Processing of Diamond for Integrated Optic Devices Using Q-Switched Nd:YAG Laser at Different Wavelengths

In the present investigation, a Q-switched Nd:YAG laser is used to study the various aspects of diamond processing for fabricating integrated optic and UV optoelectronic devices. Diamond is a better choice of substrate compared to silicon and gallium arsenide for the fabrication of waveguides to perform operations such as modulation, switching, multiplexing, and filtering, particularly in the ultraviolet spectrum. The experimental setup of the present investigation consists of two Q-Switched Nd:YAG lasers capable of operating at wavelengths of 1064 nm and 532 nm. The diamond cutting is performed using these two wavelengths by making the “V”-shaped groove with various opening angle. The variation of material loss of diamond during cutting is noted for the two wavelengths. The cut surface morphology and elemental and structural analysis of graphite formed during processing in both cases are compared using scanning electron microscopy (SEM) and laser Raman spectroscopy. Both the Q-Switched Nd:YAG laser systems (at 1064 nm and 532 nm) show very good performance in terms of peak-to-peak output stability, minimal spot diameter, smaller divergence angle, higher peak power in Q-switched mode, and good fundamental TEM₀₀ mode quality for processing natural diamond stones. Less material loss and minimal micro cracks are achieved with wavelength 532 nm whereas a better diamond cut surface is achieved with processing at 1064 nm with minimum roughness.     

Single pulse near field study on a Co(3 nm)/Cu(6 nm)/Co(20 nm) multilayer structure by using a femtosecond laser

Single pulse near field study on a Co(3 nm)/Cu(6 nm)/Co(20 nm) multilayer structure was experimentally investigated with a laser pulse width of 200 fs at a wavelength of 775 nm. For the near field experiments, we have used polystyrene colloidal particles of 700 nm diameter deposited by spin coating on top of the multilayer structure, as well on top of Co (50 nm) and Cu (50 nm) thin films. The diameter and the morphologies of the holes were investigated by scanning electron microscopy (SEM) and atomic force microscopy (AFM). We have estimated the fluence thresholds values for the near field and discuss their values in respect with the enhancement factor of the intensity of the electromagnetic field due to the use of the colloidal particles. We compare the depths and the widths of the holes obtained at the same peak laser fluence for the Co thin film (50 nm), Cu thin film (50 nm) and Co(3 nm)/Cu(6 nm)/Co(20 nm) multilayer structure. Depending on the laser fluence, the ablation depth can reach the first, the second, or the third layer. Theoretical estimations of the intensity enhancement were done using the finite-difference time-domain (FDTD) by using the RSoft software. This type of a selective distribution of the ablation depth, in the near field regime, of a planar metal/dielectric interface can open new perspective in the excitation of propagating surface plasmons.     

A Pressure Sensor Using Fiber Bragg Grating

In the present investigation, a Q-switched Nd:YAG laser is used to study the various aspects of diamond processing for fabricating integrated optic and UV optoelectronic devices. Diamond is a better choice of substrate compared to silicon and gallium arsenide for the fabrication of waveguides to perform operations such as modulation, switching, multiplexing, and filtering, particularly in the ultraviolet spectrum. The experimental setup of the present investigation consists of two Q-Switched Nd:YAG lasers capable of operating at wavelengths of 1064 nm and 532 nm. The diamond cutting is performed using these two wavelengths by making the “V”-shaped groove with various opening angle. The variation of material loss of diamond during cutting is noted for the two wavelengths. The cut surface morphology and elemental and structural analysis of graphite formed during processing in both cases are compared using scanning electron microscopy (SEM) and laser Raman spectroscopy. Both the Q-Switched Nd:YAG laser systems (at 1064 nm and 532 nm) show very good performance in terms of peak-to-peak output stability, minimal spot diameter, smaller divergence angle, higher peak power in Q-switched mode, and good fundamental TEM ₀₀ mode quality for processing natural diamond stones. Less material loss and minimal micro cracks are achieved with wavelength 532 nm whereas a better diamond cut surface is achieved with processing at 1064 nm with minimum roughness.     

