The microwave cavity perturbation (MCP) technique is used to identify the transition from magnetite (Fe3O4) to the meta-stable form of maghemite (γ-Fe2O3). In this study Fe3O4 was annealed at temperatures from 60 to 300 °C to vary the oxidation. Subsequent to annealing, the complex permittivity and magnetic permeability of the iron oxide powders were measured. The transition to γ-Fe2O3 was corroborated with x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS) and vibrating sample magnetometry (VSM). XRD, XPS and VSM implied that the starting powder was consistent with Fe3O4 and the powders annealed at more than 200 °C were transitioning to γ-Fe2O3. The MCP measurements gave large differences in both complex permittivity and magnetic permeability of the two phases in the frequency range of 2.5-10.2 GHz. Magnetic permeability decreased with annealing temperature, though magnetic losses showed frequency dependent behaviour. Complex permittivity measurements showed a large decrease in both dielectric constant and losses at all measurement frequencies, as well as a prominent loss peak centred around the phase transition temperatures. We interpret the loss peak as being a consequence of field effects due to an intermediate multi-phase mixture. Additionally, almost no frequency dependence was observed. The reduction in complex permittivity implies that the Feoct(2+) cations in the lattice provide a significant contribution to polarization at microwave frequencies and the effects of Feoct(3+) are nominal in comparison.. The change in loss can be explained as a combination of the differences in the effective conductivity of the two phases (i.e. Fe3O4 exhibits electron-hopping conduction whereas the presence of vacancies in γ-Fe2O3 nullifies this). This shows that the non-invasive MCP measurements serve as a highly sensitive and versatile method for looking at this phase transition in iron and potentially the effects of oxidation states on the polarization in other iron oxides.
The growth of >100-μm-thick diamond layers adherent on aluminum nitride with low thermal boundary resistance between diamond and AlN is presented in this work. The thermal barrier resistance was found to be in the range of 16 m2·K/GW, which is a large improvement on the current state-of-the-art. While thick films failed to adhere on untreated AlN films, AlN films treated with hydrogen/nitrogen plasma retained the thick diamond layers. Clear differences in ζ-potential measurement confirm surface modification due to hydrogen/nitrogen plasma treatment. An increase in non-diamond carbon in the initial layers of diamond grown on pretreated AlN is seen by Raman spectroscopy. The presence of non-diamond carbon has minimal effect on the thermal barrier resistance. The surfaces studied with X-ray photoelectron spectroscopy revealed a clear distinction between pretreated and untreated samples. The surface aluminum goes from a nitrogen-rich environment to an oxygen-rich environment after pretreatment. A clean interface between diamond and AlN is seen by cross-sectional transmission electron microscopy.
Broadband microwave complex permittivity measurements of nanodiamond powders are presented. Previous studies show that measurements of dielectric loss strongly correlate with the presence of nondiamond surface impurities. In this study, the frequency dependence of these losses is investigated using the microwave cavity perturbation (MCP) and broadband coaxial probe (BCP) methods. This allowed further understanding as to what mechanisms contribute to the microwave absorption (free electron conduction or dielectric loss from the disordered surfaces). A multimode MCP system is used which utilizes modes to provide partial spectral characterization. The MCP results revealed minimal frequency dependence, unlike any static conduction-related mechanism. The BCP measurements corroborate the MCP results with much higher spectral resolution, and further demonstrate that disorder related loss may dominate over free electron conduction from 1-10 GHz. From 0.1-1 GHz, free electron conduction has a greater influence with a characteristic dependence implying that conduction may dominate at lower frequencies. However, the BCP method, while repeatable, lacks in precision compared to the cavity method. Nonetheless, the major conclusion in this paper is that through simple microwave permittivity measurements, nondiamond carbon impurities in nanodiamond powders are measurable most likely because of disorder related losses as opposed to free electron conduction.
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