In Situ Tem Study of Reactions in Iron/amorphous Carbon Layered Thin Films

1995 ◽  
Vol 382 ◽  
Author(s):  
Toshio Itoh ◽  
Robert Sinclair
Keyword(s):  
Grain Size ◽  
Amorphous Carbon ◽  
Layered Structure ◽  
Annealing Temperature ◽  
In Situ Tem ◽  
Dc Sputtering ◽  
Transmission Electron ◽  
Average Grain Size ◽  
Deposited Films

ABSTRACTReactions between Fe and amorphous carbon (a-C) below 600ºC have been investigated. In situ annealing in a transmission electron microscopy (TEM) was performed on a-C/Fe/a-C trilayer films deposited by DC sputtering. As-deposited films showed a well defined tri-layered structure and an average Fe grain size of about 50Å. Cementite (Fe3C) grains appeared in the Fe layer by annealing around 300ºC. As the annealing temperature was raised, the number and size of the cementite grains increased. When the annealing temperature reached 500ºC, the Fe layer completely turned into cementite with an average grain size of 1000Å. At this point the film still kept a well defined tri-layered structure even though some parts of the cementitelayer agglomerated. Above 500ºC, the cementite layer started to “move” into the a-C leaving graphite behind. Graphite formed in this process is strongly textured with the (0002) graphite basal planes parallel to the surface of the moving cementite. This process is concluded to be carbide mediated crystallization of a-C, similar to silicide mediated crystallization of silicon in Ni-Si and Pd-Si systems.

In situ TEM Studies of agglomeration of sub-nanometer Ru layers in Ru/C multilayers

1992 ◽  
Vol 50 (1) ◽  
pp. 256-257
Author(s):  
Tai D. Nguyen ◽  
Ronald Gronsky ◽  
Jeffrey B. Kortright
Keyword(s):  
Layered Structure ◽  
Driving Force ◽  
High Energy ◽  
Superior Performance ◽  
In Situ Tem ◽  
Rayleigh Instability ◽  
Practical Applications ◽  
Transmission Electron ◽  
Diffraction Patterns

Nanometer period Ru/C multilayers are one of the prime candidates for normal incident reflecting mirrors at wavelengths < 10 nm. Superior performance, which requires uniform layers and smooth interfaces, and high stability of the layered structure under thermal loadings are some of the demands in practical applications. Previous studies however show that the Ru layers in the 2 nm period Ru/C multilayer agglomerate upon moderate annealing, and the layered structure is no longer retained. This agglomeration and crystallization of the Ru layers upon annealing to form almost spherical crystallites is a result of the reduction of surface or interfacial energy from die amorphous high energy non-equilibrium state of the as-prepared sample dirough diffusive arrangements of the atoms. Proposed models for mechanism of thin film agglomeration include one analogous to Rayleigh instability, and grain boundary grooving in polycrystalline films. These models however are not necessarily appropriate to explain for the agglomeration in the sub-nanometer amorphous Ru layers in Ru/C multilayers. The Ru-C phase diagram shows a wide miscible gap, which indicates the preference of phase separation between these two materials and provides an additional driving force for agglomeration. In this paper, we study the evolution of the microstructures and layered structure via in-situ Transmission Electron Microscopy (TEM), and attempt to determine the order of occurence of agglomeration and crystallization in the Ru layers by observing the diffraction patterns.

In-Situ TEM Observation of Electromigration Damage by Surface or Interface Diffusion in Al and Al Alloy Films

1991 ◽  
Vol 225 ◽  
Author(s):  
C. Y. Chang ◽  
R. W. Vook
Keyword(s):  
Grain Size ◽  
Diffusion Mechanism ◽  
In Situ Tem ◽  
Al Alloy ◽  
Linear Temperature ◽  
Alloy Films ◽  
Interface Diffusion ◽  
Transmission Electron ◽  
Dc Current

