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Structural and Electronic Properties of Indium Rich Nitride Nanostructures

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Structural and Electronic Properties of Indium Rich Nitride Nanostructures francesco ivaldi STRUCTURALANDELECTRONICPROPERTIESOF INDIUMRICHNITRIDENANOSTRUCTURES STRUCTURALANDELECTRONICPROPERTIESOFINDIUM RICHNITRIDENANOSTRUCTURES francesco ivaldi Institute of Physics Polish Academy of Science Laboratory of X-Ray and electron microscopy research Group of electron microscopy Promotor: Prof. nzw. dr hab. Piotr Dłuzewski˙ Warsaw, September 2015 Francesco Ivaldi: Structural and electronic properties of indium rich ni- tride nanostructures, III-V heterostructures investigated by TEM and connected methods, c September 2015 ABSTRACT New materials such as III-N ternary alloys are object of increasing interest in the field of micro- and nanotechnology due to their rel- evant optical and electronical properties. Those alloys are especially appealing to be used to form quantum nanostructures for various de- vice applications such as laser emitting diodes, high electron mobility transistors and solar cells. This thesis investigates the properties of InGaN and AlInN alloys with high indium content (> 25 %). TEM and STEM combined with EELS and EDX investigations have been used to correlate the struc- tural changes with the local electronic and optical properties of In- GaN quantum wells and InN quantum dots as a consequence of ther- mal processes. Annealing of InGaN quantum wells and capping of both InN quan- tum dots and quantum wells under different conditions have been investigated. Image processing techniques such as geometric phase analysis of HR-TEM images were used to reveal significant fluctua- tions in the indium distribution on a nanometric scale inside the wells. The growth parameters leading to improved photoemission proper- ties have been determined. MBE and MOCVD grown samples have been used to analyze the influence of the temperature of the quantum barrier growth on the structural and electronic properties of the samples. The local indium concentration was measured through strain measurements by digital processing from the lattice fringes images taken by HR-TEM. Forma- tion of indium clusters and fluctuations of indium content have been determined and analyzed. Photoluminescence spectra have been cor- related to the obtained data. Self-organized InN quantum dots grown by three different proce- dures on GaN by MOCVD were investigated by TEM. It has been shown that no wetting layer is formed during growth at low tem- perature. The quantum dots have been overgrown by a GaN cap layer at the same temperature as the dots’ growth temperature. This growth resulted in a smooth top surface. Cubic GaN inclusions were observed in the cap layer, as well as strong indium intermixing. It has been observed that the capped quantum dots had decreased di- mensions and were 90 % relaxed due to the formation of misfit dis- locations at the GaN/InN interface. The density of the dislocations was correlated to the intensity of the photoluminescence spectrum of the dots. For InN quantum dots capped with GaN at higher temper- atures HR-TEM images and EEL spectra revealed the formation of InGaN layers of various indium content and even the presence of a v metallic indium phase. Low energy EEL spectra were measured for quantum dots and wells, for which the indium content was calcu- lated by GPA method. For those spectra the plasmon peak position was determined with an accuracy in the order of meV. A strong cor- relation between the plasmon peak position and the indium content was found. The Win2k software has been used to calculate the posi- tion of the plasmon peak for InAlN and InGaN. The simulations gave full agreement with experimental data. STRESZCZENIEPRACY Nowe materiały układu potrójnego metali grupy III z azotem s ˛a obiektem wci ˛az˙ rosn ˛acegozainteresowania miko- i nano-technologii z powodu na ich wyj ˛atkowe optyczne i elektroniczne własno´sci.Te materiały w szczególno´scistosowane s ˛ado wytwarzania nanostruk- tur znajduj ˛acych zastosowanie jako diody laserowe, tranzystory o wysokiej ruchliwo´scielektronów czy baterie słoneczne. W pracy badano własno´sci nanostruktur InxGa1-xN oraz Al1-xInxN o duzej˙ koncentracji indu (> 25 at%). Badania TEM oraz STEM w poł ˛aczeniu z EELS oraz EDX były zastosowane do znalezienia zalezno´sci˙ pomi ˛edzyzmianami struktury spowodo- wanymi procesami termicznymi a lokalnymi własno´sciami elek- tronowymi i optycznymi kropek i studni kwantowych. Badano wpływ wygrzewania w roznych˙ warunkach na studnie kwantowe InGaN oraz na przykrywane studnie i kropki kwantowe InN. Technik˛eprzetwarzania obrazów tak ˛ajak metoda fazy geome- trycznej zastosowano do analizy obrazów wysokorozdzielczych, dz- i ˛ekiczemu ujawniono wyst ˛epowanie fluktuacji koncentracji indu w skali nanometrowej