Journal of Advanced Materials in Engineering (Esteghlal)

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The purpose of this work was to production of ceramic thin films by using of Sol-Gel process. For this purpose deposition of SiO2 on substrates of soda-lime glasses has been carried out. Coating treatments on prepared specimen were conducted in a Sol solution by means of dipping at various times. After drying and performing appropriate heat treatment on each sample, the thickness of coated layer was measured by means of roughness method. Some of the specimens were also exposed to heat and chemical environment to evaluate the coating resistance in such media. SEM examination and EDAX and XRD analysis of coating layers was also conducted on some samples. The results indicated that by Sol-Gel method, it is easily possible to achieve thin layers in the scale of one hundredth micron meter. Any change of the thickness layer on the surface is negligible and the quality of the coating is excellent. Also, experiments indicated that deposited coatings by Sol-Gel process, are stable and give enough durability in various environments.

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The addition of ZrO2 particles to the HA coating has received considerable attention because ZrO2 particles increase the bonding strength between HA coating and substrate. In this study, nanostructured hydroxyapatite (HA)/yttria stabilized zirconia (YSZ) coatings were prepared by a sol–gel method. It was found that at 950ºC, the dominant phases were HA and tetragonal (t)-zirconia in 3YSZ, cubic (c)-zirconia in 8 YSZ and t-c-Zirconia in 5YSZ phases with the small amounts of β-tricalcium phosphate (β-TCP) and CaZrO3. The crystallite size of the coating was about ~20-30 nm for tetragonal and cubic zirconia grain size and 40-80 nm for hydroxyapatite grain size. Crack-free and homogeneous HA/YSZ composite coatings were obtained with no observable defects. In vitro evaluation in 0.9% NaCl showed that Ca2+ dissolution rate of composite coatings was lower than that of pure HA coatings. The decrease in electrochemical performance of these coated samples in comparison with the uncoated type 316L St.St could be associated with chloride ion and water penetration into the coating, transport of ions through the coating, and the subsequent electrochemical reactions at the coating–metal interface.

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Fabrication of biomaterials with ability to form a bond with bone tissue for bone skeletal system repair is one of the biomaterial science aims. Bioactive glasses containing CaO-SiO2-P2O5 are among the most important groups used in biomedicine and dentistry such as bone defect repair and maxillo-facial reconstruction. The aim of this work was preparation and characterization of nano particle bioactive glass with optimum bioactivity. Bioactive glasses with three different compositions (45S, 49S and 58S) were prepared via sol- gel technique. X- ray diffraction (XRD) technique and X- ray fluorescent (XRF) method were utilized for the phase analysis and also to investigate the chemical composition of the obtained bioactive glass nanopowders. Transmision electron microscopy (TEM) and Scanning electron microscopy (SEM) were utilized to study the structure, morphology and particle size of synthesized bioactive glass nanopowders. In order to investigate the bioactivity, the prepared bioactive glasses were immersed in the simulated body fluid (SBF) solution at 37◦C for 30 days. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) were utilized to recognize and confirm the apatite layer on the prepared bioactive glass nanopowders. TEM images showed that the prepared bioactive glasses had the particle sizes less than 100 nanometers. SEM, FTIR and XRD confirmed the formation of bone-like apatite layer formed on the bioactive glass nanopowders surface, confirming the bioactivity of synthesized bioactive glass nanopowders. It was concluded that the amount of apatite on the 45S bioactive glasse was greater in comparison with 49S and 58S bioactive glasses. It is notable that by optimizing the chemical composition, bioactive glass nanopowder could be used in applications such as repair of bone defects and bone replacement.

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Due to its biocompatibility, bioactivity and high durability properties, hydroxyapatite (HA) has a wide range of applications in medical cases such as bone defect treatment and bone tissue regeneration. Biological apatite as the most important integrity of the mineral part of hard tissues consists of tiny hydroxyapatite crystals in nanoregime. It seems that using the artificial hydroxyapatite with similar structure and chemical composition to biological apatite could increase its durability inside the natural hard tissues. The aim of the present work was the synthesis of nano structured hydroxyapatite via different routes, comparison of their characterization and enhancement of the bioactivity and bioresorbability of prepared hydroxyapatite by controlling its crystal size and chemical composition. Nano structured hydroxyapatite was prepared by mechanical activation and sol-gel routes. X-ray diffraction technique (XRD), Fourier transform infra red spectroscopy (FTIR) and transmission electron microscopy (TEM) were used to characterize the prepared hydroxyapatite powders. The synthesized powder was soaked in simulated body fluid (SBF) for various periods of time in order to evaluate its bioresorbability and bioactivity after immersion in SBF. Atomic absorption spectroscopy (AAS) was used to determine the dissolution rate of calcium ions in SBF media. Results showed that the mechanical activation prepared HA powder had nano scale structure with mean size of 29 nm and the sol gel prepared HA powder had nano scale structure with mean size of 25 nm. Ionic dissolution rate of prepared nano structured powders was higher than the conventional HA (with micron size) and were similar to biological apatite. It could be concluded that bioactivity behavior of hydroxyapatite powder is affected by its crystalline size. By using the nano structure HA powder with less than 50 nm crystalline size, the optimum bioactivity and bioresorbability would be achieved.

