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In this study, the temperature and volume fraction distributions of liquid silicon nanoparticles in the aerosol flow in gas-phase synthesis were retrieved using tomographic reconstruction of emission and extinction spectra in the 230–700 nm range. Measurements were done in an optically accessible microwave-plasma flow reactor fed with a SiH4/H2/Ar gas mixture. Optical emission and extinction spectra in the visible spectral range were captured along a line perpendicular to the flow direction covering the entire cross-section of the Si particle stream. Particle temperature and volume fraction distributions were determined and the preferred location of the silicon particles in a 1-mm thick zone at the circumference of the cylindric flow was revealed. The combined recording of line-resolved emission/extinction spectra is a promising method for spatially-resolved detection of nanoparticles in combustion or gas-phase synthesis.

Two-dimensional thermographic particle image velocimetry (T-PIV) is presented for the in situ measurement in optically accessible internal combustion (IC) engines. Temperature and velocity measurements are combined using thermographic phosphor particles as tracers for PIV. For three commercially available phosphors (BAM:Eu2+, ZnO, and ZnO:Zn), temperature sensitivity, luminescence intensity at high temperatures and laser-fluence dependence were evaluated for phosphor-coated surfaces in a high-temperature cell. ZnO:Zn was identified as the best-suited candidate for engine in-cylinder measurements and further analyzed in the aerosolized state at temperatures up to 775 K to generate calibration data required for signal quantification in engine experiments. T-PIV was successfully applied in the IC engine to simultaneously obtain instantaneous two-dimensional velocity and temperature fields using the intensity-ratio method. Despite a measurement uncertainty (±1σ basis) of only 3.7 K at 317 K (1.2%) to 24.4 K (4.2%) at 575 K, this technique suffers from low signal intensities due to thermal quenching at increasing temperatures, which leads to reduced accuracy as the piston approaches top dead center. Thermographic measurements were successful to visualize local temperature changes due to evaporative cooling after fuel injection. The measured mean gas temperatures agreed well with zero-dimensional simulations that use additional wall-temperature measurements from thermographic phosphor measurements based on the lifetime method as input for heat transfer calculations.

Scientific reports 11(1), 22311 (2021). doi:10.1038/s41598-021-01774-6, During the last decades discussions were taking place on the existence of global, non-thermal structural changes in biological macromolecules induced by Terahertz (THz) radiation. Despite numerous studies, a clear experimental proof of this effect for biological particles in solution is still missing. We developed a setup combining THz-irradiation with small angle X-ray scattering (SAXS), which is a sensitive method for detecting the expected structural changes. We investigated in detail protein systems with different shape morphologies (bovine serum albumin, microtubules), which have been proposed to be susceptible to THz-radiation, under variable parameters (THz wavelength, THz power densities up to 6.8 mW/cm$^2$, protein concentrations). None of the studied systems and conditions revealed structural changes detectable by SAXS suggesting that the expected non-thermal THz-induced effects do not lead to alterations of the overall structures, which are revealed by scattering from dissolved macromolecules. This leaves us with the conclusion that, if such effects are present, these are either local or outside of the spectrum and power range covered by the present study., Published by Macmillan Publishers Limited, part of Springer Nature, [London]

Comprehensive characterization of crumpled graphene materials is required to understand their morphologically dependent properties. This study connects the optical properties of crumpled few-layer graphene (FLG) aerosols and colloidal suspensions with particle morphology. The mass absorption cross-section (MAC) of crumpled FLG was measured in the aerosol phase and it is shown that such aerosols absorb visible light more efficiently than soot aerosols. The UV–Vis spectra of FLG suspensions in ethanol were correlated with the mean nanoparticle layer number and the lateral size. The measured optical properties were also simulated using discrete dipole approximation (DDA) applied to volume-reconstructed particles with refractive indices of graphene and graphite from literature. The measurements were more closely reproduced using the refractive index of graphite pellets rather than flat graphene on a substrate. Moreover, we show that a simpler Rayleigh–Debye–Gans (RDG) model can predict the wavelength dependence of the crumpled FLG absorption cross-section.

The NFDI4Ing Conference 2022 took place online on 26 and 27 October2022. The authors would like to thank the Federal Government and the Heads of Government of the Länder, as well as the Joint Science Conference (GWK), for their funding and support within the framework of the NFDI4Ing consortium. Funded by the German Research Foundation (DFG) - project number 442146713. If not stated otherwise within the respective document, the files go by CC-BY 4.0 license. Please refer to the license comments in the resprective slide decks.

This paper presents a novel experiment in an atmospheric cylindrical single-jet combustor, designed to exhibit high-frequency radial thermoacoustic instabilities. The experimental configuration was...

The self-assembly of thermoresponsive amphiphilic diblock copolymer PMMA21-b-PNIPAM283 is studied in different water/methanol mixtures. It consists of a short hydrophobic poly(methyl methacrylate) block and a long thermoreponsive poly(N-isopropylacrylamide) block. Adding methanol as a cosolvent causes the PNIPAM block, which is soluble in both pure water and pure methanol, to collapse due to so-called co-nonsolvency effect. Meanwhile, the addition of methanol reduces the incompatibility of the PMMA block with water. By means of turbidimetry and differential scanning calorimetry, the solvent-composition-dependent phase diagram is constructed. Dynamic light scattering and synchrotron radiation based small-angle X-ray scattering (SAXS) provide structural information at 20 °C in dependence on the solvent composition. In water-rich solvent mixtures, self-assembled spherical core-shell micelles are formed. The internal structure of the micelles is adjusted by the solvent compositions in two ways: methanol softens the PMMA micellar core, while it causes the shrinkage of the PNIPAM micellar shell. In methanol-rich solvent mixtures beyond the miscibility gap, the copolymers are molecularly dissolved chains. They are collapsed near the coexistence line, while they become random coils as the methanol content increases. We propose that the internal morphology of the micelles and the conformation of the dissolved chains depend strongly on the solvent composition, as a consequence of the superposed co-nonsolvency effect of PNIPAM and the overall enhanced solvation of PMMA when adding m ethanol.

