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Organisationseinheit der BAM
- 6 Materialchemie (52) (entfernen)
Paper des Monats
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Bulk metallic glasses (BMG) are amorphous metal alloys known for their unique physical and mechanical properties. In the present study, the formation of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on the Zr-based BMGs Zr46Cu46Al8, Zr61Cu25Al12Ti2, Zr52.5Cu17.9Al10Ni14.6Ti5 (Vit105) and Zr57Cu15.4Al10Ni12.6Nb5 (Vit106) was investigated as a function of their different chemical composition. For this purpose, LIPSS were generated on the sample surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz). The surface topography was characterized by scanning electron microscopy and atomic force microscopy. Moreover, the impact of LIPSS formation on the structure and chemical surface composition was analyzed before and after fs-laser irradiation by X-ray diffraction and X-ray photoelectron spectroscopy as well as by transmission electron microscopy in combination with energy dispersive X-ray spectroscopy. Despite the different chemical composition of the investigated BMGs, the fs-laser irradiation resulted in almost similar properties of the generated LIPSS patterns. In the case of Zr61Cu25Al12Ti2, Vit105 and Vit106, the surface analysis revealed the preservation of the amorphous state of the materials during fs-laser irradiation. The study demonstrated the presence of a native oxide layer on all pristine BMGs. In addition, fs-laser irradiation results in the formation of laser-induced oxide layers of larger thickness consisting of an amorphous ZrAlCu-oxide. The precise laser-structuring of BMG surfaces on the nanoscale provides a versatile alternative to thermoplastic forming of BMG surfaces and is of particular interest for the engineering of functional material surfaces.
We investigate the periodic structure formation upon intense femtosecond pulsed irradiation of chrome steel (100Cr6) for linearly polarised laser beams. The underlying physical mechanism of the laser-induced periodic structures is explored, their spatial frequency is calculated and theoretical results are compared with experimental observations. The proposed theoretical model comprises estimations of electron excitation, heat transfer, relaxation processes, and hydrodynamics-related mass transport. Simulations describe the sequential formation of sub-wavelength ripples and supra-wavelength grooves. In addition, the influence of the laser wavelength on the periodicity of the structures is discussed. The proposed theoretical investigation offers a systematic methodology towards laser processing of steel surfaces with important applications.
The exciting properties of micro- and nano-patterned surfaces found in natural species hide a virtually endless potential of technological ideas, opening new opportunities for innovation and exploitation in materials science and engineering. Due to the diversity of biomimetic surface functionalities, inspirations from natural surfaces are interesting for a broad range of applications in engineering, including phenomena of adhesion, friction, wear, lubrication, wetting phenomena, self-cleaning, antifouling, antibacterial phenomena, thermoregulation and optics. Lasers are increasingly proving to be promising tools for the precise and controlled structuring of materials at micro- and nano-scales. When ultrashort-pulsed lasers are used, the optimal interplay between laser and material parameters enables structuring down to the nanometer scale. Besides this, a unique aspect of laser processing technology is the possibility for material modifications at multiple (hierarchical) length scales, leading to the complex biomimetic micro- and nano-scale patterns, while adding a new dimension to structure optimization. This article reviews the current state of the art of laser processing methodologies, which are being used for the fabrication of bioinspired artificial surfaces to realize extraordinary wetting, optical, mechanical, and biological-active properties for numerous applications. The innovative aspect of laser functionalized biomimetic surfaces for a wide variety of current and future applications is particularly demonstrated and discussed. The article concludes with illustrating the wealth of arising possibilities and the number of new laser micro/nano fabrication approaches for obtaining complex high-resolution features, which prescribe a future where control of structures and subsequent functionalities are beyond our current imagination.
