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- ItemEffect of additives on MWCNT dispersion and electrical percolation in polyamide 12 composites(Melville, NY : AIP, 2017) Socher, Robert; Krause, Beate; Pötschke, PetraThe aim of this study was to decrease the electrical percolation threshold of multiwalled carbon nanotubes (MWCNTs) in a polyamide 12 matrix by the use of additives. Different kinds of additives were selected which either interact with the π-system of the MWCNTs (imidazolium based ionic liquid (IL) and perylene-3,4,9,10-tetracarboxylic dianhydride (PTCDA)) or improve the MWCNT wettability (cyclic butylene terephthalate, CBT). The composites were melt mixed using a DACA microcompounder. The electrical percolation threshold for PA12/MWCNT without additives, measured on compression molded plates, was found between 2.0 and 2.25 wt%. With all used additives, a significant reduction of the electrical percolation threshold could be achieved. Whereas the addition of IL and CBT resulted in MWCNT percolation at around 1.0 wt%, a slightly higher percolation threshold between 1.0 and 1.5 wt% was found for PTCDA as an additive. Interestingly, the electrical resistivity at higher loadings was decreased by nearly two decades when using CBT and one decade after application of PTCDA, whereas IL did not contribute to lower values in this range. In all cases macrodispersion as assessed by light microscopy was not improved and even worse as compared to non-modified composites. In summary, the results illustrate that these kinds of additives are able to improve the performance of PA12 based MWCNT nanocomposites.
- ItemSurface cleaning and sample carrier for complementary high-resolution imaging techniques(Melville, NY : AIP, 2020) Benettoni, Pietro; Ye, Jia-Yu; Holbrook, Timothy R.; Calabrese, Federica; Wagner, Stephan; Zarejousheghani, Mashaalah; Griebe, Jan; Ullrich, Maria K.; Musat, Niculina; Schmidt, Matthias; Flyunt, Roman; Reemtsma, Thorsten; Richnow, Hans-Hermann; Stryhanyuk, HryhoriyNowadays, high-resolution imaging techniques are extensively applied in a complementary way to gain insights into complex phenomena. For a truly complementary analytical approach, a common sample carrier is required that is suitable for the different preparation methods necessary for each analytical technique. This sample carrier should be capable of accommodating diverse analytes and maintaining their pristine composition and arrangement during deposition and preparation. In this work, a new type of sample carrier consisting of a silicon wafer with a hydrophilic polymer coating was developed. The robustness of the polymer coating toward solvents was strengthened by cross-linking and stoving. Furthermore, a new method of UV-ozone cleaning was developed that enhances the adhesion of the polymer coating to the wafer and ensures reproducible surface-properties of the resulting sample carrier. The hydrophilicity of the sample carrier was recovered applying the new method of UV-ozone cleaning, while avoiding UV-induced damages to the polymer. Noncontact 3D optical profilometry and contact angle measurements were used to monitor the hydrophilicity of the coating. The hydrophilicity of the polymer coating ensures its spongelike behavior so that upon the deposition of an analyte suspension, the solvent and solutes are separated from the analyte by absorption into the polymer. This feature is essential to limit the coffee-ring effect and preserve the native identity of an analyte upon deposition. The suitability of the sample carrier for various sample types was tested using nanoparticles from suspension, bacterial cells, and tissue sections. To assess the homogeneity of the analyte distribution and preservation of sample integrity, optical and scanning electron microscopy, helium ion microscopy, laser ablation inductively coupled plasma mass spectrometry, and time-of-flight secondary ion mass spectrometry were used. This demonstrates the broad applicability of the newly developed sample carrier and its value for complementary imaging. © 2020 Author(s).
- ItemMelt mixed composites of polypropylene with singlewalled carbon nanotubes for thermoelectric applications: Switching from p- to n-type behavior by additive addition(Melville, NY : AIP, 2019) Pötschke; Petra; Krause, Beate; Luo, JinjiComposites were prepared with polypropylene (PP) as the matrix and singlewalled CNTs (SWCNTs) of the type TUBALL from OCSiAl Ltd. as the conducting component by melt processing in a small-scale twin-screw compounder. In order to switch the typical p-type behavior of such composites from positive Seebeck coefficients (S) into n-type behavior with negative Seebeck coefficients, a non-ionic surfactant polyoxyethylene 20 cetyl ether (Brij58) was used and compared with a PEG additive, which was shown previously to be able to induce such switching. For PP-2 wt% SWCNT composites Brij58 is shown to result in n-type composites. The negative S values (up to −48.2 µV/K) are not as high as in the case of previous results using PEG (−56.6 µV/K). However, due to the more pronounced effect of Brij58 on the electrical conductivity, the achieved power factors are higher and reach a maximum of 0.144 µW/(m·K2) compared to previous 0.078 µW/(m·K2) with PEG. Dispersion improvement depends on the type of SWCNTs obtained by using varied synthesis/treatment conditions. Solution prepared composites of PEG with SWCNTs also have negative S values, indicating the donation of electrons from PEG to the SWCNTs. However, such composites are brittle and not suitable as thermoelectric materials.
