TA4.4

SINTEF Mlab - Membrane laboratories for CCS

Facility Location
City & country
Trondheim (Norway)
Richard Birkelands vei
Description & contacts of the access provider
Legal name of organisation
SINTEF - Stiftelsen SINTEF
Infrastructure contact - Primary contact
Partow Henriksen
RICC contact - Secondary contact
Rune Bredesen
Facility Availability
Unit of access
Days
Availability per year
120 days
Expected duration of single experiment:
2-30 days

Fabrication facilities for inorganic membranes.

The manufacturing laboratory enables to produce a final product starting from raw powders. Final products may be flat sheet membranes of maximum 6 cm x 6 cm dimensions, symmetric or thin film coated tubular membranes of up to 20 cm long dimension. It comprises ventilated benches and hoods for synthesis of powder and its conditioning via various milling processes (planetary milling, ball milling). The powders are then shaped as tubular membranes (dense or porous) by water-based extrusion using 40 tons Loomis piston extruder located in a clean room facility (class 7). The extruder is equipped with automatic capping system for the production of close-end tubes, as well as automatic cutting tool. The tubes are delivered on an automatic air flow transport belt, thereby limiting contamination and surface damage. Planar membranes can also be prepared via tape-casting (using solvent or water based slurries). Additional milling equipment is available for tuning the rheology of pastes and slurries (sonotrode and ultrasound baths). Pastes and suspensions rheology is characterised using Kinexus rheometer and DV2t rheometer, respectively. The deposition of thin film on ceramic substrates is carried out by various techniques, including an automatic 3D spray-coater, a semi-automatic screen-printer and a multi-sample holder dip-coater, which is also located in the clean room. Necessary furnace facilities for annealing and sintering of materials of up to 1600°C are available. Furnace for annealing 30 cm long tubes are available.

A sputter for fabrication of alloy membranes such as Pd alloy is available which will be further upgraded in 2016. It is possible to produce thin films of alloy membranes on Si or glass substrate, with thickness of micron level. The sputtered layers can be used in making flat or tubular membranes. The sputtering equipment as well as electron beam deposition equipment for deposition of metal, alloys and ceramics are available in a clean room facility.

Testing units for inorganic and organic membranes.

A well-equipped membrane permeation characterisation laboratory allows studies of permeation up to 40 bars and 1000°C (e.g. for studies of Pd-based, polymericbased and ceramic membranes in Water Gas Shift, Methane Steam Reforming processes, as well as post combustion capture). The gas mass flow and pressure controllers are regulated by a PC and the gas composition of feed and permeate are monitored continuously by MS and GC units. An advanced gas distribution infrastructure for multiple gasses (O2, H2, N2, CO, CO2, CH4, Ar, He, etc) and mixtures is installed. The infrastructure will be upgraded in 2016-2017 by a furnace with three heating zones enabling to test tubular membranes of 10 to 15 cm length, and impedance spectrometer for accurate measurement of samples with low impedance.

Automated atmospheric and pressurised Thermal Gravimetric (TG) equipment.

Both TG units have automated gas feeding, switching and mixing systems (H2, CO2, CO, CH4, N2, H2O, Ar) which enable multiple cycle sorption measurements at temperatures from ambient to 1000ºC. The High Pressure TG (HPTG) is placed in a laboratory with separate ventilation system which allows experiments in a sulphur environment.

Sulphur laboratory for material and component testing.

This unique facility allows for investigation of materials from ambient conditions to high pressure-high (40 bars) and temperature (1100°C) conditions in the presence of harsh chemicals (e.g. H2S for investigation of membrane and adsorbent materials for use in power cycles based on coal, sour NG and biomass as fuel). It has high degree of automation for gas control and monitoring. It provides data for studies of reactions kinetics, transport properties, and stability of materials e.g. used as adsorbents, and membranes. Also, stability against corrosion for critical components can be studied with this type of apparatus. An advanced gas distribution infrastructure for multiple gasses (O2, H2, N2, CO, CO2, CH4, Ar, He, etc.) and mixtures is installed. The laboratory includes a well-equipped membrane permeation characterisation setup, a sorbent test station, and a high-pressure TG (thermo-gravimetric analysis). The laboratory is very flexible, and is equipped with separate ventilation system and alarms to have a safe operation condition. 

Sulphur Lab
Membrane testing
State of the art, uniqueness, & specific advantages

The major part of this infrastructure contains various experimental techniques used to evaluate the performance of sorbents and membranes. All techniques offered are modern and the results obtained are expected to be of high scientific quality. The experiments can be conducted under realistic conditions at high temperatures, pressures, and under high partial pressures of steam. Various gases are available. Also, tests in a sulphur environment (or other special gases) can be carried out in a separate laboratory with dedicated setups. The equipment are monitored and used only by skilled technicians/scientists. The choice of the right experiment/experimental conditions for a specific test can also be established through discussion with our experts.

Many of the equipment and test setups are considered unique. We have, as an example, analysed extremely high hydrogen fluxes that it is possible to obtain using ultra-thin Pd-Ag membranes (see publication list below) in our laboratory

Scientific Environment

We offer the above mentioned experiments to be carried out in one infrastructure. Skilled scientists and technicians are available to assist visiting researchers. Beside the infrastructure itself, more standard laboratories are available where sample preparation and other tasks can be performed. A number of GC, MS and IR gas analysers are available, if needed. Also, a desk with internet access will be available during the stay. SINTEF Materials and Chemistry has implemented and maintains a quality management system which fulfils the requirements of the standard NS-EN ISO 9001:2008 within research and development in material technology, advanced materials and nanotechnology, applied chemistry and biotechnology, oil and gas, and green energy and process industry.

CCS PROJECTS

EU-FUNDED CCS PROJECTS
Other Large Initiatives
OTHER CCS PROJECTS
EC DG Research - RFCS
MAIN/MAJOR NON-CCS PROJECT
Other Large Initiatives

selected publications

Egil Bakken, Paul D. Cobden, Partow Pakdel Henriksen, Silje Fosse Håkonsen, Aud I. Spjelkavik, Marit Stange, Ruth Elisabeth Stensrød, Ørnulv Vistad, Richard Blom (2011)
Development of CO2 sorbents for the SEWGS process using high throughput techniques
Energy Procedia, 4, 1104-1109
T.A. Peters, M. Stange, R. Bredesen (2011)
On the high pressure performance of thin supported Pd–23%Ag membranes—Evidence of ultrahigh hydrogen flux after air treatment
” Journal of Membrane Science 378 28– 34
Peters, T.A., Kaleta, T., Stange, M., Bredesen, R. (2013)
Development of ternary Pd-Ag-TM alloy membranes with improved sulphur tolerance
J. Membr. Sci., 429 448-458
Peters, T.A., Kaleta, T., Stange, M., Bredesen, R. (2012)
Inhibition of hydrogen transport through a selection of thin Pd-alloy membranes by H2S: membrane stability and flux recovery in H2/N2 and WGS feed mixtures
Cat. Today, 193 8-19.
Polfus, J.M., Xing, W., Sunding, M.F., Hanetho, S.M., Dahl, P.I., Larring, Y., Fontaine, M.L., Bredesen, R. (2015)
Doping strategies for increased oxygen permeability of CaTiO3 based membranes
J. Membr. Sci., 482 137-143
Polfus, J.M., Xing, W., Fontaine, M.L., Denonville, C., Henriksen, P.P., Bredesen (2015)
Hydrogen Separation Membranes based on Dense Ceramic Composites in the La27W5O55.5–LaCrO3 System
J. Membr. Sci., 479 39-45.