scholarly journals Effect of the Preparation Method on the Physicochemical Properties and the CO Oxidation Performance of Nanostructured CeO2/TiO2 Oxides

Processes ◽  
2020 ◽  
Vol 8 (7) ◽  
pp. 847 ◽  
Author(s):  
Sofia Stefa ◽  
Maria Lykaki ◽  
Dimitrios Fragkoulis ◽  
Vasileios Binas ◽  
Pavlos K. Pandis ◽  
...  

Ceria-based mixed oxides have been widely studied in catalysis due to their unique surface and redox properties, with implications in numerous energy- and environmental-related applications. In this regard, the rational design of ceria-based composites by means of advanced synthetic routes has gained particular attention. In the present work, ceria–titania composites were synthesized by four different methods (precipitation, hydrothermal in one and two steps, Stöber) and their effect on the physicochemical characteristics and the CO oxidation performance was investigated. A thorough characterization study, including N2 adsorption-desorption, X-ray diffraction (XRD), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDS), transmission electron microscopy (TEM) and H2 temperature-programmed reduction (H2-TPR) was performed. Ceria–titania samples prepared by the Stöber method, exhibited the optimum CO oxidation performance, followed by samples prepared by the hydrothermal method in one step, whereas the precipitation method led to almost inactive oxides. CeO2/TiO2 samples synthesized by the Stöber method display a rod-like morphology of ceria nanoparticles with a uniform distribution of TiO2, leading to enhanced reducibility and oxygen storage capacity (OSC). A linear relationship was disclosed among the catalytic performance of the samples prepared by different methods and the abundance of reducible oxygen species.

2020 ◽  
Vol 10 (21) ◽  
pp. 7605
Author(s):  
Sofia Stefa ◽  
Maria Lykaki ◽  
Vasillios Binas ◽  
Pavlos K. Pandis ◽  
Vassilis N. Stathopoulos ◽  
...  

The rational design of highly efficient, noble metal-free metal oxides is one of the main research priorities in the area of catalysis. To this end, the fine tuning of ceria-based mixed oxides by means of aliovalent metal doping has currently received particular attention due to the peculiar metal-ceria synergistic interactions. Herein, we report on the synthesis, characterization and catalytic evaluation of ZnO–doped ceria nanorods (NR). In particular, a series of bare CeO2 and ZnO oxides along with CeO2/ZnO mixed oxides of different Zn/Ce atomic ratios (0.2, 0.4, 0.6) were prepared by the hydrothermal method. All prepared samples were characterized by X-ray diffraction (XRD), N2 physisorption, temperature-programmed reduction (TPR), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) and transmission electron microscopy (TEM). The CO oxidation reaction was employed as a probe reaction to gain insight into structure-property relationships. The results clearly showed the superiority of mixed oxides as compared to bare ones, which could be ascribed to a synergistic ZnO–CeO2 interaction towards an improved reducibility and oxygen mobility. A close correlation between the catalytic activity and oxygen storage capacity (OSC) was disclosed. Comparison with relevant literature studies verifies the role of OSC as a key activity descriptor for reactions following a redox-type mechanism.


Catalysts ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 371 ◽  
Author(s):  
Maria Lykaki ◽  
Sofia Stefa ◽  
Sόnia Carabineiro ◽  
Pavlos Pandis ◽  
Vassilis Stathopoulos ◽  
...  

Ceria has been widely studied either as catalyst itself or support of various active phases in many catalytic reactions, due to its unique redox and surface properties in conjunction to its lower cost, compared to noble metal-based catalytic systems. The rational design of catalytic materials, through appropriate tailoring of the particles’ shape and size, in order to acquire highly efficient nanocatalysts, is of major significance. Iron is considered to be one of the cheapest transition metals while its interaction with ceria support and their shape-dependent catalytic activity has not been fully investigated. In this work, we report on ceria nanostructures morphological effects (cubes, polyhedra, rods) on the textural, structural, surface, redox properties and, consequently, on the CO oxidation performance of the iron-ceria mixed oxides (Fe2O3/CeO2). A full characterization study involving N2 adsorption at –196 °C, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), temperature programmed reduction (TPR), and X-ray photoelectron spectroscopy (XPS) was performed. The results clearly revealed the key role of support morphology on the physicochemical properties and the catalytic behavior of the iron-ceria binary system, with the rod-shaped sample exhibiting the highest catalytic performance, both in terms of conversion and specific activity, due to its improved reducibility and oxygen mobility, along with its abundance in Fe2+ species.


