The Effect of Spray-Freeze Drying of Montmorillonite on the Morphology,Dispersion, and Crystallization in Polypropylene Nanocomposites

The spray-freeze drying (SFD) technique was applied to sonicated aqueous suspensions of spray-dried montmorillonite clay (MMT) to produce highly porous agglomerates (SFD-MMT). Both MMT (used as a reference) and SFD-MMT were subsequently incorporated in polypropylene (PP) via melt compounding to produce 2 wt % nanocomposites with and without maleic anhydride grafted polypropylene (PP-g-MA). Polypropylene nanocomposites containing SFD-MMT exhibited thinner silicate flake layers compared to large agglomerates in PP/MMT nanocomposites. SFD-MMT particles became even more finer in the presence of PP-g-MA (i.e., in PP/PP-g-MA /SFD-MMT) where it hindered PP crystallization instead of serving as nucleation sites for the PP crystallization during rapid cooling. SFD-MMT improved the thermal stability of PP/PP-g-MA by 30°C compared to only 5–8°C for MMT/nanocomposites. MMT acts as a heterogeneous nucleating agent in the nucleation-controlled PP nanocomposites, but the hindrance effect was observed for the PP/PP-g-MA with SFD-MMT. PP/PP-g-MA/SFD-MMT exhibited twice the edge surface energy as compared to PP/PP-g-MA/MMT. The incorporation of both types of MMT raised the tensile moduli of PP and PP/PP-g-MA, with no improvement in their tensile strength and a decrease in the elongation at break. The PP/PP-g-MA/SFD-MMT showed brittle failure. POLYM. ENG. SCI., 60:168–179, 2020. © 2019 Society of Plastics Engineers     

Dietary effects on growth,plasma lipid and tissues of rats fed with non‐conventional oil of Telfairia occidentalis

The nutritional value of Telfairia occidentalis seed and seed oil available in local market was studied in rats. The average values of the proximate analysis on dry matter basis were 203 g kg^?1 crude protein, 536.3 g kg^?1 fat, 39 g kg^?1 ash, 95 g kg^?1 crude fibre and 43.7 g kg^?1 carbohydrate, while the moisture content was 75 g kg^?1. The mineral analyses showed that T occidentalis seeds contain potassium (3280 mg kg^?1), sodium (1230 mg kg^?1), magnesium (60.8 mg kg^?1), calcium (60.8 mg kg^?1) and iron (13.0 mg kg^?1). The oil extracted from the seed sample showed physicochemical properties that suggest its suitability for edible and industrial uses. The oil contained high levels of unsaturated fatty acids, oleic and linoleic, which accounted for 63.22% of total fatty acids recovered, while palmitic acid (27.4% of the oil by weight) was the most prevalent saturated fatty acid in the oil. No trace of eleostearic acid was detected in the oil. The effect on physical appearance, weight gain, organ weight, tissue and plasma cholesterol and triacylglycerol levels was determined in rats fed a diet containing 5% T occidentalis oil. These were compared with those of rats fed a control diet (0% T occidentalis oil) over an 8 week study period. Weekly monitoring of the rats showed good physical appearance and steady weight increase. The test rats were not anaemic and no mortality was recorded. While there was a significantly higher (p < 0.05) level of cholesterol in the heart of test rats compared with the control, there was a significantly lower (p < 0.05) plasma cholesterol level, suggesting that T occidentalis seed oil can be used to lower plasma levels of cholesterol. Histological examination of the sections of the heart, liver, kidney and spleen of the test rats revealed varying degrees of pathology. These include artherosclerotic changes in the walls of vasa vasori and lymphatics in the heart and hyaline degeneration of myofibrils, fatty infiltration of hepatocytes, and glomerular and tubular degeneration in the kidneys. These lesions may have been due to the effect of fatty acids, especially erucic acid, in the seed oil, which at 1.24% (less that the 5% conventional allowable limit for edible oils) may be intolerable for rats and may be unsuitable for human consumption. The seed oil may be used for industrial purposes such as soap making, lubrication and cosmetics for which it is well suited. Copyright © 2004 Society of Chemical Industry     

Improving the functional properties of soy glycinin by enzymatic treatment. Adsorption and foaming characteristics

