Effect of thermal treatment on the structure and texture of titania

Anatase and rutile pigments, from two sources (B and T) were thoroughly purified from sulphate and chloride contaminants, thermally treated in the temperature range 150 to 550 ° C, and investigated using thermogravimetric (TG), differential thermal analysis (DTA), X-ray diffraction (XRD), nitrogen and organic vapour adsorption techniques. TG analysis reveals two main dehydration steps, the first results from physically adsorbed water and the second from structural and ligand water. The number of ligand water molecules released through a unit surface area (nm²) is in the range 4.50 to 5.15, being evolved in the temperature range 250 to 300 ° C. Two dehydroxylation endotherms appear for the anatase samples in the temperature range 350 to 420 ° C which seem to arise from the presence of two types of hydroxyls. No transformation from the anatase to rutile sructure occurred in the temperature range investigated. Estimation of crystallite sizes showed a marked increase at temperatures >250 ° C for anatase (B), being greatest for the (101) plane, and >400 ° C for rutile (B), where the three planes (101), (110) and (111) increased distinctly. Maximum anisotropy was observed for the anatase heated at 550 ° C. Nitrogen adsorption data revealed a marked decrease in the specific area and total pore volume by thermal treatment 400 ° C for anatase and 250 ° C for rutile whereby it retains a nearly stable value with an average range of 2.62 nm. The anatase (B) samples are composed of a mixture of both meso- and micropores whereas for rutile (B) microporosity appeared only for the sample heated at 150 ° C, becoming predominantly mesoporous at higher temperatures. Most heated samples exhibited two group sizes in the mesopore range resulting from their existence in the form of particles constituted from a collection of small particulates. The rutile (B) products are generally characterized by possessing a wider pore system than those from anatase. The anatase (T) samples are predominantly microporous at 150 ° C and become mesoporous at 550 ° C — the reverse is true for rutile (T). Cyclohexane and benzene adsorption measure only a fraction of the nitrogen area. Specific interaction (H-bonding) is believed to exist in some cases between the cyclohexane molecules and titania surface hydroxyls, as well as some enhanced adsorption which is believed to occur with benzene adsorbate.     

Effects of Filler Loading and Different Preparation Methods on Properties of Cassava Starch/Natural Rubber Composites

Cassava starch-filled natural rubber (NR) composites were prepared by using direct blending and co-coagulation method. The effects of two different method and cassava starch loading on morphology, mechanical properties and thermal properties of cassava starch/NR composites were studied. X-ray diffraction results and scanning electron microscopy images proved that co-coagulation method promotes better dispersion of cassava starch than direct blending method. The composites prepared by co-coagulation method exhibited higher values of tensile strength, tear strength, hardness, and thermal stability. The optimum value of tensile strength and tear strength of cassava starch/NR composites were achieved at a 10 phr cassava starch loading.     

Linear low‐density polyethylene‐g‐poly(acrylic acid)/(organo‐montmorillonite) hydrogel composite as hydrogel electrolytes for zinc–carbon batteries

A hydrogel composite that has been prepared by using waste linear low‐density polyethylene, acrylic acid, and organo‐montmorillonite (LLDPE‐g‐PAA/OMMT) is used as a hydrogel electrolyte. An absorbency test was used to determine the percentage of ZnCl₂ solution absorbed by the hydrogel composite. The swelling behavior of the hydrogel composite in the ZnCl₂ solution was then studied. The highest absorbency was recorded when the concentration of ZnCl₂ solution was 3 M. The conductivity of ZnCl₂‐hydrogel composite electrolytes is dependent on the solution's concentration. A mixture of ZnCl₂ solution with hydrogel composite yields a good hydrogel composite electrolyte with a conductivity of 0.039 S cm^?1 at 3 M ZnCl₂. The hydrogel composite electrolyte was used to produce zinc‐carbon cells. The fabricated cell gives capacity of 7.8 mAh, has an internal resistance of 9.9 Ω, a maximum power density of 15.78 mWcm^?2, and a short‐circuit current density of 43.75 mAcm^?2 for ZnCl₂‐hydrogel composite electrolytes. J. VINYL ADDIT. TECHNOL., 22:279–284, 2016. © 2014 Society of Plastics Engineers     

