Kinetic studies of styrene-grafted natural rubber emulsion copolymerization using transmission electron microscope and thermal gravimetric analysis

Polymer ◽  
2015 ◽  
Vol 67 ◽  
pp. 249-257 ◽  
Author(s):  
Santi Jaimuang ◽  
Terdthai Vatanatham ◽  
Sunun Limtrakul ◽  
Paweena Prapainainar
Author(s):  
P. Sadhukhan ◽  
J. B. Zimmerman

Rubber stocks, specially tires, are composed of natural rubber and synthetic polymers and also of several compounding ingredients, such as carbon black, silica, zinc oxide etc. These are generally mixed and vulcanized with additional curing agents, mainly organic in nature, to achieve certain “designing properties” including wear, traction, rolling resistance and handling of tires. Considerable importance is, therefore, attached both by the manufacturers and their competitors to be able to extract, identify and characterize various types of fillers and pigments. Several analytical procedures have been in use to extract, preferentially, these fillers and pigments and subsequently identify and characterize them under a transmission electron microscope.Rubber stocks and tire sections are subjected to heat under nitrogen atmosphere to 550°C for one hour and then cooled under nitrogen to remove polymers, leaving behind carbon black, silica and zinc oxide and 650°C to eliminate carbon blacks, leaving only silica and zinc oxide.


2016 ◽  
Vol 33 (1) ◽  
pp. 92-113 ◽  
Author(s):  
Sajad Shojai Nasab ◽  
Saeed Zahmatkesh

In this study, a new diacid monomer containing amide, imide, and sulfone functional groups was successfully used to synthesize a new poly(ether-amide) for membrane-based gas separation applications. The synthesized poly(ether-amide) was soluble in organic solvents, has high thermal stability (up to 460℃ under nitrogen atmosphere, for 10% weight loss), and high glass transition temperature (Tg = 274℃). This poly(ether-amide) was combined with different amounts of surface-modified zinc oxide nanoparticles to provide organic–inorganic nanocomposites. The optically transparent and flexible membranes of these hybrid nanocomposites were prepared. The obtained materials were characterized by Fourier transform-infrared spectroscopy, thermal gravimetric analysis, differential scanning calorimetry, X-ray powder diffraction, field emission-scanning electron microscopy, and transmission electron microscopy techniques. Transmission electron microscopy of the nanocomposite film with 15 wt% zinc oxide confirms that the nanoparticles are well dispersed in the polymer matrix. Thermal gravimetric analysis data indicated that the hybrid materials had better thermal behavior with increasing surface-modified zinc oxide nanoparticles nanoparticle content. The poly(ether-amide)/surface-modified zinc oxide nanoparticles nanocomposite film mechanical properties improved with increasing surface-modified zinc oxide nanoparticles content. The permeability and selectivity of the poly(ether-amide)/zinc oxide membranes as a function of the surface-modified zinc oxide nanoparticles weight percentage were studied, and the results indicated that the CO2 and CH4 permeability increased with increasing zinc oxide content. In general, the membranes prepared from these polymers showed very good permeability and permselectivity for a pair of gases.


Author(s):  
R. A. Waugh ◽  
J. R. Sommer

Cardiac sarcoplasmic reticulum (SR) is a complex system of intracellular tubules that, due to their small size and juxtaposition to such electron-dense structures as mitochondria and myofibrils, are often inconspicuous in conventionally prepared electron microscopic material. This study reports a method with which the SR is selectively “stained” which facilitates visualizationwith the transmission electron microscope.


Author(s):  
Sanford H. Vernick ◽  
Anastasios Tousimis ◽  
Victor Sprague

Recent electron microscope studies have greatly expanded our knowledge of the structure of the Microsporida, particularly of the developing and mature spore. Since these studies involved mainly sectioned material, they have revealed much internal detail of the spores but relatively little surface detail. This report concerns observations on the spore surface by means of the transmission electron microscope.


Author(s):  
H. Tochigi ◽  
H. Uchida ◽  
S. Shirai ◽  
K. Akashi ◽  
D. J. Evins ◽  
...  

A New High Excitation Objective Lens (Second-Zone Objective Lens) was discussed at Twenty-Sixth Annual EMSA Meeting. A new commercially available Transmission Electron Microscope incorporating this new lens has been completed.Major advantages of the new instrument allow an extremely small beam to be produced on the specimen plane which minimizes specimen beam damages, reduces contamination and drift.


