Characterisation of powders using microwave cavity perturbation

The contribution in this thesis is a novel application of microwave cavity perturbation in the characterisation of the fundamental properties of powders. This thesis shows that microwave cavity perturbation is very good at characterising the magnetite to maghemite phase change through dielectric and magnetic measurements. This is very important in material science since conventional techniques, though powerful and are able to verify the change, use complex methods. Quantifying di�erent forms of magnetite and maghemite is important for magnetic drug delivery and EMI absorbers. This thesis shows that microwave cavity perturbation can be used to measure the impurities of nanodiamonds through simple dielectric measurements. This is important because other methods again may involve complex systems, while microwave cavity perturbation can provide a fast, sensitive �gure of merit. Nanodiamonds are used in drug delivery and bio-labelling which requires accurate surface characterisation. This thesis shows that microwave cavity perturbation can measure in-situ temperature dependent and photocatalytic responses in materials such as titania using a novel correction procedure. Microwave cavity perturbation has not been used with this correction procedure before which simpli�es the system when monitoring systematic errors. This work is important as it shows how simple microwave cavity perturbation systems can provide insight to thermally activated processes and veri�cation of some photocatalytic mechanisms in powders for use in pigmentation and light induced drug delivery

Temperature correction for cylindrical cavity perturbation measurements

The need for accurate material property measurements using microwave cavities requires a form of compensation to correct for changes in temperature and other external influences. This paper details a method for temperature correcting microwave cavity perturbation measurements by monitoring two modes; one which is perturbed by the sample and one which is not (referred to as a nodal mode). The nodal modes used (TM310 and TE311 for an axial sample in a cylindrical cavity) are subject only to sample-independent influences. To demonstrate this technique, the bulk permittivity of a PTFE rod has been measured under varying temperature conditions. The results show that without correction, the measured temperature-dependent dielectric constant has large variations associated with the stepped and linear temperature ramping procedures. The corrected response mitigates systematic errors in the real part. However, the correction of the imaginary part requires careful consideration of the mode coupling strength. This paper demonstrates the importance of temperature correction in dynamic cavity perturbation experiments

Measurement technique for microwave surface resistance of additive manufactured metals

Additive manufactured (AM) metals are a subject of much interest for their performance in passive microwave applications. However, limitations could arise due to artifacts, such as surface texture and/or roughness resulting from the manufacturing process. We have, therefore, adopted a parallel plate microwave resonator for the accurate measurement of the surface resistance of flat metal plates, allowing for microwave current flow in two orthogonal directions by simply exciting a different resonant mode (at 5.3 and 6.4 GHz), without the need to remove and refix the sample. The systematic and random errors associated with the measurement of surface resistance are very small, less than 1% and 0.1%, respectively. The technique is demonstrated with measurements on a range of samples of the alloys, AlSi10Mg and Ti6Al4V, manufactured by laser powder bed fusion, in addition to traditionally machined samples of bulk metal alloys of aluminum and brass. For AM samples of AlSi10Mg, we have studied the effect on the surface resistance of directional roughness features, generated by the laser raster paths, in directions transverse or parallel to microwave current flow. Importantly for passive microwave device applications, we demonstrate that these samples exhibit no systematic anisotropy of surface resistance associated with such surface features

Superconducting boron doped nanocrystalline diamond microwave coplanar resonator

A superconducting boron doped nanocrystalline diamond (B-NCD) coplanar waveguide resonator (CPR) is presented for kinetic inductance ($L_k$) and penetration depth ($\lambda_{\rm{L}}$) measurements at microwave frequencies of 0.4 to 1.2 GHz and at temperatures below 3 K. Using a simplified effective medium CPR approach, this work demonstrates that thin granular B-NCD films ($t\approx$ 500 nm) on Si have a large penetration depth ($\lambda_{\rm{L}}\approx 4.3$ to 4.4 $\mu$m), and therefore an associated high kinetic inductance ($L_{k,\square} \approx$ 670 to 690 pH/$\square$). These values are much larger than those typically obtained for films on single crystal diamond which is likely due to the significant granularity of the nanocrystalline films. Based on the measured Q factors of the structure, the calculated surface resistance in this frequency range is found to be as low as $\approx$ 2 to 4 $\mu\Omega$ at $T<2$ K, demonstrating the potential for granular B-NCD for high quality factor superconducting microwave resonators and highly sensitive kinetic inductance detectors.Comment: First draf

