Energy-dispersive small-angle X-ray scattering with cone collimation using X-ray capillary optics.

Energy-dispersive small-angle X-ray scattering (ED-SAXS) with an innovative design of cone collimation based on an ellipsoidal single-bounce capillary (ESBC) and a polycapillary parallel X-ray lens (PPXRL) had been explored. Using this new cone collimation system, scattering angle 2θ has a theoretical minimum angle related to the mean half-opening angle of the hollow cone beam of 1.42 mrad, and with the usable X-ray energy ranging from 4 to 30 keV, the resulting observable scattering vector q is down to a minimum value of about 0.003 Å-1 (or a Bragg spacing of about 2100 Å). However, the absorption of lower energies by X-ray capillary optics, sample transmission, and detector response function limits the application range to lower energy. Cone collimation ED-SAXS experiments carried out on pure water, Lupolen, and in situ temperature-dependent measurement of diacetylenic acid/melamine micelle solid were presented at three different scattering angles 2θ of 0.18°, 0.70° and 1.18° to illustrate the new opportunities offered by this technique as well as its limitations. Also, a comparison has been made by replacing the PPXRL with a pinhole, and the result shows that cone collimation ED-SAXS based on ESBC with PPXRL was helpful in improving the signal-to-noise ratio (i.e., reducing the parasitic background scattering) than ESBC with a pinhole. The cone collimation instrument based on X-ray capillary optics could be considered as a promising tool to perform SAXS experiments, especially cone collimation ED-SAXS has potential application for the in situ temperature-dependent studying on the kinetics of phase transitions.