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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.
Optical multimode fibers made of fused silica are widely used for transmission of high power laser pulses. Bending of fibers creates mechanical stress inside the material. The bend stress of a fiber can be calculated from bend radius, geometrical fiber parameters and Young's Modulus of the fiber core material and reaches typically values of 220 MPa. A thermo-elastic model of Kusov et al. predicts a quadratic dependence of laser-induced damage threshold fluence with applied stress.
In the present study, fiber preform material F300 (Heraeus) was loaded mechanically with pressures up to 220 MPa representing 20% of the pressure resistance of fused silica. Bulk laser-induced damage thresholds (LIDT) were evaluated using a longitudinal multimode Q-switched Nd:YAG laser (1064 nm) at a pulse duration of 12 ns with polarization states parallel and perpendicular to the stress direction. LIDT of fused silica samples of about 700 J/cm2 were found. LIDT did not show a dependence on mechanical pressure and polarization state which is a consequence of the small ratio of maximum applied stress (220 MPa) to Young's Modulus of fused silica (72.5 GPa).
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.
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 titanium upon irradiation with linearly polarized femtosecond (fs) laser pulses (τ = 30 fs, λ = 790 nm) in an air environment is studied experimentally and theoretically. In the experiments, the dependence on the laser fluence and the number of laser pulses per irradiation spot has been analyzed. For a moderate number of laser pulses (N < 1000) and at fluences between ~0.09 and ~0.35 J/cm², predominantly low-spatial-frequency-LIPSS with periods between 400 nm and 800 nm are observed perpendicular to the polarization. In a narrow fluence range between 0.05 and 0.09 J/cm², high-spatial-frequency-LIPSS with sub-100-nm spatial periods (~λ/10) can be generated with an orientation parallel to the polarization (N = 50). These experimental results are complemented by calculations based on a theoretical LIPSS model and compared to the present literature.
The 125-fs laser ablation behaviour (800 nm) of aluminium and anodic oxide coatings on an AlMgSi1 alloy was investigated. The multi-pulse ablation threshold of aluminium at 1.2 J cm-2 was less than that of the oxides of 23 J cm-2. Aluminium exhibited a single pulse modification (melting) threshold of 0.3 J cm-2. These values derived from an evaluation of the crater geometry coincided with on-line acoustic measurements. The detected microphone voltage amplitude increased linearly with the laser fluence. The morphology of the ablation craters on aluminium indicated melt formation and displacement of a homogeneous melt phase due to the recoil action of the expanding metal vapour. The laser-processed ceramic oxide phases, on the other hand, showed a spongy resolidified melt layer, which denotes a collocated in-depth formation both of a melt and a gas phase. These phenomena are discussed in terms of the relative dominance of penetration depth of laser light and heat affected zones in the investigated materials with strongly varying optical and thermodynamical properties.
We investigated the initial modification and ablation of crystalline silicon with single and multiple Ti:sapphire laser pulses of 5 to 400 fs duration. In accordance with earlier established models, we found the phenomena amorphization, melting, re-crystallization, nucleated vaporization, and ablation to occur with increasing laser fluence down to the shortest pulse durations. We noticed new morphological features (bubbles) as well as familiar ones (ripples, columns). A nearly constant ablation threshold fluence on the order of 0.2 J/cm2 for all pulse durations and multiple-pulse irradiation was observed. For a duration of ,100 fs, significant incubation can be observed, whereas for 5 fs pulses, the ablation threshold does not depend on the pulse number within the experimental error. For micromachining of silicon, a pulse duration of less than 500 fs is not advantageous.
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 multi-pulse ablation threshold of barium borosilicate glass was measured using 30-fs pulses of a high repetition rate (1 kHz) laser system. The threshold fluence was found to decrease with increasing beam radius ranging from 20 to 400 m. Two existing models are applied by considering thermal accumulation and point defects, respectively .
Curved substrates can be micro-structured by laser ablation, which is not possible with standard lithographic methods. The novel femtosecond-pulse laser technique allows the production of defined and reproducible micro-perforations of originally analyte-impermeable membranes. The trans-membrane analyte flux can be controlled both by the variation of the laser focus diameter resulting in different areas of single perforations, and the number of perforations in arrays on small membrane areas. This leads to a higher degree of variability as well as reproducibility of the diffusion qualities of sensor membranes, and marks the main innovation with this technique compared to the hand-made mechanical perforation by specially grinded needles used up to now. Touchless micro-perforation of small membrane areas with negligible heat damage of the structures adjacent to the perforation allows the application of analyte door membranes directly onto curved surfaces of miniaturized needle-sensors assigned for in vivo glucose monitoring, for the first time.