We demonstrate how the evaporation properties of gas-borne nanoscale materials, here liquid silicon and germanium nanoparticles, can be obtained through a novel combination of in situ time-resolved...

Gas-phase iron compounds strongly affect the flame structure already at very low concentrations, which implies the control of combustion efficiency, pollution formation, and materials synthesis in flames. The impact of iron pentacarbonyl on low-pressure premixed flames was investigated experimentally and numerically for a broad range of equivalence ratios. The burner was operated in top-to-bottom orientation, causing a strong effect of buoyancy on the flow field, a configuration, also known as buoyancy-opposed flame. The application of ultra-sensitive broadband intracavity laser absorption diagnostics enabled path-integrated measurements of gas-phase FeO in the particle-laden flow. Spatially-resolved temperature distributions were measured via OH laser-induced fluorescence. The measurements were complemented by detailed simulations of the down-firing flame to determine the (one-dimensional) flow field on the centerline of the burner. The experimental findings were the basis for extension of existing reaction schemes for iron-doped flames and a new skeletal scheme was proposed. Measured temperatures and normalized FeO concentrations were used to validate both the detailed and the skeletal scheme. The results of the optimization and reduction procedure helped to improve the understanding of the structure of the iron-doped flame and the role of iron-cluster formation in the interaction mechanisms which cause the flame inhibition or promotion by iron-compounds.

Late-evaporating liquid fuel wall-films are considered a major source of soot in spark-ignition direct-injection (SIDI) engines. In this study, a direct-injection model experiment was developed to visualize soot formation in the vicinity of evaporating fuel films. Isooctane is injected by a multi-hole injector into the optically accessible part of a constant-flow facility at atmospheric pressure. Some of the liquid fuel impinges on the quartz-glass windows and forms fuel films. After spark ignition, a turbulent flame front propagates through the chamber, and subsequently sooting combustion is detected near the fuel films. Overlapping laser light sheets at 532 and 1064 nm excite laser-induced fluorescence (LIF) of polycyclic aromatic hydrocarbons (PAH) -potential soot precursors- and laser-induced incandescence (LII) of soot, respectively. The 532 nm light sheet has low fluence to avoid the excitation of LII. The LII and LIF signals are detected simultaneously and spectrally separated on two cameras. In complementary line-of-sight imaging, the fuel spray, chemiluminescence, and soot incandescence are captured with a high-speed color camera. In separate experiments, toluene is added to the isooctane as a fluorescent tracer and excited by pulsed 266 nm flood illumination. From images of the LIF signal, the fuel-films’ thickness and mass evolutions are evaluated. The films survive the entire combustion event. PAH LIF is found in close vicinity of the evaporating fuel films. Soot is found spatially separated from, but adjacent to the PAH, both with high spatial intermittency. Average images additionally indicate that soot is formed with a much higher spatial intermittency than PAH. Images from the color camera show soot incandescence earlier and in a similar region compared to soot LII. Chemiluminescence downstream of the soot-forming region is thought to indicate the subsequent oxidation of fuel, soot, and PAH.

We report state-resolved absorption cross-section measurement and oscillator-strength evaluation of the gas-phase iron oxide (FeO) orange system near 611 nm. Intracavity absorption spectroscopy (ICAS) with a homemade broadband dye laser was applied for time-resolved measurements of absorption spectra of shock-activated mixtures of iron pentacarbonyl and carbon dioxide (diluted in argon), generating gas-phase FeO. The measurements were performed with a time resolution of 170 µs in the spectral range of 16,316–16,353 cm−1 that includes a large number of FeO absorption lines. Across the 8-cm diameter of the shock tube, ICAS leads to an effective absorption path length of 260 m. Absorption cross-section values of 0.5 × 10–18–4 × 10–18 cm2 were determined for temperatures around 2200 K and pressures of ∼1.3 bar. Pressure- and temperature-independent oscillator strengths for individual ro-vibronic transitions within the 611-nm band of FeO orange system are reported for the first time. These data are generally applicable for quantitative absorption measurements of flame studies of iron chemistry, where FeO plays a key role as intermediate species.

Ethanol is known to be prone to pre-ignition in internal combustion engines under high-load conditions and its ignition shows large deviations from ideal, spatially, and temporally-homogeneous ignition in shock tubes at moderate temperatures (800–950 K). In this context, the ignition of stoichiometric ethanol/O2 mixtures with various levels of inert gas dilution was investigated in a high-pressure shock tube at ≅20 bar between 800 and 1250 K. Ignition delay times were determined from spatially integral detection of chemiluminescence emission. Additionally, high-repetition-rate color imaging enabled the differentiation of the luminescence in time, space, and spectral range between various ignition modes. In the low-temperature range (800–860 K), different inhomogeneous ignition modes were identified. The addition of small amounts of helium into the undiluted fuel/air mixture was found to be efficient to mitigate pre-ignition, attributed to a variation in heat transfer and thus suppression of the build-up of local temperature inhomogeneities. The experiments in case of spatially homogeneous ignition show very good agreement with the predictions based on three detailed kinetics mechanisms (Zhang et al., CNF 190 (2018) 74, Frassoldati et al., CNF 159 (2012) 2295, and Zhou et al. CNF 197 (2018) 423), inhomogeneities, however, resulted in a shortening of the ignition delay times up to a factor of 2.6.

Tetramethylsilane is a precursor often used for the production of flame-synthesized silica nanoparticles or coatings. This study investigates the chemical reaction mechanism of tetramethylsilane in a series of H2/O2/Ar low-pressure (p = 30 mbar) flames from fuel-lean to slightly fuel-rich flame conditions (φ=0.8, 1.0 and 1.2). Mole fraction profiles are obtained by molecular-beam mass spectrometry. The experimental data are compared to simulations using a recently published reaction mechanism. The present study reveals the influence of the flame composition on the depletion of the precursor TMS, the formation of its main carbon-containing products (e.g. CO2 and CO) and the main silicon-containing intermediates (e.g. Si(CH3)3(CH2)OO), Si(OH)4, SiO2, Si4O10H4) appearing along the routes of particle formation. TEM images of synthesized particles reveal that the nanoparticles obtained from the gas-phase synthesis are spheres with a low degree of agglomeration. The particle size distribution appears to be dependent on the equivalence ratio of the synthesis flames and the changes can tentatively be traced to different particle formation pathways. The data set provided in this work can serve a basis for improvements to the reaction mechanisms of the Si/C/H/O system that are urgently needed to improve particle synthesis processes.

