SYNTHESIS OF NANOSIZED ZIRCONIUM DIOXIDE, COBALT OXIDE  AND RELATED PHASES IN SUPERCRITICAL CO2 FLUID

This study is devoted to obtaining nanoscale zirconium dioxide, cobalt oxide and related phases by SAS method in supercritical carbon dioxide. The synthesized compounds were characterized by a complex of physico-chemical analytical methods: infrared spectroscopy, differential scanning calorimetry, X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy. The experimental parameters for obtaining the nanoparticles were: pressure 10 MPa, temperature 40 °C, carbon dioxide supply rate 35 g/min, the initial solution supply rate 0.5 ml/min. Individual phases containing zirconium and cobalt, and also samples with zirconium to cobalt molar ratios 3:1, 2:1, 1:1, 2:1 and 1:3 were obtained. The use of zirconium and cobalt acetylacetonates as initial components leads to formation of stable products – nanoparticles of acetates of the corresponding metals in the X-ray amorphous state. When heated to 340-350 °C, the destruction of organometallic complexes to oxides occurs with formation of a continuous series of X-ray amorphous solid solutions in the ZrO2-CoO system. At temperatures above 600 °C, the phases crystallize with the decomposition of solid solutions into ZrO2 and Co3O4. When temperature is above 900 °C, further oxidation of cobalt occurs. Thus, cobalt oxide oxidation into Co3O4 proceeds in two steps, at 600 and 900 °C. For samples of zirconium dioxide with cobalt oxide admixture at a temperature of 700 °C stabilization of the cubic modification is observed which is probably due to the entry of cobalt into the cubic structure of zirconium oxide, which prevents transition to tetragonal and monoclinic modifications.

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CO2 Reduction to Propanol by Copper Foams: A Pre- and Post-Catalysis Study

10.26434/chemrxiv.12022623.v1 ◽

2020 ◽

Author(s):

Jennifer A. Rudd ◽

Ewa Kazimierska ◽

Louise B. Hamdy ◽

Odin Bain ◽

Sunyhik Ahn ◽

...

Keyword(s):

Carbon Dioxide ◽

Photoelectron Spectroscopy ◽

Carbon Capture ◽

Surface Composition ◽

Co2 Reduction ◽

Structural Rearrangement ◽

Copper Electrode ◽

Ex Situ ◽

X Ray ◽

Copper Electrodes

The utilization of carbon dioxide is a major incentive for the growing field of carbon capture. Carbon dioxide could be an abundant building block to generate higher value products. Herein, we describe the use of porous copper electrodes to catalyze the reduction of carbon dioxide into higher value products such as ethylene, ethanol and, notably, propanol. For n-propanol production, faradaic efficiencies reach 4.93% at -0.83 V vs RHE, with a geometric partial current density of -1.85 mA/cm2. We have documented the performance of the catalyst in both pristine and urea-modified foams pre- and post-electrolysis. Before electrolysis, the copper electrode consisted of a mixture of cuboctahedra and dendrites. After 35-minute electrolysis, the cuboctahedra and dendrites have undergone structural rearrangement. Changes in the interaction of urea with the catalyst surface have also been observed. These transformations were characterized ex-situ using scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. We found that alterations in the morphology, crystallinity, and surface composition of the catalyst led to the deactivation of the copper foams.

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pH-controlled synthesis of sustainable lauric acid/SiO2 phase change material for scalable thermal energy storage

Scientific Reports ◽

10.1038/s41598-021-94571-0 ◽

2021 ◽

Vol 11 (1) ◽

Author(s):

Shafiq Ishak ◽

Soumen Mandal ◽

Han-Seung Lee ◽

Jitendra Kumar Singh

Keyword(s):

