AVS 59th Annual International Symposium and Exhibition
    In Situ Microscopy and Spectroscopy Focus Topic Tuesday Sessions
       Session IS+AS+BI+ET+GR+NS-TuA

Paper IS+AS+BI+ET+GR+NS-TuA9
In Situ Sub-Micrometer Scale Chemical Imaging with Scanning Transmission X-ray Microscopy

Tuesday, October 30, 2012, 4:40 pm, Room 007

Session: In Situ Studies of Organic and Soft Materials and In Situ Microscopy
Presenter: S.T. Kelly, Lawrence Berkeley National Laboratory
Authors: S.T. Kelly, Lawrence Berkeley National Laboratory
P. Nigge, Lawrence Berkeley National Laboratory
A. Laskin, Pacific Northwest National Laboratory
B. Wang, Pacific Northwest National Laboratory
A. Tivanski, University of Iowa
S. Ghorai, University of Iowa
T. Tyliszczak, Lawrence Berkeley National Laboratory
M.K. Gilles, Lawrence Berkeley National Laboratory
Correspondent: Click to Email

Spatially resolved chemical information on length scales shorter than 50 nm has become crucial in many areas of science and engineering -- from analyzing the chemistry of geological and environmental samples to quantifying the detailed chemical structure of novel materials engineered on the nanoscale. Scanning transmission x-ray microscopy (STXM) allows collection of specific chemical speciation data on these length scales through the acquisition and analysis of near-edge x-ray absorption fine structure (NEXAFS) spectra at each image pixel. However, the full usefulness of the STXM instrument may ultimately be realized in the in situ analysis of chemical transformations by controlling the local sample environment.
In situ STXM/NEXAFS measurements have been made in several ways thus far, ranging from simple to very complex. Introducing gases directly into the microscope chamber is effective, yet the presence of the gas along the entire optical path of the x-rays reduces signal at the detector. Furthermore, gas choice with this configuration is limited to those compatible with the microscope components. Separate in situ reactor cells circumvent these limitations by confining the gaseous environment to a small region immediately around the sample. Several groups have used reactor cells to this end, with reactors ranging widely in complexity -- from simple cells with limited capability to complex systems which require substantial instrument reconfiguration.
Ideally, an in situ reactor for STXM should be capable, flexible, easy to install and configure, and easily fabricated. We have developed a gas phase STXM reactor cell to meet many of these requirements. The reactor mounts directly to the standard STXM sample mount (making installation relatively simple) and contains an integrated sensor to actively measure relative humidity inside the cell for experiments using water vapor. We present here recent results using the reactor cell to examine two different systems. In the first system, we observed the hygroscopic properties of mixed organic/inorganic aerosol particles at increasing levels of relative humidity. In the second system, we monitored carbon dioxide sorption in metal organic framework materials. The advantages afforded by this reactor (and future improvements to it) will enable new scientific discoveries across a wide range of fields.