scholarly journals Magnesium Impregnated on NaX Zeolite Synthesized from Cogon Grass Silica for Fast Production of Fructose via Microwave-Assisted Catalytic Glucose Isomerization

Catalysts ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 981
Author(s):  
Sittichai Kulawong ◽  
Saran Youngjan ◽  
Pongtanawat Khemthong ◽  
Narong Chanlek ◽  
Jatuporn Wittayakun ◽  
...  
Keyword(s):  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
Active Sites ◽  
Nitrate Solution ◽  
Conventional Heating ◽  
X Ray ◽  
Nax Zeolite ◽  
Microwave Assisted ◽  
Glucose Isomerization ◽  
Mg Content

Fructose is a crucial intermediate in the production of several chemical platforms. Fructose is mainly produced from glucose isomerization either through immobilized enzymes or heterogeneous catalysts using a conventional heating source, and this is time-consuming. Thus, this work discloses a fast production of fructose via microwave-assisted catalytic glucose isomerization using Mg catalysts supported on NaX zeolite from cogon grass silica. The catalysts were prepared by the impregnation of magnesium nitrate solution and subsequently transformed into MgO on NaX by calcination. The effect of 3, 6 and 9 wt.% Mg content on NaX on the performance of glucose isomerized to fructose was tested at 90 °C for 15 min. The best catalyst was selected for studying the effect of reaction times of 5, 15, 30 and 60 min. Results from X-ray diffraction (XRD), N2 sorption and CO2 temperature-programmed desorption (CO2-TPD) suggested that crystallinity, surface area and micropore volume decrease but basicity increases with Mg content. The X-ray photoelectron spectroscopy (XPS) result confirmed the presence of mixed phases of MgO and Mg2CO3 in all catalysts. The glucose conversion enhanced with the Mg loading but the fructose yield gave the highest value with Mg of 6 wt.%, probably due to the tuning of high active sites and surface area. The greatest fructose selectivity and yield (71.9% and 25.8%) were obtained within 15 min by microwave-assisted catalytic reaction, shorter than the reported value in the literature, indicating a suitable reaction time. Mg (6 wt.%)/NaX catalyst preserves the original catalytic performance up to three cycles, indicating that it is a promising catalyst for fructose production.

scholarly journals Study of oxygen evolution reaction on thermally prepared xPtOy-(100-x)IrO2 electrodes

2020 ◽  
Vol 10 (4) ◽  
pp. 347-360
Author(s):  
Ollo Kambiré ◽  
Lemeyonouin A. G. Pohan ◽  
Konan H. Kondro ◽  
Lassiné Ouattara
Keyword(s):  
Surface Area ◽  
Oxygen Evolution ◽  
Photoelectron Spectroscopy ◽  
Oxygen Evolution Reaction ◽  
Active Sites ◽  
Platinum Oxide ◽  
Basic Medium ◽  
X Ray ◽  
Tafel Slopes ◽  
Ohmic Drop

The mixed coupled xPtOy-(100-x)IrO2 electrodes (x = 0, 10, 20, 30, 40, 50, 60, 70, 80, 90 and 100) were thermally prepared at 450 °C on titanium supports. The prepared electrodes were firstly physically characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Afterwards, electrochemical characteri­zations were performed by voltammetric (cyclic and linear) methods in different electrolyte media (KOH and HClO4). It is shown that the prepared electrodes are composed by both PtOy (platinum and platinum oxide) and IrO2 (iridium dioxide). For xPtOy-(100-x)IrO2 electrodes having higher content of IrO2, more surface cracks and pores are formed, defining a higher surface area with more active sites. Higher surface area due to presence of both PtOy and IrO2, is for xPtOy-(100-x)IrO2 electrodes in 1 M KOH solution confirmed by cyclic voltammetry at potentials of the oxide layer region. For all prepared electrodes, voltammetric charges were found higher than for PtOy, while the highest voltammetric charge is observed for the mixed 40PtOy-60IrO2 (x = 40) electrode. The Tafel slopes for oxygen evolution reaction (OER) in either basic (0.1 M KOH) or acid (0.1 M HClO4) media were determined from measured linear voltammograms corrected for the ohmic drop. The values of Tafel slopes for OER at PtOy, 90PtOy-10IrO2 and IrO2 in basic medium are 122, 55 and 40 mV dec-1, respectively. For other mixed electrodes, Tafel slopes of 40 mV dec-1 were obtained. Although proceeding by different OER mechanism, similar values of Tafel slopes were obtained in acid medium, i.e., Tafel slopes of 120, 60 and 39 mV dec-1 were obtained for PtOy, 90PtOy-10IrO2 and IrO2, and 40 mV dec-1 for other mixed electrodes. The analysis of Tafel slope values showed that OER is more rapid on coupled mixed electrodes than on pure PtOy. For mixed xPtOy-(100-x)IrO2 electrodes, OER is more rapid when the molar percent of PtOy meets the following condition: 0 ˂ x ≤ 80. This study also showed that the mixed coupled electrodes are more electro­cata­lytically active for OER than either PtOy or IrO2 in these two media. 