Journal of materials chemistry / A 9(8), 4831-4840 (2021). doi:10.1039/D0TA11096E, Published by Royal Soceity of Chemistry, London [u.a.]

Shock-tube and flow-reactor experiments were used to study the thermal decomposition of diethyl carbonate (C2H5OC(O)OC2H5; DEC). The formation of CO2, C2H4, and C2H5OH was measured with gas chromatography/mass spectrometry (GC/MS) and high-repetition-rate time-of-flight mass spectrometry (HRR-TOF-MS) behind reflected shock waves. The same products were also detected by GC/MS in flow reactor experiments. All experiments combined span a temperature range of 663–1203 K at pressures between 1.0 and 2.0 bar. Time-resolved species concentration profiles from HRR-TOF-MS and product compositions from GC/MS measurements were simulated applying a detailed reaction mechanism for DEC combustion. A master-equation analysis was conducted based on computed energies from G4 calculations. Quantum chemical calculations confirm that DEC primarily decomposes by six-center elimination, C2H5OC(O)OC2H5 → C2H4 + C2H5OC(O)OH (1a) , followed by rapid decomposition of the alkoxy acid, C2H5OC(O)OH → C2H5OH + CO2 (1b) . Measured DEC decomposition rate constants k(T) at p ≈ 1.5 bar can be represented by the Arrhenius equation k(T) = 1013.64±0.12 exp(−204.24±1.95 kJ/mol/RT) s − 1. Theoretical predictions for k1a were in good agreement with experimentally derived values. The theoretical analysis also included dipropyl carbonate (C3H7OC(O)OC3H7; DPC) decomposition and the reactivities of DEC and DPC are compared and discussed in the context of reactivity of dialkyl carbonates under pyrolytic conditions.

To fully master a scaled-up combustion synthesis of nanoparticles toward a wide library of materials with tailored functionalities, a detailed understanding of the underlying kinetic mechanism is r...

Quantitative appraisal of real-world colloidal systems in their native state is key for knowledge-based nanoparticle formulations. Analytical centrifugation (AC) is touted as a quantitative methodology examining settling and creaming of dispersions, but an understanding of the main transmission readout is often nonintuitive and complex. Herein, we introduce a new visualization technique, called transmittograms, that readily depicts the time-resolved settling behavior of solid–liquid dispersions, measured by AC. We validate the utility of transmittogram analysis using silica particles. Further, we demonstrate the strength of the approach to study the nanoscale dynamics in complex fuel cell inks.

The objective of this study was to analyze the recycling possibility of the electric arc furnace dust (EAFD) in the form of a briquette. This paper studied the kinect behavior of the briquette's self-reduction and in contact with molten steel (steel-briquette system) and it was aimed at finding the optimal briquette composition used to recover elements such as Cr, V and W. Thermodynamic simulations with FactSage were carried out to validate the experimental results. The EAFD material as-received was magnetically separated to the form of a magnetic electric arc furnace dust (MEAFD) then characterized analytically and microstructurally. Analytical characterization demonstrated that the EAFD was rich in Cr, W and V. Microstructural analyses revealed the presence of oxides and spinel phases. Three different compositions of briquettes were prepared for the experiments: the first with 84% of MEAFD and 16% C; the second with 82% of MEAFD and 18% C; and the third with 80% of MEAFD and 20% C. Reduction experiments at the temperature of 1500 °C were carried out to study the reduction rate differences in the briquettes and the steel-briquettes systems. Reduction experiments showed that the fastest reaction occurred in the briquette with 20% C for both systems. Among the wide experimental dataset analyzed, the optimal measured recovery was 48.1% Cr, 72.7% W and 47.5% V (in wt%).