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In the present study, a bioceramic-based composite with remarkable mechanical properties and in vitro apatite forming ability was synthesized by sintering compacts made up of mixtures of hydroxyapatite (HA) and sol-gel derived bioactive glass (64SiO2-26CaO-5MgO-5ZnO) (based on mole %). HA was synthesized through co-precipitation method. The stabilization temperature of the bioactive glass was set to be 700 ºC according to simultaneous thermal analysis (STA). Laser Particle Size Analysis (LPSA) was used to compare the particle size distributions of the synthetic powders. HA matrix was mixed with different weight percentages of bioactive glass (5, 10, 15, 20, 25 and 30 wt. %) and compressed by 80 MPa pressure. After sintering the uniaxial compression test of the samples was done and the specimen with the highest compressive strength (20 wt. % bioactive glass) was selected to be immersed in the Simulated Body Fluid (SBF) for 3, 7 and 14 days. The results showed that the compressive strength of the sample decreased after keeping it in the SBF. Also, inductively coupled plasma analysis (ICP) was used to study the ion release behavior of the sample in the SBF. Finally, phase composition, microstructure and functional groups in the composite were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infra-red spectroscopy (FTIR) techniques, respectively.

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In recent years, use of Sol-gel procedure for laboratory and industrial synthesis of Nanostructures and especially silica Nano-particles has increased. In this research, silica particles were synthesized by Sol-gel procedure and their physical properties were studied by means of Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Thermal Gravimetric Analysis (TGA). Effect of structural modifiers on the morphology and diameter of Nano-particles was investigated. In addition, the reaction was carried out in the presence of ultrasonic waves in periods of 10, 30 and 60 minutes and the effect of these waves on different stages of reaction was studied by means of SEM. Finally, in this research, spherical particles of 50 to 80 nanometer sizes were synthesized and characterized. They can be very useful hosts for lanthanide complexes that can be used in drug delivery systems, radiotherapy, photoluminescence applications and manufacturing of special lasers. Also, different amounts of Lanthanum Nitrate hexahydrate were added to the mixture during the creation of Nano-particles. Then, Simulated Body Fluid (SBF) was produced for the study of ability of the Nanostructures in regulated delivery of drugs such as Lanthanides, and releasing of Lanthanides in 10 minute periods for 80 h was studied. Lanthanide concentration in SBF was also studied by means of Inductively Coupled Plasma (ICP). According to the results of ICP, loaded Lanthanide was not released from the silica network. Loaded Lanthanides in the mesopores can be used in radiation, especially in cases of liver cancer.

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The particles of ferrite Ni0.6-xCuxZn0.4Fe2O4, (0-0.5 in step with 0.1) were prepared by the sol-gel method. Sintering process of powders was carried out at 600, 800 and 1000 oC. The effect of the sintering temperature and chemical composition on the structural and magnetic properties of the Cu substituted NiZn ferrite was investigated. EDS analysis and X-ray diffraction patterns confirmed a well defined of single crystal phase with spinel structure. The thermal behavior process and particle size of samples were investigated by thermal analysis TG, DTA techniques and scanning electron microscope, respectively. VSM curves reveal that the sintering temperature and copper content affect saturation magnetization. M ssbauer spectra displays that the copper cations occupy the octahedral sites. With increasing of copper cations, the iron cations immigrate to tetrahedral site, consequently the saturation magnetization decrease.

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Refractory carbides are becoming a group of promising material due to their unique properties, such as high hardness, high wear and corrosion resistance, high thermal conductivity, high melting point, high strength even at high temperatures, and a high degree of chemical stability. Among these carbides, titanium carbide (TiC) is one of the most important engineering material, based on its promising properties. This paper presents a novel approach to preparing ultrafine TiC by sol–gel processing. This novel process would minimize kinetic barriers because carbon (coming from sucrose) was homogeneous dispersed in the precursor of TiO2 by sol–gel process. As a result, the increased contact area between reactants should make the reaction to complete at lower temperatures.

