SBIR-STTR Award

Society today faces unprecedented challenges in the areas of 1) the depletion of energy resources, 2) the increasing cost of chemicals and drugs, and 3) environmental pollution. Understanding nanoscale changes in material interfaces (gas/liquid, liquid/solid) and heterogeneous catalysts in their native working environments is key to engineering and optimizing solutions for all three of these challenges. A better understanding of the formation of gases and fluids in high-pressure geothermal systems can enable the practical application of more environmentally friendly fuels (e.g., hydrogen gas) for clean vehicles and other technologies. The development of highly effective but cheaper catalyst materials can reduce the cost of many chemicals necessary to produce cancer-treatment drugs, high-temperature lubricants, high- strength polymers, gas generation, and even catalytic converters in vehicles to reduce harmful emissions. However, there is no characterization tool that allows nanoscale probing of materials in their local reactive conditions such as at elevated pressures (above 1-2 bars) in real-time. Operando synchrotron soft X-ray based techniques such as scanning transmission x-ray microscopy (STXM) provide structural and chemical information of materials down to ~15 nm. However, current STXM characterization tools do not allow real-time analysis using multiple gases/liquids around the sample and limit the system's pressure to slightly above the ambient conditions (~ 1-2 bars). Hummingbird Scientific proposes developing and commercializing a multiport microfluidic sample holder to enable operando reaction conditions for studying materials in a high-pressure environment. In this STTR grant, we intend to collaborate with Dr. Miquel Salmeron at Lawrence Berkeley National Laboratory (LBNL) to utilize high-pressure membrane, including his recent oxide-based membranes (patent pending), to bring in the market the high-pressure microfluidic device with multiport capabilities for liquid/gas flow into the cell. The integration of the proposed product in the synchrotron beamline will allow to evaluate the material's behavior and performance suitable for many industrial applications such as chemical production, geothermal resources, and CO2 reduction, and other clean energy technologies.

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.