Mechano-chemical AFM nanolithography of metallic thin films: A statistical analysis

A mechano-chemical atomic force microscope (AFM) nanolithography on a metallic thin film (50 nm in thickness) covered by a spin-coated soft polymeric mask layer (50–60 nm in thickness) has been introduced. The surface stochastic properties of initial grooves mechanically patterned on the mask layer (grooves before chemical wet-etching) and the lithographed patterns on the metallic thin film (the grooves after chemical wet-etching) have been investigated and compared by using the structure factor, power spectral density, and AFM tip deconvolution analyses. The effective shape of cross section of the before and after etching grooves have been determined by using the tip deconvolution surface analysis. The wet-etching process improved the shape of the grooves and also smoothed the surface within them. We have indicated that relaxation of the surface tension of the deposited mask layer after the AFM scribing is independent from surface density of the grooves and also their length scale. Based on the statistical analysis, it was found that increase of the width of the grooves after the wet-etching and also relaxation of surface tension of the mask layer resulted in a down limit in the size of the metallic nanowires made by the combined nanolithography method. An extrapolation of the analyzed statistical data has indicated that, in this method, the minimum obtainable width and length of the metallic nanowires are about 55 nm and 2 μm, respectively.     

Evolution of surface morphology of NiO thin films under swift heavy ion irradiation

NiO nanoparticle thin films grown on Si substrates were irradiated by 107 MeV Ag⁸⁺ ions. The films were characterized by glancing angle X-ray diffraction and atomic force microscopy. Ag ion irradiation was found to influence the shape and size of the nanoparticles. The pristine NiO film consisted of uniform size (∼100 nm along major axis and ∼55 nm along minor axis) elliptical particles, which changed to also of uniform size (∼63 nm) circular shape particles on irradiation at a fluence of 3 × 10¹³ ions cm⁻². Comparison of XRD line width analysis and AFM data revealed that the particles in the pristine films are single crystalline, which turn to polycrystalline on irradiation with 107 MeV Ag ions.     

Patterning of indium-tin oxide on glass with picosecond lasers

The results of patterning of the indium-tin oxide (ITO) film on the glass substrate with high repetition rate picosecond lasers at various wavelengths are presented. Laser radiation initiated the ablation of the material, forming grooves in ITO. Profile of the grooves was analyzed with a phase contrast optical microscope, a stylus type profiler, scanning electron microscope (SEM) and atomic force microscope (AFM). Clean removal of the ITO film was achieved with the 266 nm radiation when laser fluence was above the threshold at 0.20 J/cm², while for the 355 nm radiation, the threshold was higher, above 0.46 J/cm². The glass substrate was damaged in the area where the fluence was higher than 1.55 J/cm². The 532 nm radiation allowed getting well defined grooves, but a lot of residues in the form of dust were generated on the surface. UV radiation with the 266 nm wavelength provided the widest working window for ITO ablation without damage of the substrate. Use of UV laser radiation with fluences close to the ablation threshold made it possible to minimize surface contamination and the recast ridge formation during the process.     

Pulsed Nd:YAG laser depositions of ITO and DLC films for OLED applications

Indium-tin oxide (ITO) films deposited on heated and non-heated glass substrates by a pulsed Nd:YAG laser at 355 nm and ∼2.5 J/cm² were used in the fabrication of simple organic light-emitting diodes (OLEDs), ITO/(PVK + Alq₃ + TPD)/Al. The ITO was deposited on heated glass substrates which possessed resistivity as low as ∼3 × 10⁻⁴ Ω cm, optical transmission as high as ∼92% and carrier concentration of about ∼5 × 10²⁰ cm⁻³, were comparable to the commercial ITO. Substrate heating transformed the ITO microstructure from amorphous to polycrystalline, as revealed by the XRD spectrum. While the polycrystalline ITO produced higher OLED brightness, it was still lower than that on the commercial ITO due to surface roughness. A DLC layer of ∼1.5 nm deposited on this ITO at laser fluence of >12.5 J/cm² improved its device brightness by suppressing the surface roughness effect.     

