Effect of Sintering Time on the Phase Composition in PFN Ceramics Prepared by Sol-Gel Process

2009 ◽  
Vol 409 ◽  
pp. 317-321 ◽  
Author(s):  
Helena Bruncková ◽  
Ľubomír Medvecký ◽  
Ján Mihalik

Lead iron niobate Pb(Fe0.5Nb0.5)O3 (PFN) ceramics were prepared using sol-gel synthesis by mixing acetates Pb and Fe with Nb-ethylene glycol-tartarate (Pechini) complex at 80°C, calcination of gels at 600°C and sintering at 1150°C for various times. The metastable pyrochlore phase Pb3Nb4O13 in stoichiometric precursor was partially decomposed to perovskite phase Pb(Fe0.5Nb0.5)O3 in ceramics sintered at temperature of 1150°C for 2, 4 and 6 hours. Excess of Pb in molar ratio (Pb:Fe:Nb = 1.2:0.5:0.5) caused the increase of the content of the perovskite phase (~50 vol.%) in nonstoichiometric PFN ceramics sintered at 1150°C for 6 hours while the decrease in perovskite phase content was found in stoichiometric PFN ceramics (~16 vol.%). In microstructures of PFN ceramics sintered at 1150°C for different times, the bimodal grain size distribution was observed with small spherical grains of perovskite phase and larger octahedral grains of pyrochlore phase. EDX analysis confirm that complex types of pyrochlore phases that differ in iron content were present in ceramics.

2013 ◽  
Vol 284-287 ◽  
pp. 41-45
Author(s):  
Chich Kuan Chen

The bioactive properties of hydroxyapatite [HA, Ca10(PO4)6(OH)2] have been demonstrated to be akin to osseous tissue, and provide quick fixation in prosthesis and orthopedics. In this study, sol-gel preparation of hydroxyapatite were arranged for Ca/P=1.67 molar ratio in calcium nitrate [Ca(NO)3.4H2O ] and triethylphosphate [TEP, C6H15PO4] and then dilute in the solvent of ethylene glycol mono-methyl ether [HOCH2CH2OCH3]. Consequently, sintering process was carried out at different temperature for various sintering time to materialize this inorganic polycrystalline phosphate. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM) are applied to investigate the as dried amorphous and calcined hydroxyapatite. Results reveal calcinations at 1000oC prolonged for 30 minutes in air can exhibit crystalline hydroxyapatite.


2014 ◽  
Vol 906 ◽  
pp. 66-71
Author(s):  
Zhen Quan Li ◽  
Qiang Zhen ◽  
Ya Li Wang

High purity ZrSiO4 powder were synthesized using Si (C2H5O)4 and ZrOCl2·8H2O as raw materials by the sol-gel method, LiCl was added as mineralizer to promote crystallization of zircon. The influences of molar ratio of Zr:Si, calcined time and calcined temperature on the synthesis of ZrSiO4 powder were investigated. XRD, SEM and TEM were used to characterize the powders. It was found that when the molar ratio of Zr:Si was 1:1.2, the calcined temperature was 1600°C and the calcined time was 4h, the high purity ZrSiO4 ultrafine powder was obtained. The ZrSiO4 formation began at 1300°C and when the gel was calcined at 1600°Cfor 4 h, the formation rate of ZrSiO4 was up to 95%. SEM and TEM studies reveal a homogeneous product with particle sizes on the order of 0.1-1μm. The IR emissivity of ultrafine ZrSiO4 is 0.892 at the whole wavelength range, and that is up to 0.951 at the wavelength range of 8-14 μm.


2009 ◽  
Vol 24 (8) ◽  
pp. 2541-2546 ◽  
Author(s):  
Eisuke Yokoyama ◽  
Hironobu Sakata ◽  
Moriaki Wakaki

ZrO2 thin films containing silver nanoparticles were prepared using the sol-gel method with Ag to Zr molar ratios [Ag]/[Zr] = 0.11, 0.25, 0.43, 0.67, 1.00, 1.50, and 2.33. After dip coating on glass substrate, coated films were annealed at 200 and 300 °C in air. X-ray diffraction peaks corresponding to crystalline Ag were observed, but a specific peak corresponding to ZrO2 was not observed. At the molar ratio [Ag]/[Zr] = 0.25, the particle size of Ag distributed broadly centered at 17 nm for an annealing temperature of 200 °C and at 25 nm for 300 °C. The films annealed in air at 200 °C showed an absorption band centered at 450 nm because of the silver surface plasmon resonance, whereas films heated at 300 °C in air caused a red shift of the absorption to 500 nm. The absorption peak was analyzed using the effective dielectric function of Ag-ZrO2 composite films modeled with the Maxwell-Garnett expression.


