Microstructural changes in porous hematite nanoparticles upon calcination

2011 ◽  
Vol 44 (3) ◽  
pp. 495-502 ◽  
Author(s):  
Rune E. Johnsen ◽  
Kenneth D. Knudsen ◽  
Alfons M. Molenbroek
Keyword(s):  
Adsorption Isotherm ◽  
Surface Area ◽  
Small Angle Neutron Scattering ◽  
Particle Sizes ◽  
X Ray ◽  
Structure Changes ◽  
Transmission Electron ◽  
Porous Microstructure ◽  
Void Structure ◽  
Sans Data

This combined study using small-angle neutron scattering (SANS), X-ray powder diffraction (XRPD), transmission electron microscopy (TEM) and adsorption isotherm techniques demonstrates radical changes in the microstructure of porous hematite (α-Fe2O3) nanoparticles upon calcination in air. TEM images of the as-synthesized hematite sample show that it consists of subrounded nanoparticles [50 (8)–61 (11) nm in average minimum and maximum diameters] with an apparent porous structure of nanosized pores/channels or cracks. SANS data confirm the presence of two characteristic sizes, one originating from the particle size and the other from the pore/void structure. Furthermore, the TEM images show that the particle sizes are nearly unaffected by calcination at 623 K, whereas their pore/void structure changes radically to an apparently pitted or spongy microstructure with cavities or/and voids. The change in microstructure also causes a reduction in the surface area as calculated by gaseous adsorption. The XRPD and SANS data show that the crystallite and SANS particle sizes are virtually unchanged by calcination at 623 K. Calcination at 973 K induces a significant alteration of the sample. The XRPD data reveal that the crystallite size increases significantly, and the SANS and adsorption isotherm studies suggest that the specific surface area decreases by a factor of ∼5–6. The TEM images show that the particles are sintered into larger agglomerates, but they also show that parts of the porous microstructure observed in the sample calcined at 623 K are retained in the sample calcined at 973 K.

scholarly journals Structural Changes of Mo/ZSM-5 Catalysts During the Methane Dehydroaromatization

2009 ◽  
Vol 12 (1) ◽  
pp. 9 ◽  
Author(s):  
Z.R. Ismagilov ◽  
E.V. Matus ◽  
I.Z. Ismagilov ◽  
M.A. Kerzhentsev ◽  
V.I. Zailovskii ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Structural Changes ◽  
Atomic Ratio ◽  
X Ray ◽  
Reducing Atmosphere ◽  
Structure Changes ◽  
Transmission Electron ◽  
Methane Dehydroaromatization ◽  
Naoh Treatment ◽  
Mo Content

<p>The structure changes of Mo/ZSM-5 catalysts with different Mo content (2 and 10 wt. % Mo) and Si/Al atomic ratio (17, 30 and 45) during the methane dehydroaromatization have been investigated by X-ray powder diffractometry, N<sub>2</sub> adsorption and transmission electron microscopy. The treatment of Mo/ZSM-5 catalysts in reducing atmosphere (CH<sub>4</sub> or H<sub>2</sub>) at about 700 °C promotes development of mesoporous system. The pores are open to the exterior of the zeolite grain and have an entrance diameter of ~ 4-10 nm. It is proposed that mesopore formation in Mo/ZSM-5 catalyst is connected with the dealumination of zeolite. The mesopore formation in the parent H-ZSM-5 zeolite by NaOH treatment does not improve the activity of /ZSM-5 catalyst.</p>

As Review Of Conventional And Non-Conventional Pore Characterization Techniques

1988 ◽  
Vol 137 ◽  
Author(s):  
Rosario Gerhardt
Keyword(s):  
Electron Microscopy ◽  
Small Angle Neutron Scattering ◽  
Colloidal Silica ◽  
Nuclear Magnetic Resonance Relaxation ◽  
X Ray ◽  
Transmission Electron ◽  
Relaxation Measurements ◽  
Pore Characterization ◽  
Nitrogen Desorption ◽  
Resonance Relaxation

AbstractA series of techniqu1es were employed to characterize the pore microstructure of a group of colloidal silica-alkali silicate gels. Methods used included mercury penetration porosimetry, nitrogen desorption measurements, transmission electron microscopy, single and multiple small angle neutron scattering, nuclear magnetic resonance relaxation measurements, x-ray tomography and dielectric constant measurements. Comparison of results of pore volume, pore size and size distribution as well as homogeneity of the pore structure are presented.

