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Zusammenfassung
The surface chemical modification of polyurethane (PU) films was performed by an UV laser-induced chemical reaction in a polysaccharide solution. This process may be applicable as hydrophilic packaging of implantable medical devices and in vivo sensors. When a PU film in contact with an aqueous alginic acid (AAC) solution was irradiated with a XeCl laser, the PU film turned hydrophilic. Contact angles of water on the film were reduced from 110° to 60°. Since light absorption of the AAC solution at 308 nm was negligibly small, reactive sites were generated solely on the PU surface. There, AAC could be immobilized by chemical bonds thus allowing for a nanometer-scaled grafting of this biomolecule. The mechanism was investigated by surface analyses with Fourier-transform infrared spectroscopy (FT-IR), dye staining, ultraviolet-visible (UV-VIS) spectroscopy, and scanning electron microscopy (SEM) techniques. A one-photon photochemical process could beidentified.
Optical filters and fabrics are important parts of laser safety equipment such as goggles and curtains. A choice of these materials with varying absorption spectra is investigated with respect to their resistance to Ti:sapphire femtosecond laser radiation (800 nm wavelength, 1 kHz repetition rate). Pulse durations down to 30 fs and multiple-pulse irradiation conditions are employed to evaluate technically relevant damage thresholds. The ablation threshold fluences of the absorbing filters are comparable to those observed for transparent materials with 30-fs-pulses. These investigations together with scanning electron microscopy of the surface morphology after laser treatment provide insight into the interaction mechanism of the short pulses with the materials.
The removal and accelerated corrosion monitoring of metal coating systems is of general interest in materials science
and engineering technology. The femtosecond and nanosecond laser ablation and delamination at 800 nm and 532 nm,
respectively, of anodic oxide layers on aluminium alloys in electrolyte contact were investigated. Laser-induced
modifications of the oxide layer resulted in an ionic contact between electrolyte and metal, which produced a current
transient and thus allowed the in-situ electrochemical monitoring of the modification. Oxide coatings with different
optical properties, almost transparent and opaque, were examined. The transparent anodic oxides showed contrasting
ablation mechanisms in the nanosecond and femtosecond pulse duration regime: nanosecond pulses caused spallation,
whereas femtosecond treatment led to ablation. Current signals measured in the transparent film were consistent with
light absorption below the metal-oxide interface and with film spallation. Irradiation of the opaque coating yielded ionic
current transients within the so-called shock-affected-zone of the oxide layer. This investigation provided insight into the
role of the penetration depth of light and the heat-affected zone, the extent of the shock-affected zone, and the defect
formation in the coating and at the solid-solid interface between metal and oxide.
Zusammenfassung
Laser pulses in the 10-fs domain provide a quality of micromachining of fused silica and borosilicate glass that is unobtainable with longer pulses in the range of several 100 femtoseconds up to picoseconds. The shortening of the pulses reduces the statistical behavior of the material removal and the ablation process thus attains a more deterministic and reproducible character. The improved reproducibility of ablation is accompanied by significantly smoother morphology. This offers the potential for lateral and vertical machining precision of the order of 100 nm and 10 nm, respectively.
Abstract Femtosecond laser micromachining has excited vivid attention in various industri-
al fields and in medicine owing to the advantages of ultrashort laser pulses compared to
long-pulse treatment.These are mainly the reduction of the laser fluence needed to induce
ablation and the improvement of the contour sharpness of the laser-generated structures.
Recently,special attention was paid to femtosecond laser experiments on nonabsorbing in-
organic dielectrics.This is due to the fact that optical damage in dielectric optical elements
limits the performance of high-power laser systems.Despite the fact that a large variety of
organic polymers can be machined with excimer lasers successfully,the involvement of
thermal processes can lead to an unsatisfactory quality of the structures.Ultrashort,fs-laser
pulses might be an alternative for the treatment of polymers.Therefore,femtosecond laser
machining investigations of dielectrics and polymers are reviewed in this paper.Similarities
and differences of the ablation behavior of both material classes are discussed.The influ-
ence of the bandgap on the ablation threshold in dependence on the pulse duration,the en-
hancement of the machining precision with a shortening of the pulse duration,incubation
phenomena,and morphological features appearing on the surface after femtosecond laser
treatment are mentioned.Possible applications,e.g.,in medicine and biosensors,are de-
scribed.
