Structure of Zirconia Nanoparticles used for Pillaring of Clay

2001 ◽  
Vol 703 ◽  
Author(s):  
V. A. Sadykov ◽  
T. G. Kuznetsova ◽  
V. P. Doronin ◽  
T. P. Sorokina ◽  
D. I. Kochubei ◽  
...  

ABSTRACTSAXS and EXAFS were applied to study genesis of polynuclear zirconium hydroxyspecies in pillaring solutions as dependent upon the zirconium concentration, addition of alkaline-earth chlorides and aging. After the montmorillonite clay pillaring, the structure of zirconium nanopillars was characterized by applying X-ray structural analysis, UV-Vis, FTIRS of adsorbed CO and nitrogen adsorption isotherms. Main pillaring species appear to be nanorods comprised of several Zr4 tetramers. Basic structural features of the tetramers are preserved in zirconia nanoparticles fixed between alumosilicate layers in pillared clays. In calcined samples, those nanoparticles contain only bridging hydroxyls and/or oxygen anions responsible for bonding within pillars and between pillars and clay sheets.

Sensors ◽  
2020 ◽  
Vol 20 (5) ◽  
pp. 1385 ◽  
Author(s):  
Andrés Rodríguez ◽  
Elio Rico ◽  
Cesar Sierra ◽  
Oscar Rodríguez

Two Covalent Organic Frameworks (COF), named TFP-BZ and TFP-DMBZ, were synthesized using the imine condensation between 1,3,5-triformylphloroglucinol (TFP) with benzidine (BZ) or 3,3-dimethylbenzidine (DMBZ). These materials were deposited, such as films over interdigitated electrodes (IDE), by chemical bath deposition, giving rise to TFP-BZ-IDE and TFP-DMBZ-IDE systems. The synthesized COFs powders were characterized by Powder X-Ray Diffraction (PXRD), Fourier Transform Infrared spectroscopy (FT-IR), solid-state Nuclear Magnetic Resonance (ssNMR), nitrogen adsorption isotherms, Scanning Electron Microscopy (SEM), and Raman spectroscopy, while the films were characterized by SEM and Raman. Ammonia and low molecular weight amine sensing were developed with the COF film systems using the impedance electrochemical spectroscopy (EIS). Results showed that the systems TFP-BZ-IDE and TFP-DMBZ-IDE detect low molecular weight amines selectively by impedimetric analysis. Remarkably, with no significant interference by other atmospheric gas compounds such as nitrogen, carbon dioxide, and methane. Additionally, both COF films presented a range of sensitivity at low amine concentrations below two ppm at room temperature.


2016 ◽  
Vol 16 (1) ◽  
pp. 21-26
Author(s):  
Irwan Irwan ◽  
Surya Lubis ◽  
Muliadi Ramli ◽  
Sheilatina Sheilatina

TiO2/activated carbon derived from waste coffee grounds (TiO2/WCGAC) has been prepared by a sol gel method . Waste coffee ground was chemically activated using hydrochloric acid 0.1 M solution and modified with titanium tetraisopropoxide as TiO2 precursor. The structural features of the photocatalyst was investigated by X-ray diffraction (XRD), scanning electron microscope energy dispersive X-ray spectroscopy (SEM EDX),  Fourier transform infrared spectroscopy (FT-IR) and nitrogen adsorption-desorption. The XRD results showed that TiO2 is anatase and rutile phase, while FTIR spectra confirmed the presence of  Ti-O groups. The specifics surface area of TiO2/WCGAC was higher than that of activated carbon derived from waste coffee grounds. The photocatalytic activity of TiO2/WGCAC has been evaluated for degradation of indigo carmine solution under UV and solar light irradiation. It was found that degradation percentage of indigo carmine under solar light was higher than that of under UV light.


