Structural Investigation of Ceria and Copper Modified Silica from Agricultural Biomass

2015 ◽  
Vol 799-800 ◽  
pp. 32-36
Author(s):  
Jeyashelly Andas ◽  
Fatin Atiqah Md Alyas

Monometallic Ce, Cu and bimetallic Ce-Cu was successfully synthesized at room temperature using silica rice husk (RH) via sol-gel route and were characterized through several physicochemical techniques such as N2adsorption-desorption, XRD and DR/UV-Vis analyses. The prepared materials were designated as RH-10Cu, RH-20Ce and RH-10Cu20Ce. High mesoporosity with Type IV characteristics were evidenced for all the materials. The BET surface area registered for RH-10Cu, RH-20Ce and RH-10Cu20Ce were 396.02, 245.54 and 194.87 m2g-1respectively. Well-dispersion of metal species was clearly evidenced from XRD analysis. The strong interaction between ceria and copper was observed over RH-10Cu20Ce through DR/UV-Vis analysis.


2015 ◽  
Vol 655 ◽  
pp. 108-113 ◽  
Author(s):  
Rui Ping Liu ◽  
Wei Ming Su ◽  
Chang An Wang

Porous Al2O3-SiO2-ZrO2 ceramic composite membranes were fabricated by the sol-gel method. The effects of constitution of the composite sol, dip-coating parameters and calcination parameters on the morphology, phase composition, pore size distribution and BET surface area of the membranes were investigated extensively. The thermogravimetric analysis (TGA)/differential scanning calorimeters (TG/DSC), scanning Electron Microscopy (SEM), XRD analysis and N2 adsorption-desorption analysis was employed for the membranes characterization. TG/DSC curve shows that the suitable calcination temperature of Al2O3-SiO2-ZrO2 membranes is 1000°C. The SEM morphology displays a smooth and free-crack layer of Al2O3-SiO2-ZrO2 composite membranes on the surface of the support after calcination at 1000°C. Furthermore, the membranes were also successfully coated with a good adhesion to the support. The optimal composite membranes were obtained when the moral ratio of Al2O3-SiO2-ZrO2 was 10:2.3:1, the dip-coating parameters were four times dip-coating with every time of 60s respectively.



2020 ◽  
Vol 307 ◽  
pp. 149-153
Author(s):  
Nurul Waheeda Mazlan ◽  
Nafisah Osman ◽  
Oskar Hasdinor Hassan ◽  
Zakiah Mohamed

Abstract. Solid oxide fuel cell (SOFC) is an electrochemical conversion device that undergoes a thermal cycling at various operating temperature where lead to the degradation of its mechanical properties. Electrolyte among the main component in SOFC plays a crucial part in defined the overall performance which facing a lattice expansion event when exposed to heating. Thus, in this paper BaCe0.54Zr0.36Y0.1O3-δ (BCZY) was selected as potential electrolyte for intermediate temperature solid oxide fuel cell (IT-SOFC) to investigate its lattice expansion as a function of temperature. The sample was prepared via a sol gel method and calcined at 1100°C for 10 hours to form a powder and then pressed to become a pellet. To ensure a good densification in such pellet, two-steps sintering processes was indicated at 1500°C and ground to a powder form prior to the lattice expansion measurements. High temperature X-ray diffraction (HT-XRD) was used to study the lattice expansion of sample in the temperature range of 25°C to 700°C with interval 100°C under air atmosphere. HT-XRD analysis was done using X’pert Highscore Plus software and Visual for Electronic and Structural Analysis (VESTA) software was used to observe the crystal structure. Phase and structural analysis of BCZY electrolyte materials were discussed. Apparently, the BCZY shows an average of 97% phase purity from room temperature to 700°C. Rietveld refinement analysis revealed that the BaCe0.54Zr0.36Y0.1O3-δ exhibits cubic symmetrical structure with unit cell, a=b=c that varied from 4.3440Å - 4.3731Å for all the temperature studied. Thus, the expansion percentage for the lattice expansion from room temperature to 700°C was about 12.6 %.



2006 ◽  
Vol 510-511 ◽  
pp. 286-289
Author(s):  
Hao Wang ◽  
Wei Min Wang ◽  
Zheng Yi Fu ◽  
Tohru Sekino ◽  
Koichi Niihara

Mullite-based nanocomposites with embedded FeCr alloy nanoparticles were synthesized by reduction of sol-gel prepared Al5.4(Fe0.8Cr0.2)0.6Si2O13 solid solution in hydrogen. The feature of the formation of FeCr alloy is characterized by XRD analysis. Structural characterization revealed that the intragranular FeCr alloy nanoparticles along with inter-granular iron grains were obtained in as reduced sample. After acid washing, the intergranular metal grains were eliminated. The static magnetic properties of nanocomposite powders were studied using Magnetic Property Measurement System. It is found that part of the intra-granular metal nanoparticles have superparamagnetic behavior at room temperature.



