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Paper des Monats
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Nanoparticles have gained increasing attention in recent years due to their potential and application in different fields including medicine, cosmetics, chemistry, and their potential to enable advanced materials. To effectively understand and regulate the physico-chemical properties and potential adverse effects of nanoparticles, validated measurement procedures for the various properties of nanoparticles need to be developed. While procedures for measuring nanoparticle size and size Distribution are already established, standardized methods for analysis of their surface chemistry are not yet in place, although the influence of the surface chemistry on nanoparticle properties is undisputed. In particular, storage and preparation of nanoparticles for surface analysis strongly influences the analytical results from various methods, and in order to obtain consistent results, sample preparation must be both optimized and standardized. In this contribution, we present, in detail, some standard procedures for preparing nanoparticles for surface analytics. In principle, nanoparticles can be deposited on a suitable substrate from suspension or as a powder. Silicon (Si) Wafers are commonly used as substrate, however, their cleaning is critical to the process. For sample preparation from suspension, we will discuss drop-casting and spin-coating, where not only the cleanliness of the substrate and purity of the suspension but also its concentration play important roles for the success of the preparation methodology.
For nanoparticles with sensitive ligand shells or coatings, deposition as powders is more suitable, although this method requires particular care in fixing the sample.
Due to the extremely high specific surface area of nanoparticles and corresponding potential for adsorption, the results of surface analysis can be highly dependent on the history of the particles, particularly regarding sample preparation and storage. The sample preparation method has, therefore, the potential to have a significant influence on the results. This report describes an interlaboratory comparison (ILC) with the aim of assessing which sample preparation methods for ToF-SIMS analysis of nanoparticles provided the most intra- and interlaboratory consistency and the least amount of sample contamination. The BAM reference material BAM-P110 (TiO2 nanoparticles with a mean Feret diameter of 19 nm) was used as a sample representing typical nanoparticles. A total of 11 participants returned ToF-SIMS data,in positive and (optionally) negative polarity, using sample preparation methods of “stick-and-go” as well as optionally “drop-dry” and “spin-coat.” The results showed that the largest sources of variation within the entire data set were caused by adventitious hydrocarbon contamination or insufficient sample coverage, with the spin-coating protocol applied in this ILC showing a tendency toward insufficient sample coverage; the sample preparation method or the participant had a lesser influence on results.
The lattice enthalpies and monotropic relationship of two dehydroepiandrosterone (DEHA) polymorphs (forms I and II) were evaluated through a combination of differential scanning calorimetry (DSC), isothermal solution microcalorimetry, and drop-sublimation Calvet microcalorimetry experiments. The standard molar enthalpy of transition between both forms was determined as ΔtrsHom (II→I, 298.15 K) = - 0.90 ± 0.07 kJ mol-1 and ΔtrsHom (II→I, 417.8 K) = - 1.7 ± 1.0 kJ mol- 1, from measurements of standard molar enthalpies of solution in dimethyl sulfoxide and enthalpies of fusion, respectively. Drop-sublimation Calvet microcalorimetry experiments on form I led to ΔsubHom (cr I, 298.15 K) = 132.0±3.3 kJ mol - 1. This result, when combined with the more precise ΔtrsHom (II→I) value obtained by solution calorimetry, afforded ΔsubHom (cr II, 298.15 K) = 131.1±3.3 kJ mol - 1. The overall data indicate that on enthalpic grounds form I is more stable than form II from 298.15 K up to fusion. This conclusion, and the fact that DSC experiments indicated that form I has also a considerably higher temperature fusion, namely, Tfus(cr I)= 422.5±0.2 K and Tfus(cr II) = 413.1±0.2 K, suggest that the two polymorphs are monotropically related.
Next-generation thermal management requires the development of low lattice thermal conductivity materials, as observed in ionic conductors. For example, thermoelectric efficiency is increased when thermal conductivity is decreased. Detrimentally, high ionic conductivity leads to thermoelectric device degradation. Battery safety and design also require an understanding of thermal transport in ionic conductors. Ion mobility, structural complexity, and anharmonicity have been used to explain the thermal transport properties of ionic conductors. However, thermal and ionic transport are rarely discussed in direct comparison. Herein, the ionic conductivity of Ag+ argyrodites is found to change by orders of magnitude without altering the thermal conductivity. Thermal conductivity measurements and two-channel lattice dynamics modeling reveal that the majority of Ag+ vibrations have a non-propagating diffuson-like character, similar to amorphous materials. It is found that high ionic mobility is not a requirement for diffuson-mediated transport. Instead, the same bonding and structural traits that can lead to fast ionic conduction also lead to diffuson-mediated transport. Bridging the fields of solid-state ionics and thermal transport, it is proposed that a vibrational perspective can lead to new design strategies for functional ionic conducting materials. As a first step, the authors relate the so-called Meyer-Neldel behavior in ionic conductors to phonon occupations.