wewn ˛atrzstudni. Okre´slonoparametry wzrostu pozwalaj ˛acepolepszy´cwłasno´scifotoemisyjne. Próbki wytwarzane metodami MBE oraz MOCVD uzyto˙ do anal- izy wpływu temperatury wzrostu bariery na struktur˛ei własno´sci elektronowe. Lokaln ˛akoncentracj ˛eindu wyznaczono na podstawie odkształce´notrzymanych na drodze numerycznej analizy wysoko- rozdzielczych pr ˛azkowych˙ obrazów płaszczyzn krystalicznych. Stwierdzono i przeanalizowano wyst ˛epowanie fluktuacji za- warto´sciindu. Otrzymane informacje powi ˛azanoz widmami fotolu- minescencjami. Samoorganizujace si ˛e kropki kwantowe wytwarzane w trzech róznych˙ procesach na podłozu˙ GaN metod ˛aMOCVD były badane za pomoc ˛a TEM. Zostało stwierdzone, ze˙ podczas wzrostu w niskiej temperaturze nie powstaje warstwa zwilzaj˙ ˛aca.Przykrywanie kropek kwantowych warstw ˛aGaN bez zmiany temperatury pro- cesu prowadziło do otrzymania gładkiej powierzchni, powstawa- nia wydziele´n GaN o strukturze sfalerytu oraz mieszania si ˛e vi indu z galem. Zaobserwowano ze˙ kropki kwantowe zmniejszyły swoje rozmiary i były zrelaksowane w 90 % w wyniku powsta- nia dyslokacji niedopasowania na granicy GaN/InN. G ˛esto´s´c dys- lokacji skorelowano z intensywno´sci˛afotoluminescencji. Dla kropek kwantowych InN przykrywanych GaN przy wyzszych˙ temperatu- rach obrazy wysokorozdzielcze i widma strat energii elektronów wykazały powstanie warstwy InxGa1-xN o zróznicowanej˙ koncen- tracji indu a nawet wydziele´nczystego indu. Niskoenergetyczne widma strat energii elektronów zmierzono dla studni i kropek kwantowych, dla których koncentracja indu została wyznaczona równiez˙ za po´srednictwem metody fazy geome- trycznej. Na podstawie widm wyznaczono z dokładno´sci˛arz ˛edumeV połozenie˙ maksimum absorpcji plazmonowej. Zastosowano opro- gramowywanie Win2k do obliczenia pozycji piku plazmonowego dla InxGa1-xN oraz Al1-xInxN. Wyniki teoretyczne i do´swiadczalne okazały si ˛ew pełni zgodne. vii PUBLICATIONS Some ideas and figures have appeared previously in the following publications: • F. Ivaldi, S. Kret, R. Czernecki, M. Krysko, M. Leszczynski, S. Grzanka, and A. Szczepanska "Impact of thin LT-GaN cap layers on the structural and composi- tional quality of MOVPE grown InGaN quantum wells investigated by TEM" Acta Phys. Pol. A 119 (5), 660-662, 2011 • F. Ivaldi, C. Meissner, J. Domagala, S. Kret, M. Pristovsek, M. Hoegele, and M. Kneissl "Influence of a GaN cap layer on the morphology and the phys- ical properties of embedded self-organized InN quantum dots on GaN(0001) grown by metal-organic vapour phase epitaxy" J. Journ. Appl. Phys. 50, 031004, 2011 • F. Ivaldi, N.A.K. Kaufmann, S. Kret, B. Kurowska, M. Klepka, J. Dabrowski, P. Dluzewski, and N. Grandjean "Effects of the annealing temperature on the structural and electronic properties of MBE grown InGaN/GaN quantum wlls" J. Phys. D 326, 012012, 2011 • S. Kret, F. Ivaldi, M. Zak, A. Feduniewicz-Zmuda, M. Siekacz, G. Cywinski, and C. Skierbieszewski "TEM investigation of a processed InGaN based laser grown by PAMBE on bulk GaN substrate" Phys. Stat. Sol. C 7 (5), 1325-1328, 2010 • S. Kret, F. Ivaldi, K. Sobczak, R. Czernecki, and M. Leszczynski "Inhomogeneities of InGaN/GaN MOVPE multi quantum wells grown with a two temperature process studied by transmission elec- tron microscopy" Phys. Stat. Sol. A 207 (5), 1101-1104, 2010 • N.A.K. Kaufmann, A. Dussaigne, D. Martin, P. Valvin, T. Guillet, B. Gil, F. Ivaldi, S. Kret, and N. Grandjean "Thermal annealing of molecular beam epitaxy-grown InGaN/GaN single quantum well" Semicond. Sci. Technol. 27, 105023, 2012 • M. Pristovsek, A. Kadir, C. Meissner, F. Ivaldi, S. Kret, T. Schwaner, M. Leyer, J. Stellmach, and M. Kneissl ix "Growth mode transition and relaxation of thin InGaN layers on GaN (0001)" J. Crys. Growth 372, 65-72, 2013 x ...by the help of microscopes, there is nothing so small, as to escape our inquiry; hence there is a new visible world discovered to the understanding. — Robert Hook, Micrographia 1655 world’s first mircroscopy book 1 ACKNOWLEDGMENTS This dissertation would not have been possible without the guidance and the help of several individuals who in one way or another con- tributed and extended their valuable assistance in the preparation and completion of this study. Foremost my gratitude to both my supervisor prof. nzw. dr hab. Piotr Dłuzewski˙ and dr hab. Sławomir Kret for their supervision and support throughout the last three years, which enabled me to develop an understanding of the subject. A special reference to dr Jarosław Domagała without whose coop- eration I could not have obtained such relevant data and who has always found time to dedicate to me helping with the interpretation of XRD results. My colleagues at the Institute of Physics of the Polish Academy of Sciences and the international members of the RAINBOW network for the fruitful cooperation and the positive knowledge and
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