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Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors.
Self-mated magnesia stabilized zirconia (Mg-PSZ) ceramic sliding couples have been investigated at 100 N load (P0max= 1324 MPa) in oscillating sliding conditions in different humidity conditions in air and in hot steam. Temperatures have been varied up to 400 °C and pressures up to 6 bars. The results show that the wear behavior of MgO-ZrO2 under high Hertzian contact pressures is strongly dependent on temperature and is similar for both dry oscillating and oscillating in hot steam. However, although the evolution in wear rates on temperature is similar and the wear rates of MgO-ZrO2 plunged above 300 °C in hot steam and air by nearly three orders of magnitude, SEM micrographs revealed in hot steam at 400 °C smooth wear tracks. In contrast, hot steam enhanced the tribochemistry of self-mated alumina couples and reduced wear rates. Hot steam decreased the coefficients of friction of MgO-ZrO2 with increasing temperature, but not the wear rates.
Multi-principal element alloys (MPEAs) are gaining interest in corrosion and electrocatalysis research due to their electrochemical stability across a broad pH range and the design flexibility they offer. Using the equimolar CrCoNi alloy, we observe significant metal dissolution in a corrosive electrolyte (0.1 M NaCl, pH 2) concurrently with the oxygen evolution reaction (OER) in the transpassive region despite the absence of hysteresis in polarization curves or other obvious corrosion indicators. We present a characterization scheme to delineate the contribution of OER and alloy dissolution, using scanning electrochemical microscopy (SECM) for OER-onset detection, and quantitative chemical analysis with inductively coupled-mass spectrometry (ICP-MS) and ultraviolet visible light (UV-Vis) spectroscopy to elucidate metal dissolution processes. In-situ electrochemical atomic force microscopy (EC-AFM) revealed that the transpassive metal dissolution on CrCoNi is dominated by intergranular corrosion. These results have significant implications for the stability of MPEAs in corrosion systems, emphasizing the necessity of analytically determining metal ions released from MPEA electrodes into the electrolyte when evaluating Faradaic efficiencies of OER catalysts. The release of transition metal ions not only reduces the Faradaic efficiency of electrolyzers but may also cause poisoning and degradation of membranes in electrochemical reactors.
Biofuels including ethanol and biodiesel (FAME) represent a renewable fuel alternative to petroleum-derived transport fuels. The aim of this work was to study the interaction between high density polyethylene (HDPE) with permeation barriers in form of polyamide (PA) and fluorination, and biofuels such as E85 (fuel with 85 % ethanol), biodiesel and B10 (heating oil with 10 % biodiesel). 10 l jerrycans made of polyethylene with permeation barrier of PA were filled with E85 and biodiesel and exposed to temperatures of 20 °C and 40 °C for 5 years. Half of the 20 l jerrycans of HDPE for filling with B10 were fluorinated at the inner layer to prevent permeation before the exposure. Tensile properties were determined once a year, and FTIR-spectroscopy was used to evaluate possible changes.
The tensile properties tensile strength and breaking elongation of HDPE jerrycan cuttings with permeation barrier decreased, but not significantly, after immersion in E85, biodiesel and B10. The elasticity modulus of the polyethylene grades was especially reduced during exposure to E85.
The FTIR spectra of HDPE jerrycan cuttings with permeation barrier showed that immersion tests for five years with the test fuels at 20 °C and 40 °C did not lead to a decomposition of the permeation barriers.
Biofuels including ethanol and biodiesel (FAME) represent a renewable fuel alternative to petroleum-derived transport fuels. The aim of this work was to study the interaction between high density polyethylene (HDPE) with permeation barriers in form of polyamide (PA) and fluorination, and biofuels such as E85 (fuel with 85 % ethanol), biodiesel and B10 (heating oil with 10 % biodiesel). 10 l jerrycans made of polyethylene with permeation barrier of PA were filled with E85 and biodiesel and exposed to temperatures of 20 °C and 40 °C for 5 years. Half of the 20 l jerrycans of HDPE for filling with B10 were fluorinated at the inner layer to prevent permeation before the exposure. Tensile properties were determined once a year, and FTIR-spectroscopy was used to evaluate possible changes.
The tensile properties tensile strength and breaking elongation of HDPE jerrycan cuttings with permeation barrier decreased, but not significantly, after immersion in E85, biodiesel and B10. The elasticity modulus of the polyethylene grades was especially reduced during exposure to E85.