One of the holy grails in chemistry is to reconstruct some of life’s functions with synthetic materials. In this contribution, we demonstrate that “simple” macromolecular architectures such as dendritic amphiphiles, Janus dendrimers, thermoresponsive and hybrid organic-inorganic (co)polymers enable to mimic some of the functions of proteins for biomineralization, natural bactericides, biological membranes or the stimuli-responsive cytoskeleton.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
Vesicles self-assembled in water from natural and synthetic phospholipids (liposomes), amphiphilic block copolymers (polymersomes), and more recently amphiphilic Janus dendrimers (dendrimersomes) -5 as hollow soft structures in the nano size regime have attracted increasing interest as they can mimic primitive and contemporary biological membranes, and can be configured into biomimetic nanocapsules with application in nanomedicine such as gene, proteins and drug carriers or theranostics.
Compared to other amphiphilic structures, the molecular structure of Janus dendrimers can be precisely controlled: by using the vast range of tools from organic chemistry their size, architecture, density, generation as well as the number of end groups of the individual dendrons can be modified as desired.
Unfortunately, the controlled production of supramolecular aggregates made thereof is still a challenging task. Conventional batch-based techniques such as the solvent injection method or the film hydration method typically go along with a lack of control over self assembly/mixing and thus over size, morphology and size distribution of the vesicles.
The micromixer technology is a promising method for the controlled preparation of supramolecular assemblies as it allows control of mixing at microscale level. In addition, such microfluidic systems benefit from a high mixing efficiency, a low mixing time as well as from a reproducible and continuous production of soft nanoparticles. Herein, we report on the microfluidic-controlled self-assembly of Janus dendrimers as dendrimersomes and the impact of the mixing parameters on the self-assembly process.
One of the holy grails in chemistry is to reconstitute some of life’s functions with or within synthetic materials. In this contribution, we demonstrate that “simple” macromolecular architectures such as dendritic amphiphiles, Janus dendrimers, thermoresponsive and hybrid organic-inorganic (co)polymers enable to mimic some of the functions of proteins for biomineralization, natural bactericides, biological membranes or the stimuli-responsive cytoskeleton.
One of the holy grails in chemistry is to reconstruct some of life’s functions within synthetic materials. In this contribution, we demonstrate that “simple” macromolecular architectures such as dendritic amphiphiles, Janus dendrimers, thermoresponsive and hybrid organic-inorganic (co)polymers enable to mimic some of the functions of proteins for biomineralization, natural bactericides, biological membranes or the stimuli-responsive cytoskeleton.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media with applications in the field of drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and/or 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications,but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or Ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and/or 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
UCST-type thermoresponsive polymers (i.e. that phase separate from solution upon cooling) present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol.
In this context, acrylamide-based monomers can be very useful building blocks for designing novel non-ionic UCST-type polymers because of their hydrophilic nature (with the appropriate side chain) and propensity to form hydrogen bonds. We will present our latest results on the UCST-type thermoresponsive behaviour of acrylamide- and/or 2,6-diaminopyridine-based homopolymers and copolymers in water or water/alcohol mixtures, and give some insights about the rational design of UCST polymers relying on H-bonding.
Clays are crucial mineral phases in Earth’s weathering engine, but we do not know how they form in surface environments under (near-)ambient pressures and temperatures. Most synthesis routes, attempting to give insights into the plausible mechanisms, rely on hydrothermal conditions, yet many geological studies showed that clays may actually form at moderate temperatures (<100 °C) in most terrestrial settings. Here, we combined high-energy X-ray diffraction, infrared spectroscopy, and transmission electron microscopy to derive the mechanistic pathways of the low-temperature (25–95 °C) crystallization of a synthetic Mg-clay, saponite. Our results reveal that saponite crystallizes via a two stage process: (1) a rapid (several minutes) coprecipitation where ∼20% of the available magnesium becomes incorporated into an aluminosilicate network, followed by (2) a much slower crystallization mechanism (several hours to days) where the remaining magnesium becomes gradually incorporated into the growing saponite sheet structure.
Equipping ZIF particles with a polyelectrolyte membrane provides functional groups at their interface, enabling further conjugations necessary for applications such as targeted drug delivery. Previous approaches to coat ZIF particles with polyelectrolytes led to surface corrosion of the template material. This work overcomes previous limitations by performing a Layer-by-Layer (LbL) polyelectrolyte coating onto ZIF-8 and ZIF-67 particles in nonaqueous environment. Using the 2-methylimidazolium salt of polystyrensulfonic acid instead of the acid itself and polyethyleneimine in methanol led to intact ZIF particles after polyelectrolyte coating. This was verified by electron microscopy. Further, zetapotential and atomic force microscopy measurements confirmed a continuous polyelectrolyte multilayer built up. The here reported adaption to the well-studied (LbL) polyelectrolyte selfassembly process provides a facile method to equip ZIF particles with a nanometer thin polyelectrolyte multilayer membrane.