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In this study, mixed metal oxides Al2O3/MgO/TiO2 coatings with Al/Mg/Ti ratios of 5:1:3 and 2.5:3:4 were coated on AA1100 aluminum by sol-gel method. The surface morphology, phase analysis and the corrosion behavior of the Al2O3/MgO/TiO2 coatings were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), and electrochemical impedance spectroscopy measurements (EIS) in 3.5 wt.% NaCl solution. The thermal behaviors, the bonds configuration, and functional groups of the coated samples were studied by thermo-gravimetric and differential thermal analysis (TG-DTA) and Fourier transform infrared spectroscopy (FTIR), respectively. The results demonstrated that heat treatment at 450 °C caused an increase in porosity and coating cracking, finally leading to the decrease of corrosion resistance. The best corrosion resistance was achieved for the sample with Al/Mg/Ti molar ratio of 5:1:3 without any heat treatment. The structure of this sample was amorphous, and heat treatment resulted in crystallization and decrease of the corrosion resistance.

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The objective of this study was to synthesize glass ionomer–forsterite nanocomposite and study the effect of incorporating forsterite nanoparticles to the ceramic part of glass ionomer cement in order to improve mechanical properties and bioactivity. So, Forsterite nanoparticles were made by the sol-gel process using different weight percentages added to the ceramic part of commercial GIC (Fuji II GC). X-ray diffraction (XRD) was used in order to characterize and determine grain size of the produced forsterite nanopowder. In order to study the mechanical properties of the produced glass ionomer cement-forsterite nanocomposite, the compressive strength (CS), three-point flexural strength (FS) and diametral tensile strength (DTS) of specimens were measured. Statistical analysis was done by one Way ANOVA and differences were considered significant if P‹0.05. The morphology of fracture surface of specimens was studied using scanning electron microscopy (SEM) technique. Bioactivity of specimens was investigated by Fourier transitioned-infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). The results of XRD analysis confirmed the nanocrystalline and pure forsterite synthesis. According to the mechanical properties measurements, the optimum weight percentages of forsterite nanoparticles for enhancement of CS, FS, and DTS were obtained equal to 3, 1 and 1 wt.%, respectively. Statistical analysis showed that the differences between all the groups were significant (P<0.05). SEM images and results of the ICP-OES and FTIR tests confirmed the bioactivity of the nanocomposite. Glass ionomer-forsterite nanocomposite containing 1 to 3 wt.%-forsterite nanoparticles can be a suitable candidate for dentistry and orthopedic applications due to the improvement of mechanical properties and bioactivity.

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With various features such as strong oxidation, biocompatibility and acceptable mechanical properties, titanium dioxide (TiO₂) is among the materials that are frequently used in biological and medical applications. Nowadays, with the aim of increasing the efficiency of titanium dioxide and practical use of this material, doping it with elements such as silver, zinc and iron has been favored. In this study, Ag-TiO₂ and ZnO-TiO₂ nanoparticles were prepared by the sol–gel method and were evaluated and compared.In order to identify the present phases in the structure, X-ray diffraction analysis was used. Also for the characterization of the nanoparticles, Ultraviolet–visible spectroscopy (UV-Vis), Energy-dispersive X-ray spectroscopy (EDS), Field Emission Scanning Electron Microscope (FESEM) and Zeta Potential were used. Inaddition, the antibacterial activities of nanoparticles were investigated and compared. The results showed that sol-gel method could successfully produce nanoparticles of Ag-TiO₂ and ZnO-TiO₂ with the expected combination. The investigation of antibacterial properties of these particles revealed that at lower inhibitory concentrations, Ag-TiO₂ composition has a higher antibacterial activity than ZnO-TiO₂ one.

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In this study, NBG was successfully achieved through a sol-gel technique, and to further improve its dispersibility, a crylate coupling agent was coupled onto the surface of the NBG. The 3-(Trimethoxysilyl)Propylmethacrylate coupling agent was used to the surface modification of the synthesized NBG by a wet-chemical method in a dynamic inert nitrogen atmosphere. The surface properties of the biomaterials before and after modification were characterized and compared using FTIR and AFM techniques. The characteristic peaks in FTIR spectra indicated that –CH2, –CH3 and C=O groups appeared on the surface of modified NBG, and also, AFM analysis revealed that the dispersibility of surface modified NBG was improved, significantly. The above results proved that the desired groups of 3-(Trimethoxysilyl)Propyl methacrylate had been covalently bonded onto the surface of NBG. Besides, a nanocomposite scaffold was synthesized using the synthesized NBG and polyurethane foam as raw materials. The morphology of pores, porosity contents, compress strength and bioactivity of the scaffold were studied. The results showed that the biological scaffolds for use in bone tissue engineering with the basic requirements (90% porosity and 200-600 μm pore diameter) were successfully prepared. The polymer component had no effect on the relationship between the scaffold pores and bioactivity of bioglass nanoparticles. Improvement of compressive strength and proper bioactivity of the resulted scaffold showed that it is an acceptable candidate for biomaterials applications.

