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Irradiation with ultra-short (femtosecond) laser beams enables the generation of sub-wavelength laser-induced periodic surface structures (LIPSS) over large areas with controlled spatial periodicity, orientation, and depths affecting only a material layer on the sub-micrometer scale. This study reports on how fs-laser irradiation of commercially available Nb foil samples affects their superconducting behavior. DC magnetization and AC susceptibility measurements at cryogenic temperatures and with magnetic fields of different amplitude and orientation are thus analyzed and reported. This study pays special attention to the surface superconducting layer that persists above the upper critical magnetic field strength Hc2, and disappears at a higher nucleation field strength Hc3. Characteristic changes were distinguished between the surface properties of the laser-irradiated samples, as compared to the corresponding reference samples (non-irradiated). Clear correlations have been observed between the surface nanostructures and the nucleation field Hc3, which depends on the relative orientation of the magnetic field and the surface patterns developed by the laser irradiation.
Laser-induced periodic surface structures (LIPSS) are a universal phenomenon and can be generated on almost any material by irradiation with linearly polarized radiation. This chapter reviews the current state in the field of LIPSS, which are formed in a “self-ordered” way and are often accompanying materials processing applications. LIPSS can be produced in a single-stage process and enable surface nanostructuring and, in turn, adaption of optical, mechanical, and chemical surface properties. Typically, they feature a structural size ranging from several micrometers down to less than 100 nm and show a clear correlation with the polarization direction of the light used for their generation. Various types of LIPSS 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. 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 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 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.
Effects of laser-induced periodic surface structures on the superconducting properties of Niobium
(2020)
It is well known that the use of ultrashort (fs) pulsed lasers can induce the generation of (quasi-) periodic nanostructures (LIPSS, ripples) on the surface of many materials. Such nanostructures have also been observed in sample’s surfaces irradiated with UV lasers with a pulse duration of 300 ps. In this work, we compare the characteristics of these nanostructures on 1-mm and on 25-μm thick niobium sheets induced by 30 fs n-IR and 300 ps UV pulsed lasers. In addition to conventional continuous or burst mode processing configurations, two-dimensional laser beam and line scanning modes have been investigated in this work. The latter allows the processing of large areas with a more uniform distribution of nanostructures at the surface. The influence of the generated nanostructures on the superconducting properties of niobium has also been explored. For this aim, magnetic hysteresis loops have been measured at different cryogenic temperatures to analyse how these laser treatments affect the flux pinning behaviour and, in consequence, the superconductor’s critical current values. It was observed that laser treatments are able to modify the superconducting properties of niobium samples.
Single Femtosecond Laser-Pulse-Induced Superficial Amorphization and Re-Crystallization of Silicon
(2021)
Superficial amorphization and re-crystallization of silicon in <111> and <100> orientation after irradiation by femtosecond laser pulses (790 nm, 30 fs) are studied using optical imaging and transmission electron microscopy. Spectroscopic imaging ellipsometry (SIE) allows fast data acquisition at multiple wavelengths and provides experimental data for calculating nanometric amorphous layer thickness profiles with micrometric lateral resolution based on a thin-film layer model. For a radially Gaussian laser beam and at moderate peak fluences above the melting and below the ablation thresholds, laterally parabolic amorphous layer profiles with maximum thicknesses of several tens of nanometers were quantitatively attained. The accuracy of the calculations is verified experimentally by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (STEM-EDX). Along with topographic information obtained by atomic force microscopy (AFM), a comprehensive picture of the superficial re-solidification of silicon after local melting by femtosecond laser pulses is drawn.
Given their unique properties, ultrashort laser pulses with durations in the femtosecond to picosecond range currently open new avenues in the field of laser materials processing, resulting in groundbreaking new applications based on laser-induced surface functionalization. This article reviews the usability of temporally distributed energy deposition via double-pulse irradiation in applications based on laser ablation. This includes simple new techniques for surface nanostructuring and improved sensitivities in spectroscopic material analyses.
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.
A promising technology in photovoltaics is based on micro-concentrator solar cells, where the photovoltaic active area is realized as an array of sub-millimeter sized cells onto which the incident light is focused via microlenses. This approach allows to increase the cell efficiency and to realize much more compact modules compared to macroscopic concentrator devices. At the same time, expensive raw materials can be saved, which is of interest, for example, with respect to indium in the case of copper-indium-gallium-diselenide (CIGSe) thin film solar cells. Two methods to produce micro-sized precursors of CIGSe absorbers on molybdenum are presented using 30-fs laser pulses at 790 nm wavelength. On the one hand, a multi pulse surface structuring of the molybdenum film or the underlying glass substrate and a subsequent physical vapor deposition were used for a site-selective aggregation of indium droplets. On the other hand, a single pulse laser-induced forward transfer was utilized to selectively deposit combined copper-indium precursor pixels on the molybdenum back contact of the solar cell. Post-processing (selenization, isolation, contacting) of the laser-generated micro-sized precursors results in functional CIGSe solar cells.
