Characterization of reactive phase formation in sputter-deposited Ni/Al multilayer thin films using TEM

Author(s):  
G. Lucadamo ◽  
K. Barmak ◽  
C. Michaelsen

The subject of reactive phase formation in multilayer thin films of varying periodicity has stimulated much research over the past few years. Recent studies have sought to understand the reactions that occur during the annealing of Ni/Al multilayers. Dark field imaging from transmission electron microscopy (TEM) studies in conjunction with in situ x-ray diffraction measurements, and calorimetry experiments (isothermal and constant heating rate), have yielded new insights into the sequence of phases that occur during annealing and the evolution of their microstructure.In this paper we report on reactive phase formation in sputter-deposited lNi:3Al multilayer thin films with a periodicity A (the combined thickness of an aluminum and nickel layer) from 2.5 to 320 nm. A cross-sectional TEM micrograph of an as-deposited film with a periodicity of 10 nm is shown in figure 1. This image shows diffraction contrast from the Ni grains and occasionally from the Al grains in their respective layers.

1981 ◽  
Vol 10 ◽  
Author(s):  
L. J. Chen ◽  
J. W. Mayer ◽  
K. N. Tu

Transmission electron microscopy has been applied to study the formation and structure of epitaxial NiSi2 and CoSi2 thin films on silicon. Bright field and dark field imaging reveal the interface planes of faceted silicides through the strain contrast, analogous to the contrast of the precipitate-matrix interface of coherent or semicoherent precipitates. Superlattice dark field imaging depicts the distribution of twin-related and epitaxial silicides in these systems. { 111 } interfaces were found to be more prominent than {001} interfaces. Twin-related silicides were observed to cover more area on the substrate silicon than epitaxial silicides did.In situ annealing of nickel and cobalt thin films on silicon provides a unique means of investigation of the transformation from polycrystalline to epitaxial silicides. The NiSi2 transformation was found to be very rapid at 820°C, whereas the CoSi2 transformation appeared to be very sluggish. Furnace annealing confirmed that only a small fraction of CoSi2 transforms to epitaxial CoSi2 after annealing at 850°C for 4h.Diffraction contrast analysis has been applied to interfacial dislocations of epitaxial NiSi2/Si and CoSi2/Si systems. The dislocations were found to be of edge type with ⅙<112> and ½<110> Burgers' vectors. The average spacings are close to their respective theoretically predicted values.


1995 ◽  
Vol 398 ◽  
Author(s):  
K. Barmak ◽  
S. Vivekanand ◽  
F. Ma ◽  
C. Michaelsen

ABSTRACTThe formation of the first phase in the reaction of sputter-deposited Nb/Al multilayer thin films has been studied by power-compensated and heat-flux differential scanning calorimetry, x-ray diffraction and transmission electron microscopy. The modulation periods of the films are in the range of 10-500 nm. Both types of calorimetrie measurements, performed at a constant heating rate, show the presence of two peaks (A and B) for the formation of the single product phase, NbAl3. Isothermal calorimetrie scans show that peak A is associated with a nucleation and growth type transformation. The formation of NbAl3 is thus interpreted as a two-stage process of nucleation and lateral growth to coalescence (peak A) followed by normal growth until the consumption of one or both reactants (peak B). Transmission electron microscopy investigations of samples annealed into the first stage of NbAl3 formation show the presence of this phase at the Nb/Al interface and its preferential growth along the grain boundaries of the Al layer. The latter highlights the role of reactant phase grain structure in product phase formation.


1995 ◽  
Vol 382 ◽  
Author(s):  
K. Barmak ◽  
C. Michaelsen ◽  
R. Bormann ◽  
G. Lucadamo

ABSTRACTWe have investigated reactive phase formation in magnetron sputter-deposited Ni/Al multilayer thin films with a 3:1 molar ratio and periodicities ranging from 2.5-320 nm. In addition, we studied the transformation of a codeposited film of the same composition. We find that an amorphous phase has already formed during deposition, and that the extentof formation of this phase increases with decreasing periodicity. The first crystalline phase then nucleates from this amorphous phase upon annealing. The formation of the amorphous phase considerably reduces the driving force and explains why during subsequent reactions nucleation kinetics become important. We obtain Ni2Al9 as the first product phase during heat treatment in some cases before NiAl3 occurs. For films with modulation periods larger than 40 nm, formation of NiAI3 is a two stage process as reported earlier, with the first stage being due to nucleation and growth to coalescence of NiAl3 grains, and the second stage being the growth of NiA13 normal to the initial interface until the reactant phases are consumed.


