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Publications (82)
Accurate knowledge of size, density and composition of nanoparticles (NPs) is of major importance for their applications. In this work the hydrodynamic characterization of polydisperse core-shell NPs by means of analytical ultracentrifugation (AUC) is addressed. AUC is one of the most accurate techniques for the characterization of NPs in the liqui...
We demonstrate how a sophisticated data analysis methodology enables us to perform multiwavelength evaluations of dynamic rotor speed gradient experiments obtained by analytical ultracentrifugation equipped with a multiwavelength detector. Our data evaluation tool HDR-MULTIFIT allows for the accurate analysis of sedimentation coefficient distributi...
The worldwide trend in nanoparticle technology towards increasing complexity must be directly linked to more advanced characterization methods of size, shape and related properties, applicable to many different particle systems in science and technology. Available techniques for nanoparticle characterization are predominantly focused on size charac...
Analytical ultracentrifugation (AUC) has proven to be a powerful tool for the study of particle size distributions, particle shapes and interactions with high accuracy and unrevealed resolution. In this work we show how the analysis of sedimentation velocity data from the AUC equipped with a multiwavelength detector (MWL) can be used to gain an eve...
Analytical centrifugation (AC) is a powerful technique for the characterisation of nanoparticles in colloidal systems. As a direct and absolute technique it requires no calibration or measurements of standards. Moreover, it offers simple experimental design and handling, high sample throughput as well as moderate investment costs. However, the full...
Access to complex multidimensional property distributions of nanoparticle systems is indispensable for the understanding of their synthesis, processing and application in modern production technologies. Plasmonic gold nanorods are a system of particular interest due to their shape-dependent localized surface plasmon resonance. In this study, we sho...
Knowledge of the structure–property relationships of functional nanomaterials, including, for example, their size‐ and composition‐dependent photoluminescence (PL) and particle‐to‐particle variations, is crucial for their design and reproducibility. Herein, the Angstrom‐resolution capability of an analytical ultracentrifuge combined with an in‐line...
In the present study, the effective thermal conductivity λeff of nanofluids containing metal oxide nanoparticles with a chemisorbed organic shell was investigated experimentally and theoretically. The model systems synthesized by a continuous-flow hydrothermal method consist of cyclohexane as organic base fluid and dispersed nearly spherical cerium...
Semiconductor quantum dots (QDs) possess unique electronic and optical properties, making them promising candidates for applications in light emitting diodes (LEDs), solar cells, bioimaging, and photocatalysis. Precise control over their size, shape, and chemical and electronic structure is crucial to ensure the desired functional properties and op...
To tailor superparamagnetic iron oxide nanoparticles (SPIONs) to the specific needs of diverse application fields, it is essential to understand not only their intrinsic properties but also their interactions with each other. Theoretical models predicting/explaining the magnetization behavior of macroscopic samples containing millions of SPIONs are...
The integrity of proteins is a decisive factor in their functionality. However, during production and processing, the flexible biomolecules are frequently exposed to external mechanical stress and interact with different surfaces, both might affect their folding. Structural changes promote aggregation induced by hydrophobic interactions. Stress-tre...
Dr. Helmut Cölfen, an exceptional interdisciplinary scientist, mentor, colleague, and dear friend, passed away in November 2023 at the age of 58. His untimely departure is a profound loss for the fields of analytical ultracentrifugation, colloid, crystallization, and polymer research. This obituary pays tribute to Helmut, honoring his remarkable ac...
As nanoparticle syntheses on a large scale usually yield products with broad size and shape distributions, the properties of nanoparticle-based products need to be tuned after synthesis by narrowing the size and shape distributions or via the removal of undesired fractions. The development of property-selective classification processes requires a u...
An advanced design of the analytical ultracentrifuge with multiwavelength emission detection (MWE-AUC) is presented which offers outstanding performance concerning the spectral resolution and range flexibility as well as the quality of the data acquired. The excitation by a 520 nm laser is complemented with a 405 nm laser. An external spectrograph...
The large-scale synthesis of nanoparticles (NPs) with defined properties requires detailed understanding of the underlying formation mechanisms and kinetics. The formation mechanisms of bimetallic NPs are still not sufficiently understood due to the complex reaction chemistry, which makes the control of the supersaturation as the thermodynamic driv...
Abstract
Carbon nano-onions (CNOs) are a unique class of carbon nanomaterials, with a concentric fullerene-like structure and sp2-hybridized carbon atoms. Onions present high mechanical strength, good conductivity, the capability to intercalate alkali metals, showing promising applications in diverse fields, such as tribology, energy storage, and n...
