Flash Synthesis of Tetragonal-ZrO2 Nanostructures by Microwave-Induced Combustion Process

2013 ◽  
Vol 750-752 ◽  
pp. 228-231 ◽  
Author(s):  
Yan Qin Xu ◽  
Sheng Wu Du ◽  
Jun Gao ◽  
Yuan Cao ◽  
Chang Guo Chen ◽  
...  

The synthesis used urea and Zr (NO3)4·5H2O as material to prepare tetragonal-ZrO2 nanocrystals through microwave-induced combustion process. The tetragonal-ZrO2 nanocrystals were characterized by X-ray diffraction (XRD). The effect of Zr4+/urea molar ratio on the synthesis of tetragonal-ZrO2 were studied. It was found that tetragonal-ZrO2 crystal would be better when the Zr4+/urea molar ratio was larger than 1:3.The SEM images of the samples showed the hollow structures formed at different levels of molar ratio of Zr4+/urea. This method is a simple but effective route to prepare tetragonal-ZrO2 nanocrystals.

2011 ◽  
Vol 695 ◽  
pp. 429-432 ◽  
Author(s):  
Jun Zhou ◽  
Xin Zhe Lan ◽  
Ping Ren ◽  
Qiu Li Zhang ◽  
Yong Hui Song ◽  
...  

The flower-sphere molybdenum disulfide has been synthesized by reaction of Na2MoO4 and CS(NH2)2 with NH2OH·HCl or H2C2O4 as reductant. The microstructure and chemical composition of the product were characterized by means of X-ray diffraction and scanning electron microscope. XRD patterns showed that the molar ratio of Mo to S had a great effect on the purity of the product. When the molar ratio of Mo to S was 1:5, the product was nearly pure MoS2. SEM images showed that the particle size increased as the molar ratio of Mo to S reduced. The MoS2 microspheres had rough surfaces and were constructed with sheet-like structures in the two systems. But the product from the system of NH2OH·HCl as reductant has the bigger particle size, clearer petal-sheets, coarser surface and weaker agglomeration than that from the system H2C2O4 as reductant. The possible chemical reactions in hydrothermal systems were preliminarily discussed.


2018 ◽  
Author(s):  
Tasneem Siddiquee ◽  
Abdul Goni

Chemical treatment of CoX<sub>2</sub><b><sup>. </sup></b>6H<sub>2</sub>O (X = Cl, Br, I) with the potentially tridentate PNP pincer ligand 2,6-bis(di-<i>tert</i>-butylphosphinomethyl)pyridine in 1:1 molar ratio results in cobalt(II) halide-PNP pincer complexes. The effect of the hydrated metal source on molecular structure and geometry of the complexes was studied by single crystal X-ray diffraction analysis. The complexes are neutral and the cobalt center adopts a penta-coordinate system with potential atropisomerization. Within the unit cell there are two distinct molecules per asymmetric unit. One of the two phosphorus atoms in the PNP ligand was observed to be partially oxidized to phosphinoxide. Disorder in the structure reflects a mixture of square pyramidal and distorted tetrahedral geometry.


Processes ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 1238
Author(s):  
Garven M. Huntley ◽  
Rudy L. Luck ◽  
Michael E. Mullins ◽  
Nick K. Newberry

Four naturally occurring zeolites were examined to verify their assignments as chabazites AZLB-Ca and AZLB-Na (Bowie, Arizona) and clinoptilolites NM-Ca (Winston, New Mexico) and NV-Na (Ash Meadows, Nevada). Based on powder X-ray diffraction, NM-Ca was discovered to be mostly quartz with some clinoptilolite residues. Treatment with concentrated HCl (12.1 M) acid resulted in AZLB-Ca and AZLB-Na, the chabazite-like species, becoming amorphous, as confirmed by powder X-ray diffraction. In contrast, NM-Ca and NV-Na, which are clinoptilolite-like species, withstood boiling in concentrated HCl acid. This treatment removes calcium, magnesium, sodium, potassium, aluminum, and iron atoms or ions from the framework while leaving the silicon framework intact as confirmed via X-ray fluorescence and diffraction. SEM images on calcined and HCl treated NV-Na were obtained. BET surface area analysis confirmed an increase in surface area for the two zeolites after treatment, NM-Ca 20.0(1) to 111(4) m2/g and NV-Na 19.0(4) to 158(7) m2/g. 29Si and 27Al MAS NMR were performed on the natural and treated NV-Na zeolite, and the data for the natural NV-Na zeolite suggested a Si:Al ratio of 4.33 similar to that determined by X-Ray fluorescence of 4.55. Removal of lead ions from solution decreased from the native NM-Ca, 0.27(14), NV-Na, 1.50(17) meq/g compared to the modified zeolites, 30 min HCl treated NM-Ca 0.06(9) and NV-Na, 0.41(23) meq/g, and also decreased upon K+ ion pretreatment in the HCl modified zeolites.


Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 346
Author(s):  
Sonam Goyal ◽  
Maizatul Shima Shaharun ◽  
Ganaga Suriya Jayabal ◽  
Chong Fai Kait ◽  
Bawadi Abdullah ◽  
...  

A set of novel photocatalysts, i.e., copper-zirconia imidazolate (CuZrIm) frameworks, were synthesized using different zirconia molar ratios (i.e., 0.5, 1, and 1.5 mmol). The photoreduction process of CO2 to methanol in a continuous-flow stirred photoreactor at pressure and temperature of 1 atm and 25 °C, respectively, was studied. The physicochemical properties of the synthesized catalysts were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The highest methanol activity of 818.59 µmol/L.g was recorded when the CuZrIm1 catalyst with Cu/Zr/Im/NH4OH molar ratio of 2:1:4:2 (mmol/mmol/mmol/M) was employed. The enhanced yield is attributed to the presence of Cu2+ oxidation state and the uniformly dispersed active metals. The response surface methodology (RSM) was used to optimize the reaction parameters. The predicted results agreed well with the experimental ones with the correlation coefficient (R2) of 0.99. The optimization results showed that the highest methanol activity of 1054 µmol/L.g was recorded when the optimum parameters were employed, i.e., stirring rate (540 rpm), intensity of light (275 W/m2) and photocatalyst loading (1.3 g/L). The redox potential value for the CuZrIm1 shows that the reduction potential is −1.70 V and the oxidation potential is +1.28 V for the photoreduction of CO2 to methanol. The current work has established the potential utilization of the imidazolate framework as catalyst support for the photoreduction of CO2 to methanol.


Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 931
Author(s):  
Ioana-Codruţa Mirică ◽  
Gabriel Furtos ◽  
Ondine Lucaciu ◽  
Petru Pascuta ◽  
Mihaela Vlassa ◽  
...  

The aim of this research was to develop new electrospun membranes (EMs) based on polycaprolactone (PCL) with or without metronidazole (MET)/nano-hydroxyapatite (nHAP) content. New nHAP with a mean diameter of 34 nm in length was synthesized. X-ray diffraction (XRD) and attenuated total reflectance Fourier transform infrared spectroscopy (FTIR-ATR) were used for structural characterization of precursors and EMs. The highest mechanical properties (the force at maximum load, Young’s modulus and tensile strength) were found for the PCL membranes, and these properties decreased for the other samples in the following order: 95% PCL + 5% nHAP > 80% PCL + 20% MET > 75% PCL + 5% nHAP + 20% MET. The stiffness increased with the addition of 5 wt.% nHAP. The SEM images of EMs showed randomly oriented bead-free fibers that generated a porous structure with interconnected macropores. The fiber diameter showed values between 2 and 16 µm. The fiber diameter increased with the addition of nHAP filler and decreased when MET was added. New EMs with nHAP and MET could be promising materials for guided bone regeneration or tissue engineering.


2003 ◽  
Vol 67 (6) ◽  
pp. 1243-1251 ◽  
Author(s):  
A. Lu ◽  
D. Zhao ◽  
J. Li ◽  
C. Wang ◽  
S. Qin

