Synthesis and Characterization of Aluminum Propionate Sol-Gel Derived Al2O 3

1986 ◽  
Vol 73 ◽  
Author(s):  
J. Covino ◽  
R. A. Nissan
Keyword(s):  
Solid State ◽  
Chemical Shifts ◽  
Sol Gel ◽  
Amorphous Powder ◽  
Synthesis And Characterization ◽  
Crystalline Powder ◽  
X Ray ◽  
Nmr Data ◽  
Half Height

ABSTRACTAl2O3 has been synthesized from aluminum propionate [A1(CO2CH2CH3)3] bySol-Gel techniques. Methods of characterization include: x-ray powder diffraction, scanning electron microscopy (SEM) and nuclear magnetic resonance(NMR). Solution and solid state 13C and 27Al NMR data is coupled with bothx-ray diffraction powder data and SEM in order to understand the transitionfrom sol + gel + amorphous powder + crystalline powder In the sonicated andunsonicated aluminum propionate precursor, and A12O3 powders. Resultsindicate that the sonicated dried powder is crystalline, having the γA12O3structure while the unsonicated dried powder is amorphous and crystallizesat 800°C with the a A12O3 structure. These differences in crystallinity arefurther substantiated by solid state 27AL NMR chemical shifts and linewidths at half height.

Synthesis and characterization of the binuclear diamido titanium chalcogenides [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, Te)

2002 ◽  
Vol 80 (11) ◽  
pp. 1524-1529 ◽  
Author(s):  
Tianle Zhang ◽  
Warren E Piers ◽  
Masood Parvez
Keyword(s):  
Solid State ◽  
Key Words ◽  
Synthesis And Characterization ◽  
Catalyst Precursor ◽  
Tellurium Atom ◽  
Titanium Complex ◽  
X Ray ◽  
X Ray Crystallography ◽  
Atom Source

Reaction of McConville's chelating amido titanium complex [(Ar)NCH2CH2CH2N(Ar)]Ti(CH3)2 (Ar = 2,6-i-Pr2C6H3) with either elemental Se or the tellurium atom source Te=PBu3 resulted in the formation of bis-µ-chalcogenido dimers [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, 2; Te, 3) with concommitant loss of EMe2. The dimers 2 and 3 were characterized spectroscopically and via X-ray crystallography. The two compounds are isostructural in the solid state. The tellurido dimer 3 may also be synthesized by reduction of the diamido dichloride [(Ar)NCH2CH2CH2N(Ar)]2TiCl2 with Na–Hg amalgam followed by treatment with Te=PBu3. This dimer is unreactive toward further Te=PBu3 or stannanes such as HSnBu3. Unlike decamethyltitanocene derivatives, the diamido complex is not an effective catalyst precursor for the heterohydrodecoupling of Te=PBu3 and HSnBu3.Key words: diamido titanium complexes, selenides, tellurides.

Potentialities of an Innovative Technique Like 129Xe NMR and of Saxs for the Characterization of Microporous Sol-Gel Derived SiO2

1996 ◽  
Vol 431 ◽  
Author(s):  
L. C. de Menorval ◽  
A. Julbe ◽  
H. Jobic ◽  
J. A. Dalmon ◽  
C. Guizard
Keyword(s):  
Chemical Shifts ◽  
High Surface ◽  
Sol Gel ◽  
Narrow Pore Size Distribution ◽  
X Ray ◽  
Porous Texture ◽  
129Xe Nmr ◽  
Line Shapes ◽  
X Ray Scattering

AbstractAddition of surfactants in TEOS derived sols leads to micro- or mesoporous materials whose porous texture can be varied by changing the surfactant quantity and/or chain length. This series of materials, with a relatively narrow pore size distribution, is well adapted to study the potentialities of an innovative characterization technique like 129Xe Nuclear Magnetic Resonance in comparison with Small Angle X-ray Scattering and N2 adsorption. SAXS revealed a high surface rugosity of the materials and a good correlation with pore hydraulic radius distributions measured by N2 adsorption. Using 129Xe NMR, we have studied the Xe chemical shifts (δXe,) as a function of pXe, and have pointed out several original results showing the importance, for microporous materials, of the NMR line shapes and of the slope of the lines δXe.=f(pXe).

