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.     

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.     

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     

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.     

Laser backside etching of fused silica due to carbon layer ablation

The backside ablation of a absorbing carbon layer onto fused silica is studied in air and water confinement in comparison. The confinement influences the etch rate and the laser fluence dependence of the etch rate significantly while the threshold fluence is almost the same. The different confinement of the laser induced plasma results in the observed rate saturation in the case of air and in a linear growing rate in the case of water confinement at medium laser fluences. The less dense air confinement permits a faster plasma expansion of the laser plume than in the case of water confinement and effects consequently the interaction time and interaction strength of the laser plume with the fused silica surface. The differences in the laser-plasma-substrate interaction cause the observed rate saturation at weak interaction (air) and the growing etch rate at strong interaction (water). Thus, the confinement situation controls the interaction process in the case of backside ablation and should be considered in indirect material processing methods such as LIBWE and LESAL, too. PACS 81.65.C; 81.05.K; 79.20.D; 61.80.B; 42.55.L; 68.45.D     

Surface plasmon scattering on polymer-bimetal layer covered fused silica gratings generated by laser induced backside wet etching

Large amplitude fused silica gratings are prepared by combining the UV laser induced backside wet etching technique (LIBWE) and the two-beam interference method. The periodic patterning of fused silica surfaces is realized by s-polarized fourth harmonic beams of a Nd:YAG laser, applying saturated solution of naphthalene in methyl-methacrylate as liquid absorber. Atomic force microscopy is utilized to analyze how the modulation amplitude of the grating can be controlled by the fluence and number of laser pulses. Three types of plasmonic structures are prepared by a bottom-up method, post-evaporating the fused silica gratings by gold-silver bimetal layers, spin-coating the metal structures by thin polycarbonate films, and irradiating the multilayers by UV laser. The effect of the bimetal and polymer-coated bimetal gratings on the surface plasmon resonance is investigated in a modified Kretschmann arrangement allowing polar and azimuthal angle scans. It is demonstrated experimentally that scattering on rotated gratings results in additional minima on the resonance curves of plasmons excited by second harmonic beam of a continuous Nd:YAG laser. The azimuthal angle dependence proves that these additional minima originate from back-scattering. The analogous reflectivity minima were obtained by scattering matrix method calculations realized taking modulation depths measured on bimetal gratings into account.     

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     

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.     

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     

104 nm period grating fabrication in fused silica by immersion two-beam interferometric laser induced backside wet etching technique

A substantial extension of the method of two-beam interferometric laser induced backside wet etching (TWIN-LIBWE), the immersion TWIN-LIBWE, is used to fabricate fused silica gratings with a 104 nm period. The spatially filtered fourth harmonic of Nd:YAG laser (λ=266 nm, τ_FWHM=8 ns) pulses were split into two parts which then interfered at the backside of the fused silica target in contact with a liquid absorber (naphthalene methyl methacrylate saturated solution with a concentration of 1.85 mol/dm³). The hypotenuse of a rectangular fused silica prism is attached to the fused silica target with the use of distilled water as the immersion liquid. On steering the beams through the sides of the prisms, the angle between the two laser beams has been substantially increased. The resulting period of 104 nm is the minimal grating constant achievable under such experimental conditions and, to our knowledge, the smallest laser generated grating period in fused silica at present. PACS 42.62; 42.79; 81.65     

Using Ion-beam etching to smooth fused silica surfaces

The roughness of fused silica, silicon, and sapphire substrates from different manufacturers is studied. Features of the substrates for imaging optics in the soft X-ray (SXR) and extreme UV (EUV) ranges are discussed. The first results from smoothing quartz substrates by etching with neutralized 50–500-eV argon beams are reported. Surface smoothing has been observed in the spatial-frequency range of 10^-1-10^-2 μm^-1.     

Indirect laser etching of fused silica: Towards high etching rate processing

The indirect laser processing approach (LIBWE) laser-induced backside wet etching allows defined microstructuring of transparent materials at low laser fluences with high quality. The optical and the thermal properties of the solid/liquid interface determine the temperatures and therefore the etching mechanism in conjunction with the dynamic processes at the interface due to the fast heating/cooling rates. The exploration of organic liquid solvents and solutions such as 0.5 M pyrene/toluene results in low etch rates (∼20 nm/pulse). By means of liquid metals as absorber here, demonstrated for gallium (Ga), etch rates up to 600 nm/pulse can be achieved. Regardless of the high etch rates a still smooth surface similar to etching with organic liquid solutions can be observed. A comparative study of the two kinds of absorbing liquids, organic and metallic, investigates the etch rates regarding the fluence and pulse quantity. Thereby, the effect of incubation processes as result of surface modification on the etching is discussed. In contrast to pyrene/toluene solution the metallic absorber cannot decompose and consequently no decomposition products can alter the solid/liquid interface to enhance the absorption for the laser radiation. Hence, incubation can be neglected in the case of the silica/gallium interface so that this system is a suitable model to investigate the primary processes of LIBWE. To prove the proposed thermal etch mechanism an analytical temperature model based on a solution of the heat equation is derived for laser absorption at the silica/gallium interface.     

