BS ISO 11894-1-2013 Fine ceramics (advanced ceramics advanced technical ceramics) Test method for conductivity measurement of ion-conductive fine ceramics Oxide-ion-conducting soli.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 11894-1:2013Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for conductivity measurement of ion-conductive fine ceramicsPart 1: Oxide-ion-conduc

2、ting solid electrolytesBS ISO 11894-1:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 11894-1:2013. The UK participation in its preparation was entrusted to T e c h n i c a l Committee RPI/13, Advanced technical ceramics.A list of organizations represented

3、 on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2013. Published by BSI Standards Limited 2013.ISBN 978 0 580 66

4、970 5 ICS 81.060.30 Compliance with a British Standard cannot confer immunityfrom legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2013.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 11894-1:20

5、13 ISO 2013Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for conductivity measurement of ion-conductive fine ceramics Part 1: Oxide-ion-conducting solid electrolytesCramiques techniques Mthode dessai pour le mesurage de la conductivit des cramiques techniques conductrice

6、s dions Partie 1: lectrolytes solides conducteurs dions oxydesINTERNATIONAL STANDARDISO11894-1First edition2013-04-01Reference numberISO 11894-1:2013(E)BS ISO 11894-1:2013ISO 11894-1:2013(E)ii ISO 2013 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2013All rights reserved. Unless otherwise spec

7、ified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or I

8、SOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 11894-1:2013ISO 11894-1:2013(E) ISO 2013 All rights reserved iiiContents PageForeword i

9、v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols 25 Test piece 35.1 Shape and dimensions 35.2 Surface roughness 35.3 Density . 35.4 Electrodes 35.5 Number of test piece 46 Test procedure 46.1 Measurement of cross-sectional area of a test-piece and the distance between voltage

10、 terminals . 46.2 Conditions of testing 46.3 Heating of a test piece . 46.4 Method for measurement 46.5 Measurement system. 56.6 AC impedance meter 66.7 Lead wires . 66.8 Preparation for measurement . 77 Measurement . 78 Calculation of oxide ion conductivity 79 Expression of oxide ion conductivity 8

11、9.1 Oxide ion conductivity 89.2 The expression of oxide ion conductivity 810 Test report . 8BS ISO 11894-1:2013ISO 11894-1:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Interna

12、tional Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with

13、ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical co

14、mmittees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.Attention is drawn to the

15、possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 11894-1 was prepared by Technical Committee ISO/TC 206, Fine ceramics.ISO 11894 consists of the following parts, under the g

16、eneral title Fine ceramics (advanced ceramics, advanced technical ceramics) Test method for conductivity measurement of ion-conductive fine ceramics : Part 1: Oxide-ion-conducting solid electrolytesiv ISO 2013 All rights reservedBS ISO 11894-1:2013INTERNATIONAL STANDARD ISO 11894-1:2013(E)Fine ceram

17、ics (advanced ceramics, advanced technical ceramics) Test method for conductivity measurement of ion-conductive fine ceramics Part 1: Oxide-ion-conducting solid electrolytes1 ScopeThis International Standard describes a test method for the determination of ionic conductivity of oxide-ion-conducting

18、solid electrolytes by the 4-terminal method with alternating current (AC 4-terminal method).This International Standard applies to solid electrolytes which have oxide ionic transference numbers higher than 0,99. The applicable conductivity range shall be 1 to 1,000 S m1.Values expressed in this Inte

19、rnational Standard are in accordance with the International System of Units (SI).2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the re

20、ferenced document (including any amendments) applies.ISO 80000-1, Quantities and units Part 0: GeneralISO 554, Standard atmospheres for conditioning and/or testing SpecificationsISO 3611, Geometrical product specifications (GPS) Dimensional measuring equipment: Micrometers for external measurements

21、Design and metrological characteristicsISO 3599, Vernier callipers reading to 0,1 and 0,05 mmISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parametersISO 6906, Vernier callipers reading to 0,02 mmISO 14704, Fine ceramics (adv

