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Title: A high-pressure atomic force microscope for imaging in supercritical carbon dioxide

Journal Article · · Review of Scientific Instruments, 82(4):Article No.: 043709
DOI:https://doi.org/10.1063/1.3580603· OSTI ID:1012855

A high-pressure atomic force microscope (AFM) that enables in-situ, atomic scale measurements of topography of solid surfaces in contact with supercritical CO2 (scCO2) fluids has been developed. This apparatus overcomes the pressure limitations of the hydrothermal AFM and is designed to handle pressures up to 100 atm at temperatures up to ~ 350 K. A standard optically-based cantilever deflection detection system was chosen. When imaging in compressible supercritical fluids such as scCO2, precise control of pressure and temperature in the fluid cell is the primary technical challenge. Noise levels and imaging resolution depend on minimization of fluid density fluctuations that change the fluid refractive index and hence the laser path. We demonstrate with our apparatus in-situ atomic scale imaging of a calcite (CaCO3) mineral surface in scCO2; both single, monatomic steps and dynamic processes occurring on the (10¯14) surface are presented. This new AFM provides unprecedented in-situ access to interfacial phenomena at solid-fluid interfaces under pressure.

Research Organization:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL)
Sponsoring Organization:
USDOE
DOE Contract Number:
AC05-76RL01830
OSTI ID:
1012855
Report Number(s):
PNNL-SA-77820; 39924; 40896; 32092; KP1704020; TRN: US1102380
Journal Information:
Review of Scientific Instruments, 82(4):Article No.: 043709, Vol. 82, Issue 4; ISSN 0034-6748
Country of Publication:
United States
Language:
English