Study of Heating Effect on Specific Surface Area, and Changing Optical Properties of ZnO Nanocrystals

2011 ◽  
Vol 403-408 ◽  
pp. 1205-1210
Author(s):  
Jaleh Babak ◽  
Ashrafi Ghazaleh ◽  
Gholami Nasim ◽  
Azizian Saeid ◽  
Golbedaghi Reza ◽  
...  
Keyword(s):  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Energy Gap ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Zno Nanocrystals ◽  
Transmission Electron ◽  
Zno Nanocrystal

In this work ZnO nanocrystal powders have been synthesized by using Zinc acetate dehydrate as a precursor and sol-gel method. Then the products have been annealed at temperature of 200-1050°C, for 2 hours. The powders were characterized using X-ray diffraction (XRD), UV-vis absorption and photoluminescence (PL) spectroscopy. The morphology of refrence ZnO nanoparticles have been studied using Transmission Electron Microscope (TEM). During the annealing process, increase in nanocrystal size, defects and energy gap quantitative, and decrease in specific surface area have been observed.

scholarly journals A green chemical route for the synthesis of Mn3O4 nanoparticles

2009 ◽  
Vol 7 (3) ◽  
pp. 555-559 ◽  
Author(s):  
Zehra Durmus ◽  
Hüseyin Kavas ◽  
Abdulhadi Baykal ◽  
Muhammet Toprak
Keyword(s):  
Room Temperature ◽  
Particle Sizes ◽  
Chemical Route ◽  
Tem Analysis ◽  
X Ray ◽  
Profile Fitting ◽  
Transmission Electron ◽  
Wide Range ◽  
Long Range Interactions ◽  
Mn3o4 Nanoparticles

AbstractA novel environmental friendly, room temperature route using an ionic liquid 1-n-butyl-3-methylimidazolium hydroxide ([BMIM]OH) for the synthesis of Mn3O4 nanoparticles is presented. The product was characterized using Fourier transform infrared spectroscopy, X-ray powder diffraction, and transmission electron microscopy. Phase purity was confirmed by XRD, and X-ray line profile fitting determined a crystallite size of 42 ± 11 nm. TEM analysis revealed various morphologies. EPR measurements have indicated the existence of long-range interactions, due to the wide range of particle sizes and morphologies observed.

Solvothermal/ Hydrothermal Synthesis of Metal Oxides and Metal Powders with and without Microwaves

2010 ◽  
Vol 65 (8) ◽  
pp. 1033-1037 ◽  
Author(s):  
Sridhar Komarneni ◽  
Young Dong Noh ◽  
Joo Young Kim ◽  
Seok Han Kim ◽  
Hiroaki Katsuki
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Hydrothermal Synthesis ◽  
Reducing Agents ◽  
Particle Sizes ◽  
Metal Powders ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Very Low Temperature

Anatase and Ca, Sr and Ca0.5Sr0.5 hydroxyapatites were synthesized by conventional-hydrothermal (C-H) as well asmicrowave-hydrothermal (M-H)methods.Microwave-assisted reactions led to accelerated syntheses of anatase but no such acceleration of reactions could be detected with the syntheses of hydroxyapatites because the crystallization of the latter materials occurred at very low temperature. Cu and Au metal powders were produced by using glucose, fructose or sucrose as reducing agents under C-H conditions at 160 ℃, where fructose and sucrose were found to be stronger reducing agents than glucose. The crystallinity of all the powders was characterized by powder X-ray diffraction, and morphology and particle sizes were determined by scanning or transmission electron microscopy

scholarly journals Effects of Size and Dispersity of Microcrystalline Celluloses on Size, Structure and Stability of Nanocrystalline Celluloses Extracted by Acid Hydrolysis

Nano LIFE ◽  
2014 ◽  
Vol 04 (04) ◽  
pp. 1441014 ◽  
Author(s):  
Qi Liu ◽  
Weiping Hao ◽  
Yongguang Yang ◽  
Aurore Richel ◽  
Canbin Ouyang ◽  
...  
Keyword(s):  
Particle Size ◽  
Acid Hydrolysis ◽  
Size Structure ◽  
Particle Sizes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Force Microscopy ◽  
Atomic Force ◽  
Transmission Electron ◽  
Sonication Treatment

Nanocrystalline celluloses (NCCs) were separated from four commercial microcrystalline celluloses (MCCs) by an acid hydrolysis–sonication treatment. Transmission electron microscopy (TEM), atomic force microscopy (AFM), Fourier transform infrared (FTIR) spectrum, X-ray diffraction (XRD) and thermogravimetric analysis (TGA) were conducted to investigate the NCCs. MCCs with different morphologies and particle sizes showed different aggregation degrees. The aggregation of MCCs followed the order MCC1 > MCC3 > MCC2 > MCC4, which is the same order of the heights of the resulting NCCs. The best uniformity and thermal stability were characterized for NCC3, which was produced by MCC3 with smallest original particle size and good dispersity among the four MCCs. This result suggests that both the original particle size and dispersity of MCCs had significant effects on separated NCCs.