22、anced ceramics, advanced technical ceramics) Test method for flexural strength of monolithic ceramics at room temperatureISO 15165, Fine ceramics (advanced ceramics, advanced technical ceramics) Classification systemISO 18754, Fine ceramics (advanced ceramics, advanced technical ceramics) Determinat

23、ion of density and apparent porosity3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1ionic conductionelectrical conduction where ions carry the electrical charges ISO 2013 All rights reserved 1BS ISO 11894-1:2013ISO 11894-1:2013(E)3.2electronic c

24、onductionelectrical conduction where electrons (or holes) carry the electrical charges3.3ionic transference numberratio of ionic conductivity relative to total conductivity, which is the sum of ionic conductivity and electronic (hole) conductivityNote 1 to entry: The region in which an ionic transfe

25、rence number is higher than 0,5 is defined as the ion conduction region, and the region in which an ionic transference number is higher than 0,99 is defined as the electrolytic conduction region.3.4oxide ion conductora substance whose electrical conduction is primarily governed by ionic conduction o

26、f oxide ionNote 1 to entry: In this standard, the term indicates an oxide solid electrolyte with an oxide ion transference number higher than 0,99.3.5AC 4-terminal methodmethod for measuring electrical conductivity using AC (Figure 1)Note 1 to entry: In this method, four electrodes are attached onto

27、 a test piece. The two outer electrodes which are called current terminals supply AC to the test piece. The two inner electrodes which are called voltage terminals measure the voltage. The electrical conductivity is determined with the applied current, the voltage measured and the geometry of the te

28、st piece.3.6reversible electrodeelectrode where the ionic species acting as the charge carrier can be injected into or removed from the test piece rapidly enough to give a negligibly small polarization at a supplied current3.7Bode diagramdiagram showing the complex impedance of materials by plotting

29、 the logarithm of the absolute value of impedance and the phase of impedance on the ordinate as a function of the logarithm of the frequency on the abscissa3.8common mode voltagein an impedance measurement using an AC 4-terminal method, the voltages generated between Hp and Lc, and between Lp and Lc

30、, voltages which have the same amplitude and the same phaseNote 1 to entry: In the measurement described in this standard, this voltage corresponds to the voltage between the Lp-Lc terminals in Figure 2.4 SymbolsThe symbols used throughout this International Standard and their designations are given

31、 in Table 1.2 ISO 2013 All rights reservedBS ISO 11894-1:2013ISO 11894-1:2013(E)Table 1 SymbolsSymbol Unit Definition S m1Ionic conductivityL m Distance between voltage terminalsR Effective resistance valueA m2Test-piece cross-sectional areaZ Impedance5 Test piece5.1 Shape and dimensionsA test piece

32、 should be prepared by cutting from a commercial product or a laboratory-made specimen which is fabricated under the similar conditions as the commercial product. The shape and dimensions should be in the dimensions of 4 mm x 3 mm x 36 mm or larger, typically 4 mm x 3 mm x 40 mm. Rounding of the edg

33、e, or chamfering is not necessary.If the test piece mentioned above cannot be made, the shape and dimensions of the test piece shall be in accordance with the agreement between the parties involved.5.2 Surface roughnessSurface roughness (Ra) of the test piece should be less than 0,20 m. In the other

34、 cases out of this condition, the surface roughness shall be reported.5.3 DensityBulk density of the test piece shall be measured in accordance with ISO 18754.5.4 Electrodes5.4.1 Configuration of electrodesAll 4 electrodes on a test piece, especially the current terminals (hc and lc in Figure 2) sha

35、ll possess high reversibility for the conductive oxide ion. The voltage terminals (hp and lp in Figure 2) shall be fabricated with a spacing of 20 mm in the centre of the test-piece. The width of a terminal should be as narrow as possible and shall be less than 2 mm. Current terminals shall be place

36、d at least 5 mm away from voltage terminals, and should be fabricated on both edges of the test piece with a wide area.5.4.2 Preparation of electrodesThe electrodes for electro-active substances of gaseous species such as oxygen shall possess the porosity to supply them at the electrode/electrolyte