X-ray emission hazards from ultrashort pulsed laser material processing in an industrial setting
(2021)
Interactions between ultrashort laser pulses with intensities larger than 10^13 W/cm^2 and solids during material processing can lead to the emission of X-rays with photon energies above 5 keV, causing radiation hazards to operators. A framework for inspecting X-ray emission hazards during laser material processing has yet to be developed. One requirement for conducting radiation protection inspections is using a reference scenario, i.e., laser settings and process parameters that will lead to an almost constant and high level of X-ray emissions. To study the feasibility of setting up a reference scenario in practice, ambient dose rates and photon energies were measured using traceable measurement equipment in an industrial setting at SCHOTT AG. Ultrashort pulsed (USP) lasers with a maximum average power of 220 W provided the opportunity to measure X-ray emissions at laser peak intensities of up to 3.3 × 10^15 W/cm^2 at pulse durations of ~1 ps. The results indicate that increasing the laser peak intensity is insufficient to generate high dose rates. The investigations were affected by various constraints which prevented measuring high ambient dose rates. In this work, a list of issues which may be encountered when performing measurements at USP-laser machines in industrial settings is identified.
The study of laser-fabricated periodic nanostructures is one of the leading topics of today’s photonics research. Such structures on the surface of metals, semiconductors, dielectrics, or polymers can generate new material properties with special functionalities. Depending on the specific material parameters and the morphology of the structures, new devices such as microlasers, optical nanoswitches, optical storage devices, sensors or antifraud features can be realized. Furthermore, laser-generated surface textures can be used to improve the tribological properties of surfaces in contact and in relative motion—to reduce friction losses or wear, to modify the wettability or the cell and biofilm growth properties of surfaces through bioinspired laser engineering, for emerging medical applications, or as decoration elements for the refinement of precious goods.
This Special Issue “Laser-Generated Periodic Nanostructures” focuses on the latest experimental and theoretical developments and practical applications of laser-generated periodic structures that can be generated in a “self-organized” way (laser-induced periodic surface structures, LIPSS, ripples) or via laser interference-based direct ablation (often referred to as direct laser interference patterning, DLIP). We aimed to attract both academic and industrial researchers in order to collate the current knowledge of nanomaterials and to present new ideas for future applications and new technologies. By 8 August 2021, 22 scientific articles have been published in the Special Issue, see www.mdpi.com/journal/nanomaterials/special_issues/laser-generated_periodic.
Bacterial biofilms pose serious problems in medical and industrial settings. One of the major societal challenges lies in the increasing resistance of bacteria against biocides used in antimicrobial treatments, e.g., via overabundant use in medicine, industry, and agriculture or cleaning and disinfection in private households. Hence, new efficient bacteria-repellent strategies avoiding the use of biocides are strongly desired. One promising route to achieve bacteria-repellent surfaces lies in the contactless and aseptic large-area laser-processing of technical surfaces. Tailored surface textures, enabled by different laser-processing strategies that result in topographic scales ranging from nanometers to micrometers may provide a solution to this challenge. This article presents a current state-of-the-art review of laser-surface subtractive texturing approaches for controlling the biofilm formation for different bacterial strains and in different environments. Based on specific properties of bacteria and laser-processed surfaces, the challenges of anti-microbial surface designs are discussed, and future directions will be outlined.
In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced.
Micro-concentrator solar cells offer an attractive way to further enhance the efficiency of planar-cell technologies while saving absorber material. Here, two laser-based bottom-up processes for the fabrication of regular arrays of CuInSe2 and Cu(In,Ga)Se2 microabsorber islands are presented, namely one approach based on nucleation and one based on laser-induced forward transfer.
Additionally, a procedure for processing these microabsorbers to functioning micro solar cells connected in parallel is demonstrated. The resulting cells show up to 2.9% efficiency and a significant efficiency enhancement under concentrated Illumination.
Spatial Period of Laser-Induced Surface Nanoripples on PET Determines Escherichia coli Repellence
(2021)
Bacterial adhesion and biofilm formation on surfaces are associated with persistent microbial contamination, biofouling, and the emergence of resistance, thus, calling for new strategies to impede bacterial surface colonization. Using ns-UV laser treatment (wavelength 248 nm and a pulse duration of 20 ns), laser-induced periodic surface structures (LIPSS) featuring different submicrometric periods ranging from ~210 to ~610 nm were processed on commercial poly(ethylene terephthalate) (PET) foils. Bacterial adhesion tests revealed that these nanorippled surfaces exhibit a repellence for E. coli that decisively depends on the spatial periods of the LIPSS with the strongest reduction (~91%) in cell adhesion observed for LIPSS periods of 214 nm. Although chemical and structural analyses indicated a moderate laser-induced surface oxidation, a significant influence on the bacterial adhesion was ruled out. Scanning electron microscopy and additional biofilm studies
using a pili-deficient E. coli TG1 strain revealed the role of extracellular appendages in the bacterial repellence observed here.
