In-situ capped nanocrystalline -Fe2O3, Co3O4, and Cu2O were prepared in 1,4-butanediol in aerobic conditions. X-ray diffraction (XRD)patterns show that the synthesised samples are nanocrystalline cubic oxides with crystallitesizes 9.5 nm, 13.4 nm, and 11 nm, respectively. Raman spectroscopy shows peaks at 350 cm−1, 500 cm−1, and 700 cm−1, indicating that the iron oxide is-Fe2O3; Mössbauer spectroscopy shows the presence of twoFe3+ sites. Transmission electron microscopy images show that the particle sizes of -Fe2O3 and Co3O4 samples are 8.9 nm and 7 nm, respectively. The absence of agglomeration indicates that the synthesised nanoparticles are capped.FT-IR spectra show the presence of an organic moiety in the sample which acts as a capping agent. Thermogravimetry showsthat the capping is stable up to 873 K in -Fe2O3, and up to 400 K in Co3O4. The samples are soluble in water to form stablehydrosols. During synthesis of -Fe2O3 a 6-line ferrihydrite is formed as an intermediate, which is stable in solution up to 473 K, and transforms to -Fe2O3 at 483 K, by rapid dissolution-reprecipitation. In the syntheses of Co3O4andCu2O, no intermediates are formed.
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