Effects of halloysite nanotubes and kaolin loading on the tensile,swelling, and oxidative degradation properties of poly(vinyl alcohol)/chitosan blends

[Halloysite nanotubes (HNT)]‐filled and kaolin filled composite films based on poly(vinyl alcohol) (PVA)/chitosan (CS) blend were prepared via solution casting method. Tensile properties, fracture morphology, FTIR spectra, thermal stability, swelling properties, moisture absorption, and oxidative degradation of the composite films were investigated. Addition of 0.5 wt% of filler led to the optimum tensile properties of the films. Increased roughness and tearing in the fracture surface morphology supported the tensile results. The FTIR results indicated there were physical interactions present in the composite films. Thermal stability of the composite films differed slightly where PVA/CS/HNT composite films showed better thermal stability than PVA/CS/kaolin composite films. Moreover, the presence of HNT and kaolin fillers in the blend reduced the swelling and moisture absorption properties of the films. Finally, the composite films were degraded by using Fenton's reagent. Degradation percentage of the composite films decreased with increasing filler loading. J. VINYL ADDIT. TECHNOL., 19:55–64, 2013. © 2013 Society of Plastics Engineers     

Facial fabrication of self-healing natural rubber foam based on zinc thiolate ionic networks

In this work, self-healing natural rubber (SHNR) foam incorporating an intrinsic zinc thiolate ionic network was successfully prepared. The materials exhibited the ability to autonomously repair damage at room temperature without the need for external triggers. The investigation focused on the effect of sodium bicarbonate, employed as a blowing agent, on the self-healing performance, as well as the physical and mechanical properties of the foam. Various concentrations of sodium bicarbonate (0, 1, 4, 8, and 10 phr) were employed. The conventional two-roller mill was used for mixing and compounding, while compression molding was utilized for the vulcanization process. With increasing sodium bicarbonate concentration, the density, tensile strength, elongation at break, and compression set of the self-healing NR foam were found to decreased. Conversely, the porosity, shrinkage, compressive strength, and water uptake of the SHNR foam increased as the concentration of sodium bicarbonate increased. Scanning electron microscopy analysis revealed that the optimal concentration of sodium bicarbonate (8 phr) resulted in smaller, finer, and more uniform porous structures. The self-healing rubber foam incorporating 8 phr sodium bicarbonate exhibited improved properties in terms of tensile modulus, elongation at break, and tear strength, with healing efficiencies of 91.27%, 69.39%, and 83.99%, respectively.     

Effects of Bonding Agents on the Mechanical Properties of the Composites Made of Natural Rubber and Oil Palm Empty Fruit Bunch

The effects of various bonding agents on natural rubber-oil palm wood flour (OPWF) composites were studied. Results indicate that the maximum torque increases with increasing OPWF loading and the incorporation of various bonding agents. Compared to the composite without a bonding agent, the incorporation of bonding agents improves the tensile modulus, tear strength, tensile strength, and hardness of the composites. Scanning electron microscopy studies and rubber-fiber interaction measurements indicate that the OPWF-rubber adhesion can be enhanced by the use of bonding agents.     

White Rice Husk Ash-Filled Natural Rubber Compounds: The Effect of Bonding Agents

White rice husk ash (WRHA)-filled natural rubber compounds were prepared by using a laboratory-size two-roll mixing mill. Curing using a conventional vulcanization system was used and cure studies were carried out on a Monsanto rheometer. The mechanical testing of the vul-canizates involves the determination of tensile properties, tear strength, hardness, and resilience. Scanning electron microscopy (SEM) and swelling measurement were also done. The effects of bonding agents on the curing and mechanical properties have been investigated using re-sorsinol formaldehyde and hexamethylene tetramine as the bonding agents. Results show that the bonding agents prolonged the cure time t ₉₀ and scorch time t ₂ and, at the same time, improved the mechanical properties of the natural rubber vulcanizates. SEM and swelling studies indicate that the rubber-filler interaction is improved with the addition of bonding agents.     