In this contribution we have determined the effect of limited enzymatic hydrolysis on the interfacial (dynamics of adsorption and surface dilatational properties) and foaming (foam formation and stabilization) characteristics of a soy globulin (glycinin, fraction 11S). The degree of hydrolysis (DH=0%, 2%, and 6%), the pH of the aqueous solution (pH=5 and 7), and the protein concentration in solution (at 0.1, 0.5 and 1 wt%) were the variables studied. The temperature and the ionic strength were maintained constant at 20 °C and 0.05 M, respectively. The rate of adsorption and surface dilatational properties (surface dilatational modulus, E, and loss angle) of glycinin at the air–water interface depend on the pH and DH. The adsorption decreased drastically at pH 5.0, close to the isoelectric point of glycinin, because of the existence of a lag period and a low rate of diffusion. The interfacial characteristics of glycinin are much improved by enzymatic treatment, especially in the case of acidic aqueous solutions. Hydrolysates with a low DH have improved functional properties (mainly foaming capacity and foam stability), especially at pH close to the isoelectric point (pI), because the native protein is more difficult to convert into a film at fluid interfaces at pH≈pI. The foam capacity depends on the rate of diffusion of protein to the interface and is much improved by the enzymatic treatment. Foam stability correlates with surface pressure and, to a minor extent, with surface dilatational modulus at long-term adsorption with few exceptions.     

Indentation Damage and Residual Stress Field in Alumina-Y2O3-Stabilized Zirconia Composites

Fracture features, residual stresses, and zirconia transformation are studied in indentation strength specimens of alumina-Y₂O₃-stabilized zirconia (3% mol of Y₂O₃, 3YTZP) ceramics in order to analyze the extension of the indentation damage in the bulk of the specimens. Two compositions, 5 vol% 3YTZP (A5) and 40 vol% 3YTZP (A40), have been prepared by stacking tape-casted tapes and sintering. After indentation with loads ranging from 50 to 300 N, samples were fractured in four-point bending and the fracture surfaces were characterized by scanning electron microscopy. Raman and piezospectroscopic techniques were used to determine the monoclinic zirconia fraction and the residual stresses through the fracture surfaces. In the A5 composition, the indentation damage morphology was clearly half-penny, whereas the A40 composition presented Palmqvist crack formation. Zirconia transformation was only observed in the plastically deformed zones underneath the imprints whereas there were significant residual compressive stresses outside the plastic zones due to the indentation damage. The intensity of this residual compressive field was dependent on the level of zirconia transformation due to indentation damage because zirconia transformation induced tensile stress fields superimposed on the compressive stresses.     

Model oxide-supported metal catalysts: energetics,particle thicknesses,chemisorption and catalytic properties

Many industrially important catalysts consist of late transition metal particles supported on the surfaces of oxide materials. Our studies of such systems using model catalysts consisting of metal films vapor deposited onto the surfaces of single-crystalline oxides are reviewed here. Systems studied include Cu on ZnO, Pt on ZnO, Au on TiO₂ and Cu, Ag and Pb on MgO. A unique adsorption microcalorimeter was developed to measure directly the energetic stability of the metal atoms on the oxide surfaces and the adhesion energy at the metal/oxide interface, which clarify the structural and chemisorption properties of the ultrathin metal particles. The structure of the oxide surface and the metal particles was elucidated by low-energy electron diffraction (LEED), low-energy ion scattering spectroscopy (ISS), angular-resolved X-ray photoelectron spectroscopy (XPS) and X-ray photoelectron diffraction (XPD). The electronic character of the metal particles was revealed by XPS, Auger electron spectroscopy (AES), band-bending and work function measurements. Sintering rates were measured by temperature-programmed ion scattering spectroscopy (TPISS). The chemisorption properties of these particles and their catalytic reactivity were monitored by mass spectroscopy and temperature-programmed desorption (TPD).     

Adsorption of 4-chlorophenol by inexpensive sewage sludge-based adsorbents

Sewage sludge was used as precursor to develop a potential inexpensive adsorbent by both simple drying and pyrolysis. The resulting materials were evaluated as adsorbents for the removal of 4-chlorophenol (4-CP) from aqueous solution. The dried biosolids showed a BET surface area lower than 3 m²/g, which yield a maximum adsorption capacity of 0.73 mmol 4-CP/g at pH 5.0 and 15 °C. The carbonization of biosolids under relatively mild conditions allowed obtaining materials with BET surface area up to 45 m²/g, which led to a significant increase of the maximum adsorption capacity (1.36 mmol 4-CP/g). The high ash content of the starting material (23%, d.b.) limits the development of porosity on a total dry-weight basis. Adsorption data were well fitted to the Redlich–Peterson isotherm equation whereas the most commonly used Langmuir and Freundlich equations were less satisfactory probably because of the occurrence of summative adsorption phenomenon. A thermodynamic study of the adsorption showed the spontaneous and exothermic nature of the process. Thus, simple drying and carbonization provide two ways of valorization of sewage sludge through its conversion into inexpensive low-rank adsorbents potentially useful for the removal of some hazardous water pollutants, like chlorophenols and related compounds.     

