Measuring Thickness Changes in Thin Films Due to Chemical Reaction by Monitoring the Surface Roughness with In Situ Atomic Force Microscopy

Measuring the changing thickness of a thin film, without a reference, using an atomic force microscope (AFM) is problematic. Here, we report a method for measuring film thickness based on in situ monitoring of surface roughness of films as their thickness changes. For example, in situ AFM roughness measurements have been performed on alloy film electrodes on rigid substrates as they react with lithium electrochemically. The addition (or removal) of lithium to (or from) the alloy causes the latter to expand (or contract) reversibly in the direction perpendicular to the substrate and, in principle, the change in the overall height of these materials is directly proportional to the change in roughness. If the substrate on which the film is deposited is not perfectly smooth, a correction to the direct proportionality is needed and this is also discussed.

[1]  S Kitsunezaki Fracture patterns induced by desiccation in a thin layer. , 1999, Physical review. E, Statistical physics, plasmas, fluids, and related interdisciplinary topics.

[2]  Kevin W. Eberman,et al.  Colossal Reversible Volume Changes in Lithium Alloys , 2001 .

[3]  J. Dahn,et al.  Reaction of Li with Grain‐Boundary Atoms in Nanostructured Compounds , 2000 .

[4]  Martin Winter,et al.  Small particle size multiphase Li-alloy anodes for lithium-ionbatteries , 1996 .

[5]  N. Bonnet,et al.  Correction of surface roughness measurements in SPM imaging , 1998 .

[6]  P. Hansma,et al.  Atomic-Resolution Electrochemistry with the Atomic Force Microscope: Copper Deposition on Gold , 1991, Science.

[7]  J. Dahn,et al.  Mechanically Alloyed Sn‐Fe(‐C) Powders as Anode Materials for Li‐Ion Batteries: I. The Sn2Fe ‐ C System , 1999 .

[8]  J. Haber,et al.  In Situ Atomic Force Microscopy Observation of Change in Thickness of Nickel Hydroxide Layer on Ni Electrode , 1996 .

[9]  E. Kaplan,et al.  An Experimental Study of Cracking Induced by Desiccation , 1994 .

[10]  J. Dahn,et al.  A system for performing simultaneous in situ atomic force microscopy/optical microscopy measurements on electrode materials for lithium-ion batteries , 2001 .

[11]  Tsutomu Miyasaka,et al.  Tin-Based Amorphous Oxide: A High-Capacity Lithium-Ion-Storage Material , 1997 .

[12]  R. Kötz,et al.  Nanoscale thickness changes of nickel hydroxide films during electrochemical oxidation/reduction monitored by in situ atomic force microscopy , 1995 .

[13]  C. Quate The AFM as a tool for surface imaging , 1994 .