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- ItemMonitoring the thermally induced transition from sp3-hybridized into sp2-hybridized carbons(Amsterdam [u.a.] : Elsevier Science, 2021) Schüpfer, Dominique B.; Badaczewski, Felix; Peilstöcker, Jan; Guerra-Castro, Juan Manuel; Shim, Hwirim; Firoozabadi, Saleh; Beyer, Andreas; Volz, Kerstin; Presser, Volker; Heiliger, Christian; Smarsly, Bernd; Klar, Peter J.The preparation of carbons for technical applications is typically based on a treatment of a precursor, which is transformed into the carbon phase with the desired structural properties. During such treatment the material passes through several different structural stages, for example, starting from precursor molecules via an amorphous phase into crystalline-like phases. While the structure of non-graphitic and graphitic carbon has been well studied, the transformation stages from molecular to amorphous and non-graphitic carbon are still not fully understood. Disordered carbon often contains a mixture of sp3-, sp2-and sp1-hybridized bonds, whose analysis is difficult to interpret. We systematically address this issue by studying the transformation of purely sp3-hybridized carbons, that is, nanodiamond and adamantane, into sp2-hybridized non-graphitic and graphitic carbon. The precursor materials are thermally treated at different temperatures and the transformation stages are monitored. We employ Raman spectroscopy, WAXS and TEM to characterize the structural changes. We correlate the intensities and positions of the Raman bands with the lateral crystallite size La estimated by WAXS analysis. The behavior of the D and G Raman bands characteristic for sp2-type material formed by transforming the sp3-hybridized precursors into non-graphitic and graphitic carbon agrees well with that observed using sp2-structured precursors.
- ItemEffect of pore geometry on ultra-densified hydrogen in microporous carbons(Amsterdam [u.a.] : Elsevier Science, 2021) Tian, Mi; Lennox, Matthew J.; O’Malley, Alexander J.; Porter, Alexander J.; Krüner, Benjamin; Rudić, Svemir; Mays, Timothy J.; Düren, Tina; Presser, Volker; Terry, Lui R.; Rols, Stephane; Fang, Yanan; Dong, Zhili; Rochat, Sebastien; Ting, Valeska P.Our investigations into molecular hydrogen (H2) confined in microporous carbons with different pore geometries at 77 K have provided detailed information on effects of pore shape on densification of confined H2 at pressures up to 15 MPa. We selected three materials: a disordered, phenolic resin-based activated carbon, a graphitic carbon with slit-shaped pores (titanium carbide-derived carbon), and single-walled carbon nanotubes, all with comparable pore sizes of <1 nm. We show via a combination of in situ inelastic neutron scattering studies, high-pressure H2 adsorption measurements, and molecular modelling that both slit-shaped and cylindrical pores with a diameter of ∼0.7 nm lead to significant H2 densification compared to bulk hydrogen under the same conditions, with only subtle differences in hydrogen packing (and hence density) due to geometric constraints. While pore geometry may play some part in influencing the diffusion kinetics and packing arrangement of hydrogen molecules in pores, pore size remains the critical factor determining hydrogen storage capacities. This confirmation of the effects of pore geometry and pore size on the confinement of molecules is essential in understanding and guiding the development and scale-up of porous adsorbents that are tailored for maximising H2 storage capacities, in particular for sustainable energy applications.
