The Absolute Calibration of a Small-Angle Scattering Instrument with a Laboratory X-ray Source

“…Previous work has established the feasibility of using glassy carbon as a stable SAXS intensity calibration standard, and various glassy (or vitreous) carbons have been recognized as potential intensity calibration standards for SAXS measurements (Dreiss et al, 2006;Fan et al, 2010;Zhang et al, 2010). This is because the glassy carbon microstructure can be controlled depending on the starting polymer from which it is made, and it can produce significant small-angle scattering from its pore structure over a large part of the Q range of interest for SAXS or SANS (Craievich, 1976).…”

Section: Introductionmentioning

confidence: 99%

NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

et al. 2017

Self Cite

View full text Add to dashboard Cite

The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certified Q range, Q = 0.008-0.25 Å À1 , together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. The validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.

show abstract

“…50; Hilgenberg, Malsfeld, Germany) at room temperature. The absolute scattered intensity for all samples was calibrated with distilled water . The absolute scattered intensity was not determined for experiments performed at 45 and 150 °C, and the absolute values for N ·(Δρ) 2 , 〈 A 〉/ V p , and 〈 L 〉 may deviate slightly.…”

Section: Methodsmentioning

confidence: 99%

Following the Kinetics of Barium Titanate Nanocrystal Formation in Benzyl Alcohol Under Near‐Ambient Conditions

Veldhuis

Stawski

Rodriguez

et al. 2018

Small

View full text Add to dashboard Cite

In complex chemical syntheses (e.g., coprecipitation reactions), nucleation, growth, and coarsening often occur concurrently, obscuring the individual processes. Improved knowledge of these processes will help to better understand and optimize the reaction protocol. Here, a form-free and model independent approach, based on a combination of time-resolved small/wide-angle X-ray scattering, is employed to elucidate the effect of reaction parameters (such as precursor concentration, reactant stoichiometry, and temperature) on the nucleation, crystallization, and growth phenomena during the formation of nanocrystalline barium titanate. The strength of this approach is that it relies solely on the total scattered intensity (i.e., scattering invariant) of the investigated system, and no prior knowledge is required. As such, it can be widely applied to other synthesis protocols and material's systems. Through the scattering invariant, it is found that the amorphous-to-crystalline transformation of barium titanate is predominantly determined by the total amount of water released from the gel-like barium hydroxide octahydrate precursor, and three rate-limiting regimes are established. As a result of this improved understanding of the effect of varying reaction conditions, elementary boundary conditions can be set up for a better control of the barium titanate nanocrystal synthesis.

show abstract

The Absolute Calibration of a Small-Angle Scattering Instrument with a Laboratory X-ray Source

Cited by 51 publications

References 27 publications

Investigating Cellular Nanoscale with X-rays

Investigating Cellular Nanoscale with X-rays

NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

Following the Kinetics of Barium Titanate Nanocrystal Formation in Benzyl Alcohol Under Near‐Ambient Conditions

Contact Info

Product

Resources

About