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- ItemApplication of sulfonated nanoporous carbons as acid catalysts for Fischer esterification reactions(Amsterdam : Elsevier, 2015) Tamborini, L.H.; Militello, M.P.; Balach, J.; Moyano, J.M.; Barbero, C.A.; Acevedo, D.F.Heterogeneous acid catalysts were prepared by sulfonation of nanoporous carbons (NPCs). The NPCs were produced by pyrolysis of resorcinol–formaldehyde nanoporous resins (NPRs). The NPRs were synthesized as wet gels by condensation of resorcinol and formaldehyde in a sol–gel polycondensation using Na2CO3 as catalyst. A cationic polyelectrolyte (poly(diallyl dimethyl ammonium chloride)) was used as pore stabilizer, allowing to dry the gels in air without any special procedures. Five NPRs with different properties were synthesized by varying the monomer to catalyst ratio (Resorcinol/Na2CO3, R/C). The morphological and textural characterizations of the NPCs were performed by scanning electron microscopy and nitrogen adsorption–desorption isotherms. The results indicate that using a molar ratio of R/C = 200, a nanoporous carbon NPC with large surface area (695 m2/g) is obtained. This NPC was sulfonated by reaction with three different sulfonating agents: (i) concentrated sulfuric acid; (ii) fuming sulfuric acid and (iii) chlorosulfonic acid in order to obtain a novel Fischer esterification catalyst. The amount of acid groups attached to the NPC surface was determined by titration using a modified Boehm method. The catalytic activity, for Fischer esterification reaction of different sulfonated NPCs, was compared with sulfonated NPRs, sulfonated commercial porous carbons and polymeric acid catalyst (cationic ion exchange resins, sulfonated fluoropolymers). The modification of NPCs with concentrated sulfuric acid seems to render the materials with more catalytic activity. The best sulfonated material NPC (PC200-H2SO4) shows a high catalytic activity for the esterification of acetic acid (90.8%) and oleic acid (60.6%) with ethanol. The conversion and conversion rate values are better than commercial acid catalysts. The results suggest that sulfonated NPC catalysts are promising materials for the synthesis of biodiesel and related reactions.
- ItemIn-situ investigations of structural changes during cyclic loading by high resolution reciprocal space mapping(Amsterdam : Elsevier, 2017) Diederichs, Annika M.; Thiel, Felix; Lienert, Ulrich; Pantleon, WolfgangA major failure reason for structural materials is fatigue-related damage due to repeatedly changing mechanical loads. During cyclic loading dislocations self-organize into characteristic ordered structures, which play a decisive role for the materials lifetime. These heterogeneous dislocation structures can be identified using advanced electron microscopy and synchrotron techniques. A detailed characterization of the microstructure during cyclic loading by in-situ monitoring the internal structure within individual grains with high energy x-rays can help to understand and predict the materials behavior during cyclic deformation and to improve the material design. While monitoring macroscopic stress and strain during cyclic loading, reciprocal space maps of diffraction peaks from single grains are obtained with high resolution. High Resolution Reciprocal Space Mapping was applied successfully in-situ during cyclic deformation of macroscopic aluminium samples at the Advanced Photon Source to reveal the structural reorganization within single grains embedded in the bulk material during fatigue.
- ItemNew electronic device for driving surface acoustic wave actuators(Amsterdam : Elsevier, 2009) Brünig, R.; Mensel, K.; Kunze, R.; Schmidt, H.Surface acoustic wave (SAW) actuators are driven by a high frequency signal. The frequency range for an ideal SAW-generation is usually very narrow banded and may shift depending on various environmental conditions. We present a new electronic device which self-aligns to the optimal excitation frequency within a wide range. Any kind of SAW-actuator can be used. The device continuously scans a certain frequency range and characterizes the SAW-component. The ideal excitation frequency is then determined and used to drive the SAW-device. In case of changes like loading conditions or temperature variations the device automatically readjusts to the optimal frequency and prevents possible damage of the device or actuator in case of an error. © 2009.