The FTIR spectra of HDPE jerrycan cuttings with permeation barrier showed that immersion tests for five years with the test fuels at 20 °C and 40 °C did not lead to a decomposition of the permeation barriers.
Tanks for heating oil made of polyethylene grades have been on the market since the early 1970s in Germany. Tank manufacturers recommend the replacement of the tanks after a period of 30 years due to guarantee safety. Polyethylene grades are subject to ageing by alteration of the properties during their life cycle. The degree of ageing and the nature of the degradation process mainly depend on the chemical degradation of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no results available on the long-term behavior of the polyethylene grades, especially after a service life of more than 30 years. The aim of this investigation was the determination of the factual degree of damage in comparison to the uncontaminated polyethylene grades. Material data of the used polyethylene grades are available because the BAM was the competent authority for the tests and expert reports for the approval of these tanks until the middle of the 1990s.
The determination of the Melt Flow Rate (MFR) and the Fourier Transmission IR Spectroscopy (FTIR) of tank sections from the bottom, the shell and the roof of 10 segregated heating oil storage tanks produced of polyethylene grades A and B were used as tests methods.
The MFR measurements of the tank sections showed differences in the values depending on the weight which was used (5 kg or 21.6 kg). A reduction of the MFR values was measured for most of the sections of tanks made of polyethylene grade B after a service life of the tanks of more than 30 years. This grade is mainly subject to the internal ageing by cross-linkages, increased degree of branched molecules and loss of the plasticizer, and to a lesser extent by oxidative degradation. The FTIR analysis, especially of tank sections of the bottom and the shell showed that the intensity of the CH2 asymmetric and symmetric stretching vibrations in the range: 2800 - 2900 cm-1 and the CH2 bending deformation vibration at 1400 cm-1 increased due chain scissions. The intensity of the carbonyl stretching vibration C=O at 1740 cm-1 is low. The carbonyl index characterizes the degree of oxidation.
Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, EDS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids were used to introduce functional groups for further conjugations. The common crosslinker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter was oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower non-specific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). A binding capacity of 1.8 mg IgG per gram of corundum powder was achieved. The advantages of corundum include the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, convenient handling, and flexible application.
Nonporous corundum powder was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices.The common crosslinker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter was oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). As a proof of concept, IgG was extracted with protein A from crude human plasma. The advantages of corundum include the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, convenient handling, and flexible application.
Physical adsorption at cryogenic temperature (cryoadsorption) is a reversible mechanism that can reduce the pressure of conventional compressed gas storage systems. Metal–organic framework (MOF) materials are remarkable candidates due to the combination of high specific surface area and density which, in some cases, provide a high volumetric storage capacity. However, such extensive use of MOFs for this application requires the selection of affordable structures, easy to produce and made from feasible metallic and organic components. Herein, we introduce a MOF database detailing the crystallographic and porous properties of 3600 existing MOFs made from industrially relevant metals and their organic composition. The comparison of the available minimum costs of linkers allowed the creation of a database to select affordable structures with high potential for volumetric hydrogen storage by cryoadsorption, considering their composition based on individual or mixed building blocks. A user interface, available online, facilitates the selection of MOFs based on the properties or names of structures and linkers.
The symmetry or structural stability of ABO3-type perovskite oxides depends largely on the size of ‘A’ and ‘B’ cations, which determines the material properties. The partial substitution of these cations may be used to tune these properties. The ionic sizes and valence states of the cations play an important role in improving the prop- erties of perovskite. In this study, the substitution of La3+ with Sr2+ with a larger ionic radius and Mn3+ with Fe3+ with a similar ionic radius favored both the crystal symmetry and the mixed ionic–electronic conductivity of the perovskite. Electrodes based on La0.7Sr0.3Mn0.5Fe0.5O3 (LSMFO55) exhibited a faradaic behavior with a specific capacity of 330 C g−1 (92 mAh g−1 ) at 12C rate, while this electrode maintained a capacity of 259 C g−1 at 240C (charge or discharge in 15 s). Additionally, exohedral carbon nano-onions (CNO) were introduced as a negative electrode to design an asymmetric hybrid supercapacitor (AHS) with a widened cell voltage. The use of CNO as a negative electrode in the AHS improved the rate capability drastically compared to the use of rGO. This device maintained a good energy density even at an extra-high charging rate (600C) owing to its outstanding rate capability. The high-rate performance of the LSMFO55//CNO AHS can be elucidated by successful fabrication with a mixed ionic–electronic conductive positive electrode and a CNO negative electrode. Tuning the electronic and ionic conductivities by cationic substitution and adopting an appropriate carbon-derived negative electrode (such as CNO) can provide a practical high-rate hybrid device using various perovskites.
