3D periodic structures grown on silicon by radiation of a pulsed Nd:YAG laser and their field emission properties

Periodic three-dimensional structures were successfully grown on single crystal Si wafers either bare or Au-covered under their exposure to a pulsed radiation of a Nd:YAG laser in vacuum. The structures protrude above the initial wafer surface for 10 μm while their spatial period is about 70 μm. The coupling of the laser radiation to Si surface is related to the thermal non-linear absorption of the near band gap radiation. The structures exhibit an efficient field emission with an average emission current of 5 mA/cm² and is sensitive to the post-treatment of samples. The drawbacks of the emission current densities are discussed.     

Modifications of He implantation induced cavities in silicon by MeV silicon implantation

Doppler broadening spectroscopy (DBS) coupled to a slow positron beam has been used to investigate the formation of He-cavities in the presence of high vacancy concentrations in Cz-Si (1 1 1). Si samples were first implanted with MeV Si ions in order to create a damaged Si layer. DBS measurements show the presence of divacancy (SV₂/SSi lattice=1.052,WV₂/WSi lattice=0.83) from the surface up to 4.2 μm depth with a concentration higher than 10¹⁸ cm⁻³. The thickness of this damaged layer was confirmed by spreading resistance measurements. In the second step, samples were implanted with 50 keV ³He with fluence of 10¹⁶ cm⁻². DBS results show that the apparent divancancy concentration decreases at ³He implantation depth ∼435 nm due to ³He passivation of vacancies that occurs during the implantation process. After 900 °C annealing, large defects are detected at depth up to 2 μm and (S, W) values suggest the detection of cavities at the implantation depth. We also report the possible presence of impurity complexes. The formation of these complexes is attributed to the gettering of metallic impurities present in the Si sample.     

A widely tunable (5-12.5 μm) continuous-wave mid-infrared laser spectrometer based on difference frequency generation in AgGaS2

A widely tunable (5-12.5 μm) continuous-wave (cw) mid-infrared (mid-IR) laser spectrometer based on difference frequency generation (DFG) by mixing an external-cavity diode laser (ECDL) with a Ti:Sapphire laser in an AgGaS₂ crystal is described. The wide tunability was achieved by tuning laser wavelength associated with crystal angle tuning under type II phase matching condition. A maximum output power of about 66 nW was obtained at 8.06 μm. High resolution spectrum of methane (CH₄) over more than 10 cm⁻¹ near 7.7 μm has been recorded to evaluate the performance of the developed DFG-based mid-IR laser spectrometer.     

Surface modifications of crystalline silicon created by high intensity 1064 nm picosecond Nd:YAG laser pulses

A study of silicon modification induced by a high intensity picosecond Nd:YAG laser, emitting at 1064 nm, is presented. It is shown that laser intensities in the range of 5 × 10¹⁰-0.7 × 10¹² W cm⁻² drastically modified the silicon surface. The main modifications and effects can be considered as the appearance of a crater, hydrodynamic/deposition features, plasma, etc. The highest intensity of ∼0.7 × 10¹² W cm⁻² leads to the burning through a 500 μm thick sample. At these intensities, the surface morphology exhibits the transpiring of the explosive boiling/phase explosion (EB) in the interaction area. The picosecond Nd:YAG laser-silicon interaction was typically accompanied by massive ejection of target material in the surrounding environment. The threshold for the explosive boiling/phase explosion (TEB) was estimated to be in the interval 1.0 × 10¹⁰ W cm⁻² < TEB ≤ 3.8 × 10¹⁰ W cm⁻².     

Investigation of a biofunctional polymeric coating deposited onto silicon microcantilevers

The paper deals with an appealing route to activate silicon microcantilevers (90, 110 and 130 μm long, 35 μm wide and 2 μm thick) for specific binding of biochemical species. The method consists in coating the underivatized microcantilevers with a biofunctional copolymer (based on N,N-dimethylacrylamide bearing silanating moieties) that was developed for low-density microarray assays on microscope glass slides. Coating deposition was obtained by dip-coating and its microstructure investigated by analyzing the resonance frequency values of bare and coated microcantilevers, by SEM and SFM imaging, SFM tip-scratch tests and XRR experiments. Results indicate that the coating is 2.5 nm thick and has a density of 1.22 g/cm³. The coating surface is nanostructured, displaying nanoblobs, which are from few up to 20 nm wide and, on average, 1.6 nm high. The diameter of the biggest nanoblobs is of the same order of magnitude of the gyration radius of the copolymer chains, suggesting that nanoblobs may identify individual macromolecules.     