Nickel tungsten alloy tapes (Ni—5 at% W, 10 mm wide, 80 µm thick, biaxially textured) used in second-generation high temperature superconductor (2G-HTS) technology were laser-processed in air with ultraviolet ps-laser pulses (355 nm wavelength, 300 ps pulse duration, 250–800 kHz pulse repetition frequency). By employing optimized surface scan-processing strategies, various laser-generated periodic surface structures were generated on the tapes. Particularly, distinct surface microstructures and nanostructures were formed. These included sub-wavelength-sized highly-regular hexagonally-arranged nano-protrusions, wavelength-sized line-grating-like laser-induced periodic surface structures (LIPSS, ripples), and larger irregular pyramidal microstructures. The induced surface morphology was characterized in depth by electron-based techniques, including scanning electron microscopy (SEM), electron back scatter diffraction (EBSD), cross-sectional transmission electron microscopy (STEM/TEM) and energy dispersive X-ray spectrometry (EDS). The in-depth EBSD crystallographic analyses indicated a significant impact of the material initial grain orientation on the type of surface nanostructure and microstructure formed upon laser irradiation. Special emphasis was laid on high-resolution material analysis of the hexagonally-arranged nano-protrusions. Their formation mechanism is discussed on the basis of the interplay between electromagnetic scattering effects followed by hydrodynamic matter re-organization after the laser exposure. The temperature stability of the hexagonally-arranged nano-protrusion was explored in post-irradiation thermal annealing experiments, in order to qualify their suitability in 2G-HTS fabrication technology with initial steps deposition temperatures in the range of 773–873 K.
Laser-induced periodic surface structures (LIPSS) represent a unique route for functionalizing materials through the fabrication of surface nanostructures. Commercial AISI 316L stainless steel (SS316L) surfaces are laser treated by ultraviolet 300 ps laser pulses in a laser line scanning (LLS) approach. Processing parameters are optimized (pulse energy of 2.08 µJ, pulse repetition frequency of 300 kHz, and suitable laser scan and sample displacement rates) for the generation of low spatial frequency LIPSS over a large 25 × 25 mm2 area. Different angles of incidence of the laser radiation (0°, 30°, and 45°) and different linear laser beam polarizations (s and p) produce a plethora of rippled surface morphologies at distinct grains. Scanning electron microscopy and 2D Fourier transforms, together with calculations of the optical energy deposited at the treated surfaces using Sipe's first-principles electromagnetic scattering theory, are used to study and analyze in detail these surface morphologies. Combined with electron backscattering diffraction, analyses allow associating site-selectively various laser-induced-surface morphologies with the underlying crystalline grain orientation. Resulting grain orientation maps reveal a strong impact of the grain crystallographic orientation on LIPSS formation and point toward possible strategies, like multi-step processes, for improving the manufacturing of LIPSS and their areal coverage of polycrystalline technical materials.
The formation of gratings on the surface of a silicon wafer by nanosecond laser irradiation through a phase mask using an ArF laser emitting at 193 nm is studied. The phase mask along with some focusing optics is capable to generate via interference a periodic intensity distribution, which can be used for surface patterning. The surface patterning strongly depends on the laser energy density and on the number of pulses, as revealed by atomic force microscopy (AFM). The results show that irradiation even with a single laser pulse produces periodic depth modulations on the surface. The spatial surface modulation is in the micrometer (1.7 µm) range while the depth modulation is in the nanometer regime (1–20 nm). With an increasing number of pulses (1–100), the depth modulation amplitude increases smoothly. Increasing the number of pulses further results in the progressive destruction of the grating, vanishing completely after ~5000 pulses. This evolution is also monitored in situ by measuring the intensity of the first order-diffracted probe beam and the behavior is in accordance with what is observed by AFM. Finally, we qualitatively explain the results invoking thermally induced effects in the melted Si: these physical processes involved are probably thermocapillary and/or Marangoni effects inducing material displacement as the surface melts.
Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects.
Hierarchical micro/-nanostructures were produced on polycarbonate polymer surfaces by employing a two-step UV-laser processing strategy based on the combination of Direct Laser Interference Patterning (DLIP) of gratings and pillars on the microscale (3 ns, 266 nm, 2 kHz) and subsequently superimposing Laser-induced Periodic Surface Structures (LIPSS; 7–10 ps, 350 nm, 100 kHz) which adds nanoscale surface features. Particular emphasis was laid on the influence of the direction of the laser beam polarization on the morphology of resulting hierarchical surfaces. Scanning electron and atomic force microscopy methods were used for the characterization of the hybrid surface structures. Finite-difference time-domain (FDTD) calculations of the laser intensity distribution on the DLIP structures allowed to address the specific polarization dependence of the LIPSS formation observed in the second processing step. Complementary chemical analyzes by micro-Raman spectroscopy and attenuated total reflection Fourier-transform infrared spectroscopy provided in-depth information on the chemical and structural material modifications and material degradation imposed by the laser processing. It was found that when the linear laser polarization was set perpendicular to the DLIP ridges, LIPSS could be formed on top of various DLIP structures. FDTD calculations showed enhanced optical intensity at the topographic maxima, which can explain the dependency of the morphology of LIPSS on the polarization with respect to the orientation of the DLIP structures. It was also found that the degradation of the polymer was enhanced for increasing accumulated fluence levels.
In this paper, the influence of the bulk temperature (BT) of Polycarbonate (PC) on the occurrence and growth of Laser-induced Periodic Surface Structures (LIPSS) is studied. Ultrashort UV laser pulses with various laser peak fluence levels F_0 and various numbers of overscans (N_OS) were applied on the surface of pre-heated Polycarbonate at different bulk temperatures. Increased BT leads to a stronger absorption of laser energy by the Polycarbonate. For N_OS < 1000 High Spatial Frequency LIPSS (HSFL), Low Spatial Frequency LIPSS perpendicular (LSFL-I) and parallel (LSFL-II) to the laser polarization were only observed on the rim of the ablated tracks on the surface but not in the center of the tracks. For N_OS ≥ 1000 , it was found that when pre-heating the polymer to a BT close its glass transition temperature (T_g), the laser fluence to achieve similar LIPSS as when processed at room temperature decreases by a factor of two. LSFL types I and II were obtained on PC at a BT close to T_g and their periods and amplitudes were similar to typical values found in the literature. To the best of the author’s knowledge, it is the first time both LSFL types developed simultaneously and consistently on the same sample under equal laser processing parameters. The evolution of LIPSS from HSFL, over LSFL-II to LSFL I, is described, depending on laser peak fluence levels, number of pulses processing the spot and bulk temperature.
Herein, Ti6Al4V alloy is surface modified by femtosecond laser ablation. The microstructure image obtained by secondary electron microscopy reveals a combination of micrometer spikes or cones superimposed by nanoripples (laser‐induced periodic surface structures). To make the surface hydrophilic, anodization is performed resulting in further smoothness of microstructure and a final thickness of 35 ± 4 nm is estimated for oxide produced after anodization at 10 V (scan rate = 0.1 V s−1) versus standard hydrogen electrode. The obtained electrochemically active surface area (ECSA) is approximately 8 times larger compared with flat mirror polished Ti6Al4V surface. Combined chemical analysis by Pourbaix diagram and X‐ray photoelectron spectroscopy (XPS) analyses reveal that titanium and aluminum are passivating into TiO2 and Al2O3, but the dissolution of aluminum in the form of solvated ion is inevitable. Finally, cell seeding experiments on anodized and laser‐treated titanium alloy samples show that the growth of murine fibroblast cells is significantly suppressed due to unique surface texture of the laser‐treated and anodized titanium alloy sample.