Cleaning of artificially soiled paper using nanosecond, picosecond and femtosecond laser pulses

Cleaning of cultural assets, especially fragile organic materials like paper, is a part of the conservation process. Laser radiation as a non-contact tool offers prospects for that purpose. For the studies presented here, paper model samples were prepared using three different paper types (pure cellulose, rag paper, and wood-pulp paper). Pure cellulose serves as reference material. Rag and wood-pulp paper represent essential characteristics of the basic materials of real-world artworks. The papers were mechanically soiled employing pulverized charcoal. Pure and artificially soiled paper samples were treated with laser pulses of 28 fs (800 nm wavelength) and 8–12 ns (532 nm) duration in a multi pulse approach. Additionally, the cellulose reference material was processed with 30 ps (532 nm) laser pulses. Damage and cleaning thresholds of pure and soiled paper were determined for the different laser regimes. Laser working ranges allowing for removal of contamination and avoiding permanent modification to the substrate were found. The specimens prior and after laser illumination were characterized by light-optical microscopy (OM) and scanning electron microscopy (SEM) as well as multi spectral imaging analysis. The work extends previous nanosecond laser cleaning investigations on paper into the ultra-short pulse duration domain.     

Analysis of materials modifications caused by UV laser micro drilling of via holes in AlGaN/GaN transistors on SiC

Pulsed UV laser drilling can be applied to fabricate vertical electrical interconnects (vias) for AlGaN/GaN high electron mobility transistor devices on single-crystalline silicon carbide (SiC) substrate. Through-wafer micro holes with a diameter of 50-100 μm were formed in 400 μm thick bulk 4H-SiC by a frequency-tripled solid-state laser (355 nm) with a pulse width of ≤30 ns and a focal spot size of ∼15 μm. The impact of laser machining on the material system in the vicinity of micro holes was investigated by means of micro-Raman spectroscopy and transmission electron microscopy. After removing the loosely deposited debris by etching in buffered hydrofluoric acid, a layer of <4 μm resolidified material remains at the side walls of the holes. The thickness of the resolidified layer depends on the vertical distance to the hole entry as observed by scanning electron microscopy. Micro-Raman spectra indicate a change of internal strain due to laser drilling and evidence the formation of nanocrystalline silicon (Si). Microstructure analysis of the vias’ side walls using cross sectional TEM reveals altered degree of crystallinity in SiC. Layers of heavily disturbed SiC, and nanocrystalline Si are formed by laser irradiation. The layers are separated by 50-100 nm thick interface regions. No evidence of extended defects, micro cracking or crystal damage was found beneath the resolidified layer. The precision of UV laser micro ablation of SiC using nanosecond pulses is not limited by laser-induced extended crystal defects.     

Three-dimensional photofabrication with femtosecond lasers for applications in photonics and biomedicine

A status report on rapidly advancing femtosecond laser technology, three-dimensional (3D) microstructuring by multiphoton illumination technique, is given. Taking its origin from multiphoton microscopy, this technique is now becoming an important microfabrication tool. In our work we apply near-infrared Ti:sapphire femtosecond laser pulses (at 800/780 nm) for 3D material processing. When tightly focused into the volume of a photosensitive material (or photoresist), they initiate 2PP process by, for example, transferring liquid into the solid state. This allows the fabrication of any computer generated 3D structure by direct laser “recording” into the volume of photosensitive material. 2PP of photosensitive materials irradiated by femtosecond laser pulses is now considered as enabling technology for the fabrication of 3D photonic crystals and photonic crystal templates. In particular, 2PP allows one to introduce defects at any desired locations, which is crucial for the practical applications. Recently, we studied possible applications of 2PP technique in biomedicine. 2PP is a very interesting technique for the fabrication of drug delivery systems, scaffolds for tissue engineering, and medical implants. These and other biomedical applications of 2PP will be reviewed.     

Solidification microstructure of AZ91D Mg alloy after laser surface melting

The solidification microstructure plays a critical role in determining the surface properties of laser-treated magnesium alloys. The purpose of this paper is to study the solidification microstructures of AZ91D Mg alloy following millisecond- and nanosecond-pulse Nd:YAG laser irradiation. The solidification microstructural evolution of laser-melt AZ91D Mg alloy was investigated using X-ray diffractometry, scanning electron microscopy, energy-dispersive X-ray spectrometer and transmission electron microscopy. Much refined α-Mg phase and β-Mg₁₇Al₁₂ intermetallics were observed in the microstructure after laser surface melting. Periodic and successive structure was observed in the millisecond irradiated surface and the melt depth was more than 100 μm. The solidification microstructure was mainly cellular/dendrite structures together with a large number of β-Mg₁₇Al₁₂ nano-particles. Micron holes were found in the nanosecond irradiated surface and the melt depth was shallow at 50 μm. Millisecond-pulse Nd:YAG laser was found to be more suitable for Mg alloy surface treatment due to sufficient melt depth.     

