Search results for "Calcination"
showing 10 items of 112 documents
Synthesis of Nd:YAG nanopowder using the citrate method with microwave irradiation
2010
Abstract Nd:YAG nanopowders were prepared using the Pechini process with microwave irradiation ( MWs ). A reference sample was also prepared using conventional heating. XRD pattern analysis showed that nanopowder obtained by means of conventional heating and calcination for 1 h at 900 °C has a structure made up of the garnet phase together with the hexagonal phase that disappeared after two additional hours of thermal treatment. The MWs powder calcined for 1 h consists of the single garnet phase. SAXS data analysis indicated that nanoparticles are characterized by a sharp interface. TEM investigation showed crystalline particles with remarkable agglomeration in both samples, although a more…
Synthesis and characterization of mesoporous Mn-MCM-41 materials
2011
Si { 1 H} CP-MAS NMR X-ray photo-emission spectroscopy a b s t r a c t MCM-41 has been synthesized at two different pH using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 ◦ C for 4 h. Mn-MCM-41 powders with different Mn/Si molar ratios were prepared using the incipient wetness method, followed by calcination at 550 ◦C for 5 h. At the end of the impregnation process the powders colour changed from white to brown whose intensity depends on manganese quantity. The materials characterization was performed by X-ray diffraction, N2 adsorption, 29 Si Cross Polarization–Mag…
Surfactant-Assisted Synthesis of Mesoporous Alumina Showing Continuously Adjustable Pore Sizes
1999
Porous materials displaying tailor-made pore sizes and shapes are particularly interesting in a great variety of real and potential applications where molecular recognition is needed, such as shape-selective catalysis, molecular sieving, and selective adsorption. Classically, apart from silica, materials most commonly used for catalysis and catalyst supports have been those based on high surface aluminas, owing to their thermal, chemical, and mechanical stability and their low cost. Earlier aluminas with high surface areas (~500 m/g) had been prepared using structure-directing agents. However, they were X-ray amorphous materials and their porosity was purely textural, characterized by wide …
In-Situ Growth of Ultrathin Films of NiFe-LDHs: Towards a Hierarchical Synthesis of Bamboo-Like Carbon Nanotubes
2014
The synthesis of ultrathin films (UTFs) of NiFe-LDHs has been achieved by means of an in situ hydrothermal approach, leading to a flat disposition of the LDH crystallites on the substrate, in clear contrast to the most common perpendicular orientation reported to date. Experimental factors like time of synthesis or the nature of the substrate, seem to play a crucial role during the growing process. The 2D morphology of the NiFe-LDH crystallites was kept after a calcination procedure, leading to a topotactic transformation into mixed-metal oxide platelets. Hereby, in order to study the catalytic behavior of our samples, a chemical vapor deposition process is explored upon the as-synthesized …
MCM-41, MCM-48 and related mesoporous adsorbents: their synthesis and characterisation
2001
MCM-41, MCM-48, MCM-41 analogue materials and disordered silica xerogels were compared with respect to their long range and short range order, their specific surface area, pore structure and pore structural parameters, pore wall thickness and their surface hydroxyl group concentration. Based on X-ray diffraction data it could be seen that the degree of long range order decreased in the order MCM-41>MCM-48>MCM-41 analogues >amorphous silica xerogels. The particle porosity and pore wall thickness increased in the same sequence such that MCM-41 analogues and amorphous silica xerogels were more stable towards water and water vapour. The concentration of the surface hydroxyl groups increased whe…
Synthesis of self-assembled α-GaOOH microrods and 3D hierarchical architectures with flower like morphology and their conversion to α-Ga2O3
2015
Abstract This report reveals the methodology for the fabrication of α-GaOOH micro rods and micro flowers from gallium nitrate with two different complexing agents. α-GaOOH self-assembled 3D hierarchical architecture, comprising of nanorods and nanoribbbons with a flower like morphology, is fabricated under benign hydrothermal conditions. Calcination of α-GaOOH results in formation of α-Ga 2 O 3 with the retention of morphology. Both gallium oxyhydroxide and gallium oxide microstructures were analyzed with SEM, EDX, TEM and powder X-ray diffraction. α-Ga 2 O 3 micro flowers are furnished with nanorods having ordered diamond like cross section with a diagonal length proportion of 2:1. The hyd…
Incorporation of Mn12single molecule magnets into mesoporous silica
2003
The incorporation of four Mn12 derivatives, namely [Mn12O12(O2CR)16(H2O)4] (R = CH3 (1), CH3CH2 (2), C6H5 (3), C6F5 (4)), into the hexagonal channels of the MCM-41 mesoporous silica has been studied. Only the smallest clusters 1 and 2, i.e. those with compatible size with the pores of MCM-41, could enter into the mesoporous silica. Powder X-ray diffraction analysis, HRTEM images and N2 adsorption–desorption isotherm experiments show that the well-ordered hexagonal structure of MCM-41 is preserved and that the Mn12 clusters are inside the pores. The magnetic properties of the MCM-41/2b nanocomposite material obtained in CH2Cl2 indicate that the structure of the cluster is maintained after in…
Ceramic/metal nanocomposites by lyophilization: Spark plasma sintering and hardness
2014
The present study is focused on the procedure of spray-drying and lyophilization techniques for the preparation of ceramic/metal nanocomposites. The results of the study at all stages are compared with those corresponding to powders conventionally dried by heating in furnace. Starting from aqueous solutions of metal salts and ceramic powders, the procedure follows with spray-drying, lyophilization, calcination of the resulting powders and subsequent Spark Plasma Sintering (SPS). X-ray diffraction analysis of the powders at different stages of the processing routes was used for phase indexing; further characterization was performed by Transmission Electron Microscopy and Energy Dispersive X-…
Preparation of Nanoporous MgAl2O4 by Combined Utilization of Sol-Gel Process and Combustion of Biorenewable Oil
2011
ABSTRACTNanoporous MgAl2O4 particulates with high porosities were successfully prepared from sol-gel reactions, solvent exchange with castor oil and subsequent combustion and calcination at 700 °C. The products were crystalline and semitransparent. Changes in the metal precursor concentrations allowed control of pore volumes from 0.7 to 1.1 cm3/g and average pore sizes from 14 to 19 nm. The specific surface areas are about 200 m2/g regardless of the precursor concentrations. After heating at 1000 °C for 10 hours, the products kept about 70% of their original pore volume and about 60% of the original surface area. Heating at 1100 °C caused a drastic reduction of pore volume and surface area …
Effects of Thermal Treatment on the Structure of Eu:YAG Nanopowder
2007
Eu:YAG nanopowder precursors were obtained by co-precipitation of aluminium, yttrium and europium nitrates solution with ammonia. The hydroxides precursors were calcined at different temperatures from 900 to 1200°C as a function of holding time (1, 2 and 6 hours). The presence of Eu3+ ions in the matrix was confirmed by Energy Dispersive X-rays analysis. X-Ray Diffraction investigation by the Rietveld method shows that the sample treated at 900°C for 1 hour is essentially the garnet phase with the minor presence of hexagonal and monoclinic metastable phases. The Eu3+ ions are incorporated into the garnet phase, as is suggested by the lattice parameter value being larger than that in literat…