Author(s):  
G. Cliff ◽  
M.J. Nasir ◽  
G.W. Lorimer ◽  
N. Ridley

In a specimen which is transmission thin to 100 kV electrons - a sample in which X-ray absorption is so insignificant that it can be neglected and where fluorescence effects can generally be ignored (1,2) - a ratio of characteristic X-ray intensities, I1/I2 can be converted into a weight fraction ratio, C1/C2, using the equationwhere k12 is, at a given voltage, a constant independent of composition or thickness, k12 values can be determined experimentally from thin standards (3) or calculated (4,6). Both experimental and calculated k12 values have been obtained for K(11<Z>19),kα(Z>19) and some Lα radiation (3,6) at 100 kV. The object of the present series of experiments was to experimentally determine k12 values at voltages between 200 and 1000 kV and to compare these with calculated values.The experiments were carried out on an AEI-EM7 HVEM fitted with an energy dispersive X-ray detector.


Author(s):  
R. Sinclair ◽  
B.E. Jacobson

INTRODUCTIONThe prospect of performing chemical analysis of thin specimens at any desired level of resolution is particularly appealing to the materials scientist. Commercial TEM-based systems are now available which virtually provide this capability. The purpose of this contribution is to illustrate its application to problems which would have been intractable until recently, pointing out some current limitations.X-RAY ANALYSISIn an attempt to fabricate superconducting materials with high critical currents and temperature, thin Nb3Sn films have been prepared by electron beam vapor deposition [1]. Fine-grain size material is desirable which may be achieved by codeposition with small amounts of Al2O3 . Figure 1 shows the STEM microstructure, with large (∽ 200 Å dia) voids present at the grain boundaries. Higher quality TEM micrographs (e.g. fig. 2) reveal the presence of small voids within the grains which are absent in pure Nb3Sn prepared under identical conditions. The X-ray spectrum from large (∽ lμ dia) or small (∽100 Ǻ dia) areas within the grains indicates only small amounts of A1 (fig.3).


Author(s):  
J.N. Chapman ◽  
P.E. Batson ◽  
E.M. Waddell ◽  
R.P. Ferrier

By far the most commonly used mode of Lorentz microscopy in the examination of ferromagnetic thin films is the Fresnel or defocus mode. Use of this mode in the conventional transmission electron microscope (CTEM) is straightforward and immediately reveals the existence of all domain walls present. However, if such quantitative information as the domain wall profile is required, the technique suffers from several disadvantages. These include the inability to directly observe fine image detail on the viewing screen because of the stringent illumination coherence requirements, the difficulty of accurately translating part of a photographic plate into quantitative electron intensity data, and, perhaps most severe, the difficulty of interpreting this data. One solution to the first-named problem is to use a CTEM equipped with a field emission gun (FEG) (Inoue, Harada and Yamamoto 1977) whilst a second is to use the equivalent mode of image formation in a scanning transmission electron microscope (STEM) (Chapman, Batson, Waddell, Ferrier and Craven 1977), a technique which largely overcomes the second-named problem as well.


Author(s):  
J. R. Fields

The energy analysis of electrons scattered by a specimen in a scanning transmission electron microscope can improve contrast as well as aid in chemical identification. In so far as energy analysis is useful, one would like to be able to design a spectrometer which is tailored to his particular needs. In our own case, we require a spectrometer which will accept a parallel incident beam and which will focus the electrons in both the median and perpendicular planes. In addition, since we intend to follow the spectrometer by a detector array rather than a single energy selecting slit, we need as great a dispersion as possible. Therefore, we would like to follow our spectrometer by a magnifying lens. Consequently, the line along which electrons of varying energy are dispersed must be normal to the direction of the central ray at the spectrometer exit.


Author(s):  
M. G. R. Thomson

The variation of contrast and signal to noise ratio with change in detector solid angle in the high resolution scanning transmission electron microscope was discussed in an earlier paper. In that paper the conclusions were that the most favourable conditions for the imaging of isolated single heavy atoms were, using the notation in figure 1, either bright field phase contrast with β0⋍0.5 α0, or dark field with an annular detector subtending an angle between ao and effectively π/2.The microscope is represented simply by the model illustrated in figure 1, and the objective lens is characterised by its coefficient of spherical aberration Cs. All the results for the Scanning Transmission Electron Microscope (STEM) may with care be applied to the Conventional Electron Microscope (CEM). The object atom is represented as detailed in reference 2, except that ϕ(θ) is taken to be the constant ϕ(0) to simplify the integration. This is reasonable for θ ≤ 0.1 θ0, where 60 is the screening angle.


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