Laser cleaning of delicate biological composite materials such as ancient parchment manuscripts from the 15th and 16th century and printed paper from the 19th century is demonstrated with an ultraviolet excimer pulsed laser at 308 nm. Laser fluence levels must stay below the ablation and destruction threshold of the parchment or paper substrate, and have to surpass the threshold of the contaminant matter. Foreign layers to be removed must exhibit a higher optical density than the artifact substrates. Synthetic carbonaceous dirt modelled by water-soluble black crayons showed a characteristically weak featureless laser-induced plasma spectroscopy spectrum near the noise limit. It turned out that laser-induced plasma spectroscopy is of limited use in monitoring halting points (or etch-stops) because it relies on the destruction not only of the laterally inhomogenously distributed contaminant but also of pigment phases on a microscopically rough parchment substrate. Laser-induced fluorescence spectroscopy, however, promises to be a valuable non-destructive testing technique for etch-stop monitoring.
We report measurements of the optical breakdown threshold and ablation depth in dielectrics with different band gaps for laser pulse durations ranging from 5 ps to 5 fs at a carrier wavelength of 780 nm. For tau <100 fs, the dominant channel for free electron generation is found to be either impact or multiphoton ionization (MPI) depending on the size of the band gap. The observed MPI rates are substantially lower than those predicted by the Keldysh theory. We demonstrate that sub-10-fs laser pulses open up the way to reversible nonperturbative nonlinear optics (at intensities greater than 1014 W/cm2 slightly below damage threshold) and to nanometer-precision laser ablation (slightly above threshold) in dielectric materials.
Ablation experiments employing Ti:sapphire laser pulses with durations from 30 to 340 fs (centre wavelength 800 nm, repetition rate 1 kHz) were performed in air. Absorbing filters (Schott BG18 and BG36) served as targets. The direct focusing technique was used under single- and multi-pulse irradiation conditions. Ablation threshold fluences were determined from a semi-logarithmic plot of the ablation crater diameter versus laser fluence. The threshold fluence decreases for a shorter pulse duration and an increasing number of pulses. The multi-pulse ablation threshold fluences are similar to those of undoped glass material (~1 J cm-2). That means that the multi-pulse ablation threshold is independent on the doping level of the filters. For more than 100 pulses per spot and all pulse durations applied, the threshold fluence is practically constant. This leads to technically relevant ablation threshold values.
Textile, aluminium and polyethylene used as components in laser protection curtains were investigated with respect to their ablation behaviour. Employing 33-fs pulses (800 nm wavelength, 1 kHz repetition rate), ex situ geometrical measurements of the ablation cavities and in situ acoustic investigations with a microphone were performed to determine the ablation thresholds in the single- and multi-pulse cases. The acoustical method proved advantageous for complex surface morphologies and/or single laser pulse interactions. Incubation phenomena can be observed for all the materials studied. Technically relevant multi-pulse ablation thresholds are presented and are compared with the single-pulse (1-on-1) irradiation.
A first investigation on the ablation of composite materials like carbon and silicon-carbide reinforced alumo- and borosilicate glasses by 300 fs laser pulses (620 nm) in comparison to experiments with 17 ns pulse excimer laser (308 nm) treatment is presented. In all composites, femtosecond laser scans with a fluence of less than 2 J cm-2 produce well defined cuts with smooth side walls in contrast to the nanosecond laser result where extremely incongruent ablation is observed. Visible lasers should not be applicable because SiC and the glasses are practically transparent. Visible subpicosecond pulses of high intensity in the TW cm-2 range allow multi-photon absorption accompanied by incubation phenomena. The morphology of the groove edges reveal the contrasting ablation thresholds and rates of the fibre and glass materials. The ablation thresholds of the transparent components, i.e. the glass matrices and SiC, are about one order of magnitude greater than that of carbon which is ~ 0.15 J cm-2. Incubation effects are important for the absorption mechanisms in the transparent materials. When a critical number of pulses has not been reached at the SiC-glass composites, only the glass is preferentially ablated, and the fibres remain intact. This is in contrast to the C-glass composites where the ablation behaviour is opposite.