We present surface micro-modifications of bariumalumoborosilicate glasses with a high transformation temperature near 700 °C. Laser processing of the glass substrate was realized by using ultra-short laser pulses at 800 nm. The morphological conversion of the laser-treated surfaces was characterized by scanning force microscopy and nano-indentation. A hardness increase by at least a factor of six on the laser ablation crater edge relative to illuminated non- ablated areas shows that the material in the crater walls underwent drastic morphological and mechanical changes. In this heat- and shock-affected zone, the material became more elastic as a result of increased stress.
Femtosecond-pulse laser ablation of dental hydroxyapatite and single-crystalline fluoroapatite
(1999)
Laser microdrilling of healthy human enamel and dentine using 300 fs pulses at a wavelength of 615 nm and 3 Hz repetition rate leads to an enhanced structuring quality in comparison with nanosecond-laser results. Microcracking and damage to neighboring tissue can be reduced. Ablation threshold fluences for 100 laser pulses of 0.3 J cm-2 (human dentine), 0.6 J cm-2 (human enamel) and 0.8 J cm-2 (single crystalline fluoroapatite) could be determined. Ablation depths per pulse below 1 7m were observed.
Zusammenfassung
The threshold fluences for laser-induced damage of fused silica with single 5-fs pulses from a Ti:sapphire laser system were determined by extrapolating the ablated volume to zero. These thresholds are about 4 times as high as the values previously obtained from multi-shot experiments. This result is interpreted in terms of an irreversible modification of the original material below the single-shot threshold (incubation).
Ablation experiments in several glasses with single and multishot irradiation by laser pulses in the 10-fs pulse duration domain are presented; physical and technological implications are discussed. We demonstrate that these short pulses offer the potential for lateral and vertical machining precision of the order of 100 nm.
Damage experiments of absorbing filters (Schott BG18 and BG36) were performed with Ti:sapphire laser pulses with durations from 30 fs to 340 fs (800 nm, 1 kHz) in air. The direct focusing technique was employed under single- and multi-pulse irradiation conditions. Ablation threshold fluences were determined from a semi-logarithmic plot of the ablation crater diameter vs. laser fluence. The damage threshold fluence decreases for shorter pulse durations. In the investigated pulse duration range, the measured multi-pulse ablation threshold fluences are practically similar to those of undoped glass material (~1 Jcm-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 saturates. This leads to technically relevant damage threshold values in the femtosecond laser pulse duration domain.
Commercially available absorption filters (Schott BG18 and BG36) were investigated with respect to their single- and
multi-pulse ablation threshold using laser pulses from a Ti:Sapphire laser in the range between 30 and 340 fs. It could be
observed, that the threshold fluence decreases for shorter pulse durations. The similarity of the measured multi-pulse
threshold fluences with those of undoped glass material (around 1 J/cm^2 for a pulse duration of 30 fs) suggests that, for
very short pulses, the threshold is independent on the doping level and therefore, linear absorption does not significantly
contribute to laser-induced damage. For >100 pulses per spot and all pulse durations applied, the threshold fluences
saturate. This independence on the number of applied pulses leads to technically relevant damage threshold values.
KrF excimer laser ablation of polyethylene terephthalate (PET), polyimide (PI) and polycarbonate (PC) in air was studied by an in situ monitoring technique using a microphone. The microphone signal generated by a short acoustic pulse represented the etch rate of laser ablation depending on the laser fluence, i.e., the ablation strength. From a linear relationship between the microphone output voltage and the laser fluence, the single-pulse ablation thresholds were found to be 30 mJ cm-2 for PET, 37 mJ cm-2 for PI and 51 mJ cm-2 for PC (20-pulses threshold). The ablation thresholds of PET and PI were not influenced by the number of pulses per spot, while PC showed an incubation phenomenon. A microphone technique provides a simple method to determine the excimer laser ablation threshold of polymer films.
