ICMCTF2003 Session F4-2: Microstructural, Microanalytical and Imaging Characterization

Monday, April 28, 2003 1:30 PM in Room Royal Palm 4-6

Monday Afternoon

Start	Invited?	Item
1:30 PM	Invited	F4-2-1 TEM Analysis of Thin Films: Specimen Preparation and Correlative Analysis Part 1 R.M. Anderson (Microscopy Today) The successful manufacture of products dependant on modern thin film technology requires a great deal of analytical characterization. Analysis is performed during all phases of the product cycle: development, resolution of parametric problems, yield improvement, identifying yield detractors, and analyzing field returns. TEM and correlative techniques, like Auger analysis and x-ray diffraction are invaluable players in this arena. TEM instrumentation has improved greatly in recent years with the introduction of field emission electron guns, CCD camera detection systems, energy filtering imaging and associated electron energy-loss spectroscopy, lens aberration correctors, and electron holography. All TEM technologies and methods are extraordinarily dependant on TEM specimen preparation. The preparation of clean, very thin (50nm and less), parallel-sided TEM specimens-sometimes with specimen preparation spatial resolutions under 500nm-places enormous demands on technical staff. Often times, it is required to prepare important, one-of-a-kind specimens in very short times (one or two hours or less). These TEM preparation requirements have led to the development of entire suites of preparation tools that barely existed a decade ago. Some preparation methods, like focused ion beam thinning, require instrumentation that rivals the cost of the TEMs themselves. This presentation will discuss these factors and offer examples of TEM analysis, both stand-alone and synergistically correlated with other techniques
2:10 PM		F4-2-3 TEM Analysis of Thin Films: Specimen Preparation and Correlative Analysis Part 2 R.M. Anderson (Microscopy Today)
3:10 PM		F4-2-6 Can Oxygen Stabilize Chromium Nitride? - Characterization of High Temperature Cycled Chromium Oxynitride P. Wilhartitz (Plansee Aktiengesellschaft - AUSTRIA); P. Ramminger (University Innsbruck, Austria) In this study, the influence of oxygen, which was built into chromium nitride during sputter deposition, on the phase formation and structure, was investigated by cyclic heat treatment of the specimens between ambient temperature and 850°C. HT-XRF, EPMA, SIMS, SEM, STEM, EELS, XPS, UPS, FT-IR and CGHE, were used to investigate the compositional and structural changes caused by the heat treatment. The presentation will show that chromium oxynitride can be formed during the film deposition process and that an enhanced oxygen content significantly slows down the recrystallisation of the films at high temperature.
3:30 PM		F4-2-7 Amorphous Carbon Matrix used to Investigate the Pressure Effect on Noble Gases F.C. Marques, R.G. Lacerda, A. Champi, P.F. Barbiere, M.H. Oliveira, Jr. (UNICAMP, Brazil) In this work we report on the study of the local environment of noble gases atoms implanted into an amorphous carbon (a-C) matrix. By intentionally changing the a-C deposition conditions we were able to trap noble gas atoms under different internal pressure (intrinsic stress) ranging from 1 GPa up to 12 GPa. This enables us to investigate the effects of the internal pressure on the implanted noble gases atoms subjected to the highly strained environment of the carbon matrix. Extended x-ray absorption fine spectroscopy (EXAFS) was performed to investigate the interatomic distance of the implanted noble gases as a function of the intrinsic stress of the carbon matrix. The analysis of XANES (x-ray near edge spectroscopy) and the EXAFS indicate the clustering of the implanted noble gas atoms. This finding gives evidence that the formation of noble gases clusters in a solid matrix in induced by the network pressure. A shift o the core level energy was also observed as a function of the carbon matrix pressure.
3:50 PM		F4-2-8 Thin ZnO Nanocomposite Copolymer Films on Si and SiO₂ Surfaces A.A. Iliadis, H.A. Ali, A.V.W. Cresce, P. Kofinas (University of Maryland) The formation of nanocomposite copolymer films with self-assembled ZnO nanoclusters on Si and SiO₂/Si surfaces, is reported. The nanocomposite films were formed using norbornene (majority block), and norbornene-dicarboxilic acid (minority block), with a block repeat ratio of 400 and 50, respectively, to obtain spherical microphase separation of the minority block and hence, a spherical morphology for the metal oxide self-assembled nanoclusters. The introduction of the inorganic precursor to the minority block was achieved at room temperature in the liquid phase by incorporating ZnCl₂ precursor dopant, then solidifying the copolymer and using wet chemical and ozone processing to convert the ZnCl₂ precursor into ZnO, in free-standing and deposited films respectively. The doped copolymer was spin-cast on Si and SiO₂/Si wafers, allowed to solidify, and then treated with ozone to form the ZnO nanoclusters. Fourier transform infrared (FTIR) and x-ray photoemission (XPS) spectroscopy, confirmed the association of the ZnCl₂ with the minority block and the formation of ZnO after treatment with the wet chemical and the ozone process. Transmission electron microscopy (TEM), and atomic force microscopy (AFM), showed the spherical morphology of the ZnO nanoclusters in the free-standing nanocomposite films, with size distribution between 7 and 15 nm, while reactive ion etching using CF4/O₂ gasses to remove the polymer matrix and reveal the ZnO nanoclusters, in the process of prototyping the nanocomposite polymer on the Si surface, showed agglomeration of the nanoclusters into spherical morphologies with significantly larger cluster sizes (diameters ranging between 1 and 2 µm), indicating the need to incorporate cluster size-inhibitors and prevent agglomeration. The process and self-assembly mechanisms for this system as well as the photolithographic patterning of the nanocomposite polymer, its properties and applications, will be discussed.
4:10 PM		F4-2-9 Characterization of TiN and TiAlN Coatings on Rough Surfaces using Focused Ion Beam Milling J.M. Cairney, L.W. Ma, M.J. Hoffman, P.R. Munroe (University of New South Wales, Australia); E.D. Doyle (Swinburne University of Technology, Australia) TiN and TiAlN physical vapor deposition (PVD) coatings are widely used in industry to enhance the life of components in high wear applications. In practice, these coatings are applied to rough, ground surfaces, rather than the smooth, flat surfaces that are usually examined in mechanical property characterisation using techniques such as nanoindentation. The properties of thin film coatings are intricately related to their microstructure. Characterization of the microstructure of coating is normally performed using techniques such as XRD, SEM, TEM, and chemical analysis techniques such as EDS, WDS, EELS and SIMS. The focused ion beam (FIB) miller is a relatively new addition to this list of materials characterization tools. The FIB can be used to prepare and image cross-sections from a coating, allowing direct examination of the cross-section with minimal specimen preparation. In this work, it was also used to prepare electron transparent sections for subsequent examination using transmission electron microscopy (TEM). In the current study, the FIB is used to analyze the structure of TiN and multilayer TiN/TiAlN coatings deposited using either the Balzers method or a cathodic arc process on a number of ground steel substrates. The microstructure, consisting of columnar grains growing perpendicular to the substrate surface is characterized, revealing the grain-growth process. A number of coating defects are observed such as macroparticles and cracking at planes of weakness where columnar grains of differing orientations meet. In the case of the multilayer TiN/TiAlN coatings TEM analysis revealed that directional-columnar grain growth was not interrupted at the compositional interface.