Infraestructure and facilities

Surface Analysis Unit

Surface Analysis Platform at the CIC energiGUNE is a laboratory equipped with the state-of-the-art techniques to deal with surfaces and thin films of different materials. We can handle materials in solid state, including powders and polymers and in some cases even liquids. Surface composition, electronic and geometric structure can be probed by combination of several complimentary spectroscopic and microscopic techniques: X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), Scanning Auger microscopy/Scanning electron microscopy (SAM/SEM), Raman spectroscopy, Near-field scanning optical microscopy (NSOM), Tip enhanced Raman spectroscopy (TERS), Scanning tunneling microscopy/Atomic force microscopy on air and in liquid. The services are provided for research groups within the center as well as to the external users like other research centers or other public organization, but also to commercial companies and private people.

SPECS Multi Technique Surface Analysis System for High Resolution XPS, AES, SEM/SAM, ISS and depth profiling.

Multi Technique Multi Chamber UHV Surface Analysis System for XPS, AES, SEM/SAM and depth profiling with high space and energy resolution on the different types of conducting and not conducting samples ranging from single crystals to polymers and powders. The system has a unique combination of methods for in-situ sample preparation and treatment provided by four e-beam evaporation sources, High Pressure Cell and Electro Chemical Cell in the Preparation Chamber. Analytical part of the System is based on the hemispherical analyzer PHOIBOS 150 (SPECS GmbH), twin anode Al/Ag- X-ray source with monochromator FOCUS 500 (SPECS GmbH), fine focus electron gun with Schottky emitter for SEM/SAM (FEI), flood gun FG15/40 (SPECS GmbH) for charge compensation and scanable small spot ion gun IQE 12/38 (SPECS GmbH) for ion treatment and precise depth profiling.

NANONICS & RENISHAW - NANONICS MULTIVIEW 2000 TERS with RAMAN SPECTROMETER

NANONICS MULTIVIEW 2000 TERS with RAMAN SPECTROMETER. SNOM microscope in transmission, in collection and reflection, atomic force microscope (AFM), non-contact mode, acoustic AC, LFM, MFM, Confocal Raman microscope and confocal microscope and optical.
This equipment allows the characterization to study chemistry and physics from a non-destructive optical nanostructures and interfaces in the materials used in batteries and supercapacitors, allowing to obtain advance information of chemical bonds and other variables of the molecules making their identification and characterization Raman spectroscopy is an important technique for microscopic study of ceramic and polymeric materials that are commonly used as electrodes and electrolytes in batteries and supercapacitors.

Stylus Profiler DektakXT (Bruker)

Main Technical Specification

- Measurement Technique Stylus profilometry (contact measurement)
- Measurement Capability Two-dimensional surface profile measurements
- Optional three-dimensional measurement/analyses
- Sample Viewing Selectable magnification, 1 to 4mm FOV
- Stylus Sensor Low Inertia Sensor (LIS 3)
- Stylus Force 1 to 15mg with LIS 3 sensor
- Low Force Option N-Lite+ Low Force with 0.03 to 15mg
- Stylus Options Stylus radius options from 50nm to 25_m
- High Aspect Ratio (HAR) tips 10_m x 2_m and 200_m x 20_m
- Sample X/Y Stage Manual 100mm (4 in.) X/Y, manual leveling
- Scan Length Range 55mm (2in.)
- Data Points Per Scan 120,000 maximum
- Max. Sample Thickness 50mm (2in.)
- Max. Wafer Size 200mm (8in.)
- Step Height Repeatability <5Å, 1sigma on 1_m step
- Vertical Range 1mm (0.039in.)
- Vertical Resolution 1Å max. (@ 6.55_m range)

AGILENT - AFM/STM Microscope AGILENT 5500

AFM/STM Microscope AGILENT 5500. Complete system for atomic force microscopy for samples of small and medium size, including: two independent scanners XY and Z, closed loop control for three axes, zero background curvature in the XY scanner, AFM head, direct optical in the Z axis, motorized focus in Z, motorized XY stage precision, electronic controller, software and cantilevers.

This equipment allows:
1. The initial characterization of the materials studied.
2. Observe their interaction with other battery components.
3. Determine the mechanisms of degradation of the electrodes during its lifetime.

