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

The accumulation of soot and lubrication-derived ash particles in a diesel particulate filter (DPF) increases exhaust flow restriction and negatively impacts engine efficiency. Previous studies have described the macroscopic phenomenon and general effects of soot and ash accumulation on filter pressure drop. In order to enhance the fundamental understanding, this study utilized a novel apparatus, that of a dual beam scanning electron microscope (SEM) and focused ion beam (FIB), to investigate microscopic details of soot and ash accumulation in the DPF. Specifically, FIB provides a minimally invasive technique to analyze the interactions between the soot, ash, catalyst/washcoat, and DPF substrate with a high degree of measurement resolution. The FIB utilizes a gallium liquid metal ion source which produces Ga+ ions of sufficient momentum to directionally mill away material from the soot, ash, and substrate layers on a nm-μm scale. As the FIB cuts into the sample, uncovering intra-layer details, the coupled high resolution SEM imaging and energy dispersive x-ray (EDX) analysis provide both morphological and chemical data. This tool was applied to investigate soot and ash accumulation in the DPF, with a specific focus on characterizing interactions between the soot/ash/DPF interfaces, such as soot penetration into the ash layer, as well as soot and ash accumulation in the DPF surface pores. In particular, ash and soot particle size, layer pore structure, and the extent of penetration or intra-layer mixing, are all parameters directly impacting DPF pressure drop, which may be quantified using this technique. The work in this study leveraged existing databases of aged DPFs containing various levels of soot and ash, originating from field trials and controlled laboratory testing. Results obtained with this technique provide a fresh and complementary perspective, as well as additional details useful to understand the macroscopic observations of the combined ash and soot effects on diesel particulate filter pressure drop.

[1]  Andrew M. Minor,et al.  Focused Ion Beam Microscopy and Micromachining , 2007 .

[2]  J. Melngailis,et al.  Focused ion beam induced deposition and ion milling as a function of angle of ion incidence , 1992 .

[3]  E. Bertagnolli,et al.  FIB processing of silicon in the nanoscale regime , 2003 .

[4]  V. Wong,et al.  Characteristics and Effects of Ash Accumulation on Diesel Particulate Filter Performance: Rapidly Aged and Field Aged Results , 2009 .

[5]  V. Wong,et al.  Detailed Chemical and Physical Characterization of Ash Species in Diesel Exhaust Entering Aftertreatment Systems , 2007 .

[6]  A. Kaldor,et al.  Lube Formulation Effects on Transfer of Elements to Exhaust After-Treatment System Components , 2003 .

[7]  Toshitaka Ishizawa,et al.  Investigation into Ash Loading and Its Relationship to DPF Regeneration Method , 2009 .

[8]  H. Dacosta,et al.  Thermal and Chemical Aging of Diesel Particulate Filters , 2007 .

[9]  C. Finney,et al.  Neutron Imaging of Diesel Particulate Filters , 2009 .

[10]  Todd J. Toops,et al.  Nondestructive X-ray Inspection of Thermal Damage, Soot and Ash Distributions in Diesel Particulate Filters , 2009 .

[11]  Alexander Sappok,et al.  Characteristics and Effects of Lubricant Additive Chemistry on Ash Properties Impacting Diesel Particulate Filter Service Life , 2010 .

[12]  G. Gaiser,et al.  Prediction of Pressure Drop in Diesel Particulate Filters Considering Ash Deposit and Partial Regenerations , 2004 .

[13]  Stephen P. Boyd,et al.  Recent Advances in Learning and Control , 2008, Lecture Notes in Control and Information Sciences.

[14]  Souzana Lorentzou,et al.  A Methodology for the Fast Evaluation of the Effect of Ash Aging on the Diesel Particulate Filter Performance , 2009 .

[15]  Jon Orloff,et al.  High‐resolution focused ion beams , 1993 .

[16]  Krishna Aravelli,et al.  Improved Lifetime Pressure Drop Management for Robust Cordierite (RC) Filters with Asymmetric Cell Technology (ACT) , 2007 .

[17]  V. Wong,et al.  Ash Effects on Diesel Particulate Filter Pressure Drop Sensitivity to Soot and Implications for Regeneration Frequency and DPF Control , 2010 .

[18]  J. Melngailis Focused ion beam technology and applications , 1987 .

[19]  Mark E. Law,et al.  Ion beams in silicon processing and characterization , 1997 .

[20]  John Durham,et al.  Effects of Lubricant Derived Chemistries on Performance of the Catalyzed Diesel Particulate Filters , 2005 .

[21]  S. Lewis,et al.  Phosphorous Poisoning and Phosphorous Exhaust Chemistry with Diesel Oxidation Catalysts , 2005 .

[22]  Takamasa Suzuki,et al.  Visualization of Combustion Phenomena in Regeneration of Diesel Particulate Filter , 2003 .

[23]  Shuji Fujii,et al.  Development of Artificial Ash Accelerated Accumulation Test Method , 2010 .

[24]  V. Wong,et al.  A Novel Accelerated Aging System to Study Lubricant Additive Effects on Diesel Aftertreatment System Degradation , 2008 .

[25]  K. Hanamura,et al.  Visualization of Oxidation of Soot Nanoparticles Trapped on a Diesel Particulate Membrane Filter , 2011 .

[26]  Klaus Edinger,et al.  Focused ion beam sputter yield change as a function of scan speed , 1997 .

[27]  C. J. Kamp,et al.  Sensitivity Analysis of Ash Packing and Distribution in Diesel Particulate Filters to Transient Changes in Exhaust Conditions , 2012 .

[28]  Katsunori Hanamura,et al.  Microscopic Visualization of PM Trapping and Regeneration in Micro-Structural Pores of a DPF Wall , 2009 .

[29]  Ampere A. Tseng,et al.  Recent developments in micromilling using focused ion beam technology , 2004 .

[30]  H. Ryssel,et al.  Nanoscale effects in focused ion beam processing , 2003 .

[31]  Robert Puers,et al.  A review of focused ion beam applications in microsystem technology , 2001 .

[32]  S. M. Shahed,et al.  Performance and Regeneration Characteristics of a Cellular Ceramic Diesel Particulate Trap , 1982 .

[33]  J. Ziegler,et al.  SRIM – The stopping and range of ions in matter (2010) , 2010 .

[34]  W. A. Cutler,et al.  Thermal Durability of Wall-Flow Ceramic Diesel Particulate Filters , 2001 .