High-power lasers in industrial and R & D applications raise the general problem of reliability and degradation of optical components. A systematic study of nonlinear interaction of various transparent dielectric materials as e.g. glasses, fused silica, and polymers, with laser-pulses in the intensity range of up to 1013 W cm-2 is presented. On the other hand, femtosecond-pulse laser processing in the visible spectral range (300 fs; 620 nm, ~ 2 eV) allows precise microstructuring of transparent dielectrics without disruption of the remnant material. Damage and ablation threshold fluences occur above 1.2 J cm-2 at both silicate glasses and fused silica. Two different photon absorption mechanisms have been observed. The first occurs during the initial laser pulses in the incubation range. There, multiphoton absorption results in moderate energy volume densities. These are sufficient to generate morphological changes and optically active defect sites (colour centres) which provide a much higher absorptivity relevant for the second mechanism. It results in gasification without participation of melt.
Hydrogen-Containing Amorphous Carbon Layers as Optical Materials in the Near-IR Spectral Range
(2007)
Hydrogenated amorphous carbon layers were deposited on various substrates by means of a plasma CVD process with a RF substrate bias as well as an ECR plasma source. The optical properties of the a-C:H layers were obtained via spectroscopic ellipsometry and correlated with their mechanical and chemical properties. The layers from pure RF plasma exhibit a higher absorption constant in the visible spectral range and a higher refractive index. All layers are nearly transparent in the NIR spectral range making them candidates for optical thin layer systems. The laser damage behaviour of the a-C:H layers was investigated with ultrashort pulses. The damage thresholds were consistent with the absorption constants of the layers. Interesting damage morphologies were observed indicating a sensitivity of this experiment to sub-structures in the layer.
High-power optical multimode fibers are essential components for materials processing and surgery and can limit the performance of expensive systems due to breakdown at the end faces. The aim of this paper is the determination of laser-induced damage thresholds (LIDT) of fibers (FiberTech) and preforms (Heraeus Suprasil F300). Preforms served as models. They were heated up to maximum temperatures of 1100, 1300 and 1500°C and cooled down to room temperature at rates of 10 K min-1 (oven) and ~105 K min-1 (quenched in air) to freeze in various structural states simulating different conditions similar to a drawing process during the production of fibers. Single- and multi-pulse LIDT measurements were done in accordance with the relevant ISO standards. Nd:YAG laser pulses with durations of 15 ns (1064 nm wavelength) and 8.5 ns (532 nm) at a repetition rate of 10 Hz were used. For the preforms, LIDT values (1-on-1) ranged from 220 to 350 J/cm² (1064 nm) and from 80 to 110 J/cm² (532 nm), respectively. A multi-pulse impact changed the thresholds to lower values. The LIDT (1064 nm wavelength) of the preforms can be regarded as a lower limit for those of the fibers.
Single- and multi-shot ablation thresholds of gold films in the thickness range of 311400 nm were determined employing a Ti:sapphire laser delivering pulses of 28 fs duration, 793 nm center wavelength at 1 kHz repetition rate. The gold layers were deposited on BK7 glass by an electron beam evaporation process and characterized by atomic force microscopy and ellipsometry. A linear dependence of the ablation threshold fluence Fth on the layer thickness d was found for d ≤ 180 nm. If a film thickness of about 180 nm was reached, the damage threshold remained constant at its bulk value. For different numbers of pulses per spot (N-on-1), bulk damage thresholds of ~0.7 J cm-2 (1-on-1), 0.5 J cm-2 (10-on-1), 0.4 J cm-2 (100-on-1), 0.25 J cm-2 (1000-on-1), and 0.2 J cm-2 (10000-on-1) were obtained experimentally indicating an incubation behavior. A characteristic layer thickness of Lc 180 nm can be defined which is a measure for the heat penetration depth within the electron gas before electronphonon relaxation occurs. Lc is by more than an order of magnitude larger than the optical absorption length of α-1 12 nm at 793 nm wavelength.
Optical multimode fibers are applied in materials processing (e.g. automotive industry), defense, aviation technology, medicine and biotechnology. One challenging task concerning the production of multimode fibers is the enhancement of laser-induced damage thresholds. A higher damage threshold enables a higher transmitted average power at a given fiber diameter or the same power inside a thinner fiber to obtain smaller focus spots.
