Proceedings of the Fifth International WLT-Conference on Lasers in Manufacturing 2009 Munich, June 2009 Machining of Transparent Materials with Short Pulse and Ultrashort Pulse Laser Sources Udo Loeschner, Stefan Mauersberger, Joerg Schille, Robby Ebert, Horst Exner Hochschule Mittweida – University of Applied Sciences, Mittweida, Germany Abstract This paper discusses the machining of transparent materials using two short pulse (nanoseconds) and one ultrashort pulse (femtoseconds) laser sources. The investigations were carried out with short pulse Nd:YAG lasers (1064 nm, 532 nm, and 355 nm) as well as a high repetition rate fslaser (1030 nm). In our experiments the laser beam was focused onto the sample with both a stationary objective and a laser scanner with an f-theta-objective. In our study we investigated in detail the dependencies of controlled defect generation inside bulk glass material on important process parameters like wavelength, pulse width, pulse repetition rate, and irradiation regime. Due to a smart arrangement of these defects in lines, planes, and shells cut surfaces can be generated. Finally, cutting of 3d parts, consisting of bulk transparent material, becomes possible. Keywords: laser machining, transparent material, glass, short pulse 1 photons and thereby they will be accelerated. By transferring their energy to electrons in the valence band via collisions these free electrons are able to generate more free electrons by impact ionization. The described mechanism results in a snowballing increase of the density of free carriers, also called avalanche ionization. By the interaction of thermalized electrons with the phonon system of the solid melting and boiling of the material is initiated. If the energy input into the material is sufficient plasma formation sets in and material damage can occur. By focussing laser radiation inside transparent bulk material several effects have to be considered. At first, due to optical aberration at the interface between air and transparent material the focal point inside the material will be blurred. Additionally, with ultrashort pulses chromatic aberration has to be taken into account because of the larger spectral band with of the laser radiation. Again, by irradiating transparent materials with high intensities, several nonlinear effects have to be considered like self focusing, the most important effect. Self focusing occurs above a critical laser pulse power which is formulated for a Gaussian pulse by Introduction Using high intensity laser pulses locally confined permanent modifications inside transparent materials, like changes in the refractive index, are possible by nonlinear absorption mechanisms. Thus optical components with tailored functions; like micro lenses, Fresnel lenses, gratings, waveguides, couplers, switches, up to complex three-dimensional integrated optical devices can be generated inside transparent bulk materials [1-5]. There are four processes involved in the interaction of laser radiation with a solid: photon-electron-interaction, electron-electron-interaction, electron-phonon-interaction, and phonon-phonon-interaction. First the electromagnetic field transfers its optical energy to electrons during several femtoseconds. Electron-electron interaction takes place on a femtosecond to picosecond time scale, electron-phonon interaction ranges from picoseconds to nanoseconds depending on the atomic bonds. The phonon system relaxation takes nanoseconds up to microseconds [6-8]. Most of the glass materials show high transparency for laser wavelengths down to 355 nm. So no single photon absorption process can be initiated because the photon energy is less than the band gap of more than 4 eV for most glass materials. However, if the material is exposed to highly intensive laser radiation, nonlinear absorption mechanisms for the generation of free electrons become more probable. There are two mechanisms involved: tunnel ionization due to the high field strength and multi-photon ionization as a result of multi-photon absorption. These electrons can absorb energy of other Pcr = 1.8962 ⋅ λ2 4⋅π ⋅n0 ⋅n2 n (I ) = n 0 + n 2 ⋅ I (1) where λ is the laser wavelength and n0 and n2 are the respective linear and nonlinear indices of refraction of the propagation medium [9,10]. 