Workpackage 2

Description of work
The work in WP2 is broken down into 3 tasks:

2.1 Material Characterization (DLR, RHM, IMDEA, PSI, USIEGEN, m04 – m42)

Characterization of both TCS material systems will be a continuous task throughout the duration of the project for qualification of newly developed material, optimization of functionality of the TCS material, and evaluation of stability and degradation effects after lab-scale and pilot-scale testing. Material characterization will concern three main aspects:

  • Chemical analysis:
    • Elemental analysis by XRFA to determine composition and purity
    • Analysis of amount of dopant and oxidation state by electronic spectroscopy (UV/VIS DRS) and H2-TPR
  • Thermo-physical analysis:
    • Thermodynamic equilibrium, heat of reaction and reaction kinetics with thermal analysis (STA, DSC, DCA)
    • Measurement of thermal conductivity by laser flash and hot wire method
    • Dilatometry for analysis of expansion of volume during reaction
  • Structural and morphological analysis:
    • Crystal phase and crystallite-size analysis by XRD and in-situ XRD under reaction conditions, Rietveld analyses, electron microscopy (SEM) and Raman spectroscopy
    • Measurement of surface area and pore distribution by gas adsorption, laser granulometry and Hg porosimetry
    • Analysis of density and porosity by helium pyknometry

2.2 Material Development (DLR, RHM, IMDEA, PSI, USIEGEN, m07 – m30)

Improvement of the TCS material systems will be focused on the achievement of the technical targets defined in WP1 and will include the increase of chemical activity (process kinetics and energy efficiency), improvement of the long-term cycling stability as well as optimization of thermo-physical and mechanical properties. The investigation and development will be directed towards:

  • Adjustments in the morphology of the materials such as primary particle size, pore size distribution and surface area by high energy milling, precipitation out of solutions, etc.
  • Chemical modifications by substitution, incorporation of dopants or coatings by using different preparation techniques such as sol-gel processing, Pechini method, microemulsions and others
  • Shaping of the active material by extrusion, prilling, pelletizing or other granulation techniques

Material preparation and development will include:

  • Screening tests of different materials on a wide basis to select the most promising samples to be prepared in sufficient amounts for laboratory-scale testing in WP4.
  • Further improvements of the TCS material to be elaborated in close cooperation with the partners involved in lab-scale testing based on the results from WP4 keeping sound process economics and minimal environmental impact in mind.
  • Study of the impact of impurities and pollutants in the reaction gases (CO2, sulphur and others)
  • Long-term testing with small samples under defined conditions.

2.3 Material Preparation for Pilot-Scale Testing (DLR, RHM, IMDEA, PSI, USIEGEN, m31 – m33) The most promising material candidate(s) in regard to reactivity, cycling stability as well as thermal and mechanical performance will be produced in adequate quantity for pilot scale testing in WP5.

  • Production units:
    • Depending on the batch size requested an existing flexible pilot facility at RHM will be adapted to the process or the plant equipment will be modified to accommodate the required changes for the production of the Mn based material.
    • USIEGEN will adapt existing facilities for production of hydroxide materials in sufficient quantities
  • Material production:
    • Pre-pilot samples (batch size up to 50kg) in sufficient numbers and quantity to demonstrate both the repeatability of the (new) processes and the quality of the (new) product.

Material insert for the pilot-scale reactor