Tecnovac (Pfeiffer) - CLASSIC 500 SP SPUTTERING SYSTEM

- Deposition at low temperature (no need to heat the blank).
- Versatility to evaporate materials of diverse nature (conductive metals, insulating ceramic type, ...), including materials with high melting point.
- Disposal of blends and alloys maintaining the composition of the target.
- Good adhesion of the deposited film as the arrival energy of pulverized atoms to the substrate surface can reach up to several units of eV.
- Easy control of the erosion rate of the target, mainly through the power applied to the discharge.

Li deposition chamber

Technical specifications:

  • Depositing material: Li. Could be modified to evaporate other kinds of alkali metals
  • Base pressure < 5E-9 mbar. Pressure during deposition ~10e-7 mbar
  • Sample size: standard 10mm x 10mm, but can be accommodated up to ~25mm x 25 mm in case of need. Up to 3 samples can be loaded in one load
  • Substrates for deposition: any vacuum compatible material.
  • Samples can be transferred in and out without exposing to air in the air tight container. The container fits to the standard glove box.

In-situ Raman spectroscopy & Electrochemistry capability

3 in 1

  • Electrochemistry
  • Raman in vacuum or Ar
  • Raman in operando

Technical specifications:

  •  Features glass electrochemical cavity to contain 5m of electrolyte
  • Allows for 3 electrode setup
  • Sample size: standard 10mm x 10mm, but can be accommodated up to ~25mm x 25 mm in case of need.
  • Samples can be transferred in and out without exposing to air in an air tight container. The container fits to the standard glove box.
  • The glass chamber is connected to the UHV XPS system and can be evacuated down to pressure of ~10-7 mbar
  • Optical access to sample from the bottom of the electrochemical cavity during electrochemical testing
  • Laser probe with integrated CCD camera connected to Raman spectrometer provides in-situ Raman spectroscopy during electrochemical testing. Laser wavelength 532 nm 

 

Photoelectron spectroscopy for chemical analysis on surfaces (SPECS)

    Electron analyzer (FOIBOS 150 2D-DLD) X-ray sources: Mg-and Al- non-monochromated and Al- and Ag- monochromated (FOCUS) UV source Ion-sources for sputtering and depth profiling
Li deposition chamber
    Depositing material: Li. Could be modified to evaporate other kinds of alkali metals Base pressure < 5E-9 mbar. Pressure during deposition ~10e-7 mbar Sample size: standard 10mm x 10mm, but can be accommodated up to ~25mm x 25 mm in case of need. Up to 3 samples can be loaded in one load Substrates for deposition: any vacuum compatible material. Samples can be transferred in and out without exposing to air in the air tight container. The container fits to the standard glove box.
Surface structure and microscopy
    LEED and SEM/SAM High Pressure Cell integrated into the XPS spectrometer: sample heating up to 800oC under gas pressure up to 20 bar Electrochemical cell (3 electrodes setup) integrated into the XPS spectrometer and coupled with Raman spectrometer for in-situ Raman characterization
Surface preparation and thin film deposition
    Electron beam evaporators Effusion cell evaporator Lithium thermal deposition source Sample heating up to 1000oC and cooling down to 100K Tool for air-free sample transferring between XPS spectrometer and glove box and/or other UHV chamber
AFM/STM Microscope (Agilent)
    Tip scanning STM/AFM Environmental control, measurements in dedicated glove box Measurements in liquids Electrochemistry Temperature measurements STM Electric and magnetic measurements: KFM, EFM, MFM Scan ranges in X and Y: 100 x 100 µm2 and 10 x 10 µm2 Sample temperature control: heating up to 250oC
Raman integrated system (Ranishaw)
    Raman spectroscopy with 532nm and 785 nm lasers Motorized sample stage provides depth profiling in X-, Y-, Z- directions Raman spectroscopy in vacuum with remote laser probe (532nm)
FTIR spectrometer Vertex 70 (Bruker)
    Platinum ATR setup, spectral range: 8000 cm-1-10 cm-1 FTIR Microscope HYPERION 2000 Room temperature Detector DLaTGS for spectral range from 6000 cm-1to 130 cm-1 LN2cooled MCT detectors Sample compartment with environmental control
Magnetron Sputtering System (Pfeiffer)
    DC and AC magnetrons - Versatility to evaporate materials of diverse nature (conductive metals, insulating ceramic type ...), including materials with high melting point. Deposition at the different temperatures of the substrate (up to 600oC). Control of deposition rate with quarts microbalance. Available gases: oxygen, nitrogen, argon
Stylus Profiler (Bruker)
    This equipment is necessary to accurately determine the thickness and roughness of the thin films and surfaces of the different materials on the length scale between 100 nm and 100 micron.

