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- ItemThe Localization Behavior of Different CNTs in PC/SAN Blends Containing a Reactive Component(Basel : MDPI, 2021-3-1) Gültner, Marén; Boldt, Regine; Formanek, Petr; Fischer, Dieter; Simon, Frank; Pötschke, PetraCo-continuous blend systems of polycarbonate (PC), poly(styrene-co-acrylonitrile) (SAN), commercial non-functionalized multi-walled carbon nanotubes (MWCNTs) or various types of commercial and laboratory functionalized single-walled carbon nanotubes (SWCNTs), and a reactive component (RC, N-phenylmaleimide styrene maleic anhydride copolymer) were melt compounded in one step in a microcompounder. The blend system is immiscible, while the RC is miscible with SAN and contains maleic anhydride groups that have the potential to reactively couple with functional groups on the surface of the nanotubes. The influence of the RC on the localization of MWCNTs and SWCNTs (0.5 wt.%) was investigated by transmission electron microscopy (TEM) and energy-filtered TEM. In PC/SAN blends without RC, MWCNTs are localized in the PC component. In contrast, in PC/SAN-RC, the MWCNTs localize in the SAN-RC component, depending on the RC concentration. By adjusting the MWCNT/RC ratio, the localization of the MWCNTs can be tuned. The SWCNTs behave differently compared to the MWCNTs in PC/SAN-RC blends and their localization occurs either only in the PC or in both blend components, depending on the type of the SWCNTs. CNT defect concentration and surface functionalities seem to be responsible for the localization differences.
- ItemBlending In Situ Polyurethane-Urea with Different Kinds of Rubber: Performance and Compatibility Aspects(Basel : MDPI, 2018-11-02) Tahir, Muhammad; Heinrich, Gert; Mahmood, Nasir; Boldt, Regine; Wießner, Sven; Stöckelhuber, Klaus WernerSpecific physical and reactive compatibilization strategies are applied to enhance the interfacial adhesion and mechanical properties of heterogeneous polymer blends. Another pertinent challenge is the need of energy-intensive blending methods to blend high-tech polymers such as the blending of a pre-made hard polyurethane (-urea) with rubbers. We developed and investigated a reactive blending method to prepare the outstanding blends based on polyurethane-urea and rubbers at a low blending temperature and without any interfacial compatibilizing agent. In this study, the polyurethane-urea (PUU) was synthesized via the methylene diphenyl diisocyanate end-capped prepolymer and m-phenylene diamine based precursor route during blending at 100 °C with polar (carboxylated nitrile rubber (XNBR) and chloroprene rubber (CR)) and non-polar (natural rubber (NR), styrene butadiene rubber (sSBR), and ethylene propylene butadiene rubber (EPDM)) rubbers. We found that the in situ PUU reinforces the tensile response at low strain region and the dynamic-mechanical response up to 150 °C in the case of all used rubbers. Scanning electron microscopy reveals a stronger rubber/PUU interface, which promotes an effective stress transfer between the blend phases. Furthermore, energy filtered transmission electron microscopy (EFTEM) based elemental carbon map identifies an interphase region along the interface between the nitrile rubber and in situ PUU phases of this exemplary blend type.
- ItemA new strategy to improve viscoelasticity, crystallization and mechanical properties of polylactide(Amsterdam [u.a.] : Elsevier Science, 2021) Huang, Ying; Müller, Michael Thomas; Boldt, Regine; Zschech, Carsten; Gohs, Uwe; Wießner, SvenBiodegradable polylactide/masticated natural rubber (PLA/mNR) blends were prepared by electron induced reactive processing (EIReP) without using any chemical additives. The PLA/mNR blends showed droplet-matrix morphology with decreased mNR particle size after EIReP treatment. The absolute value of complex viscosity and storage modulus increased significantly for the EIReP modified blends, suggesting the improved melt strength and elasticity. The crystallization investigation showed that the cold crystallization peak of PLA phase gradually disappeared after EIReP modification. Instead, the crystallization peak arose during melt cooling process. Consequently, the crystallinity of PLA phase increased from 6.2% to 39.0% as the mNR content increased from 0 to 20 wt%. It was found that the softening temperature of PLA examined by dynamic mechanical analysis increased effectively with the characters of higher modulus compared to the non-modified blends. The EIReP modified blends exhibited excellent mechanical properties with 7-fold increase of impact toughness compared with neat PLA, implying a superior interfacial adhesion and chain interactions between the two polymer phases. Furthermore, the thermogravimetric analysis demonstrated that the thermal stability was slightly enhanced for the EIReP modified blends.
