Karol Bula

The influence of filler modification on its aggregation and dispersion behaviour in silica/PBT composite

In this work, highly dispersed silica is obtained using a precipitation technique from emulsion medium. The selected emulsifier, applied in the process, allows production of silica with almost ideally spherical particles. To examine the tendency to aggregation, the silica powder is treated with commercially available silane coupling agents: 3-mercaptopropyltrimethoxysilane (A-189), N-2-(aminoethyl)-3-aminopropyltrimethoxy silane (A-1120) and 3-methacryloxypropyltrimethoxysilane (A-174). The silica microstructure is characterised by scanning electron microscopy (SEM). Size distribution of primary particles, aggregates and agglomerates structures is determined using dynamic light scattering (DLS) method. Surface treatment of silica generally enhances powder dispersibility. The pristine spherical silica and silica modified with silanes are introduced to poly(butylene terphthalate) (PBT). Dispersion of nanosize precipitated silica particles in PBT matrix is studied by SEM technique. For the visualisation of silica particles covered by polymer layer, the composite fracture surfaces are etched by air-plasma. The agglomerates of untreated silica are not efficiently destroyed during the extrusion process, whereas surface treatment by selected silanes leads to a significant reduction of agglomerate number. However, a large number of small, strongly bonded aggregates still occupied the composite structure.

Nucleation ability of advanced functional silica/lignin hybrid fillers in polypropylene composites

Novel advanced functional silica/lignin hybrid fillers were synthesized for the purpose of their application in composites with polypropylene. The use of lignin for the production of hybrid fillers is justified due to the advantages such as reduction in cost of products, improvement in biodegradability as well as antioxidant and antimicrobial properties. The study encompasses an analysis of the dispersive and morphological properties of the hybrid fillers, and investigations of phase transitions and the supermolecular structure of the composites by means of differential scanning calorimetry, polarized light microscopy, and X-ray diffractometry. The nucleation activity of the hybrid fillers was found to be strongly correlated with the chemical composition of the fillers, and their dispersive properties and porous structure characteristics. Furthermore, the particle size and area surface of the hybrid fillers play an important role in the development of polymorphic varieties of the polypropylene matrix. The study also discusses the mechanism of the formation of the β-PP variety and the transcrystalline structure in the context of the nucleation ability of the hybrid fillers. The investigations are very significant because they address the impact of the actual physicochemical parameters of the hybrid fillers on the nucleation ability and structure of composite materials.

Novel precipitated silicas: an active filler of synthetic rubber

Highly dispersed silicas have been obtained at a semi-technical scale by precipitation from sodium metasilicate solutions using appropriately diluted solutions of ammonium hydrogencarbonate or ammonium chloride. The difference, as compared to the generally applied technology of silica precipitation using acids or their anhydrides, has been the involvement of the precipitation reaction in alkaline media. Attempts have been made at changing the silica surface character from hydrophilic to more hydrophobic, using a modifier from the group of silane coupling agents. The alkoxysilanes modifiers contained groups with chemical affinity towards functional groups of butadiene–styrene rubber. Modification of silica surface using silane coupling agents has been found to improve the reinforcement of vulcanizates, by increasing the tensile and tear strength in particular.

Influence of Processing Conditions on the Thermal Stability and Mechanical Properties of PP/Silica-Lignin Composites

Functional silica-lignin dual fillers were obtained via mechanical grinding of the components (Syloid 244 silica and kraft lignin). Of particular importance here is the fact that lignin is a natural polymer and particularly that it is a waste by-product of paper production, whose recycling is highly desirable. The product underwent comprehensive dispersive-morphological and thermal analysis. SiO2-lignin hybrid fillers were also used in polypropylene-based composites, extruded via corotating a twin screw machine with different screw speeds. The thermogravimetric data obtained for the extrudates confirmed that the application of the lignin into PP produces a significant char residue. Addition of silica to lignin via this new hybrid formulation has a positive effect on the thermal stability of PP/silica-lignin composites, which can be seen even when observing the temperature for the maximum rate of weight reduction. Tensile test results show that the addition of silica by means of dual filler incorporation improves the mechanical parameters in comparison with pure PP and PP/lignin composite.

Effect of Heat Treatment on Phase Behaviour and Molecular Dynamics of Mineral-Filled PPS

Abstract Investigation concerning the structure and molecular dynamics of a nanocomposite made up of poly(p-phenylene sulfide) and silicon dioxide (SiO2) has been conducted by means of atomic force microscopy (AFM) and nuclear magnetic resonance (NMR). AFM and NMR studies of samples PPS in the neat and composite forms show that during annealing the fragmentation of big agglomerates of PPS take place. Between agglomerates and smaller aggregates there exist repulsion forces which are probably the source of fragmentation in the polymer network. The work has also proved that inside agglomerates and smaller aggregates of PPS dipolar magnetic interaction exist, whereas the electrostatic one occurs between them.

