Journal articles and book contributions

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Brokmann, Ulrike; Weigel, Christoph; Altendorf, Luisa-Marie; Strehle, Steffen; Rädlein, Edda
Wet chemical and plasma etching of photosensitive glass. - In: Solids, ISSN 2673-6497, Bd. 4 (2023), 3, S. 213-234

Photosensitive glasses for radiation-induced 3D microstructuring, due to their optical transparency and thermal, mechanical, and chemical resistance, enable the use of new strategies for numerous microscale applications, ranging from optics to biomedical systems. In this context, we investigated the plasma etching of photosensitive glasses after their exposure and compared it to the established wet chemical etching method, which offers new degrees of freedom in microstructuring control and microsystem fabrication. A CF4/H2 etching gas mixture with a constant volumetric flow of 30 sccm and a variable H2 concentration from 0% to 40% was utilized for plasma-based etching, while for wet chemical etching, diluted hydrofluoric acid (1% ≤ cHF ≤ 20%) was used. Therefore, both etching processes are based on a chemical etching attack involving fluorine ions. A key result is the observed reversion of the etch selectivity between the initial glassy and partially crystallized parts that evolve after UV exposure and thermal treatment. The crystallized parts were found to be 27 times more soluble than the unexposed glass parts during wet chemical etching. During the plasma etching process, the glassy components dissolve approximately 2.5 times faster than the partially crystalline components. Unlike wet chemical etching, the surfaces of plasma etched photostructured samples showed cone- and truncated-cone-shaped topographies, which supposedly resulted from self-masking effects during plasma etching, as well as a distinct physical contribution from the plasma etching process. The influences of various water species on the etching behaviors of the homogeneous glass and partially crystallized material are discussed based on FTIR-ATR and in relation to the respective etch rates and SNMS measurements.



https://doi.org/10.3390/solids4030014
Stauffenberg, Jaqueline; Reibe, Michael; Krötschl, Anja; Reuter, Christoph; Ortlepp, Ingo; Dontsov, Denis; Hesse, Steffen; Rangelow, Ivo W.; Strehle, Steffen; Manske, Eberhard
Tip-based nanofabrication below 40 nm combined with a nanopositioning machine with a movement range of Ø100 mm. - In: Micro and nano engineering, ISSN 2590-0072, Bd. 19 (2023), 100201, S. 1-5

In this paper, the combination of an advanced nanopositioning technique and a tip-based system, which can be used as an atomic force microscope (AFM) and especially for field emission scanning probe lithography (FESPL) is presented. This is possible through the use of active microcantilevers that allow easy switching between measurement and write modes. The combination of nanopositioning and nanomeasuring machines and tip-based systems overcomes the usual limitations of AFM technology and makes it possible to perform high-precision surface scanning and nanofabrication on wafer sizes up to 4 in. We specifically discuss the potential of nanofabrication via FESPL in combination with the nanofabrication machine (NFM-100). Results are presented, where nanofabrication is demonstrated in form of a spiral path over a total length of 1 mm and the potential of this technique in terms of accuracy is discussed. Furthermore, ten lines were written with a pitch of 100 nm and a linewidth below 40 nm was achieved, which is in principle possible over the entire range of motion.



https://doi.org/10.1016/j.mne.2023.100201
Mathew, Sobin; Reiprich, Johannes; Narasimha, Shilpashree; Abedin, Saadman; Kurtash, Vladislav; Thiele, Sebastian; Hähnlein, Bernd; Scheler, Theresa; Flock, Dominik; Jacobs, Heiko O.; Pezoldt, Jörg
Three-dimensional MoS2 nanosheet structures: CVD synthesis, characterization, and electrical properties. - In: Crystals, ISSN 2073-4352, Bd. 13 (2023), 3, 448, S. 1-14

The proposed study demonstrates a single-step CVD method for synthesizing three-dimensional vertical MoS2 nanosheets. The postulated synthesizing approach employs a temperature ramp with a continuous N2 gas flow during the deposition process. The distinctive signals of MoS2 were revealed via Raman spectroscopy study, and the substantial frequency difference in the characteristic signals supported the bulk nature of the synthesized material. Additionally, XRD measurements sustained the material’s crystallinity and its 2H-MoS2 nature. The FIB cross-sectional analysis provided information on the origin and evolution of the vertical MoS2 structures and their growth mechanisms. The strain energy produced by the compression between MoS2 islands is assumed to primarily drive the formation of vertical MoS2 nanosheets. In addition, vertical MoS2 structures that emerge from micro fissures (cracks) on individual MoS2 islands were observed and examined. For the evaluation of electrical properties, field-effect transistor structures were fabricated on the synthesized material employing standard semiconductor technology. The lateral back-gated field-effect transistors fabricated on the synthesized material showed an n-type behavior with field-effect mobility of 1.46 cm2 V^-1 s^-1 and an estimated carrier concentration of 4.5 × 10^12 cm^-2. Furthermore, the effects of a back-gate voltage bias and channel dimensions on the hysteresis effect of FET devices were investigated and quantified.