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The aim of the present study is to study the effects of adding  diopside (CaMgSi₂O₆) as well as silica sulfuric acid nanoparticles to ceramic part of glass ionomer cement (GIC) in order to improve its mechanical properties. To do this, firstly, diopside (DIO) nanoparticles with chemical formula of CaMgSi₂O₆ were synthesized using sol-gel process and then, the structural and morphological properties of synthesized diopside nanoparticles were investigated. The results of scanning electron microscopy (SEM) and particle size analyzing (PSA) confirmed that synthesized diopside are nanoparticles and agglomerated. Besides, the result of X-ray diffraction (XRD) analyses approved the purity of diopside nanoparticles compounds. Silica sulfuric acid (SSA) nanoparticles are also prepared by chemical modification of silica nanoparticles by means of chlorosulfonic acid. Fourier transform infrared spectroscopy (FTIR) technique was used to find about the presence of the (SO₃H) groups on the surface of silica sulfuric acid nanoparticles. Furthermore, various amounts (0.1, 3 and 5 wt.%) of diopside and silica sulfuric acid nanoparticles were added to the ceramic part of GIC (Fuji II GIC commercial type) to produce glass ionomer cement nanocomposites. The mechanical properties of the produced nanocomposites were measured using the compressive strength, three-point flexural strength and diametral tensile strength methods. Fourier transform infrared spectroscopy technique confirmed the presence of the (SO₃H) groups on the surface of silica nanoparticles. The compressive strength, three-point flexural strength and diametral tensile strength were 42.5, 15.4 and 6 MPa, respectively, without addition. Although adding 1% silica solfonic acid improved nanocomposite mchanical properties by almost 122%, but maximum increase in nanocomposite mechanical properties was observed in the nanocomposites with 3% diposid, in which 160% increase was seen in the mechanical properties.

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Organic–inorganic hybrid coatings were prepared by sol–gel method and deposited on aluminum alloy 6061. Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) spectroscopy and Scanning Electron Microscopy (SEM) were used for structural study of the hybrid coatings. Adhesive strength of sol–gel coatings to the substrate was evaluated quantitatively and qualitatively. Corrosion behavior of the samples was studied by cyclic potentiodynamic and linear polarization tests. Results showed that adhesion strength of the coatings to the substrates was increased with increasing tetrapropoxide of zirconium (TPOZ) and cerium content. Corrosion tests showed that corrosion current density of coated samples were decreased three to seven orders of magnitude in comparison with uncoated aluminum alloy 6061. Decreasing in corrosion current density and increasing in polarization resistance was observed by increasing zirconia and cerium content. Unlike the uncoated aluminum alloy 6061, the crack-free coatings did not show pitting tendency. 

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In this research, the nanopowders of lanthanum and neodymium co-doped yttria were synthesized by sol-gel combustion method. Citric acid and glycine were used as the gel maker and fuel respectively. The effect of molar ratio of citric acid to glycine on the grain size and morphology was evaluated. The optimized products were characterized by X-ray diffraction (XRD), field-emission scanning electron microscope (FESEM), transmission electron microscope (TEM), UV–visible (UV–Vis), thermal gravimetric-differential thermal analysis (TG/DTA), and Fourier transform infrared spectrometer (FTIR). The optimized products which are synthesized with a molar ratio citric acid to glycine 1.06:1.06 have an average grain size of 30-40nm with spherical morphology, and without agglomeration. Also, their band gap is 3.29eV.

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In this research, nickel ferrite nanoparticles were synthesized by sol-gel auto-combustion route, and the effect of calcination temperature on phase constituents, magnetic properties and microstructure of the synthesized nanoparticles was evaluated using X-ray Diffraction (XRD), Vibrating Sample Magnetometer (VSM) and Scanning Electron Microscopy (SEM). XRD results were submitted to quantitative analysis. Microstructural studies and crystallite size calculations showed formation of nanoparticles. XRD results showed that the combustion product consisted of NiFe₂O₄, α-Fe₂O₃, NiO, and FeNi₃ phases. FeNi₃ was eliminated by calcination, and the amounts of NiO and α-Fe₂O₃ were modvlated by changing in calcination temperature. Saturation magnetization changed from 37emu/g in combustion product to 30emu/g by calcination at 600°C, due to decomposition of FeNi₃ magnetic phase and formation of higher amount of antiferromagnetic hematite phase. Also, the coercivity values increased, that could be due to increasing the amount of nickel ferrite phase and eliminating FeNi₃ phase. Saturation magnetization reached to 43emu/g in calcinated sample at 1000°C due to the reaction between hematite and NiO phases that led to formation of higher amount of nickel ferrite to 43emu/g. Coercivity value dropped out to 127Oe by calcination at 1000°C, the reason of which could be incresing of particle size and formation of multi domain magnetic particles.
 

