IEC TS 62607-4-5:2017

IEC TS 62607-4-5 ®
Edition 1.0 2017-01
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 4-5: Cathode nanomaterials for nano-enabled electrical energy storage –
Electrochemical characterization, 3-electrode cell method

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IEC TS 62607-4-5 ®
Edition 1.0 2017-01
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 4-5: Cathode nanomaterials for nano-enabled electrical energy storage –

Electrochemical characterization, 3-electrode cell method

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.030; 07.120 ISBN 978-2-8322-3766-3

– 2 – IEC TS 62607-4-5:2017 © IEC 2017
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions and abbreviated terms . 7
3.1 Terms and definitions . 7
3.2 Abbreviated terms . 9
4 Sample preparation methods . 9
4.1 General . 9
4.2 Reagents . 9
4.2.1 Cathode foil . 9
4.2.2 Anode foil . 10
4.2.3 Reference electrode . 10
4.2.4 Electrolyte and separator . 10
4.3 Pre-treatment of the electrode materials . 10
4.4 Preparation of the screw cell . 11
4.5 Disassembly of the screw cell . 12
5 Measurement of electrochemical properties . 12
5.1 General . 12
5.2 Open circuit potential . 12
5.2.1 Demarcation of method . 12
5.2.2 Experimental procedures and measurement conditions . 12
5.3 Potentiostatic electrochemical impedance spectroscopy (EIS) . 13
5.3.1 Demarcation of method . 13
5.3.2 Experimental procedures and measurement conditions . 13
5.4 Charge-discharge experiment (Constant Current Constant Voltage,
CCCV/CC) . 13
5.4.1 Demarcation of method . 13
5.4.2 Experimental procedures and measurement conditions . 13
6 Data analysis / interpretation of results (see Figure A.7) . 14
6.1 Open circuit potential . 14
6.2 Electrochemical impedance spectroscopy . 14
6.3 Constant current constant voltage (CC CV) charging-discharging . 14
Annex A (informative) Case study . 16
A.1 Sample preparation . 16
A.2 Results for a LFP electrode . 19
A.2.1 Open circuit voltage/potential (OCV/P) . 19
A.2.2 Electrochemical impedance spectroscopy (EIS) . 19
A.2.3 Constant current constant voltage (CCCV/CC) charging-discharging . 20
A.2.4 Ageing tests . 20

Figure A.1 – 3-electrode screw cell . 16
Figure A.2 – Components of the electrochemical cell used for testing . 16
Figure A.3 – 3-electrode screw cell assembling steps . 18
Figure A.4 – Open circuit voltage/potential (OCV/P) . 19

Figure A.5 – Electrochemical impedance spectra . 19
Figure A.6 – Constant current constant voltage (CCCV/CC) charging-discharging . 20
Figure A.7 – Comparison of results of ageing tests using 3-electrode screw cell . 22

– 4 – IEC TS 62607-4-5:2017 © IEC 2017
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 4-5 Cathode nanomaterials for nano-enabled electrical energy
storage – Electrochemical characterization, 3-electrode cell method

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
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The main task of IEC technical committees is to prepare International Standards. In
exceptional circumstances, a technical committee may propose the publication of a Technical
Specification when
• the required support cannot be obtained for the publication of an International Standard,
despite repeated efforts, or
• the subject is still under technical development or where, for any other reason, there is the
future but no immediate possibility of an agreement on an International Standard.
Technical Specifications are subject to review within three years of publication to decide
whether they can be transformed into International Standards.
IEC TS 62607-4-5, which is a Technical Specification, has been prepared by IEC technical
committee 113: Nanotechnology standardization for electrical and electronic products and
systems.
The text of this Technical Specification is based on the following documents:
Enquiry draft Report on voting
113/317/DTS 113/342/RVC
Full information on the voting for the approval of this technical specification can be found in
the report on voting indicated in the above table.
This document has been drafted in accordance with the ISO/IEC Directives, Part 2.
A list of all parts in the IEC 62607 series, published under the general title
Nanomanufacturing – Key control characteristics, can be found on the IEC website.
The committee has decided that the contents of this document will remain unchanged until the
stability date indicated on the IEC website under "http://webstore.iec.ch" in the data related to
the specific document. At this date, the document will be
• transformed into an International Standard,
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
A bilingual version of this publication may be issued at a later date.

IMPORTANT – The 'colour inside' logo on the cover page of this publication indicates
that it contains colours which are considered to be useful for the correct
understanding of its contents. Users should therefore print this document using a
colour printer.
– 6 – IEC TS 62607-4-5:2017 © IEC 2017
INTRODUCTION
The future utilization of renewable energy technologies depends significantly on the
development of efficient systems for energy storage. Conventional approaches exist for the
storage of electrical energy from stationary power plants, currently fuelled by many new ideas
in conjunction with the emerging "Smart Grid". For future e-mobility for individual
transportation there is only one attractive solution: a battery that can store enough energy to
allow all-electric driving with a range of several hundred kilometres. The current solutions
already on the market can only be seen as temporary solutions. From today's perspective,
lithium-ion batteries and their derivative innovative concepts are regarded as the most
promising candidates. Electrodes made from nanoscale composites will play a key role in the
future. Innovative materials will be developed and systematically optimized, which implies
testing of a large number of different materials.
Characterization of the electrochemical properties of cathode nanomaterials used in electrical
energy storage devices is important for their customized development. This document
provides a standard methodology which can be used to characterize the electrochemical
properties of new cathode nanomaterials that will be employed in electrical energy storage
devices. Following this method will allow comparison of different types of cathode
nanomaterial and comparing the results of different research groups.
This document introduces a 3-electrode cell method for the electrochemical characterization
of nano-enabled cathode materials for electrical energy storage devices.
This standardized method is intended for use in comparing the characteristics of cathode
nanomaterials in the development stage, not for evaluating the electrode in end-products.
The method is applicable to materials exhibiting function or performance only possible with
nanotechnology, intentionally added to the active materials to measurably and significantly
change the capacity of electrical energy storage devices.
In this context it is important to note that the percentage content of nanomaterial of the device
in question has no direct relation to the applicability of this document, because minute
quantities of nanomaterial are frequently sufficient to improve the performance significantly.
The fraction of nanomaterials in electrodes, electrode coatings, separators or electrolyte is
not of relevance for using this method.