Synthesis and Characterization of Ti, Fe-Doped Mullite-I

2011 ◽  
Vol 217-218 ◽  
pp. 163-168 ◽  
Author(s):  
Lin Xin Tong ◽  
Jin Hong Li ◽  
Jian Cao
Keyword(s):  
Thermal Analysis ◽  
Differential Thermal Analysis ◽  
Phase Separation ◽  
Powder Diffraction ◽  
Sol Gel ◽  
Synthesis And Characterization ◽  
Formation Temperature ◽  
Gel Method ◽  
X Ray

A series of gels with 3Al2O3•2SiO2 were prepared by Sol-gel method and heated at several temperatures for 2 h to synthesize Ti, Fe-doped mullite. The powers were characterized by differential thermal analysis (DSC-TG) and X-ray powder diffraction (XRD). Phase separation was promoted by doping both TiO2 and Fe2O3; with increasing the amount of dopant ions the formation temperature of Si-Al spinel decreased and the formation temperature of mullite increased by TiO2 doping but decreased by Fe2O3 doping. The formation temperature of pure mullite was about 1250-1350 °C.

Synthesis and Characterization of Nano-Calcium Titanate-Based Coated Aluminum Oxide and its Application in Water Analysis of Cr(III) and Cr(VI) Concentration

2010 ◽  
Vol 44-47 ◽  
pp. 2136-2139
Author(s):  
Dong Zhang
Keyword(s):  
Aluminum Oxide ◽  
Sol Gel ◽  
Calcium Titanate ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Composite Adsorbent ◽  
X Ray ◽  
Ph Values ◽  
Adsorption Capability

Nano-calcium titanate-based coated aluminum oxide (ACCTO) was successfully prepared by the citrate acid sol-gel method and characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM). Its application in speciation of Cr(III) and Cr(VI) from water was studied. The conditions of adsorption and elution were investigated. The results show that nanometer calcium titanate could be immobilized on the aluminum oxide firmly, becoming a composite adsorbent. Two forms of chromium showed different adsorption capability at different pH values, Cr (III) selectively retained at pH 8-14, whereas Cr (VI) retained at pH≤2. So separation of the Cr(III) and Cr(VI) is possible. Retained species were eluted with 5mL of 1 mol•L-1 HCl and NaOH. The Cr(III) and Cr(VI) concentration was measured by atomic absorption spectroscopy. The adsorption agent has a promising prospect in removal or enriching and separation of Cr(III) and Cr(VI) in water.

Solid State Synthesis and Characterization of Spintronics Material Cd0.55 Hg0.45 Te

2010 ◽  
Vol 44-47 ◽  
pp. 2299-2306
Author(s):  
H.M.Noor Ul Huda Khan Asghar ◽  
M. Asghar ◽  
M.S. Awan
Keyword(s):  
Solid State ◽  
Synthesis And Characterization ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Conventional Solid State Reaction ◽  
Cubic Crystal ◽  
X Ray ◽  
Edx Analyses ◽  
Scanning Electron

Polycrystalline spintronic material (Cd0.55Hg0.45Te) was synthesized by conventional solid state reaction. The samples ( = 5 mm and T = 1.5 mm) were prepared by uni-axial pressing. Samples were melted at 800°C for 3-2 hours. For chemical analyses, surface morphology and structural analyses, scanning electron microscopy (SEM) equipped with EDX system and X-ray diffraction studies were performed. XRD confirmed the cubic crystal structure. The Lattice constant of (Cd0.55Hg0.45Te) as determined by XRD was 0.6464 nm. The Miller indices (hkl) have been found by using crystallography method. The observed planes were (200), (210) and (331). The EDX analyses showed the typically compositions: Te 24.8% Cd 14.8% Al 5% and O2 46.4 % & C 9% (3 hours treatment) and Te 28.1% Cd 16% Al 4.1% and O2 39.3 %, Si 0.360% & C 12.1% (2 hours treatment) however we could not find any representative peak for Hg in all of the EDX analyses.