Solubility data of carbon dioxide (CO2) in the two ionic liquids 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF4] and 1-butyl-3-methylimidazolium tetrachloroferrate [BMIM][FeCl4] at T = (273.15-413.15) K and pressures up to p = 4.5 MPa are presented. In Addition to the experiments, a literature review was done to compare the new results with published solubility data. The measurements were carried out using an isochoric method which operates in decrements of deltaT = 20 K within the investigated temperature range and at selected four different pressure steps ranging from a pressure p of around 4.5 MPa to around 0.5 MPa. The solubility of CO2 decreases in both ionic liquids with increasing temperatures. Within the p,T-range investigated, CO2 displayed a solubility in [BMIM][BF4] from a mole fraction x = 0.0117 and a corresponding molality m = 0.0526 mol/kg at T = 413.15 K and p = 0.417 MPa up to x = 0.4876 and m = 4.2094 mol/kg at T = 293.15 K and p = 4.349 MPa. The corresponding values for the solubility in [BMIM][FeCl4] start at a mole fraction x = 0.0268 and a corresponding molality m = 0.0818 mol/kg at T = 413.15 K and p = 0.443 MPa and end at x = 0.5126 and m = 3.1216 mol/kg at T = 293.15 K and p = 4.478 MPa. At a constant temperature, CO2 is better soluble in [BMIM][FeCl4] than in [BMIM][BF4] and the mean value of the solubility difference related to mole fraction x over the pressure range investigated amounts to about 4 % at T = 273.15 K and monotonously increases to about 92 % at T = 413.15 K. Henry's law constant as well as derived thermodynamic properties, such as the Gibbs energy of solvation, the enthalpy of solvation, the entropy of solvation, and the heat capacity of solvation, were calculated and discussed regarding the solute-solvent molecular interactions.
This work reports new experimental data on densities and viscosities of (CO2 + n-pentane) and (CO2 + n-hexane) mixtures at high pressures and temperatures. The densities were measured by a vibrating-tube densimeter with an expanded uncertainty (k = 2) smaller than 1.8 kg/m3 at six isotherms (from 273.15 K to 373.15 K), twelve pressures starting at 5 MPa up to 100 MPa, and at six CO2 molar compositions (from 0 to 0.6). The viscosities were measured by a vibrating-wire viscometer with the corresponding relative expanded uncertainty (k = 2) smaller than 0.016 at five isotherms (from 273.15 K to 373.15 K), twelve pressures (from 5 MPa up to 100 MPa), and at two CO2 molar compositions (0.1 and 0.3). The densities were fitted by the semiempirical Tammann-Tait equation for density data and the Vogel-Fulcher-Tammann (VFT) equation for viscosity data, respectively. The Groupe Européen de Recherches Gazières (GERG-2008) equation of state was also applied for modelling the densities. Over-all robustness and reliability of the Perturbed-Chain Statistical Association Fluid Theory (PC-SAFT) and its critical point-based modification (CP-PC-SAFT) were examined. Accuracies of the Modified Yarranton-Satyro (MYS) coupled with CP-PC-SAFT and the NIST Reference Fluid Thermodynamic and Transport Properties Database (REFPROP 10) in predicting the viscosities were evaluated.
Fused filament fabrication (FFF) is a material extrusion-based technique often used in desktop 3D printers. Polymeric filaments are melted and are extruded through a heated nozzle to form a 3D object in layers. The extruder temperature is therefore a key parameter for a successful print job but also one of the main emission driving factors as harmful pollutants (e.g., ultrafine particles) are formed by thermal polymer degradation. The awareness of potential health risks has increased the number of emission studies in the past years. However, studies usually refer their calculated emission data to the printer set extruder temperature for comparison purposes. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperature and found significant temperature deviations to the displayed set temperature among printer models. Our result shows that printing the same filament feedstocks with three different printer models and with identical printer set temperature resulted in a variation in particle emission of around two orders of magnitude. A temperature adjustment has reduced the variation to approx. one order of magnitude. Thus, it is necessary to refer the measured emission data to the actual extruder temperature as it poses a more accurate comparison parameter for evaluation of the indoor air quality in user scenarios or for health risk assessments.
