Caracterización por microscopía electrónica de transmisión de heteroestructuras InGaAs/InAIAs crecidas por epitaxia de haces moleculares sobre substratos de InP

[spa] La finalidad de la investigación es la optimización del crecimiento de estructuras InX Ga1-XAs/InYA11-YAs/InP, para la obtención de dispositivos HEMT funcionales. Previamente se ha optimizado la preparacion de muestras para su observación en microscopía electrónica de transmisión, evitando la nucleación de islas de In y homogeneizando la velocidad de adelgazamiento entre las estructuras y el InP. Se ha establecido que un tratamiento térmico del InP a una temperatura de Th=530 grados C bajo atmosfera de sobrepresión de As, elimina completamente el óxido de pasivación, proporcionando un frente de crecimiento plano. La temperatura óptima de crecimiento del INO.52 ALO.48 ha resultado de 530 grados C, con mínimas densidades de defectos y una reducción de los centros de captura de portadores. Hemos observado que las longitudes de onda de las modulaciones de contraste observadas en TEM en las capas de InGaAs, varian con las condiciones de crecimiento, considerando que las modulaciones gruesa (modulación de composición) y fina (distribución inhomogénea de agregados ricos en Ga o en In), responden a un mecanismo de autoestabilización (favorecido por la limitación cinética de la técnica MBE), para evitar una total separación de fases en InAs y GaAs si el material se ha crecido dentro del “gap” de miscibilidad. Hemos diferenciado los mecanismos de relajación de los esfuerzos en capas composicionalmente homogeneas, segun sean tensadas o comprimidas. Para las primeras hemos observado nucleación de dislocaciones en el orden 90 grados-60 grados-30 grados, con una recombinación inmediata 30 grados + 90 grados - 60 grados. En las segundas, el proceso de relajación responde a la nucleación de dislocaciones perfectas, seguida de una disociación 60 grados - 90 grados + 30 grados, y gobernado por las barreras de fricción que impiden la recombinacion de las parciales

Mapping the magnetic coupling of self-assembled Fe3O4 nanocubes by electron holography

The nanoscale magnetic configuration of self-assembled groups of magnetite 40 nm cubic nanoparticles has been investigated by means of electron holography in the transmission electron microscope (TEM). The arrangement of the cubes in the form of chains driven by the alignment of their dipoles of single nanocubes is assessed by the measured in-plane magnetic induction maps, in good agreement with theoretical calculations

Nucleation and growth of GaN nanorods on Si (111) surfaces by plasma-assisted molecular beam epitaxy - The influence of Si- and Mg-doping

The self-assembled growth of GaN nanorods on Si (111) substrates by plasma-assisted molecular beam epitaxy under nitrogen-rich conditions is investigated. An amorphous silicon nitride layer is formed in the initial stage of growth that prevents the formation of a GaN wetting layer. The nucleation time was found to be strongly influenced by the substrate temperature and was more than 30 min for the applied growth conditions. The observed tapering and reduced length of silicon-doped nanorods is explained by enhanced nucleation on nonpolar facets and proves Ga-adatom diffusion on nanorod sidewalls as one contribution to the axial growth. The presence of Mg leads to an increased radial growth rate with a simultaneous decrease of the nanorod length and reduces the nucleation time for high Mg concentrations

Clustering analysis strategies for electron energy loss spectroscopy (EELS).

In this work, the use of cluster analysis algorithms, widely applied in the field of big data, is proposed to explore and analyse electron energy loss spectroscopy (EELS) data sets. Three different data clustering approaches have been tested both with simulated and experimental data from Fe3O4/Mn3O4 core/shell nanoparticles. The first method consists on applying data clustering directly to the acquired spectra. A second approach is to analyse spectral variance with principal component analysis (PCA) within a given data cluster. Lastly, data clustering on PCA score maps is discussed. The advantages and requirements of each approach are studied. Results demonstrate how clustering is able to recover compositional and oxidation state information from EELS data with minimal user input, giving great prospects for its usage in EEL spectroscopy

Caracterización estructural de capas epitaxiadas de InGaAs/InAlAs crecidas sobre substratos (111) de InP

Se ha analizado por microscopía electrónica en transmisión (TEM) la estructura de transistores HEMT basados en un pozo cuántico tensionado de InGaAs/InAlAs crecido sobre un sustrato {111} de InP. Se han observado dislocaciones filiformes y defectos planares que cruzan la capa superior hacia la superficie, así como maclas paralelas a la interficie y grandes complejos defectivos en forma de V que se nuclean unos pocos nanometres por encima de la interficie entre el pozo cuántico y la capa superior que lo confina. La estructura de los defectos es muy diferente de la observada en heteroestructuras similares crecidas sobre sustratos {100}, hecho que sugiere que hay que tener en cuenta consideraciones sobre el proceso mismo de nucleación de los defectos junto con las convencionales relacionadas con el desajuste de redes

Competitive evolution of the fine contrast modulation and CuPt ordering in InGaP/GaAs layers

