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Changes in microstructure of Zr, Ti, and Ti-6%Al-%V resulting from ion-beam sputtering used to prepare samples for transmission electron microscopy have been correlated with hydrogen absorption. Zr was particularly sensitive to this phenomenon, resulting in extensive hydride formation in thin foil samples. Hydrogen enrichment extending to several micrometers in depth could also be produced in bulk samples in a few hours of sputtering. The performance of various sputtering units in different configurations has been examined. It is concluded that hydride formation appears to be caused primarily by the presence of hydrocarbons, for example, from the backstreaming of diffusion pump oil, in the residual vacuum background of the sputtering chamber.

The article describes the design, construction and performance of a new bench top instrument for high speed ion beam thinning and polishing of materials. In this system, the combination of very low angle ion milling and powerful ion guns has led to the rapid production of high quality TEM specimens. The main subassemblies are (1) a work chamber (2) gas control system (3) vacuum system and (4) electrical system. The work chamber consists of a pair of newly designed Penning type ion guns and Faraday cups to measure ion currents. The Whisperlok™ mechanism provides specimen rotation, pneumatically driven airlock for very fast specimen exchange and transmission/reflection illumination for specimen viewing. The ion guns are mounted to deliver a nominal, 4° milling angle on the specimen surface with precision alignment of ±2° about horizontal and vertical axes. The actual thinning is undertaken from one side using a single, post-type specimen holder which minimizes the specimen heating and contamination. The ion beam current of each gun can be individually optimized by varying the flow rate of the ionizing gas. The main chamber is evacuated by diaphragm and molecular drag pumps to produce a clean, dry vacuum in the 10−6 Torr range. The discharge and accelerating voltages required for the operation of each gun are provided by a dual high voltage power supply capable of delivering ion energies in the range; 1 keV to 6keV. TEM micrographs of typical ion polished specimens of semiconductors, metals, ceramics and composites are included to illustrate the performance of the instrument.

Chemically assisted ion beam etching (CAIBE) is widely practiced in the semiconductor industry. In the electron microscopy field, the CAIBE technique offers a new method for preparing specimens that are difficult to make by conventional inert gas milling techniques, e.g. indium containing type III-V compound semiconductors. CAIBE employs a collimated, molecular beam of a reactive species, e.g. iodine in combination with a conventional inert gas fast atom beam for thinning TEM specimens. CAIBE should not be confused with reactive ion beam etching (RIBE) which takes a chemically active species (e.g. iodine) and converts it into a beam of fast ions directed at the sample. CAIBE has three major advantages over (RIBE): i) corrosion of the ion gun components does not occur, ii) much smaller quantities of reactive gas are required and hence pump maintenance and pollution problems are minimized, iii) a wider range of chemicals may be used. Superior results are obtained if CAIBE is done on only one side of the specimen at a time. This is achieved using a new type of specimen holder post which enables very low angle milling and minimizes specimen contamination by sputtering from the holder. This new technique is described and results from iodine CAIBE milling, iodine RIBE milling and argon ion milling are compared for InP, InSb and GaAs as well as metals like tungsten. Also, the beneficial effects of very low angle (∼1°) argon ion milling in preparing specimens of silicide containing Si based IC wafers is reported.

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