Electron Microscopy ◽

Phase Change ◽

Lauric Acid ◽

Photoelectron Spectroscopy ◽

Phase Change Materials ◽

Precursor Solution ◽

Thermal Reliability ◽

Scanning Calorimetry ◽

X Ray ◽

Heating And Cooling

AbstractLauric acid (LA) has been recommended as economic, eco-friendly, and commercially viable materials to be used as phase change materials (PCMs). Nevertheless, there is lack of optimized parameters to produce microencapsulated PCMs with good performance. In this study, different amounts of LA have been chosen as core materials while tetraethyl orthosilicate (TEOS) as the precursor solution to form silicon dioxide (SiO2) shell. The pH of precursor solution was kept at 2.5 for all composition of microencapsulated LA. The synthesized microencapsulated LA/SiO2 has been characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-Ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The SEM and TEM confirm the microencapsulation of LA with SiO2. Thermogravimetric analysis (TGA) revealed better thermal stability of microencapsulated LA/SiO2 compared to pure LA. PCM with 50% LA i.e. LAPC-6 exhibited the highest encapsulation efficiency (96.50%) and encapsulation ratio (96.15%) through Differential scanning calorimetry (DSC) as well as good thermal reliability even after 30th cycle of heating and cooling process.

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Synthesis of Ce1−xPdxO2−δ Solid Solution in Molten Nitrate

Catalysts ◽

10.3390/catal10060640 ◽

2020 ◽

Vol 10 (6) ◽

pp. 640

Author(s):

Hideaki Sasaki ◽

Keisuke Sakamoto ◽

Masami Mori ◽

Tatsuaki Sakamoto

Keyword(s):

Electron Microscopy ◽

Solid Solution ◽

Solid Solutions ◽

Photoelectron Spectroscopy ◽

Synthesis Method ◽

X Ray Diffraction ◽

X Ray ◽

Transmission Electron ◽

Co Precipitation ◽

Ionic States

CeO2-based solid solutions in which Pd partially substitutes for Ce attract considerable attention, owing to their high catalytic performances. In this study, the solid solution (Ce1−xPdxO2−δ) with a high Pd content (x ~ 0.2) was synthesized through co-precipitation under oxidative conditions using molten nitrate, and its structure and thermal decomposition were examined. The characteristics of the solid solution, such as the change in a lattice constant, inhibition of sintering, and ionic states, were examined using X-ray diffraction (XRD), scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM−EDS), transmission electron microscopy (TEM)−EDS, and X-ray photoelectron spectroscopy (XPS). The synthesis method proposed in this study appears suitable for the easy preparation of CeO2 solid solutions with a high Pd content.

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A Highly Sensitive Room Temperature CO2 Gas Sensor Based on SnO2-rGO Hybrid Composite

Materials ◽

10.3390/ma14030522 ◽

2021 ◽

Vol 14 (3) ◽

pp. 522

Author(s):

Zhi Yan Lee ◽

Huzein Fahmi bin Hawari ◽

Gunawan Witjaksono bin Djaswadi ◽

Kamarulzaman Kamarudin

Keyword(s):

Electron Microscopy ◽

Carbon Dioxide ◽

Gas Sensor ◽

Photoelectron Spectroscopy ◽

Hybrid Composite ◽

Room Temperature ◽

Co2 Gas ◽

X Ray ◽

Wide Range ◽

Co2 Gas Sensor

A tin oxide (SnO2) and reduced graphene oxide (rGO) hybrid composite gas sensor for high-performance carbon dioxide (CO2) gas detection at room temperature was studied. Since it can be used independently from a heater, it emerges as a promising candidate for reducing the complexity of device circuitry, packaging size, and fabrication cost; furthermore, it favors integration into portable devices with a low energy density battery. In this study, SnO2-rGO was prepared via an in-situ chemical reduction route. Dedicated material characterization techniques including field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), energy dispersive X-ray (EDX) spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS) were conducted. The gas sensor based on the synthesized hybrid composite was successfully tested over a wide range of carbon dioxide concentrations where it exhibited excellent response magnitudes, good linearity, and low detection limit. The synergistic effect can explain the obtained hybrid gas sensor’s prominent sensing properties between SnO2 and rGO that provide excellent charge transport capability and an abundance of sensing sites.