- ItemDevelopment of joining methods for highly filled Graphite/PP composite based bipolar plates for fuel cells: Adhesive joining and welding(Melville, NY : AIP, 2019) Rzeczkowski, P.; Lucia, M.; Müller, A.; Facklam, M.; Cohnen, A.; Schäfer, P.; Hopmann, C.; Hickmann, T.; Pötschke, Petra; Krause, BeateNovel material solutions for bipolar plates in fuel cells require adapted ways of joining and sealing technologies. Safe and life time enduring leak-tight contacts must be achieved by automatic processes using reasonable joint forces. A proper sealing should manage such challenges as good ageing properties, excellent leaktightness, high thermal conductivity and low gas permeability. Hence in this work, adhesive bonding and welding are considered as suitable methods, which can fulfill the requirements mentioned above. Adhesive systems seem to be more easy to apply than conventional sealing (hand layed-up rubber gaskets), e.g. with automatic dispensers. Additionally, the properties of an adhesive joint can be enhanced by a process-specific surface pre-treatment. This work focuses on the characterization of adhesive systems and their joints with highly filled graphite composites. Mechanical properties of the joints were characterized through lap-shear tests. The influence of ageing caused by humidity or acidic solvent at increased temperature on the bond line properties as well as neat adhesive was examined. The thermal conductivities of neat adhesives and through the entire joint were examined. In order to improve above conductivities, roughening, substrate pre-heating, post-curing and various contact pressure weights were applied. Plasma treatment was chosen as surface pre-treatment method for improving substrate's surface energy. An alternative to bonding is plastic welding, which does not require the use of sealants and adhesives. Based on former study of influences of filler content on the welding process using ultrasonic, hot plate or infrared welding, a welding method for joining the graphite compounds was derived.
- ItemInfluence of graphite and SEBS addition on thermal and electrical conductivity and mechanical properties of polypropylene composites(Melville, NY : AIP, 2017) Krause, Beate; Cohnen, A.; Pötschke, Petra; Hickmann, T.; Koppler, D.; Proksch, B.; Kersting, T.; Hopmann, C.In this study, composites based on polypropylene (PP) and different graphite fillers were melt mixed using small scale microcompounder Xplore DSM15 as well as lab-scale co-rotating twin screw extruder Coperion ZSK26Mc. The measurements of the electrical and thermal conductivity as well as mechanical properties of the composites were performed on pressed plates. It was found that the addition of graphite powders having different particle size distributions leads to different increases of the thermal conductivity. For synthetic graphite, the PP composites filled with TIMCAL Timrex® KS500 reached the highest value of thermal conductivity of 0.52 W/(m·K) at 10 vol% loading, whereas this composite was not electrical conductive. Furthermore, the influence of a styrene-ethylene-butylene-styrene block copolymer (SEBS) based impact modifier on the mechanical properties of PP filled with 80 wt% of different synthetic graphites was investigated. For that the proportion of SEBS in the PP component was varied systematically. The conductivities were influenced by the type of graphite and the content of impact modifier. The results indicate that the impact strength of the composite containing TIMCAL Timrex® KS300-1250 can be increased by approx. 100 % when replacing 50 wt% of the PP component by SEBS.
- ItemElectrical and thermal conductivity of polypropylene filled with combinations of carbon fillers(Melville, NY : AIP, 2016) Krause, Beate; Pötschke, PetraThe thermal and electrical conductivity of polymer composites filled with a low content up to 7.5 vol% of different carbon fillers (carbon nanotubes, carbon fibers, graphite nanoplates) were investigated. It was found that the combination of two or three carbon fillers leads to an increase of thermal conductivity up to 193% which is higher than the sum of the effects of both fillers.