Laser and plasma nitriding of titanium using CW-CO2 laser in the atmosphere

Surface nitriding of the titanium by the mixing technology with laser and plasma (LPN) in atmosphere has been investigated. Comparing with the technique of laser nitriding, we could obtain the titanium nitride at relatively low laser power density and the oxidation was prevented without the chamber. The synthesized layers comprised of titanium nitrides were about 178 μm depth. The effect of the laser power density, scanning velocity, and plasma flow rate on the components consisting of the material of the nitrided layer was studied. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to reveal the components consisting of the material of the nitrided layer.     

Microscopic investigation of single-crystal diamond following ultrafast laser irradiation

We present a structural investigation of single-crystal diamond following ultrafast laser irradiation of the surface and the bulk material. Optical microscopy, atomic force microscopy, scanning electron microscopy, and focused-ion beam and transmission electron microscopy techniques were utilized to selectively examine the final state of the samples. Laser induced periodic surface structures (LIPSS) with high- and low-spatial frequencies were obtained with multiple-pulse surface irradiation under both stationary and translated target conditions. High magnification transmission electron microscopy analysis of cross sections of the LIPSS revealed modified layers of a few tens of nanometers in thickness capping the crystalline diamond matrix. Sub-surface irradiation of diamond at high laser fluences led to damaged regions and cracks in the bulk material. When translational bulk irradiation of the diamond was performed, substantially sub-wavelength periodic structures were observed at the unpolished side facet of the diamond plate where the laser focus was translated out of the bulk. Spatial periods were 140 nm and the structures largely consisted of single-crystal diamond with a 10 nm modified layer. Finally, preliminary studies of single-shot laser ablation craters at high laser fluences exhibited suppression of material removal for peak values above 45 J/cm².     

Direct photoetching of single crystal SiC by VUV-266 nm multiwavelength laser ablation

2 O₂:H₂O and HF:H₂O. The analysis of the etched samples by scanning electron microscopy (SEM) and scanning probe microscopy (SPM) indicates that an array of square holes having well-defined patterned structures and clean substrate surfaces were obtained. The X-ray photoelectron spectroscopy (XPS) analysis indicates that the SiC samples etched by VUV-266 nm multiwavelength laser have a similar stoichiometry after chemical post-treatment as the virgin SiC. The mechanism of high-quality ablation using VUV-266 nm multiwavelength laser is discussed in comparison with ablation using 266 nm single wavelength. The chemical post-treatment contributes to removing the residues from the laser photolysis of SiC. Received: 26 August 1996/Accepted: 17 October 1996     

Size and density control of silicon oxide nanowires by rapid thermal annealing and their growth mechanism

In this work, we demonstrate a fast approach to grow SiO₂ nanowires by rapid thermal annealing (RTA). The material characteristics of SiO₂ nanowires are investigated by field emission scanning electron microscopy, high-resolution transmission electron microscopy (HRTEM), high-angle annular dark-field (HAADF) imaging, electron energy loss spectroscopy (EELS), and energy-filtered TEM (EFTEM). The HAADF images show that the wire tip is predominantly composed of Pt with brighter contrast, while the elemental mappings in EFTEM and EELS spectra reveal that the wire consists of Si and O elements. The SiO₂ nanowires are amorphous with featureless contrast in HRTEM images after RTA at 900°C. Furthermore, the nanowire length and diameter are found to be dependent on the initial Pt film thickness. It is suggested that a high SiO₂ growth rate of >1 μm/min can be achieved by RTA, showing a promising way to enable large-area fabrication of nanowires.     

The coalescence of supported gold nanoparticles induced by nanosecond laser irradiation

Gold nanoparticles supported on a quartz substrate are fabricated by e-beam lithography and subjected to nanosecond laser irradiation to induce coalescence. In combination with ex-situ scanning electron microscopy and optical extinction spectra, transmission is monitored in-situ to determine the characteristic coalescence time, the threshold fluence for the onset of coalescence and the produced particle morphology. Parallel molecular dynamics simulation is employed and shown to reasonably predict the coalescence time, thus explaining the experimental results. PACS 82.60.Qr; 42.62.Cf; 81.07.-b; 64.70.Nd     

Direct writing of conductive silver micropatterns on flexible polyimide film by laser-induced pyrolysis of silver nanoparticle-dispersed film

