Facilities

The Department of Energy Conversion and Storage has state-of-the-art laboratories with experimental facilites covering a large range of synthesis, processing, characterization and test.

Process lab

Process laboratory

Our process lab covers powder synthesis (primarily of ceramics), porous and solid characterization, formulation and characterization of slurries, and shaping. Key facilities include

  • Gas pychnometer (Micromeritics)
  • Mercury intrusion (Quantachrome Poremaster 60 GT  -  2 low pressure staions, 1 dual high pressure station for 2 sample cells, pressure range 1.6 kPa - 414 MPa, pore diameter 950 – 0.0036 µm)
  • Gassorption equipment (Quantachrome Autosorp 1 MP - 1 sample station, 2 degassing stations, Krypton- and Micropore version, pore diameter 300 – 0.3 nm. Quantachrome NOVAe - 4 sample stations, 4 degassing stations, N2 analysis gas)
  • Colloidal chemistry (particle size distribution, Zeta potential, rheometer)
  • Shaping (tapecasting, screen printing, extrusion)

Test lab for solid oxide cells

Electrochemical test laboratory

The test lab focuses on performance and durability testing of solid oxide fuel cells and electrolysis cells. Both single cells and stacks may be tested.

Single cell test

  • 21 test stations for SOFC or SOEC testing
  • Fully automated, remote control, advanced safety control
  • Gas options for air and/or fuel side: H2, O2, air, CO, CO2, CH4, N2, Ar, H2S
  • Electrolysis of steam, CO2, or co-electrolysis of steam and CO2
  • Electronic load up to 40 A (SOFC) and power supply up to 40 A (SOEC)
  • Potentiostatic or galvanostatic testing
  • Impedance spectroscopy under current load: 100 kHz → 0.05 Hz
  • Gas cleaning: Possible removal of impurities in inlet gas stream (patented gas cleaning system)
  • Future option: Testing under high pressure (50-100 bar)

Stack test

  • 2 test stations for SOFC or SOEC testing
  • Fully automated, remote control, advanced safety control
  • Up to 25 cells in one stack. Short stack testing, e.g. with 5 cells
  • Gas options for air and/or fuel side: CH4, CO, CO2, air, H2, N2, O2
  • Steam electrolysis or co-electrolysis of steam and CO2
  • Gas cleaning: Possible removal of impurities in inlet gas stream (patented gas cleaning system)
  • Electronic load up to 1100 W (SOFC) and power supply up to 30 V and 400 A (SOEC)
  • Impedance spectroscopy under current load: 20 kHz → 0.5 Hz
  • Future option: Testing under high pressure (50-100 bar)

X-ray scattering

X-ray scattering facility

The department has two high flux rotating anode X-ray sources equipped with several instruments and with the possibility of in-situ experiments at temperatures up to 750 °C. Instruments include

  • Small Angle X-ray Scattering (SAXS) for characterization of nanoscale structures in solids, either in bulk or thin-film, or in dispersions of nanoparticles or proteins in solution
  • Wide Angle X-ray Scattering (WAXS) for examining crystalline structure and texture in bulk or in thin-film, or in dispersion
  • X-ray Reflectometry (XRR) for examining thin-film density variations and interface roughness
  • Laue, which is used to evaluate the orientation of single crystals in preparation for experiments at neutron facilities

Time-of-Flight Secondary Ion Mass Spectrometer

TOF-SIMS

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a chemical characterization technique that can be utilized on any kind of material that can withstand vacuum. The technique is operated in various modes, which enables surface mass spectra as well as surface ion images to be obtained (i.e. chemical information). By employing a sputter gun in conjunction with the analysis gun, a depth profile can be obtained. During the depth profiling process ion images are obtained as a function of depth, i.e. 3D chemical imaging. The technique offers a depth resolution of a few nanometers, an image resolution of ~200 nm (50 nm on newer instruments), and a detection limit in the ppm–ppb range.

