TY - JOUR
T1 - On the thermophoretic sampling and TEM-based characterisation of soot particles in flames
AU - Botero, Maria L.
AU - Akroyd, Jethro
AU - Chen, Dongping
AU - Kraft, Markus
AU - Agudelo, John R.
N1 - Publisher Copyright:
© 2020 Elsevier Ltd
PY - 2021/1
Y1 - 2021/1
N2 - Thermophoretic sampling and TEM imaging are common techniques used to characterise soot particles in flames. In this paper, we present a multi-scale evaluation of operating conditions and methodological aspects of these techniques, and based on our own experimental observations, show how these can influence the characterisation of the particles. Regarding the thermophoretic sampling of soot particles in flames, we evaluated the influence of exposure time, transit times, multiple-insertions, probe design and vibrations in the capture of representative samples, and present a series of recommendations. For the nano-structural characterisation of soot particles using HRTEM combined with fringe analysis we evaluated the influence of microscope alignment and image quality in the mapping of fringes and the calculation of metrics, concluding that the fringe lengths and inter-fringe spacing are very sensitive to particle focus. Also, the parameters used in the image transformation process are critical and require optimisation for different magnifications and microscopes. Finally, the effect of beam damage was studied, confirming a time of approximately 6 min during which both nascent and mature particles can be imaged without noticeable nano-structural damage. The use of lower microscope electron voltage can further minimise the impact of beam damage.
AB - Thermophoretic sampling and TEM imaging are common techniques used to characterise soot particles in flames. In this paper, we present a multi-scale evaluation of operating conditions and methodological aspects of these techniques, and based on our own experimental observations, show how these can influence the characterisation of the particles. Regarding the thermophoretic sampling of soot particles in flames, we evaluated the influence of exposure time, transit times, multiple-insertions, probe design and vibrations in the capture of representative samples, and present a series of recommendations. For the nano-structural characterisation of soot particles using HRTEM combined with fringe analysis we evaluated the influence of microscope alignment and image quality in the mapping of fringes and the calculation of metrics, concluding that the fringe lengths and inter-fringe spacing are very sensitive to particle focus. Also, the parameters used in the image transformation process are critical and require optimisation for different magnifications and microscopes. Finally, the effect of beam damage was studied, confirming a time of approximately 6 min during which both nascent and mature particles can be imaged without noticeable nano-structural damage. The use of lower microscope electron voltage can further minimise the impact of beam damage.
KW - HRTEM
KW - Image analysis
KW - Soot characterisation
KW - TEM
KW - Thermophoretic sampling
UR - http://www.scopus.com/inward/record.url?scp=85091929991&partnerID=8YFLogxK
U2 - 10.1016/j.carbon.2020.09.074
DO - 10.1016/j.carbon.2020.09.074
M3 - Article
AN - SCOPUS:85091929991
SN - 0008-6223
VL - 171
SP - 711
EP - 722
JO - Carbon
JF - Carbon
ER -