Backside etching of fused silica with Nd:YAG laser

The laser-induced backside etching of fused silica with gallium as highly absorbing backside absorber using pulsed infrared Nd:YAG laser radiation is demonstrated for the first time. The influence of the laser fluence, the pulse number, and the pulse length on the etch rate and the etched surface topography was studied. The comparable high threshold fluences of about 3 and 7 J/cm² for 18 and 73 ns pulses, respectively, are caused by the high reflectivity of the fused silica-gallium interface and the high thermal conductivity of gallium. For the 18 and 73 ns long pulses the etch rate rises almost linearly with the laser fluence and reaches a value of 350 and 300 nm/pulse at a laser fluence of about 12 and 28 J/cm², respectively. Incubation processes are almost absent because etching is already observed with the first laser pulse at all etch conditions and the etch rate is constant up to 30 pulses.The etched grooves are Gaussian-curved and show well-defined edges and a smooth bottom. The roughness measured by interference microscopy was 1.5 nm rms at an etch depth of 0.6 μm. The laser-induced backside etching with gallium is a promising approach for the industrial application of the backside etching technique with IR Nd:YAG laser.     

Laser etching of fused silica using an adsorbed toluene layer

A new method for laser etching of transparent materials with a low etch rate and a very good surface quality is demonstrated. It is based on the pulsed UV-laser backside irradiation of a transparent material that is covered with an adsorbed toluene layer. This layer absorbs the laser radiation causing the etching of the solid. The threshold fluence for etching of fused silica amounts to 0.7 J/cm². The constant etch rate of about 1.3 nm/pulse that has been observed in a fluence interval from 2 to 5 J/cm² is evidence of a saturated process. The limited thickness of the adsorbed layer causes the low etch rates and the rate saturation. The etched surface structures have well defined edges and low surface roughness values of down to 0.4 nm rms. PACS 81.65.Cf; 81.05.Kf; 79.20.Ds; 61.80.Ba; 42.55.Lt     

Backside laser etching of fused silica using liquid gallium

Laser-induced backside wet etching (LIBWE) that is regularly performed with hydrocarbon solutions is demonstrated with the liquid metal gallium as a new class of absorbers for the first time. Well-contoured square etch pits in fused silica with smooth bottoms and well-defined edges were achieved already with the first pulse from a 248 nm excimer laser. The etching is characterized by a threshold fluence of 1.3 J/cm² and a straight proportional etch rate growth with the fluence up to 8.2 J/cm². In addition, the etch depth increases linearly for onward pulsed laser irradiation and gives evidence for an only marginal incubation effect. The high fluences necessary for etching originate from the high reflection losses as well as the high thermal conductivity of the metallic absorber. The suggested etch mechanism comprises the heating of the fused silica up to or beyond the fused silica melting point by the laser heated gallium and the removing of the softened or molten fraction of the material by mechanical forces from shock waves, bubbles, high pressures, or stress fields. PACS 81.65.C; 81.05.J; 79.20.D; 61.80.B; 42.55.L     

In situ reflectivity investigations of solid/liquid interface during laser backside etching

In situ reflectivity measurements of the solid/liquid interface with a pump-probe setup were performed during laser-induced backside wet etching (LIBWE) of fused silica with KrF excimer laser using toluene as absorbing liquid. The intensity, the temporal shape, and the duration of the reflected light measured in dependence on the laser fluence are discussed referring to the surface modification and the bubble formation.The vaporisation of the superheated liquid at the solid interface causes a considerable increase of the reflectivity and gives information about the bubble lifetime. The alterations of the reflectivity after bubbles collapse can be explained with the changed optical properties due to surface modifications of the solid surface. Comparative studies of the reflectivity at different times and the etch rate behaviour in dependence on the laser fluence show that the in situ measured surface modification begins just at the etch threshold fluence and correlates further with etch rate behaviour and the etched surface appearance. The already observed surface modification at LIBWE due to a carbon deposition and structural changes of the near surface region are approved by the changes of the interface reflectivity and emphasizes the importance of the modified surface region in the laser-induced backside wet etching process.     

