The boundary lubricated friction and wear of low alloy steel

Pin on disc wear machines were used to study the boundary lubricated friction and wear of AISI 52100 steel sliding partners. Boundary conditions were obtained by using speed and load combinations which resulted in friction coefficients in excess of 0.1. Lubrication was achieved using zero, 15 and 1000 ppm concentrations of an organic dimeric acid additive in a hydrocarbon base stock. Experiments were performed for sliding speeds of 0.2, 0.35 and 0.5 m/s for a range of loads up to 220 N. Wear rate, frictional force and pin temperature were continually monitored throughout tests and where possible complementary methods of measurement were used to improve accuracy. A number of analytical techniques were used to examine wear surfaces, debris and lubricants, namely: Scanning Electron Microscopy (SEM), Auger Electron Spectroscopy (AES), Powder X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), optical microscopy, Back scattered Electron Detection (BSED) and several metallographic techniques. Friction forces and wear rates were found to vary linearly with load for any given combination of speed and additive concentration. The additive itself was found to act as a surface oxidation inhibitor and as a lubricity enhancer, particularly in the case of the higher (1000 ppm) concentration. Wear was found to be due to a mild oxidational mechanism at low additive concentrations and a more severe metallic mechanism at higher concentrations with evidence of metallic delamination in the latter case. Scuffing loads were found to increase with increasing additive concentration and decrease with increasing speed as would be predicted by classical models of additive behaviour as an organo-metallic soap film. Heat flow considerations tended to suggest that surface temperature was not the overriding controlling factor in oxidational wear and a model is proposed which suggests oxygen concentration in the lubricant is the controlling factor in oxide growth and wear.

Mild wear in dry and lubricated sliding systems

A vertical pin on horizontal disc machine has been used to conduct a series of experiments in air under dry and lubricating sliding conditions. For dry sliding low load and speed combinations were chosen to correspond to the mild wear region below the Welsh T1 transition. Lubricated tests were conducted under flooded conditions using Esso Technical White Oil alone and with a 0.1% stearic acid additive, for load and speed ranges that produced substantial amounts of asperity contact and thus a boundary lubricated regime of wear. The test material in all cases was AISI 52100 steel, for unlubricated sliding subjected to loads from 5 to 50 N and a range of speeds from 10-3 to 1.0 ms-1, and for lubricated sliding loads of 50 to 123 N and for speeds of 10-2 to 1.0 ms-1. Unlubricated wear debris was found to be a mixture of -Fe_2O_3 and -Fe. Unlubricated wear was found to occur via a thin film logarithmic oxide growth followed by agglomeration into thicker oxide plateaux 2 to 10 m in thickness. Lubricated wear occurred via thick film diffusion controlled oxide growth producing homogeneous oxide plateaux 0.1 to 0.2 m in thickness. X-ray photoelectron spectroscopy identified the presence of a surface film on pins worn in White Oil with stearic acid, which is thought to be iron stearate. A model has been developed for unlubricated wear based upon the postulated growth of thin film oxides by a logarithmic rate law. The importance of sliding geometry and environment to the dominant wear mechanism has been illustrated.

