Femtosecond laser micromilling of Si wafers

Femtosecond laser micromilling of silicon is investigated using a regeneratively amplified 775 nm Ti:Sapphire laser with a pulse duration of 150 fs operating at 1 kHz repetition rate. The morphological observation and topological analysis of craters fabricated by single-shot laser irradiation indicated that the material removal is thermal in nature and there are two distinct ablation regimes of low fluence and higher fluence with logarithmical relations between the ablation depth and the laser fluence. Crater patterns were categorized into four characteristic groups and their formation mechanisms were investigated. Femtosecond laser micromilling of pockets in silicon was performed. The effect of process parameters such as pulse energy, translation speed, and the number of passes on the material removal rate and the formation of cone-shaped microstructures were investigated. The results indicate that the microstructuring mechanism has a strong dependence on the polarization, the number of passes and laser fluence. The optimal laser fluence range for Si micromilling was found to be 2-8 J/cm² and the milling efficiency attains its maximum between 10 and 20 J/cm².     

Analyses of surface coloration on TiO2 film irradiated with excimer laser

TiO₂ film of around 850 nm in thickness was deposited on a soda-lime glass by PVD sputtering and irradiated using one pulse of krypton-fluorine (KrF) excimer laser (wavelength of 248 nm and pulse duration of 25 ns) with varying fluence. The color of the irradiated area became darker with increasing laser fluence. Irradiated surfaces were characterized using optical microscopy, scanning electron microscopy, Raman spectroscopy and atomic force microscopy. Surface undergoes thermal annealing at low laser fluence of 400 and 590 mJ/cm². Microcracks at medium laser fluence of 1000 mJ/cm² are attributed to surface melting and solidification. Hydrodynamic ablation is proposed to explain the formation of micropores and networks at higher laser fluence of 1100 and 1200 mJ/cm². The darkening effect is explained in terms of trapping of light in the surface defects formed rather than anatase to rutile phase transformation as reported by others. Controlled darkening of TiO₂ film might be used for adjustable filters.     

Laser surface treatment of screen-printed carbon nanotube emitters for enhanced field emission

This paper investigates the surface treatment of screen-printed carbon nanotube (CNT) emitters using a 248 nm (KrF) excimer laser. The field emission characteristics of the CNT emitters are measured following irradiation using laser fluences ranging from 80 to 400 mJ/cm². The results show that the turn-on electric field, the current density, and the distribution of the emission sites are highly dependent on the value of the laser fluence and are optimized at a fluence of 150 mJ/cm². Two distinct laser fluence regimes are identified. In the low fluence regime, i.e. 80-150 mJ/cm², the surface treatment process is dominated by a photo ablation mechanism, which results in the gradual removal of the binding material from the cathode surface and leads to an improvement in the emission characteristics of the CNT cathodes with an increasing fluence. However, in the high fluence regime, i.e. 150-400 mJ/cm², the thermal ablation mechanism dominates; resulting in a removal of the CNTs from the cathode surface and a subsequent degradation in the emission characteristics.     

Laser fluence, repetition rate and pulse duration effects on paint ablation

The efficiency (mm³/(J pulse)) of laser ablation of paint was investigated with nanosecond pulsed Nd:YAG lasers (λ = 532 nm) as a function of the following laser beam parameters: pulse repetition rate (1-10,000 Hz), laser fluence (0.1-5 J/cm²) and pulse duration (5 ns and 100 ns). In our study, the best ablation efficiency (η ≅ 0.3 mm³/J) was obtained with the highest repetition rate (10 kHz) at the fluence F = 1.5 J/cm². This ablation efficiency can be associated with heat accumulation at high repetition rate, which leads to the ablation threshold decrease. Despite the low thermal diffusivity and the low optical absorption of the paint (thermal confinement regime), the ablation threshold fluence was found to depend on the pulse duration. At high laser fluence, the ablation efficiency was lower for 5 ns pulse duration than for the one of 100 ns. This difference in efficiency is probably due to a high absorption of the laser beam by the ejected matter or the plasma at high laser intensity. Accumulation of particles at high repetition rate laser ablation and surface shielding was studied by high speed imaging.     

Studies of craters’ dimension for long-pulse laser ablation of metal targets at various experimental conditions

Long pulse laser shots of the PALS iodine laser in Prague have been used to obtain metal target ablation at various experimental conditions. Attention is paid mainly to the dependencies of the crater diameter on the position of minimum laser-focus spot with regard to the target surface, by using different laser wavelengths and laser energies. Not only a single one, but two minima, independently of the wavelength, of the target irradiation angle and of the target material, were recorded. Significant asymmetries, ascribed to the non-linear effects of intense laser beam with pre-formed plasma, were found, too. Estimations of ejected mass per laser pulse are reported and used to calculate the efficiency of laser-driven loading. Results on metal target ablation and crater formation at high intensities (from 2 × 10¹³ to 3 × 10¹⁶ W/cm²) are presented and compared. Crater depth, crater diameter and etching yield are reported versus the laser energy, in order to evaluate the ablation threshold fluence.     

