Activities in the carbon mitigation project will address current needs for standards and measurements in the area of membranes and solid sorbents for CO2 separation and capture applications. A new laboratory is being built for assessing the performance of CO2 sorbent materials based on capacity, kinetics, thermodynamics, life cycle, and selectivity. Equipment will include a high pressure thermogravimetric analyzer (TGA) integrated with an evolved gas analyzer (EGA) and a high pressure differential scanning calorimeter. In addition, high sensitivity volumetric measurements will be made using a custom-built, computer-controlled Sieverts apparatus.
MML Sustainability Series
Working with government, industry and academic experts in carbon mitigation, MML researchers are identifying standards and measurement gaps in the area of CO2 capture, to guide research and construct a CCS technology roadmap. This past year, MML organized a seminar series on sustainability that covered a variety of topics related to carbon mitigation. To this end, the carbon mitigation project is developing new tools and measurement methods motivated by three measurement challenges that have been identified: (1) characterization of pore architecture and “closed” porosity, (2) real-time monitoring of the structural response of sorbent materials on CO2 sorption in the presence of other gases commonly found in flue gas, and (3) in-situ identification and location of atomic adsorption sites and adsorbate species.
NIST Recommended Practice Guide SP-960-17
Proper characterization of sorbent materials with respect to specific surface area, porosity, pore size, and pore size distribution is important for ensuring the required performance. In recent years, NIST has participated in the development of a certified nanoporous reference material for mercury porosimetry (NIST SRM 1917/ CRM BAM-P127) and also published a Recommended Practice Guide (jointly with the Federal Institute for Materials Research and Testing (BAM), in Germany) on “Porosity and Specific Surface Area Measurements for Solid Materials”.
SANS data for a partially sintered nanoparticulate system
Evaluating changes in sorbent porosity after either surface functionalization or reaction with CO2 is a challenge when using methods based on gas adsorption that can only provide information about open porosity, and may be limited by diffusional hindrance of the gas used as a probe. MML expertise in the use of scattering techniques such as small angle neutron scattering (SANS) will enable a comprehensive picture of the structure that includes both open and closed porosity, pore surface characteristics, pore shape, pore size distribution and volume, spatial distribution, and pore network structure and morphology.
Changes in the crystalline structure of sorbent materials occurring during adsorption and desorption of CO2 may play a very important role in the sorption mechanism. We are developing measurement methods to monitor lattice parameters and phase transformations via in-situ high pressure X-ray diffraction integrated with EGA, to complement high pressure TGA.
NEXAFS spectra of carbon-containing species
adsorbed on LZY-52 faujasite
Another important aspect of the CO2 sorption mechanism that will play a role in designing better sorbent materials involves the identification and location of adsorption sites, adsorbate species and reaction intermediates. Near edge soft X-ray absorption fine structure spectroscopy (NEXAFS), a nondestructive synchrotron based analytical tool, will be used for in-situ surface studies under different experimental conditions to probe the molecular bond chemistry, orientation, and concentration of the CO2 adsorbed species, and reaction intermediates.