Nitrogen implantation of tool steels and engineering coatings

Ion implantation modifies the surface composition and properties of materials by bombardment with high energy ions. The low temperature of the process ensures the avoidance of distortion and degradation of the surface or bulk mechanical properties of components. In the present work nitrogen ion implantation at 90 keV and doses above 1017 ions/cm2 has been carried out on AISI M2, D2 and 420 steels and engineering coatings such as hard chromium, electroless Ni-P and a brush plated Co-W alloy. Evaluation of wear and frictional properties of these materials was performed with a lubricated Falex wear test at high loads up to 900 N and a dry pin-on-disc apparatus at loads up to 40 N. It was found that nitrogen implantation reduced the wear of AISI 420 stainless steel by a factor of 2.5 under high load lubricated conditions and by a factor of 5.5 in low load dry testing. Lower but significant reductions in wear were achieved for AISI M2 and D2 steels. Wear resistance of coating materials was improved by up to 4 times in lubricated wear of hard Cr coatings implanted at the optimum dose but lower improvements were obtained for the Co-W alloy coating. However, hardened electroless Ni-P coatings showed no enhancement in wear properties. The benefits obtained in wear behaviour for the above materials were generally accompanied by a significant decrease in the running-in friction. Nitrogen implantation hardened the surface of steels and Cr and Co-W coatings. An ultra-microhardness technique showed that the true hardness of implanted layers was greater than the values obtained by conventional micro-hardness methods, which often result in penetration below the implanted depth. Scanning electron microscopy revealed that implantation reduced the ploughing effect during wear and a change in wear mechanism from an abrasive-adhesive type to a mild oxidative mode was evident. Retention of nitrogen after implantation was studied by Nuclear Reaction Analysis and Auger Electron Spectroscopy. It was shown that maximum nitrogen retention occurs in hard Cr coatings and AISI 420 stainless steel, which explains the improvements obtained in wear resistance and hardness. X-ray photoelectron spectroscopy on these materials revealed that nitrogen is almost entirely bound to Cr, forming chromium nitrides. It was concluded that nitrogen implantation at 90 keV and doses above 3x1017 ions/cm2 produced the most significant improvements in mechanical properties in materials containing nitride formers by precipitation strengthening, improving the load bearing capacity of the surface and changing the wear mechanism from adhesive-abrasive to oxidative.

Global optimisation of cold-formed steel sections

In this thesis, standard algorithms are used to carry out the optimisation of cold-formed steel purlins such as zed, channel and sigma sections, which are assumed to be simply supported and subjected to a gravity load. For zed, channel and sigma section, the local buckling, distortional buckling and lateral-torsional buckling are considered respectively herein. Currently, the local buckling is based on the BS 5950-5:1998 and EN 1993-1-3:2006. The distortional buckling is calculated by the direct strength method employing the elastic distortional buckling which is calculated by three available approaches such as Hancock (1995), Schafer and Pekoz (1998), Yu (2005). In the optimisation program, the lateral-torsional buckling based on BS 5950-5:1998, AISI and analytical model of Li (2004) are investigated. For the optimisation program, the programming codes are written for optimisation of channel, zed and sigma beam. The full study has been coded into a computer-based analysis program (MATLAB).

The breakdown of stainless steels in strong acids

A study was made of the corrosion behaviour in the ASTM standard Nitric acid and Oxalic acid tests, of two commercial AISI type 304L steels in the as received condition and after various heat treatments. Optical microscopy and SEM, TEM and STEM in conjunction with energy dispersive x-ray analysis, were used to correlate the corrosion behaviour of these steels with their microstructure. Some evidence of phosphorus segregation at grain boundaries was found. The corrosion behaviour at microstructural level was studied by examining on the TEM thin foils of steel that had been exposed to boiling nitric acid. Banding attack in the nitric acid and oxalic acid tests was studied using SEM and EPNA and found to be due to the micro-segregation of chromium and nickel. Using two experimental series of 304L, one a 17% Cr, 91 Ni, steel with phosphorus additions from 0.006% to 0.028%, the other a 20% Cr, 121 Ni steel with boron additions from 0.0011 to 0.00B51. The effect of these elements on corrosion in the nitric acid test was studied. The effect of different cooling rates and different solution treatment temperature on the behaviour of these steels was examined. TEM and STEM in conjunction with energy-dispersive x-ray analysis were again used to study the microstructure of the steels. Phosphorus was found to affect the corrosion behaviour but no effect was found with boron.

