Award

Synchrotron soft X-ray based techniques, combined with scanning transmission x-ray microscopy (STXM) and electron microscopy can provide material structural and chemical information down to “atomic resolution”. This information is vital to optimizing many industrial and energy. However, there are no tools available for these instruments that allow scientists to observe reactions as they are implemented in many industrial settings or occur in nature. To address this need, the DOE has solicited the development of a sample holder and fluid membrane designs that can support the in-situ mixing of multiple gasses at pressures up to 100 bar. This is a significant leap in capability, as existing in-situ environmental microscopy solutions only allow 1-2 bars of pressure maximum. In Phase I Hummingbird Scientific successfully designed, built, and tested a prototype fluid holder with multiple input lines to pressure greater than 90 bar. This proof-of-concept holder has demonstrated that it is possible to build a miniature gas reaction cell that is electron and X-ray transparent, and the same time can contain very high internal pressure. We significantly improved the operating pressures by designing special reaction cell membranes and developed microfabrication techniques to successfully manufacture them. We designed our prototype holder to be compatible with both x-ray and electron beam imaging systems. Both systems showed that our reaction cell and holder can successfully facilitate high resolution imaging at high pressures. We also showed that multiple gas channels can be fed and mixed into the reaction chamber at this pressure. In Phase II of this project, we proposed to build out the features of our prototype system into a suite of commercial products that fully capture the market need. Specifically, we aim to integrate a heating element into the nanofabricated gas cell design to meet 1000°C at 100 bar reaction conditions, develop a control system and human interface for this device, and develop the core high-pressure cell technology into commercial products for x-ray, transmission electron microscopy, and scanning electron microscopy. The proposed product is vital for scientists to expand knowledge of structure-property relationships in materials and interfacial chemistry, and specifically the relationship between controlled mixing, pressure manipulation, and temperature variability for chemical and clean energy production.