2012 ◽  
Vol 2012 ◽  
pp. 1-19 ◽  
Author(s):  
Katarzyna Siwińska-Stefańska ◽  
Filip Ciesielczyk ◽  
Magdalena Nowacka ◽  
Teofil Jesionowski

The paper reports on characterisation of titanium dioxide and coprecipitated TiO2–SiO2composite material functionalised with selected alkoxysilanes. Synthetic composite material was obtained by an emulsion method with cyclohexane as the organic phase, titanium sulfate as titanium precursor, and sodium silicate solution as precipitating agent were applied. Structures of titania and composite material samples were studied by the wide angle X-ray scattering method. The chemical composition of TiO2–SiO2composite material precipitated was evaluated based on the energy dispersive X-ray spectroscopy technique. The functionalised TiO2and TiO2–SiO2composite material were thoroughly characterised to determine the yield of functionalisation with silanes. The characterisation included determination of dispersion and morphology of the systems (particle size distribution, scanning electron microscope images), adsorption properties (nitrogen adsorption isotherms), and electrokinetic properties (zeta potential).


Materials ◽  
2020 ◽  
Vol 13 (22) ◽  
pp. 5124
Author(s):  
Łukasz J. Wilk ◽  
Agnieszka Ciechanowska ◽  
Elżbieta Kociołek-Balawejder

Hybrid ion exchangers (HIX) containing manganese(IV) oxide (MnO2) based on macroporous and gel-type carboxylic cation exchangers as supporting materials were obtained. The hybrid materials were characterized using scanning electron microscopy with energy dispersive spectrometry (SEM/EDS), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD) and nitrogen adsorption isotherms at 77 K and mercury porosimetry. HIX with introduced MnO2 (20.0–32.8 wt% Mn) were tested for removal of dissolved sulfides from anoxic aqueous solutions with 100–500 mg S2−/dm3 concentrations. The process proceeded effortlessly at pH 10–13 despite unfavorable electrostatic interactions of the reactants. The highest exhibited sorption capacity was 144.3 ± 7.1 mg S2−/g. Approximately 65% of dissolved sulfides were oxidized to S2O32− ions and repelled from HIX structure. On average, 13% of sulfide removal products were adsorbed by the MnO2 surface. The impact of MnO2 load and the ionic form of HIX functional groups on removal of sulfides and resulting products was examined. The mechanism of the process is suggested.


2011 ◽  
Vol 509 (13) ◽  
pp. 4445-4451 ◽  
Author(s):  
Aleksander Zych ◽  
Anke Leferink op Reinink ◽  
Koen van der Eerden ◽  
Celso de Mello Donegá ◽  
Andries Meijerink

2020 ◽  
pp. 73-83
Author(s):  
L. V. Morozova ◽  
◽  
I. A. Drozdova ◽  

The xerogels in the system 0.88 mol.% ZrO2 − 0.12 mol.% CeO2 were obtained by the method of coprecipitation in a neutral (pH = 7) and slightly alkaline (pH = 9) medium under the influence of ultrasound with the size of the agglomerates 70 – 230 nm. It is shown that the coprecipitation of hydroxides of zirconium and cerium at pH = 9 with the use of ultrasonic treatment facilitates the formation of a primary crystal is symbolic of the particles in the xerogel, whose size is ~ 5 nm, whereas the xerogel synthesized in a neutral environment consists only of the x-ray amorphous phase. The effect of pH-precipitation on deposition processes of dehydration of the xerogels and crystallization solid solution based on zirconia oxide in the metastable pseudocubic modification (с′-ZrO2) was discovered. It was found that in the temperature range 500 – 800 °C there is a phase transition с′-ZrO2 → t-ZrO2, the size of the crystallites of the formed tetragonal solid solutions is 8 and 11 nm. The method of low-temperature nitrogen adsorption were investigated dispersion properties and characteristics of the pore structure of the powders of the solid solution Zr0.88Ce0.12O2. It is determined that the specific surface area of t-ZrO2 samples obtained after firing at 800 °C is 117 and 178 m2/g, the total pore volume reaches 0.300 − 0.325 cm3/g, the pore size distribution is monomodal and is in the range of 2 − 8 nm. The effect of thermal “aging” at a temperature of 800 °C (40 h) on the structure and dispersion of the solid solution t-ZrO2 powders was studied.