scholarly journals Effects of Thermal Annealing on the Properties of Zirconium-Doped MgxZn1−XO Films Obtained through Radio-Frequency Magnetron Sputtering

Membranes ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 373
Author(s):  
Wen-Yen Lin ◽  
Feng-Tsun Chien ◽  
Hsien-Chin Chiu ◽  
Jinn-Kong Sheu ◽  
Kuang-Po Hsueh
Keyword(s):  
Magnetron Sputtering ◽  
Radio Frequency ◽  
Photoelectron Spectroscopy ◽  
Annealing Temperature ◽  
Radio Frequency Magnetron ◽  
Radio Frequency Magnetron Sputtering ◽  
X Ray Diffraction ◽  
Free Electrons ◽  
X Ray ◽  
Mg Content

Zirconium-doped MgxZn1−xO (Zr-doped MZO) mixed-oxide films were investigated, and the temperature sensitivity of their electric and optical properties was characterized. Zr-doped MZO films were deposited through radio-frequency magnetron sputtering using a 4-inch ZnO/MgO/ZrO2 (75/20/5 wt%) target. Hall measurement, X-ray diffraction (XRD), transmittance, and X-ray photoelectron spectroscopy (XPS) data were obtained. The lowest sheet resistance, highest mobility, and highest concentration were 1.30 × 103 Ω/sq, 4.46 cm2/Vs, and 7.28 × 1019 cm−3, respectively. The XRD spectra of the as-grown and annealed Zr-doped MZO films contained MgxZn1−xO(002) and ZrO2(200) coupled with Mg(OH)2(101) at 34.49°, 34.88°, and 38.017°, respectively. The intensity of the XRD peak near 34.88° decreased with temperature because the films that segregated Zr4+ from ZrO2(200) increased. The absorption edges of the films were at approximately 348 nm under 80% transmittance because of the Mg content. XPS revealed that the amount of Zr4+ increased with the annealing temperature. Zr is a potentially promising double donor, providing up to two extra free electrons per ion when used in place of Zn2+.

scholarly journals Organosilane-functionalization of nanostructured indium tin oxide films

2016 ◽  
Vol 6 (6) ◽  
pp. 20160056 ◽  
Author(s):  
R. Pruna ◽  
F. Palacio ◽  
M. Martínez ◽  
O. Blázquez ◽  
S. Hernández ◽  
...  
Keyword(s):  
Surface Area ◽  
Indium Tin Oxide ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Annealing Treatment ◽  
Electrochemical Analysis ◽  
Cyclic Voltammograms ◽  
X Ray ◽  
Chip Technology ◽  
Significant Difference

