Reduction of NiO to Ni in Nanocrystalline Composite NiO/Ce0.9Gd0.1O2-δ Porous Thin Films: Microstructure Evolution Through in Situ Impedance Spectroscopy

ABSTRACTThe microstructural changes that occur during the reaction of sputter-deposited Nb/Al and Ti/Al multilayer thin-films with bilayer thicknesses ranging from 10 nm to 333 nm have been studied. The films were deposited with an overall stoichiometry of XAl3 (X = Nb,Ti) and subsequently annealed to different stages of the reaction in a differential scanning calorimeter (DSC). Data obtained from cross-sectional transmission electron microscopy (XTEM), and in situ synchrotron X-ray diffraction (XRD) experiments have provided evidence for a two-stage reaction mechanism for the formation of NbAl3. Microscopy results from a film with a bilayer period of 333 nm showed a microstructure that was consistent with two-dimensional growth in the plane of the interface. A uniform, 10 nm thick continuous layer of the product phase was formed followed by growth normal to the interface that initially consisted of larger, faceted grains. By the end of the reaction, an equiaxed NbAl3 grain structure was observed. High resolution elemental mapping using a scanning transmission electron microscope (STEM) revealed penetration of Nb into the Al layer and enhanced growth in regions where Al grain boundaries intersected the interface. Characterization of microstructure evolution in the Ti/Al system was complicated by the formation of two metastable structures consisting of cubic Ll2 followed by tetragonal DO23, and finally the equilibrium, tetragonal DO22 structure. However, the metastable phase transition temperatures were clearly isolated using the in situ XRD technique.

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Nucleation and Early Growth of Sputtered thin Films

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100069570 ◽

1970 ◽

Vol 28 ◽

pp. 516-517

Author(s):

Dudley M. Sherman ◽

Thos. E. Hutchinson

Keyword(s):

Thin Films ◽

Electron Beam ◽

Ion Beam ◽

Ion Source ◽

Water Cooling ◽

Stages Of Growth ◽

Lens Assembly ◽

Microscope Technique ◽

Ion Beam Sputter Deposition

The in situ electron microscope technique has been shown to be a powerful method for investigating the nucleation and growth of thin films formed by vacuum vapor deposition. The nucleation and early stages of growth of metal deposits formed by ion beam sputter-deposition are now being studied by the in situ technique.A duoplasmatron ion source and lens assembly has been attached to one side of the universal chamber of an RCA EMU-4 microscope and a sputtering target inserted into the chamber from the opposite side. The material to be deposited, in disc form, is bonded to the end of an electrically isolated copper rod that has provisions for target water cooling. The ion beam is normal to the microscope electron beam and the target is placed adjacent to the electron beam above the specimen hot stage, as shown in Figure 1.

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Epitaxy and texture analysis of Bi-Sr-Ca-Cu-O thin films on (100) MgO using Transmission Electron Microscopy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100173479 ◽

1990 ◽

Vol 48 (4) ◽

pp. 68-69

Author(s):

J. T. Sizemore ◽

D. G. Schlom ◽

Z. J. Chen ◽

J. N. Eckstein ◽

I. Bozovic ◽

...

Keyword(s):

Electron Microscopy ◽

Thin Films ◽

Transmission Electron Microscopy ◽

Critical Currents ◽

Unit Cell ◽

X Ray Diffraction ◽

Cell Axis ◽

Transmission Electron ◽

Synthesis Procedure

Investigators observe large critical currents for superconducting thin films deposited epitaxially on single crystal substrates. The orientation of these films is often characterized by specifying the unit cell axis that is perpendicular to the substrate. This omits specifying the orientation of the other unit cell axes and grain boundary angles between grains of the thin film. Misorientation between grains of YBa2Cu3O7−δ decreases the critical current, even in those films that are c axis oriented. We presume that these results are similar for bismuth based superconductors and report the epitaxial orientations and textures observed in such films.Thin films of nominally Bi2Sr2CaCu2Ox were deposited on MgO using molecular beam epitaxy (MBE). These films were in situ grown (during growth oxygen was incorporated and the films were not oxygen post-annealed) and shuttering was used to encourage c axis growth. Other papers report the details of the synthesis procedure. The films were characterized using x-ray diffraction (XRD) and transmission electron microscopy (TEM).

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The use of transmission and analytical electron microscopy in studying reactions and phase transformations in thin film

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100150046 ◽

1993 ◽

Vol 51 ◽

pp. 842-843

Author(s):

K. Barmak

Keyword(s):

Thin Film ◽

Thin Films ◽

Phase Transformations ◽

Analytical Electron Microscopy ◽

Ex Situ ◽

Multilayer Thin Films ◽

Absolute Concentration ◽

Analytical Electron ◽

Deposition Step

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.

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