Reliable surface area determination of powders and meso/macroporous materials: Small-angle X-ray scattering and gas physisorption

Author(s):  
Carola Schlumberger ◽  
Christian Scherdel ◽  
Martin Kriesten ◽  
Peter Leicht ◽  
Andreas Keilbach ◽  
...  
2018 ◽  
Author(s):  
Jorick Maes ◽  
Nicolo Castro ◽  
Kim De Nolf ◽  
Willem Walravens ◽  
Benjamin Abécassis ◽  
...  

<div> <div> <div> <p>The accurate determination of the dimensions of a nano-object is paramount to the de- velopment of nanoscience and technology. Here, we provide procedures for sizing quasi- spherical colloidal nanocrystals (NCs) by means of small-angle x-ray scattering (SAXS). Using PbS NCs as a model system, the protocols outline the extraction of the net NC SAXS pattern by background correction and address the calibration of scattered x-ray intensity to an absolute scale. Different data analysis methods are compared, and we show that they yield nearly identical estimates of the NC diameter in the case of a NC ensemble with a monodisperse and monomodal size distribution. Extending the analysis to PbSe, CdSe </p> </div> </div> <div> <div> <p>and CdS NCs, we provide SAXS calibrated sizing curves, which relate the NC diameter and the NC band-gap energy as determined using absorbance spectroscopy. In compari- son with sizing curves calibrated by means of transmission electron microscopy (TEM), we systematically find that SAXS calibration assigns a larger diameter than TEM calibration to NCs with a given band gap. We attribute this difference to the difficulty of accurately sizing small objects in TEM images. To close, we demonstrate that NC concentrations can be directly extracted from SAXS patterns normalized to an absolute scale, and we show that SAXS-based concentrations agree with concentration estimates based on absorption spectroscopy.</p></div></div></div>


2012 ◽  
Vol 7 (4) ◽  
pp. 107-116
Author(s):  
Sergey Bardakhanov ◽  
Ludmila Vikulina ◽  
Vladimir Lysenko ◽  
Andrey Nomoev ◽  
Sergey Poluyanov ◽  
...  

The possibility of application of small-angle X-ray scattering (SAXS) for nanopowders analysis was studied. The research for eight silica powders (including four powders obtained by the authors with help of electron accelerator) was conducted. The possibility of application of small angle X-ray scattering for determination of size distribution function of nanoparticles was shown


1992 ◽  
Vol 36 ◽  
pp. 355-372
Author(s):  
George D. Wignall

Scattering technigues have been employed since the beginnings of polymer science to provide information on the spatial arrangements of macromolecules. The first measurements were made in the 1920s and were concerned primarily with the determination of crystal structures via the Bragg lawnλ = 2dsinθ.


2012 ◽  
Vol 31 (2) ◽  
pp. 135-140 ◽  
Author(s):  
Trushar R. Patel ◽  
Raphael Reuten ◽  
Shawn Xiong ◽  
Markus Meier ◽  
Donald J. Winzor ◽  
...  

2013 ◽  
Vol 20 (5) ◽  
pp. 721-728 ◽  
Author(s):  
Alexandr Nasedkin ◽  
Jan Davidsson ◽  
Mont Kumpugdee-Vollrath

Small-angle X-ray scattering has been employed to study how the introduction of paracetamol and acetylsalicylic acid into a liposome bilayer system affects the system's nanostructure. An X-ray scattering model, developed for multilamellar liposome systems [Pabstet al.(2000),Phys. Rev. E,62, 4000–4009], has been used to fit the experimental data and to extract information on how structural parameters, such as the number and thickness of the bilayers of the liposomes, thickness of the water layer in between the bilayers, size and volume of the head and tail groups, are affected by the drugs and their concentration. Even though the experimental data reveal a complicated picture of the drug–bilayer interaction, they clearly show a correlation between nanostructure, drug and concentration in some aspects. The localization of the drugs in the bilayers is discussed.


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