A study of fused silica micro/nano patterning by focused-ion-beam

A dual-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system was used to pattern fused silica substrates coated with a 15 nm thin Cr layer. The dimensions of fabricated features together with their surface morphology and profiles were investigated by SEM and atomic force microscopy (AFM). The study demonstrated that with the increase of the ion beam fluence the sputtering rate of the fused silica decreased non-linearly. Also, it was found that initially the sputtering rate increased with the increase of the beam current, after reaching a maximum value, it started decreasing when further beam current increment was performed. Compared with unprocessed areas, the surface finish of the features fabricated by FIB exhibited a significant improvement, and the ion fluence influence on the surface roughness of trenches with low aspect ratios could be considered as negligible. Using a fine beam probe, nano-gratings in the form of grooves with a width down to 54 nm and an aspect ratio higher than three were fabricated. The study showed that FIB machining could be an alternative technology to e-beam lithography for producing fused silica templates for UV nanoimprinting.     

Ordered nano-scale domains in lithium niobate single crystals via phase-mask assisted all-optical poling

We report the formation of directionally ordered nano-scale surface domains on the +z face of undoped congruent lithium niobate single crystals by using UV illumination through a phase mask of sub-micron periodicity with an energy fluence between ∼90 mJ/cm² and 150 mJ/cm² at λ = 266 nm. We clearly show here that the UV-induced surface ferroelectric domains only nucleate at and propagate along maxima of laser intensity. Although the domain line separation varies and is greater than 2 μm for this set of experimental conditions, this enables a degree of control over the all-optical poling process.     

The effect of post-annealing on surface acoustic wave devices based on ZnO thin films prepared by magnetron sputtering

Zinc oxide (ZnO) thin films were deposited on unheated silicon substrates via radio frequency (RF) magnetron sputtering, and the post-deposition annealing of the ZnO thin films was performed at 400 °C, 600 °C, 800 °C, and 1000 °C. The characteristics of the thin films were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The films were then used to fabricate surface acoustic wave (SAW) resonators. The effects of post-annealing on the SAW devices are discussed in this work. Resulting in the 600 °C is determined as optimal annealing temperature for SAW devices. At 400 °C, the microvoids exit between the grains yield large root mean square (RMS) surface roughness and higher insertion losses in SAW devices. The highest RMS surface roughness, crack and residual stress cause a reduction of surface velocity (about 40 m/s) and increase dramatically insertion loss at 1000 °C. The SAW devices response becomes very weak at this temperature, the electromechanical coupling coefficient (k²) of ZnO film decrease from 3.8% at 600 °C to 1.49% at 1000 °C.     

Impact of laser produced X-rays on the surface of gold

In the paper an attempt has been made to use the laser-induced plasma as an X-ray source for the growth of nanostructures on the surface of gold. For this purpose, an Nd:YAG laser operated at second harmonics (λ = 532 nm, E = 400 mJ) is used to produce plasma from analytical grade 5N pure Al, Cu and W targets. An analytical grade (5N pure) gold substrate was irradiated by X-rays generated from Al, Cu and W plasma under the vacuum ∼10⁻⁴ Torr. The surface was analyzed by two techniques, XRD and AFM. The aberrations in the XRD peaks show that there are significant structural changes in the exposed gold, in terms of decreased reflection intensities, increased dislocation line density, changes in the d-spacing and disturbance in the periodicity of the planes. AFM used to explore the topography of the irradiated gold reveals that regardless of the source, nm sized hillocks have been produced on the gold surface. The roughness of the surface has increased due to the growth of these hillocks.     