NANOMANUFACTURING – KEY CONTROL CHARACTERISTICS –

Part 4-5 Cathode nanomaterials for nano-enabled electrical energy
storage – Electrochemical characterization, 3-electrode cell method

1 Scope
This part of IEC 62607 provides a standardized method for the determination of
electrochemical properties of cathode nanomaterials such as lithium iron phosphate (LFP) for
electrical energy storage devices. This method will enable the industry to:
a) decide whether or not a cathode nanomaterial is usable, and
b) select a cathode nanomaterial suitable for their application.
This document includes:
• recommendations for sample preparation,
• outlines of the experimental procedures used to measure cathode nanomaterial properties,
• methods of interpretation of results and discussion of data analysis, and
• case studies.
NOTE The very purpose of this method is to arrive at a detailed characterization of the electrodes so that
individual contribution of the anode and cathode for performance and degradation could be predicted. The method
can be applied for characterization of the electrode working as cathode or/and as anode.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their
content constitutes requirements of this document. For dated references, only the edition
cited applies. For undated references, the latest edition of the referenced document (including
any amendments) applies.
ISO/TS 80004-1, Nanotechnologies – Vocabulary – Part 1: Core terms
3 Terms, definitions and abbreviated terms
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO/TS 80004-1 and the
following apply.
ISO and IEC maintain terminological databases for use in standardization at the following
addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
3.1.1
cathode nanomaterial
material used as a cathode in a nano-enabled energy storage device which contains a fraction
of nanomaterial and exhibits function or performance made possible only with the application
of nanotechnology
– 8 – IEC TS 62607-4-5:2017 © IEC 2017
Note 1 to entry: The cathode is a multilayered foil consisting of (1) an aluminium current collector, (2) an optional
adhesion promoting carbon layer (to enhance cathode layer adhesion if necessary) and (3) the cathode layer. This
cathode layer consists of the active phase (e.g. lithium containing mixed oxides or phosphate, such as LFP), a
conducting phase (carbon black) and an organic binder (PVDF).
3.1.2
anode material
material used as counter electrode (CE) for the electrochemical characterization of cathodes
in the 3-electrode cell
Note 1 to entry: The anode may be a tape-cast graphite electrode consisting of (1) a copper current collector foil
and (2) the active layer composed of graphite, a conducting phase (carbon black) and organic binder (PVDF, CMC).
Alternatively, metallic lithium may be utilized as CE. Using lithium, the necessity of balancing the capacities of
cathode and anode is dropped. However, the cycling stability of lithium is strongly limited in comparison to a
graphite anode. Thus the choice of the counter electrode has to be adapted to the purpose of the investigation.
3.1.3
reference electrode
RE
electrode not actively involved in the battery cell reactions (charging, discharging)
Note 1 to entry: The reference electrode is placed in the cell arrangement to enable the measurement of the
electrode potentials of cathode and anode. Both values are determined with respect to the RE's potential. To
ensure a proper measurement, the reference electrode's potential has to be held constant. Thus a currentless
contacting of this electrode is realized to prevent the formation of overpotentials. In lithium ion battery research the
most common reference electrode material is metallic lithium in contact with a lithium ion containing electrolyte.
3.1.4
3-electrode screw cell
cell providing the geometrical conditions in the three electrode arrangement
Note 1 to entry: The independent electrochemical investigation of cathode and anode material is carried out in
3-electrode screw cells. This notion describes a cell in three electrode arrangement providing battery-like
geometrical conditions of cathode and anode. Additionally, a lithium reference electrode is included to enable the
determination of the individual electrode potentials rather than of the overall cell voltage. The cell setup includes
springs and metallic current collectors and the electrode package with anode/separators + electrolyte/cathode. The
reference electrode is placed between anode and cathode, separated from these electrodes by layers of separator.
For this purpose, various cell designs are possible. The case study in Annex A shows a cell design based on a
half-inch PFA Swagelok fitting.
3.1.5
cell voltage
U
cell
difference of the electrochemical potentials of the cathode and the anode
3.1.6
electrode potential
difference between the electrochemical potential of an electrode in the 3-electrode cell and
the potential of the RE
Note 1 to entry: Electrode potentials ϕ and ϕ are the differences between the electrochemical potential of
WE CE
the respective electrode in the 3-electrode cell and the potential of the RE. In case of intercalation electrode
materials, it is determined by the lithiation state of the material. Additionally, the overpotential of the respective
electrode reaction influences its potential. Consequently it is a valuable physical parameter to be determined, as it
includes a significant amount of information on the individual electrodes and their actual state.
3.1.7
cell resistance
R
el
ohmic internal resistance of the testing cell
______________
PFA Swagelok fitting is an example of a suitable product available commercially. This information is given for
the convenience of users of this document and does not constitute an endorsement by IEC of this product.

Note 1 to entry: R is the sum of the ohmic resistivities (e.g. electrolyte, contact resistance) within th
...