In situ study of Ge(100) surfaces with tertiarybutylphosphine supply in vapor phase epitaxy ambient

GaInP nucleation on Ge(100) often starts by annealing of the Ge(100) substrates under supply of phosphorus precursors. However, the influence on the Ge surface is not well understood. Here, we studied vicinal Ge(100) surfaces annealed under tertiarybutylphosphine (TBP) supply in MOVPE by in situ reflection anisotropy spectroscopy (RAS), X-ray photoelectron spectroscopy (XPS), and low energy electron diffraction (LEED). While XPS reveals a P termination and the presence of carbon on the Ge surface, LEED patterns indicate a disordered surface probably due to by-products of the TBP pyrolysis. However, the TBP annealed Ge(100) surface exhibits a characteristic RA spectrum, which is related to the P termination. RAS allows us to in situ control phosphorus desorption dependent on temperature.

Effect of Stress Level on the High Temperature Deformation and Fracture Mechanisms of Ti-45Al-2Nb-2Mn-0.8 vol. pct TiB2: An In Situ Experimental Study

The effect of the applied stress on the deformation and crack nucleation and propagation mechanisms of a c-TiAl intermetallic alloy (Ti-45Al-2Nb-2Mn (at. pct)-0.8 vol. pct TiB2) was examined by means of in situ tensile (constant strain rate) and tensile-creep (constant load) experiments performed at 973 K (700 �C) using a scanning electron microscope. Colony boundary cracking developed during the secondary stage in creep tests at 300 and 400 MPa and during the tertiary stage of the creep tests performed at higher stresses. Colony boundary cracking was also observed in the constant strain rate tensile test. Interlamellar ledges were only found during the tensile-creep tests at high stresses (r>400 MPa) and during the constant strain rate tensile test. Quantitative measurements of the nature of the crack propagation path along secondary cracks and along the primary crack indicated that colony boundaries were preferential sites for crack propagation under all the conditions investigated. The frequency of interlamellar cracking increased with stress, but this fracture mechanism was always of secondary importance. Translamellar cracking was only observed along the primary crack.

Effects of the correction of particle microbial contamination and particle transit model in the rumen on in situ protein evaluation of grass hays.

Effects of considering the particle comminution rate -kc- in addition to particle rumen outflow -kp- and the ruminal microbial contamination on estimates of by-pass and intestinal digestibility of DM, organic matter and crude protein were examined in perennial ryegrass and oat hays. By-pass kc-kp-based values of amino acids were also determined. This study was performed using particle transit, in situ and 15N techniques on three rumen and duodenum-cannulated wethers. The above estimates were determined using composite samples from rumen-incubated residues representative of feed by-pass. Considering the comminution rate, kc, modified the contribution of the incubated residues to these samples in both hays and revealed a higher microbial contamination, consistently in oat hay and only as a tendency for crude protein in ryegrass hay. Not considering kc or rumen microbial contamination overvalued by-pass and intestinal digestibility in both hays. Therefore, non-microbial-corrected kp-based values of intestinal digested crude protein were overestimated as compared with corrected and kc-kp-based values in ryegrass hay -17.4 vs 4.40%- and in oat hay -5.73 vs 0.19%-. Both factors should be considered to obtain accurate in situ estimates in grasses, as the protein value of grasses is very conditioned by the microbial synthesis derived from their ruminal fermentation. Consistent overvaluations of amino acid by-pass due to not correcting microbial contamination were detected in both hays, with large variable errors among amino acids. A similar degradation pattern of amino acids was recorded in both hays. Cysteine, methionine, leucine and valine were the most degradation-resistant amino acids.

Effects of the ruminal comminution rate and microbial contamination of particles on accuracy of in situ estimates of ruminal degradability and intestinal digestibility of feedstuffs.

Effects of considering the comminution rate -kc- and the correction of microbial contamination -using 15N techniques- of particles in the rumen on estimates of ruminally undegraded fractions and their intestinal digestibility were examined generating composite samples -from rumen-incubated residues- representative of the undegraded feed rumen outflow. The study used sunflower meal -SFM- and Italian ryegrass hay -RGH- and three rumen and duodenum cannulated wethers fed with a 40:60 RGH to concentrate diet -75 g DM/kgBW0.75-. Transit studies up to the duodenum with Yb-SFM and Eu-RGH marked samples showed higher kc values -/h- in SFM than in RGH -0.577 vs. 0.0892, p = 0.034-, whereas similar values occurred for the rumen passage rate -kp-. Estimates of ruminally undegraded and intestinal digestibility of all tested fractions decreased when kc was considered and also applying microbial correction. Thus, microbial uncorrected kp-based proportions of intestinal digested undegraded crude protein overestimated those corrected and kc-kp-based by 39% in SFM -0.146 vs. 0.105- and 761% in RGH -0.373 vs. 0.0433-. Results show that both kc and microbial contamination correction should be considered to obtain accurate in situ estimates in grasses, whereas in protein concentrates not considering kc is an important source of error.

