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Paper des Monats
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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.
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.
Light concentration opens up the path to enhanced material efficiency of solar cells via increased conversion efficiency and decreased material requirement. For true material saving, a fabrication method allowing local growth of high quality absorber material is essential. We present two scalable fs-laser based approaches for bottom-up growth of Cu(In,Ga)Se2 micro islands utilizing either site-controlled assembly of In(,Ga) droplets on laser-patterned substrates during physical vapor deposition, or laser-induced forward transfer of (Cu,In,Ga) layers for local precursor arrangement. The Cu(In,Ga)Se2 absorbers formed after selenization can deliver working solar devices showing efficiency enhancement under light concentration.
Laser ablation with femtosecond pulses (130 fs, wavelength 800 nm, repetition rate 2 Hz) was compared with nanosecond-pulse ablation (10 ns, wavelength 266 nm, repetition rate 2.5 Hz) of bariumalumoborosilicate glass in air using the direct focusing technique. Different ablation thresholds and heat-affected zones were observed. The lateral and vertical machining precision was evaluated. Single nanosecond laser pulses in the far UV resulted in a bubble or a circular hole in the centre of the illuminated spot, depending on the applied fluence. The ablation behaviour in the case of near-IR femtosecond pulses contrasted to this. Bubble formation was not detected. It needed repeated pulses at the same spot to modify the surface until material removal could be observed (incubation). Cavity dimensions of less than the beam diameter were achieved in this case.
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 formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences of parallel polarized Ti:sapphire femtosecond laser pulse pairs (160 fs pulse duration, 800 nm central wavelength) was studied experimentally. For that purpose, a Michelson interferometer was used to generate near-equal-energy double-pulse sequences allowing the temporal pulse delay between the parallel-polarized individual fs-laser pulses to be varied between 0 and 40 ps with ~0.2 ps temporal resolution. The surface morphologies of the irradiated surface areas were characterized by means of scanning electron and scanning force microscopy. In the sub-ps delay range a strong decrease of the LIPSS periods and the ablation crater depths with the double-pulse delay was observed indicating the importance of the laser-induced free-electron plasma in the conduction band of the solids for the formation of LIPSS.
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.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of five Ti:sapphire femtosecond (fs) laser pulse pairs (150 fs, 800 nm) is studied experimentally. A Michelson interferometer is used to generate near-equal-energy double-pulse sequences with a temporal pulse delay from -20 to +20 ps between the cross-polarized individual fs-laser pulses (~0.2 ps resolution). The results of multiple double-pulse irradiation sequences are characterized by means of Scanning Electron and Scanning Force Microscopy. Specifically in the sub-ps delay domain striking differences in the surface morphologies can be observed, indicating the importance of the laser-induced free-electron plasma in the conduction band of the solids for the formation of LIPSS.
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.
A bottom-up approach is presented for the production of arrays of indium islands on a molybdenum layer on glass, which can serve as micro-sized precursors for indium compounds such as copper-indium-gallium-diselenide used in photovoltaics. Femtosecond laser ablation of glass and a subsequent deposition of a molybdenum film or direct laser processing of the molybdenum film both allow the preferential nucleation and growth of indium islands at the predefined locations in a following indium-based physical vapor deposition (PVD) process. A proper choice of laser and deposition parameters ensures the controlled growth of indium islands exclusively at the laser ablated spots. Based on a statistical analysis, these results are compared to the non-structured molybdenum surface, leading to randomly grown indium islands after PVD.
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.
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.
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.
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.
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.
The influence of processing parameters on X‑ray emission during ultra‑short pulse laser machining
(2019)
During ultra-short laser material processing at high laser pulse repetition rates unwanted X-ray radiation can be generated in a quantity that may constitute a potential risk for health. An adequate X-ray radiation protection requires a thoroughly understanding of the influence of the laser processing parameters on the generation of X-ray radiation. In the present work, the generated X-ray dose during laser machining was investigated in air for varying beam scanning conditions at a pulse duration of 925 fs, a center wavelength of 1030 nm and a laser peak intensity of 2.6 × 10^14 W/cm^2. The X-ray radiation dose and the corresponding spectral X-ray emission were investigated in dependence on the laser’s pulse repetition rate and on the beam scanning speed. The results show a strong dependence of the X-ray emission on these laser processing parameters.