2017 ◽  
Vol 35 (3) ◽  
pp. 454-462
Author(s):  
A. Sayari ◽  
L. El Mir

AbstractZn1-xNixO aerogel nanopowders with nickel concentration in the range of 0.05 ≤ x ≤ 0.25, were synthesized by the sol-gel processing technique and post-annealed in air at 500 °C. Structural, vibrational, thermal and magnetic properties of the as-prepared and annealed Zn1-xNixO powdered samples were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman scattering, thermal gravimetric analysis (TGA) and electron paramagnetic resonance (EPR) spectroscopy. In addition to the ZnNiO phase, XRD analysis revealed the formation of a secondary NiO phase when the Ni content was greater than or equal to 10 %. The TEM images confirm that the particle size is in the range of 20 nm to 40 nm, in accordance with XRD results, and the particles are well dispersed. Raman scattering measurements confirm the wurtzite structure of the synthesized Zn1-xNixO nanopowders and show that intrinsic host-lattice defects are activated when Ni2+ ions are substituted to the Zn sites. Room temperature ferromagnetic order was observed in all of the samples and was strongly dependent on the Ni content and thermal annealing. These results indicate that the observed room temperature ferromagnetism in ZnNiO may be attributed to the substitutional incorporation of Ni at Zn sites.



2013 ◽  
Vol 06 (03) ◽  
pp. 1350031
Author(s):  
HABIBEH HADAD DABAGHI ◽  
MAHMOOD KAZEMZAD ◽  
YADOLAH GANJKHANLOU ◽  
AMIR ALI YUZBASHI

Electrochemistry has been introduced as a powerful tool in order to prepare new organometallic reagents for functionalizing of mesoporous silica. Preparation of the reagents was based on electrochemical oxidation of dihydroxybenzene derivatives in the presence of 3-(trimethoxysilyl)-1-propanethiol as a nucleophile. The mechanisms of electrochemical reactions were studied by voltammetric studies. Mesoporous silica SBA-15 was also synthesized in this work through sol-gel hydrothermal method using Genapol PF-10 as structure directing compound. The prepared mesoporous silica was characterized by FT-IR analysis and Barrett–Joiner–Halenda (BJH) pore size and Brunauer–Emmett–Teller (BET) surface area measurement methods using N2 adsorption–desorption isotherm. Finally, the organometallic reagent was covalently grafted on the surface of mesoporous silica. Functionalizing of this material with the new reagent was confirmed by Fourier transform infrared (FT-IR) spectroscopy. The functionalized mesoporous silica by new reagent can be utilized in biological applications.



2012 ◽  
Vol 455-456 ◽  
pp. 265-270 ◽  
Author(s):  
Ling Jin ◽  
Bin Dai

ZnO/vermiculite as the novel photocatalysts were prepared by two approachs: one is mixtures of ZnO and different acid treated vermiculite, and another is sol-gel method. The acid activated vermiculite as a new promising catalyst support and adsorbent has a large capacity of absorption, high surface area and thermal stability. The activity of catalyst has been interrelated to support and ZnO. Based on the important effect of support on ZnO/vermiculite photocatalysts, treatment of vermiculite by nitric acid of different concentration was studied by evaluated in the photocatalytic decomposition of MB with resulting photocatalysts. BET surface area measurement and X-ray diffraction (XRD) analysis were used to characteristic of ZnO particle in acid treated vermiculite structure and the phase structure and crystallization index of ZnO in the modified vermiculite mineral. Results showed the ZnO-vermiculite combination possessing higher photocatalytic activity due to the synergistic effect when compared to the commercial ZnO.



2013 ◽  
Vol 662 ◽  
pp. 214-217 ◽  
Author(s):  
Li Qin Wang ◽  
Yang Han ◽  
Xiu Jun Fu ◽  
Hai Tao Wu ◽  
E Chang ◽  
...  