- ItemResolving mobility anisotropy in quasi-free-standing epitaxial graphene by terahertz optical Hall effect(Amsterdam [u.a.] : Elsevier Science, 2021) Armakavicius, Nerijus; Kühne, Philipp; Eriksson, Jens; Bouhafs, Chamseddine; Stanishev, Vallery; Ivanov, Ivan G.; Yakimova, Rositsa; Zakharov, Alexei A.; Al-Temimy, Ameer; Coletti, Camilla; Schubert, Mathias; Darakchieva, VanyaIn this work, we demonstrate the application of terahertz-optical Hall effect (THz-OHE) to determine directionally dependent free charge carrier properties of ambient-doped monolayer and quasi-free-standing-bilayer epitaxial graphene on 4H–SiC(0001). Directionally independent free hole mobility parameters are found for the monolayer graphene. In contrast, anisotropic hole mobility parameters with a lower mobility in direction perpendicular to the SiC surface steps and higher along the steps in quasi-free-standing-bilayer graphene are determined for the first time. A combination of THz-OHE, nanoscale microscopy and optical spectroscopy techniques are used to investigate the origin of the anisotropy. Different defect densities and different number of graphene layers on the step edges and terraces are ruled out as possible causes. Scattering mechanisms related to doping variations at the step edges and terraces as a result of different interaction with the substrate and environment are discussed and also excluded. It is suggested that the step edges introduce intrinsic scattering in quasi-free-standing-bilayer graphene, that is manifested as a result of the higher ratio between mean free path and average terrace width parameters. The suggested scenario allows to reconcile existing differences in the literature regarding the anisotropic electrical transport in epitaxial graphene. © 2020 Elsevier Ltd
- ItemFrom microfluidics to hierarchical hydrogel materials(Amsterdam [u.a.] : Elsevier Science, 2023) Weigel, Niclas; Li, Yue; Fery, Andreas; Thiele, JulianOver the past two decades, microfluidics has made significant contributions to material and life sciences, particularly via the design of nano-, micro- and mesoscale materials such as nanoparticles, micelles, vesicles, emulsion droplets, and microgels. Unmatched in control over a multitude of material parameters, microfluidics has also shed light on fundamental aspects of material design such as the early stages of nucleation and growth processes as well as structure evolution. Exemplarily, polymer hydrogel particles can be formed via microfluidics with exact control over size, shape, functionalization, compartmentalization, and mechanics that is hardly found in any other processing method. Interestingly, the utilization of microfluidics for material design largely focuses on the fabrication of single entities that act as reaction volume for organic and cell-free biosynthesis, cell mimics, or local environment for cell culturing. In recent years, however, hydrogel design has shifted towards structures that integrate a large variety of functions, e.g., to address the demands for sensing tasks in a complex environment or more closely mimicking architecture and organization of tissue by multiparametric cultures. Hence, this review provides an overview of recent literature that explores microfluidics for fabricating hydrogel materials that go well beyond common length scales as well as the structural and functional complexity of microgels necessary to produce hierarchical hydrogel structures. We focus on examples that utilize microfluidics to design microgel-based assemblies, on microfluidically made polymer microgels for 3D bioprinting, on hydrogels fabricated by microfluidics in a continuous fashion, like fibers, and on hydrogel structures that are shaped by microchannels.
- ItemA novel approach to fabricate load-bearing Ti6Al4V-Barium titanate piezoelectric bone scaffolds by coupling electron beam melting and field-assisted sintering(Amsterdam [u.a.] : Elsevier Science, 2022) Riaz, Abdullah; Polley, Christian; Lund, Henrik; Springer, Armin; Seitz, HermannA critical-size bone defect in load-bearing areas is a challenging clinical problem in orthopaedic surgery. Titanium alloy (Ti6Al4V) scaffolds have advantages because of their biomechanical stability but lack electrical activity, which hinders their further use. This work is focused on the fabrication of Ti6Al4V-Barium Titanate (BaTiO3) bulk composite scaffolds to combine the biomechanical stability of Ti6Al4V with electrical activity through BaTiO3. For the first time, a hollow cylindrical Ti6Al4V is additively manufactured by electron beam melting and combined with piezoelectric BaTiO3 powder for joint processing in field-assisted sintering. Scanning electron microscope images on the interface of the Ti6Al4V-BaTiO3 composite scaffold showed that after sintering, the Ti6Al4V lattice structure bounded with BaTiO3 matrix without its major deformation. The Ti6Al4V-BaTiO3 scaffold had average piezoelectric constants of (0.63 ± 0.12) pC/N directly after sintering due to partial dipole alignment of the BaTiO3 tetragonal phase, which increased to (4.92 ± 0.75) pC/N after a successful corona poling. Moreover, the nanoindentation values of Ti6Al4V exhibited an average hardness and Young's modulus of (5.9 ± 0.9) GPa and (130 ± 14) GPa, and BaTiO3 showed (4.0 ± 0.6) GPa and (106 ± 10) GPa, respectively. It reveals that the Ti6Al4V is the harder and stiffer part in the Ti6Al4V-BaTiO3 composite scaffold. Such a scaffold has the potential to treat critical-size bone defects in load-bearing areas and guide tissue regeneration by physical stimulation.