Efficient synthesis of carbon nanotubes with improved surface area by low-temperature solvothermal route from dichlorobenzene

2013 ◽  
Vol 67 (11) ◽  
Author(s):  
Gantigaiah Krishnamurthy ◽  
Sarika Agarwal
Keyword(s):  
Electron Microscopy ◽  
Carbon Nanotubes ◽  
Carbon Source ◽  
Surface Area ◽  
Heating Temperature ◽  
Outer Diameter ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Electron

AbstractThe synthesis of well-aggregated carbon nanotubes in the form of bundles was achieved by the catalytic reduction of 1,2-dichlorobenzene by a solvothermal approach. The use of 1,2-dichlorobenzene as a carbon source yielded a comparably good percentage of carbon nanotubes in the range of 60–70 %, at a low reaction temperature of 200°C. The products obtained were analysed by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy techniques. The X-ray diffraction studies implied the presence of pure, crystalline, and well-ordered carbon nanotubes. The scanning electron and transmission electron microscopic images revealed the surface morphology, dimensions and the bundled form of the tubes. These micrographs showed the presence of multi-walled carbon nanotubes with an outer diameter of 30–55 nm, inner diameter of 15–30 nm, and lengths of several hundreds of nanometers. Brunauer-Emmett-Teller-based N2 gas adsorption studies were performed to determine the surface area and pore volume of the carbon nanotubes. These carbon nanotubes exhibit a better surface area of 385.30 m2 g−1. In addition, the effects of heating temperature, heating time, amount of catalyst and amount of carbon source on the product yield were investigated.

Preparation of Carbon-Encapsulated Fe Core-Shell Nanostructures by Confined Arc Plasma

2011 ◽  
Vol 688 ◽  
pp. 245-249 ◽  
Author(s):  
Zhi Qiang Wei ◽  
Xiao Yun Wang ◽  
Hua Yang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Particle Size ◽  
Specific Surface ◽  
Surface Area ◽  
Core Shell ◽  
Arc Plasma ◽  
X Ray ◽  
The Core ◽  
Transmission Electron

Special carbon encapsulated Fe core-shell nanoparticles with a size range of 15–40 nm were successfully prepared via confined arc plasma method. The composition, morphology, microstructure, specific surface area, particle size of the product by this process were characterized via X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), X-ray energy dispersive spectrometry (XEDS) and BET N2adsorption. The experiment results shown that the carbon encapsulated Fe nanoparticles with clear core-shell structure, the core of the particles is body centered cubic (BCC) structure Fe, and the shell of the particles is disorder carbons. The particle size of the nanocapsules ranges from 15 to 40nm，with an averaged value about 30nm, the particles diameter of the core is about 16nm and the thickness of the shells is about 6-8 nm, and the specific surface area is 24 m2/g.

Synthesis of NiFe2O4 Nanoparticles and its Supercapacitive Properties

2013 ◽  
Vol 275-277 ◽  
pp. 1733-1736 ◽  
Author(s):  
Zi Tao Yang ◽  
Bo Wen Cheng ◽  
Yong Nan Zhao
Keyword(s):  
Water Solution ◽  
Particle Sizes ◽  
X Ray Diffraction ◽  
Galvanostatic Charge ◽  
X Ray ◽  
Transmission Electron ◽  
Nife2o4 Nanoparticles ◽  
Diffraction Peaks ◽  
Xrd Patterns ◽  
Charge Discharge

NiFe2O4 nanoparticles was successfully synthesized by hydrothermal decomposition of a gel of Ni-Fe-EG (EG=ethylene glycol) in water solution. The crystal structure and morphologies of the products were characterized by X-ray diffraction (XRD) and Transmission electron microscopy (TEM). All the diffraction peaks in XRD patterns revealed that the as-synthesized nanoparticles were pure NiFe2O4. TEM images disclosed that the particle sizes of the nanoparticles were in the range of 10 − 25nm. The cyclic voltammetry (CV) and galvanostatic charge/discharge results tested in 6M KOH solution revealed a double layer capacitive behavior and a revisable charge/discharge property.

Sign in / Sign up

Export Citation Format

Share Document