Figure 1

Simultaneous diffraction and SAXS data obtained with high-energy ($E=77\mathrm{k}\mathrm{e}\mathrm{V}$) synchrotron x ray. The sample was heated in vacuum at a heating rate of approximately $10\mathrm{K}/\mathrm{m}\mathrm{i}\mathrm{n}$, reaching the equilibrium temperature of $T=696\mathrm{K}$ at $t=53\mathrm{m}\mathrm{i}\mathrm{n}$. The experimental data were recorded every minute, with an exposure time of 0.5 min, throughout the annealing experiment. (a) Temperature of the sample for $20<t<100\mathrm{m}\mathrm{i}\mathrm{n}$. (b) Kinetic diffraction diagram for $20<t<100\mathrm{m}\mathrm{i}\mathrm{n}$. (c) Diffraction patterns at selected annealing times. Prominent diffraction peaks appeared at $t=40\mathrm{m}\mathrm{i}\mathrm{n}$. (d) Kinetic diagram of SAXS intensity for $20<t<100\mathrm{m}\mathrm{i}\mathrm{n}$ (in log scale). (e) SAXS profiles at selected annealing times. The top axis gives the corresponding length scale ($d=\frac{2\pi }{Q}$) that is being probed.Reuse & Permissions

Figure 2

(a) Integrated diffraction $I_D$ and small angle scattering $I_S$ intensities as a function of time. (b) Evolution of $D_g$ and $\frac{I_D}{D_g^3}$. $D_g$ is a representative particle size determined from a Guinier analysis of the SAS data. For a system consisting of uniform-sized particles, $\frac{I_D}{D_g^3}\propto N$, where $N$ is the number of particles. The flat profile seen for $\frac{I_D}{D_g^3}$ indicates that $N$ is held constant during growth. The values of $I_D$, $I_S$, and $\frac{I_D}{D_g^3}$ have been normalized to unity (dashed lines) at equilibrium ($t>200\min $).Reuse & Permissions