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Focused Ion Beam (FIB) Milling and Automotive Catalysis Aging: A Novel Approach for the Direct Observation of Interfacial and Sub-Surface Chemical and Structural Properties Relevant to Catalyst Aging and Functionality

  • Carl J. Kamp (a1), Alexander G. Sappok (a1) and Victor W. Wong (a1)

Abstract

The combined focused ion beam/scanning electron microscopy/energy dispersive X-ray spectroscopy (FIB/SEM/EDX) system is a novel tool for the automotive catalysis field. Automotive emissions such as SOx, NOx, and particulate matter (PM) are regulated to various extents throughout the world, requiring the use of multiple aftertreatment components such as the diesel particulate filter (DPF), diesel oxidation catalyst (DOC), three-way catalytic converter (TWC), Lean NOx trap (LNT) and selective catalytic reduction (SCR). While these aforementioned aftertreatment components are generally multifunctional and robust in design, thermal and chemical aging over the components’ useful lifetimes results in significantly degraded performance leading to increased engine emissions levels and decreased fuel economy. While the component sizes themselves are generally large (10s of cm to ≈1/2 m), component aging mechanisms usually dominate on the nm-µm scales. In particular, this study has used the FIB/SEM/EDX system to investigate the aging of the diesel particulate filter (DPF) due to engine lubricant-derived inorganic ash accumulation. The FIB/SEM/EDX system has been used in the automotive aftertreatment field for the first time with many surprising and significant findings. Although the samples used in this study are quite different to those typically found in FIB studies, the authors have shown that the FIB/SEM/EDX system is a valuable tool in this research area, especially for the investigation of µm-size intra-particle structure and nm-µm interfacial/sub-surface details around the aged catalyst surface.

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Sappok, A., Rodriguez, R., and Wong, V., “Characteristics and Effects of Lubricant Additive Chemistry on Ash Properties Impacting Diesel Particulate Filter Service Life,” SAE Int. J. Fuels Lubr. 3(1):705722, 2010-01-1213.
Manufacturers of Emission Controls Association (MECA): “Diesel Particulate Filter Maintenance: Current Practices and Experience,” Washington D.C., 2005.
Givens, W., Buck, W., Jackson, A., Kaldor, A. et al. ., “Lube Formulation Effects on Transfer of Elements to Exhaust After-Treatment System Components,” SAE Technical Paper 2003-01-3109, 2003.
Bardasz, E., Cowling, S., Panesar, A., Durham, J. et al. ., “Effects ofLubricant Derived Chemistries on Performance of the Catalyzed DieselParticulate Filters,” SAE Technical Paper 2005-01-2168, 2005, 2005-01-2168.
Sappok, A., Beauboeuf, D., and Wong, V., “A Novel Accelerated Aging System to Study Lubricant Additive Effects on Diesel Aftertreatment System Degradation,” SAE Int. J. Fuels Lubr. 1(1):813827, 2009, 2008-01-1549.
Sappok, A. and Wong, V., “Ash Effects on Diesel Particulate Filter Pressure Drop Sensitivity to Soot and Implications for Regeneration Frequency and DPF Control,” SAE Int. J. Fuels Lubr. 3(1):380396, 2010-01-0811.
Kamp, C. J., Sappok, A. G., Wong, V. Soot and ash deposition characteristics at the catalyst-substrate interface and intra-layer interactions in aged diesel particulate Filters illustrated using focused ion beam (FIB) milling. SAE technical article 2012-01-0836, 2012.

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Focused Ion Beam (FIB) Milling and Automotive Catalysis Aging: A Novel Approach for the Direct Observation of Interfacial and Sub-Surface Chemical and Structural Properties Relevant to Catalyst Aging and Functionality

  • Carl J. Kamp (a1), Alexander G. Sappok (a1) and Victor W. Wong (a1)

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