were examined by means of Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmitt-
Teller (BET) and UV-Vis spectrometer. Based on the obtained results, different drying conditions
affect the average pore size and the total pore volume of the studied gels. The mean pore size was
found to be 8.7 nm, 2.4 nm and 3.2 nm for super critical, IR radiation and slow drying in air
atmosphere, respectively. The glass network structure was significantly changed by heat treatment temperature so that the B-O-Si bonds were formed only after 450 °C. It was found that the gel dried under super critical condition was unable to reach to its full density all over the selected sintering temperature interval.
Omid Sharifi, Mohammad Golmohammad, Mozhdeh Soozandeh, Mohammad Oskouee,
Volume 19, Issue 3 (9-2022)
Abstract
Li7La3Zr2O12 (LLZO) garnets are one of the promising materials as electrolytes for solid-state batteries. In this study, Li7-3xAlxLa3Zr2O12 (x= 0.22, 0.25, and 0.28) garnet is synthesized using the combustion sol-gel method to stabilize the cubic phase for higher ionic conductivity. The X-ray diffraction (XRD) results of as-synthesized powders reveal that by addition of 0.22 and 0.25 mole Al, the tetragonal phase still co-exist, whereas 0.28 mole Al addition resulted in a single cubic phase. Afterward, the as-synthesized powders are pressed and sintered at 1180°C for 10h. The hardness evaluation revealed that Al addition increases the hardness that shows better resistance against Li dendrite formation. Besides, the secondary electron microscopy results demonstrate that the dopant has not a huge impact on particle size and grain growth whereas the porosity content has been changed. Finally, the investigation of samples' electrochemical behavior reveals that the addition of Al increases the ionic conductivity of samples by increasing the density and stability of the cubic phase as well. The results declare that the 0.25 Al sample has the highest ionic conductivity. This behavior is thought to be due to the promotion of sintering and increment of bulk ionic conductivity by doping Al.
Parisa Rastgoo Oskoui, Mohammad Rezvani, Abbas Kianvash,
Volume 20, Issue 2 (6-2023)
Abstract
Abstract
The effect of different heat-treatment temperatures on the magnetic, crystallization, and structural properties of 20SiO2.50FeO.30CaO (mol%) glass ceramics was studied. The initial glass was synthesized by the sol-gel method at 25℃ with a precursors to solvent ratio of 1/5. After aging the resulted gel for 24 h at room temperature, it was dried in an electric dryer at 110 ℃ . By heat treatment at different temperatures, different phases such as magnetite, maghemite, and hematite were crystallized in the glass. The maximum stability temperature of magnetite and maghemite were 360℃ and 440℃ respectively. By increasing the heat treatment temperature to higher than 440℃ , the oxidation of maghemite to hematite was occureds. The highest magnetization amount (1.9 emu/g) belonged to sample heat treated at 680℃ . By increasing the heat treatment temperature to 840℃ , the magnetization decreased to 0.8 emu/g, due to the oxidation of maghemite. By increasing the heat treatment temperature from 440℃ to 680℃ , crystalline size of maghemite was increased from 40 to 200 nm. By forther increment of temperature to 840℃ , the size of maghemite crystals decreased to 17nm, due to the oxidation of maghemite to hematite.
Abstract
The effect of different heat-treatment temperatures on the magnetic, crystallization, and structural properties of 20SiO2.50FeO.30CaO (mol%) glass ceramics was studied. The initial glass was synthesized by the sol-gel method at 25℃ with a precursors to solvent ratio of 1/5. After aging the resulted gel for 24 h at room temperature, it was dried in an electric dryer at 110 ℃ . By heat treatment at different temperatures, different phases such as magnetite, maghemite, and hematite were crystallized in the glass. The maximum stability temperature of magnetite and maghemite were 360℃ and 440℃ respectively. By increasing the heat treatment temperature to higher than 440℃ , the oxidation of maghemite to hematite was occureds. The highest magnetization amount (1.9 emu/g) belonged to sample heat treated at 680℃ . By increasing the heat treatment temperature to 840℃ , the magnetization decreased to 0.8 emu/g, due to the oxidation of maghemite. By increasing the heat treatment temperature from 440℃ to 680℃ , crystalline size of maghemite was increased from 40 to 200 nm. By forther increment of temperature to 840℃ , the size of maghemite crystals decreased to 17nm, due to the oxidation of maghemite to hematite.
Amirreza Sazvar, Seyed Mohammad Saeed Alavi, Hossein Sarpoolaky,
Volume 20, Issue 2 (6-2023)
Abstract
We report a simple and practical approach for the easy production of superhydrophobic coatings based on TiO2-SiO2@PDMS. In this study, we used tetraethylorthosilicate (TEOS) and titanium tetraisopropoxide (TTIP) as a precursor for the sol-gel synthesis of SiO2 and TiO2, respectively. Afterward, the surface of nanoparticles was modified by 1,1,1,3,3,3-hexamethyldisilazane (HMDS) before being combined with polydimethylsiloxane (PDMS). The hydrophobic property of coatings was evaluated by static contact angle measurements. The phase composition and structural evolution of the coatings were examined by X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) analysis. It was shown that changing the weight ratio of the solution composition of the coating can affect the hydrophobicity of the surface. The best sample has shown a superhydrophobic property with a 153˚ contact angle which contained (75%TiO2-25%SiO2) and PDMS at a weight ratio of 1:1. Moreover, the results showed that the superhydrophobic coating retains its hydrophobic properties up to a temperature of 450 ˚C, and at higher temperatures, it converts to a super hydrophilic with a water contact angle close to 0 ˚. The SiO2-TiO2@PDMS coating degrades methylene blue by about 55% and was shown to be capable of photocatalytically decomposing organic pollutants.
Amit Bandekar, Pravin Tirmali, Paresh Gaikar, Shriniwas Kulkarni, Nana Pradhan,
Volume 21, Issue 1 (3-2024)
Abstract
The Mn-Zn ferrite with a composition of Mn0.25Mg0.08Cu0.25Zn0.42Fe2O4 has been synthesized in this study using the chemical sol-gel technique at a pH of 7. The sample was prepared and subsequently annealed at a temperature of 700°C. The nanocrystalline ferrite samples were subjected to characterization using X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), Scanning electron microscopy (SEM), Thermogravimetry (TG), and Differential thermal analysis (DTA). The findings of these observations are delineated and deliberated. The sample's phase composition was verified using X-ray diffraction examination. The crystalline size was determined using Scherrer's formula and was observed to be within the range of 20-75 nm. Two notable stretching bands were seen in the FTIR spectra within the range of 400-650 cm-1. The spinel structure of the produced nanoparticles was confirmed by these two bands. The magnetic characteristics of the powder were examined using a Vibrating Sample Magnetometer (VSM). The presence of M-H hysteresis loops suggests that the produced nanoparticles have superparamagnetic properties, as evidenced by their low coercive force, remanent magnetization, and saturation magnetization values.
