4. Summary and conclusions
We have described model supports (oxide discs) that are suitable for catalyst sintering studies at temperatures relevant to elevated temperature catalytic processes such as catalytic combustion, automotive exhaust catalysis and propulsion. Nanoparticles on these oxide discs would be otherwise difficult to image using electron microscopy techniques due to excessive charging. As we
show in this work, modern scanning electron microscopy techniques permit low kV imaging on uncoated samples. Both low vacuum SEM as well as high resolution field emission SEMs were utilized in this work. The sintering of palladium on these oxide supports is a complex phenomenon, and the prevailing sintering mechanisms are not fully understood. The model oxide supports allow us to observe the same region of the sample, before and after aging. The major observations from this work are listed below: Pre-treatment in oxygen at 700 C to form PdO, had a significant impact on the initial particle size distribution. Without oxidation, the mean particle size was larger. Deposition of a thin film of carbon to eliminate charging, and subsequent burn off after imaging, had no effect on the resulting particle size distribution. This may be a viable technique to work with samples that show excessive charging in the electron beam. For a similar loading of Pd, the mean particle size on quartz was smaller than that on sapphire. This difference persisted as the sample was aged, indicating that quartz leads to better stabilization of Pd than sapphire. Observations of the same area of the sample before and after aging at 900 C showed that the dominant sintering mechanism was Ostwald ripening (emission of atoms from small particles and capture by the larger particles). Individual nanoparticles were found to have migrated considerable distances before becoming immobile and eventually disappearing via ripening. A 50 nm particle was found to move 30 nm in 24 h.This work demonstrates that bulk oxide discs can be successfully used to study the mobility and dynamics of nanoparticles relevant to high temperature catalytic processes.
4. สรุปและบทสรุปเราได้อธิบายแบบจำลองสนับสนุน (ออกไซด์ดิสก์) ที่เหมาะสมสำหรับการเผาผนึกที่อุณหภูมิเกี่ยวข้องกับกระบวนการตัวเร่งปฏิกิริยาอุณหภูมิสูงเช่นตัวเร่งปฏิกิริยาการเผาไหม้ เร่งปฏิกิริยาไอเสียรถยนต์ และการขับเคลื่อนการศึกษาเศษ เก็บกักบนดิสก์ออกไซด์เหล่านี้จะเป็น difficult มิฉะนั้นภาพที่ใช้เทคนิค microscopy อิเล็กตรอนเนื่องจากการชาร์จมากเกินไป เป็นเรา show in this work, modern scanning electron microscopy techniques permit low kV imaging on uncoated samples. Both low vacuum SEM as well as high resolution field emission SEMs were utilized in this work. The sintering of palladium on these oxide supports is a complex phenomenon, and the prevailing sintering mechanisms are not fully understood. The model oxide supports allow us to observe the same region of the sample, before and after aging. The major observations from this work are listed below: Pre-treatment in oxygen at 700 C to form PdO, had a significant impact on the initial particle size distribution. Without oxidation, the mean particle size was larger. Deposition of a thin film of carbon to eliminate charging, and subsequent burn off after imaging, had no effect on the resulting particle size distribution. This may be a viable technique to work with samples that show excessive charging in the electron beam. For a similar loading of Pd, the mean particle size on quartz was smaller than that on sapphire. This difference persisted as the sample was aged, indicating that quartz leads to better stabilization of Pd than sapphire. Observations of the same area of the sample before and after aging at 900 C showed that the dominant sintering mechanism was Ostwald ripening (emission of atoms from small particles and capture by the larger particles). Individual nanoparticles were found to have migrated considerable distances before becoming immobile and eventually disappearing via ripening. A 50 nm particle was found to move 30 nm in 24 h.This work demonstrates that bulk oxide discs can be successfully used to study the mobility and dynamics of nanoparticles relevant to high temperature catalytic processes.
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