This article describes fabrication of Ag micropatterns on a flexible polyimide (PI) film by laser direct writing using an Ag nanoparticle-dispersed film as a precursor. Ag micropatterns are characterized by optical microscopy, atomic force microscopy (AFM), field emission scanning electron microscopy (FE-SEM), surface profilometry, and resistivity measurements. The line width of Ag micropatterns can be effectively controlled by altering the experimental parameters of laser direct writing especially laser intensity, objective lens, and laser beam scanning speed etc. Using an objective lens of 100× and laser intensity of 170.50 kW/cm², Ag micropatterns with a line width of about 6 μm have been achieved. The Ag micropatterns show strong adhesion to polyimide surface as evaluated by Scotch-tape test. The resistivity of the Ag micropatterns is determined to be 4.1 × 10⁻⁶ Ω cm using two-point probe method. This value is comparable with the resistivity of bulk Ag (1.6 × 10⁻⁶ Ω cm).     

Three dimensional accurate morphology measurements of polystyrene standard particles on silicon substrate by electron tomography

Polystyrene latex (PSL) nanoparticle (NP) sample is one of the most widely used standard materials. It is used for calibration of particle counters and particle size measurement tools. It has been reported that the measured NP sizes by various methods, such as Differential Mobility Analysis, dynamic light scattering (DLS), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM), differ from each other. Deformation of PSL NPs on mica substrate has been reported in AFM measurements: the lateral width of PSL NPs is smaller than their vertical height. To provide a reliable calibration standard, the deformation must be measured by a method that can reliably visualize the entire three dimensional (3D) shape of the PSL NPs. Here we present a method for detailed measurement of PSL NP 3D shape by means of electron tomography in a transmission electron microscope. The observed shape of the PSL NPs with 100 nm and 50 nm diameter were not spherical, but squished in direction perpendicular to the support substrate by about 7.4% and 12.1%, respectively. The high difference in surface energy of the PSL NPs and that of substrate together with their low Young modulus appear to explain the squishing of the NPs without presence of water film.     

Sphere-shaped SiGe micro/nanostructures with tunable Ge composition and size formed by laser irradiation

SiGe spheres with different diameters are successfully fabricated on a virtual SiGe template using a laser irradiation method. The results from scanning electron microscopy and micro-Raman spectroscopy reveal that the diameter and Ge composition of the SiGe spheres can be well controlled by adjusting the laser energy density. In addition, the transmission electron microscopy results show that Ge composition inside the Si Ge spheres is almost uniform in a well-defined, nearly spherical outline. As a convenient method to prepare sphere-shaped SiGe micro/nanostructures with tunable Ge composition and size, this technique is expected to be useful for Si Ge-based material growth and micro/optoelectronic device fabrication.     

Grain Orientation,Angle of Incidence,and Beam Polarization Effects on Ultraviolet 300 ps-Laser-Induced Nanostructures on 316L Stainless Steel

Laser-induced periodic surface structures (LIPSS) represent a unique route for functionalizing materials through the fabrication of surface nanostructures. Commercial AISI 316L stainless steel (SS316L) surfaces are laser treated by ultraviolet 300 ps laser pulses in a laser line scanning (LLS) approach. Processing parameters are optimized (pulse energy of 2.08 µJ, pulse repetition frequency of 300 kHz, and suitable laser scan and sample displacement rates) for the generation of low spatial frequency LIPSS over a large 25 × 25 mm² area. Different angles of incidence of the laser radiation (0°, 30°, and 45°) and different linear laser beam polarizations (s and p) produce a plethora of rippled surface morphologies at distinct grains. Scanning electron microscopy and 2D Fourier transforms, together with calculations of the optical energy deposited at the treated surfaces using Sipe's first-principles electromagnetic scattering theory, are used to study and analyze in detail these surface morphologies. Combined with electron backscattering diffraction, analyses allow associating site-selectively various laser-induced-surface morphologies with the underlying crystalline grain orientation. Resulting grain orientation maps reveal a strong impact of the grain crystallographic orientation on LIPSS formation and point toward possible strategies, like multi-step processes, for improving the manufacturing of LIPSS and their areal coverage of polycrystalline technical materials.     