Fabrication and organosilane-functionalization and characterization of nanostructured ITO electrodes are reported. Nanostructured ITO electrodes were obtained by electron beam evaporation, and a subsequent annealing treatment was selectively performed to modify their crystalline state. An increase in geometrical surface area in comparison with thin-film electrodes area was observed by atomic force microscopy, implying higher electroactive surface area for nanostructured ITO electrodes and thus higher detection levels. To investigate the increase in detectability, chemical organosilane-functionalization of nanostructured ITO electrodes was performed. The formation of 3-glycidoxypropyltrimethoxysilane (GOPTS) layers was detected by X-ray photoelectron spectroscopy. As an indirect method to confirm the presence of organosilane molecules on the ITO substrates, cyclic voltammetry and electrochemical impedance spectroscopy (EIS) were also carried out. Cyclic voltammograms of functionalized ITO electrodes presented lower reduction-oxidation peak currents compared with non-functionalized ITO electrodes. These results demonstrate the presence of the epoxysilane coating on the ITO surface. EIS showed that organosilane-functionalized electrodes present higher polarization resistance, acting as an electronic barrier for the electron transfer between the conductive solution and the ITO electrode. The results of these electrochemical measurements, together with the significant difference in the X-ray spectra between bare ITO and organosilane-functionalized ITO substrates, may point to a new exploitable oxide-based nanostructured material for biosensing applications. As a first step towards sensing, rapid functionalization of such substrates and their application to electrochemical analysis is tested in this work. Interestingly, oxide-based materials are highly integrable with the silicon chip technology, which would permit the easy adaptation of such sensors into lab-on-a-chip configurations, providing benefits such as reduced size and weight to facilitate on-chip integration, and leading to low-cost mass production of microanalysis systems.

scholarly journals Microwave-assisted preparation of ZnS and ZnSe nanocrystals with different morphologies for photodegradation process of organic dyes

2019 ◽  
Author(s):  
Katarzyna Matras-Postolek ◽  
A. Zaba ◽  
S. Sovinska ◽  
D. Bogdal
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Organic Dyes ◽  
Zinc Sulphide ◽  
Conventional Heating ◽  
Bet Surface Area ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Vis Spectroscopy

Zinc sulphide (ZnS) and zinc selenide (ZnSe) and manganese-doped and un-doped with different morphologies from 1D do 3D microflowers were successfully fabricated in only a few minutes by solvothermal reactions under microwave irradiation. In order to compare the effect of microwave heating on the properties of obtained  nanocrystals, additionally the synthesis under conventional heating was conducted additionally in similar conditions. The obtained nanocrystals were systematically characterized in terms of structural and optical properties using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-Vis spectroscopy (DR UV-Vis), Fourier-transform infrared spectroscopy (FT-IR), photoluminescence spectroscopy (PL), X-ray photoelectron spectroscopy (XPS) and Brunauer-Emmett-Teller (BET) surface area analysis. The photocatalytic activity of ZnSe, ZnS, ZnS:Mn and ZnSe:Mn nanocrystals with different morphologies was evaluated by the degradation of methyl orange (MO) and Rhodamine 6G (R6G), respectively. The results show that Mn doped NCs samples had higher coefficient of degradation of organic dyes under ultraviolet irradiation (UV).

scholarly journals Capping Agent Effect on Pd-Supported Nanoparticles in the Hydrogenation of Furfural

Catalysts ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 11 ◽  
Author(s):  
Shahram Alijani ◽  
Sofia Capelli ◽  
Stefano Cattaneo ◽  
Marco Schiavoni ◽  
Claudio Evangelisti ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Active Sites ◽  
Catalytic Performance ◽  
Shielding Effect ◽  
Capping Agents ◽  
X Ray ◽  
Supported Nanoparticles ◽  
Liquid Phase Hydrogenation ◽  
Diallyldimethylammonium Chloride ◽  
Transmission Electron

The catalytic performance of a series of 1 wt % Pd/C catalysts prepared by the sol-immobilization method has been studied in the liquid-phase hydrogenation of furfural. The temperature range studied was 25–75 °C, keeping the H2 pressure constant at 5 bar. The effect of the catalyst preparation using different capping agents containing oxygen or nitrogen groups was assessed. Polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), and poly (diallyldimethylammonium chloride) (PDDA) were chosen. The catalysts were characterized by ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The characterization data suggest that the different capping agents affected the initial activity of the catalysts by adjusting the available Pd surface sites, without producing a significant change in the Pd particle size. The different activity of the three catalysts followed the trend: PdPVA/C > PdPDDA/C > PdPVP/C. In terms of selectivity to furfuryl alcohol, the opposite trend has been observed: PdPVP/C > PdPDDA/C > PdPVA/C. The different reactivity has been ascribed to the different shielding effect of the three ligands used; they influence the adsorption of the reactant on Pd active sites.