- ItemIn situ powder X-ray diffraction during hydrogen reduction of MoO3 to MoO2(Amsterdam [u.a.] : Elsevier Science, 2022) Burgstaller, M.; Lund, H.; O'Sullivan, M.; Huppertz, H.The hydrogen reduction of molybdenum trioxide to molybdenum dioxide is not yet fully understood as evident by continuous scientific interest. Especially the effect of the potassium content on the reduction process has not yet been considered. We prepared several samples of molybdenum trioxide containing varying amounts of potassium by addition of potassium molybdate (K2MoO4). In situ powder X-ray diffraction experiments were then conducted to study the hydrogen reduction of these samples. We especially focused on the influence of the alkali content and on gaining insight into the importance of the intermediary product γ-Mo4O11. During the reduction process, MoO2 is formed from the reduction of MoO3, which then reacts with the starting material to form γ-Mo4O11. With increasing potassium content, the reduction rate is decreased and the fractional content of γ-Mo4O11 built up during the reduction process is increased. As evident from bulk sample reduction, this results in a significant increase in the grain size visualized via scanning electron microscopy. Our investigations once again underline the importance of γ-Mo4O11 on the morphology of the resulting MoO2 powder.
- ItemA review of electrical and thermal conductivities of epoxy resin systems reinforced with carbon nanotubes and graphene-based nanoparticles(Amsterdam [u.a.] : Elsevier Science, 2022) Mousavi, Seyed Rasoul; Estaji, Sara; Kiaei, Hediyeh; Mansourian-Tabaei, Mohammad; Nouranian, Sasan; Jafari, Seyed Hassan; Ruckdäschel, Holger; Arjmand, Mohammad; Khonakdar, Hossein AliEpoxy (EP) resins exhibit desirable mechanical and thermal properties, low shrinkage during cuing, and high chemical resistance. Therefore, they are useful for various applications, such as coatings, adhesives, paints, etc. On the other hand, carbon nanotubes (CNT), graphene (Gr), and their derivatives have become reinforcements of choice for EP-based nanocomposites because of their extraordinary mechanical, thermal, and electrical properties. Herein, we provide an overview of the last decade's advances in research on improving the thermal and electrical conductivities of EP resin systems modified with CNT, Gr, their derivatives, and hybrids. We further report on the surface modification of these reinforcements as a means to improve the nanofiller dispersion in the EP resins, thereby enhancing the thermal and electrical conductivities of the resulting nanocomposites.
- 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.
- ItemExamining the early stages of thermal oxidative degradation in epoxy-amine resins(Amsterdam [u.a.] : Elsevier Science, 2020) Morsch, Suzanne; Liu, Yanwen; Lyon, S.B.; Gibbon, S.R.; Gabriele, Benjamin; Malanin, Mikhail; Eichhorn, Klaus-JochenEpoxy-amine resins continue to find widespread use as the binders in protective and decorative organic coatings, as the matrix in composite materials, and as adhesives. In service, exposure to the environment ultimately results in oxidative deterioration of these materials, limiting the performance lifetime. Defining this auto-oxidation process is therefore a key challenge in developing more durable high-performance materials. In this study, we investigate oxidative degradation of a model resin based on diglycidyl ether of bisphenol-A (DGEBA) and an aliphatic amine hardener, triethylenetetraamine (TETA). Using infrared spectroscopy, we find that prior to the expected detection of formate groups (corresponding to the well-known radical oxidation mechanism of DGEBA), a band at 1658 cm−1 forms, associated with amine cross-linker oxidation. Infrared microspectroscopy, in-situ heated ATR-infrared, Raman spectroscopy and AFM-IR techniques are thus employed to investigate the early stages of resin oxidation and demonstrate strong parallels between the initial stages of cured resin degradation and the auto-oxidation of TETA cross-linker molecules.
- ItemExperimental multi-scale approach to determine the local mechanical properties of foam base material in polyisocyanurate metal panels(Amsterdam [u.a.] : Elsevier Science, 2021) Gahlen, P.; Fröbel, S.; Karbach, A.; Gabriel, D.; Stommel, M.Polyisocyanurate (PIR) foams were examined regarding their local chemical composition using ATR-IR spectroscopy. As a special parameter the PIR: Amide III intensity ratio is to be mentioned, which represents the quantity of the formed PIR groups. Based on the local PIR: Amide III intensity ratio, the mechanical properties (Young's modulus) of the foam base material were analyzed at defined positions by AFM and Nanoindentation. It turned out that the AFM method is only suitable for qualitative analysis, because the values differ strongly from macroscopic measurements. For the measurements using nanoindentation, a new embedding method was developed, which achieves significantly more realistic and reproducible results compared to the embedding method used in the literature and shows a very good agreement with the macroscopic values. In general, it has been shown that a higher PIR: Amide III intensity ratio tends to lead to a higher Young's modulus. Nevertheless, there are other, currently unknown characteristic values which also influence the Young's modulus.