This work describes the design, development and testing of a portable charge-coupled device detector system to be used for the simultaneous collection of X-ray diffraction and X-ray fluorescence data from powdered samples. The detector was designed for both terrestrial and extra-terrestrial applications that require in-situ analysis of samples, where access to a laboratory instrument is restricted. The detector system incorporates 4 e2v technologies CCD30-11 devices, employing multi-phase pinned technology for low noise operation. Geometrical calculations and thermal studies concerning the design of the detector are presented, with particular emphasis on motivations for the chosen geometry. Initial characterisation and calibration of the detector was performed in a laboratory environment using a purpose built test facility. The test facility included a high brightness X-ray micro-source from Bede Scientific Instruments, coupled with an XOS polycapillary collimating optic, which was used to deliver a focused beam of low divergent X-rays to the sample. The design of the test facility is discussed and the spectra and flux produced by the X-ray micro-source are investigated. The operational performance of the detector is highlighted and the use of the instrument in different applications is described, namely the planetary sciences and pharmaceuticals sector. Finally, based on the knowledge gained from initial testing of the instrument, improvements to the detector design are outlined, which greatly enhance the combined X-ray diffraction/X-ray fluorescence performance of the instrument.

Investigating and mapping fundamental processes in nature is a driving force for breakthroughs in research and technology. Doing so, requires knowledge of the smallest scales of the world. One way of performing measurements on these scales is through intense x-ray sources, which have improved greatly over the last decades. By combing these sources with state of the art optics, even higher flux densities can be reached, allowing for faster measurements and ground-breaking discoveries.  This study aims to explore the performance of polycapillary optics, when aligned to one of the most intense x-ray micro sources in the world, the liquid-metal-jet D2+. Knife edge scans were performed together with a photon-counting medipix x-ray camera to quantify focus properties such as, flux, flux density, transmission, gain and beam width. Measurements were conducted with a 20 μm source spot that was compared to a simulated 200 μm source spot, both at 260 W electron beam power. The data from vertical and horizontal scans were combined to reconstruct the 2D functionality of the polycapillary optic. The flux density were almost four times higher with the 20 μm spot compared to the simulated 200 μm spot. This result correlated with the condition for total external reflection and the local divergence. The conclusion is that the small source spot of the liquid-metal-jet source improves the efficiency of the polycapillary optic.  The efficiency could still be improved, if the deviation in the pointing accuracy could be minimized. Furthermore, the combination of liquid-metal-jet x-ray source and the polycapillary optic, achieved extremely high flux densities. This was specially compared to an x-ray source used for confocal micro XRF, where the flux was almost nine times higher with the liquid-metal-jet x-ray source. This allows for faster measurements within confocal micro XRF and other techniques demanding very high flux densities, but with low demands on beam divergence and spectral purity.