Head of the Unit

Miguel Ángel Muñoz
Miguel Ángel Muñoz

Education: Physics degree at the University of Valencia (Valencia, Spain)Ph.D. in Physics at the University of Warwick (Coventry, United Kingdom)

Experience: Visiting scientist at the University of Western Ontario (London, Canada); Post-doctoral researcher at the Materials Science Institute of Sevilla (Sevilla, Spain); Post-doctoral researcher at the Materials Physics Center (San Sebastian, Spain)

Research background and interests: Expertise in ion scattering (MEIS, RBS), electron related spectroscopies and diffraction (XPS, AES, LEED) and scanning probe microscopy (STM/STS)Surface structure determination of adsorbate-induced reconstructions of single crystal surfacesStructural, electronic and magnetic properties of nanostructured systems such as functionalized nanoparticles and nanocompositesSurface structure and electronic properties of thin films and nanostructured systems of conversion electrodes for Li-ion batteries.

Publications

2018
Title:
UNEXPECTED EFFECT OF NANOPARTICLES DOPING ON THE CORROSIVITY OF MOLTEN NITRATE SALT FOR THERMAL ENERGY STORAGE
Authors:
Yaroslav Grosu, Nithiyanantham Udayashankar, Oleksandr Bondarchuk, Luis González-Fernández, Abdessamad Faik
Journal:
[Solar Energy Materials and Solar Cells]
DOI:
10.1016/j.solmat.2018.01.002
Title:
THE EFFECT OF HUMIDITY, IMPURITIES AND INITIAL STATE ON THE CORROSION OF CARBON AND STAINLESS STEELS IN MOLTEN HITECXL SALT FOR CSP APPLICATION
Authors:
Yaroslav Grosu, Oleksandr Bondarchuk, Abdessamad Faik
Journal:
[Solar Energy Materials and Solar Cells]
DOI:
10.1016/j.solmat.2017.08.026
2017
Title:
PROCESSING NANOPARTICLE-NANOCARBON COMPOSITES AS BINDER-FREE ELECTRODES FOR LITHIUM-BASED BATTERIES
Authors:
Marya Baloch, Pierre Kubiak, Vladimir Roddatis, Oleksandr Bondarchuk, Carmen M. López
Journal:
[Materials for Renewable and Sustainable Energy]
DOI:
10.1007/s40243-017-0105-5
Title:
LITHIUM AZIDE AS A NOVEL ELECTROLYTE ADDITIVE FOR ALL-SOLID-STATE LI-S BATTERIES
Authors:
Gebrekidan Gebresilassie Eshetu, Xabier Judez, Chunmei Li, Alex Bondarchuk, Lide M. Rodriguez Martinez, Heng Zhang and Michel Armand
Journal:
[Angewandte Chemie International Edition]
DOI:
10.1002/ange.201709305
Title:
PREDICTING THE SUITABILITY OF AQUEOUS SOLUTIONS OF DEEP EUTECTIC SOLVENTS FOR PREPARATION OF CO-CONTINUOUS POROUS CARBONS VIA SPINODAL DECOMPOSITION PROCESSES
Authors:
E.Posada, N.López-Salas, D.Carriazo, M.A.Muñoz-Márquez, C.O.Ania, R.J.Jiménez-Riobóo, M.C.Gutiérrez, M.L.Ferrer, F. del Monte
Journal:
[Carbon]
DOI:
10.1016/j.carbon.2017.07.083
Title:
VARIATIONS ON LI3N PROTECTIVE COATING USING EX-SITU AND IN-SITU TECHNIQUES FOR LI IN SULPHUR BATTERIES
Authors:
Marya Baloch, Devaraj Shanmukaraj, Oleksandr Bondarchuk, Emilie Bekaert, Teófilo Rojo, Michel Armand
Journal:
[Energy Storage Materials]
