Fabrication of glass micro-prisms using ultra-fast laser pulses with chemical etching process

In this study, a new process of glass micro-prism structures is investigated by an ultra-fast laser irradiation with chemical etching process. The ultra-fast laser is employed by an all-in-one femtosecond laser (FS-laser) system with the amplifier as an excitation source for patterning the structures. Here, the center wavelength of laser is frequency-doubled to 517 nm. Besides, the repetition rate and pulse width of laser are 100 kHz and 350 fs, respectively. First, the embedded gratings of glass with different pitches can be fabricated using a FS-laser process. Afterwards, the glass samples are placed in the hydrofluoric acid (HF) solution for 15 min to develop structures. Finally, the results of this study demonstrated that the V-cut micro-prisms are successfully formed by controlling etching concentration between intrinsic glass material and modified areas.     

Three-dimensional structuring of sapphire by sequential He+ ion-beam implantation and wet chemical etching

We present a method for the selective two- and three-dimensional patterning of sapphire using light ion-beam implantation to generate severe lattice damage to depths exceeding 1 μm and subsequent selective wet chemical etching of the damaged regions by hot H₃PO₄. C-cut sapphire crystals were implanted through contact masks using ion fluences of 1×10¹⁶ to 5×10¹⁷ He⁺/cm² and energies up to 400 keV. The etching process is characterized by a high selectivity and a rate of approximately 19 nm/min. Whereas an implantation that produces a continuously damaged pathway results in complete etching from the surface, sole in-depth implantation using only high-energy ions leads to under-etching of the crystalline surface layer. By a combination of these processes we have fabricated three-dimensional structures such as channels and bridges in sapphire. Received: 14 October 2002 / Accepted: 15 October 2002 / Published online: 26 February 2003 RID="*" ID="*"Corresponding author. Fax +41-21/693-3701, E-mail: aurelian.crunteanustanescu@epfl.ch     

Ion synthesis of copper nanoparticles in sapphire and their modification by high-power excimer laser pulses: A review

Composite layers made in sapphire by implantation of 40-keV Cu⁺ ions at a dose of 1 × 10¹⁷ cm⁻² and an ion beam current density varying from 2.5 to 10 μA/cm² are studied. It is shown that ion implantation makes it possible to synthesize a composite layer containing copper nanoparticles at the surface of the insulator. However, the nanoparticle size distribution in this layer is nonuniform. The composite layer is exposed to high-power excimer laser radiation with the aim of modifying the size and size distribution of the metal nanoparticles in it. The resulting structures are examined by Rutherford backscattering, optical reflection spectroscopy, and atomic force microscopy. It is found that the laser irradiation diminishes copper nanoparticles in the composite layer. Experimental data on laser modification may be explained by photofragmentation and/or melting of the nanoparticles in the sapphire matrix under the action of nanosecond laser pulses.     

Femtosecond laser patterning of Ta0.1W0.9Ox/ITO thin film stack

Selective laser patterning of thin films in a multilayered structure is an emerging technology for process development and fabrication of optoelectronics and microelectronics devices. In this work, femtosecond laser patterning of electrochromic Ta_0.1W_0.9O_x film coated on ITO glass has been studied to understand the selective removal mechanism and to determine the optimal parameters for patterning process. A 775 nm Ti:sapphire laser with a pulse duration of 150 fs operating at 1 kHz was used to irradiate the thin film stacks with variations in process parameters such as laser fluence, feedrate and numerical aperture of objective lens. The surface morphologies of the laser irradiated regions have been examined using a scanning electron microscopy and an optical surface profiler. Morphological analysis indicates that the mechanism responsible for the removal of Ta_0.1W_0.9O_x thin films from the ITO glass is a combination of blistering and explosive fracture induced by abrupt thermal expansion. Although the pattern quality is divided into partial removal, complete removal, and ITO film damage, the ITO film surface is slightly melted even at the complete removal condition. Optimal process window, which results in complete removal of Ta_0.1W_0.9O_x thin film without ablation damage in the ITO layer, have been established. From this study, it is found that focusing lens with longer focal length is preferable for damage-free pattern generation and shorter machining time.     