Time-resolved measurements during backside dry etching of fused silica

The laser-induced backside dry etching (LIBDE) investigated in this study makes use of a thin metal film deposited at the backside of a transparent sample to achieve etching of the sample surface. For the time-resolved measurements at LIBDE fused silica samples coated with 125 nm tin were used and the reflected and the transmitted laser intensities were recorded with a temporal resolution of about 1 ns during the etching with a ∼30 ns KrF excimer laser pulse. The laser beam absorption as well as characteristic changes of the reflection of the target surface was calculated in dependence on the laser fluence in the range of 250-2500 mJ/cm² and the pulse number from the temporal variations of the reflection and the transmission. The decrease of the time of a characteristic drop in the reflectivity, which can be explained by the ablation of the metal film, correlates with the developed thermal model. However, the very high absorption after the film ablation probably results in very high temperatures near the surface and presumably in the formation of an absorbing plasma. This plasma may contribute to the etching and the surface modification of the substrate. After the first pulse a remaining absorption of the sample was measured that can be discussed by the redeposition of portions of the ablated metal film or can come from the surface modification in the fused silica sample. These near-surface modifications permit laser etching with the second laser pulse, too.     

Effects of halogenated organic solvents on laser-induced backside wet etching of fused silica

Laser-induced backside wet etching of fused silica using a solution of pyrene dissolved in halogenated and non-halogenated solvents is presented. A significant influence of the solvent used on the etch rate and the etched surface appearance was ascertained. The etching of uniform and smooth surfaces with rates of ∼0.1 nm/pulse for laser fluences below 500 mJ/cm² is observed only for halogenated solvents. Furthermore, reduced threshold fluences, only small incubation effects, and a constant etch rate in dependence on the pulse number were found. The experimental data suggest an additional etch process at low laser fluences characterized by the very low etch rate and the smooth etching observed only with halogen-containing solvents. The generation of halogen radicals/compounds close to the heated surface due to the decomposition of the solvent causing the attack of the surface seems the most probable mechanism. PACS 81.65.Cf; 81.05.Kf; 79.20.Ds; 61.80.Ba; 42.55.Lt; 68.45.Da     

Influence on the laser induced backside dry etching of thickness and material of the absorber, laser spot size and multipulse irradiation

Laser induced backside dry etching method (LIBDE) was developed - analogously to the well-known laser induced backside wet etching (LIBWE) technique - for the micromachining of transparent materials. In this procedure, the absorbing liquid applied during LIBWE was replaced with solid metal layers. Fused silica plates were used as transparent targets. These were coated with 15-120 nm thick layers of different metals (silver, aluminium and copper). The absorbing films were irradiated by a nanosecond KrF excimer laser beam through the quartz plate. The applied fluence was varied in the 150-2000 mJ/cm² range, while the irradiated area was between 0.35 and 3.6 mm². At fluences above the threshold values, it was found that the metal layers were removed from the irradiated spots and the fused silica was etched at the same time. In our experiments, we investigated the dependence of the main parameters (etch rate and threshold) of LIBDE on the absorption of the different metal layers (silver, copper, aluminium), on the size of the irradiated area, on the film thickness and on the number of processing laser pulses.     

Microstructuring of fused silica by laser-induced backside wet etching using picosecond laser pulses

The laser-induced backside wet etching (LIBWE) is an advanced laser processing method used for structuring transparent materials. LIBWE with nanosecond laser pulses has been successfully demonstrated for various materials, e.g. oxides (fused silica, sapphire) or fluorides (CaF₂, MgF₂), and applied for the fabrication of microstructures. In the present study, LIBWE of fused silica with mode-locked picosecond (t_p = 10 ps) lasers at UV wavelengths (λ₁ = 355 nm and λ₂ = 266 nm) using a (pyrene) toluene solution was demonstrated for the first time. The influence of the experimental parameters, such as laser fluence, pulse number, and absorbing liquid, on the etch rate and the resulting surface morphology were investigated. The etch rate grew linearly with the laser fluence in the low and in the high fluence range with different slopes. Incubation at low pulse numbers as well as a nearly constant etch rate after a specific pulse number for example were observed. Additionally, the etch rate depended on the absorbing liquid used; whereas the higher absorption of the admixture of pyrene in the used toluene enhances the etch rate and decreases the threshold fluence. With a λ₁ = 266 nm laser set-up, an exceptionally smooth surface in the etch pits was achieved. For both wavelengths (λ₁ = 266 nm and λ₂ = 355 nm), LIPSS (laser-induced periodic surface structures) formation was observed, especially at laser fluences near the thresholds of 170 and 120 mJ/cm², respectively.     