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 picosecond to femtosecond 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 or chemical properties. In this contribution current applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting, the tailoring of surface colonization by bacterial biofilms, and the improvement of the tribological performance of nanostructured metal surfaces.
Titanium nitride (TiN) was coated on different substrate materials, namely pure titanium (Ti), titanium alloy (Ti6Al4V) and steel (100Cr6), generating 2.5 μm thick TiN layers. Using femtosecond laser pulses (30 fs, 790 nm, 1 kHz pulse repetition rate), large surface areas (5 mm × 5 mm) of laser-induced periodic surface structures (LIPSS) with sub-wavelength periods ranging between 470 nm and 600 nm were generated and characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). In tribological tests, coefficients of friction (COF) of the nanostructured surfaces were determined under reciprocating sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel during 1000 cycles using two different lubricants, namely paraffin oil and engine oil. It turned out that the substrate material, the laser fluence and the lubricant are crucial for the tribological performance. However, friction and wear could not be significantly reduced by LIPSS on TiN layers in comparison to unstructured TiN surfaces. Finally, the resulting wear tracks on the nanostructured surfaces were investigated with respect to their morphology (OM, SEM), depth (WLIM) and chemical composition by energy dispersive X-ray spectroscopy (EDX) and, on one hand, compared with each other, on the other hand, with non-structured TiN surfaces.
Inorganic materials, such as steel, were functionalized by ultrashort laser pulse irradiation (fs- to ps-range) to modify the surface’s wetting behavior. The laser processing was performed by scanning the laser beam across the surface of initially polished flat sample material. A systematic experimental study of the laser processing parameters (peak fluence, scan velocity, line overlap) allowed the identification of different regimes associated with characteristic surface morphologies (laser-induced periodic surface structures, grooves, spikes, etc.). Analyses of the surface using optical as well as scanning electron microscopy revealed morphologies providing the optimum similarity to the natural skin of lizards. For mimicking skin structures of moisture-harvesting lizards towards an optimization of the surface wetting behavior, additionally a two-step laser processing strategy was established for realizing hierarchical microstructures. In this approach, micrometer-scaled capillaries (step 1) were superimposed by a laser-generated regular array of small dimples (step 2). Optical focus variation imaging measurements finally disclosed the three dimensional topography of the laser processed surfaces derived from lizard skin structures. The functionality of these surfaces was analyzed in view of wetting properties.
Indium islands on molybdenum coated glass can be grown in ordered arrays by surface structuring using a femtosecond laser. The effect of varying the molybdenum coated glass substrate temperature and the indium deposition rate on island areal density, volume and geometry is investigated and evaluated in a physical vapor deposition (PVD) process. The joined impact of growth conditions and spacing of the femtosecond laser structured spots on the arrangement and morphology of indium islands is demonstrated. The results yield a deeper understanding of the island growth and its precise adjustment to industrial requirements, which is indispensable for a technological application of such structures at a high throughput, for instance as precursors for the preparation of Cu(In,Ga)Se2 micro concentrator solar cells.
Biofilm formation poses high risks in multiple industrial and medical settings. However, the robust nature of biofilms makes them also attractive for industrial applications where cell biocatalysts are increasingly in use. Since tailoring material properties that affect bacterial growth or its inhibition is gaining attention, here we focus on the effects of femtosecond laser produced nanostructures on bacterial adhesion. Large area periodic surface structures were generated on steel surfaces using 30-fs laser pulses at 790 nm wavelength. Two types of steel exhibiting a different corrosion resistance were used, i.e., a plain structural steel (corrodible) and a stainless steel (resistant to corrosion). Homogeneous fields of laser-induced periodic surface structures (LIPSS) were realized utilizing laser fluences close to the ablation threshold while scanning the sample under the focused laser beam in a multi-pulse regime. The nanostructures were characterized with optical and scanning electron microscopy. For each type of steel, more than ten identical samples were laser-processed. Subsequently, the samples were subjected to microbial adhesion tests. Bacteria of different shape and adhesion behavior (Escherichia coli and Staphylococcus aureus) were exposed to laser structures and to polished reference surfaces. Our results indicate that E. coli preferentially avoids adhesion to the LIPSS-covered areas, whereas S. aureus favors these areas for colonization.
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.
