Characterization of an Inorganic Cryptomelane Nanomaterial Synthesized by a Novel Process Using Transmission Electron Microscopy and X-Ray Diffraction

2008 ◽  
Vol 14 (4) ◽  
pp. 328-334 ◽  
Author(s):  
Longzhou Ma ◽  
Thomas Hartmann ◽  
Marcos A. Cheney ◽  
Nancy R. Birkner ◽  
Pradip K. Bhowmik
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Surface ◽  
High Surface Area ◽  
Rietveld Analysis ◽  
X Ray ◽  
Transmission Electron ◽  
Potential Applications ◽  
Diffraction Patterns ◽  
Crystallographic Planes

Layer- and tunnel-structured manganese oxide nanomaterials are important because of their potential applications in industrial catalysis. A novel soft chemistry method was developed for the synthesis of inorganic cryptomelane nanomaterials with high surface area. Bright field transmission electron microscopy (BF-TEM) and high-resolution transmission electron microscopy (HRTEM) techniques were employed to characterize this nanomaterial. A nanosized material with fibrous texture comprised of 140–160 nm striations was identified by BF-TEM imaging. HRTEM images show multiple atomic morphologies such as “helix-type,” “doughnut-like,” and tunnel structures lying on different crystallographic planes. The crystallographic parameters of this material were analyzed and measured by X-ray powder diffraction (XRD) showing that the synthesized nanomaterial is single phased and corresponds to cryptomelane with major diffraction peaks (for 10° < 2θ < 60°) at d-spacing values of 6.99, 4.94, 3.13, 2.40, 2.16, 1.84, 1.65, and 1.54 Å. A “doughnut-like” crystal structure was confirmed based on the crystallographic data. Structure and lattice parameters refinement was performed by XRD/Rietveld analysis. Simple simulation of HRTEM images and selected area diffraction patterns were applied to interpret the HRTEM images as observed.

The Flocculation and Stability of TiO2 Nanoparticles

2012 ◽  
Vol 548 ◽  
pp. 138-142
Author(s):  
Xiao Ying Liu ◽  
Xiao Dong Hao ◽  
Chun Xiang Gu ◽  
Yu Xin Zhang ◽  
Xin Lu Li ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Digital Camera ◽  
Processing Conditions ◽  
X Ray Diffraction ◽  
Thermogravimetric Method ◽  
X Ray ◽  
Transmission Electron ◽  
Potential Applications ◽  
Solvent Washing

In this work, TiO2nanoparticles (NPs) were prepared through a well-developed hydrothermal method. The dry products were characterized by digital camera, transmission electron microscopy (TEM), X-ray diffraction (XRD) and thermogravimetric method (TGA). These results suggested that TiO2NPs were well-crystallized and oleic acid-capped (OA-capped; 33.42 wt.%). In order to investigate the flocculation and stability of TiO2NPs colloids, redispersed experiments were carried out by altering the preparative parameters (e.g., redispersion solvent, washing times). In addition, the compounding stability of TiO2NPs colloids with AuNPs colloids and MnO4-solution under processing conditions (e.g., aging with stirring and under UV irradiation) were also studied. In principle, systematic investigations of flocculation and stability of TiO2NPs will be useful for their potential applications including novel photocatalysts and biosensors.

Ni-doped, urchin-like Bi2S3 particles for electrocatalytic oxidation of glucose

2021 ◽  
pp. 2150006
Author(s):  
Biao Wang ◽  
Ya Liu ◽  
Xu Huai ◽  
Yuqing Miao
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Electrocatalytic Oxidation ◽  
High Surface ◽  
High Surface Area ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Capacitance Current ◽  
Oxidation Of Glucose

In order to develop non-noble metal-based electrocatalysts for glucose oxidation, the Ni-doped, urchin-like Bi2S3 particles were prepared by a solvothermal method using the solvent of ethylene glycol/H2O. The obtained products were characterized by scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy and X-ray diffraction. The background signal from capacitance current is relatively low and the electrocatalytic oxidation current of glucose relatively high due to the urchin-like nanostructure of Bi2S3 particles and high surface area where the presence of Bi also improves the electrocatalytic performance of NiII/NiIII shift.

scholarly journals Investigation of Lithiated Carbons by Transmission Electron Microscopy and X-Ray Diffraction Analysis

1998 ◽  
Vol 548 ◽  
Author(s):  
T. D. Tran ◽  
X. Y. Song ◽  
K. Kinoshita
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Carbon Black ◽  
Xrd Analysis ◽  
X Ray Diffraction ◽  
Lattice Image ◽  
X Ray ◽  
Storage Mechanism ◽  
Transmission Electron ◽  
Diffraction Patterns

