In this work, a series of cage siloxanes (spherosilicate [SS] type) was tested as functional additives for preparation of polyethylene (PE)‐based nanocomposites. For this purpose, the compounds were prepared by condensation and olefin hydrosilylation reactions. The effect of these products on properties of obtained nanocomposites was analyzed by means of mechanical, microscopic (scanning electron microscopy‐energy dispersive spectroscopy), crystallographic (X‐ray diffraction), thermal (differential scanning calorimetry, thermogravimetry), rheological Melt flow rate (MFR), and thermomechanical (heat deflection temperature) analyses. The results were compared with similar reports on silsesquioxane‐ and SS‐reinforced PE systems. Effects of SS functional group structure on the behavior of the additive and properties of the composite system were discussed. Aspects of thermal decomposition of PE‐containing SS were studied and a probable mechanism of these polymer systems degradation was proposed.
With the development of 3D printing technology, there is a need to produce printable materials with improved properties, e.g., sliding properties. In this paper, the authors present the possibilities of producing composites based on biodegradable PLA with the addition of graphite. The team created composites with the following graphite weight contents: 1%, 2.5%, 5%, 7.5%, and 10%. Neat material was also subjected to testing. Tribological, mechanical, and chemical properties of the mentioned materials were examined. Measurements were also made after keeping the samples in ageing and climatic ovens. Furthermore, SEM observations of samples before and after friction tests were carried out. It was demonstrated that increasing graphite content caused a significant decrease in wear (PLA + 10% graphite had a wear rate three times lower than for a neat material). The addition of graphite did not adversely affect most of the other properties, but it ought to be noted that mechanical properties changed significantly. After conditioning in a climatic oven PLA + 10% graphite has (in comparison with neat material) 11% lower fracture stress, 47% lower impact strength, and 21% higher Young’s modulus. It can be certainly stated that the addition of graphite to PLA is a step towards obtaining a material that is low-cost and suitable for printing sliding spare parts.
New composites containing a natural filler made of diatom shells (frustules), permitting the modification of polylactide matrix, were produced by Fused Deposition Modelling (3D printing) and were thoroughly examined. Two mesh fractions of the filler were used, one of <40 µm and the other of 40−63 µm, in order to check the effect of the filler particle size on the composite properties. The composites obtained contained diatom shells in the concentrations from 0% to 5% wt. (0−27.5% vol.) and were subjected to rheological analysis. The composites obtained as filaments of 1.75 mm in diameter were used for 3D printing. The printed samples were characterized as to hydrophilic–hydrophobic, thermal and mechanical properties. The functional parameters of the printed objects, e.g., mechanical characteristics, stability on contact with water and water contact angle, were measured. The results revealed differences in the processing behavior of the samples as well as the effect of secondary granulation of the filler on the parameters of the printing and mechanical properties of the composites.
The authors of this paper use an original method of diatomaceous earth fractionation, which allows for obtaining a filler with a specific particle size distribution. The method makes it possible to separate small, disintegrated and broken diatom frustules from those which maintained their original form in diatomaceous earth. The study covers a range of tests conducted to prove that such a separated diatomic fraction (3–30 µm) shows features different from the base diatomite (from 1 to above 40 µm) used as an epoxy resin filler. We have examined the mechanical properties of a series of diatomite/resin composites, considering the weight fraction of diatoms and the parameters of the composite production process. The studied composites of Epidian 601 epoxy resin cross-linked with amine-based curing agent Z-1 contained 0 to 70% vol. of diatoms or diatomaceous earth. Samples were produced by being casted into silicone molds in vacuum degassing conditions and, alternatively, without degassing. The results have shown that the size and morphology of the filler based on diatomaceous earth affects mechanical and rheological properties of systems based on epoxy resin. Elongation at rupture and flexural stress at rupture were both raised by up to 35%, and impact strength by up to 25%.