Extended X-ray absorption fine structure (EXAFS) and X-ray absorption near-edge structure (XANES) study of melt-spun Fe85Ga15 ribbons

The local structure in melt-spun Fe₈₅Ga₁₅ ribbons with a width ∼3 mm and thickness ∼60 μm produced in argon atmosphere was studied by analyzing EXAFS and XANES data. The following results were obtained: Ga–Ga bonds were not detected excluding the tendency to form clusters of Ga atoms; Ga substitutes Fe creating a local strain of about +1% on the first shell Fe–Ga bond, whereas on the second Fe–Ga shell strain quickly relaxes down to +0.3%; XANES spectra are compatible with a random substitution of Fe atoms by Ga atoms in the A2 structure. From the AFM investigation, we observed that at the surface (free side) of the ribbon the particles are elongated along the ribbon (∼2 μm×∼5 μm) and each particle is formed by small grains of average size of 200 nm.     

Surface modification of silicate glasses by nanoimprint using nanostriped NiO thin film molds

Nanoscale surface modification of silicate glasses was examined by applying nanoimprint technique using a nanostriped NiO thin film mold. The mold had the pattern composed of regularly arranged straight nanogrooves, which was formed by high-temperature annealing of the Li-doped NiO epitaxial thin film deposited on the atomically stepped sapphire (α-Al₂O₃ single crystal) substrate. The glass imprint was proceeded through the simple steps of heating (∼600 °C), pressing (∼1 kPa) and then cooling in air. The nanoimprinted glass surface transferred reversely from the mold exhibited the multi nanowire array having an interval of ∼80 nm, wire width of ∼70 nm, and wire height of ∼20 nm.     

A novel optimal sensitivity design scheme for yarn tension sensor using surface acoustic wave device

In this paper, we propose a novel optimal sensitivity design scheme for the yarn tension sensor using surface acoustic wave (SAW) device. In order to obtain the best sensitivity, the regression model between the size of the SAW yarn tension sensor substrate and the sensitivity of the SAW yarn tension sensor was established using the least square method. The model was validated too. Through analyzing the correspondence between the regression function monotonicity and its partial derivative sign, the effect of the SAW yarn tension sensor substrate size on the sensitivity of the SAW yarn tension sensor was investigated. Based on the regression model, a linear programming model was established to gain the optimal sensitivity of the SAW yarn tension sensor. The linear programming result shows that the maximum sensitivity will be achieved when the SAW yarn tension sensor substrate length is equal to 15 mm and its width is equal to 3 mm within a fixed interval of the substrate size. An experiment of SAW yarn tension sensor about 15 mm long and 3 mm wide was presented. Experimental results show that the maximum sensitivity 1982.39 Hz/g was accomplished, which confirms that the optimal sensitivity design scheme is useful and effective.     

Reactive ion etching of FePt using inductively coupled plasma

We propose a reactive ion etching (RIE) process of an L1₀-FePt film which is expected as one of the promising materials for the perpendicular magnetic recording media. The etching was carried out using an inductively coupled plasma (ICP) RIE system and an etching gas combination of CH₄/O₂/NH₃ was employed. The L1₀-FePt films were deposited on (1 0 0)-oriented MgO substrates using a magnetron sputtering system. The etching masks of Ti were patterned on the FePt films lithographically. The etch rates of ∼16 and ∼0 nm/min were obtained for the FePt film and the Ti mask, respectively. The atomic force microscopy (AFM) analyses provided the average roughness (R_a) value of 0.95 nm for the etched FePt surface, that is, a very flat etched surface was obtained. Those results show that the highly selective RIE process of L1₀-FePt was successfully realized in the present study.     

Preparation of dielectric mirrors from high-refractive index contrast amorphous chalcogenide films

We report the preparation of planar 15-layer dielectric mirrors by a thermal evaporation of alternating high refractive index contrast amorphous chalcogenide Sb-Se and Ge-S layers, exhibiting a high-reflection band around 1.55 μm. The layer deposition quality and the thickness accuracy of such prepared chalcogenide multilayers were then checked using transmission electron microscopy. The layer thickness deviation of chalcogenide layers did not exceed ∼7 nm in comparison with the desired thicknesses. The width of Sb-Se/Ge-S layer boundary was approximately ∼3 nm, which is in good agreement with the surface roughness values of thermally evaporated Sb-Se and Ge-S single layers. The optical properties of the prepared 15-layer dielectric mirrors were consistent in temperature range of 20-120 °C; however, at higher temperatures there started apparent structural changes of Sb-Se films, which were followed by their crystallization. Excellent optical properties of chalcogenide materials in the infrared range make them interesting for applications, e.g., in optics and photonics.     