AbstractSmall domestic cooking furnaces are widely used in China. These cooking furnaces release SO2 gas and dust into the atmosphere and cause serious air pollution. Experiments were conducted to investigate the effects of vermiculite, limestone or CaCO3, and combustion temperature and time on desulphurization and dust removal during briquette combustion in small domestic cooking furnaces. Additives used in the coal are vermiculite, CaCO3 and bentonite. Vermiculite is used for its expansion property to improve the contact between CaCO3 and SO2 and to convey O2 into the interior of briquette; CaCO3 is used as a chemical reactant to react with SO2 to form CaSO4; and bentonite is used to develop briquette strength. Expansion of vermiculite develops loose interior structures, such as pores or cracks, inside the briquette, and thus brings enough oxygen for combustion and sulphation reaction. Effective combustion of the original carbon reduces amounts of dust in the fly ash. X-ray diffraction, optical microscopy, and scanning electron microscopy with energy dispersive X-ray analysis show that S exists in the ash only as anhydrite CaSO4, a product of SO2 reacting with CaCO3 and O2. The formation of CaSO4 effectively reduces or eliminates SO2 emission from coal combustion. The major factors controlling S retention are vermiculite, CaCO3 and combustion temperature. The S retention ratio increases with increasing vermiculite amount at 950°C. The S retention ratio also increases with increasing Ca/S molar ratio, and the best Ca/S ratio is 2-3 for most combustion. With 12 g of the original coal, 1 to 2 g of vermiculite, a molar Ca/S ratio of 2.55 by adding CaCO3, and some bentonite, a S retention ratio >65% can be readily achieved. The highest S retention ratio of 97.9% is achieved at 950°C with addition of 2 g of vermiculite, a Ca/S ratio of 2.55 and bentonite.


2018 ◽  
Vol 25 (08) ◽  
pp. 1950025
Author(s):  
RAFIK MAIZI ◽  
ATHMANE MEDDOUR ◽  
CÉLINE ROUSSE

The deposition of Ni–Fe thin layers in boric acid and ionic liquid ([BuMePyr][Tf2N]) baths were successfully prepared. The obtained materials have been characterized by X-ray diffraction (XRD), Energy Dispersive X-ray spectroscopy (EDX) and SEM. Meanwhile, these materials were carried out by chronoamperometry or chronopotentiometry by varying the intensity of the current and the deposition potential. The results indicate that the coatings of Ni–Fe alloys were successfully obtained by electroplating on the copper substrates, and the alloys composition shows irregular behavior with polarization. The nickel content in the samples is in the range of 55–90%, but the iron content ranges from 10–30%, when potential deposits were varied from [Formula: see text]2[Formula: see text]V to [Formula: see text]4[Formula: see text]V vs Ni electrode. The results also showed that the thin layers are monophased; they contain the Ni3Fe phase. Further, SEM images of Ni–Fe alloys show the different shapes of particles.


1982 ◽  
Vol 37 (11) ◽  
pp. 1393-1401 ◽  
Author(s):  
Beatrix Milewski-Mahrla ◽  
Hubert Schmidbaur

Reactions of pentamethylantimony (CH3)5Sb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramothylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed.The crystal structures of the hydrogen-dibenzoato (1), hydrogen-ortho-plithalato (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter­actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH3)4Sb-tetrahedron in 1 is distorted by two benzoate oxygon atoms (at 304(2) and 340(2) pin). The cation in 2 is largely undistorted and the anion has a hydrogenphthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate.


2011 ◽  
Vol 412 ◽  
pp. 5-8 ◽  
Author(s):  
Ying Zhang ◽  
Ai Chen ◽  
Hai Rong Wang ◽  
Ze Song Li ◽  
Ying Ping Shen

The present article reports the results of studies related to the synthesis of nanocrystalline ceria powder by combustion process using salt combustion aid. Cerium nitrate as oxidant and urea as fuel were used as reagents, Sodium Chloride was compared as combustion aid. The phase analysis and particle size were compared. The product was characterized by X-ray diffraction, Scanning electron microscopy and Transmission electron microscopy. The results showed that employment of starting fuel with combustion aid resulted in synthesizing nanocrystalline ceria powder with fine agglomerates. By using combustion aid, the energetics of the combustion reaction and particle characteristics have been changed.


2013 ◽  
Vol 785-786 ◽  
pp. 449-454
Author(s):  
Yan Zhao ◽  
Chun Yan Wu ◽  
Dan Qin ◽  
Xin Lai ◽  
Si Wu ◽  
...  

SrWO4 octahedrons, flowers, bundles, ellipsoids and dendrites had been successfully synthesized via surfactant-assisted method. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), photo-luminescent spectra techniques (PL) and fourier transrform infrared spectrometer (FTIR). By through various comparison experiments, it can be found that some related experimental parameters including the reagent concentration, [Sr2+]/[WO42-] molar ratio (R), aging temperature and the pH value had great influences on morphology of the products.


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