Influence of surface effects on the performance of lead-niobium-germanate optical waveguides

Lead-niobium-germanate planar waveguides have been produced by pulsed laser deposition. The composition of the waveguides is found to be relatively weakly dependent on the laser fluence, while their surface morphology is affected dramatically. Smooth surfaces are obtained for a narrow fluence range centered at 2.0 J/cm², while particulates having typical diameters of <0.5 μm or droplets with typical diameters of <10 μm are observed at lower and higher fluences, respectively. The refractive index of the waveguides increases with fluence up to 2.1 at 2.0 J/cm², which is close to the value of the bulk glass, and remains constant at higher fluences. Propagation losses show instead a minimum (≈6.5 dB/cm) at 2.0 J/cm². The characteristics of the ablation process that leads to the ejection of solid particulates or molten droplets as well as the increase of the waveguides density on increasing the fluence are discussed to be responsible for the observed optical behavior.     

Ablation mechanism study on metallic materials with a 10 ps laser under high fluence

Single shot ablation of metallic materials of aluminium, titanium alloy (Ti6Al4V) and gold has been studied with 10 picoseconds (ps) laser pulses experimentally and theoretically. The ablation rate variation at high fluence was explained by a simplified predictive model based on critical-point phase separation (CPPS) theory. A comparison between experimental and numerical results inferred that CPPS may well be the dominant ablation mechanism for high fluence laser ablation at 10 ps laser duration.     

XPS studies of short pulse laser interaction with copper

The effect of laser ablation on copper foil irradiated by a short 30 ns laser pulse was investigated by X-ray photoelectron spectroscopy. The laser fluence was varied from 8 to 16.5 J/cm² and the velocity of the laser beam from 10 to 100 mm/s. This range of laser fluence is characterized by a different intensity of laser ablation. The experiments were done in two kinds of ambient atmosphere: air and argon jet gas.The chemical state and composition of the irradiated copper surface were determined using the modified Auger parameter (α′) and O/Cu intensity ratio. The ablation atmosphere was found to influence the size and chemical state of the copper particles deposited from the vapor plume. During irradiation in air atmosphere the copper nanoparticles react with oxygen and water vapor from the air and are deposited in the form of a CuO and Cu(OH)₂ thin film. In argon atmosphere the processed copper surface is oxidized after exposure to air.     

Patterning of indium-tin oxide on glass with picosecond lasers

The results of patterning of the indium-tin oxide (ITO) film on the glass substrate with high repetition rate picosecond lasers at various wavelengths are presented. Laser radiation initiated the ablation of the material, forming grooves in ITO. Profile of the grooves was analyzed with a phase contrast optical microscope, a stylus type profiler, scanning electron microscope (SEM) and atomic force microscope (AFM). Clean removal of the ITO film was achieved with the 266 nm radiation when laser fluence was above the threshold at 0.20 J/cm², while for the 355 nm radiation, the threshold was higher, above 0.46 J/cm². The glass substrate was damaged in the area where the fluence was higher than 1.55 J/cm². The 532 nm radiation allowed getting well defined grooves, but a lot of residues in the form of dust were generated on the surface. UV radiation with the 266 nm wavelength provided the widest working window for ITO ablation without damage of the substrate. Use of UV laser radiation with fluences close to the ablation threshold made it possible to minimize surface contamination and the recast ridge formation during the process.     

Target-plane deposition of diamond-like carbon in pulsed laser ablation of graphite

In pulsed Nd:YAG laser ablation of highly oriented pyrolytic graphite (HOPG) at 10⁻⁶ Torr, diamond-like carbon (DLC) are deposited at laser wavelengths of 1064, 532, and 355 nm on substrates placed in the target-plane. These target-plane samples are found to contain varying sp³ content and composed of nanostructures of 40-200 nm in size depending on the laser wavelength and laser fluence. The material and origin of sp³ in the target-plane samples is closely correlated to that in the laser-modified HOPG surface layer, and hardly from the backward deposition of ablated carbon plume. The surface morphology of the target-plane samples shows the columnar growth and with a tendency for agglomeration between nanograins, in particular for long laser wavelength at 1064 nm. It is also proposed that DLC formation mechanism at the laser-ablated HOPG is possibly via the laser-induced subsurface melting and resolidification.     