The polarization of the laser beam exhibits more substantial differences in laser micromachining as the angle of incidence deviates from zero. In the reported work, our focus was to explore the effects of circularly, p- and s-polarized laser on angled ultrashort pulse laser micromachining of micropillar arrays. The examination encompassed laser process factors, including angles of incidence, microstructure dimensions, and inter-pillar spacing. A comparison between the resulting structures demonstrated that p-polarized laser beam was the most efficient in material removal in angled laser micromachining, followed by circularly polarized laser. While the s-polarized beam exhibited the lowest ablation efficiency among the three. Such distinction is mainly attributed to the distinguishing reflectivity of the three states of polarization on tilted planes. The development of structural heights during ablation processes was examined, and potential defects in laser processing methodologies were interpreted. The dependency of structural heights on inter-pillar spacing was analyzed. This study bridges the gap between existing studies on angled ultrashort pulse laser machining and the influences of polarization on laser machining. The comparison between structures produced using laboratory-scale and industrial-scale laser systems also yielded pertinent recommendations for facilitating a smooth transition of angled laser micromachining from laboratory-scale research to industrial applications.
Nanofibers are drawing the attention of engineers and scientists because their large surface-to-volume ratio is favorable for applications in medicine, filter technology, textile industry, lithium-air batteries, and optical sensors. However, when transferring nanofibers to a technical product in the form of a random network of fibers, referred to as nonwoven fabric, the stickiness of the freshly produced and thus fragile nanofiber nonwoven remains a problem. This is mainly because nanofibers strongly adhere to any surface because of van der Waals forces. In nature, there are animals that are actually able to efficiently produce, process, and handle nanofibers, namely cribellate spiders. For that, the spiders use the calamistrum, a comb-like structure of modified setae on the metatarsus of the hindmost (fourth) legs, to which the 10–30 nm thick silk nanofibers do not stick due to a special fingerprint-like surface nanostructure. In this work, we present a theoretical model of the interaction of linear nanofibers with a sinusoidally corrugated surface. This model allows for a prediction of the adhesive interaction and, thus, the design of a suitable surface structure to prevent sticking of an artificially nonwoven of nanofibers. According to the theoretical prediction, a technical analogon of the nanoripples was produced by ultrashort pulse laser processing on different technically relevant metal surfaces in the form of so-called laser-induced periodic surface structures (LIPSS). Subsequently, by means of a newly established peel-off test, the adhesion of an electrospun polyamide fiber-based nonwoven was quantified on such LIPSS-covered aluminium alloy, steel, and titanium alloy samples, as well as on polished (flat) control samples as reference and, additionally, on samples with randomly rough surfaces. The latter revealed that the adhesion of electrospun nanofiber nonwoven is significantly lowered on the nanostructured surfaces compared with the polished surfaces.
In laser machining with ultrashort laser pulses unwanted X-ray radiation in the keV range can be generated when a critical laser intensity is exceeded. Even if the emitted X-ray dose per pulse is low, high laser repetition rates can lead to an accumulation of X-ray doses beyond exposure safety limits. For 925 fs pulse duration at a center wavelength of 1030 nm, the X-ray emission was investigated up to an intensity of 2.6 × 10^14 W/cm2. The experiments were performed in air with a thin disk laser at a repetition rate of 400 kHz. X-ray spectra and doses were measured for various planar target materials covering a wide range of the periodic table from aluminum to tungsten. Without radiation shielding, the measured radiation doses at this high repetition rate clearly exceed the regulatory limits. Estimations for an adequate radiation shielding are provided.
Ultrashort pulse laser processing of materials allows for precise machining with high accuracy. By increasing the repetition rate to several 100 kHz, laser machining becomes quick and cost-effective. Ultrafast laser processing at high repetition rates and peak intensities above 10^13 W/cm^2 can cause a potential hazard by generation of unwanted x-ray radiation. Therefore, radiation protection must be considered. For 925 fs pulse duration at a center wavelength of 1030 nm, the x-ray emission in air at a repetition rate of 400 kHz was investigated up to a
peak intensity of 2.6 × 10^14 W/cm^2. Based on the presented measurements, the properties of potential shielding materials will be discussed. By extending our previous works, a scaling of the x-ray radiation emission to higher peak intensities up to 10^15 W/cm^2 is described, and emitted x-ray doses are predicted.