Nanoparticals of MCM-41 molecular sieves were synthesized at near room temperature with cetyltrimethylammonium bromide (CTAB) as template agent. The prepared samples were characterized by the means of scanning electron microscopy (SEM), X-ray powder diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), N2 adsorption tests, thermogravimetric and differential thermal analysis (TG-DTA). The results suggested that morphology of MCM-41 molecular sieves samples with high crystallinity was almost uniform spherical, and the particles size was almost less than 100 nm. The adsorption-desorption isotherms were corresponded to typical type IV isotherms with the hysteresis loop of type H2, which showed the samples had mesoporous structure. The pore size distribution of samples were 1.69 nm and 3.58 nm, and the specific surface areas was up to 752.23 m2/g. The decomposition temperature of template agent CTAB was around 327 °C, while the framework for MCM-41molecular sieves was stable. So MCM-41 molecular sieve samples synthesized at near room temperature had excellent physical properties.



2021 ◽  
Author(s):  
NABIL BEN MANSOUR ◽  
Wahid Djeridi ◽  
Lassaad El Mir

Abstract Nanoporous carbon matrix was prepared by the sol-gel process from pyrogallol-formaldehyde (PF) mixtures in water using picric acid as catalyst. For the second sample, nickel oxide nanoparticles were added in the PF matrix to get a PF/NiO hybrid nanocomposite. The samples were heat treated at the pyrolysis temperature of 650°C for two hours. The obtained materials have been characterized by different techniques such as: X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), differential thermalanalysis (DTA),nitrogen adsorption-desorption isotherms, voltage-current characteristics, electrochemical measurementsand UV-Vis-IR absorption. The XRD analysis shows that PF matrix is amorphous while PF/NiO nanocomposite exhibited a metallic phase of nickel. The SEM and TEM images indicated the presence of nickel particles in the PF/NiO nanocomposite which are dispersed randomly in the carbon matrix. The adsorption-desorption of nitrogen revealed that the PF matrix is microporous and the PF/NiO nanocomposite is mesoporous. The adsorption capacities of carbon dioxide (CO2) and methane (CH4) show that the PF matrix has the highest adsorption at low pressures and the PF/NiO nanocomposite tends to adsorb gases better at high pressure. The V(I) characteristics showed that the PF/NiO nanocomposite can be considered as a smart material. Indeed, the characteristic behavior can be adjusted according to the maximum applied current. Electrochemical measurements have shown that the PF/NiO nanocomposite is very promising for the detection of non-enzymatic glucose. The absorption spectra showed that the addition of the NiO nanoparticles increased the disorder. The obtained materials are promoters for various applications such as gas storage, negatronic devices and glucose sensor.



Author(s):  
M. V. Rudenko ◽  
N. V. Gaponenko ◽  
E. B. Chubenko ◽  
E. I. Lashkovskaya ◽  
K. V. Shustsikava ◽  
...  

Erbium-doped barium titanate (BaTiO3:Er) xerogel film with a thickness of about 500 nm was formed on the porous strontium titanate (SrTiO[Formula: see text] xerogel film on Si substrate after annealing at 800[Formula: see text]C or 900[Formula: see text]C. The elaborated structures show room temperature upconversion luminescence under 980 nm excitation with the photoluminescence (PL) bands at 523, 546, 658, 800 and 830 nm corresponding to 2H[Formula: see text]4I[Formula: see text], 4S[Formula: see text]I[Formula: see text], 4F[Formula: see text]I[Formula: see text] and 4I[Formula: see text]4I[Formula: see text] transitions of trivalent erbium. Raman and X-ray diffraction (XRD) analysis of BaTiO3:Er\porous SrTiO3\Si structure showed the presence of perovskite phases. Its excellent up-conversion optical performance will greatly broaden its applications in perovskite solar cells and high-end anti-counterfeiting technologies.



2013 ◽  
Vol 448-453 ◽  
pp. 583-588
Author(s):  
Fen Li ◽  
Guang Hui Yang ◽  
Tao Lei ◽  
Sheng Yu Yang ◽  
Yan Hong Wang ◽  
...  

In this paper, nanocopper oxide is prepared by complexing-precipitate, and the influence of different process parameters on the removal of H2S performance are studied, and make a comparison for two other methods. The results indicate that different complexing agent, the molar ratio of Cu2+/OH- and calcination temperature, etc., effect the desulfurization activity of nanocopper oxide. nanocopper prepared under optimum conditions (the complexing agent is ammonia, the molar ratio of Cu2+/OH- is 1:3.0, calcination temperature is 400 °C) exhibits best desulfurization activity with a H2S breakthrough time of 235 min, this is much longer than that prepared by hydrothermal method and sol-gel method with breakthrough time of H2S only 20 min and 50 min, respectively; XRD analysis shows that the big grain size of nanocopper oxide and low purity are not in favor of H2S adsorption at room temperature.



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