1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 22007-3:2012Plastics Determinationof thermal conductivity andthermal diffusivityPart 3: Temperature wave analysis method(ISO 22007-3:2008)BS EN ISO 22007-3:2012 BRITISH
2、 STANDARDNational forewordThis British Standard is the UK implementation of EN ISO22007-3:2012.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee can beobtained on request to its secretary.This
3、 publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BSI StandardsLimited 2012ISBN 978 0 580 75973 4ICS 83.080.01Compliance with a British Standard cannot confer immu
4、nity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 29 February 2012.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 22007-3 January 2012 ICS 83.080.01 Englis
5、h Version Plastics - Determination of thermal conductivity and thermal diffusivity - Part 3: Temperature wave analysis method (ISO 22007-3:2008) Plastiques - Dtermination de la conductivit thermique et de la diffusivit thermique - Partie 3: Mthode par analyse de loscillation de la temprature (ISO 22
6、007-3:2008) Kunststoffe - Bestimmung der Wrmeleitfhigkeit und der Temperaturleitfhigkeit - Teil 3: Temperaturwellen-Analysenverfahren (ISO 22007-3:2008) This European Standard was approved by CEN on 24 December 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which sti
7、pulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European
8、 Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are th
9、e national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, S
10、witzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Member
11、s. Ref. No. EN ISO 22007-3:2012: EBS EN ISO 22007-3:2012EN ISO 22007-3:2012 (E) 3 Foreword The text of ISO 22007-3:2008 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 22007-3:2012 by Technica
12、l Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2012, and conflicting national standards shall be withdrawn at the l
13、atest by July 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national st
14、andards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway
15、, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 22007-3:2008 has been approved by CEN as a EN ISO 22007-3:2012 without any modification. BS EN ISO 22007-3:2012ISO 22007-3:2008(E) ISO 2008 All rights reserv
16、ed iiiContents PageForeword ivIntroduction v1Scope12Normative references13Terms and definitions .14Symbols and units.25Principle26Apparatus.26.1General26.2 Constant-temperature enclosure.36.3 Heater and sensor elements.36.4 Heating circuit56.5 Measurement circuit56.6 Phase-shift measurement device.5
17、6.7Devices for measuring the specimen temperature57Test specimen67.1 Dimensions.67.2 Thickness.67.3Specimen-backing plates68Procedure.69Analysis of results.710 Calibration and verification of apparatus and method810.1 Calibration810.2 Verification .811 Precision and bias.911.1 Uncertainty.911.2 Repe
18、atability.912 Test report9Annex A (informative) Mathematical background to temperature wave analysis10Annex B (informative) Typical thermal-diffusivitydata for a typical polyimide11Annex C (informative) Example of frequency-thickness relationships required for acceptable measurements12Annex D (infor
19、mative) Numerical simulations of the phase shift, , as a function of kd and .14Annex E (informative) Examples of uncertainties in thermal-diffusivity measurements 15Bibliography16BS EN ISO 22007-3:2012ISO 22007-3:2008(E)iv ISO 2008 All rights reservedForeword ISO (the International Organization for
20、Standardization) is a worldwide f ederation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member bodyinterested in a subject for which a technical committee has beenestablished has the ri
21、ght to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closelywith the International Electrotechnical Com mission (IEC) on all matters of electrotechnical standardization. Internationa
22、l Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standardsadopted by the technical committees are circulated to the member bodies for voting. Publication as an
23、 International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying an y or all such patent rights. ISO
24、22007-3 was prepared by Technical Committee ISO/TC61, Plastics , Subcommittee SC 5, Physical-chemical properties. ISO 22007 consists of the following parts, under the general title Plastics Determination of thermalconductivity and thermal diffusivity: Part 1: General principles Part 2: Transient pla
25、ne heat source (hot disc) method Part 3: Temperature waveanalysis method Part 4: Laser flash method BS EN ISO 22007-3:2012ISO 22007-3:2008(E) ISO 2008 All rights reserved vIntroduction Thermal-transport properties of plastics are indispensable not only in the plastics industrybut also in otherfields
26、. Plastics are used in various manufacturing processes in new application areas, such as nanotechnologies, and in the biomedical industry. Accurate but simple small-scale measurements arerequired which can be performed quickly. High sensitivity and excellent temperature resolutionare peculiar to the
27、 m odulation techniques used for the measurement of thermal-transport properties. Temperature wave analysis is amethod of measuring the thermal diffusivity of thin specimens and is also suitable for use with small specimens. BS EN ISO 22007-3:2012BS EN ISO 22007-3:2012INTERNATIONAL STANDA RD ISO 220
28、07-3:2008(E) ISO 2008 All rights reserved 1Plastics Determination of thermal conductivity and thermal diffusivity Part 3: Temperature wave analysis method 1 Scope This part of ISO 22007 specifies a temperature wave analysis method for the determination of the thermal diffusivityof thin films and pla
29、tes of plastics in the through-thickness direction. The method can be used onplastics in either the solid ormolten state, and having either an isotropic or an orthotropic structure. The method covers values of the thermal diffusivity, ,in the range 1,0 10 8 m2 s 1 1 or c (see Annex A or References 1
