Dimple Grinding Coupled with Optical Microscopy for Porosity Analysis of Metallic Coatings.

Dimple grinding is one of the steps used in a common method of preparing samples for transmission electron microscopy (TEM); the TEM sample preparation process also involves ion beam sputtering after the dimpling stage. During dimpling, a spherical depression is machined into the sample, leaving a thicker rim to support and facilitate sample handling. In this paper, an alternative application for dimple grinding is developed; dimple grinding combined with optical microscopy is utilized to quantify internal porosity present within coatings. This technique essentially permits three dimensional porosity quantification across the coating thickness using a simple polishing method which provides analysis of areas larger than those observed during standard cross sectional microscopy. The application of this technique to nine electroless nickel-phosphorus (Ni-P) coatings deposited on Mg substrates is demonstrated. An analysis linking medium P content in the Ni-P coatings and high coating thickness to lower porosity is also performed. The lowest porosity was observed for medium P content coatings (5.2 wt% P), while the largest porosity occurred for the high P content coatings (10.0 wt% P). Porosity levels decreased continuously with increasing coating thickness (from 28 µm to 57 µm).

Preparation of metallized GaN/sapphire cross sections for TEM analysis using wedge polishing.

The tripod polisher has been used successfully in the past, in the preparation of difficult Si-based TEM cross-section specimens. Good TEM specimens, with large electron transparent areas, can be prepared in a relatively short time. In addition, wedge polishing considerably reduces the ion milling time because of the thinness of the final specimen. For metallized GaN on sapphire substrates, there are problems not inherent to Si-based materials: (1) sapphire is a difficult material to thin due to its high hardness and its mechanical instability when thinned below 20 m; (2) delamination of metal layers from the GaN can occur during polishing and/or ion milling; (3) markedly different ion milling rates for the metals and semiconductors. In this paper, wedge polishing has been modified to make it suitable for preparation of metallized GaN/sapphire samples or other metallized semiconductors and ceramics for TEM analysis. Using this method, TEM cross section specimens can be prepared with reasonably large thin areas.

Microstructural and in vitro chemical investigations into plasma-sprayed bioceramic coatings.

Hydroxyapatite (HA) coatings plasma sprayed without and with bond coats (titania, zirconia) onto titanium alloy (Ti6A14V) substrates under both atmospheric and low pressure plasma spray conditions were investigated in terms of their microstructure and their resorption resistance during immersion in simulated body fluid (Hank's balanced salt solution). The microstructures of test samples were characterized using SEM on as-sprayed and leached surfaces and on the corresponding cross sections. Selected coating systems were studied by 2-dimensional secondary ion mass spectroscopy imaging to obtain information on plasma spray induced diffusional processes at the coating interfaces, as well as the spatial distribution of minor and trace elements. Coatings consisting of thin (10-15 microm) titania/zirconia (eutectic ratio) and titania bond coats, combined with a 150- to 180-microm thick HA top coat, yielded peel strengths in excess of 32 N/m, as well as sufficient resorption resistance.