We use transmission electron microscopy to characterize the morphology of InGaP epitaxial layers grown by metal‐organic vapor‐phase epitaxy over misoriented GaAs (001) substrates, with a cutoff angle in a range from 0° to 25°. The occurrence of phase separation and CuPt‐type ordered superstructures has been observed. The most ordered configuration has been found to appear in layers grown on 2° off substrates, and the strength of order decreases with increasing the misorientation angle beyond α=2°. Conversely, whereas the phase separation is less evident in the layer grown at 2°, the sample grown with a misorientation of 25° exhibits the most phase separated configuration. The completion between these two phenomena is discussed depending on the misorientation angle

Distinct magnetism in ultrathin epitaxial NiFe2O4 films on MgAl2O4 and SrTiO3single crystalline substrates

Spinel ferrites are being considered for advanced spintronic applications. Here, we report on the magnetic properties of ultrathin (3-37 nm) epitaxial films of NiFe2O4 (NFO) on MgAl2O4 (MAO) and SrTiO3 (STO) single crystalline substrates. It is found that NFO films on STO display superparamagnetic response down to 50 K, whereas films grown on MAO display ferrimagnetic response up to room temperature. Microstructural information indicates that this distinct response can be attributed to the different growth mechanisms of the spinel ferrite on the isostructural MAO substrate (two-dimensional growth) and the perovskite STO (Volmer-Weber three-dimensional growth). We discuss the reasons for this distinct behavior and its relevance for the integration of ferrites in epitaxial heterostructures for tunnel devices

Tailoring the surface density of silicon nanocrystals embedded in SiOx single layers

In this article, we explore the possibility of modifying the silicon nanocrystal areal density in SiOx single layers, while keeping constant their size. For this purpose, a set of SiOx monolayers with controlled thickness between two thick SiO2 layers has been fabricated, for four different compositions (x=1, 1.25, 1.5, or 1.75). The structural properties of the SiO x single layers have been analyzed by transmission electron microscopy (TEM) in planar view geometry. Energy-filtered TEM images revealed an almost constant Si-cluster size and a slight increase in the cluster areal density as the silicon content increases in the layers, while high resolution TEM images show that the size of the Si crystalline precipitates largely decreases as the SiO x stoichiometry approaches that of SiO2. The crystalline fraction was evaluated by combining the results from both techniques, finding a crystallinity reduction from 75% to 40%, for x = 1 and 1.75, respectively. Complementary photoluminescence measurements corroborate the precipitation of Si-nanocrystals with excellent emission properties for layers with the largest amount of excess silicon. The integrated emission from the nanoaggregates perfectly scales with their crystalline state, with no detectable emission for crystalline fractions below 40%. The combination of the structural and luminescence observations suggests that small Si precipitates are submitted to a higher compressive local stress applied by the SiO2 matrix that could inhibit the phase separation and, in turn, promotes the creation of nonradiative paths

Organización espontánea de puntos cuánticos de InSb crecidos por ALMBE sobre substratos de InP

El crecimiento autoorganizado de puntos cuánticos de InSb sobre substratos de InP mediante epitaxia de haces moleculares ha sido caracterizado mediante microscopía electrónica de transmisión y microscopía de fuerzas atómicas a fin de estudiar la morfología y establecer el mecanismo de relajación de las estructuras. Medidas de difracción de electrones de alta energía durante el crecimiento de las muestras indican una transición en el modo de crecimiento de bidimensional a tridimensional a partir de un espesor total equivalente depositado de 1.1 monocapas atómicas de InSb. Los puntos cuánticos tienen en general, una buena calidad cristalina así como una distribución superficial homogénea, pero una alta anisotropía en las dimensiones entre las direcciones [110] y [110]. Así mismo, se encuentra una rugosidad superficial, también afectada de un alto grado de anisotropía, siendo las crestas y los valles paralelos a la dirección de elongación de las islas. Las imágenes de microscopía electrónica revelan un facetado de las estructuras según planos (001) que las limitan por la parte superior y planos {111}, {113} y {114}, que las limitan lateralmente. Las tensiones son eficazmente relajadas por la presencia de una red de dislocaciones situada en la interficie InSb/InP

Quantitative parameters for the examination of InGaN QW multilayers by low-loss EELS

We present a detailed examination of a multiple InxGa1−xN quantum well (QW) structure for optoelectronic applications. The characterization is carried out using scanning transmission electron microscopy (STEM), combining high-angle annular dark field (HAADF) imaging and electron energy loss spectroscopy (EELS). Fluctuations in the QW thickness and composition are observed in atomic resolution images. The impact of these small changes on the electronic properties of the semiconductor material is measured through spatially localized low-loss EELS, obtaining band gap and plasmon energy values. Because of the small size of the InGaN QW layers additional effects hinder the analysis. Hence, additional parameters were explored, which can be assessed using the same EELS data and give further information. For instance, plasmon width was studied using a model-based fit approach to the plasmon peak; observing a broadening of this peak can be related to the chemical and structural inhomogeneity in the InGaN QW layers. Additionally, Kramers-Kronig analysis (KKA) was used to calculate the complex dielectric function (CDF) from the EELS spectrum images (SIs). After this analysis, the electron effective mass and the sample absolute thickness were obtained, and an alternative method for the assessment of plasmon energy was demonstrated. Also after KKA, the normalization of the energy-loss spectrum allows us to analyze the Ga 3d transition, which provides additional chemical information at great spatial resolution. Each one of these methods is presented in this work together with a critical discussion of their advantages and drawbacks