2019 ◽  
Vol 280 ◽  
pp. 03010 ◽  
Author(s):  
Dwi Rasy Mujiyanti ◽  
Muthia Elma ◽  
Mufidah Amalia

Interlayer-free glucose carbonized template silica membranesbased on tetraethyl orthosilicate (TEOS) and glucose were successfullyprepared using an acid-base catalysed sol-gel method for artificial brinewater desalination (7.5% wt NaCl solution %) at temperatures range from25, 40 and 60 °C. These membranes calcined at 250 and 400 °C. Themembranes were fabricated through sol-gel process by using TEOS(tetraethyl orthosilicate); ethanol; nitric acid; ammonia; aquadest andglucose as a template. By molar ratio is 1: 38: 0.0007: 0.0003: 5 and0.25%; 0.5%, 1% w/v glucose as template. The results show the highestwater fluxes of 1.8, 2.2 and 4.8 kg m−2 h−1 for 25, 40 and 60 °Cdesalination process with excellent salt rejections of 99.5, 99.5 and 99.7%, respectively. It was found that the higher the NaCl solution temperature asfeed solution as well as glucose concentration (0.25% to 1% wt) astemplate attached in the silica matrixes, the higher water fluxes eventhough the salt rejection remain the same. This study demonstrates that theorganosilica membranes offered the carbonized silica mesostructuremembranes with excellent separation of water from the hydrated salt ions, particularly for processing brine salt solutions.


2016 ◽  
Vol 697 ◽  
pp. 293-296
Author(s):  
Xiao Yang Zhang ◽  
Xi Wei Qi ◽  
Zhi Yuan Yang ◽  
Li Bao ◽  
Min Zhang

Hydrothermal method and sol-gel process were used to synthesize multiferroic BiFeO3 ceramics. X-ray diffraction, scanning electron microscopy, vickers diamond indenter and three-point bending method were used to investigate the effects of methods on the phase structure, microstructures and mechanical properties. Cold isostatic pressing on the ceramics with two different loads (10 MPa, 200 MPa) was used to illustrate the influence of pressure in mechanical properties. The results show that all samples are crystallized in the perovskite phase. A few small traces of impurity are observed at a 2θ of ~28 o, which are found to be those of Bi2Fe4O9. The SEM images depict that samples prepared by sol-gel process are more uniform and the grain size is slightly larger than that of hydrothermal processed samples. The investigations on the hardness and flexural strength demonstrate the ceramics prepared by hydrothermal method have better mechanical properties than that of sol-gel process, and the mechanical properties can be obviously enhanced by increasing pressure.


2013 ◽  
Vol 815 ◽  
pp. 765-772 ◽  
Author(s):  
Zuo Dong Li ◽  
Dan Liu

Bi3NbTiO9 (BNTO) powders were synthesized by a sol-gel chemical method using niobium oxalates, bismuth nitrate and tetra-n-butyl-titanate as starting materials. In order to determine the influence of the molar ratio of the deionized water to ethylene glycol on the particle morphology and crystallization, different molar ratios, the deionized water/ethylene glycol, were chosen to prepare BNTO powders. Single phase BNTO powders could be obtained at a calcinations temperature of 600°C. Moreover, the possible formation mechanism of BNTO powders was also proposed in this paper. In the baking process, perovskite phase BNTO was formed via a reaction between oxides and bismuth niobium.


2011 ◽  
Vol 326 (1) ◽  
pp. 175-178 ◽  
Author(s):  
Jun Hyuk Choi ◽  
Soo Min Hwang ◽  
Chang Min Lee ◽  
Ji Cheol Kim ◽  
Geun Chul Park ◽  
...  

2012 ◽  
Vol 535-537 ◽  
pp. 2563-2566 ◽  
Author(s):  
Yu Ma ◽  
Hye Ryeon Lee ◽  
Toshinori Tsuru

The synthesis of hydrophobic sol by one-step sol-gel process ammonia catalyzed was investigated. The water molar ratio and catalyst molar ratio were discussed to prevent phase segregation during the hydrolysis and co-condensation of the organic and inorganic precursors. The reactant system with water molar ratio 70 could make the reaction rate of MTES slightly less than that of TEOS, so that the hydrolysis - condensation – gelling reaction with MTES and TEOS as co-precursors could be synchronously. With the increase of the MTES/TEOS molar ratio, the reaction rate of the silica sol preparation decreased, the hydrophobicity of the sol and gel increased as the molar ratio MTES/TEOS change from 0.5~4. But the hydrophobicity of the methyl-modified silica sol and gel prepared with pure MTES in the sol-gel process were slightly lower than that of the methyl-modified silica sol and gel prepared with MTES and TEOS as co-precursors.


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