scholarly journals Nitrogen-Doped Sponge Ni Fibers as Highly Efficient Electrocatalysts for Oxygen Evolution Reaction

2019 ◽  
Vol 11 (1) ◽  
Author(s):  
Kaili Zhang ◽  
Xinhui Xia ◽  
Shengjue Deng ◽  
Yu Zhong ◽  
Dong Xie ◽  
...  
Keyword(s):  
Oxygen Evolution ◽  
Photoelectron Spectroscopy ◽  
Oxygen Evolution Reaction ◽  
Active Sites ◽  
High Performance ◽  
Active Phase ◽  
X Ray ◽  
Highly Active ◽  
N Doping ◽  
Energy Conversion Devices

Abstract Controllable synthesis of highly active micro/nanostructured metal electrocatalysts for oxygen evolution reaction (OER) is a particularly significant and challenging target. Herein, we report a 3D porous sponge-like Ni material, prepared by a facile hydrothermal method and consisting of cross-linked micro/nanofibers, as an integrated binder-free OER electrocatalyst. To further enhance the electrocatalytic performance, an N-doping strategy is applied to obtain N-doped sponge Ni (N-SN) for the first time, via NH3 annealing. Due to the combination of the unique conductive sponge structure and N doping, the as-obtained N-SN material shows improved conductivity and a higher number of active sites, resulting in enhanced OER performance and excellent stability. Remarkably, N-SN exhibits a low overpotential of 365 mV at 100 mA cm−2 and an extremely small Tafel slope of 33 mV dec−1, as well as superior long-term stability, outperforming unmodified sponge Ni. Importantly, the combination of X-ray photoelectron spectroscopy and near-edge X-ray adsorption fine structure analyses shows that γ-NiOOH is the surface-active phase for OER. Therefore, the combination of conductive sponge structure and N-doping modification opens a new avenue for fabricating new types of high-performance electrodes with application in electrochemical energy conversion devices.

Changes in kaolinite, vermiculite, and smectite clays after adsorption by hydroxy-chromium species

Soil Research ◽  
1998 ◽  
Vol 36 (3) ◽  
pp. 423 ◽  
Author(s):  
Cristina Volzone
Keyword(s):  
Surface Area ◽  
Nitrate Solution ◽  
Basal Spacing ◽  
X Ray Diffraction ◽  
Octahedral Sheet ◽  
Chromium Species ◽  
X Ray ◽  
Micropore Surface Area ◽  
Smectite Clays ◽  
Adsorption Desorption

Kaolinite, vermiculite, and montmorillonites were treated with solutions containing hydroxy-chromium (OH-Cr) species. The OH-Cr solution was prepared by adding 0·2 М NaOH to 0·1 М chromium nitrate solution and allowing the solution to stand at 60°C for 1 day. The samples were characterised by chemical analyses, N2 adsorption-desorption isotherms, and X-ray diffraction. The textural and structural behaviours of kaolinite, vermiculite, and the montmorillonites were analysed in the original samples and after treatment with the polymeric OH-Cr species. The montmorillonites showed higher retention of chromium (19·20%), higher basal spacing (2·06 nm), and higher micropore surface area (276 m2/g) than the vermiculite (3·70%, 1·49 nm, 13 m2/g) and kaolinite (1·15%, 0·73 nm, ~1 m2/g) clays after treatment with the OH-Cr species. In contrast, the external surface area increased from 6 to 9 m2/g for kaolinite and from 18 to 24 m2/g for vermiculite, and decreased from 7 to 4 m2/g for montmorillonite after treatment with the OH-Cr solution. The residual chromium, basal spacing, and texture of the clays after treatment with the OH-Cr species were primarily related to the magnitude of the negative charge originating from the octahedral sheet.

scholarly journals Evolution of the pore and framework structure of NaY zeolite during alkali treatment and its effect on methanol oxidative carbonylation over a CuY catalyst

2020 ◽  
Vol 44 (11-12) ◽  
pp. 710-720
Author(s):  
Lifei Yan ◽  
Tingjun Fu ◽  
Jiajun Wang ◽  
Nilesh Narkhede ◽  
Zhong Li
Keyword(s):  
Catalytic Activity ◽  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
Dimethyl Carbonate ◽  
Alkali Treatment ◽  
Oxidative Carbonylation ◽  
Framework Structure ◽  
Y Zeolite ◽  
Cage Structure ◽  
X Ray