The emission of ultrafine particles from small desktop Fused Filament Fabrication (FFF) 3D printers has been frequently investigated in the past years. However, the vast majority of FFF emission and exposure studies have not considered the possible occurrence of particles below the typical detection limit of Condensation Particle Counters and could have systematically underestimated the total particle emission as well as the related exposure risks. Therefore, we comparatively measured particle number concentrations and size distributions of sub-4 nm particles with two commercially available diethylene glycol-based instruments – the TSI 3757 Nano Enhancer and the Airmodus A10 Particle Size Magnifier. Both instruments were evaluated for their suitability of measuring FFF-3D printing emissions in the sub-4 nm size range while operated as a particle counter or as a particle size spectrometer. For particle counting, both instruments match best when the Airmodus system was adjusted to a cut-off of 1.5 nm. For size spectroscopy, both instruments show limitations due to either the fast dynamics or rather low levels of particle emissions from FFF-3D printing in this range. The effects are discussed in detail in this article. The findings could be used to implement sub-4 nm particle measurement in future emission or exposure studies, but also for the development of standard test protocols for FFF-3D printing emissions.
Fused filament fabrication (FFF) on desktop 3D printers is a material extrusion-based technique often used by educational institutions, small enterprises and private households. Polymeric filaments are melted and extruded through a heated nozzle to form a 3D object in layers. The extrusion temperature is therefore a key parameter for a successful print job, but also one of the main driving factors for the emission of harmful air pollutants, namely ultrafine particles and volatile organic gases, which are formed by thermal stress on the polymeric feedstock. The awareness of potential health risks has increased the number of emission studies in the past years. However, the multiplicity of study designs makes an objective comparison of emission data challenging because printer hardware factors such as the actual extruder temperature (TE) and also feedstockspecific emissions are not considered. We assume that across the market of commercial low- and mid-price FFF printers substantial deviations between actual and set extruder temperatures exist, which have a strong effect on the emissions and hence may bias the findings of exposure studies. In our last publication, we presented a standardized feedstock-specific emission test method and showed that for each investigated feedstock an increase in actual extruder temperature was accompanied by an increase in particle emissions (Tang and Seeger, 2022). Therefore, any systematic discrepancy between set and actual extruder temperature matters. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperatures at different heights. We found significant under- and overestimation of the actual extruder temperatures by the respective set temperatures in three commercial printers. This caused a broad variation of the measured total numbers of emitted particles (TP), even when the same feedstock was operated. For the determination of TP, we followed the DE-UZ 219 test guideline. In a second round we repeated the tests with all printers adjusted to exactly the same extruder temperatures, i.e., to TE=230°C for ABS and TE=210°C for PLA. All measurements were conducted in a 1 m³ emission test chamber. Particle emissions in the size range between 4 nm and 20 μm were detected. Printing on three different printer models without temperature adjustment resulted for each of the investigated feedstocks in a variation in TP of around two orders of magnitude. After temperature adjustment, this was substantially reduced to approx. one order of magnitude and hence minimizes the bias of printer hardware on the emissions. Our findings suggest that adjustment of the extruder temperature should be mandatory in emission testing standards. It also poses a more accurate benchmark and provides more reliable emission data for evaluation of indoor air quality or for health risk assessments. In addition, a proper temperature setting is in the interest of the user. Some commercial FFF printers may have a higher actual extruder temperature than displayed and unintended overheating may not only impair the print quality but may cause unnecessarily increased exposure to particle emissions.
Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability.
Twenty years ago, research involving ionic liquids was a minor field of interest, and only a few chemists and even fewer engineers were interested in salts with melting points near room temperature. In April 2000, the first NATO advanced research workshop on ionic liquids was held in Heraklion, Crete. The conference was the first international meeting devoted to ionic liquids and attracted most of the active researchers at that time. Following that meeting, activity in the field began to flourish and the first books and international conferences devoted to ionic liquids began to appear. By the end of 2018, more than 80,000 scientific papers had been published, and 17,000 patents were applied for in the field of ionic liquids! This book provides an overview of the current and emerging industrial applications of ionic liquids covering the core processes and products, the practical implementation and technical challenges involved, and the potential future directions for Research and development. The individual chapters were written by leading scientists in the field from industry and academia to address specific processes and products that are or will be soon commercialized. Examples include the use of a chloroaluminate ionic liquid as a next-generation alkylation catalyst to a new class of capillary gas chromatography (GC) columns with stationary phases based on ionic liquids. Over the past twenty years, there has been a growing realization that ionic liquids have moved from being mere academic curiosities to having genuine applications in fields as wide-ranging as advanced materials, biotechnology, catalysis, pharmaceuticals, renewable fuels, and sustainable energy. There are many optimistic indications that ionic liquids are on their way to becoming a commercial success story. This first book on “Commercial Applications of Ionic Liquids” provides over 50 applications that are either at the pilot scale or have been commercialized, which indicates that an exciting new chapter in the field of ionic liquids is about to begin!