- ItemComparison of transition metal (Fe, Co, Ni, Cu, and Zn) containing tri-metal layered double hydroxides (LDHs) prepared by urea hydrolysis(Cambridge : RSC, 2019) Naseem, Sajid; Gevers, Bianca; Boldt, Regine; Labuschagné, Frederick J. W. J.; Leuteritz, AndreasThis paper details a successful synthesis and comparison of a range of tri-metal hydrotalcite-like layered double hydroxides (LDHs) using urea hydrolysis. Transition-metal-substituted MgMAl-LDHs were synthesized with M = Fe, Co, Ni, Cu or Zn. 5 mol% and 10 mol% substitutions were performed, where Mg was substituted with Co, Ni, Cu and Zn, and Al with Fe. The successful synthesis of crystalline MgMAl-LDHs was confirmed using X-ray powder diffraction (XRD) analysis. Energy-dispersive X-ray (EDX) spectroscopy was used to identify substituted metals and determine changes in composition. Changes in morphology were studied using scanning electron microscopy (SEM). Thermogravimetric analysis was used to determine the effect of Fe-, Co-, Ni-, Cu- or Zn-substitution on the thermal degradation of the MgMAl-LDH phase. The structure, morphology and thermal behavior of the LDHs were shown to be influenced by the substituted transition metals. The observed thermal stability took the order MgNiAl- > MgFeAl- = MgAl- ≥ MgCoAl- > MgCuAl- > MgZnAl-LDH. The urea hydrolysis method was shown to be a simple preparation method for well-defined crystallite structures with large hexagonal platelets and good distribution of transition metal atoms in the substituted LDHs. © 2019 The Royal Society of Chemistry.
- ItemComplex calcium carbonate/polymer microparticles as carriers for aminoglycoside antibiotics(London : RSC Publishing, 2018) Racovita, Stefania; Vasiliu, Ana-Lavinia; Bele, Adrian; Schwarz, Dana; Steinbach, Christine; Boldt, Regine; Schwarz, Simona; Mihai, MarcelaComposite microparticles of CaCO3 and two pectin samples (which differ by the functional group ratio) or corresponding nonstoichiometric polyelectrolyte complexes with different molar ratios (0.5, 0.9 and 1.2) are obtained, characterized and tested for loading and release of streptomycin and kanamycin sulphate. The synthesized carriers were characterized before and after drug loading in terms of morphology (by SEM using secondary electron and energy selective backscattered electron detectors), porosity (by water sorption isotherms) and elemental composition (by elemental mapping using energy dispersive X-ray and FTIR spectroscopy). The kinetics of the release mechanism from the microparticles was investigated using Higuchi and Korsmeyer-Peppas mathematical models.
- ItemShear-induced crystallization of polyamide 11(Berlin ; Heidelberg ; New York : Springer, 2021) Jariyavidyanont, Katalee; Mallardo, Salvatore; Cerruti, Pierfrancesco; Di Lorenzo, Maria Laura; Boldt, Regine; Rhoades, Alicyn M.; Androsch, RenéShear-induced formation of crystal nuclei in polyamide 11 (PA 11) was studied using a conventional parallel-plate rheometer. Crystallization of PA 11 after shearing the melt at different rates for 60 s was followed by the evolution of the complex viscosity. The sheared samples showed in an optical microscope a gradient structure along the radius, due to the increasing shear rate from the center to the edge. The critical shear rate for shear-induced formation of nuclei was identified at the position where a distinct change of the semicrystalline superstructure is observed, being at around 1 to 2 s−1. Below this threshold, a space-filled spherulitic superstructure developed as in quiescent-melt crystallization. Above this value, after shearing at rates between 1 and 5 s−1, an increased number of point-like nuclei was detected, connected with formation of randomly oriented crystals. Shearing the melt at even higher rates led to a further increase of the nuclei number and growth of crystals oriented such that the chain axis is in parallel to the direction of flow. In addition, optical microscopy confirmed formation of long fibrillar structures after shearing at such condition. The critical specific work of flow of PA 11 was calculated to allow a comparison with that of polyamide 66 (PA 66). This comparison showed that in the case of PA 11 more work for shear-induced formation of nuclei is needed than in the case of PA 66, discussed in terms of the chemical structure of the repeat unit in the chains.