Near-ablation threshold investigations focusing on the generation of periodic nanostructures and their correlation with physico-chemical
properties of the solid phase such as e.g., the material-dependent surface energy, were conducted. Molecular dynamic modelling in the
sub-picosecond time domain was used to consider ultrafast opto-electronic processes triggering surface reorganization reactions.
Fluid containment of solid interfaces showed strong influence on the resulting micro- and nanostructures due to its drastic reduction of the
surface energy. The phenomena are discussed in respect to the minimization of the surface free energy in dependence of material composition
and interfacial structure.
On the damage behavior of dielectric films when illuminated with multiple femtosecond laser pulses
(2005)
The physical effects reducing the damage threshold of dielectric films when exposed to multiple femtosecond pulses are investigated.
The measured temperature increase of a Ta2O5 film scales exponentially with the pulse fluence. A polarized luminescence signal is observed that
depends quadratically on the pulse fluence and is attributed to twophoton excitation of self-trapped excitons that form after band-to-band
excitation. The damage fluence decreases with increasing pulse number, but is independent of the repetition rate from 1 Hz to 1 kHz at a constant
pulse number. The repetition rate dependence of the breakdown threshold is also measured for TiO2 , HfO2,
Al2O3, and SiO2 films. A theoretical model is presented that explains these findings.
Femto- and nanosecond laser ablation of polymethylmethacrylate (PMMA) and PMMA doped with a linear absorber was
investigated in the infrared spectral region. Ablation thresholds were determined and incubation phenomena were identified. The
degree of incubation was calculated employing a phenomenological model. The influence of the pulse duration on the
machining quality of the polymers was examined. The presence of an absorbing chromophore is not a prerequisite for a
controllable fs-laser structuring in contrast to the ns-treatment. Surface swelling always accompanied ablation.
Femtosecond laser interaction with silicon was investigated in water and in air, with 130-fs laser pulses at 800 nm wavelength. Under water confinement, higher modification thresholds, lower ablation depths and similar incubation factors were found in comparison to the dry experiment. Morphological features of the laser-induced cavities also differed. In contrast to air experiments, debris redeposition was negligible, while the ablated material remained suspended in the water layer phase. Underwater cavities obtained at high fluences and high number of pulses per spot showed anomalous profiles, consistent with a strong spatial deformation of the laser beam coupled into the target. Ripples formed at the edges of the modified area showed varying spacings: f100 and f700 nm for water and air experiments, respectively. Differences to the air experiment were related to a complex combination of fluence-dependent non-linear effects occurring in the water layer and to pulse-number-dependent shielding effects induced by cavitation bubbles and suspended ablated
material.
Femtosecond pulse laser ablation of metallic, semiconducting, ceramic, and biological materials
(1994)
Production of holes and grooves of < 30 micrometers diameter with high aspect ratio value is a delicate task either for mechanical tools, or for conventional nanosecond pulse lasers like e.g. pulsed Nd:YAG or excimer lasers. They later tend to cause microcracks extending from an annular melting zone, or substantial disruption, respectively. Experimental results are presented which demonstrate that the development of intense ultrashort pulse laser systems (>> 1012 W cm-2, (tau) < 1 ps) opens up possibilities for materials processing by cold plasma generation and ablation of metals, semiconductors, ceramics, composites, and biological materials. A femtosecond and a nanosecond dye laser with pulse durations of 300 fs (< 200 (mu) J) and 7 ns (< 10 mJ), and center wavelengths at 612 and 600 nm, respectively, both focused on an area of the order of 10-5 cm2, have been applied either to absorbing substrates, like polycrystalline gold, silicon (111), aluminum nitride ceramics, or transparent materials, like synthetic and human dental hydroxyapatite composites, bone material, and human cornea transplants. The fs-laser generates its own absorption in transparent materials by a multiphoton absorption process, and thus forces the absorption of visible radiation. Because the time is too short (< ps) for significant transport of mass and energy, the beam interaction generally results in the formation of a thin plasma layer of approximately solid state density. Only after the end of the subpicosecond laser pulse, it expands rapidly away from the surface without any light absorption and further plasma heating. Therefore, energy transfer (heat and impulse) to the target material, and thermal and mechanical disruption are minimized. In contrast to heat- affected zones (HAZ's) generated by conventional nanosecond pulse lasers of the order of 1 - 10 micrometers , HAZ's of less than 0.02 micrometers were observed.
