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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.
- 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.
- 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.
- ItemPolymer - Carbon nanotube composites for thermoelectric applications(Melville, NY : AIP, 2017) Luo, J.; Krause, Beate; Pötschke, PetraThe thermoelectric (TE) performance of electrically conductive thermoplastic composites prepared by melt mixing was investigated. A cost effective widely used in industry polymer, namely polypropylene (PP), was chosen as the matrix to fabricate the composites. Singlewalled carbon nanotubes (SWCNTs), the amount (2 wt%) of which was selected to be above the electrical percolation threshold (< 0.2 wt%), were used to form an electrical conducting network. Besides as-produced SWCNTs plasma modified tubes were employed to study the influence of the functionalization on the morphology, dispersion and TE properties of the PP composites. In addition, melt processing conditions, e.g. temperature, rotation speed, and time during mixing in a small-scale compounder were varied. Furthermore, an ionic liquid (IL, 1-methyl-3-octylimidazolium tetrafluoroborate) was used as a processing additive during melt mixing, which was confirmed to improve the electrical conductivity of the composites. Simultaneous increase in the Seebeck coefficient up to a value of 64 μV/K was recorded, leading to a much better power factor of 0.26 μW/(m·K2) compared to composites without IL. This melt mixing strategy opens new avenues for solvent-free, large scale fabrication of polymer based TE materials.
- ItemEffects of high energy electrons on the properties of polyethylene / multiwalled carbon nanotubes composites: Comparison of as-grown and oxygen-functionalised MWCNT(Melville, NY : AIP, 2014) Krause, Beate; Pötschke, Petra; Gohs, U.Polymer modification with high energy electrons (EB) is well established in different applications for many years. It is used for crosslinking, curing, degrading, grafting of polymeric materials and polymerisation of monomers. In contrast to this traditional method, electron induced reactive processing (EIReP) combines the polymer modification with high energy electrons and the melt mixing process. This novel reactive method was used to prepare polymer blends and composites. In this study, both methods were used for the preparation of polyethylene (PE)/ multiwalled carbon nanotubes (MWCNT) composites in the presence of a coupling agent. The influence of MWCNT and type of electron treatment on the gel content, the thermal conductivity, rheological, and electrical properties was investigated whereby as-grown and oxidised MWCNT were used. In the presence of a coupling agent and at an absorbed dose of 40 kGy, the gel content increased from 57 % for the pure PE to 74 % or 88 % by the addition of as-grown (Baytubes® C150P) or oxidised MWCNT, respectively. In comparison to the composites containing the as-grown MWCNTs, the use of the oxidised MWCNTs led to higher melt viscosity and higher storage modulus due to higher yield of filler polymer couplings. The melt viscosity increased due to the addition of MWCNT and crosslinking of PE. The thermal conductivity increased to about 150 % and showed no dependence on the kind of MWCNT and the type of electron treatment. In contrast, the lowest value of electrical volume resistivity was found for the non-irradiated samples and after state of the art electron treatment without any influence of the type of MWCNT. In the case of EIReP, the volume resistivity increased by 2 (as-grown MWCNT) or 3 decades (oxidised MWCNT) depending on the process parameters. © 2014 American Institute of Physics.
- ItemImpact of synthesis temperature on structure of carbon nanotubes and morphological and electrical characterization of their polymeric nanocomposites(Melville, NY : AIP, 2017) Arjmand, Mohammad; Mirkhani, Seyyed Alireza; Pötschke, Petra; Krause, Beate; Sundararaj, UttandaramanCarbon nanotubes (CNTs) were synthesized by chemical vapor deposition technique at a broad range of temperatures, i.e. 550°C to 950°C (at 100°C intervals). CNTs were synthesized by flowing source and carrier gases (ethane, argon, and hydrogen) over Fe catalyst in a quartz tubular reactor. CNTs were melt mixed with a polyvinylidene fluoride (PVDF) matrix in a miniature mixer. The resulting nanocomposites were then compression molded, and electrically and morphologically characterized. Moreover, a wide range of characterization techniques were employed to obtain detailed information about the physical and morphological characteristics of CNTs. It was surprisingly observed that, despite the ascending trend of powder conductivity with the synthesis temperature, the nanocomposites made with (CNT)650°C had significantly lower percolation threshold (around 0.4wt.%) and higher electromagnetic interference shielding (20.3dB over the X-band for 1.1mm thickness) compared to the other temperatures. The characterization of nanofillers showed that the synthesis yield and quality of (CNT)650°C were highly superior to the other types of CNTs. At 850°C and 950°C, most of the synthesized carbonaceous materials formed graphitic structures around the sintered catalyst particles. It was also observed that the dispersion state of (CNT)650°C within the PVDF matrix was much better than that of CNTs synthesized at the other temperatures. Superior electrical properties of (CNT)650°C nanocomposites can be attributed to a combination of high synthesis yield, low diameter and decent quality of CNTs coupled with good state of dispersion within the PVDF matrix.