Latex transmission electron microscopy

Paine et al. [99] tried different stabilizers [i.e., hydroxy propylcellulose, poly(N-vinylpyrollidone), and poly(acrylic acid)] in the dispersion polymerization of styrene initiated with AIBN in the ethanol medium. The direct observation of the stained thin sections of the particles by transmission electron microscopy showed the existence of stabilizer layer in 10-20 nm thickness on the surface of the polystyrene particles. When the polystyrene latexes were dissolved in dioxane and precipitated with methanol, new latex particles with a similar surface stabilizer morphology were obtained. These results supported the grafting mechanism of stabilization during dispersion polymerization of styrene in polar solvents. 

In 1997, a Chinese research group [78] used the colloidal solution of 70-nm-sized carboxylated latex particles as a subphase and spread mixtures of cationic and other surfactants at the air-solution interface. If the pH was sufficiently low (1.5-3.0), the electrostatic interaction between the polar headgroups of the monolayer and the surface groups of the latex particles was strong enough to attract the latex to the surface. A fairly densely packed array of particles could be obtained if a 2 1 mixture of octadecylamine and stearic acid was spread at the interface. The particle films could be transferred onto solid substrates using the LB technique. The structure was studied using transmission electron microscopy. 

Particle-Size Determination Particle-size of the cleaned1 latexes were determined using transmission electron microscopy after freeze-drying the samples and counting the particles with a Quantimet image analyzer. The number average particle diameters ( n) of the homopolymer, the 85/15 VA/BA and 70/30 VA/BA latexes were found to be 0.Q57/ m, 0.062/<.m and 0.073 m, respectively. 

The transmission electron microscopy results are consistent with a segregated latex particle consisting of a polystyrene rich core and a soft poly-n-butyl acrylate rich shell. 

Transmission electron microscopy (TEM) analysis (6-8) was used also to characterize the latexes in this particle growth monitoring study. The electron micrographs were taken at a magnification of 30.000X. 

Due to the high water solubility of MAA, partitioning of the MAA in the water phase was expected. After polymerization, the obtained miniemulsions (latexes) and the colloidal nanoMIPs were characterized by gravimetric analysis, dynamic light scattering (DLS), gas adsorption measurements (BET), and transmission electron microscopy (TEM) as shown in Fig. 9. 

The various latexes were characterized with respect to particle size and size distribution, surface charge and functional group density, and electrophoretic mobility behavior. As observed by transmission electron microscopy all latexes were found highly monodisperse with a uniformity ratio between 1.001 and 1.010, a property due to the short duration of the nucleation period involved in the various radical-initiated heterogeneous polymerization processes. The surface charge density was determined by a colorimetric titration method reported elsewhere [13]. 

Koehler and Provder [317] sized monodisperse PMMA latexes with a range of instruments Disc centrifugal sedimentation (DCP), sedimentation field flow fractionation (SFFF), hydrodynamic chromatography (HDC), photon correlation spectroscopy (PCS), turbidimetry and transmission electron microscopy (TEM). TEM gave the smallest sizes, DCP and SFFF were in fair agreement in the center and PCS the highest sizes. 

There are a number of procedures for determining the particle size of the latex polymer. Transmission electron microscopy (TEM) has been used for some time. The method is necessary to confirm the sphericity of the particles. Since a microscopist selects the images for further study, and the number of slides to be taken is limited for practical reasons, the statistical randomization of the measurements is somewhat questionable. Results, by the latter technique have actually been surprisingly good. 

Mondragon et al. [250] used unmodified and modified natural mbber latex (uNRL and mNRL) to prepare thermoplastic starch/natural rubber/montmorillonite type clay (TPS/NR/Na+-MMT) nanocomposites by twin-screw extrusion. Transmission electron microscopy showed that clay nanoparticles were preferentially intercalated into the mbber phase. Elastic modulus and tensile strength of TPS/NR blends were dramatically improved as a result of mbber modification. Properties of blends were almost unaffected by the dispersion of the clay except for the TPS/ mNR blend loading 2 % MMT. This was attributed to the exfoliation of the MMT. 