Análise tribo-termodinâmica da aplicação de nanopartículas de Al2O3 como aditivo lubrificante em compressor hermético de refrigeração

The thermodynamic performance of a refrigeration system can be improved by reducing the compression work by a particular technique for a specific heat removal rate. This study examines the effect of small concentrations of Al2O3 (50 nm) nanoparticles dispersion in the mineral oil based lubricant on the: viscosity, thermal conductivity, and lubrication characteristics as well as the overall performance (based on the Second Law of Thermodynamics) of the refrigerating system using R134a or R600a as refrigerants. The study looked at the influences of variables: i) refrigerant charge (100, 110, 120 and 130 g), ii) rotational speed of the condenser blower (800 and 1100 RPM) and iii) nanoparticle concentration (0.1 and 0.5 g/l) on the system performance based on the Taguchi method in a matrix of L8 trials with the criterion "small irreversibility is better”. They were carried pulldown and cycling tests according to NBR 12866 and NBR 12869, respectively, to evaluate the operational parameters: on-time ratio, cycles per hour, suction and discharge pressures, oil sump temperature, evaporation and condensation temperatures, energy consumption at the set-point, total energy consumption and compressor power. In order to evaluate the nanolubricant characteristics, accelerated tests were performed in a HFRR bench. In each 60 minutes test with nanolubricants at a certain concentration (0, 0.1 and 0.5 g/l), with three replications, the sphere (diameter 6.00 ± 0.05 mm, Ra 0.05 ± 0.005 um, AISI 52100 steel, E = 210 GPa, HRC 62 ± 4) sliding on a flat plate (cast iron FC200, Ra <0.5 ± 0.005 um) in a reciprocating motion with amplitude of 1 mm, frequency 20 Hz and a normal load of 1,96 N. The friction coefficient signals were recorded by sensors coupled to the HFRR system. There was a trend commented bit in the literature: a nanolubricant viscosity reduction at the low nanoparticles concentrations. It was found the dominant trend in the literature: increased thermal conductivity with increasing nanoparticles mass fraction in the base fluid. Another fact observed is the significant thermal conductivity growth of nanolubricant with increasing temperature. The condenser fan rotational speed is the most influential parameter (46.192%) in the refrigerator performance, followed by R600a charge (38.606%). The Al2O3 nanoparticles concentration in the lubricant plays a minor influence on system performance, with 12.44%. The results of power consumption indicates that the nanoparticles addition in the lubricant (0.1 g/L), together with R600a, the refrigerator consumption is reduced of 22% with respect to R134a and POE lubricant. Only the Al2O3 nanoparticles addition in the lubricant results in a consumption reduction of about 5%.

Análise tribo-termodinâmica da aplicação de nanopartículas de Al2O3 como aditivo lubrificante em compressor hermético de refrigeração

The thermodynamic performance of a refrigeration system can be improved by reducing the compression work by a particular technique for a specific heat removal rate. This study examines the effect of small concentrations of Al2O3 (50 nm) nanoparticles dispersion in the mineral oil based lubricant on the: viscosity, thermal conductivity, and lubrication characteristics as well as the overall performance (based on the Second Law of Thermodynamics) of the refrigerating system using R134a or R600a as refrigerants. The study looked at the influences of variables: i) refrigerant charge (100, 110, 120 and 130 g), ii) rotational speed of the condenser blower (800 and 1100 RPM) and iii) nanoparticle concentration (0.1 and 0.5 g/l) on the system performance based on the Taguchi method in a matrix of L8 trials with the criterion "small irreversibility is better”. They were carried pulldown and cycling tests according to NBR 12866 and NBR 12869, respectively, to evaluate the operational parameters: on-time ratio, cycles per hour, suction and discharge pressures, oil sump temperature, evaporation and condensation temperatures, energy consumption at the set-point, total energy consumption and compressor power. In order to evaluate the nanolubricant characteristics, accelerated tests were performed in a HFRR bench. In each 60 minutes test with nanolubricants at a certain concentration (0, 0.1 and 0.5 g/l), with three replications, the sphere (diameter 6.00 ± 0.05 mm, Ra 0.05 ± 0.005 um, AISI 52100 steel, E = 210 GPa, HRC 62 ± 4) sliding on a flat plate (cast iron FC200, Ra <0.5 ± 0.005 um) in a reciprocating motion with amplitude of 1 mm, frequency 20 Hz and a normal load of 1,96 N. The friction coefficient signals were recorded by sensors coupled to the HFRR system. There was a trend commented bit in the literature: a nanolubricant viscosity reduction at the low nanoparticles concentrations. It was found the dominant trend in the literature: increased thermal conductivity with increasing nanoparticles mass fraction in the base fluid. Another fact observed is the significant thermal conductivity growth of nanolubricant with increasing temperature. The condenser fan rotational speed is the most influential parameter (46.192%) in the refrigerator performance, followed by R600a charge (38.606%). The Al2O3 nanoparticles concentration in the lubricant plays a minor influence on system performance, with 12.44%. The results of power consumption indicates that the nanoparticles addition in the lubricant (0.1 g/L), together with R600a, the refrigerator consumption is reduced of 22% with respect to R134a and POE lubricant. Only the Al2O3 nanoparticles addition in the lubricant results in a consumption reduction of about 5%.

