1、Nanomanufacturing Key control characteristicsPart 4-5: Cathode nanomaterials for nano-enabled electrical energy storage Electrochemical characterization, 3-electrode cell methodPD IEC/TS 62607-4-5:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06National forewordT
2、his Published Document is the UK implementation of IEC/TS62607-4-5:2017. The UK participation in its preparation was entrusted to TechnicalCommittee NTI/1, Nanotechnologies.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purp
3、ort to include all the necessary provisions ofa contract. Users are responsible for its correct application. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 91371 6ICS 07.030; 07.120Compliance with a British Standard cannot confer immunity fromlegal oblig
4、ations.This Published Document was published under the authority of the Standards Policy and Strategy Committee on 28 February 2017.Amendments/corrigenda issued since publicationDate Text affectedPUBLISHED DOCUMENTPD IEC/TS 62607-4-5:2017IEC TS 62607-4-5 Edition 1.0 2017-01 TECHNICAL SPECIFICATION N
5、anomanufacturing 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 Registered trademark of the Internatio
6、nal Electrotechnical Commission Warning! Make sure that you obtained this publication from an authorized distributor. colourinsidePD IEC/TS 62607-4-5:2017 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 t
7、erms 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
8、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 spectr
9、oscopy (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 / inte
10、rpretation 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 O
11、pen 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
12、 . 16 Figure A.3 3-electrode screw cell assembling steps . 18 Figure A.4 Open circuit voltage/potential (OCV/P) 19 PD IEC/TS 62607-4-5:2017IEC TS 62607-4-5:2017 IEC 2017 3 Figure A.5 Electrochemical impedance spectra 19 Figure A.6 Constant current constant voltage (CCCV/CC) charging-discharging 20 F
13、igure A.7 Comparison of results of ageing tests using 3-electrode screw cell . 22 PD IEC/TS 62607-4-5:2017 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 stor
14、age Electrochemical characterization, 3-electrode cell method FOREWORD 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprisingall national electrotechnical committees (IEC National Committees). The object of IEC is to promoteinternational co-
15、operation on all questions concerning standardization in the electrical and electronic fields. Tothis end and in addition to other activities, IEC publishes International Standards, Technical Specifications,Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to
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18、s of opinion on the relevant subjects since each technical committee has representation from allinterested IEC National Committees.3) IEC Publications have the form of recommendations for international use and are accepted by IEC NationalCommittees in that sense. While all reasonable efforts are mad
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20、ly to the maximum extent possible in their national and regional publications. Any divergencebetween any IEC Publication and the corresponding national or regional publication shall be clearly indicated inthe latter.5) IEC itself does not provide any attestation of conformity. Independent certificat
21、ion bodies provide conformityassessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for anyservices carried out by independent certification bodies.6) All users should ensure that they have the latest edition of this publication.7) No liability shall attach
22、 to IEC or its directors, employees, servants or agents including individual experts andmembers of its technical committees and IEC National Committees for any personal injury, property damage orother damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) an
23、dexpenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IECPublications.8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications isindispensable for the correct application of this publication.9) Att
24、ention is drawn to the possibility that some of the elements of this IEC Publication may be the subject ofpatent rights. IEC shall not be held responsible for identifying any or all such patent rights.The main task of IEC technical committees is to prepare International Standards. In exceptional cir
25、cumstances, 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
26、 is thefuture 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 b
27、een prepared by IEC technical committee 113: Nanotechnology standardization for electrical and electronic products and systems. PD IEC/TS 62607-4-5:2017IEC TS 62607-4-5:2017 IEC 2017 5 The text of this Technical Specification is based on the following documents: Enquiry draft Report on voting 113/31
28、7/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, publishe
29、d 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
30、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 publi
31、cation 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. PD IEC/TS 62607-4-5:2017 6 IEC TS 62607-4-5:2017 IEC 2017 INTRODUCTION The future utilization of renewable ene
32、rgy 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
33、 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 todays perspective, lithium
34、-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 differe
35、nt 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 cat
36、hode 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 cha
37、racterization 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 materi
38、als 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 d
39、evice 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
40、 for using this method. PD IEC/TS 62607-4-5:2017IEC TS 62607-4-5:2017 IEC 2017 7 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
41、 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 na
42、nomaterial 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 pu
43、rpose 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 Normat
44、ive 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 ame
45、ndments) 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 data
46、bases 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 frac
47、tion of nanomaterial and exhibits function or performance made possible only with the application of nanotechnology PD IEC/TS 62607-4-5:2017 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
48、 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 m
49、aterial 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 cat