The Stokes–Einstein–Sutherland (SES) equation is at the foundation of statistical physics, relating a particle's diffusion coefficient and size with the fluid viscosity, temperature, and the boundary condition for the particle‐solvent interface. It is assumed that it relies on the separation of scales between the particle and the solvent, hence it...
The analysis of ions and clusters by mobility-classified mass spectrometry provides information on the mobility of analytes in the drift gas and the analyte mass. Mass equivalent and mobility equivalent diameters of globular analytes, such as ions, poly(ethylene glycol) (PEG), and ionic liquid nanodroplets, can be correlated with good accuracy by t...
Despite great progress in the synthetic chemistry of InP QDs, a predictive model to describe their temporal formation is still missing. In this work, we introduce a population balance model incorporating liquid phase reactions, homogeneous nucleation and reaction-limited growth of InP supported with the highly reproducible and reliable experimental...
The formation mechanism of plasmonic gold nanoparticles (Au NPs) by fast NaBH4 induced reduction of the precursors is still under debate. In this work we introduce a simple method to access intermediate species of Au NPs by quenching the solid formation process at desired time periods. In this way, we take advantage of the covalent binding of gluta...
Most analytical techniques used to study the surface chemical properties of superparamagnetic iron oxide nanoparticles (SPIONs) are barely suitable for in situ investigations in liquids, where SPIONs are mostly applied for hyperthermia therapy, diagnostic biosensing, magnetic particle imaging or water purification. Magnetic particle spectroscopy (M...
The increasing complexity in particle science and technology requires the ability to deal with multidimensional property distributions. We present the theoretical background for multidimensional fractionations by transferring the concepts known from one dimensional to higher dimensional separations. Particles in fluids are separated by acting force...
Multidimensional particle properties determine the product properties in numerous advanced applications. Accurate and statistically meaningful measurements of complex particles and their multidimensional distributions are highly challenging but strongly needed. 2D particle size distributions of plasmonic nanoparticles of complex regular shape can b...
The Stokes-Einstein-Sutherland (SES) equation is at the foundation of statistical physics, relating a particle's diffusion coefficient and size with the fluid viscosity, temperature and the boundary condition for the particle-solvent interface. It is assumed that it relies on the separation of scales between the particle and the solvent, hence it i...
Metallic alloy nanoparticles (NPs) exhibit interesting optical, electrical and catalytic properties, dependent on their size, shape and composition. In particular, silver-gold alloy NPs are widely applied as model systems to better understand the syntheses and formation (kinetics) of alloy NPs, as the two elements are fully miscible. Our study targ...
In this study, we introduce a method for the simultaneous retrieval of two-dimensional size-composition distributions of noble metal Ag-Au alloy nanoparticles utilizing an analytical ultracentrifuge equipped with a multiwavelength extinction detector (MWL-AUC). MWL-AUC is used to measure coupled optical and sedimentation properties of the particles...
Protein-protein interactions are essential for the understanding of biological processes. Specific protein aggregation is an important aspect for many biological systems. In particular, electrostatic interactions play the key role for protein-protein interactions, as many amino acids have pH-dependent charge states. Moreover, protein dissociation i...
Colloidal stability of nanoparticle suspensions is fundamental to apply nanomaterials in functional devices and to develop new methodologies in nanoscience. Herein, a versatile method is described to disperse and stabilize various solids with technological applications in pharmaceutical industry, batteries and fuel cells, dye sensitized solar cells...
After spilling coffee, a tell-tale stain is left by the drying droplet. This universal phenomenon, known as the coffee ring effect, is observed independent of the dispersed material. However, for many technological processes such as coating techniques and ink-jet printing a uniform particle deposition is required and the coffee ring effect is a maj...
We present guidelines to estimate the effect of electrostatic repulsion in sedimenting dilute particle suspensions. Our results are based on combined Langevin dynamics and lattice Boltzmann simulations for a range of particle radii, Debye lengths and particle concentrations. They show a simple relationship between the slope K of the concentration-d...
Anisotropic nanoparticles offer considerable promise for applications but also present significant challenges in terms of their characterization. Recent developments in the electroless deposition of silver patches directly onto colloidal silica particles have opened up a simple and scalable synthesis method for patchy particles with tunable optical...
