scholarly journals Preparation and Characterization of Immobilized Molybdenum Complex on Pillared Montmorillonite K-10

Author(s):  
Farah Wahida Harun ◽  
Siti Balkis Mahamat Nor ◽  
Siti Salhah Othman

This study was carried out to immobilize molybdenyl (VI) acetylacetonate (MoO2(acac)2) complex on alumina pillared montmorillonite K-10 (MMT K-10). Pillar MMT K-10 was produced by introducing MMT K-10 with a hydrolysis solution of NaOH with AlCl3. Different concentrations of pillaring solution were prepared in terms of OHto Al3+ ratio (0.5, 1.0, 1.5 and 2.0) to observe the structural characteristics of MMT K-10. The pillared materials were then immobilized with 0.1 M MoO2(acac)2 and were characterized using X-ray diffractometry (XRD), scanning electron microscopy coupled in an energy dispersive X-ray spectrometer (SEM-EDX) and Fourier transform infrared spectroscopy with attenuated total reflection (FTIR-ATR) techniques. FTIR bands at ca. 890 – 930 cm-1 indicate that the Mo complex was immobilized on the surface of pillared MMT K-10 not in between the layers. This is supported by the SEM and XRD analysis where the SEM micrograph showed deposition of Mo on the surface of MMT K-10 as well as no modification of basal spacing was observed by XRD. Meanwhile, the d(001) spacing of the alumina pillared MMT K10 samples were seen to increase slightly as the concentration of OH/Al3+ increased.

2008 ◽  
Vol 15 (03) ◽  
pp. 329-336 ◽  
Author(s):  
YIMIN ZHANG ◽  
SHAOXIAN SONG ◽  
MIN ZHANG ◽  
BIYANG TUO

In this work, a Ti -pillared montmorillonite with high thermal stability has been prepared by using a Na -montmorillonite as the host clay and polyhydroxy-titania ions as the pillaring precursor. The formation of Ti -pillared montmorillonite has been confirmed from the characterizations through X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric–differential scanning calorimeter, and specific surface area analyses. In the preparation of Ti -pillared montmorillonite several parameters, such as the type of solvent in which the synthesis is realized, the ratio of polyhydroxy-titania ions and montmorillonite, the intercalation time, the calcining temperature, and calcining time, were tested to understand their effects on the basal spacing. It was shown that this method could produce a Ti -pillared montmorillonite with the basal spacing of 3.74 nm, specific surface area of 409 m2/g, and mean pore size of 2.94 nm, as well as a high thermal stability up to 900°C.


2020 ◽  
Vol 849 ◽  
pp. 113-118
Author(s):  
Yayat Iman Supriyatna ◽  
Slamet Sumardi ◽  
Widi Astuti ◽  
Athessia N. Nainggolan ◽  
Ajeng W. Ismail ◽  
...  

The purpose of this study is to characterize Lampung iron sand and to conduct preliminary experiments on the TiO2 synthesis which can be used for the manufacturing of functional food packaging. The iron sand from South Lampung Regency, Lampung Province that will be utilized as raw material. The experiment was initiated by sieving the iron sand on 80, 100, 150, 200 and 325 mesh sieves. Analysis using X-Ray Fluorescence (XRF) to determine the element content and X-Ray Diffraction (XRD) to observe the mineralization of the iron sand was conducted. The experiment was carried out through the stages of leaching, precipitation, and calcination. Roasting was applied firstly by putting the iron sand into the muffle furnace for 5 hours at a temperature of 700°C. Followed by leaching using HCl for 48 hours and heated at 105°C with a stirring speed of 300 rpm. The leaching solution was filtered with filtrate and solid residue as products. The solid residue was then leached using 10% H2O2 solution. The leached filtrate was heated at 105°C for 40 minutes resulting TiO2 precipitates (powder). Further, the powder was calcined and characterized. Characterization of raw material using XRF shows the major elements of Fe, Ti, Mg, Si, Al and Ca. The highest Ti content is found in mesh 200 with 9.6%, while iron content is about 80.7%. While from the XRD analysis, it shows five mineral types namely magnetite (Fe3O4), Rhodonite (Mn, Fe, Mg, Ca) SiO3, Quart (SiO2), Ilmenite (FeOTiO2) and Rutile (TiO2). The preliminary experiment showed that the Ti content in the synthesized TiO2 powder is 21.2%. The purity of TiO2 is low due to the presence of Fe metal which is dissolved during leaching, so that prior to precipitation purification is needed to remove impurities such as iron and other metals.