Silicon, due to its high abundance and high theoretical specific capacity (~4200 mAh/g) compared to conventional graphite, has emerged as the most attractive candidate for anodes of lithium ion batteries [1]. However, commercial use of silicon-based electrodes is hindered by several degradation problems resulting mainly from high volume expansion during cycling [2], [3]. One promising approach for resolving these issues focuses on stabilizing the cycle life of the anode material by introducing electrochemically inactive components on the nanoscale. This can be achieved by a new type of Si-based nanoparticles (SiNx) that undergo irreversible conversion reactions upon cycling, producing active domains of silicon finely dispersed in an inactive matrix with high cycling stability [4]. While there is an extensive research on electrochemical reaction mechanism, there is less knowledge on electrode formulation and processing. A typical formulation of electrode systems is comprised of an active material (in this case SiNx), a binder, a conductive additive and usually a solvent mixture. Besides the composition, the energy and time input of employed dispersing techniques affect the nanoscale interactions within electrode systems. The resulting particle interactions that are responsible for observed differences in dispersibility govern macroscopic properties such as electrode microstructures, electrode slurry stability and rheology. This in turn, influences the final device manufacturing and ultimately the electrochemical performance [5]. In this work, we examined a set of probe solvents based on the concept of Hansen solubility parameters (HSP) [6], [7]. The dispersibility of solvents was measured from their settling behavior with an analytical centrifuge (AC). With this approach, it was possible to rapidly identify suitable solvents and their composition for optimal anode formulation. The effects of different dispersion methods on stability and homogeneity of the electrode slurries, the nanoscale interactions and the resulting electrode morphology were studied by AC in combination with microscopy and contact angle measurement techniques. In conclusion, processes for tailored anodes and unraveling the underlying process-structure-property relationships allows a realistic assessment of influential parameters on the final battery performance. This is key towards a knowledge-based process development of new SiNx-based lithium ion batteries with enhanced electrical and electrochemical performance. References: [1] S. Goriparti, E. Miele, F. De Angelis, E. Di Fabrizio, R. Proietti Zaccaria, and C. Capiglia, “Review on recent progress of nanostructured anode materials for Li-ion batteries,” J. Power Sources, vol. 257, pp. 421–443, 2014. [2] L. Y. Beaulieu, K. W. Eberman, R. L. Turner, L. J. Krause, and J. R. Dahna, “Colossal reversible volume changes in lithium alloys,” Electrochem. Solid-State Lett., vol. 4, pp. 7–10, 2001. [3] J. R. Szczech and S. Jin, “Nanostructured silicon for high capacity lithium battery anodes,” Energy Environ. Sci., vol. 4, pp. 56–72, 2011. [4] A. Ulvestad, J. P. Mæhlen, and M. Kirkengen, “Silicon nitride as anode material for Li-ion batteries: Understanding the SiNx conversion reaction,” J. Power Sources, vol. 399, pp. 414–421, 2018. [5] K. B. Hatzell, M. B. Dixit, S. A. Berlinger, and A. Z. Weber, “Understanding inks for porous-electrode formation,” J. Mater. Chem. A, vol. 5, pp. 20527–20533, 2017. [6] Y. H. Sehlleier, S. Dobrowolny, L. Xiao, A. Heinzel, C. Schulz, and H. Wiggers, “Micrometer-sized nano-structured silicon/carbon composites for lithium-ion battery anodes synthesized based on a three-step Hansen solubility parameter (HSP) concept,” J. Ind. Eng. Chem., vol. 52, pp. 305–313, 2017. [7] S. Süß, T. Sobisch, W. Peukert, D. Lerche, and D. Segets, “Determination of Hansen parameters for particles: A standardized routine based on analytical centrifugation,” Adv. Powder Technol., vol. 29, pp. 1550–1561, 2018.

Background Dysfunction of human respiratory and electro-cardiac activities could affect the ability of the heart to pump blood and the lungs to inhale oxygen. Thus, a device could simultaneously measure electro-cardiac signal and respiratory pressure could provide vital signs for predicting early warning of cardio-pulmonary function-related chronic diseases such as cardiovascular disease, and respiratory system disease. Results In this study, a flexible device integrated with piezo-resistive sensing element and voltage-sensing element was developed to simultaneously measure human respiration and electro-cardiac signal (including respiratory pressure, respiration frequency, and respiration rhythm; electro-cardio frequency, electro-cardio amplitude, and electro-cardio rhythm). When applied to the measurement of respiratory pressure, the piezo-resistive performance of the device was enhanced by nano-copper modification, which detection limitation of pressure can reduce to 100 Pa and the sensitivity of pressure can achieve to 0.053 ± 0.00079 kPa−1. In addition, the signal-to-noise ratio during bio-electrical measurement was increased to 10.7 ± 1.4, five times better than that of the non-modified device. Conclusion This paper presents a flexible device for the simultaneous detection of human respiration and cardiac electrical activity. To avoid interference between the two signals, the layout of the electrode and the strain sensor was optimized by FEA simulation analysis. To improve the piezo-resistive sensitivity and bio-electric capturing capability of the device, a feather-shaped nano-copper was modified onto the surface of carbon fiber. The operation simplicity, compact size, and portability of the device open up new possibilities for multi-parameter monitoring.

Factors such as not only costs, production time, reproducibility, but also the quality of the components are decisive factors in assessing the economic efficiency of a manufacturing process. With additive manufacturing processes, component production is made possible directly from a 3D CAD model. This means that small series and prototypes can already be produced economically today. In this area, the laser-sintering process, in particular, offers great potential for series production due to its high strength values and ductility. With laser-sintering systems that allow an optical widening of the laser focus, a faster exposure of the component and thus a shortening of the building time is possible. We developed a laser-sintering system whose laser focus diameter is adjustable in its cross-sectional area from 0.47 to 2 mm. The goal for the future is to produce large-area components significantly faster by widening the focus diameter, thus making laser-sintering more productive. In this paper, the focus-dependent melt pool formation is examined in correlation to different hatch distances during the laser-sintering of polyamide 12. For this purpose, a test specimen was developed which can display single tracks as well as a multitude of different track widths for all feasible focus level variations. This knowledge is required to determine and investigate the track width-dependent melt pool formation as a function of the focal diameter of the component cross sections.

Dielectric resonators are placed in front of the metallic plane plate and corner reflectors. Excitation of the resonant mode produces strong scattering of an incident plane wave which shows up as narrow notch in the mono-static radar cross section (RCS) spectral signature at the resonance frequency. Experimental proof at V-band is given with a corner reflector of centimetre size with spherical dielectric resonators of 0.8 mm diameter showing a notch at 64 GHz.

Nanocrystalline nickel-iron layers are produced electrochemically on copper discs by varying the current density and then annealed in a vacuum furnace at a temperature range between 200 and 800 °C. Grain size, iron content, texture and microstrain of the microstructure are primarily characterized by X-ray diffraction (XRD). Instrumented indentation tests and microbending tests for mechanical characterization are carried out. The iron contents of the investigated layers are 5.7, 8.8, 13.5 and 17.7 wt.-%. By varying the annealing temperature, the reduction of the microstrains is initiated at 200 °C and ends at a temperature of about 280 °C. Primary recrystallization starts slightly higher at 220 °C and is completed at 300 °C. With higher iron content, the indicated temperatures shift to slightly higher values. Indentation modulus, Young's modulus, indentation hardness and strength change considerably after the annealing treatment. Fracture strain at the edge, as a measure of ductility, decreases immediately after annealing at 200 °C to 0 %. Low annealing temperatures occurring before the beginning of primary recrystallization lead to an increase in indentation hardness and 0.01-% offset bending yield strength Rp0.01∗ as compared to the electrochemically deposited initial state. After annealing at high temperatures, the mechanical parameters are mostly below the initial values for electrochemical deposition. Hall-Petch (HP) behavior is observed for Rp0.01∗, both for the electrochemically deposited specimens down to almost 6 nm and for the specimens annealed at high temperatures. Specimens annealed at low temperatures deviate from the HP straight line to higher values. In this case, an increase in strength is assumed to be due to the very small nanocrystalline (nc) grain sizes, segregation at the grain boundaries and a decrease in dislocation density. Indentation hardness measurements show almost no dependence on D−0.5 for the electrochemically deposited specimens and also for annealed specimens below 30nm grain size. Above 30nm, the indentation hardness values are considerably higher than for the HP straight line. Overall, the hardness and strength values of the nc specimens, electrochemically deposited or additionally annealed, are significantly higher than those of the microcrystalline (mc) specimens.

