Detection of crystalline phase in cross-section multilayer thin film by High-Resolution Transmission Electron Microscopy

Abstract

High-resolution transmission electron microscopy has proven to be very useful in direct detection of crystalline phases that exist over extremely small volumes, yielding information about structure, orientation, and, under appropriate circumstances, composition. In this paper, we report the detection of a crystalline phase in the tungsten-rich layer of an annealed 7 nm-period tungsten-carbon multilayer produced at the Center for X-Ray Optics at the Lawrence Berkeley Laboratory.The multilayers were prepared by dc magnetron sputtering at floating temperature. The argon sputter gas pressure was 0.0020 torr. Different techniques were employed to produce cross-section and plan-view samples for TEM. For cross-section samples, 70 bilayers of W and C were sputtered on semiconductor-grade Si (111) wafers. For plan-view samples, the substrates on which the multilayer was grown consisted of 3 mm-diameter 300-mesh copper microscope grids, mounted on glass slide with Crystalbond® vacuum adhesive. After a deposition of 4 bilayers of W-C, keeping the same sputtering parameters as those of the Si substrates to guarantee the same layer thicknesses, the glass slide was soaked in acetone to disolve the Crystalbond®, leaving the multilayer spanning the holes of the copper grids. Both the Si-substrate and copper-grid samples were annealed at 500°C for 4 hours under vacuum of 10−6 torr. The annealed Si-substrate sample was then prepared for cross-section by mechanical grinding, and ion milling in a cold stage at 5kV. The cross-section sample was studied in a JEOL JEM 200CX with ultrahigh resolution goniometer, with the eletron beam parallel to the [112] of the Si substrate. The plan-view sample was studied in a Philips 301 operating at 100kV.