While noncovalent interactions between graphene derivatives and biosystems are extensively studied, less knowledge about their covalent multivalent interactions at biointerfaces is available. Due to the affinity of boronic acids towards cis-diol bearing biosystems, graphene sheets with this functionality were synthesized and their covalent interactions with the bacteria and nematode were investigated. As expected, graphene platforms with boronic acid functionality were able to wrap bacteria and destroy it in a short time. Surprisingly, body of nematodes was ruptured and their viability decreased to 30% after 24 h incubation with the functionalized graphene sheets. Because of their antibacterial and antiparasitic activities as well as their ability for wound dressing, graphene platforms with the boronic acid functionality were further investigated for diabetic wound healing. In vivo experiments showed that graphene platforms are more efficient than the commercially available drug, phenytoin, and restore both infected and non-infected diabetic wounds in ten days. Taking advantage of their straightforward synthesis, strong interactions with different biosystems as well as their ability to heal diabetic wounds, the boronic Acid functionalized graphene sheets are promising candidates for a broad range of future biomedical applications.
Inhibition of respiratory viruses is one of the most urgent topics as underlined by different pandemics in the last two decades. This impels the development of new materials for binding and incapacitation of the viruses. In this work, we have demonstrated that an optimal deployment of influenza A virus (IAV) targeting ligand sialic acid (SA) on a flexible 2D platform enables its binding and wrapping around IAV particles. A series of 2D sialylated platforms consisting graphene and polyglycerol are prepared with different degrees of SA functionalization around 10%, 30%, and 90% named as G-PG-SAL, G-PG-SAM, and G-PG-SAH, respectively. The cryo-electron tomography (Cryo-ET) analysis has proved wrapping of IAV particles by G-PG-SAM.
A confocal-based colocalization assay established for these materials has offered the comparison of binding potential of sialylated and non-sialylated nanoplatforms for IAV. With this method, we have estimated the binding potential of the G-PG-SAM and G-PG-SAH sheets for IAV particles around 50 and 20 times higher than the control sheets, respectively, whereas the low functionalized G-PG-SAL have not shown any significant colocalization value.
Moreover, optimized G-PG-SAM exhibits high potency to block IAV from
binding with the MDCK cells.
Proton exchange membrane fuel cells (PEMFCs) are one of the most promising alternative green energy technologies that deliver high energy density without CO2 emissions. The proton conductivity of proton exchange membranes (PEM) contributes to the overall efficiency of a PEMFC. Materials being used as PEMs must exhibit high proton conductivity at the working conditions of the targeted PEMFC. To date, Nafion and Nafion-like polymers with acidic functionality are widely used as membrane materials due to their high proton conductivity in the range of 10-1 to 10-2 Scm-1 at higher relative humidity. However, these materials suffer from high costs, hazardous production process, and poor performance at high temperatures, limiting their versatility.
In this context, crystalline porous materials are recognized as promising proton conductors for the proton exchange membrane (PEM) in fuel cell technology, owing to their tunable framework structure. However, it is still challenging bulk synthesis for real-world applications of these materials. Herein, we present mechanochemical gram-scale synthesis of series of mixed ligand metal organic frameworks (MOFs) and metal hydrogen‐bonded organic frameworks (MHOFs) using phenylene diphosphonic acid and 1-hydroxyethylidene-1,1-diphosphonic acid with different bipyridyl type of ligands, respectively. In all cases, the existence of extensive hydrogen bonds with amphiprotic uncoordinated phosphonate hydroxyl and oxygen atoms, the frameworks exhibited high proton conductivity. The study demonstrates the potential of green mechanosynthesis for preparations of framework-based proton conducting materials in bulk scale for green energy generation.
Multidrug solids have a potential use to efficiently treat and control a superfluity of medical conditions.
To address the current drawbacks of drug development in R&D, it was targeted to achieve new pharmaceutical solid forms of fenamic acids having improved solubility and thermal stability. Subsequently, five new multicomponent solids consisting of three salt hydrates of trimethoprim (TMP) with mefenamic acid (TMP-MFA-H2O), tolfenamic acid (TMP-TFA-H2O) and flufenamic acid (TMP-FFA-H2O), and two cocrystals of sulfamethazine (SFZ) with flufenamic acid (SFZ-FFA) and niflumic acid (SFZ-NFA) were prepared by liquid assisted grinding. Looking at the structures of active pharmaceutical ingredient (API) molecules, it was quite expected that a wide range of supramolecular synthons would lead to cocrystallization.
New forms were characterized thoroughly by various solid-state techniques, including single crystal X-ray diffraction (SCXRD), which provided details of hydrogen bonding, molecular packing and interactions between drug and coformer. Kinetic solubility at pH 7.4 buffer study has been carried out and a comparison is made with respect to the parent drugs. A significant enhancement of NSAIDs solubility was observed in all salt hydrate systems of TMP. Thus with increasing physicochemical properties such as improved solubility further leads to the enhancement of bioavailability, which has implications to overcoming the formulation related problems of active pharmaceutical ingredients (APIs).