Different colloidal particle characterization methods are examined for their suitability to determine the particle size distribution of particles extracted from steels. Microalloyed steels are dissolved to extract niobium and titanium carbonitride particles that are important for the mechanical properties of these steels. Such particles have sizes...
Analytical centrifugation is a versatile technique for the quantitative characterization of colloidal systems including colloidal stability. The recent developments in data acquisition and evaluation allow the accurate determination of particle size, shape anisotropy and particle density. High precision analytical sedimentation is in particular sui...
In this work, a widely applicable routine to characterize the core, surface, stability, and optical properties of CdSe/CdS/ZnS core–shell–shell nanorods after multiple growth steps is established. First, size, shape, and shell thickness of the nanorods are characterized by transmission electron microscopy (TEM), analytical ultracentrifugation (AUC)...
We present guidelines to estimate the effect of electrostatic repulsion in sedimenting dilute particle suspensions. Our results are based on combined Langevin dynamics and lattice Boltzmann simulations for a range of particle radii, Debye lengths and particle concentrations. They show a simple relationship between the slope $K$ of the sedimentation...
Analytical centrifugation (AC) has recently shown great potential for the accurate determination of particle size distributions. The well‐established LUMiSizer(R) is customized by a new design allowing for higher rotor speeds, improved thermal insulation, and measurement cell assembly. The latter enables sedimentation analysis of nanoparticles (NPs...
The controlled aggregation of colloidal particles is not only a widespread natural phenomenon but also serves as a tool to design complex building blocks with tailored shape and functionalities. However, the quantitative characterization of such heteroaggregation processes remains challenging. Here, we demonstrate the use analytical centrifugation...
In this study, a new detector for multiwavelength emission analytical ultracentrifugation (MWE-AUC) is presented, which allows measuring size- or composition-dependent fluorescence properties of nanoparticle ensembles. Validation of the new setup is carried out via comparison to a benchtop photoluminescence spectrometer and the established extincti...
Brownian Dynamics (BD) has been applied as a comprehensive tool to model sedimentation and diffusion of nanoparticles in analytical ultracentrifugation (AUC) experiments. In this manuscript, we extend the BD algorithm by considering space-dependent diffusion and solvent compressibility. With this, the changes in the sedimentation and diffusion coef...
By combining analytical ultracentrifugation (AUC) in liquid phase and scanning mobility particle sizer (SMPS) in the gas phase, additional information on the particle size and morphology has been obtained for rigid particles. In this paper, we transfer this concept to soft particles, allowing us to analyze the size and molar mass of the short side...
This work highlights significant advancements in detector hardware and software for multiwavelength analytical ultracentrifugation (MWL-AUC) experiments, demonstrating improvement in both, the spectral performance and UV capabilities of the instrument. The hardware is an extension of the Open AUC MWL detector developed in academia and first introdu...
Hydrodynamic and thermodynamic non-ideality are important phenomena when studying concentrated and interacting systems in analytical ultracentrifugation (AUC). Here we present an extended Brownian Dynamics (BD) based algorithm which incorporates hydrodynamic and thermodynamic non-ideality. It can serve as an independent and versatile approach for t...
Knowledge about the size, density, shape and optical properties of nanoparticles (NPs) is of high importance for many processes due to the fact that product proper-ties are directly influenced by these parameters. So far, combined analysis of size and density or shape or the determination of size, density and shape dependent op-tical properties has...
Graphene oxide materials can be prepared in manifold synthesis approaches and allow for further post-functionalization to adopt the properties of the desired application. Small sized sheets with lateral dimensions on the 100 nm scale are e.g. beneficial for cell applications. Breakage of sheets by liquid phase processing is an ideal way to generate...
A combination of orthogonal measurement techniques is utilized in this study to predict the average lengths and diameters of colloidal nanorods. Sedimentation coefficient distributions and electrical mobility distributions obtained from analytical ultracentrifugation and a scanning mobility particle sizer, respectively, are used for the hydrodynami...
The hot injection technique for the synthesis of quantum dots (QDs) is a well-established and widely used method in the lab. However, scale-up rules do not exist. One reason is that in particular the role of process parameters like mixing on particle formation is largely unknown, as systematic examination of the latter is impossible for the laborio...
In colloidal semiconductor nanocrystal synthesis, many activities have been focused on the control over the mean particle size of the product. However, for device applications additional requirements apply, e.g. the necessity for a narrow particle size distribution (PSD). In the present work, we investigate the impact of reactor characteristics on...