The present work aims at the modelling and simulation of the hot rolling process for wire rod and bars. After the fundamentals of plasticity, which are essential for the understanding of the process characteristics have been described, typical section deviations that can be expected in wire rod and bar mills are calculated with help of a numerical simulation model. The model allows the calculation of section shapes under the influence of elastic rolling stand deformations and interstand tensions. From this computational assessment of section faults, the necessity of inline measurement and process control for wire rod and bar mills is shown. This work is part of the PIREF project which incorporates the development of sensors, control systems and process models in order to control the dimensional accuracy of hot rolled wire rod and bars. The metal forming process model, as described here is used internally as a model for the static and kinematic interactions in the rolling process inside of the control model.

Thin films of crystalline silicon nanoparticles (Si NPs) processed from liquid dispersions of NPs (NP inks) using printing-type deposition methods are currently being intensively investigated for t...

Synthesis and characterization of FexOy nanoparticles were carried out in order to study reaction parameters influence in a spray flame reactor. FexOy powders were prepared with three different precursors aiming to understand how the reactor conditions, dispersion gas flow, and precursor solution flow affect morphology, shape, particle size distribution, crystalline phases, and residue content of the obtained materials. Thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy (TEM), x-ray diffraction (XRD), and Raman spectroscopy were employed to characterize the materials. In addition, magnetic behavior of the obtained samples was evaluated. It was found that the evaluated parameters influenced the residue contents obtaining weight changes from 10 to 35%. Particle size distribution centers also showed differences between 17 and 24 nm. By XRD, Raman, and TEM, the presence of hematite (a-Fe2O3), maghemite (γ-Fe2O3), and magnetite (Fe3O4) was evidenced and explained based on the gas and liquid content in the flame. Additionally, the saturation magnetization was measured for selected samples, obtaining values between 26 and 32 emu g−1. These magnetic measurements were correlated with the crystalline phase composition and particle size distributions.

Computational modelling is a vital tool in the research of batteries and their component materials. Atomistic models are key to building truly physics-based models of batteries and form the foundation of the multiscale modelling chain, leading to more robust and predictive models. These models can be applied to fundamental research questions with high predictive accuracy. For example, they can be used to predict new behaviour not currently accessible by experiment, for reasons of cost, safety, or throughput. Atomistic models are useful for quantifying and evaluating trends in experimental data, explaining structure-property relationships, and informing materials design strategies and libraries. In this review, we showcase the most prominent atomistic modelling methods and their application to electrode materials, liquid and solid electrolyte materials, and their interfaces, highlighting the diverse range of battery properties that can be investigated. Furthermore, we link atomistic modelling to experimental data and higher scale models such as continuum and control models. We also provide a critical discussion on the outlook of these materials and the main challenges for future battery research.

To make ceramic based all-solid-state batteries competitive for the battery market, a shift from the separator supported cell-design for lab cells to a scalable, cathode-supported one is necessary to improve the energy density. Using tape casting, we were able to demonstrate for the first time all-ceramic free-standing LiCoO2 (LCO)/Li6.45Al0.05La3Zr1.6Ta0.4O12 (LLZO) mixed cathodes with high capacities and active material utilization. Further morphology engineering by introduction of a sequential layer casting enabled us to tailor the microstructure of the mixed cathodes resulting in opposite concentration gradients for the active material and the electrolyte over the thickness of the cathode. With this optimized microstructure, we were able to increase the discharge capacity of the free-standing mixed cathodes to 2.8 mA h cm(-2) utilizing 99% of the theoretical capacity. For the oxide garnet-based system, both the scalable fabrication method and the achieved electrochemical performance demonstrates industrial relevance for the first time. Additionally, the obtained free-standing cathodes have sufficient mechanical stability to allow the application of hybrid and ultra-thin separators to further increase the energy density on the full cell level.

Spatially and temporally resolved information on thermochemical conditions in hydrocarbon/air flames requires concentration and temperature data obtained by spontaneous Raman/Rayleigh scattering. During the combustion of renewable and more complex fuels, such as ethanol, partially oxidized hydrocarbons are created as intermediates in concentrations large enough to have an influence on the turbulence-chemistry interaction. To obtain concentrations and temperature in flames at atmospheric pressure with a high spatial and temporal resolution, information on the temperature dependent shape and scattering cross section of the major as well as the minor intermediate species is required. Therefore, a novel gas heater based on mixing the hydrocarbons with helium at high temperatures in combination with a multipass Raman spectrometer were developed, able to characterize ro-vibrational Raman scattering of gaseous ethanol in the gaseous phase up to high temperatures and in different spectral regions. The setup is described, its performance evaluated and Raman spectra of gaseous ethanol at atmospheric pressure up to high temperatures is demonstrated.

