Resist-substrate interface tailoring for generating high density arrays of Ge and Bi2Se3 nanowires by electron beam lithography

The authors report a chemical process to remove the native oxide on Ge and Bi2Se3 crystals, thus facilitating high-resolution electron beam lithography (EBL) on their surfaces using a hydrogen silsesquioxane (HSQ) resist. HSQ offers the highest resolution of all the commercially available EBL resists. However, aqueous HSQ developers such as NaOH and tetramethylammonium hydroxide have thus far prevented the fabrication of high-resolution structures via the direct application of HSQ to Ge and Bi2Se3, due to the solubility of components of their respective native oxides in these strong aqueous bases. Here we provide a route to the generation of ordered, high-resolution, high-density Ge and Bi2Se3 nanostructures with potential applications in microelectronics, thermoelectric, and photonics devices.                         

Thermal expansion of the V(5)Si(3) and T(2) phases of the V-Si-B system investigated by high-temperature X-ray diffraction

The thermal expansion anisotropy of the V(5)Si(3) and T(2)-phase of the V-Si-B system were determined by high-temperature X-ray diffraction from 298 to 1273 K. Alloys with nominal compositions V(62.5)Si(37.5) (V5Si3 phase) and V(63)Si(12)B(25) (T(2)-phase) were prepared from high-purity materials through arc-melting followed by heat-treatment at 1873 K by 24 h, under argon atmosphere. The V(5)Si(3) phase exhibits thermal expansion anisotropy equals to 1.3, with thermal expansion coefficients along the a and c-axis equal to 9.3 x 10(-6) K(-1) and 11.7 x 10(-6) K(-1), respectively. Similarly, the thermal expansion anisotropy value of the T(2)-phase is 0.9 with thermal expansion coefficients equal to 8.8 x 10(-6) K(-1) and 8.3 x 10(-6) K(-1) along the, a and c-axis respectively. Compared to other isostructural silicides of the 5:3 type and the Ti(5)Si(3) phase, the V(5)Si(3) phase presents lower thermal expansion anisotropy. The T(2)-phase present in the V-Si-B system exhibits low thermal expansion anisotropy, as the T(2)-phase of the Mo-Si-B, Nb-Si-B and W-Si-B systems. (C) 2009 Elsevier Ltd. All rights reserved.

Effect of argon purity on mechanical properties, microstructure and fracture mode of commercially pure (cp) Ti and Ti-6Al-4V alloys for ceramometal dental prostheses

Provision of an inert gas atmosphere with high-purity argon gas is recommended for preventing titanium castings from contamination although the effects of the level of argon purity on the mechanical properties and the clinical performance of Ti castings have not yet been investigated. The purpose of this study was to evaluate the effect of argon purity on the mechanical properties and microstructure of commercially pure (cp) Ti and Ti-6Al-4V alloys. The castings were made using either high-purity and/or industrial argon gas. The ultimate tensile strength (UTS), proportional limit (PL), elongation (EL) and microhardness (VHN) at different depths were evaluated. The microstructure of the alloys was also revealed and the fracture mode was analyzed by scanning electron microscopy. The data from the mechanical tests and hardness were subjected to a two-and three-way ANOVA and Tukey`s test (alpha = 0.05). The mean values of mechanical properties were not affected by the argon gas purity. Higher UTS, PL and VHN, and lower EL were observed for Ti-6Al-4V. The microhardness was not influenced by the argon gas purity. The industrial argon gas can be used to cast cp Ti and Ti-6Al-4V.

Recuperação de 241Am de para-raios e detectores de fumaça

A method is described for recovering and purifying 241Am from lightning-conductors and smoke detectors. The method is based on the precipitation of silver, as AgCl, the main impurity, and extraction of americium with TBP. Further purification with ion-exchange resin is also used. The results have shown that by this method the americium is obtained with high purity.

Magnesium hydroxide-based peroxide bleaching of high-brightness mechanical pulps

A high final brightness is desired in most paper and board products. This requires bleaching processes that are able to produce high-brightness pulps. Mechanical pulps are widely bleached for high brightness using alkaline hydrogen peroxide with traditional sodium hydroxide and sodium silicate as additives. With high doses however, peroxide bleaching causes high organic loads in the mill effluent and anionic trash carry-over to papermaking. To alleviate the problems that arise from the use of sodium-based additives in peroxide bleaching, interest in the use of alternative magnesium-based chemicals has increased. In this study, a new, technical high-purity magnesium hydroxide-based bleaching additive was evaluated on laboratory-scale, pilot-scale and mill-scale experiments and trials for its ability to produce a high brightness in peroxide bleaching without the known problems of sodium-based chemicals. The key findings of this study include: a high brightening potential of peroxide bleaching using the Mg(OH)2-based additive, significant reductions (40-70%) in all categories of environmental load, and cationic demand lowered by 60-70% in bleached pulp with no loss in strength properties or in sheet bulk. When used in TMP refiner bleaching, the Mg(OH)2-based additive resulted in savings in specific energy consumption and provided a good bleaching response.