Micromachining of quartz crystal with excimer lasers by laser-induced backside wet etching

We fabricated a well-defined pattern of lines and spaces on the surface of a quartz crystal plate (c-SiO₂) with micron-sized features, using laser-induced backside wet etching (LIBWE). The line patterns obtained using LIBWE showed a high aspect ratio of about 3. The etch rates of fused silica (a-SiO₂) ranged from 5 to 25 nm/pulse with KrF laser irradiation from 0.4-1.3 J/cm². Threshold fluences for a-SiO₂ and c-SiO₂ were 0.23 and 0.34 J/cm², respectively. The single-pulse etch depth was not affected by the repetition rates of laser pulses from 1-50 Hz.     

Processing of transparent materials using visible nanosecond laser pulses

Laser micromachining of transparent materials is an intensively studied research area from the point of view of microoptical element fabrication. One of the most promising indirect processing methods is the laser-induced back-side dry etching (LIBDE). During this method, transparent targets are contacted with solid thin layers, which absorb and transform the pulse energy resulting in etching. The applicability of LIBDE technology for processing of fused silica using a visible nanosecond dye laser (λ=500 nm, FWHM=11 ns) and a 100-nm-thick aluminium absorbing layer was investigated. The applied fluence was varied in the range of 0–3050 mJ/cm²; the illuminated area was 0.1 mm². The threshold fluence of the LIBDE etching of fused silica was found to be approximately 540 mJ/cm². The chemical composition of the surface layers on and around the etched holes was investigated by field-emission scanning electron microscopy and energy-dispersive X-ray spectrometry. It was found that on average 0.4±0.3 at. % aluminium is built into the upper ∼1-μm-thick volume of the illuminated fused silica, while the aluminium content fell below the detection limit in the case of the original surface. Our experiments proved that the LIBDE procedure is suitable for microprocessing of transparent materials using visible nanosecond laser light. PACS 42.62.-b; 61.80.Ba; 81.16.Rf; 81.65.Cf     

Time-resolved transmission study of fused silica during laser-induced backside dry etching

Laser-induced backside dry etching (LIBDE) is a promising technique for micro- and nanomachining of transparent materials. Although several experiments have already proved the suitability and effectiveness of the technique, there are several open questions concerning the etching mechanism and the concomitant processes. In this paper time-resolved light transmission investigations of etching process of fused silica are presented. 125 nm thick silver coating was irradiated through the carrying 1 mm thick fused silica plate by single pulses of a nanosecond KrF excimer laser. The applied fluences were 0.38, 0.71 and 1 J/cm². During the etching process the irradiated spots were illuminated by an electronically delayed nitrogen laser pumped dye laser. The delay between the pump and probe pulses was varied in the range of 0 ns and 20 μs. It was found that the transmitted probe beam intensity strongly depends on the applied delays and fluences. Scanning electron microscopy and energy dispersive X-ray spectrometry of the etched surface showed the existence of silver droplets and fragments on the illuminated surfaces and silver atoms built into the treated surface layer influencing the transmission behavior of the studied samples.     