Controlled Atmosphere High Temperature Scanning Probe Microscopes

Controlled atmosphere high temperature scanning probe microscope

We have developed unique Controlled Atmosphere High Temperature Scanning Probe Microscopes which are capable of performing in operando surface studies at up to 850 °C in a controlled atmosphere. A fine probe is scanned over the surface while acquiring topographic and electrical information. The available modes are contact and tapping mode topography, surface conductance, scanning tunneling microscopy (STM) and Kelvin probe microscopy. Local electrochemical impedance spectroscopy (EIS) and scanning tunneling spectroscopy (STS) can be performed in selected points.

Transmission Electron Microscope

Transmission electron microscope

With transmission electron microscopy (TEM) we study materials at high magnification and an ultimate resolution of 1.4 Å. The atomic lattice spacings in the material crystals can be observed in high resolution TEM images and from electron diffraction in the TEM. TEM therefore offer the possibility of studying the size, shape and crystal structure of nano-scaled objects. Information about the sample composition at the nanoscale is also provided either from characteristic x-ray signals emitted from the sample or from characteristic energy losses from the electrons transmitted through the sample.

Scanning Electron and Focused Ion Beam Microscopy

Scanning electron microscope

The department operates and maintains two easy-to-use table top SEMs that enable rapid imaging and elemental mapping up to magnifications of 30,000 X in addition to a high-end FIB-FEGSEM used for high resolution SEM, TEM sample preparation and 3D imaging by serial sectioning. Specifically these instruments are

  • Hitachi TM 1000
  • Hitachi TM 3000 interfaced to a Bruker SDD EDS detector
  • Zeiss CrossBeam 1540XB with an Oxford Instruments EBSD detector and a Thermo Fisher Scientific EDS detector.

In addition, the department has open access to several SEMs maintained and operated by DTU Wind Energy. These include a Zeiss SUPRA 35 with Bruker SDD and Thermo Fisher Scientific EDS detectors and an Oxford Instruments EBSD detector, a Zeiss EVO 60 LaB6 ESEM with a Thermo Fisher Scientific EDS detector and a Bruker SkyScan X-ray micro tomography camera, and a JEOL 840 LaB6 SEM.

DTU Imaging

The department participates in DTU Imaging, a joint effort between a number of DTU departments with the aim of establishing a 3D Imaging Center using X-rays and neutrons for 3D characterization of the microstructure of materials. You can read more about this effort here (in Danish).

Electron Microscopy Sample Preparation Laboratory

Sample preparation

We have a comprehensive electron microscopy sample preparation laboratory and, most essentially, the know-how to prepare a wide range of specimens for SEM, TEM and SPM etc. We routinely prepare samples spanning from basic SEM work to high-resolution TEM applications, but also samples for tomography related applications.

Thin film and crystal growth

Pulsed laser deposition facility

  • large-area pulsed laser deposition (PLD) facility for manufacture of high-quality oxide thin films and heterostructures. The PLD is equipped with RHEED (reflection high energy electron diffraction), allowing control of the oxide growth at the atomic level.
  • dual-source RF-magnetron sputtering deposition system for thin film production
  • versatile magnetron with up to four sputtering cathodes available for sputtering and co-sputtering of thin films in DC or RF under inert or reactive gas atmosphere.
  • UHV deposition of thin films using molecular beam epitaxy: 2-inch UHV magnetron sputtering cathode and 3 MBE cells for deposition on a 1 inch substrate with UHV transfer to Auger electron spectroscopy (AES) for surface characterization.
  • Ellipsometer for estimation of thin film thickness.
  • Mirror furnace for single crystal growth, up to 2000 °C and gas pressure up to 10 bars. Standard rod length 12 cm, diameter up to 10 mm.

Advanced consolidation

Spark Plasma Sintering

Apart from traditional sintering we have a number of advanced consolidation techniques available, including

  • spark plasma sintering (SPS) system (DR. Sinter Lab 515S) for rapid densification of bulk samples by localized joule heating of powders at the grain interfaces. It is capable of delivering high current (up to 1400 amperes) through powder samples in combination with an applied uniaxial pressure of 10 to a few hundred MPa in a variety of atmospheres (including vacuum).
  • arc melter for alloying of low and high melting point metals, using high current discharge melting of metal powders under an inert atmosphere.
  • melt spinning for producing thin ribbon-type samples with unique micromorphology and/or nanoscale structures. The samples are made by rapid solidification of molten mixtures or compounds ejected onto a rapidly rotating wheel of high thermal mass.