Surface topography of ultrashort laser-irradiated CaF2

A single-crystal CaF₂ (111) was irradiated with single and multiple laser (Ti:sapphire, 800 nm, 25 fs) shots at fluences ranging from 0.25 to 1.5 J cm^?2. In this fluence regime, a single laser pulse usually leads to typical bump-like features ranging from 200 nm to 1.5 μm in diameter and 10–50 nm in height. These bumps are related to compressive stresses due to a pressure build-up induced by fast laser heating and their subsequent relaxation. When CaF₂ is irradiated with successive (in our case 20) shots at a laser fluence of 1.5 J cm^?2, nanocavities at the top of the microbumps are observed. The formation of these nanocavities is regarded as an explosion and is attributed to the explosive expansion generated by shock waves due to laser-induced plasma after the nonlinear absorption of the laser energy by the material. Such kinds of surface structures at the nanometre scale could be attractive for nanolithography.     

Femtosecond laser ablation of cemented carbides: properties and tribological applications

Laser ablation with fs laser pulses was performed in air on cobalt cemented tungsten carbide by means of a Ti : sapphire laser (800 nm, 100 fs). Small and moderate fluences (2, 5, 10 J/cm²) and up to 5×10⁴ pulses per irradiated spot were used to drill holes with aspect ratios up to 10. Cross-section cuts from laser-irradiated samples were produced and they were analysed with optical microscopy and SEM. EDX analyses were carried out on selected zones. Quasi-cylindrical holes were found for 2 J/cm², whereas for 5 and 10 J/cm² irregular shapes (lobes, bottoms wider than hole entrances) were found to occur after a given number of incident pulses. Layers with modified structure were evidenced at pore walls. SEM revealed a denser structure, while EDX analyses showed uniform and almost similar contents of W, C, and Co in these layers. As a direct application, patterning of coated WC-Co was carried out with 2 J/cm² and 100 pulses per pore. The resulted surfaces were tribologically tested and these tests revealed an improved friction and wear behaviour. PACS 42.65.Cs; 79.60.Ds     

Study on sapphire removal for thin-film LEDs fabrication using CMP and dry etching

Mechanical grinding, chemical mechanical polishing (CMP) and dry etching process are integrated to remove sapphire substrate for fabricating thin-film light-emitting diodes. The thinning of sapphire substrate is done by fast mechanical grinding followed by CMP. The CMP can remove or reduce most of the scratches produced by mechanical grinding, recovering both the mechanical strength and wafer warpage to their original status and resulting in a smoother surface. The surface morphology and surface roughness on grinded and polished sapphire substrate are measured by using atomic force microscopy (AFM). The etch rates of sapphire by BCl₃-based dry etching are reported. Pattern transfer to the physical and chemical stability of sapphire is made possible by inductively coupled plasma (ICP) etch system that generates high density plasma. The patterning of several microns period in sapphire wafer by using a combination of BCl₃/Ar plasma chemistry and SiO₂ mask is presented. The anisotropic etch profile formed on sapphire wafer is obtained from scanning electron microscopy (SEM) images.     

Generation of strong coherent extreme ultraviolet radiation from the laser plasma produced on the surface of solid targets

We demonstrate the generation of high harmonics (up to the 65th order, λ=12.24 nm) of a Ti:sapphire laser radiation after the propagation of femtosecond laser pulses through the low-excited plasma produced by a picosecond prepulse radiation on the surface of different targets. High-order harmonics generated from the surface plasma of most targets showed a plateau pattern. It is assumed that the harmonic generation in these conditions occurs due to the interaction of the femtosecond pulses with the ions. The conversion efficiencies at the plateau region were varied between 1×10^-7 to 8×10^-6, depending on the target. The main contribution to the limitation of harmonic generation efficiency and cutoff energy was attributed to the self-defocusing of main pulse. A considerable restriction of the 27th harmonic generation was observed at different focusing conditions in the case of chromium plasma. Our observation of the resonance-induced enhancement of a single harmonic (λ=61.2 nm) at a plateau region with the efficiency of 8×10^-5 in the case of In plasma can offer some expectation that analogous processes can be realized in other plasma samples in the shorter wavelength range where the highest harmonics were achieved. PACS 42.65.Ky; 52.35.Mw; 52.38.-r     