scholarly journals Synthesis and Characterization of Sr2CeO4 Phosphor Doped with Erbium

2010 ◽  
Vol 13 (1-2) ◽  
pp. 17
Author(s):  
K.V.R. Murthy ◽  
K. Suresh ◽  
B. Nageswara Rao ◽  
B. Walter Ratna Kumar ◽  
Ch. Atchyutha Rao ◽  
...  
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
Sem Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Rare Earth Ion ◽  
Solid State Reaction Technique ◽  
X Ray ◽  
Pl Emission

<p>The present paper reports the Photoluminescence (PL) of the Sr<sub>2</sub>CeO<sub>4</sub> phosphor, singly doped with Erbium rare-earth ion with different concentrations (0.01, 0.1, 0.2, 0.5 and 1%).The phosphor samples were synthesized using the standard solid state reaction technique. The effect of Er dopant on the structural, morphological, and Photoluminescent properties of the samples are studied with X-ray diffraction (XRD), PL and SEM analysis. The PL emission of undoped Sr<sub>2</sub>CeO<sub>4</sub> phosphor was observed at 470 nm with high intensity followed by the primary Er emissions with good intensity at 525, 530, 549, 557 and 565 nm.</p>

scholarly journals Synthesis and Characterization of Titania-Rice Husk Silica Composites as Photocatalyst

2015 ◽  
Vol 15 (1) ◽  
pp. 36-42 ◽  
Author(s):  
Posman Manurung ◽  
Rudy Situmeang ◽  
Ediman Ginting ◽  
Indra Pardede
Keyword(s):  
Rice Husk ◽  
Sol Gel ◽  
Bet Surface Area ◽  
Synthesis And Characterization ◽  
Ultraviolet Rays ◽  
X Ray Diffraction ◽  
Titanium Butoxide ◽  
X Ray ◽  
Scanning Electron

This article describes the synthesis of titania-silica composites by a sol-gel method using a mixture of silica of rice husk and titanium butoxide sols. Microstructures were examined at calcination temperature in the range of 500 to 700 °C, with temperatures interval of 50 °C. The sintered catalysts were subsequently tested for photodegradation of methylene blue (MB) under ultraviolet and sunlight rays. Physical characteristics were analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM)/energy dispersive X-ray spectroscopy (EDS), and Brunauer-Emmett-Teller (BET). The XRD results did not show the presence of silica crystal phase in each sample. The results showed that the highest BET surface area of samples was obtained at the temperature of 650 °C. In sample calcined 500 °C, the activity of the catalyst on MB was relatively similar in both sunlight and ultraviolet rays.

Synthesis and Characterization of Ag/TiO2 Thin Film via Sol-Gel Method

2018 ◽  
Vol 273 ◽  
pp. 140-145 ◽  
Author(s):  
Dewi Suriyani Che Halin ◽  
Norsuria Mahmed ◽  
Mohd Arif Anuar Mohd Salleh ◽  
A.N. Mohd Sakeri ◽  
Kamrosni Abdul Razak
Keyword(s):  
Surface Morphology ◽  
Spin Coating ◽  
Sol Gel ◽  
Synthesis And Characterization ◽  
Drying Process ◽  
X Ray Diffraction ◽  
X Ray ◽  
Coating Method ◽  
Structural Surface

