New Insights on the Morphology of Nanocomposite Prepared by In Situ Emulsion Polymerization

2015 ◽  
Vol 775 ◽  
pp. 170-175
Author(s):  
José Costa de Macêdo Neto ◽  
João Evangelista Neto ◽  
Nayra Reis do Nascimento ◽  
Sheila Contant ◽  
Liliane Maria Ferrareso Lona

In order to better understand the morphology and properties of polymer nanocomposites it is necessary to conduct their characterization by Transmission Electron Microscopy (TEM). This work shows a technique through which the nanocomposite powder is mixed with a resin, and after cured, thin sections can be obtained by ultramicrotomy. Another technique presented in this work deals with the observation of clay powder in solution. In this work High Resolution Electron Microscopy (HRTEM) was used to obtain images of the nanocomposites and clay. Images with a high level of details were showed. Through the use of such techniques, it was possible to observe two types of clay morphology in polymer matrix and its distribution. The dimensions and hexagonal layers of the natural clay used as nanofiller for the nanocomposite were also observed. The X-ray Diffraction (XRD) was used to investigate the kaolinite and nanocomposite.

2001 ◽  
Vol 16 (8) ◽  
pp. 2189-2191 ◽  
Author(s):  
Guo-Dong Zhan ◽  
Mamoru Mitomo ◽  
Young-Wook Kim ◽  
Rong-Jun Xie ◽  
Amiya K Mukherjee

Using a pure α–SiC starting powder and an oxynitride glass composition from the Y–Mg–Si–Al–O–N system as a sintering additive, a powder mixture was hot-pressed at 1850 °C for 1 h under a pressure of 20 MPa and further annealed at 2000 °C for 4 h in a nitrogen atmosphere of 0.1 MPa. High-resolution electron microscopy and x-ray diffraction studies confirmed that a small amount of β–SiC was observed in the liquid-phase-sintered α–SiC with this oxynitride glass, indicating stability of β–SiC even at high annealing temperature, due to the nitrogen-containing liquid phase.


1995 ◽  
Vol 401 ◽  
Author(s):  
P. A. Langjahr ◽  
T. Wagner ◽  
M. RÜhle ◽  
F. F. Lange

AbstractCubic and pseudocubic perovskite films on perovskite substrates are used to study the influence of the lattice mismatch on the epitaxial growth of thin films on substrates of the same structure. For the growth of the films, a metalorganic decomposition route (MOD) using 2-ethylhexanoates and neodecanoates as precursors, was developed. The decomposition of the precursors was investigated with thermogravimetric analysis (TGA) and x-ray diffraction (XRD). The films were spin-coated on (001)-oriented SrTiO3- and LaAlO3-substrates, pyrolyzed and afterwards annealed between 600°C and 1200°C. XRD-nvestigations and conventional transmission electron microscopy (CTEM) show, that epitaxial films with the orientation relationship [100](001) film ║ [100](001) substrate can be grown. With XRD, it could be shown, that not only ternary oxide films (SrZrO3, BaZrO3 and BaCeO3), but also perovskite solid solution films (SrTi0.5Zr0.5O3and BaCe0.5Zr0.5O3) can be prepared. Strong interdiffusion, detected by a shift of the film lattice parameter towards the substrate lattice parameter was found in SrZrO3- and BaZrO3-films on SrTiO3, annealed at temperatures above 1050°C. High resolution electron microscopy (HREM) studies of SrZrO3 on SrTiO3 show that a crystalline semicoherent interface with a periodical array of misfit dislocations is present.


MRS Bulletin ◽  
1994 ◽  
Vol 19 (6) ◽  
pp. 26-31 ◽  
Author(s):  
Robert Sinclair

Processing has always been a key component in the development of new materials. Basic scientific understanding of the reactions and transformations that occur has obvious importance in guiding progress. Invaluable insight can be provided by observing the changes during processing, especially at high magnification by in situ microscopy. Now that this can be achieved at the atomic level by using high-resolution electron microscopy (HREM), atomic behavior can be seen directly. Accordingly, many deductions concerning reactions in materials at the atomic scale are possible.The purpose of this article is to illustrate the level reached by in situ HREM. The essential procedure is to form a high-resolution image of a standard transmission electron microscope (TEM) sample and then to alter the structure by some means in a controlled manner, such as by heating. Continual recording on videotape allows subsequent detailed analysis of the behavior, even on a frame-by-frame (1/30 second) basis. The most obvious advantage is to follow the atomic rearrangements directly in real time. However, in addition, by continuous recording no stages in a reaction are missed, which can often occur in a series of conventional ex situ annealed samples because of the limited number of samples that can realistically be examined by HREM. One can be sure that the same reaction, in the same area, is being studied. Furthermore, by changing the temperature systematically, extremely precise kinetic measurements can be made (e.g., for activation energies and kinetic laws) and the whole extent of a material transformation can be investigated in one sample, something that would take months of work if studied conventionally. The information provided by in situ HREM is often unique and so it can become an important technique for fundamental materials investigations.


Nanoscale ◽  
2017 ◽  
Vol 9 (30) ◽  
pp. 10684-10693 ◽  
Author(s):  
Ana R. Ribeiro ◽  
Arijita Mukherjee ◽  
Xuan Hu ◽  
Shayan Shafien ◽  
Reza Ghodsi ◽  
...  

In situliquid cell transmission electron microscopy and graphene liquid cells were used to investigate, thein situnano–bio interactions between titanium dioxide nanoparticles and biological medium.


Author(s):  
M. M. Disko ◽  
S. K. Behal ◽  
R. D. Sherwood ◽  
F. Cosandey ◽  
P. Lu ◽  
...  