In this study, it is demonstrated how Brownian dynamics (BD) simulations can be used as a comprehensive forward model for analytical ultracentrifugation (AUC) and analytical centrifugation experiments. BD simulations are a versatile alternative to the numerical solution of Lamm's equation. Time dependent concentration profiles can be accurately pre...
No abstract is available for this article.
We report an unsurpassed solution characterization technique based on analytical ultracentrifugation, which demonstrates exceptional potential for resolving particle sizes in solution with sub-nm resolution. We achieve this improvement in resolution by simultaneously measuring UV/Vis spectra while hydrodynamically separating individual components i...
Wir berichten über eine Weiterentwicklung auf Grundlage der analytischen Ultrazentrifugation, durch welche Partikelgrößen direkt in Lösung mit Sub-nm-Auflösung charakterisiert werden können. Erreicht wird diese Auflösung durch die simultane Messung von UV/Vis-Spektren, während die einzelnen Komponenten der Mischung hydrodynamisch aufgetrennt werden...
We discuss the use of carbon nanodots (CNDs) as sensitizers in mesoscopic solar cells. The CNDs are synthesized using a one-step, bottom-up microwave approach with citric acid, urea and formic acid as precursors in aqueous media. Their light harvesting capabilities are tuneable by adjusting the synthetic parameters. Comprehensive spectroscopic and...
The optical performance of an analytical ultracentrifuge equipped with a fiber-coupled detector is investigated with special emphasis on the influence of oil leakage on the long-term deep ultraviolet stability. Two strategies for enhanced optical performance are presented. The first includes regeneration of fiber transmittance under atmospheric con...
In the view of technical and medical applications we examined the effect of ultrasonication and ball milling of oxo-functionalized graphene bearing an almost intact carbon lattice (oxo-G) with respect to the lateral flake size reduction and defect formation in the carbon lattice for the first time. The energy input was screened for both methods and...
Assumption-free and in situ resolving of the kinetics of ligand binding to colloidal nanoparticles (NPs) with high time resolution is still a challenge in NP research. A unique concept of using spectra library and stopped-flow together with a "search best-match" Matlab algorithm to access the kinetics of ligand binding in colloidal systems is repor...
In this work we performed a detailed investigation of the photostability of bottom-up produced carbon nanodots (CDs) prepared from citric acid and urea by solvothermal synthesis. Analytical ultracentrifugation (AUC) reveals that the CDs have a hydrodynamic diameter < 1 nm and a very narrow size distribution. In the community it is widely assumed th...
Properties of small semiconductor nanoparticles (NPs) are strongly governed by their size. Precise characterization is a key requirement for tailored dispersities and thus for high-quality devices. Results of a careful analysis of particle size distributions (PSDs) of ZnO are presented combining advantages of UV/Vis absorption spectroscopy, analyti...
In this work we investigated fundamental properties of CuInS2 quantum dots in dependence of the particle size distribution (PSD). Size-selective precipitation (SSP) with acetone as poor solvent was performed as an adequate post-processing step. Our results provide deep insight into the correlation between particle size and various optical character...
A scalable industrial method for graphene and Few-Layer-Graphene (FLG) production by graphite delamination in N-methylpyrrolidone and water-surfactant mixtures using a high pressure homogenizer is presented. This paper is focused on processing conditions and extensive subsequent analysis of the delaminated products by a combination of Analytical Ul...
We report the characterization of carbon nanodots (CND) synthesized under mild and controlled conditions, that is, in a microwave reactor. The CNDs thus synthesized exhibit homogeneous and narrowly dispersed optical properties. They are thus well suited as a testbed for studies of the photophysics of carbon-based nanoscopic emitters. In addition to...
In this paper, a method to determine the lateral dimensions of 2D nanosheets directly in suspension by analytical ultracentrifugation (AUC) is shown. The basis for this study is a well-characterized and stable dispersion of graphene oxide (GO) monolayers in water. A methodology is developed to correlate the sedimentation coefficient distribution me...
The surface chemistry of ions, water molecules, and proteins as well as their ability to form stable networks in foams can influence and control macroscopic properties such as taste and texture of dairy products considerably. Despite the significant relevance of protein adsorption at liquid interfaces, a molecular level understanding on the arrange...
Mixed self-assembled monolayers (SAM) of alkyl phosphonic acids and C60 functionalized octadecyl phosphonic acids (C60C18–PA) are deposited on alumina substrates from solution and are shown to form well-ordered structures with an insulating layer of alkyl chains and a semiconducting layer that comprises mainly C60. Such an ordered structure is a ne...