Zhang et al. [63] prepared styrene-butadiene nanocomposites by dispersing an aqueous dispersion of montmoril-lonite and latex and flocculating the dispersion with acid. The performance of the rubber nanocomposites were compared with clay, carbon black, and silica rubber composites prepared by standard compotmding methods. The montmoriUonite loadings for the rubber nanocomposite were up to 60 phr. The morphology of the rubber nanocomposites by transmission electron microscopy appears to indicate intercalated structures. The mechanical properties of the rubber nanocomposites were superior to all of the other additives up to about 30 phr. However, rebound resistance was inferior to all of the additives except sUica. The state of cure was not evaluated. 

Mondragon et al ° reported that unmodified and modified NR latex were used to prepare thermoplastic starch/NR/MMT nanoeomposites by twin-screw extrusion. After drying, the nanoeomposites were injection moulded to produce test specimens. SEM of fractured samples revealed that chemical modification of NR latex enhanced the interfacial adhesion between NR and thermoplastic starch (TPS), and improved their dispersion. X-ray diffraction (XRD) showed that the nanoeomposites exhibited partially intercalated/exfoKated structures. Surprisingly, transmission electron microscopy (TEM) showed that clay nanoparticles were preferentially intercalated into the rubber phase. Elastic modulus and tensile strength of TPS/NR blends were dramatically improved from 1.5 to 43 MPa and from 0.03 to 1.5 MPa, respectively, as a result of rubber modification. 

Aniline was added to a monodisperse cationic polystyrene latex and polymerisation initiated by the addition of ammonium persulphate solution, forming a core-shell latex, which was characterised by infrared spectroscopy, and scanning and transmission electron microscopy. The composites exhibited electrical conductivity comparable to that of pure polyaniline, with a percolation threshold of approximately 3 wt% polyaniline. 12 refs. 

A novel process for the preparation of latex with high solid content, but maintaining the characteristics of microemulsion polymerisation latex, small particle size (less than 50 nm) and polymer with high molecular weight (more than 10 6) is presented. With the PS latex obtained by microemulsion polymerisation as seed, core shell, styrene-butyl acrylate polymers functionalised with itaconic acid are prepared. Materials were characterised by differential scanning calorimetry, dynamic mechanical thermal analysis and transmission electron microscopy. These polymers have better mechanical properties than the non functionalised or those prepared by emulsion polymerisation. 11 refs. 

The clay plates were found to be located at the external surface of the polymer latex particles (Fig. 4.19a). These authors demonstrated in a subsequent study thata similar morphology was achieved when the clay was previously ion-exchanged with a cationic initiator (AIBA, structure 1, Table 4.4) or a cationic monomer (MADQLfAT, structure 5, Table 4.4) as illustrated in transmission electron microscopy (TEM) images (Fig. 4.19b and c) [138],... 

Figure 6.11. Idealized image intensities for transmission electron microscopy of latex particles (a) homogeneous latex, (b) core-shell latex, (c) ultramicrotomed thin section through core-shell latex. Core/shell ratio, calculated assuming 50 wt % PVC/50 wt % P(B-co-AN) and polymer densities of 1.39 and 1.06 g/cm, respectively, gives T2 = 1.31ri. ...

Cationic latex particles with surface amino groups were prepared by a multi-step batch emulsion polymerisation. Monodisperse cationic latex particles to be used as the seed were synthesised first. Then the amino-functionalised monomer, aminoethylmethacrylate hydrochloride, was used to synthesise the final functionalised latex particles. Three different azo initiators were used 2,2 -azobisisobutyramidine dihydrochloride, 2,2 -azobisdimethyleneisobutyramidine dihydrochloride, and 2,2 -azobisisobutyronitrile. Hexadecyltrimethylammonium bromide was used as the emulsifier. The latices were characterised by photon correlation spectroscopy to study the mean particle diameters, transmission electron microscopy to deteimine the particle size distributions, and hence the number- and weight-average diameters and the polydispersity index. The conversion was determined gravimetrically, the surface density of the amino groups was detemiined by conductimetric titrations, and the... 

Figure 5.12 Scaling law time dependence for two polystyrene latexes. The H135 material was composed of latexes of 325,000 g/mol polymer having hydrogen end groups. The SI35 material had —SO3 groups at the end of each molecule, with a molecular weight of 325,000 g/mol also. Particle sizes by transmission electron microscopy were in the range of 100-120 nm in all cases. Measurements were by SANS on samples annealed for interdiffusion at 135°C (79).

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