Nanostructured substrate with nanoparticles fabricated by femtosecond laser for surface-enhanced Raman scattering

A simple and fast method to fabricate nanostructured substrates with silver nanoparticles over a large area for surface-enhanced Raman scattering (SERS) is reported. The method involves two steps: (1) dip the substrate into a silver nitrate solution for a few minutes, remove the substrate from the solution, and then air dry and (2) process the silver nitrate coated substrate by femtosecond (fs) laser pulses in air. The second step can create silver nanoparticles distributed on the nanostructured surface of the substrate by the photoreduction of fs multiphoton effects. This study demonstrates that an enhancement factor (EF) greater than 5×10⁵, measured by 10⁻⁶ M Rhodamine 6G solution, can be achieved. The proposed technique can be used to integrate the SERS capability into a microchip for biomedical and chemical analysis.     

Identification of ultra-fast electronic and thermal processes during femtosecond laser ablation of Si

Ultra-fast electronic and thermal processes for the energy deposition mechanism during femtosecond laser ablation of Si have been identified by means of atomic force microscopy and Raman scattering techniques. For this purpose, Si targets were exposed with 800-nm, 25-fs Ti:sapphire laser pulses for different laser fluencies in air and under UHV (ultra high vacuum) conditions. Various nano- and microstructures on the surface of the irradiated samples are revealed by a detailed surface topography analysis. Ultra-fast electronic processes are dominant in the lower-fluence regime. Therefore, by starting from the ablation threshold three different fluence regimes have been chosen: a lower-fluence regime (0.06–0.5 J?cm^?2 single-shot irradiation under UHV condition and 0.25–2.5 J?cm^?2 single-shot irradiation in ambient condition), a moderate-fluence regime (0.25–1.5 J?cm^?2 multiple-shot irradiation), and a higher-fluence regime (2.5–3.5 J?cm^?2 multiple-shot irradiation). Around the ablation threshold fluence, most significant features identified at the Si surface are nanohillock-like structures. The appearance of these nanohillocks is regarded as typical features for fast electronic processes (correlated with existence of hot electrons) and is explained on the basis of Coulomb explosion. The growth of these typical features (nanohillocks) by femtosecond laser irradiation is an element of novelty. At moderate irradiation fluence, a ring-shaped ablation with larger bumps and periodic surface structures is observed and is considered as a footprint of ultra-fast melting. Further increase in the laser fluence, i.e. a higher-fluence regime, resulted in strong enhancement of the thermal process with the appearance of larger islands. The change in surface topography provides an innovative clue to differentiate between ultra-fast electronic processes, i.e. Coulomb explosion (sub-100 fs) at a lower-fluence regime and ultra-fast melting (hundreds of fs) at a moderate-fluence regime, and slow thermal processes (ps time scale) at a higher-fluence regime. These fast electronic and thermal processes are well correlated to structural and crystallographic alterations, inferred from Raman spectroscopy.     

Study of 2<Emphasis Type="Italic">ω</Emphasis> and 3/2<Emphasis Type="Italic">ω</Emphasis> harmonics in ultrashort high-intensity laser plasma interaction

An experimental study is presented on measurements of optical spectrum of the laser light scattered from solid surface irradiated by Ti:sapphire laser pulses up to an intensity of 1.2 × 10¹⁸ W cm⁻². The spectrum has well-defined peaks at wavelengths corresponding to 2ω and 3/2ω radiations. The spectral features vary with the laser intensity and show blue-shift with increasing laser intensity. At a constant laser fluence, the spectrum is red-shifted with increasing laser pulse duration. The observed results are explained in terms of the density scale length variation of the plasma and laser chirp.     

