Transmission electron microscopy and x-ray structural investigation of La0.7Ca0.3MnO3 thin films

1998 ◽  
Vol 13 (8) ◽  
pp. 2161-2169 ◽  
Author(s):  
Y. H. Li ◽  
K. A. Thomas ◽  
P. S. I. P. N. de Silva ◽  
L. F. Cohen ◽  
A. Goyal ◽  
...  

The structural changes and magnetoresistance (MR) properties of as-grown and post-annealed La0.7Ca0.3MnO3 films were investigated by transmission electron microscopy (TEM) and x-ray diffraction (XRD). The data for the films were compared to that for bulk La0.7Ca0.3MnO3 post-annealed under the same conditions. The main structure of the as-grown films was face-centered pseudo-cubic with a doubled perovskite unit cell, of size ∼2ap × ∼2ap × 2ap, where ap is the single perovskite parameter. The phase showed a cube-on-cube epitaxy with the underlying LaAlO3 substrate. Upon annealing to a saturation point, a minor primitive pseudo-tetragonal structure evolved, of cell parameters . A total of four possible orientations of the two structures was observed by TEM, comprised of one orientation of the ∼ 2ap × ∼ 2ap × ∼ 2ap cell, i.e., the cube-on-cube epitaxy, giving rise to (00l) peaks in x-ray, and three orientations of the cell, giving rise to a single (00l)/(hk0) peak in x-ray. The bulk La0.7Ca0.3MnO3 sample also contains the × structure. The difference between the bulk and the film and the effects of annealing on films can be ascribed to the influence of strain between the film and substate, induced by lattice mismatch.

1995 ◽  
Vol 10 (6) ◽  
pp. 1546-1554 ◽  
Author(s):  
G.M. Chow ◽  
L.K. Kurihara ◽  
K.M. Kemner ◽  
P.E. Schoen ◽  
W.T. Elam ◽  
...  

Nanocrystalline CoxCu100−x (4 ⋚ x ⋚ 49 at. %) powders were prepared by the reduction of metal acetates in a polyol. The structure of powders was characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), extended x-ray absorption fine structure (EXAFS) spectroscopy, solid-state nuclear magnetic resonance (NMR) spectroscopy, and vibrating sample magnetometry (VSM). As-synthesized powders were composites consisting of nanoscale crystallites of face-centered cubic (fcc) Cu and metastable face-centered cubic (fcc) Co. Complementary results of XRD, HRTEM, EXAFS, NMR, and VSM confirmed that there was no metastable alloying between Co and Cu. The NMR data also revealed that there was some hexagonal-closed-packed (hcp) Co in the samples. The powders were agglomerated, and consisted of aggregates of nanoscale crystallites of Co and Cu. Upon annealing, the powders with low Co contents showed an increase in both saturation magnetization and coercivity with increasing temperature. The results suggested that during preparation the nucleation of Cu occurred first, and the Cu crystallites served as nuclei for the formation of Co.


1996 ◽  
Vol 11 (12) ◽  
pp. 3146-3151 ◽  
Author(s):  
E. Czerwosz ◽  
P. Byszewski ◽  
R. Diduszko ◽  
H. Wronka ◽  
P. Dluźewski ◽  
...  

C60/C70: Ni films with 1.5 wt. % Ni concentration obtained by vacuum deposition under different thermal conditions have been investigated. The structural changes of the layers were investigated by transmission electron microscopy, electron and x-ray diffraction, and Raman spectroscopy. The polycrystalline structure was detected for the layers grown at approximately 450 K on the substrate. At elevated temperature and maintained temperature gradient on the substrate during the process, the changes of the layer's structure and the formation of Ni microcrystals were observed. The Ni microcrystals (5–10 nm in the diameter) and the elongated shapes dimensioned 10 × 150 nm were perceived.