https://doi.org/10.3390/cryst13030448
Moritz, Dominik Christian; Calvet, Wolfram; Zare Pour, Mohammad Amin; Paszuk, Agnieszka; Mayer, Thomas; Hannappel, Thomas; Hofmann, Jan Philipp; Jaegermann, Wolfram
Dangling bond defects on Si surfaces and their consequences on energy band diagrams: from a photoelectrochemical perspective. - In: Solar RRL, ISSN 2367-198X, Bd. 7 (2023), 9, 2201063, S. 1-10

Using silicon in multijunction photocells leads to promising device structures for direct photoelectrochemical water splitting. In this regard, photoelectron spectra of silicon surfaces are used to investigate the energetic condition of contact formation. It is shown that the Fermi-level position at the surface differs from the values expected from their bulk doping concentrations, indicating significant surface band bending which may limit the overall device efficiency. In this study, the influence of different surface preparation procedures for p- and n-doped Si wafers on surface band bending is investigated. With the help of photoemission and X-ray absorption spectroscopy, Si dangling bonds are identified as dominating defect centers at Si surfaces. These defects lead to an occupied defect band in the lower half and an unoccupied defect band in the upper half of the Si bandgap. However, partial oxidation of the defect centers causes a shift of defect bands, with only donor states remaining in the Si bandgap. Source-induced photovoltages at cryogenic temperatures indicate that partial surface oxidation also decreases the recombination activity of these defect centers. It is shown that defect distribution, defect concentration, and source-induced photovoltages need to be considered when analyzing Fermi-level pinning at Si surfaces.



https://doi.org/10.1002/solr.202201063
Shekhawat, Deepshikha; Sudhahar, Dwarakesh; Döll, Joachim; Grieseler, Rolf; Pezoldt, Jörg
Phase formation of cubic silicon carbide from reactive silicon-carbon multilayers. - In: MRS advances, ISSN 2059-8521, Bd. 8 (2023), 9, S. 494-498

Silicon carbide layers were fabricated using self-propagating high-temperature synthesis of binary silicon-carbon based reactive multilayers. The silicon and carbon bilayers were fabricated with two different bilayer thicknesses. They are deposited by magnetron sputtering in an alternating layer system with a total thickness of 1 μm. The entire system is annealed by rapid thermal annealing at different temperatures ranging from 500 to 1100 ˚C. From XRD analysis we could find that the formation of the silicon carbide phase was initiated from 700 ˚C. With increasing bilayer thickness the silicon carbide phase formation was partially suppressed by the silicon recrystallization due to resulting lower carbon diffusion into silicon. The transformation process proceeds in a four-step process: densification/recrystallization, interdiffusion, nucleation and transformation. From this, it was noted that when compared to low bilayer thickness samples, the formation of the silicon carbide phase is delayed with increasing bilayer thickness and needs higher reaction initiation temperatures.



https://doi.org/10.1557/s43580-023-00531-3
Kurtash, Vladislav; Jacobs, Heiko O.; Pezoldt, Jörg
Energy-efficient operation conditions of MoS2-based memristors. - In: Physica status solidi, ISSN 1862-6319, Bd. 220 (2023), 13, 2200893, S. 1-12

Sufficient energy consumption for conventional information processing makes it necessary to look for new computational methods. One of the possible solutions to this problem is neuromorphic computations using memristive devices. Memristors based on molybdenum disulfide (MoS2) are a promising way to provide a sizeable amount of hysteresis at low energy costs. Herein, different configurations of MoS2 memristors as well as the mechanisms involved in hysteresis formation are shown. Bottom gated configuration is beneficial in terms of hysteresis area and energy efficiency. The impact of device channel dimensions on the hysteresis area and energy consumption is discussed. Different operation conditions with triangular, rectangular, sinusoidal, and sawtooth drain-to-source pulses are simulated, and rectangular pulses demonstrate the highest energy efficiency. The study shows the potential to realize low-power neuromorphic systems using MoS2 memristive devices.



https://doi.org/10.1002/pssa.202200893
Shekhawat, Deepshikha; Baloochi, Mostafa; Sudhahar, Dwarakesh; Raheja, Vishal Amarbhai; Döll, Joachim; Jacobs, Heiko O.; Pezoldt, Jörg
Influence of environment on self-propagating reactions in Al/Ni multilayer foils. - In: MRS advances, ISSN 2059-8521, Bd. 8 (2023), 9, S. 477-483

Reactive aluminum-nickel multilayer system shows exothermic energetic materials which act as a heat source for packaging and bonding of microsystems. The main challenge is controlling the self-propagation reaction velocity and temperature generated by thermal management through different thermal conductive substrate materials. The current work investigates the heat distribution of Al/Ni multilayer foils from different thermal conductive substrates which act as heat sink materials during the self-propagating reaction. A two-dimensional numerical model was developed to study thermal conductive heat loss and substrate thermal properties on the self-propagating reaction in Al/Ni multilayer foils. The self-propagating reaction was introduced on the surface of the foils by an electrical spark. Here we investigate the minimum critical thickness of Al/Ni multilayer foils which shows the self-propagation reaction on different substrates and verified from the two-dimensional numerical model. The outcomes of this investigation will facilitate the integration of Al/Ni multilayer foils on different substrates as intrinsic heat sources for different applications of micro/nanodevices.