1 and an off-axis camera for exact positioning of the sample. The entire focussing unit can be moved in the zdirection allowing the precise adjustment of the focal plane on the sample surface or inside the material. In the experiments both, an f-theta-objective with a 56 mm focal length and a stationary focussing aspheric lens with a 15 mm focal length, were used. The sample can be fixed on a high precision xy-positioning stage and thus exactly positioned and moved relative to the incident laser beam. The optical properties of the materials used in the study are presented in Tab. 2. BK9 is a boron-crown glass, free of streaks, bubbles, and stress, mainly used for laser engraving. The other glasses, BK7, B270, and Lithosil (fused silica), are commercial optical materials produced by Schott AG. In this paper detailed results of controlled defect generation inside bulk glass material in dependence on relevant process parameters like wavelength, pulse length, pulse repetition rate, and irradiation regime are discussed and evaluated. Finally these results are utilized to arrange defects in order to generate a cut surface that results in the excision of a defined 3D part from the bulk volume. 2 Experimental Details In the investigations four laser systems differing in their laser pulse length and wavelength were used: two short pulse Nd:YVO4 lasers (1064 nm, 532 nm) from Edgewave, a DPSS UV laser (355 nm) from Coherent, and an ultrashort pulse laser from Clark MXR Inc. Laser parameters of all types are listed in detail in Tab. 1. Tab. 1: Laser parameters ns-laser fs-laser wavelength 1064 nm 532 nm 355 nm 1030 nm (central) photon energy 1.16 eV 2.32 eV 3.49 eV 1.2 eV min. pulse length 6 ns 4 ns 40 ns 250 fs (sech²) max. repetition rate 30 kHz 30 kHz 300 kHz 25 MHz max. pulse energy 2.2 mJ 0.8 mJ 0.29 mJ 8 µJ 0.2 MW 7 kW 28 MW pulse peak 0.3 MW power band gap [eV] refractive index n0 BK7 Lithosil B270 ~4.7 4.7 9 4.5 1.5 1.51 1.45 1.51 ? 3.45 3 3.4 ? 3.3 4.0 3.3 Results and Discussion 3.1 Short-pulse ns-laser As already discussed above, in transparent materials multi-photon processes are necessary to absorb energy. That means by irradiation with a wavelength of 1064 nm at least a four-photon excitation is necessary. The probability of multi-photon absorption strongly depends on the intensity of the laser radiation – twophoton absorption sets in at several MW/cm², three- and more-photon absorption requires intensities in the GW/cm² and TW/cm² range. A comparison of the maximum laser peak power of the nanosecond laser sources and the critical power for self focussing (Tab. 1 vs. Tab. 2) reveals, that the self focussing effect is not existent. By focussing short-pulse ns-laser radiation with the fundamental wavelength (1064 nm) in combination with the f-theta objective inside a block of BK 9 glass defect formation could be obtained at pulse energies around 1 mJ corresponding to an applied intensity of the laser radiation of 50 GW/cm². This agrees with the required intensity range for four-photon absorption. As can be seen in Fig.1 the produced defects consist each of a set of radiant cracks with a dark centre representing the original position of the laser focus within the material. In [19] the occurring laser-material interaction is described more detailed. Tab. 2: Optical properties of the investigated materials [9,11-18] BK9 3 (1060 nm) nonl. refract. index n2 [10-16 cm² W-1] critical power [MW] 200 µm (1060 nm) 200 µm Fig. 1: optical microscope image of defects in BK9 (1064 nm, pulse energy 1.2 mJ, pulse length 6 ns, pulse distance 150 µm) - left: lateral view, right: axial view The optical system consists of separated attenuators for each laser, turning mirrors, and a focussing unit containing a laser scanner, a mount for stationary objectives, 2 wavelength for defect generation in Lithosil considerable more pulse energy is needed - at a level of 0.66 mJ a 100% yield was achieved. The extension of the defects is increased by 80% compared to the other glasses. Latest experiments have been conducted by using the third harmonic wavelength (355 nm) and the f-theta objective. In BK9 defects with a yield of 100% can be generated with a pulse energy of 0.04 mJ corresponding to an intensity of 3.6 GW/cm². In theory, with the third harmonic wavelength, analogue to the second harmonic wavelength, a two-photon excitation is required. So the observed drastically lower intensity value for defect generation at the third harmonic wavelength is not explainable. If the single photon absorption curve of BK glasses vs. the wavelength is considered, an exponential rise of the absorption coefficient can be noticed for wavelengths lower than 375 nm because of Urbachs rule, which describes optical absorption in disordered solids like disordered semiconductors and glasses [20,21]. The coefficient is increased by a factor of 20 compared to the second harmonic wavelength as well as the fundamental wavelength. So single photon absorption is contributing to the energy