2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
L. M. Artem ◽  
D. M. Santos ◽  
A. R. De Andrade ◽  
K. B. Kokoh ◽  
J. Ribeiro

This work consisted in the preparation of platinum-based catalysts supported on carbon (Vulcan XC-72) and investigation of their physicochemical and electrochemical properties. Catalysts of the C/Pt-Ni-Sn-Me (Me = Ru or Ir) type were prepared by the Pechini method at temperature of350∘C. Four different compositions were homemade: C/Pt60Sn10Ni30, C/Pt60Sn10Ni20Ru10, C/Pt60Sn10Ni10Ru20, and C/Pt60Sn10Ni10Ir20. These catalysts were electrochemically and physically characterized by cyclic voltammetry (CV), chronoamperometry (CA) in the presence of glycerol 1.0 mol dm-3, X-ray diffraction (XRD), and high-resolution transmission electron microscopy (HRTEM). XRD results showed the main peaks of face-centered cubic Pt. The particle sizes obtained from XRD and HRTEM experiments were close to values ranging from 3 to 8.5 nm. The CV results indicate behavior typical of Pt-based catalysts in acid medium. The CV and CA data reveal that quaternary catalysts present the highest current density for the electrooxidation of glycerol.


2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Sanja Ćulubrk ◽  
Željka Antić ◽  
Vesna Lojpur ◽  
Milena Marinović-Cincović ◽  
Miroslav D. Dramićanin

Herein we presented hydrolytic sol-gel synthesis and photoluminescent properties of Eu3+-doped Gd2Ti2O7pyrochlore nanopowders. According to Gd2Ti2O7precursor gel thermal analysis a temperature of 840°C is identified for the formation of the crystalline pyrochlore phase. Obtained samples were systematically characterized by powder X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The powders consist of well-crystalline cubic nanocrystallites of approximately 20 nm in size as evidenced from X-ray diffraction. The scanning and transmission electron microscopy shows that investigated Eu3+-doped Gd2Ti2O7nanopowders consist of compact, dense aggregates composed entirely of nanoparticles with variable both shape and dimension. The influence of Eu3+ions concentration on the optical properties, namely, photoluminescence emission and decay time, is measured and discussed. Emission intensity as a function of Eu3+ions concentration shows that Gd2Ti2O7host can accept Eu3+ions in concentrations up to 10 at.%. On the other hand, lifetime values are similar up to 3 at.% (~2.7 ms) and experience decrease at higher concentrations (2.4 ms for 10 at.% Eu3+). Moreover, photoluminescent spectra and lifetime values clearly revealed presence of structural defects in sol-gel derived materials proposing photoluminescent spectroscopy as a sensitive tool for monitoring structural changes in both steady state and lifetime domains.


Clay Minerals ◽  
2002 ◽  
Vol 37 (3) ◽  
pp. 465-471 ◽  
Author(s):  
Seung Yeop Lee ◽  
Soo Jin Kim

AbstractThe morphological and structural changes in smectite caused by hexadecyltrimethylammonium (HDTMA) treatment were studied using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The HDTMA-exchanged smectite shows not only morphological features such as irregular, wavy surface with curled edges, but also structural features such as large d-spacings (20 – 26 Å ) and lattice distortions. The surface morphological heterogeneity is assumed to be related to the inhomogeneous intercalation of HDTMA cations into the interlayer of smectite.


2007 ◽  
Vol 561-565 ◽  
pp. 1685-1688 ◽  
Author(s):  
Takahiko Kato ◽  
Haruo Akahoshi ◽  
Takeshi Terasaki ◽  
Tomio Iwasaki ◽  
Masato Nakamura ◽  
...  

Tin/copper (Sn/Cu) coatings on Cu leadframes (CUFE), in which Fe atoms are doped as a minor element, showed whisker initiation at room temperature over a long period of 47 months. By means of the planar slice method and electron back scattering pattern (EBSP) measurement, the whisker roots were consistently found to be located at the intersections of grain boundaries in the coating. Whisker roots were also located above the peaks and ridge lines of intermetallic compound (IMC) Cu6Sn5, which was formed with a pyramid-shaped configuration between the Sn/Cu coating and Cu leadframe. Using finite element analysis (FEA), we calculated stress distribution in the coating. The results indicated that compressive stress normal to the grain boundary was induced with a gradient toward the surface in the coating. Therefore, the compressive stress gradient induced by the pyramid-shaped IMC is thought to be the root cause of whisker initiation in Sn/Cu coatings on Cu leadframes. When the Cu leadframe with a minor doped element of Cr atoms (CUCR) was used as the substrate with the same Sn/Cu coating, no whisker initiation was observed even after a longer storage time of 65 months. Through field-emission scanning transmission electron microscopy (FE-STEM) and field-emission transmission electron microscopy (FE-TEM) microstructural observations of vertical sections of each sample, the shape of the IMCs formed between the coating and the leadframe in the Sn/Cu-CUFE sample was found to be different from that in the Sn/Cu-CUCR sample. The difference in whisker initiation tendency can therefore be explained by the difference in compressive stress depending on the shape of the Cu-Sn IMCs, because stress distribution in the coating of the Sn/Cu-CUCR sample calculated using FEA revealed a smaller stress gradient than that in the Sn/Cu-CUFE sample.