Designing of endlessly single mode polarization maintaining highly birefringent nonlinear micro-structure fiber at telecommunication window by FV-FEM

An endlessly single mode highly polarization maintaining nonlinear microstructure fiber at telecommunication window is reported via full-vector finite element method. By taking three ring hexagonal PCF with suitable fiber parameter such as air hole diameter in cladding region d = 0.8 μm, pitch 2.3 μm and introducing four symmetrical large air holes near core region d′ = 2 μm, single mode (V_eff ≤ π), small effective mode area 2.7 μm², nonlinear co-efficient 44.39 W⁻¹ km⁻¹, high phase birefringence of the order of 10⁻³ and group birefringence of the order of 10⁻⁴ with beat length 0.3 μm at wavelength 1.55 μm are achieved.     

In vivo imaging of dynamic biological specimen by real-time single-shot full-field optical coherence tomography

We demonstrate the feasibility of a compact single-shot full-field time domain optical coherence tomography (OCT) for imaging dynamic biological sample in real-time. The system is based on a Linnik type polarization Michelson interferometer and a four-quadrature phase-stepper optics, which can simultaneously capture four quadraturely phase-stepped interferograms on a single CCD. Using a superluminescent diode as light source with center wavelength of 842 nm and spectral width of 16.2 nm, the system yields an axial resolution of 19.8 μm, and covers a field of view of 280 × 320 μm² (220 × 250 pixels) with a transverse resolution of 4.4 μm by using a 10× microscope objective (0.3 NA). Three-dimensional OCT images of biological samples such as an onion slice and a diaptomus were obtained without any image averaging or pixel binning. In addition, in vivo depth resolved dynamic imaging was demonstrated to show the beating internal structure of a diaptomus with a fame rate of 5 fps.     

Infrared electroluminescence from erbium-doped spark-processed silicon

The infrared (IR) electroluminescence (EL) of erbium-doped spark-processed silicon (sp-Si) was investigated. For this, a device was constructed which consisted of a silicon wafer on which an erbium layer was vapor deposited, followed by spark-processing and rapid thermal annealing for 15 min at 900 °C in air. The metallization consisted of a 200 nm Ag layer (above the spark-processed area) and a 50 nm thick Al film (on the “back side”), containing a window through which the light could escape. Maximal light emission occurred near 1.55 μm, that is, at a wavelength where commonly used fiber optical materials have their minimum in energy loss. The processing parameters for most efficient light emission were an Er thickness of 200-300 nm, a spark-processing time of about 30 s, an n-type Si wafer having a low (3-5 Ω cm) resistivity, an operating temperature near room temperature, and an operating voltage between 25 and 40 V under reverse bias. The results are interpreted by postulating an energy transfer from sp-Si to the Er³⁺ ions involving the first excited state ⁴I_13/2 to ground state ⁴I_15/2. Further, impact excitation and hot electrons that are accelerated into the erbium doped sp-Si by the applied field (100 kV/cm) are considered.     

Field emission behavior of cuboid zinc oxide nanorods on zinc-filled porous silicon

Single-crystalline zinc oxide (ZnO) nanorods with cuboid morphology have been prepared on the zinc-filled porous silicon substrate using a vapor phase transport method. Field-emission measurements showed that the turn-on field and threshold field of the cuboid ZnO nanorods film were about 3.2 and 8.2 V/μm respectively. From the emitter surface, a homogeneous emission image was observed with emission site density (ESD) of ∼10⁴ cm⁻². The better emission uniformity and the high ESD may be attributed to a large number of ZnO nanocrystallites as emitter on the surface of the nanorod end contributing to emission.     

