Thesis (Ph. D.)--University of Missouri-Columbia, 1999. / Typescript. Vita. Includes bibliographical references (leaves 193-197). Also available on the Internet.

Polypropylene has proven to be the ideal material for the outer shell of the lead acid batteries. Due to its mold-ability and inert properties the material provides a capsule for the functioning components of the lead acid battery and can withstand a variety conditions encountered during its application, such as impact shock resistance, high and low temperatures and acid resistance. Polypropylene has however become of great concern with regards to environmental pollution since it is generally resistant to normal conditions of degradation and can only be properly disposed of by incineration. This factor has encouraged the industry to find ways to regenerate spent polypropylene. A good example of such a process is the recycling of lead acid batteries. This allows not only for the regeneration of lead, but also for the recycling of polypropylene in the manufacturing of battery cases. There are some cost advantages in using recycled polypropylene. However it does have its disadvantages in that the material does start to deteriorate after multiple processes. A common practice amongst battery manufacturers is to add virgin polypropylene to the recycled material in order to ensure performance consistency. The comparative study investigated the use of various ratios of virgin and recycled PP in the manufacturing of lead acid battery cases and their influence on the physical properties and performance of the final material. The degradation of PP was also investigated as the material was subjected to multiple manufacturing processes where the influence of stabilizers was further considered. A common technique of PP analysis such as MFI was shown to be an effective technique to maintain good quality control. The study further showed that it is important that the material grade of PP used in the manufacturing of the battery case and lid is compatible in order to allow for effective heating sealing of the two components. Polypropylene has a waxy surface finish and it is generally difficult to label or write on. Labels tend to fall off in application and make it difficult to maintain a track record of the manufactured batteries with time. This study showed successfully that a laser activated dye can be added to the PP without influencing its color or its performance. This allows for successful labeling of battery cases by various bar coding writers that can trace the battery through its manufacturing process. Lead acid batteries are often operated outside the specified temperature range that is determined by battery manufacturers resulting in premature failure. These failures can occur within the warranty period of the battery and result in illicit claims since the monitoring of the batteries in its application was not possible. A suitable temperature monitoring device was designed that would be incorporated into the vent cap or lid of the battery case. The device contained temperature sensitive indicators that would undergo a permanent color change at specified temperatures thereby giving the battery manufacturer an indication as to the maximum temperature the battery was exposed to.

D.Ing. (Civil Engineering) / Polypropylene (PP) fibre is one of the most widely used fibres for reinforcing concrete. Due to its unique material properties such as economic production cost, relatively high melting point and alkaline resistance, PP fibres in concrete are found to increase the toughness, provide restrained plastic and drying shrinkage cracking resistance, increase impact resistance and flexural loading capacity (especially during the post-crack stage) of concrete structures and components. The wettability of PP fibre surfaces is poor due to the hydrophobic surface nature of polypropylene. The bonding between the PP fibre and the concrete matrix is recognized as poor and currently the PP fibre / concrete interfacial bonding depends upon interlocking and keying (mechanical bonding). As the interfacial bond strength between the PP fibre and the concrete is much smaller than the tensile strength of PP fibre and concrete, in order to fully explore the reinforcing effect of PP fibres in concrete, further improvement of interfacial bonding is necessary. In this investigation, the research work was conducted on the surface oxyfluorinated PP fibre newly developed by the Atomic Energy Corporation of South Africa Limited. Examining the feasibility of using this fibre in concrete, as well as evaluating its superiority over unmodified PP fibres, is the key task of this investigation. This new type of oxyfluorinated PP fibre shows a large increase in interfacial bond strength compared to the unmodified PP fibres. The surface free energy concept and Lewis acid-base interfacial interaction theory were innovatively used to examine the interfacial bonding between the PP fibre and the concrete matrix. The purpose of this study was to develop the background of such oxyfluorinated PP fibres, to establish the mechanism of the increase in interfacial bonding and to investigate the basic properties of the concrete incorporating oxyfluorinated PP fibres. The experimental results on the properties of oxyfluorinated PP fibre reinforced concrete compared with those of unmodified PP fibre reinforced concrete and plain concrete are presented, with some field test results focused on the improvement in shrinkage cracking control capacity. It is concluded in this investigation that the surface oxyfluorinated PP fibres possess significantly increased PP fibre / concrete interfacial bonding due to the chemical bond arising from the acid base interfacial interaction and the intimate interfacial contact arising from the improved fibre surface wettability. When combining oxyfluorinated pp fibre with concrete, a general improvement in the physical and mechanical properties of fibrous concrete compared to that created with unmodified PP fibres, is obtained.

