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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (43) (entfernen)
Non-linear optical emitters are promising materials for energy applications and biotechnologies. Solid-state multi-band emitters like lanthanide doped up-conversion nanoparticles (UCNPs) show excellent photostability, are excitable in the near infrared (NIR), and show emission bands from the UV to SWIR spectral regions. The optical properties of these materials strongly depend on the excitation power density, i.e., the number of photons absorbed per time interval. The upconversion (ΦUC) and downshifting quantum efficiencies (ΦDS) of these materials, the excitation power dependent population, and the deactivation dynamics are influenced by nanoparticle architecture, doping concentration, and the microenvironment. We studied the fundamental changes of the luminescence properties of ß-NaYF4 UCNPs doped with Yb3+ and Er3+ depending on size, different surroundings such as aqueous and organic media, and different surface chemistries. We obtained further insights into shelling procedures, FRET optimization, influence of doping concentration, and advantages of different sensitizer ions.
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
An alternative method for lithium isotope amount ratio analysis is proposed by combining atomic absorption spectrometry with spectra data analysis by machine leaning. It is based on the well-known isotope shift of around 15 pm for the electronic transition at wavelength 670.7845 nm which can be measured by a high-resolution continuum source atomic absorption spectrometer (HR-CS-AAS). For isotope amount ratio analysis, a scalable three boosting machine learning algorithm (XGBoost) was employed and calibrated with a set of samples with a 6Li isotope amount fraction ranging from 99% to 6%. The absolute Li isotope amount fractions of these calibration samples were previously measured by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) and used as ab-initio data for the machine learning algorithm. Validation of the machine leaning model was performed with two standard reference materials (LSVEC and IRMM-016). The procedure was employed for the isotope amount ratio determination of a set of stock chemicals (Li2CO3, LiNO3, LiCl, LiOH, and LiF) as well as a BAM candidate LiMNC cathode reference material. Achieved uncertainties are one order of magnitude higher than those obtained by MC-ICP-MS. This precision and accuracy is nonetheless sufficient to resolve natural occurring variations in Lithium isotope ratios. Also, the LiMNC material was analyzed by HR-CS-AAS with and without matrix purification. The results are comparable within statistical error.
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs.[1] Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
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.
Current challenges and objectives for non-invasive optical bioimaging are deep tissue penetration, high detection sensitivity, high spatial and temporal resolution, and fast data acquisition. A promising spectral window to tackle these challenges is the short-wave infrared (SWIR) ranging from 900 nm to 1700 nm where scattering, absorption, and autofluorescence of biological components are strongly reduced compared to the visible/NIR. At present, the best performing SWIR contrast agents are based on nanomaterials containing toxic heavy-metal ions like cadmium or lead, which raises great concerns for biological applications. Promising heavy-metal free nanoscale candidates are gold nanoclusters (AuNCs) and Ag2S nanoparticles (NPs). The photoluminescence (PL) of both types of nanomaterials is very sensitive to their size, composition of their surface ligand shell, and element composition, which provides an elegant handle to fine-tune their absorption and emission features and boost thereby the size of the signals recorded in bioimaging studies.
Aiming for the development of SWIR contrast agents with optimum performance, we dived deeper into the photophysical processes occurring in these nanomaterials, thereby exploring in depth how the environment, surface ligand composition, and the incorporation of transition metals influence the optical properties of AuNCs and Ag2S NPs. We observed a strong enhancement of the SWIR emission of AuNCs upon exposure to different local environments (in solution, polymer, and in the solid state). Addition of metal ions such as Zn2+ to Ag2S based NPs led to a strong PL enhancement, yielding PL quantum yields of about 10% and thus making them highly suitable for non-invasive deep imaging of vascular networks and 3D fluid flow mapping.
SWIR luminescent nanomaterials – key chemical parameters for bright probes for in vivo bioimaging
(2024)
A current challenge for studying physio-pathological phenomena and diseaserelated processes in living organisms with non-invasive optical bioimaging is the development of bright optical reporters that enable deep tissue penetration, a high detection sensitivity, and a high spatial and temporal resolution. The focus of this project are nanomaterials, which absorb and emit in the shortwave infrared (SWIR) between ~900–2500 nm where scattering, absorption, and autofluorescence of the tissue are strongly reduced compared to the visible and NIR.
The unique optoelectronic properties of semiconductor nanocrystals, also termed quantum dots (QDs), have led to many advances in optoelectronic devices, bioimaging, and biosensing. This strong potential in a wide range of applications sparked the interest for a better understanding of the QD formation mechanisms. Recent studies have shown that atomically defined, zero-dimensional magic-size clusters (MSCs) play a crucial role during the nucleation and growth of QDs. Thereby MSCs consist of discrete numbers of ions leading to narrow size distributions and thus narrow absorption peaks, which evolve in discrete steps from one stable size to the next. The formation of MSCs was found in the synthesis of II-VI and III-V QDs but only limited synthesis approaches are available for the synthesis of MSCs in single-ensemble form without coexistence of other-size QDs. These MSCs can further self-assemble into two- and three-dimensional hybrid structures using organic ligands like diamines, leading to enhanced photoluminescence properties and catalytic activities.
In this contribution, we present a synthesis strategy for the preparation of single-sized ZnSe MSCs. With a band gap of 2.7 eV and being an earth-abundant material, ZnSe QDs are interesting for light-emitting devices, blue-green lasers, photocatalysis, and fluorescence probes. In contrast to other studies, our approach is based on a one-pot heat-up synthesis and uses less toxic and dangerous zinc precursors (e.g. zinc stearate). Knowing that thiol-based ligands can alter the formation process of ZnSe QDs, we investigated the influence of 1-dodecanethiol on the ZnSe MSC formation using absorption spectroscopy, TEM, XPS, and XRD. By variation of the thiol ligand concentration and reaction temperature, we were able to synthesize two new ZnSe MSC sizes, the largest so far, by using easy-to-handle precursors.
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.
Functionalized nanomaterials (NM) with their unique size-dependent properties are of increasing relevance for current and future developments in various fields such as medical and pharmaceutical industry, computing, electronics or food and consumer products. The performance and safety of NM are determined by the sum of their intrinsic physicochemical properties.1 Besides other key parameters, the particle surface chemistry, which is largely controlled by the chemical nature and density of functional groups and ligands, must be considered for a better performance, stability, and processibility of NM, as well as their interaction with the environment. Thus, particle standards with well-designed surfaces and methods for functional group quantification can foster the sustainable development of functional and safe(r) NM.2 Here we provide a brief overview of the ongoing research in division Biophotonics to design tailored amorphous silica reference particles with bioanalytically relevant functional groups and ligands, for the development of standardized and validated surface functional group quantification methods.