Transmission Electron Microscopy study of lead sulfide whiskers

Abstract

This paper describes a transmission electron microscopy (TEM) study of the structure and growth mechanism of lead sulfide (PbS) whiskers. PbS whiskers were grown inside the stainless steel nozzle of a kerosene burner. The nozzle had a 0.5 mm aperture, and was fitted with an Al-spiral coil to filter kerosene impurities. The burner was operated continuously for four weeks at a kerosene pressure of 2-3 bars and a flame temperature of about 350°C before the nozzle clogged. A thick black deposit of fine PbS whiskers was found inside the nozzle.TEM specimens were prepared by ultrasonically suspending the fine black powder in alcohol. The suspended particles were deposited on a perforated carbon film supported on a copper grid, and examined with a JEM-1200EX transmission electron microscope operated at 120kV accelerating voltage. A JEM-4000EX transmission electron microscope was used for high resolution electron microscopy.Fig. 1. shows an EM micrograph of typical PbS whiskers. Each appears to have a high-contrast core encapsulated in a lower contrast shell. The electron diffraction pattern of a single whisker protruding over a hole in the carbon film is shown in Fig. 2.