Estudo da evolução das tensões residuais através da difratometria de raios x em aço rolamento submetido a esforços cíclicos

The micro-deformations caused by cyclic loading origins the variation of the distances between atoms of the crystal lattice producing the irreversible component. In order to study and understand the microstructural behavior of the material this paper investigated the influence suffered by residual stresses in thrust rolling bearing races fabricated in AISI 52100 steel, after tests by cyclic rolling contact in a tribometer at 1m/s under two contact pressures (500 MPa and 1400 MPa) in dry and boundary lubrication conditions. Procedures of tests thermo-acustically isolated were developed for monitoring the contact temperature and sound pressure level signals to establish a comparison between the residual stress measurements, micro-hardness Vickers and micrographic registers searching an indication of wear evolution. The sin²ψ method by X-ray diffraction technique was used to quantify the residual stresses. Three raceway zones were selected for the evaluation of wear and surface morphology after predetermined cycling, comparing with their new condition ("as received"). Micro-hardness and residual stress measurements showed significant changes after the tests and it was possible to observe the relationship between the increase of sound pressure level and the residual stress for dry and lubricated conditions.

Estudo da evolução das tensões residuais através da difratometria de raios x em aço rolamento submetido a esforços cíclicos

The micro-deformations caused by cyclic loading origins the variation of the distances between atoms of the crystal lattice producing the irreversible component. In order to study and understand the microstructural behavior of the material this paper investigated the influence suffered by residual stresses in thrust rolling bearing races fabricated in AISI 52100 steel, after tests by cyclic rolling contact in a tribometer at 1m/s under two contact pressures (500 MPa and 1400 MPa) in dry and boundary lubrication conditions. Procedures of tests thermo-acustically isolated were developed for monitoring the contact temperature and sound pressure level signals to establish a comparison between the residual stress measurements, micro-hardness Vickers and micrographic registers searching an indication of wear evolution. The sin²ψ method by X-ray diffraction technique was used to quantify the residual stresses. Three raceway zones were selected for the evaluation of wear and surface morphology after predetermined cycling, comparing with their new condition ("as received"). Micro-hardness and residual stress measurements showed significant changes after the tests and it was possible to observe the relationship between the increase of sound pressure level and the residual stress for dry and lubricated conditions.