2021 ◽  
Vol 10 (1) ◽  
pp. 189-200
Author(s):  
Yuan She ◽  
Chong Zou ◽  
Shiwei Liu ◽  
Keng Wu ◽  
Hao Wu ◽  
...  

Abstract Thermoanalysis was used in this research to produce a comparative study on the combustion and gasification characteristics of semi-coke prepared under pyrolytic atmospheres rich in CH4 and H2 at different proportions. Distinctions of different semi-coke in terms of carbon chemical structure, functional groups, and micropore structure were examined. The results indicated that adding some reducing gases during pyrolysis could inhibit semi-coke reactivity, the inhibitory effect of the composite gas of H2 and CH4 was the most observable, and the effect of H2 was higher than that of CH4; moreover, increasing the proportion of reducing gas increased its inhibitory effect. X-ray diffractometer and Fourier-transform infrared spectrometer results indicated that adding reducing gases in the atmosphere elevated the disordering degree of carbon microcrystalline structures, boosted the removal of hydroxyl- and oxygen-containing functional groups, decreased the unsaturated side chains, and improved condensation degree of macromolecular networks. The nitrogen adsorption experiment revealed that the types of pore structure of semi-coke are mainly micropore and mesopore, and the influence of pyrolytic atmosphere on micropores was not of strong regularity but could inhibit mesopore development. Aromatic lamellar stack height of semi-coke, specific surface area of mesopore, and pore volume had a favorable linear correlation with semi-coke reactivity indexes.


Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1519
Author(s):  
Jong Gyeong Kim ◽  
Sunghoon Han ◽  
Chanho Pak

The price and scarcity of platinum has driven up the demand for non-precious metal catalysts such as Fe-N-C. In this study, the effects of phosphoric acid (PA) activation and phosphorus doping were investigated using Fe-N-C catalysts prepared using SBA-15 as a sacrificial template. The physical and structural changes caused by the addition of PA were analyzed by nitrogen adsorption/desorption and X-ray diffraction. Analysis of the electronic states of Fe, N, and P were conducted by X-ray photoelectron spectroscopy. The amount and size of micropores varied depending on the PA content, with changes in pore structure observed using 0.066 g of PA. The electronic states of Fe and N did not change significantly after treatment with PA, and P was mainly found in states bonded to oxygen or carbon. When 0.135 g of PA was introduced per 1 g of silica, a catalytic activity which was increased slightly by 10 mV at −3 mA/cm2 was observed. A change in Fe-N-C stability was also observed through the introduction of PA.


2020 ◽  
Vol 2020 ◽  
pp. 1-9 ◽  
Author(s):  
N. Cruz-González ◽  
O. Calzadilla ◽  
J. Roque ◽  
F. Chalé-Lara ◽  
J. K. Olarte ◽  
...  

In the last decade, the urgent need to environmental protection has promoted the development of new materials with potential applications to remediate air and polluted water. In this work, the effect of the TiO2 thin layer over MoS2 material in photocatalytic activity is reported. We prepared different heterostructures, using a combination of electrospinning, solvothermal, and spin-coating techniques. The properties of the samples were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, UV-Vis diffuse reflectance spectroscopy (UV-Vis-DRS), and X-ray photoelectron spectroscopy (XPS). The adsorption and photocatalytic activity were evaluated by discoloration of rhodamine B solution. The TiO2-MoS2/TiO2 heterostructure presented three optical absorption edges at 1.3 eV, 2.28 eV, and 3.23 eV. The high adsorption capacity of MoS2 was eliminated with the addition of TiO2 thin film. The samples show high photocatalytic activity in the visible-IR light spectrum.


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