Fabrication of 550 nm gratings in fused silica by laser induced backside wet etching technique

A series of 550 nm spacing gratings were fabricated in fused silica by laser induced backside wet etching (LIBWE) method using the fourth harmonic of a Q-switched Nd:YAG laser (wavelength: λ = 266 nm; pulse duration: FWHM = 10 ns). During these experiments we used a traditional two-beam interference method: the spatially filtered laser beam was split into two parts, which were interfered at a certain incident angle (2θ = 28°) on the backside surface of the fused silica plate contacting with the liquid absorber (saturated solution of naphthalene-methyl-methacrylate c = 1.85 mol/dm³). We studied the dependence of the quality and the modulation depth of the prepared gratings on the applied laser fluence and the number of laser pulses. The surface of the etched gratings was characterized by atomic force microscope (AFM). The maximum modulation depth was found to be 180-200 nm. Our results proved that the LIBWE procedure is suitable for production of submicrometer sized structures in transparent materials.     

Laser backside etching of fused silica with ultra-short pulses

Laser backside etching of transparent materials like fused silica at the interface to liquids with sub-picosecond UV laser pulses using a pyrene/toluene solution is achieved. For the experimental conditions applied, the etching effect is rather weak with measured rates of the order of 0.1 nm/pulse. A linear dependence of the etched volume upon the laser pulse energy or the pulse number was extracted from the experimental data obtained. At low pulse numbers the etched surface exhibits a feature-free, smooth morphology, while quasi-periodic ripple formation is observed for prolonged laser exposure. In addition, the etching process is accompanied by enhanced carbon deposition at and in the vicinity of the etched surface. The etching mechanism proposed comprises the primary interaction of the laser radiation with the liquid, a surface-modification phase, and the etching of the modified fused-silica surface. PACS 81.65.Cf; 81.05.Kf; 79.20.Ds; 61.80.Ba; 42.55.Lt; 68.45.Da     

Laser-assisted etching of gallium arsenide in chlorine at 308 nm

Xenon chloride (308 nm) excimer laser-assisted etching of GaAs (100) in Cl₂ was demonstrated and characterized with respect to laser and gas parameters. The etch rate increased linearly with laser fluence from thresholds in the range of 50 to 75 mJ/cm² to the highest fluence studied, 650 mJ/cm². For a laser fluence of 370 mJ/cm², the etch rate varied with Cl₂ pressure reaching a maximum at a Cl₂ pressure of about 2 Torr. The etch rate decreased monotonically with Ar buffer gas pressure because of redeposition of GaCl₃ products into the etched channel. The redeposited GaCl₃ affected the etch rate and the etch morphology. The etch rate and morphology also varied with laser repetition rate. The mobility of chlorine on the surface also plays an important role in the etching mechanism.     

Mechanism of backside etching of transparent materials with nanosecond UV-lasers

In consequence of high interest in micro- and nanomachining of transparent materials by laser irradiation, studies on the mechanism of laser-induced backside wet etching (LIBWE) are presented. To reveal the role of the surface modification due to LIBWE the backside ablation (BSA) of LIBWE-modified fused silica (mFS) surfaces at 248 nm was investigated. The threshold fluence and the etch rate of BSA are similar to that of LIBWE and amount ∼250 mJ/cm² and 30 nm for 1 J/cm², respectively. The sample transmission after backside ablation of mFS increases and proves the decreasing thickness of the absorbing layer. Time-resolved reflection studies at LIBWE and BSA of mFS show similar patterns in the backside reflection that can be assigned an ablation process as the comparison to thin polymer films demonstrates. By fitting the BSA data to an exponential decay absorption model a modification depth and a surface absorption of about 38 nm and α ^S ∼1.3×10⁷ m⁻¹ were calculated, respectively. In conclusion of the results a new model for LIBWE is proposed.     