The fractionation of diatomaceous earth (DE) using sedimentation made it possible to obtain separate unbroken diatom fractions from broken or agglomerated bodies with a range of particle sizes. The produced filler was used to prepare polylactide (PLA)/diatomaceous earth biocomposite samples containing different particle sizes, which were subjected to mechanical testing (tensile strength, flexural strength, impact strength), colloidal testing (contact angle, color change test, SEM/EDS), and thermal testing (TGA, DSC, DMA). Modification of the PLA containing the smallest particle size with diatomaceous earth (Fraction 5) resulted in a higher impact strength compared to both the pure PLA and the PLA/DE composite that contained base diatomaceous earth. Furthermore, the melt flow rate was improved by more than 80 and 60% for the composite modified with fractionated diatomaceous earth (Fraction 4) compared to pure PLA and base diatomaceous earth, respectively. The elasticity of the composite was also improved from 3.3 GPa for pure polylactide to 4.4 GPa for the system containing the smallest diatomaceous earth particles (Fraction 5).
In this study, the influence of carbonate lake sediments (Polylactide/Carbonate Lake Sediments–PLA/CLS) on the mechanical and structural properties of polylactide matrix composites was investigated. Two fractions of sediments originating from 3–8 and 8–12 m were analysed for differences in particle size by distribution (Dynamic Light Scattering–DLS), phase composition (X-ray Diffraction–XRD), the presence of surface functional groups (Fourier Transform-Infrared–FT-IR), and thermal stability (Thermogravimetric Analysis–TGA). Microscopic observations of the composite fractures were also performed. The effect of the precipitate fraction on the mechanical properties of the composites before and after conditioning in the weathering chamber was verified through peel strength, flexural strength, and impact strength tests. A melt flow rate study was performed to evaluate the effect of sediment on the processing properties of the PLA/CLS composite. Hydrophobic-hydrophilic properties were also investigated, and fracture analysis was performed by optical and electron microscopy. The addition of carbon lake sediments to PLA allows for the obtention of composites resistant to environmental factors such as elevated temperature or humidity. Moreover, PLA/CLS composites show a higher flow rate and higher surface hydrophobicity in comparison with unmodified PLA.
In this work, silsesquioxane and spherosilicate compounds were assessed as novel organosilicon coupling agents for surface modification of TiO2 in a green process, and compared with their conventional silane counterparts. The surface-treated TiO2 particles were then applied in preparation of epoxy (EP) composites and the aspects of pigment dispersion, suspension stability, hiding power, as well as the composite mechanical and thermal properties were discussed. The studied compounds loading was between 0.005–0.015% (50–150 ppm) in respect to the bulk composite mass and resulted in increase of suspension stability and hiding power by over an order of magnitude. It was found that these compounds may be an effective alternative for silane coupling agents, yet due to their low cost and simplicity of production and manipulation, silanes and siloxanes are still the most straight-forward options available. Nonetheless, the obtained findings might encourage tuning of silsesquioxane compounds structure and probably process itself if implementation of these novel organosilicon compounds as surface treatment agents is sought for special applications, e.g., high performance coating systems.
Diatomaceous earth are sediments of unicellular algal skeletons with a well-defined hierarchical structure. Despite many tests conducted on systems using diatomaceous earth and epoxy resins, we can find many differences in the methods of acquisition and characteristics of the composite, which may considerably affect the results. In our study, we have conducted tests to verify the impact of the method of obtaining samples and the degassing of the composite on its mechanical properties and standard deviation. The samples were cast in glass moulds and silicone moulds and then subjected to testing for their mechanical and functional properties, imaging with the use of an optical microscope and a scanning electron microscope. The tests have shown that, for samples cast in glass moulds, there is no heterogeneity within the area of the tested sample, as in the case of samples cast in silicone moulds. Silicone moulds allow for quite effective self-degassing of the resin due to the large area-to-mass ratio, and the small remaining air vesicles have a limited effect on the mechanical properties of the samples. The filler used also played a significant role. For systems containing base and rinsed diatomite, it is clear that the degassing of mixtures increases the tensile strength. For treated diatomite, the elongation at break grew along with increasing filler concentration, while for base diatomite, the improvement was observed for flexural strength and impact strength. A non-modified epoxy resin shows a tensile strength at 19.91 MPa (silicone mould cast). At the same time, the degassed, glass mould-cast systems containing 12% of base and rinsed diatoms showed a tensile strength of 27.4 MPa and 44.7 MPa, respectively. We have also observed that the higher the filler concentration, the higher were the tensile strength values, which for the rinsed diatoms reached over 55.1 MPa and for the base diatoms were maximum of 43.8 MPa. The tests, therefore, constitute a set of guidelines and recommendations for testing with the use of fillers showing an extended inner structure.
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