ABSTRACTIn-situ transmission electron microscope (TEM) electromigration damage (EMD) tests were performed on pure Al films which were thermally evaporated onto oxidized silicon wafers under different deposition conditions. Three different aluminum alloy films, Al-2wt%Cu, Al-8wt%Cu, and Al-2wt%Cu-lwt%Si were also examined. TEM images were recorded photographically and by a video camcorder. The sample stripes were stressed by a high DC current density (≈1.5 MA/cm2). A linear temperature ramp (5°C/min) was supplied by an external, computer controlled heater. The morphology of EMD-induced voids was found to be strongly dependent on microstructure. In small grain size Al stripes, EMD occurred by the formation of void “fingers” which propagated in an almost random manner. In large grain size Al and Al alloy stripes, the EMD-elongated voids propagated approximately parallel to each other and along the field direction. They were preceded with clearly identifiable local thinning. The thinned regions often had crystallographic edges. Contrary to the commonly held belief that EMD occurs only by a grain boundary diffusion mechanism, the present study clearly shows that surface or interface diffusion was the dominant, latter stage EMD failure mode in large grain size films.

In Situ TEM Studies of Metal–Carbon Reactions

2002 ◽  
Vol 8 (4) ◽  
pp. 288-304 ◽  
Author(s):  
Robert Sinclair ◽  
Toshio Itoh ◽  
Richard Chin
Keyword(s):  
Amorphous Carbon ◽  
Crystallization Process ◽  
Metal Layer ◽  
In Situ Tem ◽  
Scanning Calorimetry ◽  
Transmission Electron ◽  
Precipitation Type ◽  
Silicon And Germanium ◽  
Film Form

The reactions which occur between amorphous carbon and a number of first transition metals (Ti, Cr, Fe, Co, Ni, and Cu) have been studied by transmission electron microscopy (TEM). The materials are in thin-film form with the metal layer sandwiched between thicker carbon layers. In four cases, the predominant reaction is the graphitization of the amorphous carbon, at temperatures well below 800°C. This is brought about by the elements themselves in the case of Co and Ni, and by metastable carbides in the case of Fe (Fe3C) and Cr (Cr3C2−x). The Ti–C and Cu–C systems do not exhibit graphitization. For the former, only TiC is produced up to 1000°C, while the carbon does not react at all with copper. In situ TEM studies show the mechanism to be of the dissolution-precipitation type, which is equivalent to the metal-mediated crystallization process for amorphous silicon and germanium. The heat of graphitization is found to be 18–19 kcal/mol-C by differential scanning calorimetry.

Dopant Diffusion and Grain Growth in Arsenic-Implanted Poly-Si

1987 ◽  
Vol 106 ◽  
Author(s):  
L. R. Zheng ◽  
L. S. Hung ◽  
J. W. Mayer
Keyword(s):  
Grain Size ◽  
Grain Growth ◽  
Amorphous Layer ◽  
Crystal Nucleation ◽  
Initial Size ◽  
Diffusion Behavior ◽  
Transmission Electron ◽  
Average Grain Size ◽  
Si Films

ABSTRACTThe diffusion behavior of arsenic and the grain growth of Si in arsenic doped poly-Si were investigated by MeV4 He2+ backscattering techniques and transmission electron microscopy. By implanting arsenic ions into poly-Si films the surface portion was made amorphous and crystallized upon annealing. In-situ mssurements showed crystal nucleation and growth at temperatures of 650 – 700° C with a dimension comparable to the thickness of the amorphous layer. Annealing at temperatures up to 850°C increased the number of the large grains, but the average grain size did not change significantly. In the unimplanted region grains retained their initial size until 885°C, although implanted arsenic was found to diffuse into this region along grain boundaries. At 885°C penetration of arsenic into the interior of grains caused significant grain growth. We also found that single implants of boron somewhat increased grain size, whereas boron codoped with arsenic appeared to reduce the effect of arsenic doping. These observations support the hypothesis that the enhanced growth rate and the electrical activity of Si near the grain boundary are closely interrelated.