Process Monitoring and Defect Detection of Additive Manufacturing Using Inline Coherent Imaging

With applications ranging from aerospace to biomedicine, additive manufacturing (AM) has been revolutionizing the manufacturing industry. The ability of additive techniques, such as selective laser melting (SLM), to create fully functional, geometrically complex, and unique parts out of high strength materials is of great interest. Unfortunately, despite numerous advantages afforded by this technology, its widespread adoption is hindered by a lack of on-line, real time feedback control and quality assurance techniques. In this thesis, inline coherent imaging (ICI), a broadband, spatially coherent imaging technique, is used to observe the SLM process in 15 - 45 $\mu m$ 316L stainless steel. Imaging of both single and multilayer builds is performed at a rate of 200 $kHz$, with a resolution of tens of microns, and a high dynamic range rendering it impervious to blinding from the process beam. This allows imaging before, during, and after laser processing to observe changes in the morphology and stability of the melt. Galvanometer-based scanning of the imaging beam relative to the process beam during the creation of single tracks is used to gain a unique perspective of the SLM process that has been so far unobservable by other monitoring techniques. Single track processing is also used to investigate the possibility of a preliminary feedback control parameter based on the process beam power, through imaging with both coaxial and 100 $\mu m$ offset alignment with respect to the process beam. The 100 $\mu m$ offset improved imaging by increasing the number of bright A-lines (i.e. with signal greater than the 10 $dB$ noise floor) by 300\%. The overlap between adjacent tracks in a single layer is imaged to detect characteristic fault signatures. Full multilayer builds are carried out and the resultant ICI images are used to detect defects in the finished part and improve upon the initial design of the build system. Damage to the recoater blade is assessed using powder layer scans acquired during a 3D build. The ability of ICI to monitor SLM processes at such high rates with high resolution offers extraordinary potential for future advances in on-line feedback control of additive manufacturing.

Chemistry of potassium halides and their role in corrosion in biomass and waste firing

Compared to the use of traditional fossil fuels (coal, oil, natural gas), combustion of biomass and waste fuels has several environmental and economic advantages for heat and power generation. However, biomass and waste fuels might contain halogens (Cl, Br, F), alkali metals (Na, K) and heavy metals (Zn, Pb), which may cause harmful emissions and corrosion problems. Hightemperature corrosion occurs typically on furnace waterwalls and superheaters. The corrosion of the boiler tube materials limits the increase of thermal efficiency of steam boilers and leads to costly shutdowns and repairs. In recent years, some concerns have been raised about halogen (Cl, Br, and F)-related hightemperature corrosion in biomass- and waste-fired boilers. Chlorine-related high-temperature corrosion has been studied extensively. The presence of alkali chlorides in the deposits is believed to play a major role in the corrosion observed in biomass and waste fired boilers. However, there is much less information found in literature on the corrosion effect of bromine and fluorine. According to the literature, bromine is only assumed to play a role similar to chlorine; the role of fluorine is even less understood. In this work, a series of bubbling fluidized bed (BFB) bench-scale tests were carried out to characterize the formation and sulfation behaviors of KCl and KBr in BFB combustion conditions. Furthermore, a series of laboratory tests were carried out to investigate the hightemperature corrosion behaviors of three different superheater steels (10CrMo9-10, AISI 347 and Sanicro 28) exposed to potassium halides in ambient air and wet air (containing 30% H2O). The influence of H2O and O2 on the high-temperature corrosion of steels both with and without a salt (KCl) in three gas atmospheres (2% H2O-30% O2-N2, 2% H2O-2% O2-N2 and 30% H2O-2% O2-N2) was also studied. From the bench-scale BFB combustion tests, it was found that HBr has a clearly higher affinity for the available K forming KBr than HCl forming KCl. The tests also indicated that KCl has a higher tendency for sulfation than KBr. From the laboratory corrosion tests in ambient air (also called “dry air” in Paper III and Paper IV), it was found that at relatively low temperatures (≤ 550 °C) the corrosivity of KBr and KF are similar to KCl. At 600 °C, KF showed much stronger corrosivity than KBr and KCl, especially for 10CrMo9-10 and AISI 347. When exposed to KBr or KF, 10CrMo9-10 was durable at least up to 450 °C, while AISI 347 and Sanicro 28 were durable at least up to 550 °C. From the laboratory corrosion tests in wet air (30% H2O), no obvious effect of water vapor was detected at 450 °C. At 550 °C, the influence of water vapor became significant in some cases, but the trend was not consistent. At 550 °C, after exposure with KBr, 10CrMo9-10 suffered from extreme corrosion; after exposure with KF and KCl, the corrosion was less severe, but still high. At 550 °C, local deep pitting corrosion occurred on AISI 347 and Sanicro 28 after exposure with KF. Some formation of K2CrO4 was observed in the oxide layer. At 550 °C, AISI 347 and Sanicro 28 suffered from low corrosion (oxide layer thickness of < 10 μm) after exposure with KBr and KCl. No formation of K2CrO4 was observed. Internal oxidation occurred in the cases of AISI 347 with KBr and KCl. From the laboratory corrosion tests in three different gas atmospheres (2% H2O-30% O2-N2, 2% H2O-2% O2-N2 and 30% H2O-2% O2-N2), it was found that in tests with no salt, no corrosion occurred on AISI 347 and Sanicro 28 up to 600 °C in both the “O2-rich” (2% H2O-30% O2-N2) and “H2O-rich” (30% H2O-2% O2-N2) gas atmospheres; only 10CrMo9-10 showed increased corrosion with increasing temperature. For 10CrMo9-10 in the “O2-rich” atmosphere, the presence of KCl significantly increased the corrosion compared to the “no salt” cases. For 10CrMo9-10 in the “H2O-rich” atmosphere, the presence or absence of KCl did not show any big influence on corrosion. The formation of K2CrO4 was observed only in the case with the “O2-rich” atmosphere. Considering both the results from the BFB tests and the laboratory corrosion tests, if fuels containing Br were to be combusted, the corrosion damage of superheaters would be expected to be higher than if the fuels contain only Cl. Information generated from these studies can be used to help the boiler manufacturers in selecting materials for the most demanding combustion systems.

