For characterization of Pd/C catalyst often use methods TEM and HTEM and other methods for determining size of particales palladium, what are other methods?
Hi Hussein Al-Wadhaf
TEM and HRTEM are certainly the most commonly used methods to determine Pd particle size and size distribution. The reason is obvious, these methods are quick and can typically resolve very small Pd nanoparticles (~1 nm or less)
For larger Pd nanoparticles (diameter > 3 nm), powder XRD can be used since the full-width at half maximum (FWHM) of the Pd(111) reflection, once corrected for instrument broadening, can be related to crystallite size according to the Scherrer equation. For such small Pd nanoparticles, crystallite size and particle size are the same thing.
High-resolution solution 1H NMR spectroscopy has been used to characterize the size of Pd dendrimer-encapsulated nanoparticles (DENs) containing 55, 147, 200, or 250 Pd atoms.
J. Am. Chem. Soc., 2009, 131 (41), pp 14634–14635
DOI: 10.1021/ja9065442
EXAFS can also provide meaningful information about Pd cluster size, though the analysis routines are laborious compared with a simple TEM experiment.
J. Phys. Chem. C, 2015, 119 (1), pp 854–861
DOI: 10.1021/jp510730a
There are probably also a wide range of chemical titration and electrochemical experiments that could be used to determine the number of surface Pd atoms in you Pd/C materials. Knowledge of the number of surface Pd atoms to the total number of Pd atoms in your catalyst (which can be calculated from the Pd loading), will give a good feel for the mean Pd particle size in your Pd/C catalyst.
Best regards
Geoff
Hi. You can use XRD for determination of particle Size of your nano structure especially metal nanoparticles. You can use Scherrer equation. And you can determination particle geometry and crystal structure. There are some peaks along Pd metal on the C when you take XRD spectra. And you must use main peak for particle size calculation. This generally Pd (111) that appearing at 40 degree. You can take more information from our studies about depostion.
Best regards
Fatma
As Geoffrey explained , TEM electron microscope/AFM will be useful for particle size analysis. In addition, you can also use Dynamic Light Scattering method to analyse hydrodynamic size of nanoparticle.
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