Mechanically flexible single crystals of molecular materials offer potential for a multitude of new directions in advanced materials design. Before the full potential of such materials can be exploited, insight into their mechanisms of action must be better understood. Such insight can be only obtained through synergistic use of advanced experimentation and simulation. We herein report the first detailed mechanistic study of elasto-plastic flexibility in a molecular solid. An atomistic origin for this mechanical behaviour is proposed through a combination of atomic force microscopy, μ-focus synchrotron X-ray diffraction, Raman spectroscopy, ab initio simulation, and computed elastic tensors. Our findings suggest that elastic and plastic bending are intimately linked and result from extensions of the same molecular deformations. The proposed mechanism bridges the gap between contested mechanisms, suggesting its applicability as a general mechanism for elastic and plastic bending in organic molecular crystals.
Crystalline molecular materials with mechanical flexibility are promising for technological development. This is particularly true for the development of advanced materials with optoelectronic and biomedical applications. While a growing number of mechanically flexible crystalline molecular materials are being reported,1 they remain scarce. At present, most discoveries are serendipitous, as limited design strategies are currently known. Amongst these strategies Desiraju et. al. suggested that elastic materials must contain herringbone structures.2 For plastic crystals, the so-called ‘shape-synthon’ strategy has been developed, in which weak non-covalent interactions are introduced into structures to facilitate mobility of molecules.3 This includes formation of slip planes. Generally, these models have performed very well at predicting and rationalizing the mechanical properties of new materials. Recently, however, a family of one-dimensional covalent networks (coordination polymers; CPs) has been described, which show mechanical elasticity. With drastically different structural chemistry, these systems do not seem to adhere to the currently established rules. Herein, we present the first such system: a plastically bendable crystal of a 1D CP, [Zn(-Cl)2(3,5-Cl2Py)2]n (where 3,5-Cl2Py = 3,5-dichloro pyridine). This CP crystallizes in a tetragonal, and can therefore be bent over two major faces to acute angles without fracturing. We conducted bending and indentation experiments to quantify the mechanical properties of the CP crystal. This was complimented by Vibrational (Raman and Terahertz) spectroscopy and theoretical calculations for deeper understanding of molecular level structural deformation.
Mechanical flexibility in single crystals of covalently bound materials is a fascinating and poorly understood phenomenon. We present here the first example of a plastically flexible one-dimensional (1D) coordination polymer. The compound [Zn(m-Cl)2(3,5-dichloropyridine)2]n is flexible over two crystallographic faces. Remarkably, the single crystal remains intact when bent to 1808. A combination of microscopy, diffraction, and spectroscopic studies have been used to probe the structural response of the crystal lattice to mechanical bending. Deformation of the covalent polymer chains does not appear to be responsible for the observed macroscopic bending. Instead, our results suggest that mechanical bending occurs by displacement of the coordination polymer chains. Based on experimental and theoretical evidence, we propose a new model for mechanical flexibility in 1D coordination polymers. Moreover, our calculations propose a cause of the different mechanical properties of this compound and a structurally similar elastic material
An airborne high repetition rate laser-induced plasma was applied as a versatile ambient ionization source for mass-spectrometric determinations of polar and nonpolar analytes in solution. The laser plasma was sustained between a home-built pneumatic nebulizer and the inlet capillary of an Orbitrap mass spectrometer. To maintain stable conditions in the droplet-rich spray environment, the plasma was directly fed by the fundamental output (λ = 1064 nm) of a current state-of-the-art diode-pumped solid-state laser. Ionization by the laser-driven plasma resulted in signals of intact analyte ions of several chemical categories. The analyte ions were found to be fully desolvated since no further increase in ion signal was observed upon heating of the inlet capillary. Due to the electroneutrality of the plasma, both positive and negative analyte ions could be formed simultaneously without altering the operational parameters of the ion source. While, typically, polar analytes with pronounced gas phase basicities worked best, nonpolar and amphoteric compounds were also detected. The latter were detected with lower ion signals and were prone to a certain degree of fragmentation induced during the ionization process. All the described attests the laser-induced microplasma by a good performance in terms of stability, robustness, sensitivity, and general applicability as a self-contained ion source for the liquid sample introduction.
Laser-induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any material upon irradiation of solids with intense laser radiation. Nowadays processing rates of up to m^2/min are enabling new industrial applications in medicine, optics, tribology, biology, etc. Depending on the specific type of LIPSS, their structural sizes typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, however, a vivid, controversial, and long-lasting debate has emerged during the last two decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter reorganization processes (distinctly after the laser irradiation). This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches.