Thermoelectrics lab

We have several facilities for characterization of thermoelectric materials at temperatures from room temperature and up to about 1000 °C. They include

  • Ulvac ZEM3 high temperature thermopower and resistivity probe capable of measuring both parameters simultaneously from room temperature to 1000 °C.
  • Netsch LFA 457 laser flash analysis system. It applies a pulsed laser heat input at the bottom of the sample and uses the top surface temperature versus time profile to determine the thermal diffusivity, which can be combined with the bulk density and specific heat to calculate the thermal conductivity of a sample. The system may measure from room temperature up to 1100 °C in a variety of atmospheres.
  • Module testing for evaluation of thermoelectric module performance, operating from room temperature to 1000 °C in a variety of atmospheres.

Magnetic characterization lab

Vibrating Sample Magnetometer

In connection with our research in magnetocalorics and magnetic refrigeration we have facilities for characterizing permanent magnet assemblies, magnetocaloric materials, and evaluating the performance of active magnetic regenerators. Key facilities include

  • 3D Hall probe for measurement the spatial distribution of magnet fields
  • Direct measurement of the adiabatic temperature change of magnetocaloric materials, from –40 to 30 °C
  • LakeShore 7407 vibrating sample magnetometer (VSM) for measuring the magnetization of magnetic materials as a function of temperature (–190 - 180 °C) and applied magnetic field (0-1.6 tesla). It can handle a large variety of sample masses and shapes.
  • Differential scanning calorimeter (DSC) capable of measuring heat capacity as a function of temperature (–40-50 °C) and applied magnetic field (0-1.5 tesla). It uses very sensitive Peltier elements as heat flux sensors and high vacuum (10–10 bar) to give high sensitivity measurements. A planned update will enable the DSC to operate at fixed constant temperature (rather than scanning) while varying the magnetic field. This will enable direct measurements of the isentropic entropy change involved in the magnetocaloric effect.
  • Single-blow setup for analyzing heat transfer and flow resistance properties of thermal regenerators. By combining this experiment with sophisticated numerical models the intrinsic heat transfer properties of thermal regenerators can be determined. This is very important for accurately predicting the performance of magnetic refrigeration devices.

Plasma facilities

  • Microwave plasma device: a versatile plasma source that can be used for plasma assisted sputtering, plasma immersion ion implantation, etching and ion beam extraction. For detailed plasma diagnostics mass spectrometry, optical emission spectroscopy and different probes are available.
  • Inductively coupled plasma etcher for plasma etching of different materials using Ar, CF4, SF6 and other reactive gases. Ashing or dry surface cleaning are also available.
  • Low temperature oxidation reactor: A 6 m long reactor for investigation of gas purification (removal of NOx, SOx, VOC, etc.) using ozone injection, direct plasma treatment and catalytic materials. Up to 250 standard liter per minute flue gas with process control including measurement of ozone, NO, NO2, and other gas species by Fourier transform infrared spectroscopy (FTIR).

Solar cell testing

Characterization Laboratory for Organic Photovoltaics

Our Characterization Laboratory for Organic Photovoltaics (CLOP) includes standardized performance testing with a class A solar simulator, IPCE testing, 1000 h lifetime tests using thermal cycling and weathering chambers and outdoor testing.More info here.

Organic solar cell processing

  • Lab-scale roll slot-die coating of polymer solar cells using a Mini Roll Coater for printed organic photovoltaics (OPV). The MRC allows fully coated/printed cells using less than 100 mg material for a width of 100 mm and 1 m length substrate.
  • Glove box processing line including thermal evaporator. The standard layout comprises spin coated solar cells on a glass substrate with metalized electrodes patterned to fit in rapid testing equipment.
  • Roll-to-Roll coating with various printing and coating techniques like slot-die coating for up-scaling of OPV processing.

Polymer chemical and spectroscopic characterization

  • Nuclear Magnetic Resonance (NMR) for chemical characterization of organic molecules.
  • Infrared and UV-VIS-NIR spectroscopy.
  • Dielectric spectroscopy.
  • Size exclusion chromatography.