Picosecond pulsed laser ablation and micromachining of 4H-SiC wafers

Ultra-short pulsed laser ablation and micromachining of n-type, 4H-SiC wafer was performed using a 1552 nm wavelength, 2 ps pulse, 5 μJ pulse energy erbium-doped fiber laser with an objective of rapid etching of diaphragms for pressure sensors. Ablation rate, studied as a function of energy fluence, reached a maximum of 20 nm per pulse at 10 mJ/cm², which is much higher than that achievable by the femtosecond laser for the equivalent energy fluence. Ablation threshold was determined as 2 mJ/cm². Scanning electron microscope images supported the Coulomb explosion (CE) mechanism by revealing very fine particulates, smooth surfaces and absence of thermal effects including melt layer formation. It is hypothesized that defect-activated absorption and multiphoton absorption mechanisms gave rise to a charge density in the surface layers required for CE and enabled material expulsion in the form of nanoparticles. Trenches and holes micromachined by the picosecond laser exhibited clean and smooth edges and non-thermal ablation mode for pulse repetition rates less than 250 kHz. However carbonaceous material and recast layer were noted in the machined region when the pulse repetition rate was increased 500 kHz that could be attributed to the interaction between air plasma and micro/nanoparticles. A comparison with femtosecond pulsed lasers shows the promise that picosecond lasers are more efficient and cost effective tools for creating sensor diaphragms and via holes in 4H-SiC.     

Fixation of bioactive calcium alkali phosphate on Ti6Al4V implant material with femtosecond laser pulses

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.     

Small size TiO2 nanoparticles prepared by laser ablation in water

Titanium dioxide nanoparticles in distilled H₂O solvent were prepared by laser ablation. The experiments were performed irradiating a Ti target with a second harmonic (532 nm) output of a Nd:YAG laser varying the operative fluence between 1 and 10 J cm⁻² and for an ablation time ranging from 10 to 30 min. Electron microscopy measurements have evidenced the predominant presence of nanoparticles with diameter smaller than 10 nm together with agglomerations of 100-200 nm whose content increases with the laser fluence. At low laser fluence the particles’ size distribution shows that more than 85% of the nanoparticles have a size smaller than 5 nm while at mid and high fluences the presence of 5-7 nm nanoparticles is predominant. XPS analysis has revealed the presence of different titanium suboxide phases with the prevalence of Ti-O bonds from TiO₂ species. The optical bandgap values, determined by UV-vis absorption measurements, are compatible with the anatase phase.     

Characterization of the laser ablation plasma used for the deposition of amorphous carbon

The plasma produced by laser ablation of a graphite target was studied by means of optical emission spectroscopy and a Langmuir planar probe. Laser ablation was performed using a Nd:YAG laser with emission at the fundamental line with pulse length of 28 ns. In this work, we report the behavior of the mean kinetic energy of plasma ions and the plasma density, as a function of the laser fluence (J/cm²), and the target to probe (substrate) distance. The characterized regimes were employed to deposit amorphous carbon at different values of kinetic energy of the ions and plasma density. The mean kinetic energy of the ions could be changed from 40 to 300 eV, and the plasma density could be varied from 1 × 10¹² to 7 × 10¹³ cm⁻³. The main emitting species were C⁺ (283.66, 290.6, 299.2 and 426.65 nm) and C⁺⁺ (406.89 and 418.66 nm) with the C⁺ (426.65 nm) being the most intense and that which persisted for the longest times. Different combinations of the plasma parameters yield amorphous carbon with different structures. Low levels (about 40 eV) of ion energy produce graphitic materials, while medium levels (about 200 eV) required the highest plasma densities in order to increase the CC sp³ bonding content and therefore the hardness of the films. The structure of the material was studied by means of Raman spectroscopy, and the hardness and elastic modulus by depth sensitive nanoindentation.     

Protons’ generation by laser irradiation at 5 × 10 W/cm from silicon dielectric targets containing an excess of hydrogen

A study of silicon plasma generated in vacuum by 532 nm Nd:YAG laser at intensities of about 5 × 10⁹ W/cm² from dielectric targets containing a relatively huge quantity of hydrogen was presented.Time-of-flight technique was employed to measure the particles’ energy and the relative yield with respect to other ion species. Plasma-accelerated ions show Coulomb-Boltzmann-shifted distributions depending on their charge state.Mass quadrupole spectrometry allowed the estimation of the relative hydrogen amount inside the different samples considered: silicon (Si), silicon nitride (Si₃N₄) and hydrogenated annealed silicon (Si(H)) as a function of the ablation depth and irradiation time.Depth profiles of the laser craters permit to calculate the ablation yield at the used laser fluence. The plasma temperature and density was evaluated by the experimental data. A special regard is given to the protons’ generation process occurring inside the plasma, due to the possible influence of the hydrogen excess on the treated samples in comparison to the not-hydrogenated silicon ones.     