High harmonic generation in a laser plasma

The results of investigation of high harmonics of radiation of a Ti:sapphire laser propagating through a laser plasma generated on the surface of different targets are presented. For most of the targets, the intensity distribution of the high harmonics generated is found to form a plateaulike pattern similar to that observed in the case of gas jets. The generation of high harmonics (up to the 65th harmonic, λ = 12.24 nm) is caused by the interaction of femtosecond laser radiation with ions. The conversion efficiency in the plateau region varies from 10^?7 to 8 × 10^?5 depending on the target. The main restriction on the conversion efficiency and the peak intensity of the harmonics generated is caused by the self-defocusing of the femtosecond radiation due to free charge carriers formed as a result of tunnel ionization.     

Evaporation of millimeter water drops in the field of IR laser radiation

The evaporation of large (∼10⁻³ m across) water drops in the field of IR (10.6 μm) laser radiation of power density (4–12)×10⁵ W/m² is considered. Qualitative analysis shows that the process is described well with an optical cavity model. A mechanism of water evaporation is found to be associated with surface electromagnetic waves, which break hydrogen bonds in the high-frequency (≈3×10¹³ s⁻¹) field of the laser. The theory is in good agreement with experimental data. Original Russian Text ? V.I. Trigub, 2006, published in Zhurnal Tekhnicheskoĭ Fiziki, 2006, Vol. 76, No. 4, pp. 120–123.     

Development of ultra-short pulse VUV laser system for nanoscale processing

We have developed intense vacuum ultraviolet (VUV) radiation sources for advanced material processing, such as photochemical surface reactions and precise processing on a nanometer scale. We have constructed a new VUV laser system to generate sub-picosecond pulses at the wavelength of 126 nm. A seed VUV pulse was generated in Xe as the 7th harmonic of a 882-nm Ti:sapphire laser. The optimum conversion was achieved at the pressure of 1.2 Torr. The seed pulse will be amplified by the Ar₂^*\mathrm{Ar}_{2}^{*} media generated by an optical-field-induced ionization Ar plasma produced by the Ti:sapphire laser. We have obtained a gain coefficient of g=0.16 cm⁻¹. Our developing system will provide VUV ultra-short pulses with sub-μJ energy at a repetition rate of 1 kHz.     

Novel method to determine the actual surface area of a laser-nanotextured sensor

The actual surface area of a gold-coated conductive layer over the laser nano-textured surface of sapphire is determined using an electrochemical cyclic voltammetry. The method is down scaled to measure the sensing surface area of 200 × 200 μm² on a laser-ablated ripple sensor used for surface-enhanced Raman spectroscopy/scattering (SERS). Ripple SERS sensors made on different substrates of high refractive index materials such as GaP, diamond, SiC, and Al₂O₃ make a versatile sensing platform with the detection of analyte (here a thiophenol) down to 10 nM concentrations. Direct measurement of the surface area provides a powerful tool to investigate roughness, porosity, and morphology of coatings used for SERS or other light harvesting surfaces such as solar cells. Novelty of the proposed method is in the use of cathodic peak of surface passivation–activation cycle for calculation of surface charge. The method enables high-accuracy surface area measurements from as small as 0.01 mm² pads up to functional solar cells.     

Identification of non-thermal and thermal processes in femtosecond laser-ablated aluminum