In principle, different material parameters affect the damage threshold. Besides the quality of the preform bulk material itself, the drawing process during the production of the fiber and the preparation of the fiber end surfaces influence the resistance. Therefore, the change of the laser-induced damage threshold of preform materials was investigated in dependence on a varying thermal treatment and preparation procedure.
Single and multi-pulse laser-induced damage thresholds of preforms (F300, Heraeus) were measured using a Q-switched Nd:YAG laser at 1064 nm wavelength emitting pulses with a duration of 15 ns, a pulse energy of 12 mJ and a repetition rate of 10 Hz. The temporal and spatial shape of the laser pulses were controlled accurately.
Laser-induced damage thresholds in a range from 150 J cm-2 to 350 J cm-2 were determined depending on the number of pulses applied to the same spot, the thermal history and the polishing quality of the samples, respectively.
High-power optical multimode fibers are essential components for materials processing
and surgery and can limit the reliability of expensive systems due to breakdown at the end faces.
The breakdown threshold of fibers is determined by intrinsic materials properties and parameters of
the technology applied. The aim of this paper is the identification of technological parameters that
are crucial for the fiber quality.
Fibers were drawn from preforms of Heraeus SWU with core material F300 and a low amount of
OH-. Both, the cladding (fluorine doped SiO2) to core diameter ratio (CCDR) and the drawing speed
were varied. CCDR values between 1.05 and 1.4 were used. Afterwards, the laser-induced damage
thresholds (LIDT) of the fibers were determined. For comparison, also samples from preforms,
which underwent different thermal treatments above the transition temperature, were tested with
respect to their damage resistivity. Single and multi pulse LIDT measurements were done in
accordance with the relevant ISO standards. Nd:YAG laser pulses with durations of 15 ns (1064 nm
wavelength) and 8.5 ns (532 nm) at a repetition rate of 10 Hz were utilized. For the fibers, LIDT
values (1-on-1, 1064 nm and 532 nm) increased with growing CCDR and with decreasing drawing
velocities.
Cleaning of paper is a challenging task due to the fact that a contamination should be removed and a fragile organic original material has to be preserved. Pulsed laser cleaning of artificially soiled Whatman© filter paper samples serving as models for historical paper was performed. Different cleaning strategies employing 8-ns laser pulses at 532 nm wavelength were applied to clean paper avoiding undesired effects like discoloration (yellowing) and mechanical deterioration of the substrate. Multi shot experiments with low-energy pulses were compared with single pulse investigations utilizing high pulse energies achieving a constant energy load incident on the samples in both cases. The cleaning efficiency and possible yellowing effects were evaluated by means of a multi spectral imaging system. An extensive microscopic analysis of the cleaned parts of the samples provided insight into the remaining soiling on the surface and in the bulk of the paper material after laser treatment. As a reference, a hard and a soft eraser were used to clean the samples.
The influence of different laser pulse lengths on the removal of a polymer layer from metal substrates was investigated. As model systems, doped poly(methylmetacrylate) (PMMA) on titanium and tungsten substrates were selected.
The ablation threshold and irradiation spot morphology of titanium and tungsten were compared for femtosecond (fs) and nanosecond (ns) laser irradiation and different pulse numbers. Nanosecond laser treatment resulted in a non-homogeneous surface morphology for both titanium and tungsten substrates. Femtosecond irradiation of tungsten revealed a homogeneous ablation spot with little changes in the surface morphology. For titanium, the formation of columnar structures within the irradiation spot was observed.
Two different dopant concentrations were used for PMMA to achieve an equal linear absorption coefficient for the femto- and nanosecond laser wavelengths of 790 and 1064 nm. The best results were achieved for the removal of doped PMMA by femtosecond laser irradiation, where only a minimal modification of the metal surface was detected. In the case of nanosecond laser exposure, a pronounced change of the structure was observed, suggesting that damage-free cleaning of the selected metal may only be possible using femtosecond laser pulses. Different experimental parameters, such as laser fluence, pulse repetition rate and sample speed were also investigated to optimize the cleaning quality of doped PMMA from tungsten substrates with femtosecond laser pulses.