Structuring of dielectric and metallic materials with ultrashort laser pulses between 20 fs and 3 ps
(1997)
Laser-micromachining of barium aluminum borosilicate glass, fused silica and stainless steel has been extended down to a pulse duration of 20 fs generated by a Ti:sapphire laser system at a wavelength of 0.8 micrometer. A systematic study shows that, below 100 fs, an enhanced precision and a substantial decrease of the ablation threshold fluence in comparison to pulse laser processing with pulses in the picosecond and nanosecond range could be achieved. The physical mechanism and the technical relevance of this novel microtechnology is discussed.
In situ optical second-harmonic generation (SHG) on centrosymmetric crystalline semiconductor electrodes opens up a new field of in situ investigations of hurried solid state interfaces and metal front contacts relevant to electronic and photovoltaic devices, which are rarely accessible by other methods. Photoelectrochemical nanosecond- and femtosecond-pulse laser investigations of silicon (111) electrodes show that in situ SHG is feasible in such complex interfacial systems. In a p-p polarization configuration, the azimuthal dependence of the SHG from oxide-covered and bare n-Si (111) electrodes, with and without Ni contact deposits, have been studied. Etching and regrowth of silicon oxides as well as burried interfacial electric field distributions were monitored. In situ SHG is shown to be extremely sensitive to trapped interfacial charge, crystal misorientations and surface step arrays. An advantage of femtosecond-pulses is the fact that illumination fluences that are well below the damage threshold, but still with sufficient power density, can be applied. (Author)
In situ second harmonic generation measurements during the electrodeposition of Ni on n-Si(111)
(1993)
A femtosecond pulse laser in the visible spectral region shows promise as a potentially new powerful corneal sculpting tool. It combines the clinical and technical advantages of visible wavelengths with the high ablation quality observed with nanosecond-pulse excimer lasers at 193 nm. A femtosecond and a nanosecond dye laser with pulse durations of 300 fs and 7 ns, and centre wavelengths at 615 nm and 600 nm, respectively, both focused to an area of the order of 105 cm2, have been applied to human corneal ablation. Nanosecond laser pulses caused substantial tissue disruption within a 30100 m range from the excision edge at all fluences above the ablation threshold of F th60 J cm2 (I th9 GW cm2). Completely different excisions are produced by the femtosecond-pulse laser: high quality ablations of the Bowman membrane and the stroma tissue characterised by damage zones of less than 0.5 m were observed at all fluences above ablation threshold of F th1 J cm2 or I th3 TW cm2 (3×1012 W cm2). The transparent cornea material can be forced to absorb ultrashort pulses of extremely high intensity. The fs laser generates its own absorption by a multiphoton absorption process.
Ultra-short pulse laser seeding techniques for silicon crystallite growth on amorphous substrates
(1999)
Censorship of parts of written text was and is a common practice in totalitarian regimes. It is used to destroy information not approved by the political power. Recovering the censored text is of interest for historical studies of the text. This paper raises the question, whether a censored postcard from 1942 can be made legible by applying multispectral imaging in combination with laser cleaning. In the fields of art conservation (e.g. color measurements), investigation (e.g. Analysis of underdrawings in paintings), and historical document analysis, multispectral imaging techniques have been applied successfully to give visibility to information hidden to the human eye.
