scholarly journals Solvothermally derived Me2(H2O)4(5SSA)3·DMF and Me2(H2O)4(4NSA)2·DMF: Application as Biginelli reaction catalysts

Chemija ◽  
2019 ◽  
Vol 30 (2) ◽  
Author(s):  
Andrius Laurikėnas ◽  
Fatma Yalçin ◽  
Robertas Žilinskas ◽  
Ayse Uztetik Morkan ◽  
Albinas Žilinskas ◽  
...  

The solvothermal synthesis between Me(NO3)x ∙ yH2O (Mex+ = Fe3+, Ni2+, Mn2+, Co2+, Cu2+) and respectively 4-nitrosalycilic (4NSA) and 5-sulfosalicylic (5SSA) acids produced hybrid organic-inorganic compounds composed of Mex+ ions and organic fragments which include three different functional groups, carboxylic, hydroxyl and sulfonic, each coordinated to the Mex+ ions. The phase and chemical composition, microstructure and properties of Me2(H2O)4(5SSA)3·DMF and Me2(H2O)4(4NSA)2·DMF (DMF – dimethylformamide) hybrid compounds were evaluated and discussed. The synthesised materials were characterised by X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and nuclear magnetic resonance (NMR) spectroscopy. The catalytic properties of the obtained compounds were also investigated.

2021 ◽  
Vol 33 (3) ◽  
pp. 583-590
Author(s):  
V.T. Geetha ◽  
S. Induja

Nanocrystalline powder of neodymium substituted iron oxides samples were synthesized through the microwave approach. The synthesized pristine Fe3O4 and Nd-doped Fe3O4 structural properties were analyzed by the X-ray diffraction technique. The microstructural details, morphology and elemental composition were assessed by transmission and scanning electron microscopy attached with EDX. The Fe3O4 nanostructures possess spherical morphology as well as consistent particle size distribution, which is confirmed by HR-SEM. The formation of Fe3O4 with high purity was confirmed by EDX and XRD analysis. The particle size calculated by HR-TEM images and crystallite size through the XRD study showed that the value obtained by both the methods is nearly the same. The catalytic properties of Fe3O4 nanoparticles are examined in the selective oxidation of styrene.


2011 ◽  
Vol 236-238 ◽  
pp. 1712-1716 ◽  
Author(s):  
Hai Tao Liu ◽  
Jun Dai ◽  
Jia Jia Zhang ◽  
Wei Dong Xiang

Bismuth selenide (Bi2Se3) hexagonal nanosheet crystals with uniform size were successfully prepared via a solvothermal method at 160°C for 22 h using bismuth trichloride(BiCl3) and selenium powder(Se) as raw materials, sodium bisulfite(NaHSO3) as a reducing agent, diethylene glycol(DEG) as solvent, and ammonia as pH regulator. Various techniques such as X-ray diffraction (XRD), field-emission scanning electron microscope (FESEM), high-resolution transmission electron microscope (HRTEM), and selected area electron diffraction (SAED) were used to characterize the obtained products. Results show that the as-synthesized samples are pure Bi2Se3 hexagonal nanosheet crystals. A possible growth mechanism for Bi2Se3 hexagonal nanosheet crystals is also discussed based on the experiment.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Hassan Ilyas ◽  
Ishtiaq A. Qazi ◽  
Wasim Asgar ◽  
M. Ali Awan ◽  
Zahir-ud-din Khan

Pure and Ag-TiO2nanoparticles were synthesized, with the metallic doping being done using the Liquid Impregnation (LI) method. The resulting nanoparticles were characterized by analytical methods such as scanning electron micrographs (SEMs), Energy Dispersive Spectroscopy (EDS), and X-ray diffraction (XRD). XRD analysis indicated that the crystallite size ofTiO2was 27 nm to 42 nm while the crystallite size of Ag-TiO2was 11.27 nm to 42.52 nm. The photocatalytic activity of pureTiO2and silver dopedTiO2was tested by photocatalytic degradation ofp-nitrophenol as a model compound. Ag-TiO2nanoparticles exhibited better results (98% degradation) as compared to pureTiO2nanoparticles (83% degradation) in 1 hour for the degradation ofp-nitrophenol. Ag-TiO2was further used for the photocatalytic degradation of 2,4-dichlorphenol (99% degradation), 2,5-dichlorophenol (98% degradation), and 2,4,6-trichlorophenol (96% degradation) in 1 hour. The degree of mineralization was tested by TOC experiment indicating that 2,4-DCP was completely mineralized, while 2,5-DCP was mineralized upto 95 percent and 2,4,6-TCP upto 86 percent within a period of 2 hours.