1999 ◽  
Vol 14 (4) ◽  
pp. 1645-1652 ◽  
Author(s):  
Toshiki Shimizu ◽  
Masaki Tsuji ◽  
Shinzo Kohjiya

Thin films of polychloroprene (CR; Neoprene-W) were made by casting its solution (2.0 wt%) in benzene onto the water surface, and some of them were stretched by a desired amount of strain (ε) in their “molten” state. The specimens thus prepared were then crystallized and examined by transmission electron microscopy. Morphological observations in bright- and dark-field imaging modes and selected-area electron diffraction analysis revealed directly that filamentous entities observed in the bright-field image are the edge-on lamellar crystals. It was, therefore, confirmed that the morphological results obtained from the thin specimens of CR without any electron staining are basically in accord with those reported so far for the OsO4-stained thin films of CR.


1995 ◽  
Vol 403 ◽  
Author(s):  
Kuan-Lun Cheng ◽  
Chih-Chien Liu ◽  
Chung-Min Fu ◽  
Huang-Chung Cheng ◽  
Chiapyng Lee ◽  
...  

AbstractPolycrystalline β-SiC, with grain size up to 0.2 μm, was grown on silicon substrate by electron cyclotron resonance chemical vapor deposition (ECR-CVD) from SiH4/CH4/H2 at 178–500 °C. The nucleation process and surface structure of polycrystalline SiC were investigated via observing the film surface by atomic force microscopy (AFM). Reaction species which promote polycrystalline SiC was in-situ monitored by quadruple mass spectrum analysers during deposition process, which is crucial for the control of polycrystalline SiC growth. The microstructure of SiC films were inspected by bright-field imaging, dark-field imaging, and electron diffraction in cross-sectional transmission electron microscopy. This paper will also discuss the key parameters for the nucleation and growth of polycrystalline β-SiC at very low temperature in ECR-CVD system.


2002 ◽  
Vol 91 (12) ◽  
pp. 9575 ◽  
Author(s):  
G. Lucadamo ◽  
K. Barmak ◽  
C. Lavoie ◽  
C. Cabral ◽  
C. Michaelsen

1988 ◽  
Vol 140 ◽  
Author(s):  
Michael R. Hilton ◽  
Paul D. Fleischauer

AbstractThe relationship between the morphologies and crystal structures of sputter-deposited MoS2 films and their lubricating capabilities is discussed. In particular, aspects of plastic deformation processes are presented. Scanning elecron microscopy (top surface and cross sectional), transmission electron microscopy (lattice imaging and dark field), and x-ray diffraction techniques were used to characterize film structure. The asdeposited morphology, which can be described in terms of zone models, was found to influence the initial nature of the wear debris and the loadbearing capabilities of the films. In many cases a highly deformed region confined to the surface of the films was found. Applied stress was found to reorient crystallites and to induce crystallization, with the degree of both processes being related to the initial structure of the film. Criteria are presented for selecting the film type and preparation conditions to fit various applications.


1998 ◽  
Vol 4 (S2) ◽  
pp. 636-637
Author(s):  
K. Dovidenko ◽  
S. Oktyabrsky ◽  
J. Narayan

High-resolution transmission electron microscopy (HRTEM), multislice image simulation and multiple dark field TEM imaging techniques have been used to investigate the structure of extended defects in AlN and GaN thin films grown on (0001) α-Al2O3 by metal-organic chemical vapor deposition (MOCVD). AlN layers were grown directly on the (0001) sapphire. In the case of GaN thin films, 300-500 Å AlN buffer was deposited first.Cross-sectional TEM revealed the presence of domain boundaries in these Ill-nitride films. In this study we investigated these defects by multiple dark field imaging technique and proved some of them to be IDBs lying in planes. The multiple dark field images of several adjacent domains of AlN film are shown in Fig. 1 (a, b). The images were obtained exactly in [110] zone of AlN using (0002) and (000) reflections.


2003 ◽  
Vol 18 (1) ◽  
pp. 195-200 ◽  
Author(s):  
David E. Ruddell ◽  
Brian R. Stoner ◽  
Jeffrey Y. Thompson

Transmission electron microscopy (TEM) was used to investigate the structural properties of sputter-deposited yttria-stabilized zirconia (YSZ) thin films. YSZ films were deposited over a range of temperatures and background oxygen levels. Additionally, a multilayered structure was produced by cyclic application of a substrate bias. Plan-view TEM showed that temperature and oxygen levels did not have a significant effect on grain size but did alter the phases present in the thin films. Cross-sectional TEM showed the development of texture in the multilayer film, both within the individual layers and in the entire film.


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