Ultrashort laser pulses with durations in the fs-to-ps range were used for large area surface processing of steel aimed at mimicking the morphology and extraordinary wetting behaviour of bark bugs (Aradidae) found in nature. The processing was performed by scanning the laser beam over the surface of polished flat sample surfaces. A systematic variation of the laser processing parameters (peak fluence and effective number of pulses per spot diameter) allowed the identification of different regimes associated with characteristic surface morphologies (laser-induced periodic surface structures, i.e., LIPSS, grooves, spikes, etc.). Moreover, different laser processing strategies, varying laser wavelength, pulse duration, angle of incidence, irradiation atmosphere, and repetition rates, allowed to achieve a range of morphologies that resemble specific structures found on bark bugs. For identifying the ideal combination of parameters for mimicking bug-like structures, the surfaces were inspected by scanning electron microscopy. In particular, tilted micrometre-sized spikes are the best match for the structure found on bark bugs. Complementary to the morphology study, the wetting behaviour of the surface structures for water and oil was examined in terms of philic/ phobic nature and fluid transport. These results point out a route towards reproducing complex surface structures inspired by nature and their functional response in technologically relevant materials.
Miniaturized pacemakers with a surface consisting of a Ti alloy may have to be removed after several years from their implantation site in the heart and shall, therefore, not be completely overgrown by cells or tissue. A method to avoid this may be to create at the surface by laser-ablation self-organized sharp conical spikes, which provide too little surface for cells (i.e., fibroblasts) to grow on. For this purpose, Ti-alloy substrates were irradiated in the air by 790 nm Ti:sapphire femtosecond laser pulses at fluences above the ablation threshold. The laser irradiation resulted in pronounced microstructure formation with hierarchical surface morphologies. Murine fibroblasts were seeded onto the laser-patterned surface and the coverage by cells was evaluated after 3–21 days of cultivation by means of scanning electron microscopy. Compared to flat surfaces, the cell density on the microstructures was significantly lower, the coverage was incomplete, and the cells had a clearly different morphology. The best results regarding suppression of cell growth were obtained on spike structures which were additionally electrochemically oxidized under acidic conditions. Cell cultivation with additional shear stress could reduce further the number of adherent cells.
A procedure to fabricate CuInSe2 (CISe) micro-absorbers and solar cells for concentrator applications is presented. The micro-absorbers are developed from indium precursor islands, which are deposited on a molybdenum coated glass substrate (back contact), followed by deposition of copper on top and subsequent selenization as well as selective etching of copper selenides. In order to compare the properties of the locally grown absorbers to those of conventional large area CISe films, we systematically examine the compositional and morphological homogeneity of the micro absorbers and carry out photoluminescence measurements. Preliminary devices for micro-concentrator solar cell applications are fabricated by optimizing the copper to indium ratio and the size of the indium precursor islands. The resulting micro solar cells provide a characteristic I–V curve under standard illumination conditions (1 sun).
Single-pulse femtosecond laser-induced forward transfer (LIFT, 30 fs, 790 nm) is used to deposit micron-sized dots of copper and/or indium onto a molybdenum layer on glass. Such systems can serve as precursors for the bottom-up manufacturing of micro-concentrator solar cells based on copper-indium-gallium-diselenide. The influence of the thickness of the copper, indium and combined copper-indium donor layers on the quality of the transferred dots was qualified by scanning electron microscopy, energy-dispersive X-ray analysis, and optical microscopy. The potential for manufacturing of a spatial arrangement adapted to the geometry of micro-lens arrays needed for micro-concentrator solar cells is demonstrated.
The chemical characteristics of two different types of laser-induced periodic surface structures (LIPSS), so-called high and low spatial frequency LIPSS (HSFL and LSFL), formed upon irradiation of titanium surfaces by multiple femtosecond laser pulses in air (30 fs, 790 nm, 1 kHz), are analyzed by various optical and electron beam based surface analytical techniques, including micro-Raman spectroscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, and Auger electron spectroscopy. The latter method was employed in a high-resolution mode being capable of spatially resolving even the smallest HSFL structures featuring spatial periods below 100 nm. In combination with an ion sputtering technique, depths-resolved chemical information of superficial oxidation processes was obtained, revealing characteristic differences between the two different types of LIPSS. Our results indicate that a few tens of nanometer shallow HSFL are formed on top of a ∼150 nm thick graded superficial oxide layer without sharp interfaces, consisting of amorphous TiO2 and partially crystallized Ti2O3. The larger LSFL structures with periods close to the irradiation wavelength originate from the laser-interaction with metallic titanium. They are covered by a ∼200 nm thick amorphous oxide layer, which consists mainly of TiO2 (at the surface) and other titanium oxide species of lower oxidation states underneath.