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Yes / Orientation direction dependency of whitening activated at large strains was studied using four pre-oriented isotactic polypropylene (iPP) samples with different molecular weights stretched along different directions with respect to the pre-orientation (0°, 45°, and 90°) by means of in situ wide-, small-, and ultra-small-angle X-ray scattering techniques. A macroscopic fracture of iPP materials was also observed following the stress whitening at large strains. These two associated processes in pre-oriented iPP samples at elevated temperatures were found to be governed by not only the molecular weight of iPP but also the pre-orientation direction. For a certain pre-orientation direction of iPP, both the critical stress of cavitation induced-whitening and failure stress increased with increasing molecular weight. For one given molecular weight, the pre-oriented iPP showed the smallest critical stress for whitening and failure stress along the pre-orientation direction (0°) while the samples displayed larger values for the same behaviors when stretched at 45° or 90° with respect to the pre-orientation direction. Such behavior suggested that oriented amorphous networks, with different mechanical strengths, can be generated during the second deformation processes in these pre-oriented iPP samples. The evolution of inter-fibrillar tie chains in highly oriented amorphous networks was considered as the main factor controlling the response of the inner network to the external stress since the cavitation-induced whitening activated at large strains was caused by the failure of load bearing inter-fibrillar tie chains in the oriented amorphous network.

ABSTRACT SYNTHESIS AND CHARACTERIZATION OF SURFACE SULFONATED POLYPROPYLENE FILMS Ecevit, Safiye Tuba M.S., The Department of Polymer Science and Technology Supervisor: Leyla Aras, Prof. Dr. Co- Supervisor: Teoman Tin&ccedil / er, Prof. Dr. March 2004, 44 pages The basic reseach on the surface sulfonation of the polypropylene is very important due to the surface design for higher functionalization. For this purpose, liquid-phase sulfonation of the polypropylene surfaces at various temperatures for different time periods were performed by concentrated sulphuric acid. The physical and chemical changes formed by the effect of the sulfonation on the polypropylene surfaces were determined by contact angle measurement, mechanical analysis, UV-Vis spectrometer, differential scanning calorimeter (DSC) and scanning electron microscopy (SEM). The surface polarity and wetting properties of the samples were evaluated by contact angle measurement. It is seen that, sulfonation at low temperatures and short time periods improve these two properties of the polypropylene surfaces. Sulfonation at high temperatures and long time periods however, cause the partial breakdown of the polymer by degradation. Noticeable color change due to the degradation and carbonization of the polypropylene films sulfonated at high temperature and long time were supported by the UV-Vis spectra of the samples. Mechanical properties of sulfonated PP films were investigated. Consequently, after the sulfonation process the mechanical properties of the PP films showed a general trend of decrease with sulfonation time for a given temperature and a very fast decrease at high temperature of sulfonation. Thermal characteristics were found by differential scanning calorimeter (DSC). Thermal analysis revealed that sulfonated PP film samples displayed an additional endothermic peak. The physical effects of the sulfonation were examined by scanning electron microscopy (SEM) which showed a hexagonal hole formations due to the bursting of the air bubbles within the PP films by the effect sulfonation. The lamelae formations were also seen around these holes.

A potential alternative to acrylonitrile-butadiene-styrene (ABS) and polycarbonate+ABS (PC+ABS), pigmented mineral-filled polypropylene (PP) finds an opening in automotive interior components such as instrument panels, knee bolsters, consoles, etc. Because of the lack of surface aesthetics, pigmented mineral-filled PP is experiencing a limitation to its acceptance in many applications. This study focuses on exploring various mineral fillers and additives in polypropylene to provide a material with enhanced scratch resistance. Several physical properties including Rockwell and Shore D hardness are investigated, and it is determined that Filler W improves scratch resistance. It is also determined that Filler T-filled-PP has poor scratch resistance even with the addition of a lubricant.