Recent advances in imaging of properties and growth of low dimensional structures for photonics and electronics by XPEEM

Spectroscopic Photoemission and Low Energy Electron Microscopy (SPELEEM) is a very powerful and diverse microscopy technique for the investigation of surfaces, interfaces, buried layers and nanoscale objects like nanoparticles and nanowires. The many significant results from photoemission Electron microscopy (PEEM) in recent years are linked with the exploitation of advanced light sources such as synchrotrons and new advanced laser systems. Combined also with low energy electron microscopy (LEEM) it allows a complementary chemical and structural analysis making LEEM/PEEM a versatile multitechnique instrument. To illustrate the extreme diversity, we give a summary of the recent studies with the SPELEEM installed at the soft X-ray beamline I311 at the MAXII synchrotron storage ring and a portable electrostatic PEEM used with ultra-fast XUV laser technology. The examples cover topics such as full-cone 3D band mapping by using the photoelectron diffraction mode of the microscope, growth mechanism and detailed doping profile of III–V nanowires, growth and intercalation of graphene on SiC substrates, droplet dynamics on GaP(1 1 1) surface, surface chemistry and control of nanostructure fabrication. Moreover, the first results of PEEM experiments using extreme ultraviolet attosecond pulse trains are discussed.     

Fabrication of microstructures in Foturan glass using infrared femtosecond laser pulses and chemical etching

In this study, a method for the fabrication of microstructures on the surface and inside Foturan glass by femtosecond laser-induced modification was developed. This technique was followed by heat treatment to crystallize the modified area, and the specimen was then placed in an 8% HF acid solution for chemical etching. The fabricated microstructures were observed using scanning electron microscopy (SEM). The results demonstrated that the etching time is an important parameter in the fabrication of microstructures on Foturan glass. An example of a tapered U-shaped microchannel with a minimized neck diameter of about 5 μm at the central point for cell detection is presented.     

Confocal laser scanning microscopy and scanning electron microscopy of tissue Ti-implant interfaces.

Microscopic inspection of heterogenous three-dimensional (3D) objects such as oral implants, or implants in general, is conventionally performed either on ground sections of methyl-metacrylate-embedded material, at the cellular level by histologic analysis of the peri-implant tissue by light microscopy (LM), or at the supramolecular level by transmission electron microscopy (TEM). Alternatively, the architecture of the tissue/implant interface is visualized by scanning electron microscopy (SEM). The two approaches exclude each other because of the sample preparation.We elaborate conditions for the non-invasive analysis of tissue/implant interfaces by confocal laser scanning microscopy (CLSM) in buffer, hoping to obtain a 3D view of fluorescently labeled tissue constituents at the tissue implant interface and, through subsequent SEM, of the metal surface. The use of water-immersion objectives, originally developed for high LM under physiological conditions is essential.In an exploratory approach, the tissue/Ti-interfaces of two retrieved dental implants were analyzed. One was a step-cylinder used for orthodontic anchoring and the other was an endosseous step-screw implant retrieved after infection-related loosening prior to load. The adhering tissue fragments were fluorescently triple-labeled for actin, fibronectin, and sm-alpha-actin. Optical sections for fluorescent images and for the laser reflection map were registered concomitantly. This approach allowed the labeled structures to be located on the metal surface. Subsequently, the same implants were prepared for SEM of the tissue/implant interface, and upon removal of the adhering structures, of the underlying metal surface. Thus, specific proteins can be identified and their spatial architecture as well as that of the underlying metal surface can be visualized for one and the same implant. The immediate visualization after fluorescence labeling in buffer by means of water immersion objective lenses proved most critical.     

Formation and Characteristics of Through Holes with Picosecond-Laser Helical Drilling on Alloy Material

Precision drilling can improve the microhole quality by yielding a reduced recast layer thickness and no heat-affected zone. We evaluate the quality of the helical drilled holes, e.g., the recast layer, microcracks, and circularity by scanning electron microscopy. We investigate the overlap rate of the laser beam and find its influence on the efficiency of through-hole machining. The microhole entrance, exit, and side walls are smooth, without an accumulation of spattering material and the formation of a recast layer and microcracks. Optimum parameters for drilling through holes on alloy material GH2132 are a thickness of 500 μm, a laser fluence of 3.06 · 10^?2 J/mm², a pulse repetition rate of 100 kHz, and a helical speed of 60 rev/s. The tapering phenomenon can be avoided by using a helical system with a rotating stage, and the hole circularity is fairly good. Picosecond laser helical drilling can be effective for manufacturing microholes with a high quality. The development of high-power picosecond laser would promote picosecond laser drilling with future industrial relevance.