The formation of near-wavelength laser-induced periodic surface structures (LIPSS) on silicon upon irradiation with sequences of Ti:sapphire femtosecond laser pulse pairs (pulse duration 150 fs, central wavelength 800 nm) is studied theoretically. For this purpose, the nonlinear generation of conduction band electrons in silicon and their relaxation is numerically calculated using a two-temperature model approach including intrapulse changes of optical properties, transport, diffusion and recombination effects. Following the idea that surface plasmon polaritons (SPP) can be excited when the material turns from semiconducting to metallic state, the 'SPP active area' is calculated as function of fluence and double-pulse delay up to several picoseconds and compared to the experimentally observed rippled surface areas. Evidence is presented that multi-photon absorption explains the large increase of the rippled area for temporally overlapping pulses. For longer double-pulse delays, relevant relaxation processes are identified. The results demonstrate that femtosecond LIPSS on silicon are caused by the excitation of SPP and can be controlled by temporal pulse shaping.
The formation of nearly wavelength-sized laser-induced periodic surface structures (LIPSSs) on single-crystalline silicon upon irradiation with single or multiple femtosecond-laser pulses (pulse duration τ=130 fs and central wavelength λ=800 nm) in air is studied experimentally and theoretically. In our theoretical approach, we model the LIPSS formation by combining the generally accepted first-principles theory of Sipe and co-workers with a Drude model in order to account for transient intrapulse changes in the optical properties of the material due to the excitation of a dense electron-hole plasma. Our results are capable to explain quantitatively the spatial periods of the LIPSSs being somewhat smaller than the laser wavelength, their orientation perpendicular to the laser beam polarization, and their characteristic fluence dependence. Moreover, evidence is presented that surface plasmon polaritons play a dominant role during the initial stage of near-wavelength-sized periodic surface structures in femtosecond-laser irradiated silicon, and it is demonstrated that these LIPSSs can be formed in silicon upon irradiation by single femtosecond-laser pulses.
The formation of nearly wavelength-sized laser-induced periodic surface structures (LIPSS) on
single-crystalline silicon upon irradiation with single (N = 1) and multiple (N ≤ 1000) linearly
polarized femtosecond (fs) laser pulses (pulse duration τ = 130 fs, central wavelength λ = 800 nm)
in air is studied experimentally. Scanning electron microscopy (SEM) and optical microscopy are
used for imaging of the ablated surface morphologies, both revealing LIPSS with periodicities close
to the laser wavelength and an orientation always perpendicular to the polarization of the fs-laser
beam. It is experimentally demonstrated that these LIPSS can be formed in silicon upon irradiation
by single fs-laser pulses—a result that is additionally supported by a recent theoretical model.
Two-dimensional Fourier transforms of the SEM images allow the detailed analysis of the
distribution of the spatial frequencies of the LIPSS and indicate, at a fixed peak fluence, a
monotonous decrease in their mean spatial period between ~770 nm (N = 1) and 560 nm (N
= 1000). The characteristic decrease in the LIPSS period is caused by a feedback-mechanism acting
upon excitation of surface plasmon polaritons at the rough silicon surface which is developing under
the action of multiple pulses into a periodically corrugated surface.
A new approach is presented to quantify the so-called "heat affected zone" (HAZ) during
femtosecond laser pulse processing. Ablation of titanium nitride (TiN) thin films (~3 μm
thickness) by multiple femtosecond laser pulses (τ=130 fs, λ=800 nm) in air environment was
studied by means of two different surface analytical methods both being sensitive to chemical
alterations at the surface. Scanning Auger electron microscopy was applied for a visualization of the
spatial distribution of specific elements (Ti, O) within the laser-modified areas. The chemical state
of the irradiated surface was revealed by complementary x-ray photoelectron spectroscopy. Both
methods were used for a depth-profiling chemical analysis (tracking the elements Ti, N, O, and C)
using an Ar-ion beam for surface sputtering. In a narrow laser fluence range slightly below the
ablation threshold of TiN significant superficial oxidation can be observed leading to the formation
of substoichiometric TiO2-x. At fluences above the ablation threshold, an increased titanium
concentration is observed within the entire ablation craters. Following upon sputter removal the
elemental distribution into the depth of the nonablated material, the results allow an estimation of
the heat-affected zone for femtosecond laser ablation in air environment. According to our analyses,
the HAZ extends up to a few hundreds of nanometers into the nonablated material.
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 removal of a 75- to 90-nm-thick passivating silicon nitride antireflection coating from standard textured multicrystalline silicon photovoltaic wafers with a typical diffused 90-Ω/sq-emitter upon irradiation with near-infrared femtosecond laser pulses (790 nm central wavelength, 30 fs pulse duration) is studied experimentally. The laser irradiation areas are subsequently characterized by complementary optical microscopy, scanning electron microscopy and depth profiling chemical analyses using secondary ion mass spectrometry. The results clarify the thin-film femtosecond laser ablation scenario and outline the process windows for selective antireflection coating removal.
Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications.
Ultrashort pulse laser processing can result in the secondary generation of unwanted X-rays if a critical laser irradiance of about 10^13 W/cm^2 is exceeded. Spectral X-ray emissions were investigated during the processing of tungsten and steel using three complementary spectrometers (based on CdTe and silicon drift detectors) simultaneously for the identification of a worst-case spectral scenario. Therefore, maximum X-ray photon energies were determined, and corresponding dose equivalent rates were calculated. An ultrashort pulse laser workstation with a pulse duration of 274 fs, a center wavelength of 1030 nm, pulse repetition rates between 50 kHz and 200 kHz, and a Gaussian laser beam focused to a spot diameter of 33 µm was employed in a single pulse and burst laser operation mode. Different combinations of laser pulse energy and repetition rate were utilized, keeping the average laser power constant close to the maximum power of 20 W. Peak irradiances ranging from 7.3 × 10^13 W/cm^2 up to 3.0 × 10^14 W/cm^2 were used. The X-ray dose equivalent rate increases for lower repetition rates and higher pulse energy if a constant average power is used. Laser processing with burst mode significantly increases the dose rates and the X-ray photon energies. A maximum X-ray photon energy of about 40 keV was observed for burst mode processing of tungsten with a repetition rate of 50 kHz and a peak irradiance of 3 × 10^14 W/cm^2.
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.
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.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of silicon by multiple (N = 100) linearly polarized Ti:sapphire femtosecond laser pulses (duration τ = 30 fs, center wavelength λ0 ~ 790 nm) is studied experimentally in air and water environment. The LIPSS surface morphologies are characterized by scanning electron microscopy and their spatial periods are quantified by two-dimensional Fourier analyses. It is demonstrated that the irradiation environment significantly influences the periodicity of the LIPSS. In air, so-called low-spatial frequency LIPSS (LSFL) were found with periods somewhat smaller than the laser wavelength (ΛLSFL ~ 0.7 × λ0) and an orientation perpendicular to the laser polarization. In contrast, for laser processing in water a reduced ablation threshold and LIPSS with approximately five times smaller periods ΛLIPSS ~ 0.15 × λ0 were observed in the same direction as in air. The results are discussed within the frame of recent LIPSS theories and complemented by a thin film based surface plasmon polariton model, which successfully describes the tremendously reduced LIPSS periods in water.
Laser-induced periodic surface structures (LIPSS, ripples) were generated on stainless steel (100Cr6) and titanium alloy (Ti6Al4V) surfaces upon irradiation with multiple femtosecond laser pulses (pulse duration 30 fs, central wavelength 790 nm). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning geometry for the processing of large surface areas (5 × 5 mm²) covered homogeneously by the nanostructures. The irradiated surface regions were subjected to white light interference microscopy and scanning electron microscopy revealing spatial periods around 600 nm. The tribological performance of the nanostructured surface was characterized by reciprocal sliding against a ball of hardened steel in paraffin oil and in commercial engine oil as lubricants, followed by subsequent inspection of the wear tracks. For specific conditions, on the titanium alloy a significant reduction of the friction coefficient by a factor of more than two was observed on the laser-irradiated (LIPSS-covered) surface when compared to the non-irradiated one, indicating the potential benefit of laser surface structuring for tribological applications.
The formation of laser-induced periodic surface structures (LIPSS, ripples) upon irradiation of silicon with multiple irradiation sequences consisting of femtosecond laser pulse pairs (pulse duration 150 fs, central wavelength 800 nm) is studied numerically using a rate equation system along with a two-temperature model accounting for one- and two-photon absorption and subsequent carrier diffusion and Auger recombination processes. The temporal delay between the individual equal-energy fs-laser pulses was varied between 0 and ~4 ps for quantification of the transient carrier densities in the conduction band of the laser-excited silicon. The results of the numerical analysis reveal the importance of carrier generation and relaxation processes in fs-LIPSS formation on silicon and quantitatively explain the two time constants of the delay-dependent decrease of the low spatial frequency LIPSS (LSFL) area observed experimentally. The role of carrier generation, diffusion and recombination is quantified individually.
