Raman spectroscopy investigation of magnetite nanoparticles in ferrofluids

Raman spectroscopy is used to investigate magnetite nanoparticles dispersed in two types of β-cyclodextrin suspensions. An approach is presented for characterization of the magnetic core in liquid surrounding at room temperature and atmospheric pressure. The effect of elevating laser power on the structural stability and chemical composition of magnetite in the ferrofluids is discussed. The data are compared with data from dry by-products from the fluids. Powder samples undergo total phase transition from magnetite to hematite at laser power of 1.95 mW. The same nanoparticles in the fluid undergo transformation at 9 mW, but no hematite positions appear throughout that investigation. The Raman spectra revealed that the main phase of the magnetic core in the fluids is magnetite. That is indicated by a strong and non-diminishing in intensity peak at 670 cm⁻¹. A second phase is present at the nanoparticle’s surface with Raman spectroscopy unveiling maghemite-like and small fractions of goethite-like structures. The Fourier transform infrared spectroscopy investigations confirm deviations in the surface structure and also point to the fact that the oxidation process starts at an early stage after formation of the nanoparticles. The analyses of the infrared data also show that β-cyclodextrin molecules retain their cyclic character and the coating does not affect the oxidation process once the particles are evicted from the fluids. A Mössbauer spectroscopy measurement on a ferrofluidic sample is also presented.