Ag/TiO2thin films were prepared via sol-gel spin coating method. Structural, surface morphology and optical properties were investigated with the addition of two different amount of silver (Ag). X-ray diffraction pattern shows the sample with pure TiO2, the only phase presence was brookite TiO2. When the Ag content added into the solution, the phase existed for the samples with TiO2doped 0.5g Ag and TiO2doped 1.0g Ag were anatase TiO2with no peak corresponds to Ag phase. The surface morphology of film was characterized by scanning electron microscopy (SEM). The films were annealed at 450 °C and it shows non-uniform films. The films have a large flaky and cracks film which was attributed to surface tension between the film and the air during the drying process. When the solution of sol was added with Ag content, it shows the porous structure with flaky-crack films. With the increasing of the Ag content from 0.5g to 1.0g, the structure is more porous and it is good for the photocatalytic activity. The UV-Vis spectra shows that the film exhibits a low absorbance which was due to the substrate is inhomogeneously covered by the flaky-crack films.

Bioglasses in the SiO2-CaO-P2O5 System

2008 ◽  
Vol 47-50 ◽  
pp. 1063-1066 ◽  
Author(s):  
Costel Birsan ◽  
Cristina Ghitulica ◽  
Ecaterina Andronescu ◽  
Cristina Ionita ◽  
Mihaela Birsan
Keyword(s):  
Body Fluid ◽  
Sol Gel ◽  
Xrd Analysis ◽  
Silica Content ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Physiological Serum ◽  
P2o5 System

The aim of the study was the synthesis and characterization of bioactive osteoinductive glasses, in the SiO2 – CaO – P2O5 system. In order to maintain the bioactive character of bioglasses, for SiO2 contents higher than 60%, the sol – gel method was used for preparation. On the obtained powders, thermal, grain size and X - ray diffraction analysis were performed. The X - ray diffraction emphasized the formation of phosphate phases, whose proportion decreases as the silica content is increased. Later, the powders were thermally treated at temperatures between 1000 and 14000C, the phase composition evolution being monitored through XRD analysis. On the powder suspensions in physiological serum, the evolution of pH was investigated, in order to establish the chemical stability. The behavior of the obtained powders in physiological medium was studied, by immersing samples in simulated body fluid and excerpted after different periods of time.

Synthesis and characterization of molybdenum–tin complexes derived from the molybdenum tricarbonyl anion, [MeGapz3]Mo(CO)3−, and organotin chlorides. X-ray crystal structure of [MeGapz3]Mo(CO)3SnPh3 (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 321-327 ◽  
Author(s):  
Emmanuel C. Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Full Matrix ◽  
X Ray ◽  
Tin Complexes ◽  
Interesting Solution ◽  
Single Bonds

The reaction of the molybdenum tricarbonyl anion, [MeGapz3]Mo(CO)3−, with the organotin chlorides, Ph3SnCl, Me3SnCl, and Me2SnCl2, has yielded a series of complexes in which direct Mo—Sn single bonds are featured. The [MeGapz3]Mo(CO)3SnMe2Cl complex shows an interesting solution behavior in which a transition from a 3:4, or piano stool structure, to a 3:3:1, or capped octahedral arrangement, is thought to occur. The 3:3:1 structure has been demonstrated in the solid state for the [MeGapz3]Mo(CO)3SnPh3 compound by means of a crystal structure determination. Crystals of [methyltris(1-pyrazolyl)gallato-N,N,N](triphenylstannyl)tricarbonylmolybdenum are monoclinic, a = 11.4439(8), b = 19.5116(8), c = 15.2686(12) Å β = 111.370(3)°, Z = 4, space group P21/c. The structure was solved by conventional heavy-atom methods and was refined by full-matrix least-squares procedures to R = 0.025 and Rw = 0.031 for 5259 reflections with I ≥ 3σ(I). Important bond lengths include: Mo—Sn = 2.8579(3), Mo—N = 2.239(2)–2.244(2), Mo—C = 1.967(3)–2.000(3), Sn—C = 2.151(3)–2.166(3), Ga—N = 1.920(3)–1.931(3), and Ga—C = 1.943(4) Å.

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