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.     

Micro-channel etching characteristics enhancement by femtosecond laser processing high-temperature lattice in fused silica glass

A fused silica glass micro-channel can be formed by chemical etching after femtosecond laser irradiation, and the successful etching probability is only 48%. In order to improve the micro-channel fabrication success probability,the method of processing a high-temperature lattice by a femtosecond laser pulse train is provided. With the same pulse energy and scanning speed, the success probability can be increased to 98% by optimizing pulse delay.The enhancement is mainly caused by the nanostructure, which changes from a periodic slabs structure to some intensive and loose pore structures. In this Letter, the optimum pulse energy distribution ratio to the etching is also investigated.     

熔石英的快速激光刻蚀

使用10.6μm连续波CO_2激光和几种工作气体,对熔石英实现了快速的激光刻蚀.得到了刻蚀速度高于200μm/s的干净、光滑的表面;并根据所提出的机理对观察到的实验结果进行了解释.     

Precise etching of fused silica for refractive and diffractive micro-optical applications

One of the challenges of current laser material processing is the high-quality etching of transparent materials for micro-optical applications. The ablation of transparent materials with UV-, ultrashort pulse and even of VUV-lasers is characterized by a high etch rate and a high laser fluence and causes considerable surface roughness evolution. The combination of specific laser processing techniques, e.g., scanning contour mask technique and direct writing with a small laser spot, with laser-induced backside wet etching (LIBWE) allows the direct machining of dielectric materials with an almost optical quality for the fabrication of diffractive as well as refractive topographic features. The etching of multi-level elements, gratings with variable depth, micro-lenses as well as free-form surface topographies with PV-values from some 100 nm to a few micrometers, a nanometer depth accuracy and a low roughness of less than 10 nm rms is presented and demonstrates the capabilities of this approach for precision engineering.     

Laser-induced backside wet etching of fluoride and sapphire using picosecond laser pulses

Laser-induced backside wet etching (LIBWE) is a promising process for microstructuring of rigid chemical resistant and inert transparent materials. LIBWE with nanosecond laser pulses has been successfully demonstrated in a number of studies. LIBWE in a time scale of femtosecond and picosecond pulse durations has been investigated only in a few studies and just on fused silica. In the present study LIBWE of fluorides (CaF₂, MgF₂) and sapphire with a mode-locked picosecond (t _p=10 ps) laser at a UV wavelength of λ=355 nm using toluene as absorbing liquid has been demonstrated. The influence of the laser fluence and the pulse number on the etching rate and the achieved surface morphology was investigated. The etching rate grows linearly with the laser fluence in the low and high-fluence ranges with different slopes. The achieved etching rates for CaF₂ and for sapphire were in the same range. Contrary to CaF₂ and sapphire the etching rates of MgF₂ were one magnitude less. For backside etching on sapphire at high fluences smooth surfaces and at low fluences ripples pattern were found, whereas fluoride surfaces showed a trend towards crack formation.     

Femtosecond laser-assisted etching of three-dimensional inverted-woodpile structures in fused silica

Three-dimensional inverted-woodpile (WP) structures were embedded in a microchannel by femtosecond laser direct-writing of fused silica followed by chemical etching with diluted hydrofluoric acid. We show the hole size is linearly dependent on laser-scanning depth for various pulse energies, permitting the control of laser exposures to facilitate close 5 μm periodic packing of uniform microcapillary arrays. Exposure compensation for depth-dependent etching rate and optical beam aberrations yielded stable and crack-free uniform inverted-WP structures. The direct formation of the inverted-WP structure together with microchannels in an all-fused silica substrate, offers chemical stability and inertness, and biocompatibility to be exploited as new microfluidic systems for chromatography and electro-osmotic pumps.     

IR spectra of fused silica irradiated by fast neutrons

IR spectroscopy has been used to study the process of structural damage and changes in some characteristics of fused silica irradiated by fast neutrons over a very broad fluence range (10¹⁷–10²¹ cm⁻²). Features of the change in spectral characteristics of the bending and stretching vibrations of the bridge bonds have been identified, and also a comparative analysis has been carried out with radiation-induced changes in a series of optical spectra in the UV and visible regions, and structural parameters and other characteristics of wafers irradiated by different fluences. A correspondence has been established between the features of the radiation-induced changes in the optical, luminescence, and structural properties, and extremal points have been observed on the dose dependences. Based on the results obtained, a mechanism of radiation-induced rearrangement of the silica structure is suggested. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 4, pp. 494–497, July–August, 2006.