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The consortium of the EPISTORE projects holds distinguished facilities for the development and characterization of new ceramic materials and new energy storage/production technologies based on thin films. In addition, the EPISTORE project aims to take some ground-breaking concepts for implementation in mainstream microelectronic industry. In this sense, the wafer-scale capabilities of our industrial partners will be employed to ensure the mass production viability of the new paradigm technology and the intermediate products.

Large-area Pulsed Laser Deposition (at IREC)

PLD 5000 (PVD Products, US) is a large area pulsed laser deposition system. It allows growing ceramic thin films on substrates of up to 10 millimeters of diameter for direct post-processing in the micro electronics industry. A 240 nm excimer laser (Coherent Compex Pro 205F) sends a high energy beam (up to 700 mJ) to the surface of the target material. The system is capable to hold four large area targets. The installed combinatorial option can produce a gradient of compositions along the substrate, which allows exploring the properties of a wide range of species in a single sample.High quality complex oxide thin films deposited in substrates up to 4” in diameter.

Ellipsometry/Raman (at IREC)

Horiba iHR320 monochromators UVISEL ellipsometry system and Horiba superhead Raman with Horiba syncerity CCD.

SLA ceramic 3D printer (at IREC)

Ceramaker (3DCeram) is aunique facility based on a hybrid ceramic 3D printer which hybridise SLA and Robocasting techniques.  With a printing volume of 300x300x120mm and a resolution of 25 microns, it can print multimaterial ceramic pieces conformed by 4 different materials integrating horizontal or vertical channels.

Electrochemistry Measurement Stations (at IREC)

An extensive amount of electrochemical and electrical characterization facilities are available at IREC. Some of the most relevant equipments for the current project are: ProboStatTM (Norecs), Linkam, High temperature Probe Station MicoXact CPS-100HT (Euris).

Probostat/Linkam (at IREC)

High temperature measuring chambers adaptable to the particular electrical characterization needed:

  • High temperature microprobe station (Linkam, UK THMS600).
  • Semiautomatic high temperature probe station adapted for 4” wafer samples.
  • Ceramic-based gas stations coupled with tubular furnaces for high temperature multi-chamber measurements (Probostat NorECs AS).
Characterization equipments (at IREC)
  • Scanning Electron Microscopy -Zeiss Auriga / Gemini 30kV schottky FESEM column
  • Transmission Electron Microscopy – Zeiss Libra 120 (LaB6)
  • Confocal microscopy – Sensofar Plu Neox
  • X-Ray Diffraction – Brucker
  • AFM – Park Systems XE7
  • Contact angle – Dataphysics
Micro and nanofabrication facility (at CSIC)

The IMB-CNM Integrated Clean Room includes equipment for micro and nanofabrication processes mainly based on silicon technologies for wafers of 100mm and 150mm, but can also operate with substrates of different materials and sizes on demand. Its structure allows flexible operation, which makes it especially suitable for R+D+i. The main available techniques include Thermal Processes and CVD, Ion Implantation, Dry Etching, Inspection and measurement equipments, Metallization, Microsystems Processes, Nanolithography, Wet Etching and Cleaning Processes, Photolithography, Packaging, Electrical Characterisation techniques. For detailed information visit CNM’s website.

Pulsed Laser Deposition (at UCAM)

The pulsed laser deposition laboratory systems are built for great flexibility, allowing easy change of targets and adjustment of growth parameters in multiple deposition chambers served by three Coherent COMPex 248nm KrF lasers. Films requiring up to six different targets can be produced in one deposition sequence, facilitating the growth of complex device structures and multilayers. Use of different gases (including Ar, O2, and N2) enables growth of pure elements, alloys and compounds. Substrate temperature can be controlled to 950° C. Multiple target holders, and rotating sample supports with computer controlled stepper motors enable extremely accurate control of film thickness and composition (e.g. for combinatorial studies). In-situ cleaning of sample surfaces and interfaces can be carried out with either a hydrogen or argon ion gun. In-situ RHEED characterisation allows layer by layer growth control for PLD grown films.

Electrochemical Impedance Spectroscopy (at UCAM)

Electrical characterisation suite equipped with an Everbeing C-Series 4-probe station, enabling precise DC characterisations. Meanwhile, AC characterisations over a frequency range of 10 µHz – 1MHz are supported by a MaterialsLab XM impedance analyser, capable of measuring impedances ranging from µohms to >100 Tohms with best in class measurement accuracy. This is further complemented by a THMS600 Linkam stage, enabling measurements over a temperature range of < -195°C to 600°C with 0.01°C accuracy and stability.

Environmental XPS (at UCAM)

EnviroESCA  near-ambient-pressure X-ray photoemission spectroscopy (XPS) system is optimised for high-throughput chemical surface analysis under application relevant environmental conditions. The system overcomes barriers of traditional XPS systems by enabling analyses at a wide range of atmospheres, ranging from 10-7 mbar up to 100 mbar. A wide range of reactive environments are enabled through three separate gas inlets, allowing direct probing of materials and devices under application relevant conditions, with temperatures up to 1000° C.