In situ control of the GE(100)surface domain structure for III-V multijunction solar cells

Vicinal Ge(100) is the common substrate for state of the art multi-junction solar cells grown by metal-organic vapor phase epitaxy (MOVPE). While triple junction solar cells based on Ge(100) present efficiencies mayor que 40%, little is known about the microscopic III-V/Ge(100) nucleation and its interface formation. A suitable Ge(100) surface preparation prior to heteroepitaxy is crucial to achieve low defect densities in the III-V epilayers. Formation of single domain surfaces with double layer steps is required to avoid anti-phase domains in the III-V films. The step formation processes in MOVPE environment strongly depends on the major process parameters such as substrate temperature, H2 partial pressure, group V precursors [1], and reactor conditions. Detailed investigation of these processes on the Ge(100) surface by ultrahigh vacuum (UHV) based standard surface science tools are complicated due to the presence of H2 process gas. However, in situ surface characterization by reflection anisotropy spectroscopy (RAS) allowed us to study the MOVPE preparation of Ge(100) surfaces directly in dependence on the relevant process parameters [2, 3, 4]. A contamination free MOVPE to UHV transfer system [5] enabled correlation of the RA spectra to results from UHV-based surface science tools. In this paper, we established the characteristic RA spectra of vicinal Ge(100) surfaces terminated with monohydrides, arsenic and phosphorous. RAS enabled in situ control of oxide removal, H2 interaction and domain formation during MOVPE preparation.

Modelización del proceso de eliminación de la contaminación de suelos con hidrocarburos mediante desorción térmica “in situ” Comprobación de Modelo

El objetivo definitivo de esta investigación es contribuir con la profundización del conocimiento en las tecnologías de remediación, específicamente las térmicas, debido a que la contaminación de suelos es motivo de preocupación por ser uno de los graves impactos ambientales que origina el hombre con sus actividades, especialmente las industriales, afectando a la salud de los seres humanos, y el medio ambiente, representando elevados costes de saneamiento y en ocasiones problemas graves de salud de las comunidades aledañas. Se establecen tres fases de investigación. En la primera se diseña el sistema de termodesorción a escala piloto, se desarrolla las corridas experimentales, la segunda con corridas en laboratorio para investigar sobre los parámetros que intervienen en el proyecto. Se hacen las corridas respectivas para determinar la eficacia del sistema, y la tercera fase que consiste en comparar los modelos teóricos de Hartley, con los de Hartley Graham –Bryce y el de Hamaker para determinar su aproximación con los resultados reales. Apoyado en investigaciones anteriores, se diseñó y construyó un sistema de desorción térmica, el cual consiste en un horno tipo caja con 4 calentadores (resistencias), y una campana con un filtro para evitar la contaminación atmosférica, así mismo, se diseñó un sistema de control que permitió hacer las corridas con 1/3 de la potencia, con una relación de encendido apagado 3:1 respectivamente. Para validar los resultados obtenidos en el estudio matemático, se compararon dos modelos con la finalidad cuál de ellos se aproxima más a la realidad, se tomaron los ensayos con sus tiempos de operación a las temperaturas y se trabajó a distintas bandas de temperaturas para verificar la fiabilidad del proceso matemático. La temperatura es un variable importante en los procesos de desorción, como los son también la humedad del suelo, pues esta va influir directamente en el tiempo de remediación, por lo que es importante tomarla en cuenta. De igual forma el tipo de suelo va influir en los resultados, siendo las arenas más aptas para este tipo de remediación. Los resultados de la modelización son presentados para temperaturas constantes, el cual difiere de la realidad, pues el proceso de calentamiento es lento y va en accenso dependiendo del contenido de humedad y de las propiedades del suelo. La experimentación realizada concluye con buenos resultados de la aplicación de sistemas de desorción de acuerdo a las variables de Panamá. Con relación al grado de cumplimiento respecto a las normativas actuales relacionadas a los límites máximos permitidos. Los resultados garantizan las posibilidades del proceso de remediación térmica de suelos contaminados con combustibles en rango de diésel, garantizando niveles aceptables de limpieza en un tiempo menor a otras metodologías no destructivas pudieran tomar. ABSTRACT The ultimate goal of this investigation is to enhance the pool of knowledge related to remediation technologies, specifically thermal desorption. The motivation for this study is based on concerns due to pollution of land as one of the most serious environmental impacts caused by anthropogenic effects, specially industrial activities, affecting human health and the environment in general, which represents high reclamation costs, and in some cases, serious health issues in nearby communities. Three phases have been established for this study. The first phase involves the design of a thermal desorption system as a pilot experiment, and associated tests. The second phase consists of laboratory testing to investigate the parameters that affect the investigation, as well as to determine the efficacy of the system. The third phase covers the comparison of theorical models as proposed by Hartley, Hartley Graham – Bryce, and Hamaker, as well as the evaluation of these models versus the laboratory results. Supported by previous researches, the thermal desorption system was designed and installed as a “box” type oven with four heaters (resistances) and one absorption hood with a filter to avoid atmospheric contamination. In the same way, a control system was designed allowing testing with 1/3 of the power, with an on/off rate of 3:1 respectively. In order to validate the results, two mathematical models were compared to identify which model is closer to the experimental results; test results were documented with respective durations and temperatures; and experiments were executed using different ranges of temperature to validate the consistency of the mathematical process. Temperature is an important variable that should be considered for the desorption processes, as well as the humidity content within the soil, that has direct influence over the required duration to achieve remediation. In the same manner, the type of soil also influences the results, where sands are more efficient for this type of remediation process. The results from this experiment are according to constant temperatures, which is not a complete representation of the reality, as the heating process is slow and the temperature gradually increases according to the humidity content and other properties of the soil. The experiment shows good results for the application of thermal desorption systems according to the variables in Panama, as well as the level of compliance required to fulfill current regulations and mandatory maximum limits. The results guarantee the possibility of soil thermo-remediation as a resource to clean sites that have been polluted with diesel-like combustibles, allowing acceptable levels in a period of time that is lower than with other non-destructive remediation technics.