Functional alkali tantalate 2D structures for microelectronics and related applications

Alkali tantalates and niobates, including K(Ta / Nb)O3, Li(Ta / Nb)O3 and Na(Ta / Nb)O3, are a very promising ferroic family of lead-free compounds with perovskite-like structures. Their versatile properties make them potentially interesting for current and future application in microelectronics, photocatalysis, energy and biomedics. Among them potassium tantalate, KTaO3 (KTO), has been raising interest as an alternative for the well-known strontium titanate, SrTiO3 (STO). KTO is a perovskite oxide with a quantum paraelectric behaviour when electrically stimulated and a highly polarizable lattice, giving opportunity to tailor its properties via external or internal stimuli. However problems related with the fabrication of either bulk or 2D nanostructures makes KTO not yet a viable alternative to STO. Within this context and to contribute scientifically to the leverage tantalate based compounds applications, the main goals of this thesis are: i) to produce and characterise thin films of alkali tantalates by chemical solution deposition on rigid Si based substrates, at reduced temperatures to be compatible with Si technology, ii) to fulfil scientific knowledge gaps in these relevant functional materials related to their energetics and ii) to exploit alternative applications for alkali tantalates, as photocatalysis. In what concerns the synthesis attention was given to the understanding of the phase formation in potassium tantalate synthesized via distinct routes, to control the crystallization of desired perovskite structure and to avoid low temperature pyrochlore or K-deficient phases. The phase formation process in alkali tantalates is far from being deeply analysed, as in the case of Pb-containing perovskites, therefore the work was initially focused on the process-phase relationship to identify the driving forces responsible to regulate the synthesis. Comparison of phase formation paths in conventional solid-state reaction and sol-gel method was conducted. The structural analyses revealed that intermediate pyrochlore K2Ta2O6 structure is not formed at any stage of the reaction using conventional solid-state reaction. On the other hand in the solution based processes, as alkoxide-based route, the crystallization of the perovskite occurs through the intermediate pyrochlore phase; at low temperatures pyrochlore is dominant and it is transformed to perovskite at >800 °C. The kinetic analysis carried out by using Johnson-MehlAvrami-Kolmogorow model and quantitative X-ray diffraction (XRD) demonstrated that in sol-gel derived powders the crystallization occurs in two stages: i) at early stage of the reaction dominated by primary nucleation, the mechanism is phase-boundary controlled, and ii) at the second stage the low value of Avrami exponent, n ~ 0.3, does not follow any reported category, thus not permitting an easy identification of the mechanism. Then, in collaboration with Prof. Alexandra Navrotsky group from the University of California at Davis (USA), thermodynamic studies were conducted, using high temperature oxide melt solution calorimetry. The enthalpies of formation of three structures: pyrochlore, perovskite and tetragonal tungsten bronze K6Ta10.8O30 (TTB) were calculated. The enthalpies of formation from corresponding oxides, ∆Hfox, for KTaO3, KTa2.2O6 and K6Ta10.8O30 are -203.63 ± 2.84 kJ/mol, - 358.02 ± 3.74 kJ/mol, and -1252.34 ± 10.10 kJ/mol, respectively, whereas from elements, ∆Hfel, for KTaO3, KTa2.2O6 and K6Ta10.8O30 are -1408.96 ± 3.73 kJ/mol, -2790.82 ± 6.06 kJ/mol, and -13393.04 ± 31.15 kJ/mol, respectively. The possible decomposition reactions of K-deficient KTa2.2O6 pyrochlore to KTaO3 perovskite and Ta2O5 (reaction 1) or to TTB K6Ta10.8O30 and Ta2O5 (reaction 2) were proposed, and the enthalpies were calculated to be 308.79 ± 4.41 kJ/mol and 895.79 ± 8.64 kJ/mol for reaction 1 and reaction 2, respectively. The reactions are strongly endothermic, indicating that these decompositions are energetically unfavourable, since it is unlikely that any entropy term could override such a large positive enthalpy. The energetic studies prove that pyrochlore is energetically more stable phase than perovskite at low temperature. Thus, the local order of the amorphous precipitates drives the crystallization into the most favourable structure