Effect of the ceramic grain size and concentration on the dynamical mechanical and dielectric behavior of poly(vinilidene fluoride)/Pb(Zr<Subscript>0.53</Subscript>Ti<Subscript>0.47</Subscript>)O<Subscript>3</Subscript> composites

Laser-induced backside wet and dry etching (LIBWE and LIBDE) methods were developed for micromachining of transparent materials. Comparison of these techniques is helpful in understanding the etching mechanism but was not realized due to complications in setting up comparable experimental conditions. In our comparative investigations we used a solid tin film for dry and molten tin droplets for wet etching of fused-silica plates. A tin–fused-silica interface was irradiated through the sample by a KrF excimer laser beam (λ=248 nm, FWHM=25 ns); the fluence was varied between 400 and 2100 mJ/cm². A significant difference between the etch depths of the two investigated methods was not found. The slopes of the lines fitted to the measured data (sl_LIBDE=0.111 nm/mJ cm⁻², sl_LIBDE=0.127 nm/mJ cm⁻²) were almost similar. Etching thresholds for LIBDE and LIBWE were approximately 650 and 520 mJ/cm², respectively. To compare the dependence of etch rates on the pulse number, target areas were irradiated at different laser fluences and pulse numbers. With increasing pulse number a linear rise of depth was found for wet etching while for dry etching the etch depth increase was nonlinear. Secondary ion mass spectroscopic investigations proved that this can be due to the reconstruction of a new thinner tin-containing surface layer after the first pulse.     

The influence of laser-induced surface modifications on the backside etching process

Spectroscopic measurements in the UV/VIS region show reduced transmission through laser-induced backside wet etching (LIBWE) of fused silica. Absorption coefficients of up to 10⁵ cm⁻¹ were calculated from the transmission measurements for a solid surface layer of about 50 nm. The temperatures near the interface caused by laser pulse absorption, which were analytically calculated using a new thermal model considering interface and liquid volume absorption, can reach 10⁴ K at typical laser fluences. The high absorption coefficients and the extreme temperatures give evidence for an ablation-like process that is involved in the LIBWE process causing the etching of the modified near-surface region. The confinement of the ablation/etching process to the modified near-surface material region can account for the low etch rates observed in comparison to front-side ablation.     

248 nm laser etching of GaAs in chlorine and ozone gas environments

KrF laser etching of GaAs in Cl₂ and O₃ gas ambients by direct laser illumination is reported. The etch depth per pulse in Cl₂ was found to be linear versus the laser fluence on the sample in the 0.2–1.1 J/cm² range. It increased as a function of the Cl₂ pressure up to 6 Torr and slightly decreased for pressures above this value. It also decreased as a function of the laser repetition rate. Very smoothly etched surfaces were obtained after irradiation using the Cl₂ and O₃ etching gases. Auger analysis of the etched GaAs surfaces shows almost no traces of chlorine after etching in Cl₂, whereas a thick oxide layer of about 1500 Å thickness was found after etching in ozone.     

Comparing study of subpicosecond and nanosecond wet etching of fused silica

The effectiveness of the laser induced backside wet etching (LIBWE) of fused silica produced by subpicosecond (600 fs) and nanosecond (30 ns) KrF excimer laser pulses (248 nm) was studied. Fused silica plates were the transparent targets, and naphthalene-methyl-methacrylate (c = 0.85, 1.71 M) and pyrene-acetone (c = 0.4 M) solutions were used as liquid absorbents. We did not observe etching using 600 fs laser pulses, in contrast with the experiments at 30 ns, where etched holes were found. The threshold fluences of the LIBWE at nanosecond pulses were found to be in the range of 360-450 mJ cm⁻² depending on the liquid absorbers and their concentrations. On the basis of the earlier results the LIBWE procedure can be explain by the thermal heating of the quartz target and the high-pressure bubble formation in the liquid. According to the theories, these bubbles hit and damage the fused silica surface. The pressure on the irradiated quartz can be derived from the snapshots of the originating and expanding bubbles recorded by fast photographic setup. We found that the bubble pressure at 460 mJ cm⁻² fluence value was independent of the pulse duration (600 fs and 30 ns) using pyrene-acetone solution, while using naphthalene-methyl-methacrylate solutions this pressure was 4, 5 times higher at 30 ns pulses than it was at 600 fs pulses. According to the earlier studies, this result refers to that the pressure should be sufficiently high to remove a thin layer from the quartz surface using pyrene-acetone solution. These facts show that the thermal and chemical phenomena in addition to the mechanical effects also play important role in the LIBWE procedure.