The growth of gold nanocrystals prepared by the reduction of tetrachloroauric acid by tetrakis(hydroxymethyl)phosphonium chloride, which allows slow reduction, is investigated by small-angle X-ray scattering and isothermal titration calorimetry in combination with transmission electron microscopy. The growth of the nanocrystals does not follow the diffusion-limited Ostwald ripening but instead follows a sigmoidal rate curve. The activation energy obtained from the temperature-dependent growth study is very small. The heat change associated with the growth is determined for the first time as approximately 10 kcal mol(-1) per 1 nm increase in the nanocrystals' diameter.
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