2005
DOI: 10.1063/1.2137872
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Comparison of extended x-ray absorption fine structure and Scherrer analysis of x-ray diffraction as methods for determining mean sizes of polydisperse nanoparticles

Abstract: Curve fitting of extended x-ray absorption fine structure (EXAFS) spectra, transmission electron microscopy (TEM) imaging, and Scherrer analysis of x-ray diffraction (XRD) are compared as methods for determining the mean crystallite size in polydisperse samples of platinum nanoparticles. By applying the techniques to mixtures of pure samples, it is found that EXAFS correctly determines the relative mean sizes of these polydisperse samples, while XRD tends to be weighted more toward the largest crystallites in … Show more

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Cited by 79 publications
(73 citation statements)
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“…from 46% to 100% in relative measure. This result was consistent with the approximate formula for spherical clusters given by Calvin et al [30]. The value 6.572 neighbours found in EXAFS modelling for both thin films suggested very small clusters (diameter 1-2 nm, less than 100 Ce atoms).…”
Section: Resultssupporting
confidence: 80%
See 1 more Smart Citation
“…from 46% to 100% in relative measure. This result was consistent with the approximate formula for spherical clusters given by Calvin et al [30]. The value 6.572 neighbours found in EXAFS modelling for both thin films suggested very small clusters (diameter 1-2 nm, less than 100 Ce atoms).…”
Section: Resultssupporting
confidence: 80%
“…5. The average number of first Ce neighbours vs. cluster diameter for spherical clusters as counted from the list of atom sites (dots) and calculated by Calvin's formula [30] (solid line). The EXAFS best fit value and uncertainty region for the thin film samples are marked with solid and dotted horizontal lines, respectively.…”
Section: Resultsmentioning
confidence: 99%
“…Such estimates depend on the shape of the model particle and are generally regarded as lower-bound estimates: for our q values and a spherical particle model, they are given in Table 2. The values are consistently smaller than the Debye-Scherrer estimates for a factor between 1.5 and 3; the relation between the different size estimates has been comprehensively discussed by Calvin et al (2005).…”
Section: Discussionmentioning
confidence: 95%
“…The particle sizes obtained from XRD-peak broadening are listed in Table 1. These values, although known to overshoot the average size systematically (Calvin et al 2005), will be used throughout this article for characterization of nanoparticles. Another lower estimate will be obtained below from EXAFS data.…”
Section: Resultsmentioning
confidence: 99%
“…Isochronal annealing was carried out by warming the sample to a series of higher temperatures (T A = 35, 45,55,65,75,95,105,115,125,135,156,200, and 300 K), holding at that temperature for 5 minutes, then cooling back down to 15 K for EXAFS measurements. Heating to and cooling from the T A = 35 K took less than 10 minutes, rising to around 2 hours each direction for the T A = 300 K. Although the EXAFS for each data point for each edge took approximately 1 hour to collect, the measurements lasted over 2.5 days of beamtime due to extra time spent heating and cooling.…”
Section: Methodsmentioning
confidence: 99%