For many applications, optical multimode fibers are used for the transmission of powerful laser radiation. High light throughput and damage resistance are desirable. Laser-induced breakdown at the end faces of fibers can limit their performance. Therefore, the determination of laser-induced damage thresholds (LIDT) at the surface of fibers is essential.
Nanosecond (1064 nm and 532 nm wavelength) single-shot LIDT were measured according to the relevant standard on SiO2 glass preforms (Suprasil F300) as basic materials of the corresponding fibers. For 10 kinds of fused silica fibers (FiberTech) with core diameters between 180 µm and 600 µm, an illumination approach utilizing a stepwise increase of the laser fluence on a single spot was used. For both wavelengths, the LIDT values (0% damage probability) obtained by means of the two methods were compared. The influence of surface preparation (polishing) on damage resistance was investigated. For equal surface finishing, a correlation between drawing speed of the fibers and their surface LIDT values was found. In addition to the surface measurements, bulk LIDT were determined for the preform material.
Single and multi pulse laser-induced damage thresholds (LIDT) of core, cladding, and coating materials of high-power
optical multimode fibers were determined in accordance with ISO 11254 for 532 nm and 1064 nm wavelength in the 10-ns
pulse duration regime with spatial Gaussian beam shape. For all-silica fibers, LIDT increases with rising core diameter in a range between 100-600 µm for a constant cladding-core ratio of 1.2. The damage resistance of the low refracting cladding (0.3 % fluorine doped fused silica) is comparable to the undoped SiO2 core. Coating materials show significantly lower LIDT than light-guiding parts of the fibers.
Hydrogenated amorphous carbon layers were deposited on BK7 glass in a plasma-assisted chemical vapor deposition
process. Low and high refracting films with thicknesses d ranging from 11 nm to 5.8 µm were produced having refractive
indices n between 1.68 and 2.41 and linear absorption coefficients of α~100 cm-1 and α~20000 cm-1 at 800 nm wavelength as a result of different plasma modes. Laser ablation thresholds Fth in dependence on d were determined using 30-fs laser pulses. Low absorbing layers show a constant Fth while Fth increases with rising d up to the optical penetration depth of light α-1 for high absorbing films.
Femtosecond lasers provide a novel method of attaching bioceramic material to a titanium alloy, thereby improving the quality of bone implants. The ultrashort 30 fs laser pulses (790 nm wavelength) penetrate a thin dip-coated layer of fine ceramic powder, while simultaneously melting a surface layer of the underlying metal. The specific adjustment of the laser parameters (pulse energy and number of pulses per spot) avoids unnecessary melting of the bioactive calcium phosphate, and permits a defined thin surface melting of the metal, which in turn is not heated throughout, and therefore maintains its mechanical stability. It is essential to choose laser energy densities that correspond to the interval between the ablation fluences of both materials involved: about 0.1-0.4 J cm-2. In this work, we present the first results of this unusual technique, including laser ablation studies, scanning electron microscopy and optical microscope images, combined with EDX data.
The formation of laser-induced periodic surface structures (LIPSS) upon irradiation of silicon wafer surfaces by linearly polarized Ti:sapphire femtosecond laser pulses (pulse duration 130 fs, central wavelength 800 nm) is studied experimentally and theoretically. In the experiments, so-called low-spatial frequency LIPSS (LSFL) were found with periods smaller than the laser wavelength and an orientation perpendicular to the polarization. The experimental results are analyzed by means of a new theoretical approach, which combines the widely accepted LIPSS theory of Sipe et al. with a Drude model, in order to account for transient (intra-pulse) changes of the optical properties of the irradiated materials. It is found that the LSFL formation is caused by the excitation of surface plasmon polaritons, SPPs, once the initially semiconducting material turns to a metallic state upon formation of a dense free-electron-plasma in the material and the subsequent interference between its electrical field with that of the incident laser beam resulting in a spatially modulated energy deposition at the surface. Moreover, the influence of the laser-excited carrier density and the role of the feedback upon the multi-pulse irradiation and its relation to the excitation of SPP in a grating-like surface structure is discussed.