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X-ray photoelectron spectroscopy study of sodium germanate glass containing cobalt oxide

Journal of Non-Crystalline Solids ◽

10.1016/0022-3093(92)90011-8 ◽

1992 ◽

Vol 151 (1-2) ◽

pp. 71-80 ◽

Cited By ~ 3

Author(s):

M.A. Salim ◽

E.E. Khawaja

Keyword(s):

Cobalt Oxide ◽

Photoelectron Spectroscopy ◽

Spectroscopy Study ◽

Germanate Glass ◽

X Ray

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Preparation and Characterization of Ni2+-Montmorillonite/Polyvinyl Alcohol Water-Soluble Nanocomposite Film

Polymers and Polymer Composites ◽

10.1177/096739110501300811 ◽

2005 ◽

Vol 13 (8) ◽

pp. 839-846 ◽

Cited By ~ 4

Author(s):

Li-Ping Wang ◽

Yun-Pu Wang ◽

Fa-Ai Zhang

Keyword(s):

Polyvinyl Alcohol ◽

Photoelectron Spectroscopy ◽

Thermal Characteristics ◽

Water Soluble ◽

Scanning Calorimetry ◽

Xps Spectra ◽

X Ray ◽

Alcohol Water ◽

Ft Ir ◽

Silicate Layers

A new type of nano-composite film was prepared from polyvinyl alcohol, Ni2+-montmorillonite (Ni2+-MMT), defoamer, a levelling agent and a plasticizer. Its thermal characteristics were studied by Differential Scanning Calorimetry (DSC). The intermolecular interactions were measured by Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the tensile strength (TS) and elongation at break (%E) were measured. The microstructures were studied by X-ray diffraction (XRD) and atomic force microscopy (AFM). FT-IR and XPS spectra indicated that cross-linking has taken place between PVA and Ni2+-MMT. XRD and AFM indicate that the PVA molecules had inserted themselves into the silicate layers of MMT, exfoliating them and dispersing them randomly into the PVA matrix. Compared to pure PVA film, the TS of the films was increased and %E decreased when the Ni2+-Montmorillonite was added and the dissolution temperature of the film was also reduced.

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Thermal solid-state Z/E isomerization of 2-alkylidene-4-oxothiazolidines: Effects of non-covalent interactions

Journal of the Serbian Chemical Society ◽

10.2298/jsc100607038d ◽

2011 ◽

Vol 76 (3) ◽

pp. 317-328 ◽

Cited By ~ 4

Author(s):

Zdravko Dzambaski ◽

Milovan Stojanovic ◽

Marija Baranac-Stojanovic ◽

Dragica Minic ◽

Rade Markovic

Keyword(s):

Solid State ◽

1H Nmr Spectroscopy ◽

Amorphous State ◽

Intramolecular Hydrogen Bonding ◽

Scanning Calorimetry ◽

X Ray ◽

Configurational Isomerization ◽

Non Covalent Interactions ◽

Intramolecular Hydrogen ◽

Covalent Interactions

Configurational isomerization of stereo-defined 5-substituted and unsubstituted 2-alkylidene-4-oxothiazolidines 1 in the solid state, giving the Z/E mixtures in various ratios, was investigated by 1H-NMR spectroscopy, X-ray powder crystallography and differential scanning calorimetry (DSC). The Z/E composition can be rationalized in terms of non-covalent interactions, involving intermolecular and intramolecular hydrogen bonding and directional non-bonded 1,5-type S...O interactions. X-Ray powder crystallography, using selected crystalline (Z)-4- oxothiazolidine substrates, revealed transformation to the amorphous state during the irreversible Z ? E process. A correlation between previous results on the Z/E isomerization in solution and now in the solid state was established.

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