On the stabilizing behavior of zirconia: A Combined experimental and theoretical study

Reactive zirconia powder was synthesized by the complexation of zirconium metal from zirconium hydroxide using a solution of 8-hydroxiquinoline. The kinetics of zirconia crystallization was followed by X-ray diffraction, scanning electron microscopy and surface area measured by the nitrogen adsorption/desorption technique. The results indicated that zirconia with a surface area as high as 100 m²/g can be obtained by this method after calcination at 500°C. Zirconia presents three polymorphic phases (monoclinic, tetragonal and cubic), which are reversibly interconversible. The cluster model Zr₄O₈ and Zr₄O₇ ⁺² was used for a theoretical study of the stabilization process. The ab initio RHF method was employed with the Gaussian94 program and the total energies and the energy gap of the different phases were calculated and compared with the experimental energy gap. The theoretical results show good reproducibility of the energy gap for zirconia.     

A demonstration of melt rate control during VAR of “Cracked” electrodes

A particularly challenging problem associated with vacuum arc remelting occurs when trying to maintain accurate control of electrode melt rate as the melt zone passes through a transverse crack in the electrode. As the melt zone approaches the crack, poor heat conduction across the crack drives the local temperature in the electrode tip above its steady-state value, causing the controller to cut back on melting current in response to an increase in melting efficiency. The difficulty arises when the melt zone passes through the crack and encounters the relatively cold metal on the other side, giving rise to an abrupt drop in melt rate. This extremely dynamic melting situation is very difficult to handle using standard load-cell based melt rate control, resulting in large melt rate excursions. We have designed and tested a new generation melt rate controller that is capable of controlling melt rate through crack events. The controller is designed around an accurate dynamic melting model that uses four process variables: electrode tip thermal boundary layer, electrode gap, electrode mass and melting efficiency. Tests, jointly sponsored by the Specialty Metals Processing Consortium and Sandia National Laboratories, were performed at Carpenter Technology Corporation wherein two 0.43 m diameter Pyromet® 718 electrodes were melted into 0.51 m diameter ingots. Each electrode was cut approximately halfway through its diameter with an abrasive saw to simulate an electrode crack. Relatively accurate melt rate control through the cuts was demonstrated despite the observation of severe arc disturbances and loss of electrode gap control. Subsequent to remelting, one ingot was sectioned in the “as cast” condition, whereas the other was forged to 0.20 m diameter billet. Macrostructural characterization showed solidification white spots in regions affected by the cut in the electrode.     

HRTEM observation of the monoclinic-to-tetragonal m-t) phase transition in nanocrystalline ZrO2

The orientation relations m(100) || t(001), m[001] || t[110]; m(011) || t(100), m[100] || t[001]; m(100) || t(110), m[001] || t[001]; m(013) || t(116), m[001] || t[001] (indices for the primitive tetragonal cell) have been found between the tetragonal (t) and monoclinic (m) domains during the electron irradiation-induced m-t phase transition observed in-situ with HREM within isolated zirconia nanoparticles. Geometric models of the m-t interfaces are proposed.     

Potential for integration of electrophoretic deposition into electronic device manufacture; demonstrations using silver/palladium

A silver palladium (Ag/Pd) alloy powder is used as an example material to illustrate potential applications of electrophoretic deposition (EPD) in electronics manufacturing, in particular the forming of multilayer devices. The dispersion and deposition of the Ag/Pd powder in acetic acid is characterized. It is found that deposition can be explained by the direct action of electrostatic force on individual particles. Depositions of this Ag/Pd powder are then used to demonstrate: forming of a continuous layer on a rigid substrate; forming of continuous layers in laminated and sintered BaTiO₃ multilayers; and incorporation of patterned depositions into a multilayer by either overcasting the patterned deposition with a particulate slip to form a multicomponent tape, or direct lamination of the patterned deposition to a low temperature co-fired ceramic (LTCC) tape. It is shown that electrically conducting layers can be formed at an average thickness of only two times the diameter of the starting powder. Continuous conductor lines thirty times the average diameter of the starting powder were formed.     

Microscale wear of vitrified abrasive materials

The study of bonding hard materials such as aluminium oxide and cubic boron nitride (cBN) and the nature of interfacial cohesion between these materials and glass is very important from the perspective of high precision grinding. Vitrified grinding wheels are typically used to remove large volumes of metal and to produce components with very high tolerances. It is expected that the same grinding wheel be used for both rough and finish machining operations. Therefore, the grinding wheel, and in particular its bonding system, is expected to react differently to a variety of machining operations. In order to maintain the integrity of the grinding wheel, the bonding system that is used to hold abrasive grains in place will react differently to forces that are placed on individual bonding bridges. This paper examines the role of vitrification heat treatment on the development of strength between abrasive grains and bonding bridges, and the nature of fracture and wear in vitrified grinding wheels that are used for precision grinding applications.     

Electrophoretic deposition of monochrome and color phosphor screens for information displays

This paper reviews our research on the electrophoretic deposition (EPD) of phosphors for the processing of monochromatic and color screens for information displays. Our investigation began with the study of the fundamentals of the EPD process for phosphors. The processing variables which enhance the adhesion strength of phosphor deposits were determined. The optical performance of phosphors deposited by EPD was shown to be not affected by the process itself nor by the conditions which enhance phosphor adhesion. Processes developed to produce high-resolution color screens by combining EPD and photolithography techniques are described. Also, a method to electrophoretically deposit phosphor in a thermo-reversible gel from mixtures of poly(butyl methacrylate) and isopropanol was examined.