2019 ◽  
Vol 56 ◽  
pp. 17-27
Author(s):  
Van Dat Doan ◽  
Van Thuan Le ◽  
Hoang Sinh Le ◽  
Dinh Hien Ta ◽  
Hoai Thuong Nguyen

In this work, nanosized calcium deficient hydroxyapatite (nCDHA) was synthesized by the precipitation method, and then utilized as an adsorbent for removal of Fe (II), Cu (II), Ni (II) and Cr (VI) ions from aqueous solutions after characterizing it by various techniques as scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX) and BET method. A possible structure of synthesized nCDHA was proposed. The adsorption study indicated that the adsorption equilibrium is well fitted with Langmuir isotherm model with the maximum adsorption capacities followed the order of Fe (II) > Cu (II) > Ni (II) > Cr (VI) with the values of 137.23, 128.02, 83.19 and 2.92 mg/g, respectively. The ion-exchange mechanism was dominant for the adsorption of metal ions onto nCDHA at initial metal concentrations lower than 0.01 mol/L. Along with the ion-exchange mechanism, there was an additional precipitation occurred on the surface of nCDHA in the case of Fe (II) and Cu (II) at initial concentrations higher than 0.01 mol/L.


2011 ◽  
Vol 284-286 ◽  
pp. 684-687
Author(s):  
Chang Yu Li ◽  
Li Li Liu ◽  
Shou Xin Liu

Without using any templates or surfactants, flowerlike α-nickel hydroxide (Ni(OH)2) was successfully synthesized by homogeneous precipitation method. The prepared products were characterized by X-ray powder diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and N2 adsorption-desorption. The prepared Ni(OH)2 is α-phase with specific surface area of 245.0 m2/g and shows flowerlike structure with 4-6 um in diameter.


Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1712
Author(s):  
Appusamy Muthukrishnaraj ◽  
Salma Ahmed Al-Zahrani ◽  
Ahmed Al Otaibi ◽  
Semmedu Selvaraj Kalaivani ◽  
Ayyar Manikandan ◽  
...  

Towards the utilization of Cu2O nanomaterial for the degradation of industrial dye pollutants such as methylene blue and methyl orange, the graphene-incorporated Cu2O nanocomposites (GCC) were developed via a precipitation method. Using Hummers method, the grapheme oxide (GO) was initially synthesized. The varying weight percentages (1–4 wt %) of GO was incorporated along with the precipitation of Cu2O catalyst. Various characterization techniques such as Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), UV–visible diffused reflectance (UV-DRS), Raman spectroscopy, thermo gravimetric analysis (TGA), energy-dispersive X-ray analysis (EDX), and electro chemical impedance (EIS) were followed for characterization. The cabbage-like morphology of the developed Cu2O and its composites were ascertained from field-emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM). In addition, the growth mechanism was also proposed. The results infer that 2 wt % GO-incorporated Cu2O composites shows the highest value of degradation efficiency (97.9% and 96.1%) for MB and MO at 160 and 220 min, respectively. Further, its catalytic performance over visible region (red shift) was also enhanced to an appreciable extent, when compared with that of other samples.


2021 ◽  
Author(s):  
Fatma Unal

Abstract Terbium oxide (Tb2O3) particles (NPs) were synthesized by precipitation method using ammonium carbonate as precipitation agent. Effects of precursor molarity (0.1, 0.15 and 0.2 M) on photoluminescence (PL) behaviour of the NPs were investigated. The presence of the Tb2O3 phase was confirmed by X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR) analyses. Morphological investigations of the produced powders were made by Field Emission Gun-Scanning Electron Microscopy (FEG-SEM). It showed that the morphology of Tb2O3 particles transformed from the nanograin chain to bundles morphology of rod-like as the amount of precursor molarity increased. Emission spectrum were investigated by Photoluminescence (PL) Spectroscopy. All the Tb2O3 particles exhibited the strongest peak at 493 nm ascribed to 5D4-7F6 (magnetic dipole (MD), C2) transition. The increase in the number of C2 sites released from the MD transition with the increase of the precursor molarity caused a negative increase in the b* (yellowness/blueness of the emission) value in the CIE diagram, indicating that the colour shifted to the blue region. The Tb2O3 particles produced by the precipitation method exhibited novel strong cyan colour and the PL emission intensity increased with increasing molarity.


2021 ◽  
Vol 234 ◽  
pp. 00106
Author(s):  
Houda Labjar ◽  
Hassan Chaair

The synthesis of apatite silicated Ca10(PO4)6-x(SiO4)x(OH)2-x (SiHA) with 0≤x≤2 was investigated using a wet precipitation method followed by heat treatment using calcium carbonate CaCO3 and phosphoric acid H3PO4 and silicon tetraacetate SiC8H20O4 (TEOS) in medium of water ethanol, with three different silicate concentrations. After drying, the samples are ground and then characterized by different analytical techniques like X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning electron Microscopy (SEM) and chemical analysis.