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.
Ultrashort pulse laser materials processing can be accompanied by the production of X-rays. Small doses per laser pulse can accumulate to significant dose rates at high laser pulse repetition rates which may exceed the permitted X-ray limits for human exposure. Consequently, a proper radiation shielding must be considered in laser machining. A brief overview of the current state of the art in the field of undesired generation of X-ray radiation during ultrashort pulse laser material processing in air is presented.
Review of x-ray exposure and safety issues arising from ultra-short pulse laser material processing
(2021)
Laser processing with ultra-short laser pulses enables machining of materials
with high accuracy and throughput. The development of novel laser Technologies with laser pulse repetition rates up to the MHz range opened the way for industrial manufacturing processes. From a radiological point of view this evolution is important, because x-ray radiation can be generated as an unwanted side effect in laser material processing. Even if the emitted x-ray dose per pulse is comparably low, the x-ray dose can become hazardous to health at high laser repetition rates. Therefore, radiation protection must be considered. This article provides an overview on the generation and detection of x-rays in laser material processing, as well as on the handling of this radiation risk in the framework of radiological protection.
Physical and chemical phenomena resulting from irradiation of silicon and indium phosphide with ultrashort laser pulses (~100fs) were investigated
with respect to the difference between single- and multiple-pulse treatment. In the single-pulse case, several processes were identified: modification,
recrystallization and ablation. All processes exhibit a distinct treshold behaviour. A two photon-absorption coefficient can be determined from a single
spatial ablation profile. Accumulation effects were observed for multi-pulse illumination. Different morphological features like bubbles, rippels and
microcolumns were found.
Summary form only given. Machining investigations of crystalline silicon have been performed with laser pulses at a wavelength of 780 nm in the range between 5 fs and 400 fs. Applying 100 pulses per spot, surface damage thresholds were determined by the measurement of the damage diameter. In this pulse duration regime, the threshold fluences were nearly constant. Single-pulse investigations with 5 fs pulses yielded a value of about 0.15 J cm-2 identical to the multi-pulse experiment. This is in contradiction to the behaviour of dielectrics where incubation effects alter the optical properties down to the 5 fs pulse regime. Employing laser pulses with a duration of 130 fs at a wavelength of 800 nm, single-pulse ablation thresholds of 0.23 J cm-2 and 0.16 J cm-2 were determined for Si and InP in air, respectively. The threshold fluence was calculated from the linear relation between the square of the diameters versus the logarithm of the laser fluences.
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.
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.
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.
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.
The ultrafast laser ablation of silicon has been investigated experimentally and theoretically. The theoretical description is based on molecular dynamics (MD) simulations combined with a microscopic electronic model. We determine the thresholds of melting and ablation for two different pulse durations =20 and 500 fs. Experiments have been performed using 100 Ti:Sap-phire laser pulses per spot in air environment. The ablation thresholds were determined for pulses with a duration of 25 and 400 fs, respectively. Good agreement is obtained between theory and experiment.
The formation of laser-induced periodic surface structures (LIPSS) on two different silica polymorphs (single-crystalline synthetic quartz and commercial fused silica glass) upon irradiation in air with multiple linearly polarized single- and double-fs-laser pulse sequences (τ = 150 fs pulse duration, λ = 800nm center wavelength, temporal pulse separation Δt < 40 ps) is studied experimentally and theoretically. Two distinct types of fs-LIPSS [so-called low-spatial-frequency LIPSS (LSFL) and high-spatial-frequency LIPSS (HSFL)] with different spatial periods and orientations were identified. Their appearance was characterized with respect to the experimental parameters peak laser fluence and number of laser pulses per spot. Additionally, the 'dynamics' of the LIPSS formation was addressed in complementary double-fs-pulse experiments with varying delays, revealing a characteristic change of the LSFL periods. The experimental results are interpreted on the basis of a Sipe-Drude model considering the carrier dependence of the optical properties of fs-laser excited silica. This new approach provides an explanation of the LSFL orientation parallel to the laser beam polarisation in silica—as opposed to the behaviour of most other materials.