Methods for the preparation of significant quantities of C60 clusters separated from carbon soot were recently reported by Krätschmer and co-workers. Evidence that these clusters have the “Buckminsterfullerene” structure with five-fold and six-fold carbon rings on the surface of a sphere (soccer-ball structure) has been provided by several techniques. NMR shows a single type of carbon bonding, and IR peaks consistent with modes characteristic of this system have been identified. Since C60 can be isolated and has stable “graphitic” bonding, it represents a unique opportunity to observe individual stable carbon molecules with transmission electron microscopy in order to test the morphology deduced from other techniques. Also, the study of packing sequences and defect structures in C60 crystals found by x-ray diffraction to have an FCC lattice constant of 1.41 nm provides important new information on variations of crystallization with conditions such as solvent type and crystallization rate.


Author(s):  
J. L. Daniel ◽  
S. J. Mayhan

Transmission electron microscopy of several nuclear ceramics has been extended to thin sections of as - fabricated poly-crystalline materials, by use of a thinning technique utilizing only common metallographic practices. The method is based on work by Doherty and Leombruno. However, while mechanical thinning (polishing) produces large, evenly thinned specimens, the surface of ceramic materials retains many shallow scratches and defects introduced by the polishing medium. On the other hand, the chemical thinning methods commonly applied produce only very small areas which are thin enough for examination by transmission electron microscopy, since preferential attack occurs on grain boundaries, inclusions, second phases, etc. By combining the chemical polish with the mechanical thinning procedures, large, relatively clean areas of ceramic materials can be produced. Another significant advantage is that in the course of thinning, the same specimens can be examined frequently and in detail by light microscopy, some physical measurements can be made along the way (e.g., microhardness, spectral transmission, autoradiography), and all observations can be closely correlated finally with the high resolution electron microscopy.


2008 ◽  
Vol 8 (12) ◽  
pp. 6338-6343
Author(s):  
K. F. Cai ◽  
L. Y. Huang ◽  
A. X. Zhang ◽  
J. L. Yin ◽  
H. Liu

SiCN nanowires are synthesized by pyrolysis of hexamethyldisilazane (HMDSN) using ferrocene as a catalyst precursor at 1200 °C in a flowing argon atmosphere on the surface of mullite substrate, polycrystalline alumina wafer and quartz tube. In oxygen-contained argon atmosphere, SiCN/SiO2 nanocables are synthesized. The as-synthesized products are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and high-resolution electron microscopy equipped with energy dispersive X-ray spectroscopy. The lengths of the nanowires and nanocables are in the millimeter range. The diameter of the SiCN nanowires grown on mullite substrate and alumina wafer ranges from about 10–70 nm, while that of the nanowires grown on quartz tube surface is in the range of around 7–10 nm. The diameters of the SiCN/SiO2 nanocables are relatively large. A vapor-liquid-solid growth mechanism of the nanostructures is proposed. The electrical resistivity of a single SiCN/SiO2 nanocable is reported for the first time.


2011 ◽  
Vol 236-238 ◽  
pp. 2019-2023
Author(s):  
Xiao Min Meng ◽  
Ai Min He

Nano-sized hollow spheres self-assembled by ZnO nanocrystals have been prepared by microemulsion method with dodecyl benzene sulfonic acid sodium salt (DBS) as the modifying and protecting agent. The product was characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high High-resolution electron microscopy (HRTEM) energy dispersive spectroscopy (EDS) and photoluminescence (PL) spectra. The results showed that the hollow sphere was composed of ZnO nanocrystals. And the PL spectrum showed a different emission at 438 nm. After heated the product, PL emission peak changed. A possible formation mechanism was also proposed.


1996 ◽  
Vol 434 ◽  
Author(s):  
R. Banerjee ◽  
S. Swaminathan ◽  
R. Wheeler ◽  
H. L. Fraser

AbstractMultilayered Ti/Al thin films (with nominally equal layer thickness of Ti and Al) have been sputter deposited on oxidized silicon substrates at room temperature. Transmission electron microscopy (TEM) and high resolution electron microscopy have been used to characterize the structure of these multilayers as a function of the layer thickness. Ti changed from an hcp to an fcc and back to an hcp structure on reduction of the layer thickness. Al too changed from an fcc to an hcp structure at a layer thickness of 2.5 nm. The observed structural transitions have been explained on the basis of the Redfield-Zangwill model. Subsequently Ti-aluminide thin films were deposited using a γ-TiAl target. These films were found to be amorphous in the as-deposited condition with crystallites of α-Ti(Al) embedded in the amorphous matrix. On annealing under a protective Ar atmosphere at a temperature of 550 °C, the Ti-aluminide film crystallized into a nanocrystalline two phase microstructure consisting of γ-TiAl and α2-Ti3Al. The crystallization of the aluminide film has been investigated in detail by in-situ annealing experiments on a hot stage in the TEM. The results of this investigation have been discussed in this paper.


1986 ◽  
Vol 41 (3) ◽  
pp. 478-482 ◽  
Author(s):  
G. W. Qiao ◽  
J. Zhou ◽  
K. H. Kuo

Application of high resolution electron microscopy (HREM) to the study of Pt-Sn/γ-Al2O3 supported catalyst, zeolites, iron catalyst for ammonia synthesis, rare-earth oxide catalysts, etc., is described. Micro-twins, dislocations and other crystallographic imperfections are observed. Moreover, the structure images of channels representing columns of cages in several kinds of zeolites as well as radiation damage processes in them have been recorded in situ. The observed images of zeolites were found to be in good agreement with the structure model projections and computer simulated images.


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