Reducing the background of ultra-low-temperature X-ray diffraction data through new methods and advanced materials

Abstract

New methods and advanced materials that significantly reduce the background when collecting single-crystal X-ray diffraction data at ultra-low temperatures using a closed-cycle helium refrigerator are presented here. These include a magnetically controlled internal beamstop and a separate internal collimator that together completely remove the scattering contribution to the background from the beryllium vacuum chamber. Additionally, a new radiation shield made from flexible graphite significantly reduces the background and maintains excellent thermal properties. In combination these improvements have led to a sixfold reduction in the average intensity and a 15-fold reduction in peak intensity of the background observed for diffraction experiments conducted with a closed-cycle helium refrigerator. Moreover, access to ultra-low base temperatures, 2.05 K, has been maintained. The design and implementation of these methods are discussed along with a case study of vitamin C to demonstrate the effectiveness of the improvements.