ABSTRACTThe microstructures of lithiated synthetic graphite and carbon black were studied by high- resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) analysis. Information about the crystal structure of carbon containing various Li compositions can provide useful insights to our understanding of the Li storage mechanism in carbonaceous materials. Samples with compositions of Li0.93C6or Li0.45C6 were found to contain both stage-one and stage-two compounds. These observations are consistent with XRD data. The changes in sample microstructure as the results of lithiation and exposure to electron irradiation were observed by TEM and recorded over several minutes in the microscope environment. Selected area electron diffraction patterns indicated that the lithiated samples quickly changed composition to LiC 24, which appeared to dominate during the brief analysis period. The layer planes in the lattice image of a disordered carbon black after Li insertion are poorly defined, and changes in the microstructure of these lithiated carbons was not readily apparent. Observations on these lithium intercalation compounds as well as the limitation of the experimental procedure will be presented.

SYNTHESIS AND CHARGE–DISCHARGE PROPERTIES OF POROUS CO3O4 NANOROD BUNDLE ELECTRODE

NANO ◽  
2012 ◽  
Vol 07 (05) ◽  
pp. 1250036 ◽  
Author(s):  
FEI TENG ◽  
JUN WANG ◽  
MINDONG CHEN ◽  
DENNIS DESHENG MNEG
Keyword(s):  
Electron Microscopy ◽  
High Surface ◽  
High Surface Area ◽  
Lithium Ion ◽  
Nitrogen Adsorption ◽  
X Ray ◽  
Transmission Electron ◽  
Rate Capacity ◽  
Nanorod Bundle ◽  
Charge Discharge

The Co3O4 nanorod bundles are synthesized by a hydrothermal method. The samples are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), electron diffraction (ED), X-ray powder diffractometer (XRD), and nitrogen adsorption. It is important that the as-obtained Co3O4 nanorod bundles are assembled by nanoparticles. The porous nanorod bundle electrode exhibits a higher rate capacity and a higher reverse capability for lithium ion battery than the solid nanorods, which is attributed to the high surface area and the porous structure.

The Formation of New Periodicities after N-Implantation in 4H- and 6H-SiC Samples

2013 ◽  
Vol 740-742 ◽  
pp. 447-450
Author(s):  
Konstantinos Zekentes ◽  
Katerina Tsagaraki ◽  
Aikaterini Breza ◽  
Nikolaos Frangis
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Resolution ◽  
Periodic Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Nitrogen Ions ◽  
Diffraction Patterns ◽  
Post Implantation

The purpose of the present study is to study the crystal periodicities that appear in 4H- and 6H-SiC material after the implantation with nitrogen and prior to post-implantation annealing. High Resolution X-Ray diffraction (HRXRD) and Transmission Electron Microscopy (TEM) have been employed towards this purpose. Extra peaks at smaller, than the main (00n) peak, diffraction angles in HRXRD scans and extra spots in the electron diffraction patterns have been observed due to the presence of these periodicities. Higher lattice constant periodic structures are apparently formed from the implanted nitrogen ions located at interstitial sites and disappear after the annealing and the resulting positioning of nitrogen atoms in substitutional sites.

Substructure Measurements by Statistical Fluctuations in X-Ray Diffraction Intensity

1965 ◽  
Vol 9 ◽  
pp. 74-90 ◽  
Author(s):  
E. F. Sturcken ◽  
W. E. Gettys ◽  
E. M. Bohn
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Grain Size ◽  
X Ray Diffraction ◽  
Diffraction Intensity ◽  
Laue Diffraction ◽  
X Ray ◽  
Statistical Fluctuations ◽  
Transmission Electron ◽  
Diffraction Patterns

AbstractThe substructures of a bet a-quenched and a recrystallized form of high-purity uranium were measured by a method based on statistical fluctuations in X-ray diffraction intensity. For these measurements, Warren's statistical equation for determining grain size was modified to make the equation applicable to materials with high absorption coefficients or moderate-to-large grain size ( > 20 microns) or both, since many metals fall into this category, and to allow for defocusing of the X-ray beam which occurs as a natural consequence of the experiment.The beta-quenched uranium was found to have numerous subgrains with a range of misorientation angles that was smaller and larger than the limits of the X-ray measurements (Ω = 10−4 to 10−2 steradians). The presence of the large subgrains was corroborated by optical microscopy. The presence of very small subgrains was corroborated by transmission electron microscopy which showed 0.1- to 1-micron subgrains relatively free of dislocations bounded by dense dislocation networks, and by micro Laue diffraction patterns (30-micron beam diameter) which showed partial rings similar to a powder pattern.The recrystallized uranium had no misorientation within the grains greater than 5.5 × 10−3 steradians. In contrast to the beta-quenched case, no subgrains were found either by transmission electron microscopy (TEM) or micro Laue diffraction patterns. The TEM micrographs showed a uniform distribution of dislocation networks. Since no other substructural elements were observed, the dislocations are believed to be the cause of the misorientation within the grains for solid angles of less than 5 × 10−3 steradiflns.These preliminary experiments show that the statistical method may be used in conjunction with transmission electron microscopy and micro Laue diffraction for the study of substructure. The statistical method gives quantitative data on “bulk” specimens that can be given a meaningful interpretation with the aid of the other techniques.