2019 ◽  
Vol 969 ◽  
pp. 169-174
Author(s):  
R. Sivanand ◽  
S. Chellammal ◽  
S. Manivannan

In this paper, the effect of size variation of cadmium sulphide nanocrystallites which have been prepared by precipitation method is analyzed. These prepared samples were studied using X-ray diffraction (XRD), Scanning electron microscopy (SEM), and Energy dispersive analysis of spectroscopy (EDAX) techniques. SEM analysis represents the morphological nature of prepared samples and EDAX indicates the confirmation of elements present in the sample. XRD analysis determines the size of the samples and identifies the structure using miller indices (h k l values) of the nanocrystallies matches with JCPDS. From the XRD analysis, the size variation which depends on dopant, capping agent are discussed and corresponding results are reported in this paper.


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).


2010 ◽  
Vol 173 ◽  
pp. 102-105 ◽  
Author(s):  
Khairul Arifah Saharudin ◽  
Srimala Sreekantan

In this paper, anodization of Ti foil was carried out in ethylene glycol (EG) containing 5 wt% NH4F solution and 0 to 1.5 wt% of water at 50 V for 60 min. The pH of the bath was kept constant at ~pH7. The crystal structure was studied by X-Ray Diffraction (XRD) analysis, and the morphology was observed via field emission scanning electron microscopy (FESEM). TiO2 nanotube with aspect ratio of 100 was obtained in EG containing less than 1wt % water. The nanotubes wall was very smooth. Increasing the water content > 1wt % results in short nanotubes of approximately 6.2μm with aspect ratio of 62. As anodized, nanotubes were amorphous and annealed at 400 °C promote 100 % anatase phase. Photocatalytic activity of the nanotubes produced at different water content was also evaluated by the degradation of methyl orange and the detail of the observation was discussed thoroughly in this paper.


2014 ◽  
Vol 1019 ◽  
pp. 302-310 ◽  
Author(s):  
Kalenda Mutombo ◽  
Christina Kgomo ◽  
P. Rossouw

The interaction between the Ti6Al4V alloy and the mould materials was investigated. The alpha-case was characterized by Vickers hardness tester, optical and scanning electron microscopy equipped with electron dispersive X-ray spectrometry (EDX). X-ray diffraction (XRD) analysis was performed on as cast and on YFSZ or YZ-Blended face-coats. From the experimental results, a distinct alpha-case formation was revealed. The YFSZ led to a thicker and harder alpha-case than the YZ-Blended face-coat. The EDX revealed the presence of Zr and Si elements in both alpha-cases. Therefore, from experimental results and thermodynamic calculations, pure ZrO2and SiO2may react with Ti.


2010 ◽  
Vol 03 (02) ◽  
pp. 125-129 ◽  
Author(s):  
CAIQUAN ZHANG ◽  
YALI CUI ◽  
DIDI ◽  
KUNPING YAN ◽  
CHAO CHEN ◽  
...  

Facile procedures to synthesize large quantities of uniform and well dispersed magnetite particles in water were developed through a solvothermal method. Magnetite microspheres were obtained by using FeCl 3 · 6H 2 O , urea and polyethylene glycol as the starting materials in ethylene glycol at 200°C for 8 h. The samples were characterized by using X-ray diffraction, transmission electron microscopy, scanning electron microscopy and vibrating sample magnetometry. Experimental results revealed that the particles were well dispersed with uniform particle size and diameters in the range 260 to 280 nm. The saturation magnetization value was 71.5 emu/g with negligible remanence.


2013 ◽  
Vol 738 ◽  
pp. 26-29 ◽  
Author(s):  
Ting Ting Yan ◽  
Yong Shun Cui ◽  
Qing Hua Chen

Hydroxyapatite is well used as bone repair materials, due to its properties that can be combined with strontium to improve mechanical property and degradation property. In this article, hydroxyapatite whiskers with different amount of doped strontium were prepared with diammonium phosphate, calcium nitrate and strontium nitrate at 94 °C. Fourier transform infrared spectroscopy (FTIR) was used to identify the functional groups. X-ray diffraction (XRD) analysis was carried out to study the phase composition and crystallinity of the whisker. The morphology of the whiskers was characterized by scanning electron microscope (SEM). It was indicated that strontium can be doped in hydroxyapatite with proper process and then the strontium-doped hydroxyapatite whiskers were produced successfully.


2012 ◽  
Vol 620 ◽  
pp. 12-16 ◽  
Author(s):  
Abdul Rashid Jamaludin ◽  
Shah Rizal Kasim ◽  
Zainal Arifin Ahmad

The effects of calcium carbonate (CaCO3) addition on the physical properties of ZnO-based crystal glaze batches were investigated. Samples were fired at different gloss firing temperatures ranging from 1180-1220°C with 3 hours soaking at 1060°C crystallization temperature. X-ray diffraction (XRD) analysis identifiedthe crystal phase occurred as willemite (Zn2SiO4) and the scanning electron microscope (SEM) analysis indicated that willemite crystals are in the acicular needle like shape that formed spherulite. The intensities of willemite peaks decreased with CaCO3 addition and completely vanished at 5.0 wt% CaCO3. Varied formation of spherulites developed of the surface of crystal glaze as the flows of the glaze stretched further as the amount of CaCO3 increased.


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