- ItemDetermination of fluoride component in the multifunctional refining flux used for recycling aluminum scrap(Amsterdam : Elsevier, 2020) Wan, Bingbing; Li, Wenfang; Liu, Fangfang; Lu, Tiwen; Jin, Shuoxun; Wang, Kang; Yi, Aihua; Tian, Jun; Chen, WeipingIn this paper, the optimum fluoride component in the multifunctional refining flux used for recycling aluminum scrap was determined. Theoretical analysis of solid fluxing shows that strong stripping ability of oxide layer on aluminum surface for the flux and appropriate interfacial tensions between Al melt / inclusion (σM-I), flux / inclusion (σF-I), and flux / Al melt (σF-M) are indispensable for making the flux achieve the properties of covering, drossing, and cleaning simultaneously. In term of four preliminarily selected fluoride salts, i.e., KF, AlF3, K3AlF6 and KAlF4, the results of interfacial tension measurements indicates that, combined addition of A-type fluoride (KF) and B-type fluoride (AlF3, K3AlF6 and KAlF4) to equimolar NaCl-KCl can just offset the shortage of single addition of KF which means worsening the separating effect of flux from melt surface and weakening the wettability of flux on the inclusions due to the lower σF-M and the higher σF-I respectively. Additionally, coalescence behaviors of aluminum droplets in molten fluxes reveals that, KF, K3AlF6 or KAlF4 possesses stronger stripping ability of oxide layer, while the stripping ability of oxide layer for AlF3 is weaker. Ultimately, the combination of KF with K3AlF6 or/and KAlF4 is ascertained to be an optimum selection for fluoride component in the multifunctional refining flux.
- ItemElectrodeposition of Sr-substituted hydroxyapatite on low modulus beta-type Ti-45Nb and effect on in vitro Sr release and cell response(Amsterdam : Elsevier, 2019) Schmidt, Romy; Gebert, Annett; Schumacher, Matthias; Hoffmann, Volker; Voss, Andrea; Pilz, Stefan; Uhlemann, Margitta; Lode, Anja; Gelinsky, MichaelBeta-type Ti-based alloys are promising new materials for bone implants owing to their excellent mechanical biofunctionality and biocompatibility. For treatment of fractures in case of systemic diseases like osteoporosis the generation of implant surfaces which actively support the problematic bone healing is a most important aspect. This work aimed at developing suitable approaches for electrodeposition of Sr-substituted hydroxyapatite (Srx-HAp) coatings onto Ti-45Nb. Potentiodynamic polarization measurements in electrolytes with 1.67 mmol/L Ca(NO3)2, which was substituted by 0, 10, 50 and 100% Sr(NO3)2, and 1 mmol/L NH4H2PO4 at 333 K revealed the basic reaction steps for OH– and PO4 3− formation needed for the chemical precipitation of Srx-HAp. Studies under potentiostatic control confirmed that partial or complete substitution of Ca2+- by Sr2+-ions in solution has a significant effect on the complex reaction process. High Sr2+-ion contents yield intermediate phases and a subsequent growth of more refined Srx-HAp coatings. Upon galvanostatic pulse-deposition higher reaction rates are controlled and in all electrolytes very fine needle-like crystalline coatings are obtained. With XRD the incorporation of Sr-species in the hexagonal HAp lattice is evidenced. Coatings formed in electrolytes with 10 and 50% Sr-nitrate were chemically analyzed with EDX mapping and GD-OES depth profiling. Only a fraction of the Sr-ions in solution is incorporated into the Srx-HAp coatings. Therein, the Sr-distribution is laterally homogeneous but non-homogeneous along the cross-section. Increasing Sr-content retards the coating thickness growth. Most promising coatings formed in the electrolyte with 10% Sr-nitrate were employed for Ca, P and Sr release analysis in Tris-Buffered Saline (150 mM NaCl, pH 7.6) at 310 K. At a sample surface: solution volume ratio of 1:200, after 24 h the amount of released Sr-ions was about 30–35% of that determined in the deposited Srx-HAp coating. In vitro studies with human bone marrow stromal cells (hBMSC) revealed that the released Sr-ions led to a significantly enhanced cell proliferation and osteogenic differentiation and that the Sr-HAp surface supported cell adhesion indicating its excellent cytocompatibility. © 2019 The Authors
- ItemRare-earth-free MnAl-C-Ni permanent magnets produced by extrusion of powder milled from bulk(Amsterdam : Elsevier, 2020) Feng, Le; Freudenberger, Jens; Mix, Torsten; Nielsch, Kornelius; Woodcock, Thomas GeorgeRare-earth-free MnAl-C-Ni permanent magnets have been produced for the first time by extruding powders milled from bulk. The resulting materials, fabricated using different conditions, contained a large volume fraction (> 0.92) of the desired τ-phase. In terms of the maximum energy product, the best performance obtained for a whole, transverse section of the extruded material was (BH)max = 46 kJm−3, and was (BH)max = 49 kJm−3 for a sample taken from near the edge of this section. Analysis showed that this material was comparable to the long-established benchmark, comprising MnAl-C-based magnets extruded in industry from bulk or from gas-atomised powder. Such materials are no longer available. The microstructure of the materials produced here consisted of fine, recrystallised grains, which exhibited an <001> fibre texture with intermediate texture quality and of larger, non-recrystallised regions, which contained hierarchical twinning and a high density of defects. The volume fraction and size of the non-recrystallised regions was greatly reduced by decreasing the size of the initial powder particles. This led to a large increase in the squareness factor of the demagnetisation curve and consequently to the high (BH)max values observed.