input, which results in a lesser demand of intensity in respect to multi-photon processes. The defect dimensions could be reduced further down to 35 µm in lateral direction shown in Fig. 2. In addition, the described sets of radiant cracks show a preferred direction. Unexpectedly, the defects in axial direction are more extended in comparison to the second harmonic wavelength. These peculiarities may be caused by the astigmatism of the laser beam profile in the focal region, which was attested by beam profile measurements. There exist two focal planes in axial different positions - each focus is characterized by an elliptical beam profile. In the experiments the preferred direction of the radiant cracks and the orientation of the ellipse agree very well. Also, the astigmatism is probably responsible for the increased axial elongation compared to the second harmonic wavelength. The minimal lateral extension of the cracks from a single defect achieved in BK 9 glass with optimized parameters is around 130 µm (Fig.1). The shape of the defects along the axis of the incident laser beam (axial direction) is more channel-like with an approximate length of 400 µm. Within the same focal plane the axial position of these “channels” varies up to 200 µm. At this pulse energy level defect generation is not very reproducible because of the stochastic nature of multiphoton absorption. To achieve a 100% yield of defects the pulse energy was increased to 1.6 mJ corresponding to an intensity value of 80 GW/cm². Simultaneously the size of the defect dimensions increases slightly. Investigations in BK7 glass lead to similar results in respect of defect dimensions. However, only at a pulse energy level of 2 mJ defects can be generated reproducibly. Results in B270 glass are equivalent to those of BK7 glass. By contrast, in Lithosil considerably more pulse energy above a level of 1.2 mJ is needed to generate defects. Even at the highest available pulse energy of 2.2 mJ the yield of defects is around 90%. By application of higher energy an increase up to 100% should be achievable. The higher pulse energy level in Lithosil can be discussed as follows: the band gap of Lithosil is twice as large as the gap of other materials, so instead of a 4-photon process an 8-photon excitation process is necessary. Assuming equivalent intensity values of the laser radiation the probability of an 8-photon-process is considerably lower. As observed in the experiments, with rising pulse energy, that means at higher intensities, the probability of an 8-photon process and therefore the yield of defects increases. In experiments with the aspheric lens a 100% yield of defects is achieved already at a pulse energy of 0.2 mJ, which is equivalent to an intensity value of 71 GW/cm². A comparison of the results obtained with the two focussing optics in respect of pulse energy and intensity shows, that the intensity level is nearly the same, but the pulse energy is reduced by a factor of eight. So the intensity level is the dominant parameter for defect generation. In addition, due to the stronger focussing using the aspheric lens the defect dimensions can be reduced considerably down to 75 µm in lateral direction and 100 µm in axial direction. Analogue to the investigations discussed above experiments using the second harmonic wavelength (532 nm) and the f-theta objective were performed. In BK9 glass defects with a yield of 100% can be generated with a pulse energy of 0.26 mJ corresponding to an intensity value of 26 GW/cm². In comparison to the results obtained with the fundamental wavelength and the same focussing optic the intensity level for defect generation is reduced by a factor of three with the second harmonic wavelength. Therefore only a two-photon absorption process is necessary, by which a comparable yield is obtained at lower intensities. The dimensions of the defects can be reduced drastically down to 60 µm in lateral direction and 100 µm in axial direction compared to the fundamental wavelength. Also, the axial position of the defects varies only in a range of 20 µm. In the other glasses BK7 and B270 similar defect dimensions were gained. As already observed with the fundamental 50 µm 200 µm Fig. 2: optical microscope image of defects in BK9 (355 nm, pulse energy 40 µJ, pulse length 60 ns, pulse distance 50 µm) - left: lateral view, right: axial view It should be noted, that the pulse energy of the laser source can not be varied without influencing the pulse length. The shortest pulse length of less than 40 ns requires the maximum pulse energy of the laser. At the chosen pulse energy of 0.04 mJ the pulse length amounts already to 