Author(s):  
M.T. Blatchford ◽  
A.J. Horlock ◽  
D.G. McCartney ◽  
P.H. Shipway ◽  
J.V. Wood

Abstract In this paper, the production of NiCr-TiC powder by SHS, suitable for HVOF spraying, is discussed together with results on the microstructure and coating properties. Compacts for SHS were prepared by mixing elemental Ti and C with pre-alloyed Ni-20wt.% Cr powder to give an overall composition of 35wt.% NiCr and 65wt.% TiC. These were then ignited and a self-sustaining reaction proceeded to completion. Reacted compacts were crushed, sieved, and classified to give feedstock powders in size ranges of 10-45 µm and 45-75 µm. All powder was characterized prior to spraying based on particle size distribution, x-ray diffraction (XRD), and scanning electron microscopy (SEM/EDS). Thermal spraying was performed using both H2 and C3H6 as fuel gases in a UTP/Miller Thermal HVOF system. The resulting coatings were characterized by SEM and XRD analysis, and the microstructures correlated with powder size and spray conditions. Abrasive wear was determined by a modified 'dry sand rubber wheel' (DSRW) test and wear rates were measured. It has been found that wear rates comparable to those of HVOF sprayed WC-17wt% Co coatings can be achieved.


Author(s):  
Tarun Goyal ◽  
T. S. Sidhu ◽  
R. S. Walia

This study reveals the successful low pressure cold spray deposition of near-uniform, defect free and dense copper coatings approximately 700-1900 µm thick, on Al alloy for electro-technical applications. The micro structural characteristics of the deposits have been studied using the combined techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS) and electron-probe micro analysis (EPMA). The coatings exhibited characteristic splat-like, layered morphologies due to the deposition of solid powder particles which appeared to have been plastically deformed on impact to the substrate. The developed coatings have a dense (in the range of 3090-5015 kg/m3)and nearly uniform microstructure, with almost uniform hardness values in the range of 120 -140 Hv, and electrical conductivity in the range of 23-30 MS/m. EDAX, XRD and EPMA results revealed that the main constituent in the coating is Cu.


Clay Minerals ◽  
1988 ◽  
Vol 23 (4) ◽  
pp. 367-377 ◽  
Author(s):  
D. H. Doff ◽  
N. H. J. Gangas ◽  
J. E. M. Allan ◽  
J. M. D. Coey

AbstractPillared smectites in which the pillars consist of iron oxide are expected to have interesting and unusual magnetic properties. Several possible routes by which such materials might be made have been investigated, namely intercalation of hydroxy-Fe(III) polycations, mixed hydroxy-Fe(III)/Al polycations, phenanthroline-Fe(II) cations, and trinuclear Fe(III) acetato cations into Na-montmorillonite. Only the last of these yielded a pillared clay (PILC) on calcination. The products have been characterized using X-ray powder diffraction and 57Fe Mössbauer spectroscopy. The precursor Fe-PILC has a d-spacing of 21 Å and expands to 23 Å on solvation with glycol. The calcined Fe-PILC has a d-spacing of 19 Å (gallery height 9·4 Å) and does not expand with glycol, confirming cross-linking of the layers. From Mössbauer spectra at 4·2 K it is estimated that there are of the order of some hundred Fe atoms per pillar.