- ItemTailoring biocompatible Ti-Zr-Nb-Hf-Si metallic glasses based on high-entropy alloys design approach(Amsterdam : Elsevier, 2020) Calin, Mariana; Vishnu, Jithin; Thirathipviwat, Pramote; Popa, Monica-Mihaela; Krautz, Maria; Manivasagam, Geetha; Gebert, AnnettPresent work unveils novel magnetic resonance imaging (MRI) compatible glassy Ti-Zr-Nb-Hf-Si alloys designed based on a high entropy alloys approach, by exploring the central region of multi-component alloy phase space. Phase analysis has revealed the amorphous structure of developed alloys, with a higher thermal stability than the conventional metallic glasses. The alloys exhibit excellent corrosion properties in simulated body fluid. Most importantly, the weak paramagnetic nature (ultralow magnetic susceptibility) and superior radiopacity (high X-ray attenuation coefficients) offer compatibility with medical diagnostic imaging systems thereby opening unexplored realms for biomedical applications.
- ItemDevelopment and characterization of a metastable Al-Mn-Ce alloy produced by laser powder bed fusion(Amsterdam : Elsevier, 2021) Gabrysiak, Katharina; Gustmann, Tobias; Freudenberger, Jens; Neufeld, Kai; Giebeler, Lars; Leyens, Christoph; Kühn, UtaLaser powder bed fusion (LPBF) can help to overcome two challenges occurring by casting of metastable Al alloys: (1) the high amount of casting defects and (2) the limited part size while maintaining rapid solidification of the whole cross-section. In this study, an Al92Mn6Ce2 alloy was processed crack-free without baseplate heating by LPBF. The high cooling rate during fabrication has a significant impact on the microstructure, which was characterized by SEM, TEM and XRD. The processing through LPBF causes a high amount and a strong refinement of the intermetallic Al20Mn2Ce precipitates. This leads, compared to suction-cast specimens, to a higher hardness (180 HV 5) and a higher tolerable compressive stress (>1200 MPa) associated with a pronounced plasticity without failure up to a strain of 40%. The extraordinary mechanical properties of additively manufactured Al92Mn6Ce2 can extend the possibilities of producing novel LPBF lightweight structures for potential applications under harsh conditions.
- ItemNano energy for miniaturized systems(Amsterdam : Elsevier, 2021) Zhu, Minshen; Zhu, Feng; Schmidt, Oliver G.Skin mountable electronic devices are in a high-speed development at the crossroads of materials science, electronics, and computer science. Sophisticated functions, such as sensing, actuating, and computing, are integrated into a soft electronic device that can be firmly mounted to any place of human body. These advanced electronic devices are capable of yielding abilities for us whenever they are needed and even expanding our abilities beyond their natural limitations. Despite the great promise of skin mounted electronic devices, they still lack satisfactory power supplies that are safe and continuous. This Perspective discusses the prospects of the development of energy storage devices for the next generation skin mountable electronic devices based on their unique requirements on flexibility and miniaturized size.
- ItemEditorial for a special issue “Nano energy materials and devices for miniaturized electronics and smart systems”(Amsterdam : Elsevier, 2021) Zhu, Feng; Schmidt, Oliver G.[No abstract available]