https://doi.org/10.1557/s43580-023-00574-6
Böttcher, René; Ispas, Adriana; Bund, Andreas
Binary aluminum alloys from 1-ethyl-3-methylimidazolium-based ionic liquids for cathodic corrosion protection. - In: Metals, ISSN 2075-4701, Bd. 13 (2023), 2, 377, S. 1-15

Aluminum cannot provide continuous cathodic corrosion protection under ambient conditions due to the formation of an insulating oxide layer and therefore it should be alloyed. Binary aluminum alloys with Cr, Zn and Sn from AlCl3/1-ethyl-3-methylimidazolium chloride ([EMIm]Cl) containing CrCl2, ZnCl2 or SnCl2 have been deposited and their morphology and composition were investigated using SEM/EDS. The corrosion behavior of alloys with 2–4 wt% Cr, Zn or Sn was investigated using potentiodynamic polarization in 3.5 wt% NaCl solution, neutral salt spray test (NSS) and environmental exposure (EE). Pure aluminum provides excellent corrosion protection of steel in a chloride-containing environment, but not under ambient conditions. AlCr alloys show poor corrosion protection while AlZn alloys provide excellent corrosion protection in the NSS test and superior cathodic protection in the EE test compared to aluminum. AlSn alloys are highly active at even low tin contents and dissolve rapidly in chloride-containing electrolytes. However, a slightly improved cathodic protection in the EE test compared to pure aluminum has been observed. The results prove the necessity of alloying aluminum to achieve effective cathodic corrosion protection under mild atmospheric conditions.



https://doi.org/10.3390/met13020377
Arciniega, Luciano Bellatin; Yapu, Raúl Meza; Valencia, Daniel Obregón; Hadzich, Antonella; Costa, Marcus A.; Ispas, Adriana; Bund, Andreas; Flores, Santiago
Alkyds with artistic applications based on drying oils, multifunctional polyalcohols and different polybasic acids. - In: Journal of applied polymer science, ISSN 1097-4628, Bd. 140 (2023), 16, e53746, S. 1-12

Today's requirements in the art field have challenged researchers to create artistic paintings with attractive appearance and long-term color stability. Alkyd-based art mediums have become an important group in the art field, because of their similar characteristics to traditional oils and exceptional drying properties. In this work, high solid alkyd-based art mediums have been synthesized by the monoglyceride and acidolysis processes. Multifunctional polyols and high unsaturated fatty acid sources were compared and used for alkyd synthesis. The use of a non-traditional oil of Peruvian origin is proposed. Resins have been characterized according to their physicochemical (acid number, viscosity, color and density) and drying properties. Drying tendencies were verified with the use of quartz crystal microbalance. Also, the behavior of the art mediums mixed with commercial oil paintings and a dry pigment, have also been evaluated. Results indicate that resins containing the polyol with the highest functionality are more viscous and have fewer tendencies to yellowing, while non-traditional Peruvian oil is the best option for creating light-colored art mediums. Alkyd mediums prepared by the monoglyceride method gave to oil paintings better characteristics and drying behavior on canvas.



https://doi.org/10.1002/app.53746
Nandy, Manali; Paszuk, Agnieszka; Hanke, Kai Daniel; Kleinschmidt, Peter; Hannappel, Thomas
Optical in situ studies of Ge(100) interfacial exchange reactions in GaAs-rich MOVPE reactors for low-defect III-P growth. - In: ACS applied electronic materials, ISSN 2637-6113, Bd. 5 (2023), 2, S. 1295-1301

For vertical-cavity surface-emitting lasers (VCSELs) or photoelectrochemical devices and high efficient III-V/Ge(100) photovoltaics, preparation of double-atomic steps on Ge(100) substrates is highly recommended in order to avoid anti-phase boundaries in the III-V buffer layers. These Ge(100) surfaces were investigated in detail under As- and GaAs-rich MOVPE reactor conditions. During initial growth of III-P buffer layers, however, on an atomically well-ordered Ge(100):As surface, As-P exchange takes place, during which double-layer steps should be preserved. Here, we apply in situ monitoring to study the interaction of P with vicinal Ge(100):As surfaces under realistic, GaAs-rich CVD reactor conditions at growth temperature. In situ optical spectroscopy in combination with surface science techniques in ultra-high vacuum ambience is used to investigate the Ge(100) surface. We show that different Ge(100):As/P heterointerfaces are formed depending on the applied molar flow of phosphorus precursors. Despite the lattice-matched quality of the probing III-P layer, this critical heterointerface impacts significantly the surface roughness and the formation of crystal defects in the subsequently grown III-P buffer layers.



https://doi.org/10.1021/acsaelm.2c01775