The influence of growth parameters on the optical properties and morphology of UHV deposited Ni thin films

Nickel films of different thickness ranging from 15 nm to 350 nm were deposited on glass substrates, at different substrate temperatures (313-600 K) under UHV condition. The nano-structure of the films was obtained, using X-ray diffraction (XRD) and atomic force microscopy (AFM). The nano-strain in these films was obtained using the Warren-Averbach method. Their optical properties were measured by spectrophotometry in the spectral range of 190-2500 nm. Kramers-Kronig method was used for the analysis of the reflectivity curves. The absorption peaks of Ni thin films at ∼1.4 eV (transition between the bands near W and K symmetry points) and ∼5.0 eV (transition from L_2^′ to L₁ upper) are observed, with an additional bump at about 2 eV. The over-layer thickness was calculated to be less than 3.0 nm, using the Transfer Matrix method. The changes in optical data are related to different phenomena, such as different crystallographic orientations of the grains in these polycrystalline films (film texture), nano-strain, and film surface roughness.     

X-ray and AFM studies of polydisperse TiO2 (anatase) particles

Titanium dioxide (TiO₂) materials of a high chemical purity, as-prepared by the thermal hydrolysis, as well as subsequently modified by adsorption of different metal cations (Fe³⁺, Co²⁺, Cu²⁺), have been investigated by the X-ray diffraction, X-ray fluorescence and AFM microscopy methods. All TiO₂ powders have a fine-dispersated anatase structure and consist of grown together nanocrystallites of ∼8-17 nm. TiO₂ particles, usually ranging from 100 to 600 nm, show the ability to form large agglomerates, up to 2 μm in size. Contrary to the pure anatase, metal-modified TiO₂ particles possess a positive charge on their surface and can be lifted away by the AFM tip from the substrate surface during the scanning. This effect is mostly pronounced for the Fe-modified TiO₂ sample, where particles up to 250 nm are removed. The possible interaction mechanisms between different TiO₂ particles and the silicon tip are discussed. The electrostatic force has been found to play an essential role in the sample-tip interaction processes, and its value depends on the type of metal cation used.     

Formation of gold nanoparticles in heat-treated reactive co-sputtered Au-SiO2 thin films

In this work, formation of gold nanoparticles in radio frequency (RF) reactive magnetron co-sputtered Au-SiO₂ thin films post annealed at different temperatures in Ar + H₂ atmosphere has been investigated. Optical, surface topography, chemical state and crystalline properties of the prepared films were analyzed by using UV-visible spectrophotometry, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD) techniques, respectively. Optical absorption spectrum of the Au-SiO₂ thin films annealed at 800 °C showed one surface plasmon resonance (SPR) absorption peak located at 520 nm relating to gold nanoparticles. According to XPS analysis, it was found that the gold nanoparticles had a tendency to accumulate on surface of the heat-treated films in the metallic state. AFM images showed that the nanoparticles were uniformly distributed on the film surface with grain size of about 30 nm. Using XRD analysis average crystalline size of the Au particles was estimated to about 20 nm.     

InSb quantum dots and quantum rings on InAs-rich surface

We report a study of InSb nanoobjects (quantum dots and quantum rings) grown on InAs-rich surface by liquid phase epitaxy. Characterization of the sample surface was performed using atomic force microscopy (AFM). The bimodal formation of the uncapped InSb quantum dots (QDs) was observed for the growing on a binary InAs substrate. Uniform high-density (1 × 10¹⁰ cm⁻²) quantum dots with a height of 3 nm were obtained at T = 420-430 °C, whereas low-density (5 × 10⁸ cm⁻²) big quantum dots were 9 nm in height. As a buffer layer, lattice-matched InAsSb_0.12P_0.25 solid solution was deposed on InAs substrate using metal-organic vapour phase epitaxy. Deposition from the InSb melt on the buffer layer resulted in the formation of InSb nanoobjects with density as high as 3 × 10¹⁰ cm⁻².     