Hypothesis Understanding deagglomeration, agglomerate formation and structure for very small nanoparticles (NPs), due to their more facile agglomeration, is critical for processing or tailoring agglomerates for nanostructured materials. We propose that by controlling and fine-tuning the interplay of agglomeration (colloidal interaction) and deagglomeration (hydrodynamic forces), the design of agglomerate size, microstructure and morphology is possible even for very small NPs. Experiments Here, we investigate very small SnO2 NPs (10 nm) generated in the gas phase as model system. Small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS) are used to study dispersions in aqueous media across the entire pH range (2–12) at various NaCl concentrations treated with ultrasound. Parallel to size and size distribution, agglomerate morphology and microstructure are analyzed by means of the mass fractal dimension, dm and modeled with ab initio shape simulations. The critical coagulation concentration (CCC) is determined for the alkaline region where the SnO2 NPs are highly charged. Findings Quantitative analysis of SAXS and DLS data reveals that size and size distribution of the agglomerates depend similarly on the electrostatic interaction influenced by pH and salinity as observed by the zeta potential. In contrast dm is mainly influenced by the salt concentration. Ab initio shape simulations support these experimental findings.

Boron has been of considerable interest as fuel for propellants and explosives due to its high gravimetric and volumetric calorific values. In this study, the effects of different mixed modes, blending ratios, and packing densities on ignition and combustion characteristics of boron-aluminum mixture were explored using flash ignition facility and thermobalance. The results showed that the boron nanoparticles can be ignited upon exposure to the flash with a certain amount of aluminum nanoparticles addition and the flame luminous intensity increased with content of the added aluminum. The boron-aluminum mixture in loose contact performed better combustion characteristics than those in tight contact because of more access to the oxygen and less heat dissipation into the bulk sample. The main combustion products were detected and analyzed by the X-ray diffraction (XRD) and scanning electron microscopy (SEM). The temperatures of the ignited nanoparticles were measured and mostly distributed between 1273 K and 1473 K. The burning time decreased significantly with the increase of aluminum addition at the high packing density condition. The boron combustion efficiency increased with the addition of aluminum content in loose contact. The thermogravimetric experimental results showed that the aluminum addition could decrease the primary ignition temperature of boron. Moreover, the photothermal effect and plasmon resonance effect of aluminum were the potential flash ignition mechanism of the boron-aluminum mixture.

The governing of steam turbines is often realised by a set of two or more valves, which control the amount of steam entering the turbine. During part-load operation forces caused by pressure fluctuations, turbulence etc. are acting on the throttling valve and lead to spindle vibrations. Besides these mechanisms, it is assumed that there is also an interaction between the control valves, which leads to another source of vibration. In this paper, the design of a new test rig using air with two parallel control valves is presented. One aspect of the design is the chosen scaling method, which includes material selection for the valve spindle, and ensures comparability and transferability of the vibrational behaviour to the full scale with steam. Another aspect is the selection of measurement equipment. The results show that the reasons for valve vibrations can be located both upstream and downstream of the valve seat. Forces caused by pressure fluctuations in and behind the valve gap lead to similar oscillations at both valves. In addition, the upstream valve causes disturbances that lead to partly differing behaviour of the second valve.

The potential of dimethyl ether (DME) and dimethoxymethane (DMM), representatives of the attractive oxymethylene ether (OME) alternative fuel family, are explored here as reactivity enhancers for methane-fueled polygeneration processes. Typically, such processes that can flexibly generate power, heat, or chemicals, operate under fuel-rich conditions in gas turbines or internal combustion engines. To provide a consistent basis for the underlying reaction mechanisms, it is recognized that speciation data for the DME/CH4 fuel combination are available for such conditions while such information for the DMM/CH4 system is largely lacking. In addition, it should be noted that a detailed speciation study in flames, i.e., combustion systems involving chemistry and transport processes over a large temperature range, is still missing in spite of the potential of such systems to provide extended species information. In a systematic approach using speciation with electron ionization molecular-beam mass spectrometry (EI-MBMS), we thus report, as a first step, investigation of six fuel-rich premixed flames of DME and DMM and their blends with methane with special attention on interesting chemicals. Secondly, a comprehensive but compact DME/DMM/CH4 model (PolyMech2.1) is developed based on these data. This model is then examined against available experimental data under conditions from various facilities, focusing preferentially on elevated pressure and fuel-rich conditions. Comparison with existing literature models is also included in this evaluation. Thirdly, an analysis is given on this basis, via the extensively tested PolyMech2.1 model, for assumed polygeneration conditions in a homogeneous charge compression ignition (HCCI) engine environment. The main interest of this model-assisted exploration is to evaluate whether addition of DME or DMM in a polygeneration process can lead to potentially useful conditions for the production of syngas or other chemicals, along with work and heat. The flame results show that high syngas yields, i.e., up to similar to 78% for CO and similar to 35% for H-2, can be obtained in their burnt gases. From the large number of intermediates detected, predominantly acetylene, ethylene, ethane, and formaldehyde show yields of 2.1-4.4% (C-2 hydrocarbons) and 3.4-8.7% (CH2O), respectively. Also, methanol and methyl formate show comparably high yields of up to 0.6-6.7% in the flames with DMM, which is 1-2 orders of magnitude higher than in those with DME as the additive. In the modeling-assisted exploration of the engine process, the PolyMech2.1 model is seen to perform at significantly reduced computational costs compared to a recently validated model without sacrificing the prediction performance. Promising conditions for the assumed polygeneration process using fuel combinations in the DME/DMM/CH4 system are identified with attractive syngas yields of up to 77% together with work and heat output at exergetic efficiencies of up to 89% with DME. (C) 2021 The Combustion Institute. Published by Elsevier Inc. All rights reserved.