Effect of Polyethylene Functionalization on Mechanical Properties and Morphology of PE/SiO2 Composites

In this study composites of high density polyethylene (HDPE) with various SiO2 content were prepared by melt compounding using maleic anhydride grafted polyethylene (PE-g-MAH) as a compatibilizer. The composites containing 2, 4 and 6% by weight of SiO2 particles were melt-blended in a co-rotating twin screw extruder. In all composites, polyethylene-graft-maleic anhydride copolymer (PE-g-MAH, with 0.85% maleic anhydride content) was added as a compatibilizer in the amount of 2% by weight. Morphology of inorganic silica filler precipitated from emulsion media was investigated. Mechanical properties and composite microstructure were determined by tensile tests and scanning electron microscopy technique (SEM). Tensile strength, yield stress, Youngs modulus and elongation at break of PE/SiO2 composites were mainly discussed against the properties of PE/PE-g-MAH/SiO2 composites. The most pronounced increase in mechanical parameters was observed in Youngs modulus for composites with polyethylene grafted with maleic anhydride. The increase in the E-modulus of PE/PE-g-MAH/SiO2composites was associated with the compatibility and improvement of interfacial adhesion between the polyethylene matrix and the nanoparticles, leading to an increased degree of particle dispersion. This finding was verified on the basis of SEM micrographs for composites of PE/PE-g-MAH/4% by weight of SiO2. The micrographs clearly documented that addition of only 2 wt% of the compatibilizer changed the composite morphology by reducing filler aggregates size as well as their number. Increased adhesion between the PE matrix and SiO2 particles was interpreted to be a result of interactions taking place between the polar groups of maleic anhydride and silanol groups on the silica surface. These interactions are responsible for reduction of the size of silica aggregates, leading to improved mechanical properties.

Functional polypropylene composites filled with ultra-fine magnesium hydroxide

Abstract Magnesium hydroxide was prepared under controlled conditions from aqueous Mg(NO3)2 and NaOH solutions. The small, nanoplate-shaped particle size distribution was monomodal from 164 to 459 nm. Functional polypropylene/Mg(OH)2 and polypropylene/polypropylene 1% maleic anhydride/Mg(OH)2 composites were prepared containing 10% or 30% Mg(OH)2. The composites have a high Young’s modulus (twice that of polypropylene) and comparable tensile strength but less ductility. EDX examination of the fractured composite surfaces suggested a homogeneous Mg(OH)2 distribution for composites produced with the addition of polypropylene grafted with maleic anhydride. The polypropylene/Mg(OH)2 composites showed good antibacterial activity. The polypropylene/polypropylene 1% maleic anhydride/Mg(OH)2 composites were less effective. Graphical Abstract

Evaluation of Synthetic Magnesium Silicate as a New Polymer Filler

The paper reports on the performance of highly dispersed synthetic magnesium silicate as a filler of the styrene–butadiene rubber (SBR). The magnesium silicate has been precipitated and characterized by determination of particle size distribution, electrokinetic potential, nitrogen adsorption/desorption isotherms and SEM observation. At the subsequent stage of the study its surface has been modified by silane coupling agents. The unmodified and silane-grafted magnesium silicate samples have been used as fillers of SBR of standard testing composition. The vulcanizates obtained with the fillers have been tested as to their physical and mechanical performance. The vulcanizates filled with synthetic magnesium silicate have been found to show much better mechanical parameters than unfilled rubber. Modification of the synthetic magnesium silicates with silane coupling agents has further improved the mechanical characteristics of the vulcanizates.

The use of IR thermography to show the mold and part temperature evolution in injection molding

Abstract This study concerns the application of infrared camera for injection molding analysis by measuring temperatures of both injection molded parts and injection mold cavities in a function of injection cycles. The mold with two cavities, differing in thickness (1 and 3 mm), and a cold direct runner was used. Isotactic polypropylene homopolymer was utilized to produce parts. Mold temperature was set at 22°C and controlled by a water chiller. Five measuring points were determined: SP1, SP2 (placed in the 3 mm cavity), SP3, SP4 (located in the 1 mm cavity) and SP5 around an injection molding gate. Our investigations showed that the highest temperature is localized around SP2 point and the lowest at SP4. Also, it was proved that even after 62 injection molding cycles, temperatures of cavities were not stable, revealing their further increase with each cycle.