Kinetics and Microstructure of Transiently Annealed Implanted Polycrystalline Silicon Layers

1989 ◽  
Vol 157 ◽  
Author(s):  
J.M.C. England ◽  
P.J. Timans ◽  
R.A. Mcmahon ◽  
H. Ahmed ◽  
C. Hill ◽  
...  
Keyword(s):  
Grain Size ◽  
Polycrystalline Silicon ◽  
Annealing Temperature ◽  
Solid Phase ◽  
Interface Roughness ◽  
Cross Sectional ◽  
Time Resolved ◽  
Microstructural Changes ◽  
Transmission Electron

ABSTRACTMicrostructural changes occurring during the early stages of rapid thermal annealing of polycrystalline silicon bipolar emitters crucially affect the final dopant distribution and hence the performance of these devices. The first stage of annealing is epitaxial regrowth in the solid phase of the layer amorphised by the implantation. In-situ studies using time-resolved reflectivity measurements, combined with cross-sectional transmission electron microscopy of partly annealed structures, have determined the effects of initial grain size, annealing temperature and amorphising species (Si or As) on the rate of regrowth and the microstructural changes which occur during annealing. As the grain size is reduced, the regrowth rate decreases and the interface roughness increases. Arsenic implantation alters the rate of regrowth in such a manner as to produce a smoother interface than that in silicon implanted material.

In situ TEM measurements of the electrical properties of interface dislocations

1992 ◽  
Vol 50 (2) ◽  
pp. 1338-1339
Author(s):  
F. M. Ross ◽  
R. Hull ◽  
D. Bahnck ◽  
J. C. Bean ◽  
L. J. Peticolas ◽  
...  
Keyword(s):  
Electrical Properties ◽  
Electronic Device ◽  
In Situ Tem ◽  
Device Performance ◽  
Misfit Dislocations ◽  
Electrical Characteristics ◽  
Strained Layer ◽  
Transmission Electron ◽  
Interfacial Dislocations

We describe an investigation of the electrical properties of interfacial dislocations in strained layer heterostructures. We have been measuring both the structural and electrical characteristics of strained layer p-n junction diodes simultaneously in a transmission electron microscope, enabling us to correlate changes in the electrical characteristics of a device with the formation of dislocations.The presence of dislocations within an electronic device is known to degrade the device performance. This degradation is of increasing significance in the design and processing of novel strained layer devices which may require layer thicknesses above the critical thickness (hc), where it is energetically favourable for the layers to relax by the formation of misfit dislocations at the strained interfaces. In order to quantify how device performance is affected when relaxation occurs we have therefore been investigating the electrical properties of dislocations at the p-n junction in Si/GeSi diodes.

In situ TEM observations of melting in nanosized eutectic Pb-Cd inclusions embedded in Al

1996 ◽  
Vol 54 ◽  
pp. 986-987
Author(s):  
S. Hagège ◽  
U. Dahmen ◽  
E. Johnson ◽  
A. Johansen ◽  
V.S. Tuboltsev
Keyword(s):  
Electron Microscope ◽  
Melt Spinning ◽  
Ternary Alloys ◽  
Solid Matrix ◽  
Eutectic System ◽  
In Situ Tem ◽  
In Situ Observation ◽  
Orientation Relationships ◽  
Transmission Electron

Small particles of a low-melting phase embedded in a solid matrix with a higher melting point offer the possibility of studying the mechanisms of melting and solidification directly by in-situ observation in a transmission electron microscope. Previous studies of Pb, Cd and other low-melting inclusions embedded in an Al matrix have shown well-defined orientation relationships, strongly faceted shapes, and an unusual size-dependent superheating before melting.[e.g. 1,2].In the present study we have examined the shapes and thermal behavior of eutectic Pb-Cd inclusions in Al. Pb and Cd form a simple eutectic system with each other, but both elements are insoluble in solid Al. Ternary alloys of Al (Pb,Cd) were prepared from high purity elements by melt spinning or by sequential ion implantation of the two alloying additions to achieve a total alloying addition of up to lat%. TEM observations were made using a heating stage in a 200kV electron microscope equipped with a video system for recording dynamic behavior.

