Observation of Crystallization, Precipitation, and Phase Transformation Phenomena in Si Rich Titanium Silicide Thin Films

1995 ◽  
Vol 398 ◽  
Author(s):  
A. Domenicucci ◽  
G. Gifford ◽  
L.A. Clevenger

ABSTRACTCrystallization, precipitation, and phase transformation phenomena were observed in titanium suicide thin film samples during in situ heating experiments in a transmission electron microscope. The as-deposited TixSiy films were 110 nm in thickness with a composition of 1 Ti to 2.33 Si. Crystallization of the C49 phase was followed isothermally near the sputter deposition temperature. The movement of individual grain boundaries was recorded so that a “velocity of crystallization” could be calculated. The precipitation of excess silicon from the C49 phase was first observed in the 650°C to 750°C temperature range. The precipitates were predominantly of the incoherent type, with a smaller number existing at the grain boundaries. Ostwald ripening then occurred up to the C49 to C54 phase transformation which was accompanied by a dramatic increase in grain size. Grain boundary movement during the phase transformation was such that large precipitates, which were originally at C49-C49 boundaries, ended up within resulting C54 crystals. Many of these larger precipitates were found to exist as epitaxial “islands” at the TiSi2/Si substrate interface.

2005 ◽  
Vol 20 (7) ◽  
pp. 1808-1813 ◽  
Author(s):  
X.-G. Ma ◽  
K. Komvopoulos

Transmission electron microscopy (TEM) and nanoindentation, both with in situ heating capability, and electrical resistivity measurements were used to investigate phase transformation phenomena and thermomechanical behavior of shape-memory titanium-nickel (TiNi) films. The mechanisms responsible for phase transformation in the nearly equiatomic TiNi films were revealed by heating and cooling the samples inside the TEM vacuum chamber. Insight into the deformation behavior of the TiNi films was obtained from the nanoindentation response at different temperatures. A transition from elastic-plastic to pseudoelastic deformation of the martensitic TiNi films was encountered during indentation and heating. In contrast to the traditional belief, the martensitic TiNi films exhibited a pseudoelastic behavior during nanoindentation within a specific temperature range. This unexpected behavior is interpreted in terms of the evolution of martensitic variants and changes in the mobility of the twinned structures in the martensitic TiNi films, observed with the TEM during in situ heating.


2007 ◽  
Vol 26-28 ◽  
pp. 1199-1202
Author(s):  
Se Ahn Song ◽  
Wei Zhang ◽  
Hong Sik Jeong ◽  
Jin Gyu Kim ◽  
Youn Joong Kim

Phase transformation and crystal growth behavior of Ge2Sb2Te5 were investigated systematically by means of in situ heating (from room temperature to 500 oC) of amorphous Ge2Sb2Te5 alloy in a high voltage electron microscope with real-time monitoring. Large-scale crystallization occurred to amorphous Ge2Sb2Te5 around 200 oC. Large crystal growth developed on heating from 200 oC to 400 oC, and single crystalline grains grew up to 150 nm. Eventually the onset of partial melting of thin Ge2Sb2Te5 foil was at 500 oC and liquid Ge2Sb2Te5 was observed for the first time by high-resolution transmission electron microscopy. Hexagonal Ge2Sb2Te5 phase remains after a subsequent cooling.


Author(s):  
Mihaela Albu ◽  
Bernd Panzirsch ◽  
Hartmuth Schröttner ◽  
Stefan Mitsche ◽  
Klaus Reichmann ◽  
...  

Powder and SLM additively manufactured parts of X5CrNiCuNb17-4 maraging steel were systematically investigated by electron microscopy to understand the relationship between the properties of the powder grains and the microstructure of the printed parts. We prove that satellites, irregularities and superficial oxidation of powder particles can be transformed into an advantage through the formation of nanoscale (AlMnSiTiCr)-oxides in the matrix during the printing process. The nano-oxides showed extensive stability in terms of size, spherical morphology, chemical composition and crystallographic disorder upon in situ heating up to 950°C in the scanning transmission electron microscope. Their presence thus indicates a potential for oxide-dispersive strengthening of this steel, which may be beneficial for creep resistance at elevated temperatures. The nucleation of copper clusters and their evolution into nanoparticles as well as the precipitation of Ni and Cr particles upon in situ heating have as well been systematically documented.


2008 ◽  
Vol 1066 ◽  
Author(s):  
Ram Kishore ◽  
Renu Sharma ◽  
Satoshi Hata ◽  
Noriyuki Kuwano ◽  
Yoshitsuga Tomokiyo ◽  
...  

ABSTRACTThe interaction of amorphous silicon and aluminum films to achieve polycrystalline silicon has been investigated using transmission electron microscope equipped with in-situ heating holder. Carbon coated nickel grids were used for TEM studies. An ultra high vacuum cluster tool was used for the deposition of a ∼50nm a-Si films and a vacuum deposition system was used to deposit a ∼50nm Al films on a-Si film. The microstructural features and electron diffraction in the plain view mode were observed with increase in temperature starting from room temperature to 275 °C. The specimen was loaded inside TEM heating holder. The temperature was measured and kept constant for 5 minutes during which the microstructure at fixed magnification of X63K was recorded and the electron diffraction pattern of the same area was also recorded. The temperature was then increase and fixed at desired value and microstructure and EDP were again recorded. The temperatures used in this experiment were 30, 100, 150, 200, 225, 275°C. A sequential change in microstructural features and electron diffraction pattern due to interfacial diffusion of boundary between Al and amorphous Si was investigated. Evolution of polycrystalline silicon with randomly oriented grains as a result of a-Si and Al interaction was revealed. After the in-situ heating experiment the specimen was subjected to high resolution TEM and EDS investigations after removing the excess Al. The EDS analysis of the crystallized specimen was performed to locate the Al distribution in the crystallized silicon. These studies show that the Al induced crystallization process can be used to prepare polycrystalline as well as nanocrystalline silicon by controlling the in-situ annealing parameters. The investigations are very useful as the nanocrystalline silicon is being investigated for its use in developing high efficiency silicon solar structures.


1995 ◽  
Vol 404 ◽  
Author(s):  
Kalpana S Katti ◽  
Maoxu Qian ◽  
Mehmet Sarikaya

AbstractIn this work a transmission electron microscopy (TEM) technique was used in obtaining local dielectric properties calculated from optical parameters for dynamic investigation of the effect of cubic to tetragonal phase transformation in barium titanate. In order to obtain in situ local dielectric during phase transformation, Kramers-Kronig relations were applied using the transmission electron energy loss (EELS) measurements. The optical excitations in the EELS spectra were consistent with the band structure results. The Re (1/ε) (real part of the dielectric function) obtained from the energy loss data indicated a change at the phase transformation. A broadening of the valence plasmon excitation suggested an order-disorder nature to the cubic to tetragonal transformation. In situ electron energy loss near edge structure (ELNES) studies from 500–700 eV energy range near the O-K edge exhibited a pre-edge feature that is associated with the Ti-L1, edge which further indicates an order-disorder nature to the phase transformation. The significance of the results is discussed.


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