Hydrometallurgical recovery of valuable metals from secondary raw materials

Wastes and side streams in the mining industry and different anthropogenic wastes often contain valuable metals in such concentrations their recovery may be economically viable. These raw materials are collectively called secondary raw materials. The recovery of metals from these materials is also environmentally favorable, since many of the metals, for example heavy metals, are hazardous to the environment. This has been noticed in legislative bodies, and strict regulations for handling both mining and anthropogenic wastes have been developed, mainly in the last decade. In the mining and metallurgy industry, important secondary raw materials include, for example, steelmaking dusts (recoverable metals e.g. Zn and Mo), zinc plant residues (Ag, Au, Ga, Ge, In) and waste slurry from Bayer process alumina production (Ga, REE, Ti, V). From anthropogenic wastes, waste electrical and electronic equipment (WEEE), among them LCD screens and fluorescent lamps, are clearly the most important from a metals recovery point of view. Metals that are commonly recovered from WEEE include, for example, Ag, Au, Cu, Pd and Pt. In LCD screens indium, and in fluorescent lamps, REEs, are possible target metals. Hydrometallurgical processing routes are highly suitable for the treatment of complex and/or low grade raw materials, as secondary raw materials often are. These solid or liquid raw materials often contain large amounts of base metals, for example. Thus, in order to recover valuable metals, with small concentrations, highly selective separation methods, such as hydrometallurgical routes, are needed. In addition, hydrometallurgical processes are also seen as more environmental friendly, and they have lower energy consumption, when compared to pyrometallurgical processes. In this thesis, solvent extraction and ion exchange are the most important hydrometallurgical separation methods studied. Solvent extraction is a mainstream unit operation in the metallurgical industry for all kinds of metals, but for ion exchange, practical applications are not as widespread. However, ion exchange is known to be particularly suitable for dilute feed solutions and complex separation tasks, which makes it a viable option, especially for processing secondary raw materials. Recovering valuable metals was studied with five different raw materials, which included liquid and solid side streams from metallurgical industries and WEEE. Recovery of high purity (99.7%) In, from LCD screens, was achieved by leaching with H2SO4, extracting In and Sn to D2EHPA, and selectively stripping In to HCl. In was also concentrated in the solvent extraction stage from 44 mg/L to 6.5 g/L. Ge was recovered as a side product from two different base metal process liquors with Nmethylglucamine functional chelating ion exchange resin (IRA-743). Based on equilibrium and dynamic modeling, a mechanism for this moderately complex adsorption process was suggested. Eu and Y were leached with high yields (91 and 83%) by 2 M H2SO4 from a fluorescent lamp precipitate of waste treatment plant. The waste also contained significant amounts of other REEs such as Gd and Tb, but these were not leached with common mineral acids in ambient conditions. Zn was selectively leached over Fe from steelmaking dusts with a controlled acidic leaching method, in which the pH did not go below, but was held close as possible to, 3. Mo was also present in the other studied dust, and was leached with pure water more effectively than with the acidic methods. Good yield and selectivity in the solvent extraction of Zn was achieved by D2EHPA. However, Fe needs to be eliminated in advance, either by the controlled leaching method or, for example, by precipitation. 100% Pure Mo/Cr product was achieved with quaternary ammonium salt (Aliquat 336) directly from the water leachate, without pH adjustment (pH 13.7). A Mo/Cr mixture was also obtained from H2SO4 leachates with hydroxyoxime LIX 84-I and trioctylamine (TOA), but the purities were 70% at most. However with Aliquat 336, again an over 99% pure mixture was obtained. High selectivity for Mo over Cr was not achieved with any of the studied reagents. Ag-NaCl solution was purified from divalent impurity metals by aminomethylphosphonium functional Lewatit TP-260 ion exchange resin. A novel preconditioning method, named controlled partial neutralization, with conjugate bases of weak organic acids, was used to control the pH in the column to avoid capacity losses or precipitations. Counter-current SMB was shown to be a better process configuration than either batch column operation or the cross-current operation conventionally used in the metallurgical industry. The raw materials used in this thesis were also evaluated from an economic point of view, and the precipitate from a waste fluorescent lamp treatment process was clearly shown to be the most promising.