Material characterization techniques (at ICL)

Equipment: The department of materials has a wide range of equipment that will be applied to this project including the ToFSIMS V and LEIS Qtac 100 instruments (IONTOF GmbH), the Hi5 pFIBSIMS (Oregon Physics/Hiden Analytical) as well as ambient pressure XPS (Thermofisher) and Atom Probe Tomography (Cameca), all of which is complemented with standard electrochemical and structural characterisation capabilities (EIS, XRD, SEM, TEM, AFM). SIMS-LEIS in the image.

Home-made Atomic Layer Deposition (ALD) reactor (at CNRS)

Particularities: in situ ellipsometry
Deposition Area:  Up to ~Ø 5 cm (2’’)
Temperature range:  100 °C – 600 °C

Several Metal-Organic Chemical Vapour Deposition (MOCVD) reactors (at CNRS)

Particularities: Pulsed Injection of the precursors solution
Deposition Area:  Up to ~Ø 5 cm (2’’) or ~Ø 10 cm (4’’)
Temperature range:  500 °C – 750 °C
Examples of materials:  LaNiO3, La2NiO4, LaMnO3, (La,Sr)MnO3

Two home-made Spatial Atomic Layer Deposition (SALD) reactors (at CNRS)

Particularities:

  • in situ ellipsometry,
  • adaptable to sample shape,
  • R2R possible,
  • direct Area Selective Deposition and 3D printing of functional materials (nm resolution in Z, mm in XY)
  • atmospheric O2 plasma

Deposition Area:  Up to 25 cm2
Temperature range:  RT – 350 °C
Growth rate:  Up to 2 nm/s (depending on the material and temp)
Substrates:  Any (metal, glass, plastic, fabric, …)
Maximum thickness:  Several Microns
Materials available:   ZnO, Al2O3, Al:ZnO, Cu2O, Cu, CuO, TiO2, SiOx, MgO, SnO2, hybrid materials (metalcones, MOF)

TEM Microscope: MET JEOL 2010 LaB6 (at CNRS)
  • Voltage 200kV
  • Resolution 0.194nm
  • Operating modes: Conventional Microscopy, high resolution, electron diffraction, EDX
  • Uniqueness: Geometric phase analysis (GPA): strain calculation. Visualization of defects/dislocations, field of displacements and deformations in a HR image
XRD: 5-circle diffractometer Rigaku Smartlab (at CNRS)
  • 2 D detector
  • Single crystals, textured or epitaxial thin films, poly-crystallized samples
  • High resolution X-ray diffraction (HRXRD), Non coplanar grazing incidence x-ray diffraction (in plane diffraction), coplanar grazing incidence X-ray diffraction (GIXRD), X-ray reflectrometry (XRR), Texture measurements, determination of residual strain, Bragg-Brentano geometry
  • Anton-Paar DHS1100 chamber for measurement in temperature (25-1100°C) and different gas atmospheres (air/N2)
Raman setup for in situ/operando characterisation (at CNRS)
  • Jobin Yvon/Horiba Labram spectrometer
  • LN2 cooled CCD detector
  • Spot size ≈ 1µm (manual stage)
  • Objectives: 10×, 50×, 100×
  • Wavelengths: 488nm, 514.5nm (Ar+ laser) and 633nm (He/Ne laser)

Experimental cells:

  • Nextron micro probe station
    • sapphire single crystal window
    • 6 tungsten tips for electrical contacts
  • Temperature range: RT – 735°C (450°C w/o cooling system)
  • pO2 range: 0.01mbar – 1bar at 1atmo (via mixing N2+O2 gas)
  • Several Linkam heating stages (covering T range from -185°C to 1500°C)
  • Possibility of coupling with Electrical Conductivity Relaxation (ECR) measurements
Pulsed Laser Deposition (at KIT)

The PLD system (Surface systems + technology GmbH & Co. KG) enables the deposition of complex oxide thin film heterostructures. The PLD system consist of an infrared-laser heated manipulator (up to 1000 °C), a 5 × 1” target revolver, a Coherent CompexPro 205 KrF excimer laser and a differentially pumped RHEED system for in-situ analysis.

High-resolution XRD/XRR (at KIT)

The Bruker D8 Discover Thin Film XRD uses an X-ray tube generating Cu-radiation and it is equipped with an Eulerian-cradle and a xyz stage for sample mount. It can be used in two different setups, HRXRD/XRR and GIXRD.

ThermoFisher Themis-Z / Double Corrected Analytical (S)TEM (at KIT)

Imaging and Analysis Techniques:

  • BF-TEM & HRTEM
  • BF-/DF-/HAADF-STEM
  • 4D-STEM: DPC/iDPC/PDF
  • EFTEM, EELS, EDX Analysis
  • (S)TEM & EDX tomography
  • Electron diffraction
  • Lorentz imaging
  • Low-dose techniques & cryo imaging
  • AXON & Clarity in-situ integration
Facilities for ceramic powder synthesis techniques (at KIT)
  • Solid state reaction
  • Mechanochemical synthesis
  • Nebulized spray pyrolysis