Synthesis of Fe/Ti oxides from a single source alkoxide precursor under inert atmosphere

Journal of the Brazilian Chemical Society

Norwich Research Park, Norwich, England¹  Soares, Jaísa F.¹  Nunes, Giovana G.¹  Camargo, Pedro H. C.¹  Zarbin, Aldo J. G.¹  Sá, Eduardo L. de¹  Universidade de São Paulo, São Carlos, Brazil¹  Evans, David J.¹  Universidade Federal do Paraná, Curitiba, Brazil¹  Tremiliosi-Filho, Germano¹ 

关键词: oxides;    sol-gel;    single source precursor;    inert atmosphere;    electron microscopy;   

DOI  :  10.1590/S0103-50532008000800009

学科分类：化学（综合）

来源: SciELO

【 摘 要 】

The heterometal alkoxide [FeCl{Ti2(OPri)9}] (1) was employed as a single source precursor for the preparation of Fe/Ti oxides under inert atmosphere. Three different synthetic procedures were adopted in the processing of 1, either employing aqueous HNO3 or HCl solutions, or in the absence of mineral acids. Products were characterised by powder X-ray diffractometry, scanning electron microscopy combined with energy dispersive X-ray spectroscopy (SEM/EDS) and Raman, electron paramagnetic resonance (EPR) and Mössbauer spectroscopies. Oxide products contained titanium(IV) and either iron(III) or iron(II), depending on reaction conditions and thermal treatment temperatures. An interesting iron(III)→iron(II) reduction was observed at 1000 oC in the HNO3-containing system, leading to the detection of ilmenite (FeTiO3). SEM/EDS studies revealed a highly heterogeneous metal distribution in all products, possibly related to the presence of a significant content of carbon and of structural defects (oxygen vacancies) in the solids.

【 授权许可】

Unknown