The CMS experiment at the CERN LHC

The Compact Muon Solenoid (CMS) detector is described. The detector operates at the Large Hadron Collider (LHC) at CERN. It was conceived to study proton-proton (and lead-lead) collisions at a centre-of-mass energy of 14 TeV (5.5 TeV nucleon-nucleon) and at luminosities up to 10(34)cm(-2)s(-1) (10(27)cm(-2)s(-1)). At the core of the CMS detector sits a high-magnetic-field and large-bore superconducting solenoid surrounding an all-silicon pixel and strip tracker, a lead-tungstate scintillating-crystals electromagnetic calorimeter, and a brass-scintillator sampling hadron calorimeter. The iron yoke of the flux-return is instrumented with four stations of muon detectors covering most of the 4 pi solid angle. Forward sampling calorimeters extend the pseudo-rapidity coverage to high values (vertical bar eta vertical bar <= 5) assuring very good hermeticity. The overall dimensions of the CMS detector are a length of 21.6 m, a diameter of 14.6 m and a total weight of 12500 t.

On Ti-18Si-6B and Ti-7.5Si-22.5B powder alloys prepared by high-energy ball milling and sintering

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Crystallographic structure of Ti-6Al-4V, Ti-HP and Ti-CP under high-pressure

The phase stability of a commercial purity (Ti-CP), high purity (Ti-HP) and Ti-6Al-4V alloy were investigated in a diamond anvil cell up to 32 GPa and 298 K using a polychromatic X-ray beam. The Ti-CP and Ti-HP shown the same HCP (c/a∼0.632) to Hexagonal (c/a∼1.63) non reversible martensitic transition at about 9 GPa. The as received Ti-6Al-4V shows a very low relative volume fraction β-Ti / α-Ti. No phase changes were observed in the Ti-6Al-4V alloy in the pressure range of this study. The α phase of the Ti-6Al-4V shows monotonic volume cell pressure dependence. This volume change is reversible and non-hysteretic. The cell of the a phase recovered its original volume when the pressure was released. © 2010 IOP Publishing Ltd.

Identification of b-quark jets with the CMS experiment

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

On Ti-18Si-6B and Ti-7.5Si-22.5B powder alloys prepared by high-energy ball milling and sintering

Recently, a new ternary phase was discovered in the Ti-Si-B system, located near the Ti6Si2B composition. The present study concerns the preparation of titanium alloys that contain such phase mixed with α-titanium and other intermetallic phases. High-purity powders were initially processed in a planetary ball-mill under argon atmosphere with Ti-18Si-6B and Ti-7.5Si-22.5B at. (%) initial compositions. Variation of parameters such as rotary speed, time, and ball diameters were adopted. The as-milled powders were pressureless sintered and hot pressed. Both the as-milled and sintered materials were characterized by X-ray diffraction, scanning electron microscopy and energy-dispersive spectrometry. Sintered samples have presented equilibrium structures formed mainly by the α-Ti+Ti6Si2B+Ti5Si3+TiB phases. Silicon and boron peaks disappear throughout the milling processes, as observed in the powder diffraction data. Furthermore, an iron contamination of up to 10 at. (%) is measured by X-ray spectroscopy analysis on some regions of the sintered samples. Density, hardness and tribological results for these two compositions are also presented here.

Applications of High Speed Configurable Logic Devices in Modern Particle Physics Experiments

