Capsule-free fluid delivery and beam-induced electrodeposition in a scanning electron microscope

Abstract

Gold coated borosilicate nanocapillaries are used to locally deliver aqueous, electrolytic CuSO4 solution into the low vacuum chamber of an environmental scanning electron microscope (ESEM). Capillary flow of the liquid is induced by bringing a nanocapillary into contact with a substrate. A microscopic droplet is stabilized by controlling the droplet evaporation rate with the substrate temperature and the pressure of H2O vapor injected into the vacuum chamber. An electron beam is admitted to the droplet through a pressure limiting aperture. Electrochemical reduction of aqueous Cu2+ to solid, high purity, deposited Cu is achieved by biasing the nanocapillary and supplying current by the beam which acts as a virtual cathode and enables electrodeposition on both conductive and insulating substrates. Delivery of liquids into vacuum enables localized, capsule-free beam induced electrochemistry, opening new pathways for direct-write nano and micro-lithography via beam induced electrodeposition.