An environmentally benign process, which uses supercritical carbon dioxide (sc-CO₂) as a processing aid, was developed in this work to help exfoliate and disperse nanoclay into the polymer matrices at high clay content. The process involves the use of a pressurized CO₂ chamber to assist in the exfoliation and delivery of the clay into a stream of polypropylene (PP) melt within the extruder. This CO₂ method was evaluated and compared to other conventional processing techniques. It was observed that the conventional direct-melt compounding methods, with and without the direct injection of CO₂, did not show much improvement in the mechanical properties due to their inability to adequately exfoliate the nanoparticles into the polymer matrix. The commercial RTP sample prepared using a TSE and a MA compatibilizer showed moderate improvements in the clay dispersion and properties due to high shear forces and mixing capabilities of TSE. The most improvements were seen from the technique of using the pressurized CO₂ chamber, which directly injected pre-mixed sc-CO₂ and nanoclay into the polypropylene melt during extrusion. It was observed that the mechanical properties of the PP nanocomposites prepared using the CO₂ chamber technique, especially when combined with maleic anhydride (MA) compatibilizer, outperformed those of the commercial RTP samples and those of samples prepared using conventional melt compounding techniques. WAXD and TEM data showed a good degree of exfoliation for clay concentrations as high as 6.8 wt% when the clay was expanded and mixed with CO₂. At this concentration, mechanical properties such as yield strength and modulus increased by as much as 13% and 69%, respectively, relative to the pure PP, and approximately 15% higher than those of samples prepared by direct melt compounding (without the use of CO₂). Furthermore, yield-like behavior in the viscosity and a plateau in the low-frequency behavior of storage modulus, Gâ , was also attributed to polymer-clay interaction due to strong hydrogen bonding between MA groups and the hydroxyl groups on the clay surface, not just solely to the formation of percolation network due to exfoliation between clay platelets that is commonly reported in literature for clay-filled functionalized polypropylene. / Ph. D.

The main objective of this study was the application of strength, fracture and creep/relaxation tests to plain and fibre-reinforced high-strength concretes. Initially, five grades of concrete were developed and evaluated. Target 28 day compressive strengths were 40,60,80 100 and 120 N/mm2, the latter three being high-strength concretes (HSCs) containing a süperplasticiser and 10% silica fume. The others were normal-strength mixes used for comparison purposes. Each grade was made with 10 mm maximum-sized crushed limestone and gravel coarse aggregates making ten mixes in total. All were required to have sufficiently high workability and stability to accept reasonable amounts of fibre reinforcement. The data reported allows estimates of mix proportions for a range of HSC mixes to be determined. Various amounts of steel and polypropylene fibres were then added to the ten mixes to determine their optimum and maximum practical concentrations. The traditional type of toughness test based on un-notched beams in four-point loading was not employed. Instead, notched beams in three-point loading (equivalent to the RILEM work-of-fracture arrangement) and compact compression specimens were used. Both were tested under closed-loop conditions using crack-mouth opening displacement (CMOD) control. Post-cracking toughness was determined by means of the 15a nd 110to ughness indices given in ASTM C 1018. It was found that though fracture-based tests under CMOD control were an improvement on more traditional techniques, 15 and 110 were too insensitive to allow fibre type and volume to be differentiated. Next, work-of-fracture tests to measure the fracture energy, GF, were carried out on the plain concretes, initially under quasi-static loading. Both load/deflection and load/CMOD curves were recorded. GF showed little change with strength for a given aggregate type. Even though similar grades of crushed limestone and gravel HSCs had different GF values, the measure was still considered unsuitable for characterising the fracture properties of concrete. Similar experiments were then carried out on all ten mixes at five orders of magnitude of test duration (30 seconds to 2 days). GF appeared to be independent of strain rate. Both types of test highlighted the greater suitability of load/CMOD rather than load/deflection curves when evaluating GF. Finally, combined fracture and relaxation tests were undertaken in an attempt to obtain medium term fracture parameters. Though the CMOD was locked at 90,70 and 50% of the peak load in the strain-softening region, the deflection, when measured, showed a noticeable reduction over the seven days of each experiment, suggesting that significant cracking and stress redistribution within the fracture process zone was taking place. This finding has opened up a major area of important future research by confirming that the use of quasi-static fracture parameters in finite element studies is suspect.