2009 ◽  
Vol 24 (11) ◽  
pp. 3321-3330 ◽  
Author(s):  
Y.F. Han ◽  
T. Fu ◽  
Y.G. Shen

The effects of Al incorporation and post-deposition annealing on the structural properties of C-Al-N thin films prepared by reactive unbalanced dc-magnetron sputtering were investigated using x-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and high-resolution transmission electron microscopy (HRTEM). XPS studies demonstrated the presence of abundant Al-N bonds in addition to C-C and N-C bonds. At low incorporations of Al and N, the films were found to be essentially amorphous. By Raman and HRTEM, the formation of ∼5 nm fullerene-like carbon nitride (FL-CNx) nanostructures in an amorphous (C, CNx) matrix was evidenced with increasing Al content in the films. Crystalline improvement of FL-CNx nanostructures was seen, as well as the precipitation of ∼3–4 nm face centered cubic (fcc-) AlN nanograins by thermal annealing at 500 °C or above. Through these improvements, C-Al-N nanocomposite thin films were achieved. The effects of the incorporated Al and annealing on stabilizing fcc-AlN nanograins and FL-CNx nanostructures are elucidated and explained through the use of thermodynamic considerations.


1993 ◽  
Vol 8 (9) ◽  
pp. 2143-2148 ◽  
Author(s):  
H. Sakai ◽  
Y. Shiohara ◽  
S. Tanaka

The thin films (Y/Ba/Cu = 1.0/2.7/4.7) which have a strong intensity corresponding to the c-axis peaks of the 124 phase (YBa2Cu4O8) in x-ray diffraction (XRD) patterns were prepared. The film structure and surface morphology of these films were observed by scanning electron microscopy (SEM), energy dispersive x-ray (EDX), transmission electron microscopy (TEM), and atomic force microscopy (AFM). It was found that the film on MgO(100) clearly has grain boundaries with many a-axis oriented grains of the 123 phase (YBa2Cu3O7−x). However, the film on SrTiO3(100) had a smooth surface, and a-axis oriented grains of the 123 phase couldn't be observed. This difference could not be explained by only the difference in the lattice mismatch.


Author(s):  
S. Fujishiro

The mechanical properties of three titanium alloys (Ti-7Mo-3Al, Ti-7Mo- 3Cu and Ti-7Mo-3Ta) were evaluated as function of: 1) Solutionizing in the beta field and aging, 2) Thermal Mechanical Processing in the beta field and aging, 3) Solutionizing in the alpha + beta field and aging. The samples were isothermally aged in the temperature range 300° to 700*C for 4 to 24 hours, followed by a water quench. Transmission electron microscopy and X-ray method were used to identify the phase formed. All three alloys solutionized at 1050°C (beta field) transformed to martensitic alpha (alpha prime) upon being water quenched. Despite this heavily strained alpha prime, which is characterized by microtwins the tensile strength of the as-quenched alloys is relatively low and the elongation is as high as 30%.


Author(s):  
Ann M. Thomas ◽  
Virginia Shemeley

Those samples which swell rapidly when exposed to water are, at best, difficult to section for transmission electron microscopy. Some materials literally burst out of the embedding block with the first pass by the knife, and even the most rapid cutting cycle produces sections of limited value. Many ion exchange resins swell in water; some undergo irreversible structural changes when dried. We developed our embedding procedure to handle this type of sample, but it should be applicable to many materials that present similar sectioning difficulties.The purpose of our embedding procedure is to build up a cross-linking network throughout the sample, while it is in a water swollen state. Our procedure was suggested to us by the work of Rosenberg, where he mentioned the formation of a tridimensional structure by the polymerization of the GMA biproduct, triglycol dimethacrylate.


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