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Periodic Report Summary 2 - HI-C (Novel in situ and in operando techniques for characterization of interfaces in electrochemical storage systems)

Project Context and Objectives:
Novel in situ and in operando techniques for characterization of interfaces in electrochemical storage systems

Project website:

FP7 Collaborative project, Grant agreement no: 608575
Project period: 01-09-2013 – 28-02-2017

Periodic report, month 30, 26/2 2016, Publishable Summary

The objective of the Hi-C project is to develop methodologies for determining in detail the role of interface boundaries and interface layers on transport properties and reactivity in lithium batteries and supercapacitors, and to use the knowledge gained to improve performance.

The methods used include multi-technique in situ characterization combined with computational methods. The findings will be used e.g. in design of artificial Solid Electrolyte Interface (SEI) layers, in optimization of morphology and particle-coating in cathode materials and in improving intra particle ionic mobility across buried interfaces.

In the project the primary goals are to:

• Understand the important interfaces in an operating battery on an atomic and molecular scale.
• Characterize the formation and nature of interfaces in situ.
• Devise methods to control and design interface formation, stability and properties.
• Prepare ion-conducting membranes, mimetic of the polymeric part of the SEI, in order to study their mechanical and electrochemical properties.

The Hi-C consortium addresses the scientific challenges that are limiting power density, storage capacity, safety, lifetime and state of health of electrochemical storage devices such as lithium-ion batteries, conversion batteries and super-capacitors.

A number of advanced experimental and computational methods will be developed and applied to well-known battery chemistries such as LiFePO4 and Li(Ni1/3Mn1/3Co1/3)O2 vs. graphite electrode materials used in lithium-ion batteries. The results will be used for increasing the stability of silicon as negative electrode material and of positive electrode materials such as LiFeBO3 and LiVO2F. In operando cell monitoring will be developed for batteries and super capacitors.

The consortium includes five renowned universities and institutions and three industrial partners (two large companies and one SME).

The Hi-C consortium:

Technical University of Denmark, DTU, Denmark
Universite Francois Rabelais De Tours Universite Francois, UT, France
Commissariat A L Energie Atomique Et Aux Energies Alternatives, CEA, France
Karlsruher Institut fuer Technologie, KIT, Germany
Uppsala Universitet Uppsala Universitet, UU, Sweden
Haldor Topsoe AS, TOP, Denmark
Uniscan Instruments Limited, UNI, United Kingdom
Varta Microbattery GMBH, VARTA, Germany

Project Results:

The first 30 months: During the first 30 months of the Hi-C project the focus has been on developing the tools and methods for the project and to apply them to specific battery and supercapacitor systems.

• Materials specification, selection, preparation, characterization and distribution to partners.
• Developing processes for preparation of silicon nanowires.
• Synthesis method for high-performance LiFeBO3.
• Synthesis and characterization of LiVO2F and (LiV1-xMxO2F, M = Cr, Al) as new cathode materials.
• High resolution synchrotron powder diffraction characterization of LiFeBO3 and LiFePO4.
• Development of capillary based in situ battery cells for in situ studies.
• In situ high resolution powder diffraction studies of LFP and LFB batteries.
• In situ diffraction studies of conversion batteries.
• TEM and EELS studies of partially delithiated LFP samples.
• TERS (Tip enhanced Raman spectroscopy) instrument installed and tested.
• SECM (Scanning electrochemical microscopy) in situ cell developed.
• Method for fabrication of micro electrodes for SECM developed.
• Targeted SEI formation by additives and characterization by XPS.
• Formation and mechanical properties of SEI mimetic membranes.
• Sensor monitoring strategy and set-up for in operando monitoring.
• Testing heat flux sensors for in operando monitoring.
• Computational study of overpotentials across interfaces in LiFeBO3.
• Computational studies of trandport across interfaces in LiFeBO3.
• Investigation of acoustic characterization as an operando tool.
• 1-Dimensional FEM (Finite element method) models for supercapacitor and SEI developed.
• DFT calculations of ionic and electronic transport, pathways and barriers in LixBO3.
• Fabrication and charge/discharge tests of NMC/C based coin cells.
• Studies of additive effect by gas analysis using NMC/C pouch cells.
• Structural in situ investigations of Li2VO2F and LiV1-xCrxO2F in order to determine the role of intracrystalline diffusion and structural re-arrangement.
• Supercapacitors and ion capacitors; effect and improvement by additives

Potential Impact:
The outcome of the Hi-C project will be a number of developed in situ methods and equipment to be generally available for studies of interfaces in electrochemical systems. The general outcome will also be more stable cell chemistries for rechargeable lithium batteries, conversion batteries and supercapacitors.

To achieve these goals, the consortium includes five renowned universities and knowledge institutes that are indispensable for the R&D and testing. In addition, three industrial partners are part of the consortium (two large companies and one SME): A battery manufacturer, a materials producer and a company developing equipment for e.g. scanning electrochemical microscopy.

The challenges addressed are to a very large extend associated with interface properties: ionic and electronic transport, reactivity/degradation, stability, kinetic barriers and phase mobility. A deep understanding of degradation, ionic and electronic transport and SEI formation cannot be obtained only from post-mortem analysis due to the multiplicity of phenomena which occur in an operating battery during charge, discharge, storage and abuse tests. We intend to combine in situ studies of interfaces with advanced materials characterization, computational methods and modelling and experimental studies of the role of electrolyte and additives on formation and properties of interface layers.

Some of the significant advances of the state-of-the-art will be:

• First in situ studies of internal interface regions in single grains between lithiated and non-lithiated phases
• First in situ determination of chemical gradients in electrode layers during high current charge/discharge of lithium batteries
• Development of new in situ electrochemical scanning probe microscopy methods for studies of interface reactions in lithium batteries and super capacitors
• First in situ TERS (tip enhanced Raman spectroscopy) studies of SEI layer formation in lithium batteries.
• Development of novel high pressure and in situ XPS methods for detailed characterization of the atomic and electronic state during SEI formation
• In operando acoustic emission spectroscopy monitoring of commercial-type lithium batteries.

We will utilize the fundamental knowledge gained to improve batteries and supercapacitors by interface manipulation and interface design.

The impact of the Hi-C project on the society is linked to utilization of sustainable energy sources. The challenges regarding improvement of electrochemical storage devices, batteries and supercapacitors, are attacked via a fundamental understanding of interface processes and formation.

• Environmental and Societal impact: Reduced CO2 emission from transport and efficient utilization of intermittent renewable energy sources. Creation of new green jobs
• Economical and Industrial impact: Improved opportunities for European battery and supercapacitor industry. Strengthening of European competitiveness
• Technological impact: Improved electrochemical storage devices through interface manipulation
• Methodological and conceptional impact: Development of novel in situ methods for fundamental knowledge and understanding of interfaces

List of Websites:


Poul Norby, (Senior Scientist)
Tel.: +45 46774726
Fax: +45 46775758
Record Number: 188211 / Last updated on: 2016-08-24