30、 to 3 for details).Liquid specimens are inserted betwe en backing plates, using a quantity of liqu id sufficient to cover an arealarger than that of the heater and sensor elem ents on the backing plates see Figure 2 b). The thickness shallbe kept constantwith a spacer, the thickness of which shall b
31、e measured in accordance with 7.2.NOTE A practical example of the frequency-thickness relationships required for acceptable measurements is shown in Annex C.7.2 Thickness The specimen thickness shall be measured by means of a suitable calibrated instrument, such as a mechanical micrometer oran optic
32、al, electronic, capacitive or inductive gauge. It shall be measured before the specimen is placed in the specimen holder. The variation in the thickness of the specimen should preferably be less than 1 % of the mean thickness or 1 m, whichever is the smaller.7.3 Specimen-backing plates The thickness
33、 of the backing plates used should preferably exceed that of the specimen. It is also desirablethat the backing-plate material and specimen have similar thermal properties (i.e. similar values of theparameter k ) in order to obtain a wide linear range in the plot of phase shift versus the square roo
34、t of theangular frequencyof the temperature wave (see Figure 3 and Annexes A and D).NOTE The backing plates are not necessarily limited to solid materials: liquids, gases (including air) or a vacuumcould be used. 8 Procedure 8.1 Measure the thickness of the specimen. 8.2 In the case of a solid film,
35、 sputter a thin metal layer on each of the surfaces of the specimen to f orm the heater and sensor. Sputter the metal leads and insertthe specimen between the backing plates. 8.3 If the test is performed on a liquid, insert the specimen between backing platesonto which the heaterand sensor have alre
36、ady been attached and which are separated by a spacer of known thickness.8.4 If the heater and sensor cannot be sputtered onto the specimen, mechanical loading of the assembleddevice can be used to ensure good electrical contact between the leads and the heater and sensor and goodthermal contact bet
37、ween the heater and sensor elements and the specimen. 8.5 Place the assembled device containing the specimen in the constant-temperature enclosure. Connectthe heater to the power source and the sensor to the phase detector. 8.6 Raise or lower the temperature of the enclosure to thetest temperature a
38、t not more than 10 K/min. 8.7 Check the specimen temperature. If the resistance of the sensor is not constant throughout the test, thiscould indicate either that too much power is being supplied to the heater or a lack of thermal equilibrium in theenclosure. In such circumstances, repeat the testwit
39、h less electric power and/or wait longer to allow theenclosureto come to equilibrium.BS EN ISO 22007-3:2012ISO 22007-3:2008(E) ISO 2008 All rights reserved 7Figure 3 Example of a plot of phase shift, , versus square root of angular frequency, 1/28.8 Close the measurement circuit, generate an a.c. cu
40、rrent in the heater element and apply a bias d.c.current to the sensor. Adjust the power supplied to the heater as a function of the electrical resistance of theheater element and the wave frequencyin order to limit the specimen temperature rise to less than 1 K.8.9 Measure the phase difference of t
41、he temperature wave between the front and rear surfaces of the specimen at a fixed temperature wave angular frequencywith a phase detector, such as a lock-in amplifier,using a reference signal from the function synthesizer.8.10 Repeat the procedure described in 8.8 and 8.9 to obtain further measurem
42、ents of the phase shift atother frequencies. Select at least five frequencies for which the empirical criterion 1 (i.e. c ) issatisfied. This criterion is useful to estimate a suitable frequency range when the thermal properties of the specimen are not known (see also Annex D). 8.11 If the test is a
43、lso performed at one or more higher or lower temperatures, raise or lower the temperatureof the constant-temperature enclosure to the next temperature at not more than 10 K/min. Perform again theprocedure specified in 8.7 to 8.10 after the temperature has stabilized, in order to obtain the measureme
44、nts ofthe phase shifts. 9 Analysis of results 9.1 For a given specimen thickness and temperature, the thermal diffusivity is calculated from the slope, A , of a plot of phase shift, , versus the square root of the angular frequency, ,of the temperature wave 1 . 9.2 Plotting the phase shift as a func
45、tion of the square root of the angular frequency should produce a straight-line plot (see AnnexA and Figure3). If this isnot the case, it is likely that the angular frequencyusedBS EN ISO 22007-3:2012ISO 22007-3:2008(E)8 ISO 2008 All rights reserveddoes not fulfil the conditions necessary for this t
46、est. In such circumstances, repeat the test overa differentfrequency range. 9.3 Calculate the specimen thickness at the test temperature, taking into account the change in itsthickness due to thermal expansion. 9.4 The thermal diffusivity, , in square metres per second, of the materialis given (see
47、Annex A) by theequation222dA =where A is the slope of the plot of phase shift, , versus the square root of the angular frequency, , of the temperature wave; d is the thickness of the specimen. 9.5 Check that the condition c for the calculation in 9.4 is fulfilled. If it is not fulfilled, repeat the
48、testsusing higher angular frequencies.10 Calibration and verification of apparatus and method 10.1 Calibration 10.1.1 Temperature wave analysis is an absolute method which allows the user to perform measurements that are directlytraceable to primarySI units without calibration using referencemateria
49、ls. All elements of the apparatus for temperature wave analysis shall be calibrated separately.10.1.2 Calibrate the thickness-measurement instrument (see 7.2) to an accuracy of at least 0,1 m. 10.1.3 Calibrate the device used to measure the steady-state temperature of the test specimen assembly(see 6.7) to an accuracy ofat least 0,3 K.10.1.4 The frequencies of the power supply and the phase-shift measurement device maybe calibrated inaccordance with the instrument ma