The formation of laser-induced periodic surface structures upon irradiation of titanium, silicon, and fused silica with multiple irradiation sequences consisting of parallel polarized Ti:sapphire femtosecond laser pulse pairs (pulse duration 50–150 fs, central wavelength ~800 nm) is studied experimentally. The temporal delay between the individual near-equal energy fs-laser pulses was varied between 0 and 5 ps with a temporal resolution of better than 0.2 ps. The surface morphology of the irradiated surface areas is characterized by means of scanning electron microscopy (SEM). In all materials a decrease of the rippled surface area is observed for increasing delays. The characteristic delay decay scale is quantified and related to material dependent excitation and energy relaxation processes.
Femtosecond diffraction dynamics of laser-induced periodic surface structures on fused silica
(2013)
The formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration, 800?nm center wavelength) is studied experimentally using a transillumination femtosecond time-resolved (0.1 ps-1 ns) pump-probe diffraction approach. This allows to reveal the generation dynamics of near-wavelength-sized LIPSS showing a transient diffraction at specific spatial frequencies even before a corresponding permanent surface relief was observed. The results confirm that the ultrafast energy deposition to the materials surface plays a key role and triggers subsequent physical mechanisms such as carrier scattering into self-trapped excitons.
Single- and two-color double-fs-pulse experiments were performed on titanium to study the dynamics of the formation of laser-induced periodic surface structures (LIPSS). A Mach-Zehnder inter-ferometer generated polarization controlled (parallel or cross-polarized) double-pulse sequences in two configurations – either at 800 nm only, or at 400 and 800 nm wavelengths. The inter-pulse delays of the individual 50-fs pulses ranged up to some tens of picoseconds. Multiple of these single- or two-color double-fs-pulse sequences were collinearly focused by a spherical mirror to the sample surface. In both experimental configurations, the peak fluence of each individual pulse was kept below its respective ablation threshold and only the joint action of both pulses lead to the formation of LIPSS. Their resulting characteristics were analyzed by scanning electron microscopy and the periods were quantified by Fourier analyses. The LIPSS periods along with the orientation allow a clear identification of the pulse which dominates the energy coupling to the material. A plasmonic model successfully explains the delay-dependence of the LIPSS on titanium and confirms the importance of the ultrafast energy deposition stage for LIPSS formation.
In order to study the temporally distributed energy deposition in the formation of laser-induced periodic surface structures (LIPSS) on single-crystalline zinc oxide (ZnO), two-colour double-fs-pulse experiments were performed. Parallel or cross-polarised double-pulse sequences at 400 and 800 nm wavelength were generated by a Mach–Zehnder interferometer, exhibiting inter-pulse delays up to a few picoseconds between the sub-ablation 50-fs-pulses. Twenty two-colour double-pulse sequences were collinearly focused by a spherical mirror to the sample surface. The resulting LIPSS periods and areas were analysed by scanning electron microscopy. The delay-dependence of these LIPSS characteristics shows a dissimilar behaviour when compared to the semiconductor silicon, the dielectric fused silica, or the metal titanium. A wavelength-dependent plasmonic mechanism is proposed to explain the delay-dependence of the LIPSS on ZnO when considering multi-photon excitation processes. Our results support the involvement of nonlinear processes for temporally overlapping pulses. These experiments extend previous two-colour studies on the indirect semiconductor silicon towards the direct wide band-gap semiconductor ZnO and further manifest the relevance of the ultrafast energy deposition for LIPSS formation.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica and silicon with multiple (NDPS) irradiation sequences consisting of linearly polarized femtosecond laser pulse pairs (pulse duration ~150 fs, central wavelength ~800 nm) is studied experimentally. Nearly equal-energy double-pulse sequences are generated allowing the temporal pulse delay Δt between the cross-polarized individual fs-laser pulses to be varied from -40 ps to +40 ps with a resolution of ~0.2 ps. The surface morphologies of the irradiated surface areas are characterized by means of scanning electron and scanning force microscopy. Particularly for dielectrics in the sub-ps delay range striking differences in the orientation and spatial characteristics of the LIPSS can be observed. For fused silica, a significant decrease of the LIPSS spatial periods from ~790 nm towards ~550 nm is demonstrated for delay changes of less than ~2 ps. In contrast, for silicon under similar irradiation conditions, the LIPSS periods remain constant (~760 nm) for delays up to 40 ps. The results prove the impact of laser-induced electrons in the conduction band of the solid and associated transient changes of the optical properties on fs-LIPSS formation.