Manufacture and measurement of combinatorial libraries of dielectric ceramics: Part II. Dielectric measurements of Ba1−xSrxTiO3 libraries

Applying combinatorial methods to materials science offers the opportunity to accelerate the discovery of more efficient dielectric ceramics. High-throughput methods have the potential to investigate the effects of a wide range of dopants on the dielectric properties, and to optimise existing systems, encouraging the short innovation cycles that the communications technology industry requires. The London University Search Instrument (LUSI) is a fully automated, high-throughput combinatorial robot that has the potential capability to produce large numbers of sintered bulk ceramic samples with varying composition in 1 day, as combinatorial libraries on alumina substrates. Ba_1−xSr_xTiO₃ (BST) libraries were produced by LUSI as a proof-of-principle, with x = 0–1 in steps of 0.1, and fired to 1350 and 1400 °C for 1 h. Part I of this paper described the manufacture and physical characterisation of BST libraries, showing a regular change in composition with x across the libraries. In this second part, the dielectric properties of BST libraries produced by LUSI are assessed at frequencies between 100 Hz and 1 MHz, and at temperatures between 150 and 500 K. Local piezoelectric properties were also characterised by scanning probe microscope (SPM). All measurements showed evidence of a clear functional gradient varying with x across the library, with measured _r corresponding to expected values for BST.     

rGO Sheets/ZnFe2O4 Nanocomposities as an Efficient Electro Catalyst Material for I3−/I− Reaction for High Performance DSSCs

In this paper, Reduced Graphene Oxide (rGO)/ZnFe₂O₄ (rZnF) nanocomposite is synthesized by a simple hydrothermal method and employed as a counter electrode (CE) material for tri-iodide redox reactions in Dye sensitized solar cells (DSSC) to replace the traditional high cost platinum (Pt) CE. X-ray diffraction analysis and High resolution Transmission electron microscopy, clearly indicated the formation of rZnF nanocomposite and also amorphous rGO sheets were smoothly distributed on the surface of ZnFe₂O₄ (ZnF) nanostructure. The rZnF-50 CE shows excellent electro catalytic activity toward I₃^? reduction, which has simultaneously been confirmed by cyclic voltammetry, electrochemical impedance spectroscopy and Tafel polarization measurements. A DSSC developed by rZnF-50 CE (η?=?8.71%) obtained quite higher than the Pt (η?=?8.53%) based CE under the same condition. The superior performances of rZnF-50 CE due to addition of graphene in to Spinel (ZnF) nanostructure results in creation of highly active electrochemical sites, fast electron transport linkage between CE and electrolyte. Thus it’s a promising low cost CE material for DSSCs.

     

Multiferroic Consequence of Porous (BiFeO_3)_x–(BiCrO_3)_(1-x) Composite Thin Films by Novel Sol–Gel Method

In this work, we have presented a spin-coating method to produce thin films started with pure BiCrO_3(BCO) and ended up with BiFeO_3(BFO) by increasing x values in the(BiFeO_3)_x–(BiCrO_3)_(1-x)composites. All the produced thin films have been crystallized at the annealing temperatures of 400 °C for 0.5 h. The XRD and EDAX spectrums give insight that the two crystal phases related to BCO and BFO stayed together within the thin film matrices. SEM analysis showed that the prepared composite had macroporous morphology with interconnected pores and its width(size) decreased with increasing x values. The strong correlations are observed among the microstructure, dielectric, ferroelectric, ferromagnetic properties and Fe concentration. Among all composites, the composition of 0.75 shows an attractive magnetization, polarization, switching and improved dielectric behaviors at room temperature. Significant increase in the multiferroic characteristics of 0.75 composition is due to arise of lower leakage current by causing reduction in oxygen vacancy density, and enhancement of super-exchange magnetic interaction between Fe~(3+) and Cr~(3+) at BFO/BCO interface layers. Our result shows that the thin layer on Pt(111)/Ti/SiO_2/Si substrate possesses simultaneously improved ferroelectric and ferromagnetic properties which make an inaccessible potential application for nonvolatile ferroelectric memories.