Advances in ultrafast laser manufacturing: nanostructures, thin films, and scaling perspectives
(2024)
Advanced ultrafast laser technology is a rapidly growing field that currently enables many new industrial and scientific applications. During the last decades, this has been significantly driven by the availability of high-repetition-rate laser sources and novel beam delivery concepts. At the laser side, Moore’s law equally manifests for ultrafast laser technologies, since the average output power of such lasers doubles approximately every two years. This development is mainly driven by the increase of the pulse repetition rates of energetic laser pulses, currently enforcing the development of smart beam control and novel scanning strategies for preventing heat-accumulation and plasma-shielding effects during laser-based materials processing. This keynote presentation addresses the advantages, recent developments, and perspectives of laser processing with ultrashort laser pulses. A special focus is laid on the tailored structuring of thin films as well as the manufacturing and probing of sub-diffraction surface nanostructures – an ongoing race to extreme scales. Current limitations are identified and an outlook to future scaling perspectives will be provided.
Laser-Induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any material upon irradiation of solids with intense laser radiation. Nowadays, processing rates of up to m^2/min are enabling new industrial applications in medicine, optics, tribology, biology, etc. Depending on the specific type of LIPSS, their structural sizes typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, however, a controversial and vivid debate has emerged during the last two decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter reorganization processes, i.e. distinctly after the laser irradiation. This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches.
This presentation reviews current and expected developments in the field of laser-induced periodic surface structures (LIPSS, ripples). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized radiation. LIPSS are formed in a “self-ordered” way and are often accompanying laser material processing applications. The structures can be produced in a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their spatial periods typically range from several micrometers down to less than 100 nanometers, exhibiting a clear correlation with the polarization direction of the laser radiation used. Various types of LIPSS have been classified, relevant control parameters were identified, and material specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics, through time-resolved optical experiments and theoretical simulations. Special attention will be paid to a comparison of the currently available formation theories for LIPSS with a discussion of their respective strengths and weaknesses. Currrently explored applications featuring surface functionalization in the fields of optics, surface wetting, medicine, and tribology will be discussed.
During the past few years significantly increasing research activities in the field of laser-induced periodic surface structures (LIPSS, ripples) have been reported since the generation of LIPSS in a single-step process provides a simple way of surface nanostructuring towards a control of optical, mechanical or chemical surface properties. In this contribution the current research state in this field is reviewed. The formation of LIPSS upon irradiation of metals, semiconductors and dielectrics by multiple linearly polarized Ti:sapphire fs-laser pulses (30-150 fs) is studied experimentally and theoretically. Different types of LIPSS with periods even below 100 nm can be generated. Their dynamics and formation mechanisms are analyzed and identified in ultrafast optical experiments. Complementing theoretical calculations of the laser-induced carrier dynamics address transient changes of the optical properties of the irradiated materials and reveal the importance of surface plasmon polaritons in the early stage of LIPSS formation. Various applications of these nanostructures are outlined.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the femtosecond to picosecond range.
During the past few years significantly increasing research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical, biological, or chemical surface properties. In this contribution the mechanisms of formation and current applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting properties, the mimicry of the natural texture of animal integuments, the tailoring of surface colonization by bacterial biofilms, the advancement of medical pacemakers, and the improvement of the tribological performance of nanostructured metal surfaces.
Der Vortrag gibt einen Überblick über die vielfältigen Möglichkeiten der Oberflächenfunktionalisierung mittels Mikro- und Nanostrukturierung durch Ultrakurzpuls-Lasermaterialbeabeitung. Dies schließt eine Diskussion des Phänomens der Laser-induzierten periodischen Oberflächenstrukturen (LIPSS, engl.: Laser-induced Periodic Surface Structures, Ripples), sowie deren Klassifikation und Bildungsmechanismen mit ein. Ein Schwerpunkt der Präsentation liegt auf der Diskussion verschiedener Anwendungsmöglichkeiten der LIPSS in Bereichen der Optik, Fluidik, Tribologie und Medizin, sowie auf einem Ausblick auf die industrielle Skalierbarkeit der LIPSS-Technologie.
Ultrashort laser pulse micromachining features a high precision. By increasing the repetition rate of the applied laser to several 100 kHz, laser processing becomes quick and cost-effective and make this method attractive for industrial applications. Upon exceeding a critical laser intensity, hard X-ray radiation is generated as a side effect. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose becomes significant for high-repetition-rate laser systems so that radiation safety must be considered.