Several activities were conducted during my PhD activity. For the NEMO experiment a collaboration between the INFN/University groups of Catania and Bologna led to the development and production of a mixed signal acquisition board for the Nemo Km3 telescope. The research concerned the feasibility study for a different acquisition technique quite far from that adopted in the NEMO Phase 1 telescope. The DAQ board that we realized exploits the LIRA06 front-end chip for the analog acquisition of anodic an dynodic sources of a PMT (Photo-Multiplier Tube). The low-power analog acquisition allows to sample contemporaneously multiple channels of the PMT at different gain factors in order to increase the signal response linearity over a wider dynamic range. Also the auto triggering and self-event-classification features help to improve the acquisition performance and the knowledge on the neutrino event. A fully functional interface towards the first level data concentrator, the Floor Control Module, has been integrated as well on the board, and a specific firmware has been realized to comply with the present communication protocols. This stage of the project foresees the use of an FPGA, a high speed configurable device, to provide the board with a flexible digital logic control core. After the validation of the whole front-end architecture this feature would be probably integrated in a common mixed-signal ASIC (Application Specific Integrated Circuit). The volatile nature of the configuration memory of the FPGA implied the integration of a flash ISP (In System Programming) memory and a smart architecture for a safe remote reconfiguration of it. All the integrated features of the board have been tested. At the Catania laboratory the behavior of the LIRA chip has been investigated in the digital environment of the DAQ board and we succeeded in driving the acquisition with the FPGA. The PMT pulses generated with an arbitrary waveform generator were correctly triggered and acquired by the analog chip, and successively they were digitized by the on board ADC under the supervision of the FPGA. For the communication towards the data concentrator a test bench has been realized in Bologna where, thanks to a lending of the Roma University and INFN, a full readout chain equivalent to that present in the NEMO phase-1 was installed. These tests showed a good behavior of the digital electronic that was able to receive and to execute command imparted by the PC console and to answer back with a reply. The remotely configurable logic behaved well too and demonstrated, at least in principle, the validity of this technique. A new prototype board is now under development at the Catania laboratory as an evolution of the one described above. This board is going to be deployed within the NEMO Phase-2 tower in one of its floors dedicated to new front-end proposals. This board will integrate a new analog acquisition chip called SAS (Smart Auto-triggering Sampler) introducing thus a new analog front-end but inheriting most of the digital logic present in the current DAQ board discussed in this thesis. For what concern the activity on high-resolution vertex detectors, I worked within the SLIM5 collaboration for the characterization of a MAPS (Monolithic Active Pixel Sensor) device called APSEL-4D. The mentioned chip is a matrix of 4096 active pixel sensors with deep N-well implantations meant for charge collection and to shield the analog electronics from digital noise. The chip integrates the full-custom sensors matrix and the sparsifification/readout logic realized with standard-cells in STM CMOS technology 130 nm. For the chip characterization a test-beam has been set up on the 12 GeV PS (Proton Synchrotron) line facility at CERN of Geneva (CH). The collaboration prepared a silicon strip telescope and a DAQ system (hardware and software) for data acquisition and control of the telescope that allowed to store about 90 million events in 7 equivalent days of live-time of the beam. My activities concerned basically the realization of a firmware interface towards and from the MAPS chip in order to integrate it on the general DAQ system. Thereafter I worked on the DAQ software to implement on it a proper Slow Control interface of the APSEL4D. Several APSEL4D chips with different thinning have been tested during the test beam. Those with 100 and 300 um presented an overall efficiency of about 90% imparting a threshold of 450 electrons. The test-beam allowed to estimate also the resolution of the pixel sensor providing good results consistent with the pitch/sqrt(12) formula. The MAPS intrinsic resolution has been extracted from the width of the residual plot taking into account the multiple scattering effect.

Fabrication of high quality optical coherence tomography (OCT) calibration artefacts using femtosecond inscription

Optical coherence tomography (OCT) is a non-invasive three-dimensional imaging system that is capable of producing high resolution in-vivo images. OCT is approved for use in clinical trials in Japan, USA and Europe. For OCT to be used effectively in a clinical diagnosis, a method of standardisation is required to assess the performance across different systems. This standardisation can be implemented using highly accurate and reproducible artefacts for calibration at both installation and throughout the lifetime of a system. Femtosecond lasers can write highly reproducible and highly localised micro-structured calibration artefacts within a transparent media. We report on the fabrication of high quality OCT calibration artefacts in fused silica using a femtosecond laser. The calibration artefacts were written in fused silica due to its high purity and ability to withstand high energy femtosecond pulses. An Amplitude Systemes s-Pulse Yb:YAG femtosecond laser with an operating wavelength of 1026 nm was used to inscribe three dimensional patterns within the highly optically transmissive substrate. Four unique artefacts have been designed to measure a wide variety of parameters, including the points spread function (PSF), modulation transfer function (MTF), sensitivity, distortion and resolution - key parameters which define the performance of the OCT. The calibration artefacts have been characterised using an optical microscope and tested on a swept source OCT. The results demonstrate that the femtosecond laser inscribed artefacts have the potential of quantitatively and qualitatively validating the performance of any OCT system.

