Polycapillary X-ray optics for microdiffraction

Polycapillary optics, i.e. shaped arrays consisting of hundreds of thousands of hollow glass capillary tubes, can be used to redirect, collimate or focus X-ray beams. X-rays emitted over a large angular range from conventional laboratory-based sources can be transformed into a beam with a small angular divergence or focused onto a small sample or sample area. Convergent beams of X-rays, with convergence angles as high as 15°, have been produced using polycapillary X-ray optics. Focused-spot sizes as small as 20 µm have been achieved, with flux densities two orders of magnitude larger than that produced by pinhole collimation. This results in a comparable decrease in data collection times because of the increase in direct-beam intensity and reciprocal-space coverage. In addition, the optics can be employed to reduce background and provide more convenient alignment geometries. The inverse dependence of the critical angle for total external reflection on photon energy results in suppression of high-energy photons. This effect can be employed to allow the use of higher tube potentials to increase the characteristic line emission and has also been employed to increase significantly the Kα/Kβ ratio in Cu radiation. Measurements of X-ray diffraction data and crystallographic analyses have been performed for systems ranging from elemental crystals to proteins. Data from a lysozyme protein `standard' with a slightly convergent beam, taken in 3 min per frame with 2° oscillation with a 2.8 kW source, refined to an intensity variance of 5% compared to a standard data set. High-quality data were also obtained with a 0.03 kW fixed-anode source and a 2° convergent lens in 5 min per frame.