Laser-induced periodic surface structures (LIPSS) enable a large variety of different surface functionalizations for applications in the fields of optics, fluidics, tribology, or medicine. Moreover, high spatial frequency LIPSS (HSFL) provide an appealing and straightforward way for the generation of surface nanostructures featuring spatial periods even below 100 nm – far beyond the optical diffraction limit. However, the imposed surface functionalities are usually caused by both, topographic and chemical surface alterations. For exploring these effects in detail, multi-method characterization was performed here for HSFL processed on Ti-6Al-4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 1 – 400 kHz pulse repetition rate) under different scan processing conditions. The subsequent sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), stylus profilometry (SP), as well as near-surface chemical analyses by X-ray photoelectron spectroscopy (XPS), hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS). The results allow to qualify the laser ablation depth, the geometrical HSFL characteristics and provide detailed insights into the depth extent and the nature of the ps-laser-induced near-surface oxidation arising from the laser-processing in ambient air and into the relevance of heat-accumulation effects at high pulse repetition rates. Moreover, the direct comparison of the HAXPES and XPS data reveals the role of surface-covering organic contaminants adsorbed from the ambient atmosphere without ion-sputter depth profiling. Furthermore, reduction of the oxides by sputtering can be avoided.
Surfaces of metallic copper and copper alloys effectively inactivate microorganisms and viruses. However, the exact inactivation mode is still under debate. Main factors are assumed to include direct contact with the metallic surface, influx of Cu(I)/Cu(II) ions and the generation of reactive oxygen species (ROS). Laser-induced periodic surface structures (LIPSS) are frequently reported to act antibacterial, mainly by prevention of bacterial adhesion due to a limited number of possible adhesion points or by increasing the overall surface of intrinsically antibacterial materials. In time-kill experiments with E. coli and S. aureus we analyzed the impact of LIPSS on the toxicity of metallic copper and brass. We also conducted ROS accumulation assays and conclude that the application of LIPSS is not generally straight forward to obtain or improve antibacterial surfaces. Thus, the antibacterial effects of LIPPS.
Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the femtosecond to picosecond range. During the past years significantly increasing industrial and research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical, biological, or chemical surface properties. In this contribution the mechanisms of formation and current trends and applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting properties, the mimicry of the natural texture of animals, the tailoring of surface colonization by bacterial biofilms, the advancement of leadless medical pacemakers, and the improvement of the tribological performance of nanostructured metal surfaces.
Lasermaterialbearbeitung ist eine sich schnell entwickelnde Technologie, um eine Vielzahl von Oberflächenfunktionalitäten auf Basis optischer, mechanischer oder chemischer Eigenschaften zu realisieren. Die Verwendung ultrakurzer Laserimpulse mit Dauern im Femtosekundenbereich ermöglicht dabei neben einer herausragenden Bearbeitungs-präzision auch die selbstorganisierte Erzeugung verschiedener charakteristischer Ober-flächenstrukturen mit Größenskalen im Mikrometer- bis hinunter in den sub-100-nm-Bereich, z.B. sogenannte Ripples („Laser-Induced Periodic Surface Structures“, LIPSS), Grooves, oder Spikes.
In dem Vortrag wird ein Überblick über die in den vergangenen Jahren in Zusammenarbeit mit dem BAM Fachbereich 6.3 durchgeführten tribologischen Experimente gegeben. Besonderes Augenmerk liegt dabei auf den tribologischen Eigenschaften (Reibung und Verschleiß) der unterschiedlichen Femtosekunden-Laser-generierten Oberflächen-morphologien auf gängigen Metallen (z.B. Stahl, Titan). Einflüsse durch die Veränderungen der Härte des Werkstoffs infolge Laser-induzierter Oxidation, der Dicke und Struktur der Oxidschicht, und die Wirksamkeit unterschiedlicher Schmiermittel (z.B. additiviertes Motoröl) werden diskutiert.
This presentation reviews the current state in the field of Laser-induced Periodic Surface Structures (LIPSS). These surface nanostructures are a universal phenomenon and can be generated on almost any material by irradiation with intense linearly polarized laser radiation. LIPSS are formed in a “self-ordered” way and are often accompanying material processing applications. They can be produced following a single-step process and enable surface functionalization through the adaption of optical, mechanical and chemical surface properties. Their structural sizes typically range from several micrometers down to less than 100 nanometers exhibiting a clear correlation with the polarization direction of the laser radiation. Various types of surface structures are classified, relevant control parameters are identified, and their material specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics, through time-resolved optical experiments and theoretical simulations. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Laser-induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any type of solid upon irradiation with intense laser pulses. They represent a (quasi-)periodic modulation of the surface topography in the form of a linear grating and are typically formed in a “self-ordered” way in the focus of a laser beam. Thus, they are often accompanying laser material processing applications. The structural sizes of LIPSS typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation.
From a theoretical point of view, a controversial debate has emerged during the last decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter-reorganization processes (distinctly after the laser irradiation). From a practical point of view, however, LIPSS represent a simple and robust way for the nanostructuring of solids that allows creating a wide range of different surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc.
This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas behind the LIPSS, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches.
Fourth generation light sources, namely short wavelength, short pulse free electron lasers (FELs) are offering new and fascinating possibilities to resolve laser-induced structure formation at surfaces on the sub-micrometer to nanometer length scale and in temporal regimes ranging from picoseconds to several nanoseconds with sub-picosecond resolution. This unique spatio-temporal resolution allows to reveal early signatures of coherent/plasmonic electromagnetic scattering effects followed by the excitation of hydrodynamic capillary waves – providing new insights to the above-mentioned debate.