Alkali treatment is widely used on aluminosilicate zeolites with high Si/Al ratios in order to fabricate mesopores in the framework. However, for zeolites with low Si/Al ratios, the effect of alkali treatment on the pore and framework structure needed further study. In this work, Y zeolite is treated with NaOH solutions of different concentrations and is used as the support for Cu-based catalysts for oxidative carbonylation of methanol to dimethyl carbonate. The physicochemical properties of the supports and corresponding catalysts are characterized by N2 adsorption–desorption, X-ray diffraction, X-ray fluorescence, transmission electron microscopy, inductively coupled plasma mass spectrometry, X-ray photoelectron spectroscopy, and H2-temperature-programmed reduction analyses. The results show that no obvious mesopores are formed under alkali treatment, even at high NaOH concentration. However, amorphous species present in the micropores of Y zeolite are removed, which increases the micropore surface area as well as the crystallinity. Simultaneously, the cage structure is partially destroyed, which also leads to a slight increase of the pore volume and surface area. The altered micropore structure eventually increases the content and accessibility of the exchanged Cu species, which is beneficial to the catalytic activity. When the concentration of NaOH is 0.6 M, the space time yield of dimethyl carbonate for the corresponding catalyst was 151.4 mg g−1 h−1 which is 3.3-fold higher than that of the untreated-Y-zeolite-supported Cu catalyst. However, further increasing the alkali treatment strength can seriously destroy the basic aluminosilicate structure of the Y zeolite and decrease its intrinsic ion-exchange capacity. This results in the formation of agglomerated CuO on the catalyst surface, which was not conducive to catalytic activity.

Pulsed Laser Deposition in a Zinc Alloy Corrosion Study

2003 ◽  
Vol 780 ◽  
Author(s):  
R. Guerrero-Penalva ◽  
M.H. Farías ◽  
L. Cota-Araiza
Keyword(s):  
Pulsed Laser Deposition ◽  
Photoelectron Spectroscopy ◽  
Active Sites ◽  
Pulsed Laser ◽  
Laser Deposition ◽  
Reactive Element ◽  
General Mechanism ◽  
Zinc Alloy ◽  
Reactive Element Effect ◽  
X Ray

AbstractA significant improvement in corrosion resistance of the protecting oxide of alloys has been observed when adding small amounts of reactive elements, such as yttrium, this effect has been called reactive element effect (REE). The general mechanism of the REE has not been determined yet. In this work, we study a growing of a yttrium oxide film and its interaction with the phases η and α that constitutes the alloy Zn-22Al-2Cu named ZinalcoTM The alloy's surface was coated by a pulsed laser deposition technique. The deposit is controlled and characterized by x-ray photoelectron spectroscopy. The mechanism by which the reactive element produce its effects in this alloy is explained by the preferential interaction among the active sites related to the zinc rich phase and enhancing aluminum movement toward the surface where it is oxidized and the protection film formed.

Surface Characterization of an Extruded 6060 Al Alloy

2007 ◽  
Vol 29-30 ◽  
pp. 67-70
Author(s):  
Wei Zhang ◽  
Jim Metson ◽  
C.L. Nguyen ◽  
S. Chen
Keyword(s):  
Aluminium Alloy ◽  
Photoelectron Spectroscopy ◽  
Surface Characterization ◽  
Extrusion Direction ◽  
Surface Characteristics ◽  
Al Alloy ◽  
X Ray ◽  
Film Instability ◽  
Mg Content

The surface characteristics of an extruded 6060 aluminium alloy were investigated with X-ray Photoelectron Spectroscopy (XPS). The results revealed that the extruded surface was covered by oxides of aluminium and magnesium. The thickness of aluminium oxide was found to change along the extrusion direction with the thinnest and thickest oxide at the beginning and end of the extrudate, respectively. Magnesium segregation was found on the surface of the extrusion with the highest and lowest Mg concentration at the beginning and end of the extrudate, respectively. This is the inverse result of that expected where increasing Mg content was believed to be associated with film instability and thicker films.

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