The formation of laser-induced periodic surface structures (LIPSS) on different materials (silicon, fused silica, quartz) with linearly polarized fs-laser irradiation is studied experimentally. In dielectrics, the importance of transient excitation stages in the LIPSS formation is demonstrated by using (multiple) cross-polarized double-fs-laser-pulse irradiation sequences. A characteristic decrease of the spatial LIPSS periods is observed for double-pulse delays of less than 2 ps along with a characteristic 90°-rotation of the LIPSS orientation.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of fused silica with multiple irradiation sequences consisting of laser pulse pairs (50 fs single-pulse duration) of two different wavelengths (400 and 800 nm) is studied experimentally. Parallel polarized double-pulse sequences with a variable delay Δt between -10 and +10 ps and between the individual fs-laser pulses were used to investigate the LIPSS periods versus Δt. These two-color experiments reveal the importance of the ultrafast energy deposition to the silica surface by the first laser pulse for LIPSS formation. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS frequencies.
The dynamics of the formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration) is studied by cross-polarized two-color double-fs-pulse experiments. In order to analyze the relevance of temporally distributed energy deposition in the early stage of LIPSS formation, a Mach-Zehnder interferometer was used for generating multiple double-pulse sequences at two different wavelengths (400 and 800 nm). The inter-pulse delay between the individual cross-polarized pulses of each sequence was systematically varied in the sub-ps range and the resulting LIPSS morphologies were characterized by scanning electron microscopy. It is found that the polarization of the first laser pulse arriving to the surface determines the orientation and the periodicity of the LIPSS. These two-color experiments further confirm the importance of the ultrafast energy deposition to the silica surface for LIPSS formation, particularly by the first laser pulse of each sequence. The second laser pulse subsequently reinforces the previously seeded spatial LIPSS characteristics (period, orientation).
Two-color double-fs-pulse experiments were performed on silicon wafers to study the temporally distributed energy deposition in the formation of laser-induced periodic surface structures (LIPSS). A Mach-Zehnder interferometer generated parallel or cross-polarized double-pulse sequences at 400 and 800 nm wavelength, with inter-pulse delays up to a few picoseconds between the sub-ablation 50-fs-pulses. Multiple two-color double-pulse sequences were collinearly focused by a spherical mirror to the sample. The resulting LIPSS characteristics (periods, areas) were analyzed by scanning electron microscopy. A wavelength-dependent plasmonic mechanism is proposed to explain the delay-dependence of the LIPSS. These two-color experiments extend previous single-color studies and prove the importance of the ultrafast energy deposition for LIPSS formation.