Interfacial analysis of InP surface preparation using atomic hydrogen cleaning and Si interfacial control layers prior to MgO deposition

The objective of this study is to investigate how the surface characteristics of indium phosphide (InP) can be modified through the use of atomic hydrogen (H^*) cleaning and silicon interfacial control layers (Si ICL), prior to the deposition of MgO dielectric layers. X-ray photoelectron spectroscopy (XPS) analysis shows that the InP native oxide can be successfully removed using atomic hydrogen cleaning at a substrate temperature of 300 °C. However, atomic force microscopy (AFM) images display evidence for the growth of metallic In island features after H^* cleaning, and subsequent deposition of MgO thin films on the H^* cleaned surface resulted in high levels of interfacial indium oxide growth. It has also been shown that the deposition of thin (∼1 nm) Si layers on InP native oxide surfaces results in the transfer of oxygen from the InP substrate to the Si ICL and the formation of Si-InP bonds. XPS analysis indicates that MgO deposition and subsequent 500 °C annealing results in further oxidation of the Si layer. However, no evidence for the re-growth of interfacial In or P oxide species was observed, in contrast to observations on the H^* cleaned surface.     

Dual N/Pb ion-implanted Si: Temperature dependence of the novel shift of the Pb peak under electron beam annealing

(1 0 0) Si was dual ion-implanted with 24 keV N and 7 keV Pb to peak concentrations ∼10 at.%. Implanted samples were then electron beam annealed (EBA) at a peak temperature T for 30 s with T ranging from 100 °C to 900 °C and for 15 s at 1000 °C. Pb profiles were measured using RBS and surfaces characterised by AFM. For T up to 500 °C there was no shift in the profile from the implanted depth ∼10 nm. For higher values of T a striking feature was the large movement of the Pb profile away from the surface without a significant change in width or Pb content. The profile depths were: ∼40 nm for 600 °C, ∼68 nm for 700-900 °C and ∼80 nm for 1000 °C. The response to EBA was found to be strongly dependent on both ion implantation order and Si starting structure. For (1 0 0) Si nanowhiskers formed on the treated surfaces for T = 900 °C and 1000 °C. A model is developed based on the restructuring of the amorphous implanted layer under EBA. It is proposed that a compaction starting at the surface sweeps the Pb before it via a stress interaction as it advances into the Si.     

Vacuum-deposited wave-guiding layers on STW resonators based on LiTaO3 substrate as love wave sensors for chemical and biochemical sensing in liquids

A promising approach to apply the Love wave concept to commercially available low-loss surface acoustic wave (SAW) devices of the type Murata SAF 380 is presented. Thin wave-guiding layers of variable thickness are coated on the piezoelectric substrate of the devices. Two different layer materials were used: sputtered SiO₂ and a new polymer in this field, parylene C (poly-[2-chloro-p-xylylene]). Insertion loss, resonance frequency, frequency changes during protein precipitation and noise of the devices are discussed as a function of the thickness of the wave-guiding layer. It is demonstrated that the application of an optimized wave-guiding layer increases the sensitivity. When using SiO₂ as wave-guiding layer, an optimum layer thickness of 4 μm leads to a detection limit of 1.7 pg/mm². Therefore, the detection limit is improved by factor 7.7 as compared to uncoated SAW devices. Parylene-coated devices reach a detection limit of 2.9 pg/mm² at an optimum layer thickness of 0.5 μm. This corresponds to an improvement by factor 4.3. As the SAW devices used in this study are commercially available at low costs, applying appropriate wave-guiding layers permits an application as chemical or biochemical sensors with excellent sensitivities. Moreover, parylene-coated devices combine the sensitivity increase by excitation of Love waves with an excellent protective effect against corrosive attacks by the surrounding medium. Therefore, these sensors are most suitable for biosensing in conducting buffer solutions.