Bone implants made of metal, often titanium or the titanium alloy Ti6Al4V, need to be surface treated to become bioactive. This enables the formation of a firm and durable connection of the prosthesis with the living bone. We present a new method to uniformly cover Ti6Al4V with a thin layer of ceramics that imitates bone material. These calcium alkali phosphates, called GB14 and Ca10, are applied to the metal by dip coating of metal plates into an aqueous slurry containing the fine ceramic powder. The dried samples are illuminated with the 790 nm radiation of a pulsed femtosecond laser. If the laser fluence is set to a value just below the ablation threshold of the ceramic (ca. 0.4 J/cm²) the 30 fs laser pulses penetrate the partly transparent ceramic layer of 20–40 µm thickness. The remaining laser fluence at the ceramic–metal interface is still high enough to generate a thin metal melt layer leading to the ceramic fixation on the metal. The laser processing step is only possible because Ti6Al4V has a lower ablation threshold (between 0.1 and 0.15 J/cm²) than the ceramic material. After laser treatment in a fluence range between 0.1 and 0.4 J/cm², only the particles in contact with the metal withstand a post-laser treatment (ultrasonic cleaning). The non-irradiated rest of the layer is washed off. In this work, we present results of a successful ceramic fixation extending over larger areas. This is fundamental for future applications of arbitrarily shaped implants.
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.
Cleaning of artificially soiled paper using nanosecond, picosecond and femtosecond laser pulses
(2010)
Cleaning of cultural assets, especially fragile
organic materials like paper, is a part of the conservation
process. Laser radiation as a non-contact tool offers
prospects for that purpose. For the studies presented here,
paper model samples were prepared using three different paper
types (pure cellulose, rag paper, and wood-pulp paper).
Pure cellulose serves as reference material. Rag and woodpulp
paper represent essential characteristics of the basic
materials of real-world artworks. The papers were mechanically
soiled employing pulverized charcoal. Pure and artificially soiled paper samples were treated with laser pulses of
28 fs (800 nm wavelength) and 8–12 ns (532 nm) duration in
a multi pulse approach. Additionally, the cellulose reference
material was processed with 30 ps (532 nm) laser pulses.
Damage and cleaning thresholds of pure and soiled paper
were determined for the different laser regimes. Laser working
ranges allowing for removal of contamination and avoiding
permanent modification to the substrate were found.
The specimens prior and after laser illumination were characterized
by light-optical microscopy (OM) and scanning
electron microscopy (SEM) as well as multi spectral imaging
analysis. The work extends previous nanosecond laser
cleaning investigations on paper into the ultra-short pulse
duration domain.
The possibility to excite surface plasmon polaritons (SPPs) at the interface between two media depends on the optical properties of both media and geometrical aspects. Specific conditions allowing the coupling of light with a plasmon-active interface must be satisfied. Plasmonic effects are well described in noble metals where the imaginary part of the dielectric permittivity is often neglected ('perfect medium approximation (PMA)'). However, some systems exist for which such approximation cannot be applied, hence requiring a refinement of the common SPP theory. In this context, several properties of SPPs such as excitation conditions, period of the electromagnetic field modulation and SPP lifetime then may strongly deviate from that of the PMA. In this paper, calculations taking into account the imaginary part of the dielectric permittivities are presented. The model identifies analytical terms which should not be neglected in the mathematical description of SPPs on lossy materials. These calculations are applied to numerous material combinations resulting in a prediction of the corresponding SPP features. A list of plasmon-active interfaces is provided along with a quantification of the above mentioned SPP properties in the regime where the PMA is not applicable.
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).
Laser-induced periodic surface structures (LIPSS, ripples) were processed on steel (X30CrMoN15-1) and titanium (Ti) surfaces by irradiation in air with linear polarized femtosecond laser pulses with a pulse duration of 30 fs at 790 nm wavelength. For the processing of large LIPSS covered surface areas (5 mm × 5 mm), the laser fluence and the spatial spot overlap were optimized in a sample-scanning geometry. The laser-processed surfaces were characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). Spatial LIPSS periods between 450 and 600 nm were determined. The nanostructured surface regions were tribologically tested under reciprocal sliding conditions against a 10-mm diameter ball of hardened 100Cr6 steel. Paraffin oil and engine oil were used as lubricants for 1000 sliding cycles at 1 Hz with a normal load of 1.0 N. The corresponding wear tracks were analyzed by OM and SEM. In particular cases, the laser-generated nanostructures endured the tribological treatment. Simultaneously, a significant reduction of the friction coefficient and the wear was observed in the laser-irradiated (LIPSS-covered) areas when compared to the non-irradiated surface. The experiments reveal the potential benefit of laser surface structuring for tribological applications.
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.
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.