that is the pyrochlore one with similar local organization; the distance between nearest neighbours in the amorphous or short-range ordered phase is very close to that in pyrochlore. Taking into account the stoichiometric deviation in KTO system, the selection of the most appropriate fabrication / deposition technique in thin films technology is a key issue, especially concerning complex ferroelectric oxides. Chemical solution deposition has been widely reported as a processing method to growth KTO thin films, but classical alkoxide route allows to crystallize perovskite phase at temperatures >800 °C, while the temperature endurance of platinized Si wafers is ~700 °C. Therefore, alternative diol-based routes, with distinct potassium carboxylate precursors, was developed aiming to stabilize the precursor solution, to avoid using toxic solvents and to decrease the crystallization temperature of the perovskite phase. Studies on powders revealed that in the case of KTOac (solution based on potassium acetate), a mixture of perovskite and pyrochlore phases is detected at temperature as low as 450 °C, and gradual transformation into monophasic perovskite structure occurs as temperature increases up to 750 °C, however the desired monophasic KTaO3 perovskite phase is not achieved. In the case of KTOacac (solution with potassium acetylacetonate), a broad peak is detected at temperatures <650 °C, characteristic of amorphous structures, while at higher temperatures diffraction lines from pyrochlore and perovskite phases are visible and a monophasic perovskite KTaO3 is formed at >700 °C. Infrared analysis indicated that the differences are due to a strong deformation of the carbonate-based structures upon heating. A series of thin films of alkali tantalates were spin-coated onto Si-based substrates using diol-based routes. Interestingly, monophasic perovskite KTaO3 films deposited using KTOacac solution were obtained at temperature as low as 650 °C; films were annealed in rapid thermal furnace in oxygen atmosphere for 5 min with heating rate 30 °C/sec. Other compositions of the tantalum based system as LiTaO3 (LTO) and NaTaO3 (NTO), were successfully derived as well, onto Si substrates at 650 °C as well. The ferroelectric character of LTO at room temperature was proved. Some of dielectric properties of KTO could not be measured in parallel capacitor configuration due to either substrate-film or filmelectrode interfaces. Thus, further studies have to be conducted to overcome this issue. Application-oriented studies have also been conducted; two case studies: i) photocatalytic activity of alkali tantalates and niobates for decomposition of pollutant, and ii) bioactivity of alkali tantalate ferroelectric films as functional coatings for bone regeneration. Much attention has been recently paid to develop new type of photocatalytic materials, and tantalum and niobium oxide based compositions have demonstrated to be active photocatalysts for water splitting due to high potential of the conduction bands. Thus, various powders of alkali tantalates and niobates families were tested as catalysts for methylene blue degradation. Results showed promising activities for some of the tested compounds, and KNbO3 is the most active among them, reaching over 50 % degradation of the dye after 7 h under UVA exposure. However further modifications of powders can improve the performance. In the context of bone regeneration, it is important to have platforms that with appropriate stimuli can support the attachment and direct the growth, proliferation and differentiation of the cells. In lieu of this here we exploited an alternative strategy for bone implants or repairs, based on charged mediating signals for bone regeneration. This strategy includes coating metallic 316L-type stainless steel (316L-SST) substrates with charged, functionalized via electrical charging or UV-light irradiation, ferroelectric LiTaO3 layers. It was demonstrated that the formation of surface calcium phosphates and protein adsorption is considerably enhanced for 316L-SST functionalized ferroelectric coatings. Our approach can be viewed as a set of guidelines for the development of platforms electrically functionalized that can stimulate tissue regeneration promoting direct integration of the implant in the host tissue by bone ingrowth and, hence contributing ultimately to reduce implant failure.