Physical bounds of metallic nanofingers obtained by mechano-chemical atomic force microscope nanolithography

To obtain metallic nanofingers applicable in surface acoustic wave (SAW) sensors, a mechano-chemical atomic force microscope (AFM) nanolithography on a metallic thin film (50 nm in thickness)/piezoelectric substrate covered by a spin-coated polymeric mask layer (50-60 nm in thickness) was implemented. The effective shape of cross-section of the before and after etching grooves have been determined by using the AFM tip deconvolution surface analysis, structure factor, and power spectral density analyses. The wet-etching process improved the shape and aspect ratio (height/width) of the grooves and also smoothed the surface within them. We have shown that the relaxed surface tension of the polymeric mask layer resulted in a down limitation in width and length of the lithographed nanofingers. The surface tension of the mask layer can be changed by altering the initial concentration of the polymer in the deposition process. As the surface tension reduced, the down limitation decreased. In fact, an extrapolation of the analyzed statistical data has indicated that by decreasing the surface tension from 39 to 10 nN/nm, the minimum obtainable width and length of the metallic nanofingers was changed from about 55 nm and 2 μm to 15 nm and 0.44 μm, respectively. Using the extrapolation’s results, we have shown that the future SAW sensors buildable by this nanolithography method possess a practical bound in their synchronous frequency (∼58 GHz), mass sensitivity (∼6125 MHz-mm²/ng), and the limit of mass resolution (∼4.88 × 10⁻¹⁰ ng/mm²).     

Influence of the vacuum level upon the growth of carbon nanotubes on silicon carbide surface

We have investigated the influence of the vacuum level upon the growth of carbon nanotubes (CNTs) on 6H-SiC () surface.CNTs of about 160 nm in length were formed densely and uniformly on the 6H-SiC surface during annealing at 1700 °C in a high vacuum (∼10⁻² Pa). CNTs of about 1 μm in length were formed during annealing at 1700 °C in an ultra-high vacuum (∼10⁻⁷ Pa). However, CNTs were not formed and SiO₂ layers were formed on the SiC surface at 1700 °C in air. It is found that longer CNTs can grow up in an ultra-high vacuum, moreover, a little aligned and low-density graphite layers, or carbon nanofibers can also grow up.     

Photoluminescence from Er-doped silicon rich oxide thin films

 Photoluminescence (PL) properties of Er-doped silicon rich oxide thin films deposited on Si substrate by co-evaporation of silicon monoxide and Er under different atmospheres are investigated. The samples exhibit luminescence peak at 1.54 μm which could be assigned to the recombination in intra-4f Er³⁺ transition. PL shows that this transition is highest when ammonia atmosphere is used during deposition followed by an annealing temperature at 850 °C in 95% N₂+5% H₂ gas (forming gas). In fact, we believe that the presence of the N atoms around Er ions increases the intensity of the 1.54 μm luminescence.     

Laser shock wave consolidation of nanodiamond powders on aluminum 319

A novel coating approach, based on laser shock wave generation, was employed to induce compressive pressures up to 5 GPa and compact nanodiamond (ND) powders (4-8 nm) on aluminum 319 substrate. Raman scattering indicated that the coating consisted of amorphous carbon and nanocrystalline graphite with peaks at 1360 cm⁻¹ and 1600 cm⁻¹ respectively. Scanning electron microscopy revealed a wavy, non-uniform coating with an average thickness of 40 μm and absence of thermal effect on the surrounding material. The phase transition from nanodiamond to other phases of carbon is responsible for the increased coating thickness. Vicker's microhardness test showed hardness in excess of 1000 kg_f/mm² (10 GPa) while nanoindentation test indicated much lower hardness in the range of 20 MPa to 2 GPa. Optical surface profilometry traces displayed slightly uneven surfaces compared to the bare aluminum with an average surface roughness (R_a) in the range of 1.5-4 μm depending on the shock wave pressure and type of confining medium. Ball-on-disc tribometer tests showed that the coefficient of friction and wear rate were substantially lower than the smoother, bare aluminum sample. Laser shock wave process has thus aided in the generation of a strong, wear resistant, durable carbon composite coating on aluminum 319 substrate.     