- ItemThe influence of matrix viscosity on MWCNT dispersion and electrical properties in different thermoplastic nanocomposites(Oxford : Elsevier Science, 2012) Socher, Robert; Krause, Beate; Müller, Michael T.; Boldt, Regine; Pötschke, PetraComposites of MWCNTs having each three different levels of matrix viscosity with five different polymers (polyamide 12, polybutylene terephthalate, polycarbonate, polyetheretherketone and low density polyethylene) were melt mixed to identify the general influence of matrix viscosity on the electrical properties and the state of MWCNT dispersion. Huge differences in the electrical percolation thresholds were found using the same polymer matrix with different viscosity grades. The lowest percolation thresholds were always found in the composites based on the low viscosity matrix. The state of primary MWCNT agglomerate dispersion increased with increasing matrix viscosity due to the higher input of mixing energy. TEM investigations showed nanoagglomerated structures in the low viscosity samples which are obviously needed to achieve low resistivity values. The effect of nanotube shortening was quantified using two different viscosity grades of polycarbonate. Due to the higher mixing energy input the nanotube shortening was more pronounced in the high viscosity matrix which partially explains the higher percolation threshold. © 2011 Elsevier Ltd. All rights reserved.
- ItemEffect of Molar Mass on Critical Specific Work of Flow for Shear-Induced Crystal Nucleation in Poly (l-Lactic Acid)(Basel : MDPI, 2021) Du, Mengxue; Jariyavidyanont, Katalee; Kühnert, Ines; Boldt, Regine; Androsch, RenéThe concept of specific work of flow has been applied for the analysis of critical shearing conditions for the formation of crystal nuclei in poly (l-lactic acid) (PLLA). Systematic variation in both time and rate of shearing the melt in a parallel-plate rheometer revealed that these parameters are interconvertible regarding the shear-induced formation of crystal nuclei; that is, low shear rate can be compensated for by increasing the shear time and vice versa. This result supports the view that critical shearing conditions can be expressed by a single quantity, providing additional options for tailoring polymer processing routes when enhanced nuclei formation is desired/unwanted. Analysis of PLLA of different mass-average molar masses of 70, 90, 120, and 576 kDa confirmed improved shear-induced crystal nucleation for materials of higher molar mass, with critical specific works of flow, above which shear-induced nuclei formation occurs, of 550, 60, 25, and 5 kPa, respectively.
- ItemCorrelation between Processing Parameters, Morphology, and Properties of Injection-Molded Polylactid Acid (PLA) Specimens at Different Length Scales(Basel : MDPI, 2023) Meinig, Laura; Boldt, Regine; Spoerer, Yvonne; Kuehnert, Ines; Stommel, MarkusPolylactic acid (PLA) is one of the most promising bioplastic representatives that finds application in many different areas, e.g., as single-use products in the packaging industry, in the form of mulch film for agriculture, or in medical devices. For the development of new areas, especially in terms of long-term applications and the production of recyclable products, the material properties controlled by processing must be known. The state of the art is investigations at the global scale (integral values) without consideration of local structure inhomogeneities and their influence on the material properties. In this work, morphological, thermal, and mechanical properties of injection-molded PLA tensile bars are investigated at different length scales (global and local) as a function of processing parameters. In addition to the processing parameters, such as melt temperature, mold temperature, and cooling time in the mold, the influence of the D-isomer content on the crystallization behavior and the resulting material properties are investigated. The material was found to form crystalline structures only when cooled in a mold tempered above Tg. In addition, PLA with a lower content of D-isomer was found to have a higher degree of crystallinity. Since the mechanical properties obtained by tensile tests could not be correlated with the degree of crystallinity, detailed analysis were performed showing a characteristic inhomogeneous morphology within the tensile bars. By means of micromechanical investigations on samples with different microstructure ranges, the relationship between local morphology and failure behavior could be explained.
- ItemSolubility and selectivity effects of the anion on the adsorption of different heavy metal ions onto chitosan(Basel : MDPI, 2020) Weißpflog, Janek; Gündel, Alexander; Vehlow, David; Steinbach, Christine; Müller, Martin; Boldt, Regine; Schwarz, Simona; Schwarz, DanaThe biopolymer chitosan is a very efficient adsorber material for the removal of heavy metal ions from aqueous solutions. Due to the solubility properties of chitosan it can be used as both a liquid adsorber and a solid flocculant for water treatment reaching outstanding adsorption capacities for a number of heavy metal ions. However, the type of anion corresponding to the investigated heavy metal ions has a strong influence on the adsorption capacity and sorption mechanism on chitosan. In this work, the adsorption capacity of the heavy metal ions manganese, iron, cobalt, nickel, copper, and zinc were investigated in dependence on their corresponding anions sulfate, chloride, and nitrate by batch experiments. The selectivity of the different heavy metal ions was analyzed by column experiments. © 2020 by the authors.