The basic principle of laser cleaning is to transfer laser pulse energy to a contamination layer by an absorption process that leads to heating and evaporation of the layer. Partial laser cleaning of postcards is possible; dirt on the surface can be removed and the obscured pictures and writings made visible again. We applied both techniques to the postcard. The text could not be restored since the original ink seems to have suffered severe chemical damage.
Optical fibers made of fused silica are a common method of transmitting high laser pulse energies. Failure of those fibers is a significant risk. The determination of laser-induced damage thresholds (LIDT) on fiber end facets according to ISO 21254 standard is needed. In the past, single pulse nanosecond laser experiments showed an improvement of LIDT with increasing fiber core diameter for 1064 nm wavelength and a constant beam diameter of 50 µm.
This paper pays particular attention to the influence of the laser beam diameter on damage resistance. All-silica fiber types (LEONI) with different core diameters (100–600 µm) were investigated using beam diameters in a range from 30 µm to 100 µm. For comparison experiments on fused silica preform material (Heraeus F300) were performed. On one hand, surface LIDT of fused silica preform material decreases significantly with increasing beam size. A model considering a random distribution of point defects explains the experimental data qualitatively. On the other hand, LIDT of fiber end facets stays constant. White light microscopy results suggest that the point defect density on fiber end facets is lower compared to the preform surface due to an excellent surface polish quality.
The surface of a titanium alloy (Ti6Al4V) implant material was covered with a bioactive calcium alkali phosphate ceramic with the aim to accelerate the healing and to form a stronger bond to living bone tissue. To fix the ceramic powder we used a femtosecond laser, which causes a thin surface melting of the metal. It is a requirement to prove that the laser irradiation would not reduce the lifetime of implants. Here we present the results of mechanical stability tests, determined by the rotating bending fatigue strength of sample rods. After describing the sample surfaces and their modifications caused by the laser treatment we give evidence for an unchanged mechanical stability. This applies not only to the ceramic fixation but also to a comparatively strong laser ablation.
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.
One of the most important materials presenting and witnessing human culture is paper. The cleaning of paper is often necessary because contamination must be removed so that the fragile organic substrate can be preserved. The conventional cleaning methods are mechanical or involve the application of chemicals. These methods can damage drawings or print layers to some extent or make the original paper substrate brittle. More specifically, the use of a scalpel blade can cause damage to fibers. Chemical cleaning is difficult to perform locally, can dissolve foreign matter that then migrates into the paper substrate, or involves volatile organic compounds that can be harmful to the conservator. There is, therefore, a need for new conservation technologies aimed at the safe cleaning of paper. Lasers have proved to be an appropriate tool for cleaning as the energy dose and penetration depth at the specific point of contamination can be controlled. Additionally, if used properly, laser cleaning is not destructive to the paper.
Because of the increasingly stringent requirements for fibers in high Performance applications, the Business Unit Fiber Optics of the Leoni Group and the German BAM Federal Institute for Materials Research and Testing are jointly tackling the challenge of investigating the damage thresholds of selected large core special fibers for the first time.
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 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.
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.
Laser-induced damage threshold (LIDT) testing of oxide and metal coatings with sub-30 fs pulses
(2007)
Laser-induzierte Zerstörung von optischen Komponenten bei Anwendung von Femtosekunden-Impulsen
(2008)
Laser cleaning of soiled paper is a challenging task due to the fact that a contamination has to be removed and a fragile organic material has to be preserved. The ejection of particles forms a significant channel for the removal of unwanted surface contaminations and can be exploited for an in-situ monitoring of the cleaning procedure. 532-nm-nanosecond single and multi pulse laser cleaning of artificially soiled Whatman© paper was performed. Particles were registered with a dust monitor. These in-situ experiments were combined with ex-situ investigations of cleaning and substrate damage thresholds by means of light and scanning electron microscopic techniques. The cleaning efficiency measured by a multi-spectral imaging system was compared to the in-situ particle monitoring. Additionally, possible color changes of the paper substrate were evaluated.