Modeling of plasma-controlled surface evaporation and condensation of Al target under pulsed laser irradiation in the nanosecond regime

Phase transition on the surface of an aluminium target and vapour plasma induced by laser irradiation in the nanosecond regime at the wavelengths of 1.06 and 0.248 μm with an intensity of 10⁸-10⁹ W/cm² in vacuum are analysed. Particular attention is paid to the wavelength dependence of the observed phenomena and the non-one-dimensional effect caused by the Gaussian laser intensity distribution. A transient two-dimensional model is used which includes conductive heat transfer in the condensed phase, radiative gas dynamics and laser radiation transfer in the plasma as well as surface evaporation and back condensation at the phase interface. It is shown that distinctions in phase transition dynamics for the 1.06 and 0.248 μm radiation result from essentially different characteristics of the laser-induced plasmas. For the 1.06 μm radiation, evaporation stops after the formation of hot optically thick plasma, can occasionally resume at a later stage of the pulse, proceeds non-uniformly in the spot area, and the major contribution to the mass removal occurs in the outer part of the irradiated region. Plasma induced by the 0.248 μm laser is much more transparent therefore evaporation does not stop but continues in the subsonic regime with the Mach number of about 0.1.     

Surface temperature evolution in pulsed laser action of millisecond range

An originally developed multi-wavelength pyrometer (12 wavelengths in the range 1.001-1.573 μm, 50 μs acquisition time for each photodiode, 800 μm spatial resolution, 900-3500 °C brightness temperature range) is used to measure brightness temperature under the pulsed action of Nd:YAG laser (HAAS-HL62P) on stainless steel (INOX 304L) substrates. Specially developed “notch” filters (10⁻⁶ transparency at 1.06 μm wavelength) are applied to avoid the influence of laser radiation on temperature measurements. The true temperature is restored on the basis of method of multi-colour pyrometry. The accuracy of brightness temperature measurements is examined by comparing the temperature evolution for pulses with different durations but with the same value of energy density flux.The influence of the following parameters is studied keeping the remaining ones constant: pulse duration (6-20 ms, rectangular pulse shape), energy per pulse (10-33 J, rectangular pulse shape), pulse shape (three types of triangulars and one rectangular). Finally the evolution of surface temperature for pulses with more complex shapes but with the same pulse duration and energy per pulse is compared.     

Two-dimensional optical micro-scanner on silicon technology

A two-dimensional optical micro-scanner, which main components are two mobile flat and a concave micro-mirrors, is designed such that, all optical components can be fabricated on the same substratum. The optical parameters, which physical dimensions are between 50 and 500 μm, are obtained within the geometrical optics. The optical performance is evaluated by means of the MTF and Rayleigh resolution criteria, given 80% of modulation for a frequency of 8 cycles/mm with a Gaussian source, the resolution limit is 30 μm.     

Poly(3-methylthiophene)-based porous silicon substrates as a urea-sensitive electrode

Poly(3-methylthiophene) (P3MT)-based porous silicon (PS) substrates were fabricated and characterized by cyclic voltammetry, scanning electron microscopy, and auger electron spectroscopy. After doping urease (Urs) into the polymeric matrix, sensitivity and physicochemical properties of the P3MT-based PS substrate was investigated compared to planar silicon (PLS) and bulk Pt substrates. PS substrate was formed by electrochemical anodization in an etching solution composed of HF, H₂O, and ethanol. Subsequently, Ti and Pt thin-films were sputtered on the PS substrate. Effective working electrode area (A_eff) of the Pt-deposited PS substrate was determined from a redox reaction of Fe(CN)₆³⁻/Fe(CN)₆⁴⁻ redox couple in which nearly reversible cyclic voltammograms were obtained. The i_p versus v^1/2 plots showed that A_eff of the PS-based Pt thin-film electrode was 1.62 times larger than that of the PLS-based electrode.Electropolymerization of P3MT on both types of electrodes were carried out by the anodic potential scanning under the given potential range. And then, urease molecules were doped to the P3MT film by the chronoamperometry. Direct electrochemistry of a Urs/P3MT/Pt/Ti/PS electrode in an acetonitrile solution containing 0.1 mol/L NaClO₄ was introduced compared to a P3MT/Pt/Ti/PS electrode at scan rates of 10 mV s⁻¹, 50 mV s⁻¹, and 100 mV s⁻¹.Amperometric sensitivity of the Urs/P3MT/Pt/Ti/PS electrode was ca. 1.67 μA mM⁻¹ per projected unit square centimeter, and that of the Urs/P3MT/Pt/Ti/PLS electrode was ca. 1.02 μA mM⁻¹ per projected unit square centimeter in a linear range of 1-100 mM urea concentrations. 1.6 times of sensitivity increase was coincident with the results from cyclic voltammetrc analysis.Surface morphology from scanning electron microscopy (SEM) images of Pt-deposited PS electrodes before and after the coating of Urs-doped P3MT films showed that pore diameter and depth were 2 μm and 10 μm, respectively. Multilayered-film structures composed of metals and organics for both electrodes were also confirmed by auger electron spectroscopy (AES) depth profiles.     