Finally, some unsolved scientific problems related to LIPSS are identified and the pending technological limitations are discussed. While the currently available laser and scanner technology already allows large area surface processing with rates at the m2/min level, industrial applications of LIPSS are sometimes limited by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. Strategies for overcoming such limitations are outlined.
Der Vortrag gibt einen Überblick über die Erzeugung und Charakterisierung anisotroper Nanostrukturen mittels ultrakurzgepulster Laserstrahlung. Besonderes Augenmerk liegt dabei auf dem Phänomen der sogenannten Laser-induzierten periodischen Oberflächen-Nanostrukturen auf dielektrischen Werkstoffen und ihrer zeitlichen Dynamik. Weitere Beispiele von Volumen-Nanostrukturen aus der Literatur werden diskutiert.
Laser-induced periodic surface structures (LIPSS) have gained remarkable attention as they represent a universal phenomenon that is often accompanying laser-processing. Such LIPSS enable a large variety of different surface functionalizations for applications in the fields of optics, fluidics, tribology, or medicine. Moreover, so-called “high spatial frequency LIPSS” (HSFL) provide an appealing and straightforward way for surface nanostructuring featuring spatial periods even below 100 nm – far beyond the optical diffraction limit. However, the imposed surface functionalities are usually caused by both, topographic and chemical surface alterations. For exploring these effects in detail, multi-method characterizations were performed here for HSFL on processed Ti- 6Al- 4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 1 – 400 kHz pulse repetition rate) under different laser and scan processing conditions. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), stylus profilometry (SP), and white light interference microscopy (WLIM), as well as near-surface chemical analyses by X-ray photoelectron spectroscopy (XPS), hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS). The results allow to qualify the laser ablation depth, the geometrical HSFL characteristics and provide detailed insights into the depth extent and the nature of the ps-laser-induced near-surface oxidation. Significance for medical applications will be outlined.
Laser-induced periodic surface structures (LIPSS) and their combination with self-ordered microstructures forming hierarchical Spikes enable a large variety of different surface functionalizations for applications in the fields of optics, fluidics, tribology, or medicine. Moreover, high spatial frequency LIPSS (HSFL) provide an appealing and straightforward way for surface nanostructuring featuring spatial periods even below 100 nm – far beyond the optical diffraction limit. However, the imposed surface functionalities are usually caused by both, topographic and chemical surface alterations. For exploring these effects in detail, multi-method characterizations were performed here for HSFL and hierarchical Spikes processed on Ti-6Al-4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ~1 ps pulse duration, 1 – 400 kHz pulse repetition rate) under different laser and scan processing conditions. The following sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), stylus profilometry (SP), and white light interference microscopy (WLIM), as well as near-surface chemical analyses by X-ray photoelectron spectroscopy (XPS), hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (TOF-SIMS). The results allow to qualify the laser ablation depth, the geometrical HSFL/Spikes characteristics and provide detailed insights into the depth extent and the nature of the ps-laser-induced near-surface oxidation arising from the laser-processing in ambient air and into the relevance of heat-accumulation effects at high pulse repetition rates. Moreover, the direct comparison of the HAXPES and XPS data reveals the role of surface-covering organic contaminants adsorbed from the ambient atmosphere without the uncertainties and potential sputter reduction potentially caused by ion-sputter depth profiling.
Irradiation of solid surfaces with intense ultrashort laser pulses represents a unique way of depositing energy into materials. It allows to realize states of extreme electronic excitation and/or very high temperature and pressure and to drive materials close to and beyond fundamental stability limits. As a consequence, structural changes and phase transitions often occur along unusual pathways and under strongly nonequilibrium conditions. Due to the inherent multiscale nature — both temporally and spatially—of these irreversible processes, their direct experimental observation requires techniques that combine high temporal resolution with the appropriate spatial resolution and the capability to obtain good quality data on a single pulse/event basis. In this respect, fourth-generation light sources, namely, short wavelength and short pulse free electron lasers (FELs), are offering new and fascinating possibilities. As an example, this talk will discuss the results of scattering experiments carried out at the FLASH free electron laser at DESY (Hamburg, Germany), which allowed us to resolve laser-induced structure formation at surfaces on the nanometer to submicron length scale and in temporal regimes ranging from picoseconds to several nanoseconds with sub-picosecond resolution. The current status and future perspectives in this field via exploiting the unique possibilities of these 4th-generation light sources will be discussed.
The presentation reviews the BAM activities in the field of surface processing by ultrashort laser pulses. A focus is laid on the generation of laser-induced periodic surface structures (LIPSS) which allow various surface functionalizations for applications in optics, tribology, liquid management, and medicine.