60 ns. However, variation of the 3 lateral dimension [µm] pulse energy at the shortest pulse length is necessary for the investigations. So further efforts, focused on the elimination of the discussed drawbacks of the laser system, are required in order to improve the defect generation process and downsize the defect dimensions. Additional experiments in BK7 glass reveal the same defect dimensions in respect to BK9. Again, the pulse energy level for a 100% yield of defects is identical. Also, as already observed at the other wavelengths, at the third harmonic wavelength considerably more pulse energy is necessary for defect generation in Lithosil. Because of the larger band gap at least a three-photon excitation is required. Even at the highest available pulse energy of 0.29 mJ the yield of defects is around 30%. Defect dimensions are in the same range as with BK7 and BK9 glass. But at the higher pulse energies required for a yield of 100%, the dimensions will probably be slightly increased. A comparison of the respective defect dimensions obtained in the nanosecond regime with the three wavelengths is given in Fig. 3. It can be seen clearly, that the lateral as well as the axial dimensions are strongly reduced with shorter wavelengths. At 355 nm the dimensions in lateral direction could be reduced by a factor of 4 - the axial extension amounts to one-fifth at 532 nm and 355 nm in comparison to 1064 nm. So the smallest defects can be achieved with the third harmonic wavelength because of the shorter wavelength and therefore the smaller focal spot. axial dimension [µm] Ultrashort pulse fs-laser radiation As reported in [19] throughout the whole range of adjustable laser parameters (pulse length 250 fs - 3 ps, pulse energy up to 8 μJ corresponding to 13 TW/cm², pulse repetition rate 200 kHz - 1.8 MHz) no single defects inside the transparent material can be generated. During irradiation a shining channel along the laser beam path could be observed in the focal region inside the material. The shining channel is attributed to filament formation due to nonlinear effects like self focussing causing laser induced structural modifications inside the transparent material [1,9]. Neither successful have been additional tests with a CPA laser system, delivering high pulse energies up to 0.8 mJ at low repetition rates and comparable pulse lengths between 180 fs and 3 ps. With increasing pulse energy only strong filament formation occurs. However, at certain parameters, that means with strongly overlapping laser pulses (<1 µm), longer pulse length (>700 fs), and a minimum repetition rate of 500 kHz imbricative material damage occurs – the defect formation is entirely different from the results obtained with the nanosecond regime. As can be seen clearly in Fig. 4, the lateral material damage extends across the whole scanned area of 500 µm x 500 µm. Because there are no single defects an estimation of the lateral defect dimension is not possible – in axial direction the defect dimension ranges from 80 µm to 100 µm. If the laser pulse overlap is to strong the defect generation becomes uncontrollable and the defects extend beyond the irradiated area. 150 BK9 BK7 100 Lithosil 50 0 1064 a) b) 3.2 532 355 100 µm wavelength [nm] Fig. 4: optical microscope image of defects in BK9 (pulse energy 7.6 µJ, pulse length 2 ps, pulse distance 0.5 µm) - left: lateral view, right: axial view 600 500 BK9 400 BK7 300 Lithosil The formation of material damage may be caused by thermal accumulation effects. Due to strongly overlapping laser pulses, that means very short pulse distances, successive pulses impact at virtually the same position. Additionally, the time interval of 2 µs between two pulses (for a pulse repetition rate of 500 kHz) and the time for heat diffusion for glasses [7,22-24] are on the same time scale, so heating of the material is beginning, because the material is not able to cool down completely between two successive laser pulses. Again, the need of longer pulses for defect generation can be discussed as follows: the excitation processes described in the introduction chapter appear on different time scales. First, absorption of laser radiation, i.e. generation of free 200 100 0 1064 532 100 µm 355 wavelength [nm] Fig. 3: comparison of defect dimensions achieved with nanosecond laser sources in different glasses using the f-theta objective: a) lateral, b) axial 4 electrons, via multi-photon processes takes place during the first several femtoseconds. Free electrons can absorb single photons and thereby they will be accelerated. By transferring their energy to valence electrons via collisions more free electrons can be generated. This process results in a snowballing increase of free carriers, which is called avalanche ionisation. This mechanism is starting with a time delay in respect to the multi-photon process and takes femtoseconds up to picoseconds. Further on the energy is transferred to the phonon system and heating is initiated – the supposed effect responsible for the observed material damage. If the laser pulse length is to short, the excitation stops and the avalanche process will not be activated completely. So no material damage can occur. 