Transmission Electron Microscopy Studies of Pd Encapsulation by Ceria-Zirconia Oxides

1998 ◽  
Vol 4 (S2) ◽  
pp. 724-725
Author(s):  
J. C. Jiang ◽  
X. Q. Pan ◽  
G. W. Graham ◽  
R. W. McCabe ◽  
J. Schwank
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Temperature ◽  
Surface Area ◽  
High Speed ◽  
High Surface ◽  
Silicon Crystal ◽  
High Surface Area ◽  
Thermal Environments ◽  
Transmission Electron

High-temperature catalysts containing Pd supported on high-surface area ceria-zirconia are optimum materials for fuel economy when automotive engines operate under high speed or load conditions. A prerequisite for developing such thermally stable catalysts is to gain a good understanding of the thermal deactivation modes contributing to the aging and degradation of catalysts in harsh thermal environments. It was discovered by X-ray diffraction that upon hightemperature aging, Pd may sinter into large (about 10 nm diameter) particles and become encapsulated in the ceria-zirconia. To confirm this conclusion, a prototype high-temperature catalyst containing Pd supported on high-surface area ceria-zirconia, aged at temperature above 1100 °C is studied by transmission electron microscopy (TEM).The ceria-zirconia supported Pd (0.25 wt%) catalyst was aged at 1105 °C and calcined at 700 °C for 2 h. For TEM sample preparations, first of all, a large-size aggregate with diameter about 1 mm was selected and sandwiched between by two pieces of silicon crystal.

scholarly journals Synthesis and characterization of LaMnO3 nanocrystals and graphene oxide: fabrication of graphene oxide–LaMnO3 sensor for simultaneous electrochemical determination of hydroquinone and catechol

2019 ◽  
Vol 9 (4) ◽  
pp. 255-267 ◽  
Author(s):  
Sedighe Akbari ◽  
Mohammad Mehdi Foroughi ◽  
Hadi Hassani Nadiki ◽  
Shohreh Jahani
Keyword(s):  
Electron Microscopy ◽  
Graphene Oxide ◽  
Simultaneous Determination ◽  
High Surface ◽  
High Surface Area ◽  
Electrochemical Determination ◽  
Great Decrease ◽  
X Ray ◽  
Transmission Electron

For the first time, a new method for preparation of graphene oxide-LaMnO3 (GO-LaMnO3) nanocompositeas a material of electrochemical sensor for simultaneous determination of catechol (CT) and hydroquinone (HQ) is developed. LaMnO3 nanoparticles have been characterized by Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and energy dispersive X-ray analysis (EDX) technique. Due to the excellent catalytic activity, enhanced electrical conductivity and high surface area, the simultaneous determination of HQ and CT with two well-defined peaks has been achieved at the GO-LaMnO3 modified electrode. Comparing with unmodified electrodes, the oxidation currents of HQ and CT increased remarkably. Also, the result exhibited a great decrease in anodic overpotentialresulting in about 150 mV negative shift of potential. The catalytic peak current values are found linearly dependent on the HQ and CT concentrations in the range of 0.5–433.3 and 0.5–460.0 μM with sensitivity of 0.0719 and 0.0712 μA μM-1, respectively. The detection limits for HQ and CT are determined as 0.06 and 0.05 μM, respectively.

Electron microscopy characterization of monoclinic SiAs precipitates in heavily As+-implanted silicon

1991 ◽  
Vol 6 (8) ◽  
pp. 1701-1710 ◽  
Author(s):  
A. Armigliato ◽  
A. Parisini
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Annealing Temperature ◽  
X Ray ◽  
Transmission Electron ◽  
Small Precipitate ◽  
Diffraction Patterns ◽  
Microscopy Characterization ◽  
First Time

Silicon wafers have been implanted with As+ ions at an energy of 100 keV and a dose of 1 × 1017 cm−2 and subsequently annealed at 1050°for 15 min. This results in a peak As concentration of 7 × 1021 cm−3, which is far beyond the solid solubility value of arsenic in silicon at this annealing temperature. Rod-like precipitates, dislocations, and small precipitate-like defects have been observed by transmission electron microscopy. From the analysis of several diffraction patterns taken on a number of rod-like particles at different tilt angles, it has been unambiguously found that they have the structure of the monoclinic SiAs compound previously reported in literature. The stoichiometry of the precipitates has been confirmed by x-ray microanalysis. To our knowledge, this is the first time that this SiAs phase is detected in As+-implanted silicon.

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