Non-thermal and thermal processes due to femtosecond laser ablation of aluminum (Al) at low, moderate, and high-fluence regimes are identified by Atomic Force Microscope (AFM) surface topography investigations. For this purpose, surface modifications of Al by employing 25 fs Ti: sapphire laser pulses at the central wavelength of 800 nm have been performed to explore different nano- and microscale features such as hillocks, bumps, pores, and craters. The mechanism for the formation of these diverse kinds of structures is discussed in the scenario of three ablation regimes. Ultrafast electronic and non-thermal processes are dominant in the lower fluence regime, whereas slow thermal processes are dominant at the higher fluence regime. Therefore, by starting from the ablation threshold three different fluence regimes have been chosen: a lower fluence regime (0.06–0.5 J cm^?2 single-shot irradiation under ultrahigh vacuum condition and 0.25–2.5 J cm^?2 single-shot irradiation in ambient condition), a moderate-fluence regime (0.25–1.5 J cm^?2 multiple-shot irradiation), and a high-fluence regime 2.5–3.5 J cm^?2 multiple-shot irradiation. For the lower fluence (gentle ablation) regime, around the ablation threshold, the unique appearance of individual, localized Nano hillocks typically a few nanometers in height and less than 100 nm in diameter are identified. These Nano hillock-like features can be regarded as a nonthermal, electronically induced phase transition process due to localized energy deposition as a result of Coulomb explosion or field ion emission by surface optical rectification. At a moderate-fluence regime, slightly higher than ablation threshold multiple-pulse irradiation produces bump-formation and is attributed to ultrafast melting (plasma formation). The high-fluence regime results in greater rates of material removal with highly disturbed and chaotic surface of Al with an appearance of larger protrusions at laser fluence well above the ablation threshold. These nonsymmetrical shapes due to inhomogeneous nucleation, cluster formation, and resolidification of a metallic surface after melting are attributable to slow thermal processes (ps time scale).     

Optical properties of sapphire in its opacity range

We have studied the reflection spectrum of leucosapphire in the range of 2.5–25.0 μm. Based on the analysis of the known frequency and temperature dependences of the absorption coefficient in the range of 2.5–7.0 μm, its extrapolation to the range of 10.6 μm has been performed. We have shown that the absorption coefficient in the range of 10.6 μm and in the temperature interval 300–2300 K can be evaluated as β = (2–3) × 10⁴ cm^–1. It has also been shown that the value of this characteristic correlates with the results of investigations of the action of a powerful radiation pulse of a СО₂ laser on the surface of anodized aluminum. These data can be used in the development of technologies of laser processing of articles made of sapphire and ceramics based on aluminum oxide, as well as anodized articles made of aluminum alloys.     

ZnO nanowall networks grown on DiMPLA pre‐patterned thin gold films

ZnO nanowall networks grown by a high pressure pulsed laser deposition (PLD) technique on a pre‐patterned thin gold film are presented. The thin gold film on a c ‐plane oriented sapphire substrate was structured with diffraction mask projection laser ablation (DiMPLA). It is shown that only areas processed with the laser patterning technique reveal homogeneous growth of ZnO nanowall networks. Photoluminescence measurements prove the higher material quality of the pre‐patterned regions compared to the untreated ones. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Micro patterning of fused silica by laser ablation mediated by solid coating absorption

Precise patterning by laser ablation requires sufficient absorption. For weak absorbers like fused silica indirect methods using external absorbers have been developed. A novel approach using a solid SiO absorber coating is described. Irradiation by an ArF excimer laser (wavelength 193 nm) is leading to ablation of the coating and, at sufficiently high fluence, of the fused silica substrate. The remaining coating in the unexposed areas is removed afterwards by large area irradiation. The fluence threshold for substrate ablation using a 28 nm thick absorber layer is about 1.1 J/cm². Single pulse ablation rates of up to 800 nm and a surface roughness of R _a<5 nm are obtained. High resolution grating patterns with 400 nm period and a modulation depth of 80 nm are possible. The process can be described as controlled plasma mediated ablation.     

一种测量高温中间包的蓝宝石光纤温度计

介绍了一种测量高温的蓝宝石光纤温度计.蓝宝石单晶光纤由于其极好的高温物理化学性能,适用于高温下光纤测温应用,可用作辐射型光纤温度传感器.蓝宝石光纤温度计采用激光加热小基座法生长出端部掺Cr3+的蓝宝石光纤荧光温度传感头.用激光加热小基座,把对荧光有温度反应的材料如红宝石晶体光纤生长在蓝宝石光纤上,制成具有结构紧凑,耐高温,功能稳定的传感探头.通过荧光寿命的检测,可以测量所对应的温度.根据表面温度,可以依据温度场得到内部温度,用于测量连铸炉中的中间包钢水温度,并给出了温度计的实验系统以及原始实验数据.实验数据表明,此结果精度高,可实现非接触测量.