A new approach of heat treating 17–4 PH stainless steel parts generated by Binder Jet Additive Manufacturing (BJAM) was developed. Age hardening of 17–4 PH usually consists of two steps: solution treatment followed by quenching and subsequent aging for precipitation hardening. For 17–4 PH, the solution treatment is done at 1050 °C for 30 min while the aging temperatures range from 480 °C to 760 °C with a duration of two to four hours. When using N2-atomized powder, BJAM of 17–4 PH followed by conventional H900 heat treatment results in an undesired reduction of hardness below 170 HV10 which is attributed to a microstructure displaying more than 30 vol% of retained austenite (RA). N originating from the powder atomization process stabilizes austenite and, therefore, suppresses the martensitic transformation during quenching down to room temperature. This contribution shows the effect of increasing the solution annealing time to max. 90 min as well as additional deep-cooling (DC) at −90 °C for 120 min on hardness, tensile properties, phase distribution and chemical composition of 17–4 PH specimens. By increasing the solution annealing time from 30 to 90 min and additional deep-cooling after quenching, the amount of RA can be reduced to less than 5%. In combination with conventional H900 aging, the hardness of the specimens increased well above 380 HV10, while over-aging (H1150M) caused the desired increase in ductility. The tensile properties achieved by the modified heat treatments involving prolonged solution annealing and deep-cooling, referred to as H900* and H1150M* in this study, are YS = 1081 ± 86, UTS = 1235 ± 9, A = 9.4 ± 3.3% and YS = 504 ± 18 MPa, UTS = 813 ± 20 MPa, A = 18.6 ± 1.3%, respectively.

A new process combination route consisting of additive manufacturing (AM) with a subsequent forming operation is proposed. The process route has the opportunity to increase the efficiency of the AM process route up to 360%. Stainless steel 316L sheets with different core structures (similar to sandwich sheets) are produced by AM, characterized, and formed in a die bending operation. The bending characteristics of this novel semi-finished product can be accurately predicted in a numerical simulation. The new process route is discussed in detail and compared to conventional AM parts in terms of the production efficiency., International journal of precision engineering and manufacturing;Vol. 9, 2022, Issue 4, pp 1021-1034

To evaluate the collection efficiency of water spray on the release of airborne composite particles during grinding of composite materials. Composite sticks (L:35 mm × W:5.4 mm × H:1.6 mm) of seven commercial dental composites were ground with a rough diamond bur (grain size 100 μm, speed 200,000 rpm). All experiments were performed in an enclosed 1-m3 chamber with low particulate background (< 1,000 #/cm3), and airborne particles were evaluated based on their electrical mobility. The number size distribution was determined by scanning mobility particle sizer (SMPS). Particles were collected by an electrostatic precipitator (ESP), and were ultramorphologically and chemically analyzed by a transmission electron microscope equipped with energy-dispersive X-ray spectroscopy (TEM-EDS). SMPS measurements confirmed that both dry and wet grinding generated high concentrations of nanoparticles particles with the highest concentration recorded during the last minute of grinding (1.80 × 106 − 3.29 × 106#/cm3), after which a gradual decline in particle concentration took place. Nevertheless, grinding with water spray resulted in a significant reduction of the number of released particles (5.6 × 105 − 1.37 × 106#/cm3). The smallest particle diameter was recorded during the last minute of grinding followed by a continuous growth for every next measurement. TEM of composite dust revealed a high concentration of particles varying in both size and shape. Regardless of whether the water cooling spray system was used during bur manipulation of composite materials, predominately nanoparticles were released. However, the particle concentrations were significantly decreased with water spray. Clinical relevance: Since water spray might not be sufficient in nanoparticle collection, special care should be taken to prevent inhalation of composite dust.

In this paper, we performed the numerical and experimental study of unsteady cavitation surge around a semi-circular leading-edge flat plate using a passive flow control method. We mounted a miniature spanwise wedge-type vortex generator on the suction side of the model close to its leading edge. To mitigate the destructive impact of this type of cavitation on the hydrofoil performance, we analyzed the effects of the passive control on the dynamics of cavitation surge. First, we investigated experimentally the unsteady cavitating flow around the semi-circular leading-edge flat plate without passive control using high-speed visualization, acoustic measurements and particle image velocimetry method. Next, we simulated numerically the dynamics of unsteady flow under the cavitation surge conditions with an open source code and validated the numerical results using the experimental data. We used a proper interaction between turbulence and cavitation model to capture a highly unsteady behavior of cavitation surge. Finally, we considered the effects of the passive control device on the mechanism of the cavitation surge instability. Our results revealed that using the passive control method, it is possible to stabilize the attached cavity on the suction side of the flat plate, to hinder the development of the spanwise instability of the attached cavity and to mitigate large-scale cavity structures. Furthermore, high-pressure pulsations in the wake region induced by unsteady cavitation surge were considerably reduced.

Sodium-ion batteries (NIBs) utilise cheaper materials than lithium-ion batteries (LIBs), and can thus be used in larger scale applications. The preferred anode material is hard carbon, because sodium cannot be inserted into graphite. We apply experimental entropy profiling (EP), where the cell temperature is changed under open circuit conditions. EP has been used to characterise LIBs; here, we demonstrate the first application of EP to any NIB material. The voltage versus sodiation fraction curves (voltage profiles) of hard carbon lack clear features, consisting only of a slope and a plateau, making it difficult to clarify the structural features of hard carbon that could optimise cell performance. We find additional features through EP that are masked in the voltage profiles. We fit lattice gas models of hard carbon sodiation to experimental EP and system enthalpy, obtaining: 1. a theoretical maximum capacity, 2. interlayer versus pore filled sodium with state of charge.

Fuel-rich operated HCCI engines are suitable for the polygeneration of work, heat, and base chemicals like synthesis gas (CO + H2). Under favorable conditions, these engines are exergetically more efficient than separate steam reformer and cogeneration gas engines. However, to achieve ignition, reactive fuel additives like dimethyl ether or ozone must be supplied, which have some, probably negative and not yet quantified, impacts on the exergetic efficiency.

The survivability of two thermographic phosphors, YAG:Pr3+ and SMP:Sn2+ ((Sr,Mg)3(PO4)2:Sn2+), in a combustion environment is studied in the post-flame regime of a premixed propane/air flame. While the laser-induced luminescence of YAG:Pr3+ can be exploited for in situ temperature measurements in the exhaust gas above the flame, there is no in situ detectable luminescence for SMP:Sn2+ for any reaction conditions within the stability limits of the flame. The phosphor particles are recaptured above the flame and ex situ analyzed for chemical or structural changes using microscopic analysis (SEM/EDX) and x-ray diffraction. The microscopic analysis of post-flame YAG:Pr3+ does not show any alteration, whereas morphology and chemical composition of SMP:Sn2+ have been modified upon passing through the reaction zone, which is responsible for the loss of its luminescence properties.