3.3 3D parts 1 mm Using these results in order to produce first 3D parts a suitable irradiating strategy was developed. Starting at the bottom of the part a layer by layer irradiation regime was realized leading to a cut surface consisting of defects which encloses the part to be excised. To release the 3D part easily from the glass bulk volume additional well-arranged cut outs are inserted. Fig. 6: sphere in BK9 glass (parameters: wavelength 1064 nm, pulse energy 0.25 mJ, pulse length 6 ns, aspheric lens, lateral pulse distance 100 µm, axial pulse distance 100 µm 1 mm 1 mm a) b) 200 µm Fig. 7: cuboid in BK9 glass (parameters: wavelength 1030 nm, pulse energy 3 µJ, pulse length 700 fs, f-theta objective, lateral pulse distance 0.5 µm, axial pulse distance 150 µm): a) optical microscope image of the cuboid, b) SEM micrograph of one corner Fig. 5: pyramid in BK9 glass (parameters: wavelength 1064 nm, pulse energy 0.23 mJ, pulse length 6 ns, aspheric lens, lateral pulse distance 75 µm, axial pulse distance 150 µm 5 Figs. 5-7 demonstrate the current status of the developed technique. The nanosecond laser sources as well as the femtosecond laser source are suitable tools to cut transparent material. To characterize the surface quality of the walls roughness measurements were conducted with a confocal point sensor μScan from NanoFokus. The measurements reveal, that the average roughness values achieved with the nanosecond laser sources at the fundamental wavelength as well as at the second harmonic wavelength amount to approximately 3 µm. By comparing the quality of the parts produced with the femtosecond laser source with the optimum results obtained with short nanosecond pulses it can be observed that the surface roughness of this specimen is three times higher. So at the present time the nanosecond laser sources are the preferred tool for cutting of transparent material. 4 References [1] D.G. Papazoglou, I. Zergioti, S. Tzortzakis, G. Sgouros, G. Maravelias, S. Christopoulos, C. Fotakis: Sub-picosecond ultraviolet laser filamentation-induced bulk modifications in fused silica; Appl. Phys. A 81, (2005), p.241–244 [2] K.M. Davies, K. Miura, N. Sugimoto, K. Hirao: Writing waveguides in glass with a femtosecond laser, Opt. Lett. 21, (1996), p.1729 [3] E.N. Glezer, M. Milosavljevic, L. Huang, R.J. Finlay, T.-H. 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The defects consist each of a set of radiant cracks with a dark centre representing the original position of the laser focus within the material. The spatial extension of the defects strongly depends on the chosen laser wavelength. With the third harmonic wavelength minimum dimensions in lateral direction of 35 µm were achieved. With the femtosecond laser source no single defect formation inside the transparent material can be generated throughout the whole range of adjustable laser parameters – pulse length, pulse energy, and pulse repetition rate. Only strong formation of filaments occurs. But with strongly overlapping laser pulses (<1 µm), longer pulse length (>700 fs), and a minimum repetition rate of 500 kHz imbricative material damage takes place as a result of thermal accumulation effects. Finally, 3d parts, cut from bulk material, are presented. Roughness measurements reveal, that the specimens machined with nanosecond laser sources are 3 times smoother than the ones produced with the femtosecond laser source. Acknowledgement The authors gratefully acknowledge financial support of the present work by the Bundesministerium für Bildung und Forschung (project number 03IP506). Our thanks go to Prof. Frank Mueller at Hochschule Mittweida (FH) dep. MB/FWT for expert SEM recordings. 6 of B270 glass WechLaserThesis, Hoch- issue: [15] R. Menzel: Photonics, Springer Verlag Berlin 2001 [16] J. S. Aitchison, Y. Silberberg, A. M. Weiner, D. E. Leaird, M. K. Oliver, J. L. Jackel, E. M. Vogel, P. W E. Smith: Spatial optical solitons in planar glass waveguides; J. Opt. Soc. Am. B/Vol. 8, No. 6/June 1991, p.1290-1297 [17] D.M. Rayner, A. Naumov, P.G. 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