Periodic self-organization of matter beyond the diffraction limit is a puzzling phenomenon, typical both for surface and bulk ultrashort laser processing. Here we compare the mechanisms of periodic nanostructure formation on the surface and in the bulk of fused silica. We show that volume nanogratings and surface nanoripples having subwavelength periodicity and oriented perpendicular to the laser polarization share the same electromagnetic origin. The nanostructure orientation is defined by the near-field local enhancement in the vicinity of the inhomogeneous scattering centers. The periodicity is attributed to the coherent superposition of the waves scattered at inhomogeneities. Numerical calculations also support the multipulse accumulation nature of nanogratings formation on the surface and inside fused silica. Laser surface processing by multiple laser pulses promotes the transition from the high spatial frequency perpendicularly oriented nanoripples to the low spatial frequency ripples, parallel or perpendicular to the laser polarization. The latter structures also share the electromagnetic origin, but are related to the incident field interference with the scattered far-field of rough non-metallic or transiently metallic surfaces. The characteristic ripple appearances are predicted by combined electromagnetic and thermo-mechanical approaches and supported by SEM images of the final surface morphology and by time-resolved pump-probe diffraction measurements.
The industrial use of ultrashort laser pulses has made considerable progress in recent years. The reasons for this lie in the availability of high average powers at pulse repetition rates in the several 100 kHz range. The advantages of using ultrashort laser pulses in terms of processing precision can thus be fully exploited. However, high laser intensities on the workpiece can also lead to the generation of unwanted X-rays. Even if the emitted X-ray dose per pulse is low, the accumulated X-ray dose can become significant for high-repetition-rate laser systems so that X-ray exposure safety limits must be considered. The X-ray emission during ultrashort pulse laser processing was investigated for a pulse duration of 925 fs at 1030 nm wavelength and 400 kHz repetition rate. Industrially relevant materials such as steel,aluminum and glass were treated. Tungsten served as reference. X-ray spectra were recorded, and X-ray dose measurements were performed for laser treatment in air. For laser intensities > 2 × 10^13 W/cm2, X-ray doses exceeding the regulatory exposure limits for members of the public were found. Suitable X-ray protection strategies are proposed.
X‑ray emission during the ablative processing of biological materials by ultrashort laser pulses
(2023)
The ablative laser processing with ultrashort pulsed laser beams may cause secondary emission of hazardous X-rays. While the effect has recently been proven to be considered in working safety regulations when processing technical materials, such as metals, the X-ray emission rates during the ablative processing of biological tissue materials are widely unexplored yet.
Therefore, biological materials like water, isotonic saline solution, pig eyes, and human teeth were ablated with ultrashort laser pulses of 1030 nm wavelength, 600 fs pulse duration and 5 kHz pulse repetition rate, aiming to mimic typical surgery situations. Simultaneously, in-situ X-ray dose rate measurements were performed at a short distance from the plasma to display potential X-ray emission. For all four studied biological materials, our measurements prove the secondary emission of laser-induced X-rays.
Unwanted X-ray emission in ultrashort pulse laser processing: From metallic to biological materials
(2023)
X-rays can be generated as an unwanted side effect during ultrashort pulse laser material processing of technical work pieces and even biological samples with laser intensities above 10^13 W/cm^2. First studies demonstrate the need to address this effect in industrial as well as in medical applications. This secondary hazard should be considered in work safety and risk assessment.
Surface nanostructures provide the possibility to create and tailor surface functionalities mainly via controlling their topography along with other chemical and physical material properties. One of the most appealing technologies for surface functionalization via micro- and nanostructuring is based on laser processing. This can be done either via direct contour-shaping of the irradiated material using a tightly focused laser beam or in a self-ordered way that allows employing larger laser beam diameters along with areal scanning to create a variety of laser-induced periodic surface structures (LIPSS). For the latter approach, particularly ultrashort pulsed lasers have recently pushed the borders across long-lasting limitations regarding the minimum achievable feature sizes and additionally boosted up the production times. This chapter reviews the plethora of recently investigated applications of LIPSS—for example, via imposing diffractive or plasmonic structural colors, the management of liquids and surface wetting properties, biomedical and bioinspired functionalities, beneficial effects in tribology for reducing friction and wear, the manipulation of optical scattering and absorption in photovoltaics, or the modification of magnetic or superconducting surface properties in other energy applications. The footprint of the LIPSS-based technology is explored in detail regarding the current state of industrialization, including an analysis of the market and associated LIPSS production costs.
Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms.
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.
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.