The paramagnetic ionic liquid 1-butyl-3-methylimidazolium tetrachloroferrate [BMIM][FeCl4] was subject to multiple high-precision thermophysical property measurements under both ambient and high pressure. Density rho(p0,T) / kg m-3 and speed of sound u(p0,T) / m s-1 data at ambient pressure were recorded at temperatures T = (278.15 to 343.16) K using a DSA 5000 M combined vibrating tube densimeter and speed of sound analyser with a standard uncertainty of delta rho(p0,T) = ±0.001 kg m-3 and delta u(p0,T) = ±0.1 m s-1, respectively. High-pressure volumetric (p,rho,T) data were measured on an Anton Paar DMA HPM vibrating tube densimeter at T = (273.16 to 413.15) K and at pressures up to p = 140 MPa with an estimated experimental relative combined average percentage deviation (APD) of delta rho(p,T) / rho(p,T) = ±(0.01 to 0.08) %.
The specific isobaric heat capacity cp(p0,T) / J kg-1 K-1, a caloric property, was determined at T = (273.15 to 413.15) K with an uncertainty delta cp / cp = ±0.5 % using a Perkin Elmer Pyris 1 DSC differential scanning calorimeter. To gain knowledge of transport properties, the dynamic viscosity eta(p0,T) / mPa s at ambient pressure was recorded at T = (275.03 to 413.18) K by an Anton Paar SVM 3000 Stabinger viscometer and additionally an Anton Paar rheometer MCR 302 device with uncertainties of delta eta / eta = ±0.35 % and delta eta / eta = ±1 %, respectively.
The obtained data were first correlated by empirical polynomial equations of state and further processed by the application of classic thermodynamic potentials to determine isothermal compressibility kappa T(p,T) / MPa-1, isobaric thermal expansivity alpha p(p,T) / K-1, thermal pressure coefficient gamma(p,T) / MPa K-1, internal pressure pint(p,T) / MPa, specific heat capacity at constant pressure cp(p,T) / J kg-1 K-1 and at constant volume cv(p,T) / J kg-1 K-1, the difference of isobaric and isochoric heat capacity (cp–cv)(p,T) / J kg-1 K-1, speed of sound u(p,T) / m s-1 and ultimately isentropic exponent kappa s(p,T).
This work extends knowledge about the thermophysical properties of [BMIM][FeCl4] particularly to high temperatures and pressures.
Solubility data of carbon dioxide (CO2) in the ionic liquid 1-ethyl-3-methylimidazolium methanesulfonate [EMIM][CH3SO3] at T= (273.15 to 413.15) K and pressures up to p= 5.0 MPa are reported. The solubility measurements were carried out using an isochoric method which operates in decrements of ΔT = 20 K within the investigated temperature range and at selected four different pressure steps ranging froma pressure p of around 5.0 MPa down to around 0.4 MPa. The solubility of CO2 in the ionic liquid monotonously decreases with increasing temperatures at a constant pressure. Within the p,T-range investigated, CO2 displayed a solubility in [EMIM] [CH3SO3] from a mole fraction x= 0.0160 mol·mol−1 and a corresponding molality m = 0.0791 mol·kg−1 at T = 413.15 K and p =0.432 MPa up to x = 0.4049 mol·mol−1 and m = 3.2982 mol·kg−1 at T = 293.15 K and p = 4.577 MPa. Henry's law constant was calculated from the solubility data reported here, and literature data were reviewed for comparison. Additionally, thermodynamic state properties that can be derived from Henry's law constant, such as the Gibbs energy of solvation ΔsolG, the enthalpy of solvation ΔsolH, the entropy of solvation ΔsolS, and the heat capacity of solvation ΔsolCp, were calculated.