Fig. 4

‘Solidification-like’ behavior upon heating. a Synchrotron small-angle X-ray scattering (SAXS) profiles for the electrodeposition (ED) Ni₈₂P₁₈ alloy during heating. The inset shows the 3D plot of wide-angle X-ray scattering (WAXS) patterns acquired simultaneously during heating. A rapid development of SAXS intensity is observed above the crystallization temperature of T_x ~ 633 K. Error bars are defined as the standard deviation of photon count. b The turquoise circles are the normalized integrated intensity of WAXS patterns over Q range, 5.5007–5.5056 Å⁻¹. The blue triangles are the normalized integrated intensity of SAXS patterns over Q range, 0.049–0.1 Å⁻¹. The red line is the differential scanning calorimetry (DSC) scan of ED sample heating from room temperature to 700 K. The red dotted lines indicate the transition temperature T_S and crystallization temperature T_x. The heating rate for the simultaneous SAXS/WAXS measurement and the DSC scan is 10 K min⁻¹