In vitro corrosion behavior of Ti-O film deposited on fluoride-treated Mg-Zn-Y-Nd alloy

In this paper, a new composite coating was fabricated on magnesium alloy by a two-step approach, to improve the corrosion resistance and biocompatibility of Mg-Zn-Y-Nd alloy. First, fluoride conversion layer was synthesized on magnesium alloy surface by immersion treatment in hydrofluoric acid and then, Ti-O film was deposited on the preceding fluoride layer by magnetron sputtering. FE-SEM images revealed a smooth and uniform surface consisting of aggregated nano-particles with average size of 100 nm, and a total coating thickness of ∼1.5 μm, including an outer Ti-O film of ∼250 nm. The surface EDS and XRD data indicated that the composite coating was mainly composed of crystalline magnesium fluoride (MgF₂), and non-crystalline Ti-O. Potentiodynamic polarization tests revealed that the composite coated sample have a corrosion potential (E_corr) of −1.60 V and a corrosion current density (I_corr) of 0.17 μA/cm², which improved by 100 mV and reduced by two orders of magnitude, compared with the sample only coated by Ti-O. EIS results showed a polarization resistance of 3.98 kΩ cm² for the Ti-O coated sample and 0.42 kΩ cm² for the composite coated sample, giving an improvement of about 100 times. After 72 h immersion in SBF, widespread damage and deep corrosion holes were observed on the Ti-O coated sample surface, while the integrity of composite coating remained well after 7 d. In brief, the data suggested that single Ti-O film on degradable magnesium alloys was apt to become failure prematurely in corrosion environment. Ti-O film deposited on fluoride-treated magnesium alloys might potentially meet the requirements for future clinical magnesium alloy stent application.     

Optical reflectivity study of silicon ion implanted poly(methyl methacrylate)

The optical reflectivity (both specular and off-specular) of poly(methyl methacrylate) (PMMA) implanted with silicon ions (Si⁺) at energy of 50 keV, is studied in the spectral range 0.25-25 μm. The effect from the Si⁺ implantation on the reflectivity of two PMMA materials is examined in the dose range from 10¹⁴ to 10¹⁷ ions/cm² and is linked to the structure formed in this ion implanted plastic. As compared to the pristine PMMA, an enhancement of the reflectivity of Si⁺ implanted PMMA is observed, that is attributed to the modification of the subsurface region of PMMA upon the ion implantation. The ion-produced subsurface organic interface is also probed by laser-induced thermo-lens.     

Chemical etching to dissolve dislocation cores in multicrystalline silicon

Multicrystalline silicon wafers are used for approximately half of all solar cells produced at present. These wafers typically have dislocation densities of up to ∼10⁶ cm⁻². Dislocations and associated impurities act as strong recombination centres for electron–hole pairs and are one of the major limiting factors in multicrystalline silicon substrate performance. In this work we have explored the possibility of using chemical methods to etch out the cores of dislocations from mc-Si wafers. We aim to maximise the aspect ratio of the depth of the etched structure to its diameter. We first investigate the Secco etch (1K₂Cr₂O₇ (0.15 M): 2HF (49%)) as a function of time and temperature. This etch removes material from dislocation cores much faster than grain boundaries or the bulk, and produces tubular holes at dislocations. Aspect ratios of up to ∼7:1 are achieved for ∼15 μm deep tubes. The aspect ratio decreases with tube depth and for ∼40 μm deep tubes is just ∼2:1, which is not suitable for use in bulk multicrystalline silicon photovoltaics. We have also investigated a range of etches based on weaker oxidising agents. An etch comprising 1I₂ (0.01 M): 2HF (49%) attacked dislocation cores, but its etching behaviour was extremely slow (<0.1 μm/h) and the pits produced had a low aspect ratio (<2:1).