In order to address the dynamics and physical mechanisms of LIPSS formation for three different classes of materials (metals, semiconductors, and dielectrics), two-color double-fs-pulse experiments were performed on Titanium, Silicon and Fused Silica. For that purpose a Mach–Zehnder interferometer generated polarization controlled (parallel or cross-polarized) double-pulse sequences at 400 nm and 800 nm wavelength, with inter-pulse delays up to a few picoseconds. Multiple of these two-color double-pulse sequences were collinearly focused by a spherical mirror to the sample surfaces. The fluence of each individual pulse (400 nm and 800 nm) was always kept below its respective ablation threshold and only the joint action of both pulses lead to the formation of LIPSS. Their resulting characteristics (periods, areas) were analyzed by scanning electron microscopy. The periods along with the LIPSS orientation allow a clear identification of the pulse which dominates the energy coupling to the material. For strong absorbing materials (Silicon, Titanium), a wavelength-dependent plasmonic mechanism can explain the delay-dependence of the LIPSS. In contrast, for dielectrics (Fused Silica) the first pulse always dominates the energy deposition and LIPSS orientation, supporting a non-plasmonic formation scenario. For all materials, these two-color experiments confirm the importance of the ultrafast energy deposition stage for LIPSS formation.
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.
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).
A laser-based bottom-up technique for the fabrication of Cu(In,Ga)Se2 (CIGSe) micro solar cells is presented.
We use femtosecond laser-induced forward transfer (LIFT) to transport a metallic precursor composed of copper, indium, and gallium onto a molybdenum back contact layer on a glass substrate. A CIGSe absorber forms by subsequent selenization. An array of micro absorbers with defined spacing is fabricated to solar cells and characterized under concentrated light illumination. The solar cell array exhibited a conversion efficiency of 1.4‰ at 1 sun as well as a significant efficiency enhancement of 68% rel. under 20-fold concentration. This work demonstrates the possibility of directly grown micrometer-sized solar cells based on chalcogenide absorber layers, enabling effective material usage.
The selective emitter is a well-known technology for producing highly doped areas under the metallization grid to improve the solar cell performance. In this work, the influence of laser irradiation on phosphoric acid coated multicrystalline silicon PV-wafers on the wafer surface structure, the phosphorous depth distribution and the electrical contact resistance within the laser treated area as well as the electrical series resistance of laserprocessed solar cells was evaluated. Different laser processing settings were tested including pulsed and continuous wave (cw) laser sources (515 nm, 532 nm, 1064 nm wavelength). Complementary numerical simulations using the finite element method (FEM) were conducted to explain the impact of the laser parameters on the melting behavior (melt duration and geometry). It was found that the melt duration is a key parameter for a successful laser Doping process. Our simulations at a laser wavelengths of 515 nm reveal that low-repetition rate (<500 kHz) laser pulses of 300 ns duration generate a melt duration of ~0.35 µs, whereas upon scanning cw-laser radiation at 532 nm prolongates the melt duration by at least one order of magnitude. Experimentally, the widely used ns-laser pulses did not lead to satisfying laser irradiation results. In contrast, cw-laser radiation and scan velocities of less than 2 m/s led to suitable laser doping featuring low electrical resistances in the laser treated areas.
In this contribution, chemical, structural, and mechanical alterations in various types of femtosecond laser-generated surface structures, i.e., laser-induced periodic surface structures (LIPSS, ripples), Grooves, and Spikes on titanium alloy, are characterized by various surface analytical techniques, including X-ray diffraction and glow-discharge optical emission spectroscopy. The formation of oxide layers of the different laser-based structures inherently influences the friction and wear performance as demonstrated in oil-lubricated reciprocating sliding tribological tests (RSTTs) along with subsequent elemental mapping by energy-dispersive X-ray analysis. It is revealed that the fs-laser scan processing (790 nm, 30 fs, 1 kHz) of near-wavelength-sized LIPSS leads to the formation of a graded oxide layer extending a few hundreds of nanometers into depth, consisting mainly of amorphous oxides. Other superficial fs-laser-generated structures such as periodic Grooves and irregular Spikes produced at higher fluences and effective number of pulses per unit area present even thicker graded oxide layers that are also suitable for friction reduction and wear resistance. Ultimately, these femtosecond laser-induced nanostructured surface layers efficiently prevent a direct metal-to-metal contact in the RSTT and may act as an anchor layer for specific wear-reducing additives contained in the used engine oil.