Evolution of the microstructure of unconsolidated geopolymers by thermoporometry

This paper studies the evolution of the pore size distribution of a fresh unconsolidated geopolymer paste between one day and a week, using thermoporometry. This was made possible by following a careful protocol for sample preparation and for analysis by differential scanning calorimetry. In contrast with nitrogen gas adsorption, this method quantifies directly the amount of water in pores. It also does not require heat and vacuum drying, thus maintaining the fragile pore structure of the unconsolidated paste. Moreover, it was found that, in a typical metakaolin-based sodium geopolymer with a 10 to 20 hours workability period, the porosity gradually refines during the first week while the mesoporous volume is cut in half. This is probably due to the fact that the geopolymer network was still actively condensing from the activation solution. Part of the pore water never froze and, from mass balance, this residual water was attributed to the water bound in the hydration shell of the sodium counter ions. Only a minor occurrence of covalently bound protons as silanol groups was observed. The results presented here usefully complement data obtained by conventional techniques at later ages on consolidated geopolymers. It supports the growing body of literature on the structural evolution of geopolymers with time.     

Effect of partial replacement of chitosan with halloysite nanotubes on the properties of polylactic acid hybrid biocomposites

In this study, hybrid chitosan/halloysite nanotubes (Cs/HNTs) reinforced polylactic acid (PLA) were prepared via melt compounding and compression molding techniques. In the fabrication of PLA/Cs/HNTs hybrid biocomposites, the partial replacement of Cs with HNTs was performed at filler loading of 2.5 parts per hundred parts of polymer (php), proceeding from the highest tensile strength of PLA/Cs obtained in our previous study. Cs was partially replaced with different HNTs loadings (0.5, 1, 1.5, 2, and 2.5) php and its effects on the functional group, thermal, tensile, morphological, and water absorption properties were investigated systematically. The results revealed that the combined loading of 1 php Cs and 1.5 php HNTs hybrid fillers into PLA showed the best performance in all properties. Fourier transform infrared spectroscopy (FTIR) analysis indicated that the siloxane (Si O) group of HNTs had chemically interacted with the amine group of Cs. The thermal analysis demonstrated that partial replacement of Cs with 1.5 php HNTs improved the thermal stability of PLA/2.5Cs/0HNTs biocomposite by ~12%. Yet, the percentage of crystallinity (χ_c) reduced with HNTs addition due to the phase adhesion improvement. Moreover, PLA/1Cs/1.5HNTs hybrid biocomposites showed the highest tensile strength and elongation at break of 59 MPa and 2.72%, respectively. This correlated with the uniform dispersion and better interfacial adhesion between Cs/HNTs fillers in the PLA matrix, as confirmed by the field emission scanning electron microscopy (FESEM). In addition, partial replacement of Cs with HNTs exhibited a lower water absorption percentage, which suggested the advantage of hybrid fillers to reduce water uptake, and is beneficial in a wide range of applications.     

Oil palm wood flour filled natural rubber composites: fatigue and hysteresis behaviour

The fatigue and hysteresis behaviour of oil palm wood flour (OPWF) filled natural rubber composites was studied. The stress at any strain decreased with increasing OPWF loading in the composites. As the filler loading increased, the poor wetting of the OPWF by the rubber matrix gave rise to poor interfacial adhesion between the filler and rubber matrix. Results also indicate that the composite with the highest loading of OPWF was the most sensitive towards changes in strain energy, and hence exhibited the highest hysteresis. Thermal ageing not only reduced the fatigue life, but also increased the hysteresis of the composites. © 2000 Society of Chemical Industry