- ItemEpitaxial synthesis of unintentionally doped p-type SnO (001) via suboxide molecular beam epitaxy(Melville, NY : AIP, 2023) Egbo, Kingsley; Luna, Esperanza; Lähnemann, Jonas; Hoffmann, Georg; Trampert, Achim; Grümbel, Jona; Kluth, Elias; Feneberg, Martin; Goldhahn, Rüdiger; Bierwagen, OliverBy employing a mixed SnO2 + Sn source, we demonstrate suboxide molecular beam epitaxy (S-MBE) growth of phase-pure single-crystalline metastable SnO (001) thin films on Y-stabilized ZrO2 (001) substrates at a growth rate of ∼1.0 nm/min without the need for additional oxygen. These films grow epitaxially across a wide substrate temperature range from 150 to 450 °C. Hence, we present an alternative pathway to overcome the limitations of high Sn or SnO2 cell temperatures and narrow growth windows encountered in previous MBE growth of metastable SnO. In situ laser reflectometry and line-of-sight quadrupole mass spectrometry were used to investigate the rate of SnO desorption as a function of substrate temperature. While SnO ad-molecule desorption at TS = 450 °C was growth-rate limiting, the SnO films did not desorb at this temperature after growth in vacuum. The SnO (001) thin films are transparent and unintentionally p-type doped, with hole concentrations and mobilities in the range of 0.9-6.0 × 1018 cm-3 and 2.0-5.5 cm2 V-1 s-1, respectively. These p-type SnO films obtained at low substrate temperatures are promising for back-end-of-line (BEOL) compatible applications and for integration with n-type oxides in pn heterojunctions and field-effect transistors.
- ItemPP/SWCNT composites modified with ionic liquid(Melville, NY : AIP, 2017) Krause, Beate; Predtechenskiy, M.; Ilin, E.; Pötschke, PetraPolypropylene composites filled with singlewalled carbon nanotubes TUBALL® (SWCNTs) were studied with regard to the effect of ionic liquid (IL) addition in different SWCNT:IL ratios (1:0.5 - 1:6). The incorporation of IL leads to a decrease of the electrical percolation threshold and already at 0.025 wt% SWCNT loading reduced resistivity values can be observed. However, the SWCNT macro dispersion, already relatively good without IL, was not affected by the IL incorporation. In addition, the nucleation effect of the SWCNT in polypropylene is not influenced when simultaneously adding IL, whereas the crystallization enthalpy slightly decreases with its addition.
- ItemInfluence of mixing conditions on carbon nanotube shortening and curling in polycarbonate composites(Melville, NY : AIP, 2017) Krause, Beate; Carval, J.; Pötschke, PetraPolycarbonate composites containing multiwalled carbon nanotubes (MWCNTs, 0.2-2.0 wt%) were melt mixed in small scale at different conditions of screw speed and mixing time to vary the specific mechanical energy (SME) input between 0.4 and 4.0 kWh/kg. Next to the electrical properties of compression molded plates and the MWCNT macrodispersion also the nanotube length and shape were analyzed. For this, the matrix of the composites with 0.75 wt% MWCNT loading was dissolved and the remaining nanotubes were investigated using TEM. It was found that with increasing SME input the number of remaining CNT agglomerates decreases. The MWCNT length decreased from initially about 1.4 micrometers towards 350 nanometers at a SME of 4 kWh/kg and the mean curling values were also reduced. The electrical percolation threshold increases with SME from about 0.4 wt% to 0.6 wt%.
- ItemDevelopment of a polymer composite with high electrical conductivity and improved impact strength for the application as bipolar plate(Melville, NY : AIP, 2016) Hopmann, C.; Windeck, C.; Cohnen, A.; Onken, J.; Krause, Beate; Pötschke, Petra; Hickmann, T.Bipolar plates constitute the most important structural component in fuel cell stacks. Highly filled thermoplastic composites with high electrical conductivity obtain an increasing importance in the design of bipolar plates as alternative to conventional metallic systems. Thermoplastics (e.g. PP) have suitable properties such as a good processability, chemical resistance, light weight and low production costs. As thermoplastics have low electrical conductivities, conductive fillers have to be included in the matrix. A high content of such fillers (e.g. graphite) in excess of 80 wt.-% is necessary to achieve the desired electrical properties. However, materials with such high filler contents embrittle readily. The workability in injection and compression molding is difficult and the mechanical stability is insufficient in case of strain deformation. As consequence, material failure and an inacceptable amount of damaged goods can be observed during the processing. As no suitable thermoplastic system is available for better mechanical properties, the induction and dispersion of a rubber phase in the thermoplastic matrix can be used to increase the impact strength of the conductive composite. In this research work a ternary composite, based on PP as matrix, EPDM as impact modifier and synthetic graphite as conductive filler, was developed. The material was produced using a 26 mm co-rotating, intermeshing twin-screw extruder. The amounts of PP, EPDM and graphite were varied systematically and a process window was defined that enables improved impact strength and high electrical conductivity of the new material. The results indicate that impact strength can be enhanced by about 99 % with an EPDM content of 30 wt.-% in the PP matrix. The electrical conductivity decreases in a small range with increasing content of EPDM, but the conductivity is still excellent for producing bipolar plates.