Growth kinetics of Al2Cu in an Al-1.5Cu thin film by in Situ TEM

1993 ◽  
Vol 51 ◽  
pp. 1172-1173
Author(s):  
M. Park ◽  
S.J. Krause ◽  
S.R. Wilson
Keyword(s):  
Thin Film ◽  
In Situ Tem ◽  
Collector Plate ◽  
Transmission Electron ◽  
Device Processing ◽  
Corrosion Susceptibility ◽  
Precipitation Phenomena ◽  
Semiconductor Chips ◽  
Kinetics Of

Cu alloying in Al interconnection lines on semiconductor chips improves their resistance to electromigration and hillock growth. Excess Cu in Al can result in the formation of Cu-rich Al2Cu (θ) precipitates. These precipitates can significantly increase corrosion susceptibility due to the galvanic action between the θ-phase and the adjacent Cu-depleted matrix. The size and distribution of the θ-phase are also closely related to the film susceptibility to electromigration voiding. Thus, an important issue is the precipitation phenomena which occur during thermal device processing steps. In bulk alloys, it was found that the θ precipitates can grow via the grain boundary “collector plate mechanism” at rates far greater than allowed by volume diffusion. In a thin film, however, one might expect that the growth rate of a θ precipitate might be altered by interfacial diffusion. In this work, we report on the growth (lengthening) kinetics of the θ-phase in Al-Cu thin films as examined by in-situ isothermal aging in transmission electron microscopy (TEM).

scholarly journals In-Situ TEM Annealing Observation of Helium Bubble Evolution in Pre-Irradiated FeCoNiCrTi0.2 Alloys

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3727
Author(s):  
Huanhuan He ◽  
Zhiwei Lin ◽  
Shengming Jiang ◽  
Xiaotian Hu ◽  
Jian Zhang ◽  
...  
Keyword(s):  
Vacuum Arc ◽  
In Situ Tem ◽  
Face Centered Cubic ◽  
Helium Bubble ◽  
High Entropy ◽  
Helium Bubbles ◽  
Transmission Electron ◽  
Bubble Evolution ◽  
Face Centered

The FeCoNiCrTi0.2 high-entropy alloys fabricated by vacuum arc melting method, and the annealed pristine material, are face centered cubic structures with coherent γ’ precipitation. Samples were irradiated with 50 keV He+ ions to a fluence of 2 × 1016 ions/cm2 at 723 K, and an in situ annealing experiment was carried out to monitor the evolution of helium bubbles during heating to 823 and 923 K. The pristine structure of FeCoNiCrTi0.2 samples and the evolution of helium bubbles during in situ annealing were both characterized by transmission electron microscopy. The annealing temperature and annealing time affect the process of helium bubbles evolution and formation. Meanwhile, the grain boundaries act as sinks to accumulate helium bubbles. However, the precipitation phase seems have few effects on the helium bubble evolution, which may be due to the coherent interface and same structure of γ’ precipitation and matrix.

In-Situ Study of Ti/TiN Stability under Nitrogen Anneal

1999 ◽  
Vol 564 ◽  
Author(s):  
P. W. DeHaven ◽  
K. P. Rodbell ◽  
L. Gignac
Keyword(s):  
Annealing Temperature ◽  
Time Range ◽  
Second Phase ◽  
Transformation Rate ◽  
Transformation Mechanism ◽  
Second Stage ◽  
Transmission Electron ◽  
Reaction Proceeds ◽  
Two Stages

AbstractThe effectiveness of a TiN capping layer to prevent the conversion of α-titantium to titanium nitride when annealed in a nitrogen ambient has been studied over the temperature range 300–700°C using in-situ high temperature diffraction and transmission electron microscopy. Over the time range of interest (four hours), no evidence of Ti reaction was observed at 300°C. At 450°C. nitrogen was found to diffuse into the Ti to form a Ti(N) solid solution. Above 500°C the titanium is transformed to a second phase: however this reaction follows two different kinetic paths, depending on the annealing temperature. Below 600°C. the reaction proceeds in two stages, with the first stage consisting of Ti(N) formation, and the second stage consisting of the conversion of the Ti(N) with a transformation mechanism characteristic of short range diffusion (grain edge nucleation). Above 600°C, a simple linear transformation rate is observed.

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