X-Ray Diffraction Study of Boron Produced by Pyrolysis of Boron Tribromide

The goal of this research was to determine the composition of boron deposits produced by pyrolysis of boron tribromide, and to use the results to (a) determine the experimental conditions (reaction temperature, etc.) necessary to produce alpha-rhombohedral boron and (b) guide the development/refinement of the pyrolysis experiments such that large, high purity crystals of alpha-rhombohedral boron can be produced with consistency. Developing a method for producing large, high purity alpha-rhombohedral boron crystals is of interest because such crystals could potentially be used to achieve an alpha-rhombohedral boron based neutron detector design (a solid-state detector) that could serve as an alternative to existing neutron detector technologies. The supply of neutron detectors in the United States has been hampered for a number of years due to the current shortage of helium-3 (a gas used in many existing neutron detector technologies); the development of alternative neutron detector technology such as an alpha-rhombohedral boron based detector would help provide a more sustainable supply of neutron detectors in this country. In addition, the prospect/concept of an alpha-rhombohedral boron based neutron detector is attractive because it offers the possibility of achieving a design that is smaller, longer life, less power consuming, and potentially more sensitive than existing neutron detectors. The main difficulty associated with creating an alpha-rhombohedral boron based neutron detector is that producing large, high purity crystals of alpha-rhombohedral boron is extremely challenging. Past researchers have successfully made alpha-rhombohedral boron via a number of methods, but no one has developed a method for consistently producing large, high purity crystals. Alpha-rhombohedral boron is difficult to make because it is only stable at temperatures below around 1100-1200 °C, its formation is very sensitive to impurities, and the conditions necessary for its formation are not fully understood or agreed upon in the literature. In this research, the method of pyrolysis of boron tribromide (hydrogen reduction of boron tribromide) was used to deposit boron on a tantalum filament. The goal was to refine this method, or potentially use it in combination with a second method (amorphous boron crystallization), to the point where it is possible to grow large, high purity alpha-rhombohedral boron crystals with consistency. A pyrolysis apparatus was designed and built, and a number of trials were run to determine the conditions (reaction temperature, etc.) necessary for alpha-rhombohedral boron production. This work was focused on the x-ray diffraction analysis of the boron deposits; x-ray diffraction was performed on a number of samples to determine the types of boron (and other compounds) formed in each trial and to guide the choices of test conditions for subsequent trials. It was found that at low reaction temperatures (in the range of around 830-950 °C), amorphous boron was the primary form of boron produced. Reaction temperatures in the range of around 950-1000 °C yielded various combinations of crystalline boron and amorphous boron. In the first trial performed at a temperature of 950 °C, a mix of amorphous boron and alpha-rhombohedral boron was formed. Using a scanning electron microscope, it was possible to see small alpha-rhombohedral boron crystals (on the order of ~1 micron in size) embedded in the surface of the deposit. In subsequent trials carried out at reaction temperatures in the range of 950 °C – 1000 °C, it was found that various combinations of alpha-rhombohedral boron, beta-rhombohedral boron, and amorphous boron were produced; the results tended to be unpredictable (alpha-rhombohedral boron was not produced in every trial), and the factors leading to success/failure were difficult to pinpoint. These results illustrate how sensitive of a process producing alpha-rhombohedral boron can be, and indicate that further improvements to the test apparatus and test conditions (for example, higher purity/cleanliness) may be necessary to optimize the boron deposition. Although alpha-rhombohedral boron crystals of large size were not achieved, this research was successful in (a) developing a pyrolysis apparatus and test procedure that can serve as a platform for future testing, (b) determining reaction temperatures at which alpha-rhombohedral boron can form, and (c) developing a consistent process for analyzing the boron deposits and determining their composition. Further experimentation is necessary to achieve a pyrolysis apparatus and test procedure that can yield large alpha-rhombohedral boron crystals with consistency.

Limitations of high pressure sputtering for amorphous silicon deposition

Amorphous silicon thin films were deposited using the high pressure sputtering (HPS) technique to study the influence of deposition parameters on film composition, presence of impurities, atomic bonding characteristics and optical properties. An optical emission spectroscopy (OES) system has been used to identify the different species present in the plasma in order to obtain appropriate conditions to deposit high purity films. Composition measurements in agreement with the OES information showed impurities which critically depend on the deposition rate and on the gas pressure. We prove that films deposited at the highest RF power and 3.4 × 10^−2 mbar, exhibit properties as good as the ones of the films deposited by other more standard techniques.