Surface patterning is a recent promising approach to promote performance of pressure-driven membranes in water treatment and desalination. Nevertheless, knowledge about foulant deposition mechanisms, especially at early stage of filtration, is still lacking. The applicability of particle imaging velocimetry to study fluid characteristics atop surface patterned thin-film composite membranes was investigated at different operating conditions. This work is an important first step toward reliable understanding of the impacts of topographical membrane surface modification on hydrodynamic conditions and foulant deposition mechanisms.

Catalyst layers (CL), as an active component of the catalyst coated membrane (CCM), form the heart of the proton electrolyte membrane fuel cell (PEMFC). For optimum performance of the fuel cell, obtaining suitable structural and functional characteristics for the CL is crucial. Direct tuning of the microstructure and morphology of the CL is non-trivial; hence catalyst inks as CL precursors need to be modulated, which are then applied onto a membrane to form the CCM. Obtaining favorable dispersion characteristics forms an important prerequisite in engineering catalyst inks for large scale manufacturing. In order to facilitate a knowledge-based approach for developing fuel cell inks, this work introduces new tools and methods to study both the dispersion state and stability characteristics, simultaneously. Catalyst inks were prepared using different processing methods, which include stirring and ultrasonication. The proposed tools are used to characterize and elucidate the effects of the processing method. Structural characterization of the dispersed particles and their assemblages was carried out by means of transmission electron microscopy. Analytical centrifugation (AC) was used to study the state and stability of the inks. Herein, we introduce new concepts, S score, and stability trajectory, for a time-resolved assessment of inks in their native state using AC. The findings were validated and rationalized using transmittograms as a direct visualization technique. The flowability of inks was investigated by rheological measurements. It was found that probe sonication only up to an optimum amplitude leads to a highly stable colloidal ink.

Recently, the energy market has seen a shift towards renewable energies due to changing demands. Gas turbines are used as a transitional technology to cope with grid fluctuations. The changing conditions have increased the interest in applying Wet Compression in order to increase the power output during peak demands. The novelty of this paper arises from the experimental results of Interstage Injection by analysing the stage and overall pressure ratios at different operating points in the four stage axial compressor “eco.MAC” (“evaporative cooling Multiphase Axial Compressor”). An innovative injection design is realized with twin jet nozzles in the trailing edge of SLM printed stator blades. A variation of water mass fraction, inlet temperature and rotational speed is performed and shows a gain in pressure ratio up to 1.5 %. Moreover, a polynomial approach is used for the dry data to compare wet and dry results at equal air mass flow rates. For the first time, a linear dependency of the pressure gain on the compressor’s gas temperature is experimentally found. It can be concluded that Interstage Injection is an effective technology to be applied in later stages of axial compressors due to the strong influence of local gas temperatures on the evaporation rate and thus the pressure gain. Furthermore, reducing the local injection rate decreases aerodynamic losses between the liquid and gas phase. Hence, a multiple injection and reduced local injection rates should be targeted.

Dry gas lubricated non-contacting mechanical seals (DGS) are acknowledged as the sophisticated shaft end sealing solution which is most commonly found in turbo-compressors. Especially under demanding conditions where high speed is combined with high pressure, DGS becomes the preferred choice over other sealing alternatives. A reliable operation of DGS, due to the non-contact running between its rotating and stationary rings, is secured by the gas film in the region of a few microns in thickness. This paper presents the measurement method of obtaining the thickness of the running gap in two radial positions, namely the inner and outer diameter of the sealing gap, by integrating the proximity sensors in the stationary ring. The experimental investigations concerning film thicknesses, pressure distributions in the gas film and axial vibrations are carried out in an industry DGS up to 50 bar and 10,000 rpm, whereby a good insight into the dynamic behaviour of the sealing gap is provided. The results demonstrate the practicability of obtaining the gas film parameters in a grooved gas seal, bridging the gap between theory and practice. In combination with the experimental work presented in this paper, the numerical model for simulating the seal performance programmed in MATLAB is compared and validated. The comparisons for various operating conditions and groove profiles are discussed with the focus lying on the hydrodynamic effect in the gas film.

The diffusive behavior of nanoparticles inside porous materials is attracting a lot of interest in the context of understanding, modeling, and optimization of many technical processes. A very powerful technique for characterizing the diffusive behavior of particles in free media is dynamic light scattering (DLS). The applicability of the method in porous media is considered, however, to be rather difficult due to the presence of multiple sources of scattering. In contrast to most of the previous approaches, the DLS method was applied without ensuring matching refractive indices of solvent and porous matrix in the present study. To test the capabilities of the method, the diffusion of spherical gold nanoparticles within the interconnected, periodic nanopores of inverse opals was analyzed. Despite the complexity of this system, which involves many interfaces and different refractive indices, a clear signal related to the motion of particles inside the porous media was obtained. As expected, the diffusive process inside the porous sample slowed down compared to the particle diffusion in free media. The obtained effective diffusion coefficients were found to be wave vector-dependent. They increased linearly with increasing spatial extension of the probed particle concentration fluctuations. On average, the slowing-down factor measured in this work agrees within combined uncertainties with literature data.

This work develops flamelet tabulation methods for solid fuel combustion with and without fuel-bound nitrogen based on computations in particle-laden counterflow flames. The proposed flamelet tabulation methods for NO prediction are evaluated for two different coal types. The results show that extracting the NO mass fraction from the flamelet library directly results in significant discrepancies in the studied fuel nitrogen-free flame, while reasonable predictions can be obtained by using the same method in the fuel-bound nitrogen flames for both coal types. In contrast, solving a transport equation for the NO mass fraction tends to improve the NO prediction. The NO concentration is well predicted by splitting the NO source term into a formation part and a rescaled consumption part. The best NO prediction is obtained by extracting the formation part and the rescaled consumption part with a modified reaction progress variable.