Diseño estructural de una vivienda de dos plantas con perfiles laminados en caliente

El tema tratado en el trabajo trata la como se debe analizar, modelar y diseñar una estructura en nuestro caso es una edificación de dos pisos. En el capítulo 1 se trata una breve introducción, antecedentes y beneficios del acero, también se encuentran los objetivos planteados en el presente trabajo. En el capítulo 2 se describe los tipos de carga que pueden actuar en la edificación, el uso de los requisitos del código ecuatoriano de la construcción, la distribución de la fuerza cortante, y las diferentes combinaciones de carga que se pueden realizar. En el capítulo 3 se describe la modelación de la estructura, la concepción estructural que se debe tener, y el empleo del Programa SAP 2000. El capitulo 4 trata sobre las consideraciones que se debe de realizar en los elementos de acuerdo al método LRFD, elementos, anchos efectivos de los elementos no rigidizados, y conjuntos estructurales. En el capítulo 5 se trata del diseño de miembros en flexión el diseño de la viga principal y secundaria con respecto a las especificaciones AISI. En el capítulo 6 se encuentra el diseño de miembros comprimidos con las respectivas combinaciones de carga axial y de flexión. En el capítulo 7 se encuentra el diseño del entrepiso de acuerdo a las especificaciones del fabricante. En el capitulo 8 trata el diseño de las uniones con sueldas y tornillos respectivamente.

Efeito da radiação micro-ondas na sinterização em fases sólida e líquida de pós de aço inoxidável 3I6L

Tese submetida à Universidade de Coimbra, Faculdade de Ciências e Tecnologia e aprovada em provas públicas para a obtenção do Grau de Doutor em Engenharia Mecânica (especialidade de Ciência dos Materiais)

Metodología experimental para la caracterización de proceso de rectificado cilíndrico en penetración

El objetivo principal de este proyecto consiste en presentar una metodología experimental, que permita caracterizar el comportamiento de un conjunto de muelas en el rectificado cilíndrico exterior en penetración, para un acero especial típico de sistemas de transmisión (AISI 52100), utilizado especialmente en el sector de la automoción, empleándose en elementos como rodamientos.