Microwave plasma modelling in clamshell chemical vapour deposition diamond reactors

A microwave plasma model of a chemical vapour deposition (CVD) reactor is presented for understanding spatial heteroepitaxial growth of polycrystalline diamond on Si. This work is based on the TM0(n>1) clamshell style reactor (Seki Diamond/ASTEX SDS 6K, Carat CTS6U, ARDIS-100 style) whereby a simplified H2 plasma model is used to show the radial variation in growth rate over small samples with different sample holders. The model uses several steps: an electromagnetic (EM) eigenfrequency solution, a frequency-transient EM/plasma fluid solution and a transient heat transfer solution at low and high microwave power densities. Experimental growths provide model validation with characterisation using Raman spectroscopy and scanning electron microscopy. This work demonstrates that shallow holders result in non-uniform diamond films, with a radial variation akin to the electron density, atomic H density and temperature distribution at the wafer surface. For the same process conditions, greater homogeneity is observed for taller holders, however, if the height is too extreme, the diamond quality reduces. From a modelling perspective, EM solutions are limited but useful for examining electric field focusing at the sample edges, resulting in accelerated diamond growth. For better accuracy, plasma fluid and heat transfer solutions are imperative for modelling spatial growth variation

Superconducting boron doped nanocrystalline diamond on boron nitride ceramics

In this work we have demonstrated the growth of nanocrystalline diamond on boron nitride ceramic. We measured the zeta potential of the ceramics to select the diamond seeds. Diamond was then grown on the seeded ceramics using a microwave chemical vapour deposition system. A clear difference was found between the samples which were seeded with nanodiamond and the ones not seeded before growth. Raman spectroscopy confirmed the excellent quality of the diamond film. Dielectric measurements showed an increase in the dielectric constant of the material after diamond growth. The diamond was also doped with boron to make it superconducting. The film had a transition temperature close to 3.4K. Similar strategies can be applied for growth of diamond on other types of ceramics

Evaluating the coefficient of thermal expansion of additive manufactured AlSi10Mg using microwave techniques

In this paper we have used laser powder bed fusion (PBF) to manufacture and characterize metal microwave components. Here we focus on a 2.5 GHz microwave cavity resonator, manufactured by PBF from the alloy AlSi10Mg. Of particular interest is its thermal expansion coefficient, especially since many microwave applications for PBF produced components will be in satellite systems where extreme ranges of temperature are experienced. We exploit the inherent resonant frequency dependence on cavity geometry, using a number of TM cavity modes, to determine the thermal expansion coefficient over the temperature range 6–450 K. Our results compare well with literature values and show that the material under test exhibits lower thermal expansion when compared with a bulk aluminium alloy alternative (6063)

Evaluating the coefficient of thermal expansion of additive manufactured AlSi10Mg using microwave techniques

In this paper we have used laser powder bed fusion (PBF) to manufacture and characterize metal microwave components. Here we focus on a 2.5 GHz microwave cavity resonator, manufactured by PBF from the alloy AlSi10Mg. Of particular interest is its thermal expansion coefficient, especially since many microwave applications for PBF produced components will be in satellite systems where extreme ranges of temperature are experienced. We exploit the inherent resonant frequency dependence on cavity geometry, using a number of TM cavity modes, to determine the thermal expansion coefficient over the temperature range 6–450 K. Our results compare well with literature values and show that the material under test exhibits lower thermal expansion when compared with a bulk aluminium alloy alternative (6063)