DOI:
10.1016/j.ensm.2017.06.016
2016
Title:
INVERSE VULCANIZATION OF SULFUR WITH DIVINYLBENZENE: STABLE AND EASY PROCESSABLE CATHODE MATERIAL FOR LITHIUM-SULFUR BATTERIES
Authors:
Iñaki Gomez, David Mecerreyes , J. Alberto Blazquez, Olatz Leonet, Hicham Ben Youcef, Chunmei Li, Juan Luis Gómez-Cámer, Oleksandr Bundarchuk, Lide Rodriguez-Martinez
Journal:
[Journal of Power Sources]
DOI:
10.1016/j.jpowsour.2016.08.046
Title:
THIN FILMS OF PURE VANADIUM NITRIDE: EVIDENCE FOR ANOMALOUS NON-FARADAIC CAPACITANCE
Authors:
Oleksandr Bondarchuk, Alban Morel, Daniel Bélanger, Eider Goikolea, Thierry Brousse, Roman Mysyk
Journal:
[Journal of Power Sources]
DOI:
10.1016/j.jpowsour.2016.05.093
Title:
HIGHER VOLTAGE PLATEAU CUBIC PRUSSIAN WHITE FOR NA-ION BATTERIES
Authors:
María José Piernas-Muñoz, Elizabeth Castillo-Martínez, Oleksandr Bondarchuk, Michel Armand, Teófilo Rojo
Journal:
[Journal of Power Sources]
DOI:
10.1016/j.jpowsour.2016.05.050
2015
Title:
STABLE AND ACTIVE CUXO/TIO2 NANOSTRUCTURED CATALYST FOR PROFICIENT HYDROGEN PRODUCTION UNDER SOLAR LIGHT IRRADIATION
Authors:
D. Praveen Kumar, N. Lakshmana Reddy, B. Srinivas, V. Durgakumari, V. Roddatis, O. Bondarchuk, M. Karthik, Y. Ikuma, M.V. Shankar
Journal:
[Solar Energy Materials & Solar Cells]
DOI:
doi:10.1016/j.solmat.2015.11.030
Title:
CU2O-SENSITIZED TIO2 NANORODS WITH NANOCAVITIES FOR HIGHLY EFFICIENT PHOTOCATALYTIC HYDROGEN PRODUCTION UNDERS OLAR IRRADIATION
Authors:
D. PraveenKumar, N. Lakshmana Reddy, M. MamathaKumari, B. Srinivas, V. DurgaKumari, B. Sreedhar, V. Roddatis, O. Bondarchuk, M. Karthik, B. Neppolian, M.V. Shankar
Journal:
[English]
DOI:
0927-0248
2014
Title:
SINTERING IN A GRAPHITE POWDER BED OF ALUMINA-TOUGHENED ZIRCONIA/CARBON NANOTUBE COMPOSITES:A NOVEL WAY TO DELAY HYDROTHERMAL DEGRADATION
Authors:
Mehdi Estili, J.Echeberria, J.Vleugels, K.Vanmeensel, Oleksandr Bondarchuk, N. Rodríguez, L.Larrimbe, A.Reyes-Rojas, A.Garcia-Reyes, C.Domínguez-Rios, M.H. Bocanegra-Bernal, A.Aguilar-Elguezabal
Journal:
[English]
DOI:
0272-8842
Title:
HIGH FIELD ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY UNDER ULTRAHIGH VACUUM CONDITIONS?A MULTIPURPOSE MACHINE TO STUDY PARAMAGNETIC SPECIES ON WELL DEFINED SINGLE CRYSTAL SURFACES
Authors:
J. Rocker, D. Cornu, E. Kieseritzky, A. Seiler, O. Bondarchuk, W. Hänsel-Ziegler, T. Risse and H.-J. Freund
Journal:
[Review of Scientific Instruments]
DOI:
10.1063/1.4893729
2013
Title:
IN-SITU GENERATION OF METAL?METAL OXIDE CATALYSTS FOR THE GROWTH OF HIGHLY ORIENTED GRAPHITIC NANOWIGGLES
Authors:
Javier Carretero-González, Sofía Pérez-Villar, Vladimir V. Roddatis , Nuria Gómez, Oleksandr B. Bondarchuk, Sergei Lopatin, Cármen M. López
Journal:
[English]
DOI:
0008-6223

You will find the fees on the pdf attached.

Fees Surface Analysis Unit

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