Morphology of ablation craters generated by fs laser pulses in LiNbO3

The surface morphology of the ablation craters generated in LiNbO₃ by 130 fs laser pulses at 800 nm has been investigated by AFM/SNOM microscopy. The single pulse fluence corresponding to the ablation threshold has been estimated to be ≈1.8 J/cm².A complex structure including random cone-shaped protrusions is observed inside the ablated crater. The scale of the protrusion spacing is in the submicron range and the heights are typically of a few tens of nanometers. At and outside the crater rim a novel quasi-periodic wave-like topography pattern is observed in both types of microscopy techniques. The average wavelength, that is slightly dependent on pulse fluence, is (500-800 nm) comparable to the light wavelength. This novel topography feature keeps a close similarity with a Fresnel diffraction pattern by an absorbing circular obstacle or impact wave pattern produced by a combination of heat and shock wave (resemble that of impact crater). It is proposed that the obstacle is associated to the strongly nonlinear multiphoton absorption at the peak of the pulse profile. The energy deposited by nonlinear absorption of such profile causes ablation of both the crater and the rippled structure.     

Comparison of the laser ablation process on Zn and Ti using pulsed digital holographic interferometry

Pulsed digital holographic interferometry has been used to compare the laser ablation process of a Q-switched Nd-YAG laser pulse (wavelength 1064 nm, pulse duration 12 ns) on two different metals (Zn and Ti) under atmospheric air pressure. Digital holograms were recorded for different time delays using collimated laser light (532 nm) passed through the volume along the target. Numerical data of the integrated refractive index field were calculated and presented as phase maps. Intensity maps were calculated from the recorded digital holograms and are used to calculate the attenuation of the probing laser beam by the ablated plume. The different structures of the plume, namely streaks normal to the surface for Zn in contrast to absorbing regions for Ti, indicates that different mechanisms of laser ablation could happen for different metals for the same laser settings and surrounding gas. At a laser fluence of 5 J/cm², phase explosion appears to be the ablation mechanism in case of Zn, while for Ti normal vaporization seems to be the dominant mechanism.     

Characterization of Ag and Au nanoparticles created by nanosecond pulsed laser ablation in double distilled water

Pulsed laser ablation of Ag and Au targets, immersed in double-distilled water is used to synthesize metallic nanoparticles (NPs). The targets are irradiated for 20 min by laser pulses at different wavelengths—the fundamental and the second harmonic (SHG) (λ = 1064 and 532 nm, respectively) of a Nd:YAG laser system. The ablation process is performed at a repetition rate of 10 Hz and with pulse duration of 15 ns. Two boundary values of the laser fluence for each wavelength under the experimental conditions chosen were used—it varied from several J/cm² to tens of J/cm². Only as-prepared samples were measured not later than two hours after fabrication. The NPs shape and size distribution were evaluated from transmission electron microscopy (TEM) images. The suspensions obtained were investigated by optical transmission spectroscopy in the near UV and in the visible region in order to get information about these parameters. Spherical shape of the NPs at the low laser fluence and appearance of aggregation and building of nanowires at the SHG and high laser fluence was seen. Dependence of the mean particle size at the SHG on the laser fluence was established. Comments on the results obtained have been also presented.     

Femtosecond laser ablation of silver foil with single and double pulses

The average ablation depth per pulse of silver foil by 130 fs laser pulses has been measured in vacuum over a range of three orders of magnitude of pulse fluence up to 900 J cm⁻². In addition, double pulses with separations up to 3.4 ns have been used to probe time scales of relevance for femtosecond ablation. The double pulse ablation depth, when each pulse fluence is 0.7 J cm⁻², falls to that of a single pulse as the pulse separation is increased from 0 ps to 700 ps. This time scale decreases to only 4 ps as the fluence is increased to 11 J cm⁻². It then jumps to 500 ps across a transition fluence where the slope of the ablation depth versus logarithmic fluence characteristic changes abruptly to a higher value. In addition, for pulse separations near 1000 ps, the second pulse can cause re-deposition of ejecta from the first pulse resulting in a double pulse ablation depth only 40% that of the first pulse alone. This has important implications for the interpretation of double pulse femto-LIBS intensities. Our results suggest that the optical properties of nano or mesoparticles play a significant role in double pulse ablation with large pulse separations.     

High power single-shot laser ablation of silicon with nanosecond 355 nm

We report on high intensity single-shot laser ablation of monocrystalline silicon with a nanosecond Nd:YAG at 355 nm. It is shown that for incident laser intensities exceeding ∼11.5 GW/cm² on the silicon surface, unusually high etch depths can be achieved reaching values up to 60 μm. The results support previous observations of dramatic increase in etch rates in single-shot laser ablation at 266 nm. A laser-induced explosive boiling mechanism together with secondary plasma heating is believed to be associated with this effect.