Mikromaterialbearbeitung mit ultrakurzen Laserimpulsen: Vorzüge, Probleme, Sicherheitsaspekte
(2005)
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.
Analyse häufig verwendeter europäischer Papiere. Im Fokus: Fasermaterial, Füllstoffe und Leimung
(2007)
Restauratoren können verschiedene Papierarten mit dem bloßen Auge aufgrund von Merkmalen in der Textur und der Oberflächenbeschaffenheit, seinem Aussehen im Durchlicht sowie an Griff und Klang grob unterscheiden. Dabei ist sich der Restaurator stets der Tatsache bewusst, dass es sich lediglich um eine erste grobe Einschätzung handeln kann. Erst bei mikroskopischen Analysen und physikalischen Experimenten treten Charakteristika zu Tage, die eine weitere Annäherung an die Zusammensetzung des Papiers und damit seiner Provenienz erlauben. Gegenstand dieser Arbeit war es, ein europäisches Hadernpapier, ein holzhaltiges Zeichenpapier und ein Whatman®-Filterpapier mit zwei mikroskopischen Methoden und einer Verbrennungstechnik zu untersuchen. Das Fasermaterial, die Füllstoffe, die Leimung und eventuelle Verunreinigungen wurden detailliert evaluiert. Neben konventioneller Lichtmikroskopie kam die weniger bekannte Umweltrasterelektronenmikroskopie (ESEM = Environmental Scanning Electron Microscopy) zum Einsatz, die neben der bildlichen Darstellung der Probenoberflächen zusätzlich eine Elementanalyse derselben gestattet. Letzteres erfordert allerdings das Vorhandensein eines zusätzlichen Röntgenspektrometers. Darüber hinaus wurden die verschiedenen Papiere trocken verascht. Es wurde eine oxidative Zerstörung der organischen Stoffe gewährleistet bis nur noch nichtbrennbare mineralische Asche zu verzeichnen war. Die Komplementarität der eingesetzten Methoden wird demonstriert und ein Einblick in die Zusammensetzung und Struktur der Papiere ermöglicht. Die Analysemethoden sind durch ihren partiell zerstörenden Charakter bzw. Limitierungen hinsichtlich der Objektgröße nur bedingt für die Untersuchung am Original geeignet, sehr wohl aber dafür, das Probenmaterial für Versuchsreihen genau zu definieren und zu standardisieren.
In recent years, femtosecond lasers matured from sensitive research setups to turnkey systems for an increasing number of applications. Now that running an ultra-short pulse laser system needs no longer a specialized scientist, safety issues become more crucial. Ultrashort laser pulses have extremely high peak powers and even scattered radiation may possess severe risks to the unprotected eye. Accordingly,
special protection schemes are necessary for these unique laser systems.
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.
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.
Characterization of laser-generated microparticles by means of a dust monitor and SEM imaging
(2006)
Nanosecond laser (1064 nm wavelength) cleaning of artificially soiled paper as a model sample simulating a real-world artwork was performed. During the cleaning process, the ejection of particles was monitored in situ by means of a dust monitor (8 size classes, ranging from 0.3 µm to >2 µm) and ex situ using a mini-cascade impactor (MKI, 5 stages). The cleaning result was analyzed by scanning electron microscopy (SEM) considering possible laser-induced damages to the substrate. Size distributions of emitted particles were measured depending on the processing parameters: laser fluence, F, and pulse number per spot, N. High numbers of large (>2 µm) particles were collected by the mini-cascade impactor indicating a gas dynamical liftoff process. Obviously, these particles were not affected by the laser-matter interaction. The different methods (SEM, MKI, and dust monitor) are compared with respect to their usefulness for a proper interpretation of the cleaning results.
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.
Subpicosecond Emission from Mercury and Silver into Electrolyte Solution: An Experimental Study
(1997)
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.