writer：Dianbin Qin, Jinhui Yu, Guomin Bian, Yonglin Qi, Dongwei Zhang, Xinlin Yang*
keywords：double-shelled microspheres, hollow microspheres, ZrO2/TiO2 microspheres
source：期刊
specific source：Chin. J. Chem., 32 (2), 163-171 (2014). DOI: 10.1002/cjoc.201300676
Issue time：2014年
Double-shelled zirconia/titania (ZrO2/TiO2) hollow microspheres were prepared by the selective removal of the polymer components via the calcination of the corresponding tetra-layer poly(N,N''-methylenebisacryl amide-comethacrylic acid) (P(MBA-co-MAA))/Zr(OH)4/poly(ethyleneglycol dimethacrylate-co-methacrylic acid) (P(EGDMAco-MAA))/TiO2 hybrid microspheres. These tetra-layer microspheres were synthesized by the combination of the distillation copolymerization of N,N′-methylenebisacryl amide-co-methacrylic acid (MBA) or ethyleneglycol dimethacrylate (EGDMA) crosslinker and methacrylic acid (MAA) for the preparation of polymer core and thirdlayer as well as the controlled sol-gel hydrolysis of inorganic precursors for the construction of zirconium hydroxide
(Zr(OH)4) and titania (TiO2) layers. The thicknesses of zirconia and titania shell-layers were conveniently controlled via varying the feed of zirconium n-butoxide (Zr(OBu)4) and titanium tetrabutoxide (TBOT) during the sol-gel hydrolysis, while the sizes of polymer layers were tuned through a multi-stage distillation precipitation copolymerization.
The structure and morphology of the resultant microspheres were characterized by transmission electron microscopy (TEM), X-ray diffractometer (XRD), X-ray photoelectronic spectroscopy (XPS), and thermogrametric analysis (TGA).