Laser-induced Periodic Surface Structures (LIPSS): Mechanisms, Applications, and unsolved Problems
(2022)
Laser-induced Periodic Surface Structures (LIPSS, ripples) are a universal phenomenon and can be generated in a contactless, single-step process on almost any type of solid upon irradiation with intense laser pulses. They represent a (quasi-)periodic modulation of the surface topography in the form of a linear grating and are typically formed in a “self-ordered” way in the focus of a laser beam. Thus, they are often accompanying laser material processing applications. The structural sizes of LIPSS typically range from several micrometers down to less than 100 nanometers – far beyond the optical diffraction limit – while their orientations exhibit a clear correlation with the local polarization direction of the laser radiation. From a theoretical point of view, a controversial debate has emerged during the last decades, whether LIPSS originate from electromagnetic effects (seeded already during the laser irradiation) – or whether they emerge from matter-reorganization processes (distinctly after the laser irradiation). From a practical point of view, however, LIPSS represent a simple and robust way for the nanostructuring of solids that allows creating a wide range of different surface functionalities featuring applications in optics, tribology, medicine, energy technologies, etc. While the currently available laser and scanner technology already allows surface processing rates at the m^2/min level, industrial applications of LIPSS are sometimes limited by the complex interplay between the nanoscale surface topography and the specific surface chemistry. This typically manifests in difficulties to control the processing of LIPSS and in limitations to ensure the long-term stability of the created surface functions. This presentation reviews the currently existent theories of LIPSS. A focus is laid on the historic development of the fundamental ideas behind the LIPSS, their corresponding mathematical descriptions and numerical implementations, along with a comparison and critical assessment of the different approaches. Moreover, some unsolved scientific problems related to LIPSS are identified and the pending technological limitations are discussed. Hereby, it is intended to stimulate further research and developments in the field of LIPSS for overcoming these limitations and for supporting the transfer of the LIPSS technology into industry
Nanotechnology and lasers are among the most successful and active fields of research and technology that have boomed during the past two decades. Many improvements are based on the controlled manufacturing of nanostructures that enable tailored material functionalization for a wide range of industrial applications, electronics, medicine, etc., and have already found entry into our daily life. One appealing approach for manufacturing such nanostructures in a flexible, robust, rapid, and contactless one-step process is based on the generation of laser-induced periodic surface structures (LIPSS). This Perspectives article analyzes the footprint of the research area of LIPSS on the basis of a detailed literature search, provides a brief overview on its current trends, describes the European funding strategies within the Horizon 2020 programme, and outlines promising future directions.
Different types of laser-generated surface structures, i.e., Laser-induced Periodic Surface Structures (LIPSS, ripples), Grooves, and Spikes are generated on titanium and Ti6Al4V surfaces by means of femtosecond (fs) laser scan processing (790 nm, 30 fs, 1 kHz) in ambient air. Morphological, chemical and structural properties of the different surface structures are characterized by various surface analytical techniques, including scanning electron microscopy (SEM), X-ray diffraction (XRD), Glow discharge optical emission spectroscopy (GD-OES), and depth-profiling Auger electron spectroscopy (AES). It is revealed that the formation of near-wavelength sized LIPSS is accompanied by the formation of a graded oxide extending several tens to a few hundreds of nanometers into depth. GD-OES performed on other superficial fs-laser generated structures produced at higher fluences and effective number of pulses per spot area such as periodic Grooves and irregular Spikes indicate even thicker graded oxide layers. These graded layers may be suitable for applications in prosthetics or tribology.
The role of electromagnetic scattering in the formation of laser-induced periodic surface structures
(2021)
Laser-induced periodic surface structures (LIPSS) are a universal phenomenon that is accompanying laser materials processing. These surface nanostructures pave a simple way for surface functionalization with numerous applications in optics, fluidics, tribology, medicine, etc. During the last decade remarkable experimental and theoretical improvements in understanding of their formation mechanisms were obtained - all pointing toward polarization-dependent energy deposition by absorption of optical radiation that is scattered at the surface roughness and interfering with the laser beam. This contribution reviews the current state-of-the-art on the role of electromagnetic scattering in the formation of LIPSS by ultrashort laser pulses. Special attention is drawn to recent finite-difference time-domain (FDTD) calculations that allow to visualize the radiation patterns formed in the vicinity of the sample surface and to the impact of a thin superficial laser-induced oxidation layer.
Die Reduktion von Reibung und Verschleiß in technischen Systemen bietet ein großes Potenzial zur Reduktion von CO2-Emissionen. Dieser Beitrag diskutiert die Erzeugung und tribologische Charakterisierung von Ultrakurzpuls-generierten Nano- und Mikrostrukturen auf Metallen (Stahl, Titan). Besonderes Augenmerk wird dabei auf die Rolle der laserinduzierten Oxidschicht im Zusammenspiel mit verschleißreduzierenden Additiven in ölbasierten Schmiermitteln gerichtet.