RSC Advances ◽  
2014 ◽  
Vol 4 (22) ◽  
pp. 11322-11330 ◽  
Author(s):  
Putla Sudarsanam ◽  
Baithy Mallesham ◽  
D. Naga Durgasri ◽  
Benjaram M. Reddy

Fe-doped CeO2 nano-oxide exhibited superior CO oxidation activity compared to pristine CeO2 due to its facile reducible nature, enhanced lattice strain, and ample oxygen vacancies.


Nanomaterials ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 1173 ◽  
Author(s):  
Guangping Zeng ◽  
Qiaoling Zhang ◽  
Youzhi Liu ◽  
Shaochuang Zhang ◽  
Jing Guo

Nano-TiO2 has always been one of the most important topics in the research of photocatalysts due to its special activity and stability. However, it has always been difficult to obtain nano-TiO2 with high dispersion, a small particle size and high photocatalytic activity. In this paper, nano-TiO2 powder was prepared by combining the high-gravity technique and direct precipitation method in an impinging stream-rotating packed bed (IS-RPB) reactor followed by Fe3+ in-situ doping. TiOSO4 and NH3·H2O solutions were cut into very small liquid microelements by high-speed rotating packing, and the mass transfer and microscopic mixing of the nucleation and growth processes of nano-TiO2 were strengthened in IS-RPB, which was beneficial to the continuous production of high quality nano-TiO2. Pure TiO2 and iron-doped nano-TiO2 (Fe-TiO2) were obtained in IS-RPB and were investigated by means of X-ray diffraction (XRD), Raman, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS) and Brunauer–Emmett–Teller (BET) analysis, which found that pure TiO2 had a particle size of about 12.5 nm, good dispersibility and a complete anatase crystal at the rotating speed of packing of 800 rpm and calcination temperature of 500 °C. The addition of Fe3+ did not change the crystalline structure of TiO2. Iron was highly dispersed in TiO2 without the detection of aggregates and was found to exist in a positive trivalent form by XPS. With the increase of iron doping, the photoresponse range of TiO2 to visible light was broadened from 3.06 eV to 2.26 eV. The degradation efficiency of gaseous toluene by Fe-TiO2 under ultraviolet light was higher than that of pure TiO2 and commercial P25 due to Fe3+ effectively suppressing the recombination of TiO2 electrons and holes; the highest efficiency produced by 1.0% Fe-TiO2 was 95.7%.


Catalysts ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 613
Author(s):  
Hussein Mahdi S. Al-Aani ◽  
Mihaela M. Trandafir ◽  
Ioana Fechete ◽  
Lucia N. Leonat ◽  
Mihaela Badea ◽  
...  

To improve the catalytic performance of an active layered double hydroxide (LDH)-derived CuCeMgAlO mixed oxide catalyst in the total oxidation of methane, it was promoted with different transition-metal cations. Thus, two series of multicationic mixed oxides were prepared by the thermal decomposition at 750 °C of their corresponding LDH precursors synthesized by coprecipitation at constant pH of 10 under ambient atmosphere. The first series of catalysts consisted of four M(3)CuCeMgAlO mixed oxides containing 3 at.% M (M = Mn, Fe, Co, Ni), 15 at.% Cu, 10 at.% Ce (at.% with respect to cations), and with Mg/Al atomic ratio fixed to 3. The second series consisted of four Co(x)CuCeMgAlO mixed oxides with x = 1, 3, 6, and 9 at.% Co, while keeping constant the Cu and Ce contents and the Mg/Al atomic ratio. All the mixed oxides were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) coupled with X-ray energy dispersion analysis (EDX), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption-desorption at −196 °C, temperature-programmed reduction under hydrogen (H2-TPR), and diffuse reflectance UV-VIS spectroscopy (DR UV-VIS), while thermogravimetric and differential thermal analyses (TG-DTG-DTA) together with XRD were used for the LDH precursors. The catalysts were evaluated in the total oxidation of methane, a test reaction for volatile organic compounds (VOC) abatement. Their catalytic performance was explained in correlation with their physicochemical properties and was compared with that of a reference Pd/Al2O3 catalyst. Among the mixed oxides studied, Co(3)CuCeMgAlO was found to be the most active catalyst, with a temperature corresponding to 50% methane conversion (T50) of 438 °C, which was only 19 °C higher than that of a reference Pd/Al2O3 catalyst. On the other hand, this T50 value was ca. 25 °C lower than that observed for the unpromoted CuCeMgAlO system, accounting for the improved performance of the Co-promoted catalyst, which also showed a good stability on stream.


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