37、interface.The electrode layer can be fabricated by one of the following methods of applying/firing conductive paste, sputtering or vapor deposition. Platinum or silver should be selected as the electrode material. The choice of the electrode material should be performed taking the melting point into

38、 consideration. In the case of using a commercially available metal paste composed of metal particles, it is strongly recommended not to use the pastes containing inorganic components as binder, particularly silica-based flux. In order to maintain the reversibility of the oxygen exchange reaction at

39、 the electrode/electrolyte interface, the firing procedure should be optimized to ensure the appropriate porosity. After firing the electrodes, lead wires of the same metal as the electrodes should be wound onto the electrodes with the conductive paste. The test piece should be fired again to tightl

40、y fix the electrodes. ISO 2013 All rights reserved 3BS ISO 11894-1:2013ISO 11894-1:2013(E)5.5 Number of test pieceThe number of test piece shall be at least three.6 Test procedure6.1 Measurement of cross-sectional area of a test-piece and the distance between volt-age terminalsCross-sectional area o

41、f a test-piece (A) shall be determined by using the callipers specified in ISO 3599 or ISO 6906, or the micrometer specified in ISO 3611. The distance between voltage terminals (L) is defined as the distance between central positions of two terminals and shall be measured by using the calliper.6.2 C

42、onditions of testingThe testing should be done in the condition specified in ISO 554. The recommended temperature is 296 2 K and the relative humidity is 50 5 %.6.3 Heating of a test pieceTesting shall use an electric furnace with a hot zone of uniform temperature in which the test piece can be enti

43、rely placed. The following conditions should also be satisfied:a) Permissible tolerance of temperature of test piece is 2 K at temperatures lower than 773 K, and 3 K at temperatures between 773 K and 1273 K.b) The effects of electromagnetic noise produced by the electric furnace shall be adequately

44、minimized. To achieve this, it is recommended to use a DC power supply, or a non-inductive coil heater if an AC power supply is used.6.4 Method for measurementImpedance of a test piece shall be measured by the AC 4-terminal method as shown in Figure 1. The oxide ion conductivity () can be determined

45、 from the impedance measured.4 ISO 2013 All rights reservedBS ISO 11894-1:2013ISO 11894-1:2013(E)AV1234455Key1 Oscillator2 Voltmeter3 Amperemeter4 Voltage terminal5 Current terminalFigure 1 AC 4-terminal method6.5 Measurement systemThe measurement system shall be basically composed of an electric fu

46、rnace in which a test piece is placed, an AC impedance meter and 4 lead wires as shown in Figure 2. ISO 2013 All rights reserved 5BS ISO 11894-1:2013ISO 11894-1:2013(E)123456789101112131415Key1 AC Oscillator 9 hp (Voltage terminal)2 Voltmeter 10 lp (Voltage terminal)3 Amperemeter 11 lc (Current term

47、inal)4 Hc (Current terminal) 12 Test piece5 Hp (Voltage terminal) 13 Measurement unit (AC impedance meter)6 Lp (Voltage terminal) 14 Lead wires for measurement7 Lc (Current terminal) 15 Electric furnace8 hc (Current terminal)Figure 2 Measurement system6.6 AC impedance meterThe AC impedance meter sha

48、ll be capable of measurement using 4 terminals with a precision of at least 3 significant digits in the impedance range of measurement. In the measurement, the instrument shall satisfy the following conditions:a) The input impedance of the voltage terminals (Hp and Lp) shall be sufficiently greater

49、than the impedance of the test piece, electrodes and lead wires. The input resistance shall be higher than 1 M, and the input capacity shall be less than 20 pF.b) In the AC 4-terminal measurement, the effect of the common mode voltage generated between Lp and Lc on the measured impedance should be smaller than 1 % of the measured impedance.c) The voltage measurement of Hp and Lp shall be guaranteed for the operation within the range of measured voltage.NOTE Some AC impedance meters limit their wor