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In this paper, Ni-doped lead hexaferrites (PbFe12-xNixO19) nanoparticles with x = 0.2 were prepared by sol- gel method. Then, the effect of annealing temperature on its structural, magnetic and dielectric properties was studied. First, the dryed gel was evaluated by Thermogravimetry-Differential Thermal Analysis (TG/DTA) and then, the structural morphology, magnetic and dielectric properties of samples have been characterized by Fourier Transform Infrared (FT-IR) spectroscopy, X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Vibrating Sample Magnetometer (VSM) and LCR meter. The results of x-ray diffraction patterns show that by increasing annealing temperature up to 800 °C, PbFe11.8Ni0.2O19 phase percentage in the samples increases. Also, by increasing annealing temperature, the magnetization increases because the unwanted phases disappear and pure and single-phase lead hexaferrite are formed. By increasing frequency, first the AC electrical conductivity of the samples decreases and then increases. These variations have been explained by Maxwell- Wanger model. The result measurements show that the best sample is PbFe11.8Ni0.2O19 with annealing temperature of 800 °C for 3 h.
 

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In this research, nanoparticles of La_0.8Sr_0.2MnO₃ with mean crystallite size of 20 nm have been prepared by sol gel method. The sample has been characterized by X-Ray Diffraction (XRD) using Rietveld refinement, Field Emission Scanning Electron Microscope (FESEM) and Fourier Transform Infrared (FTIR) spectroscopy. The static magnetic properties such as saturation magnetization, effective magnetic moment and ferromagnetic phase fraction of the nanoparticles are determined by different techniques using magnetic hysteresis loop at room temperature. The magnetic dynamic properties of crystalls are studied by measuring AC magnetic susceptibility versus temperature at different frequencies. Néel-Brown, Vogel-Fulcher, critical slowing down models and empirical parameters are used to distinguish between superparamagnetic and superspin glass behaviour in the nanoaprticles. By fitting the experimental data with the models, relaxation time, critical view, magnetic anisotropy energy and effective magnetic anisotropy constant have been estimated. The obtained results support the presence of interacting superparamagnetic behaviour between magnetic nanoparticles of La_0.8Sr_0.2MnO₃.
 

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TiO₂/MWCNT nanocomposite thin films containing different percentages of multi-walled carbon nanotubes were coated on fluorinated tin oxide substrates by sol-gel dip coating method. Results of X-ray diffraction analysis indicated that the crystal structure of the coatings was anatase TiO₂. It was also understood that the size of crystallites reduced with CNT but structural properties and equilibrium phase remain intact. Field emission scanning electron microscope images showed that CNTs dispersed uniformly among 45 nm spherical TiO₂ particles of close relations. These images also showed that CNT promoted cracks on the coated surface. Results of the UV-Vis spectroscopy showed that the visible light range adsorption  increased with CNT and the absorption edge did not significantly differ with the pure TiO₂ layers.. Results of the photoluminescence spectroscopy revealed that the presence of CNT could reduce the pair electron–electron holes recombination which is considered totally undesirable.
 

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In the present study, silica aerogel was evaluated by a two-step catalytic process at the ambient pressure drying, under different synthesis conditions. The effects of  the catalyst and water content in the hydrolysis step on the physical properties of silica aerogel, including density, porosity and shrinkage, were investigated. The results showed that increasing the water content in the hydrolysis step increased the shrinkage of gel network and density of obtained aerogel. Moreover, in the presence of insufficient water, NH₄OH as the condensation catalyst in the gel formation step was more effective on the physical properties of silica aerogel, as compared to HCl as  thehydrolysis catalyst; Moreover, the increase in the NH₄OH content led to lower density and higher porosity. On the other hand, NH₄OH effect on the physical properties of silica aerogel was not noticeable in the presence of enough water content. In the NH₄OH/HCl molar ratio of 6, the best silica aerogel sample was obtained with the density of 0.214 g/cm³, porosity of 90% and shrinkage of 23%