SINTEF AS
Forskningsveien 1, Oslo, Norway

CAPTURE

MLAB (NO3.3)

SINTEF MEMBRANE LABORATORIES FOR CCS – OSLO

SINTEF MLAB is dedicated to fabrication, testing and characterisation of membranes for separation of gases. It offers a broad range of fabrication equipment applicable for producing ceramic and metallic membranes, as well as characterisation and test installations for studying the performance and durability of all kinds of membranes. The membranes can be shaped as tubes, flat sheets, or thin layers on supporting structures. They can be porous or dense depending on the separation and transport mechanisms. The laboratory includes installations for testing of membrane durability under harsh and poisonous chemical conditions, such as in H2S.

Areas of research

  • Membrane development for CO2, H2 and O2 separation, including:
    • High temperature proton conductors for H2 separation
    • High temperature oxygen ionic conductors for O2 separation
    • Dual phase and facilitated transport membranes CO2 separation
    • Pd-based metal alloy membranes for H2 separation
    • Polymeric and hybrid membranes for CO2 separation and natural gas sweetening
  • Membranes applied in fuel cells and electrolysers
  • Testing and characterisation of membranes and membrane materials
  • Studies of membranes and components exposed to harsh chemical environments

Installations

Fabrication facilities for inorganic membranes

The laboratory integrates various shaping and deposition techniques with the necessary quality control tools for qualification of materials and parts along the process chain. These include ventilated benches and hoods for synthesis and conditioning of powders via various milling processes. Shaping of membranes is carried out by water-based extrusion or calendering and tape casting (organic or water-based solvent). The 40 tons Loomis piston extruder is in a clean room facility (ISO class 7) and is equipped with an automatic capping system to produce close-end tubes, as well as an automatic cutting tool. The parts are delivered on an automatic air flow transport belt, thereby limiting contamination and surface damage. Deposition techniques include an automatic 3D spray-coater, a semi-automatic screen-printer and a multi-sample holder dip-coater, which are also located in a clean room. Furnace facilities for annealing and sintering of planar membranes (up to 15 cm x 15 cm) and long tubes (up to 70 cm) are available up to 1600 °C. Quality control methods include rheology study, particle size and shape analysis, humidity measurement, leak detection, etc.

Magnetron sputtering is a versatile tool for deposition of thin films of metal/alloys and oxides. The laboratory is equipped with two state-of-the-art magnetron sputtering systems; one for sputtering on large areas, up to 50 x 30 cm, while the other system contains two magnetron sputtering chambers connected via a central transfer chamber, offering the possibility to sputter metals/alloys, oxides, nitrides, oxynitrides with in situ crystallisation at a maximum deposition temperature of 800 °C. Depositions can be done on flat samples with various shapes (fitting into a sample holder for a 6'' wafer) or tubes with maximum length 10 cm. Deposition at glancing angle (GLAD) can be done to obtain thin films with micro-porous structures. The machine is equipped with DC, pulsed DC and RF power supplies and a wafer etching station. Co-deposition from three different targets is possible. The sputtering units are placed in the clean room facility.

 

Testing units for inorganic and organic membranes

A well-equipped membrane permeation characterisation laboratory with various units allows studies of permeation up to 150 bars and 1000 °C (e.g. for studies of Pd-based, polymeric-based and ceramic membranes in water gas shift, methane steam reforming processes, as well as post combustion capture and natural gas sweetening). 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 has a furnace with three heating zones enabling to test tubular membranes of 10 to 15 cm length, and an impedance spectrometer for accurate measurement of samples with low impedance.

 

Automated atmospheric and pressurised thermogravimetric analysers (TGA)

Both TGA units have automated gas feeding, switching and mixing systems (H2, CO2, CO, CH4, N2, H2O, Ar) that enable multiple cycle sorption measurements at temperatures from ambient to 1000 ºC. The high-pressure TG (HPTG – 30 bar) is placed in a laboratory with a 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 (30 bars) and high 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 natural gas and biomass as fuel). It has a 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 sulphur 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 a separate ventilation system and alarms for safe operation.

Major equipment

 

Unit type

Model

Applications

Particle analysers

Malvern Morphology G3 and Mastersizer 2000

Particle size, shape and morphology analyser for both wet and dry powder, and for suspensions with micro and macro measuring cell, solvent compatible.

Rheometers

Brookfield DV2T Malvern Kinexus Pro

For characterisation and adjustment of the rheology of slurries and pastes.

Mixer

Winkworth Z-bra

Robust high shear mixer suitable for high viscosity and dense materials.

Extruder

Loomis

40-ton ram/piston extruder with automated capping system. The extruder is mainly used for extrusion of 'green' ceramic tubes.

Screen printer

DEK 248

Semi-automatic screen printer for deposition of thick films

Dip coater

LRC

Capacity up to 8 tubes of 1 m length. Is used for thin and thick film coating of ceramic tubes or planar substrates.

Spray coater

Sono-Tek ExactaCoat

Automated coating system with coordinated XYZ motion control thin and thick film coatings.

Thin film cluster deposition unit

Polyteknik Flexura 200

The cluster unit is used for deposition of metal, alloy, oxide and nitride films on various substrates by magnetron sputtering and electron beam deposition. The unit has 2 chambers for sputtering and one for e-beam chamber for deposition of silicon. Maximum substrate temperature is 1000 °C. Maximum substrate size is 6''.

Thin film large area deposition unit

TFE BVE3F

This magnetron sputtering unit is used for deposition of thin film Pd alloy membranes on glass or Si substrates. Maximum substrate size is 300 x 500 mm.