2012 ◽  
Vol 727-728 ◽  
pp. 1473-1478
Author(s):  
Mariaugusta Ferreira Mota ◽  
Fabricio Machado ◽  
Meiry Glaúcia Freire Rodrigues

This work presents an experimental study focusing on the preparation and characterization of modified natural green clay-mud with quaternary ammonium salts of chloride and alkyl dimethyl benzyl ammonium chloride (Dodigen) and dimethyl stearyl ammonium chloride (Praepagen). X ray Diffraction (XRD), infrared spectroscopy (IR) and expansion tests (adsorption capacity and Foster swelling) measurements were performed in order to evaluate the performance of the ion exchange reactions and the degree of affinity with oil products. It is observed an increasing in the XRD basal spacing of the modified clays (1.96 nm and 2.25 nm for Praepagen and Dodigen salts, respectively) in comparison to the observed value (1.56 nm) for the natural clay. The IR results showed that salts were successfully incorporated to natural clay structure. Based on the expansion tests the organoclays presented the best efficiency independent on the kind of solvent used in comparison with the natural clay performance.


2013 ◽  
Vol 746 ◽  
pp. 49-52 ◽  
Author(s):  
Peng Quan Yao ◽  
Lin Hua Zhu ◽  
Jin Yang ◽  
Tian Si

In this work, the liquid phase catalytic isomerization of α-pinene over alumina-pillared montmorillonitewas investigated, and the influence of reaction temperature, reaction time and amount of the catalyston the conversion of α-pinenewere discussed systematically, and the optimum reaction conditions forisomerization of α-pineneover alumina-pillared montmorillonitewere obtained. The basal spacing of thealumina-pillared montmorillonite was characterized by X-ray diffraction, and the liquid reactant was separated and identified by gas chromatography. The result showed that alumina-pillared montmorillonite with 1.83nm of basal spacing exhibited a high catalytic activity for the isomerization of α-pinene, and 97.4% conversion of α-pinene was achievedat 373K for 3hwhen the mass ratio of catalyst to α-pinene was 1/10.


CrystEngComm ◽  
2018 ◽  
Vol 20 (20) ◽  
pp. 2861-2867 ◽  
Author(s):  
Yanfang Lou ◽  
Chulho Song ◽  
Yanna Chen ◽  
Loku Singgappulige Rosantha Kumara ◽  
Natalia Palina ◽  
...  

The structural characteristics of a selective growth GaN substrate were inherited from an Al2O3 substrate and then transferred to homoepitaxial thin films.


Materials ◽  
2019 ◽  
Vol 12 (5) ◽  
pp. 821 ◽  
Author(s):  
H.S. Ali ◽  
Ali Alghamdi ◽  
G. Murtaza ◽  
H.S. Arif ◽  
Wasim Naeem ◽  
...  

In this work, microemulsion method has been followed to synthesize vanadium-doped Zn1−xVxO (with x = 0.0, 0.02, 0.04, 0.06, 0.08, and 0.10) nanoparticles. The prepared samples are characterized by several techniques to investigate the structural, morphology, electronic, functional bonding, and optical properties. X-ray diffractometer (XRD) analysis confirms the wurtzite phase of the undoped and V-doped ZnO nanoparticles. Variation in the lattice parameters ensures the incorporation of vanadium in the lattice of ZnO. Scanning electron microscopy (SEM) shows that by increasing contents of V ions, the average particle size increases gradually. X-ray Absorption Near Edge Spectroscopy (XANES) at the V L3,2 edge, oxygen K-edge, and Zn L3,2 edge reveals the presence and effect of vanadium contents in the Zn host lattice. Furthermore, the existence of chemical bonding and functional groups are also asserted by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). UV–Visible analysis shows that by increasing V+ contents, a reduction up to 2.92 eV in the energy band gap is observed, which is probably due to an increase in the free electron concentration and change in the lattice parameters.


2012 ◽  
Vol 616-618 ◽  
pp. 1732-1735 ◽  
Author(s):  
Xi Hai Shen ◽  
Yu Gang Zheng ◽  
Liang Chang ◽  
Jin Jia Guo ◽  
Song Bin Ye ◽  
...  

Aiming at the glass-to-metal seals serving in the Solar Thermal Power (STP), glass-to-metal vacuum brazed joints were studied. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis were performed to examine the microstructure and element contents of interface seam on the glass-to-metal vacuum brazed joints. Also, the compositional concentration of the interface seam was measured by using energy dispersive spectroscopy (EDS).


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