Thermogravimetric analysers (TGA)

Setaram Setsys Evolution

The laboratory has four TGA units, all including automatic gas handling. Maximum temperature is 1100 °C and pressure up to 30 bar.

Impedance spectroscopy

Several Gamry and Solartron frequency response analysers with integrated Pot/Gal-Stat

A range of potentiostats and FRAs for electrochemical analysis within a frequency range of 1MHz-0.001Hz and currents up to 30 A. 

Permeation testing

 

Variable volume method

Various units are available for permeation testing of membranes. These measurements are carried out in crossflow modules using gas chromatography (GC) analysis of the gas composition. Depending on the membrane type, gas compositions representative for WGS, steam reforming, post-combustion and natural gas sweetening can be generated. Maximum temperature is 1100 °C and pressure up to 150 bar.

Variable-pressure constant-volume equipment

Home-made equipment for the determination of low permeation rates, relevant for example for barrier materials. In addition, the measurement results in accurate determination of gas solubility and diffusivity in materials.

Multiple ProboStat™ systems

The ProboStat™ is a cell for measurements of electrical properties, transport parameters, and kinetics of materials, solid/gas interfaces and electrodes under controlled atmospheres at elevated temperatures up to 1600 ºC.

Custom-made and commercial modules for membrane testing

Several membrane modules are available for permeation testing, both custom-made and commercial.

Gas analysis

Several Agilent 490 micro-GCs and a Pfeiffer Vacuum ThermoStar® GSD 350 mass spectrometer

Gas composition of feed and permeate are monitored continuously by MS and GC units.

Clean room

ISO Class 6 and 7

The SONATE cleanroom is a 115 mPP2PP lab with a controlled low level of airborne contamination. The main room (ISO class 7) contains equipment for extrusion, drying, spray coating, dip coating and sintering of ceramics, and has two laminar flow benches for general work. The lithography room (ISO class 6) is cleaner and is suited for deposition of thin and thick films of functional oxides and metals. The rooms have a controlled temperature of 20 °C ± 3 °C and a controlled relative humidity of 50% ± 10%.

State of the Art, uniqueness & specific advantages

A 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 is monitored and used only by skilled technicians and scientists. The choice of the right experiment and 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 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. Several GC, MS and IR gas analysers are available, if needed. A desk with internet access will be available during the stay.

SINTEF Industry has implemented and maintains a quality management system that fulfils the requirements of the standard NS-EN ISO 9001:2008 within research and development in materials technology, advanced materials and nanotechnology, applied chemistry and biotechnology, oil and gas, and green energy and process industry.

Operating by

SINTEF AS

SINTEF AS
Norway
CAPTURE technologies:
Membranes
Research Fields:
Material science, Physical processes, Thermodynamics

Location & Contacts

Location
Forskningsveien 1, Oslo, Norway
Contacts
Marie-Laure Fontaine
RICC Contacts - Secondary contact
Rune Bredesen

Facility Availability

Availability per year (in UA)
120 UA (days)
Duration of a typical access (average) and number of external users expected for that access
2-30 UA (days)

Quality Control / Quality Assurance (QA)

Activities / tests / data are:
Controlled: ISO 9001
Link to your institution QA webpages if available:
www.sintef.no/en/sintef-group/a-certified-institute/

Operational or other constraints

Specific risks:
n/a
Legal issues:
n/a

CCUS Projects

EU-Funded CCUS Projects
FP7 CP
HIPERCAP
H2020 RIA
GENESIS
H2020 RIA
CHEERS
FP7 CP
2011-2015
HETMOC
H2020 RIA
2019-2023 https://ecocoo.eu/
ECOCO2
Other CCUS Projects
Research Council of Norway
2016-2024
NCCS
Research Council of Norway
2019-2022
MACH-2
Research Council of Norway
2017-2020
MOCO3
H2020 RIA
2019-2022
BIZEOLCAT
H2020 RIA
GAMER
H2020 RIA
AUTORE
H2020 RIA
OXIGEN
H2020 RIA
WINNER

Selected Publications

J. Membr. Sci., 429 (2013) 448-458 (2013)
Development of ternary Pd-Ag-TM alloy membranes with improved sulphur tolerance
Peters, T.A., Kaleta, T., Stange, M., Bredesen, R.
J. Membr. Sci., 482 (2015) 137-143 (2015)
Doping strategies for increased oxygen permeability of CaTiO3 based membranes
Polfus, J.M., Xing, W., Sunding, M.F., Hanetho, S.M., Dahl, P.I., Larring, Y., Fontaine, M.L., Bredesen, R.
J. Membr. Sci., 479 (2015) 39-45 (2015)
Hydrogen Separation Membranes based on Dense Ceramic Composites in the La27W5O55.5–LaCrO3 System
Polfus, J.M., Xing, W., Fontaine, M.L., Denonville, C., Henriksen, P.P., Bredesen
Sep. Pur. Techn., 212 (2020) 115858 (2020)
High-pressure CO2/CH4 separation of Zr-MOFs based mixed matrix membranes
Ahmad, M.Z., Peters, T.A., Konnertz, N.M., Visser, T., Téllez, C., Coronas, J., Fila, V., de Vos, W.M., Benes, N.E
Energy Procedia, 114 (2017) 37-45 (2017)
Palladium (Pd) membranes as key enabling technology for pre-combustion CO2 capture and hydrogen production
Peters, T.A., Rørvik, P.M., Sunde, T.O., Stange, M., Roness, F., Reinertsen, T.R., Ræder, J.H., Larring, Y., Bredesen, R

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