DIN EN ISO 22007-3-2012 Plastics - Determination of thermal conductivity and thermal diffusivity - Part 3 Temperature wave analysis method (ISO 22007-3 2008) German version EN ISO .pdf

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1、April 2012 Translation by DIN-Sprachendienst.English price group 12No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、83.080.01!$/“1882712www.din.deDDIN EN ISO 22007-3Plastics Determination of thermal conductivity and thermal diffusivity Part 3: Temperature wave analysis method (ISO 22007-3:2008)English translation of DIN EN ISO 22007-3:2012-04Kunststoffe Bestimmung der Wrmeleitfhigkeit und der Temperaturleitfhigke

3、it Teil 3: Temperaturwellen-Analysenverfahren (ISO 22007-3:2008)Englische bersetzung von DIN EN ISO 22007-3:2012-04Plastiques Dtermination de la conductivit thermique et de la diffusivit thermique Partie 3: Mthode par analyse de loscillation de la temprature (ISO 22007-3:2008)Traduction anglaise de

4、DIN EN ISO 22007-3:2012-04www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.2203.12 DIN EN ISO 22007-3:2012-04 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee ISO/TC 6

5、1 “Plastics” (Secretariat: SAC, China) in collaboration with Technical Committee CEN/TC 249 “Plastics”, (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-01-03 AA Physikali

6、sche, rheologische und analytische Prfungen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 472 DIN EN ISO 472 ISO 22007-1 DIN EN ISO 22007-1 National Annex NA (informative) Bibliography DIN EN ISO 472, Plastics Vocabulary DIN EN ISO 2

7、2007-1, Plastics Determination of thermal conductivity and thermal diffusivity Part 1: General principles EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 22007-3 January 2012 ICS 83.080.01 English Version Plastics - Determination of thermal conductivity and thermal Plastiques - Dtermination

8、 de la conductivit thermique et de la diffusivit thermique - Partie 3: Mthode par analyse de loscillation de la temprature (ISO 22007-3:2008) Kunststoffe - Bestimmung der Wrmeleitfhigkeit und der Temperaturleitfhigkeit - Teil 3: Temperaturwellen-Analysenverfahren (ISO 22007-3:2008) This European Sta

9、ndard was approved by CEN on 24 December 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerni

10、ng such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European 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 i

11、ts own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland,

12、 Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marn

13、ix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 22007-3:2012: Ediffusivity - Part 3: Temperature wave analysis method (ISO 22007-3:2008) Contents DIN EN ISO 22007-3:2012-04 EN ISO 22007-3:2012 (E) 2

14、Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Symbols and units .6 5 Principle 6 6 Apparatus .6 6.1 General 6 6.2 Constant-temperature enclosure .7 6.3 Heater and sensor elements .7 6.4 Heating circuit 9 6.5 Measurement circuit 9 6.6 Phase-shift meas

15、urement device .9 6.7 Devices for measuring the specimen temperature 9 7 Test specimen 10 7.1 Dimensions .10 7.2 Thickness .10 7.3 Specimen-backing plates 10 8 Procedure .10 9 Analysis of results .11 10 Calibration and verification of apparatus and method 12 10.1 Calibration 12 10.2 Verification .12

16、 11 Precision and bias .13 11.1 Uncertainty .13 11.2 Repeatability .13 12 Test report 13 Annex A (informative) Mathematical background to temperature wave analysis 14 Annex B (informative) Typical thermal-diffusivity data for a typical polyimide 15 Annex C (informative) Example of frequency-thicknes

17、s relationships required for acceptable measurements 16 Annex D (informative) Numerical simulations of the phase shift, , as a function of kd and .18 Annex E (informative) Examples of uncertainties in thermal-diffusivity measurements 19 Bibliography 20 Foreword The text of ISO 22007-3:2008 has been

18、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 Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given the status of a

19、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 latest by July 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

20、 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 standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croat

21、ia, 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, Switzerland, Turkey and the United Kingdom. Endorsement notice Th

22、e text of ISO 22007-3:2008 has been approved by CEN as a EN ISO 22007-3:2012 without any modification. DIN EN ISO 22007-3:2012-04 EN ISO 22007-3:2012 (E) 3 Introduction Thermal-transport properties of plastics are indispensable not only in the plastics industry but also in other fields. Plastics are

23、 used in various manufacturing processes in new application areas, such as nanotechnologies, and in the biomedical industry. Accurate but simple small-scale measurements are required which can be performed quickly. High sensitivity and excellent temperature resolution are peculiar to the modulation

24、techniques used for the measurement of thermal-transport properties. Temperature wave analysis is a method of measuring the thermal diffusivity of thin specimens and is also suitable for use with small specimens. DIN EN ISO 22007-3:2012-04 EN ISO 22007-3:2012 (E) 4 1 Scope This part of ISO 22007 spe

25、cifies a temperature wave analysis method for the determination of the thermal diffusivity of thin films and plates of plastics in the through-thickness direction. The method can be used on plastics in either the solid or molten state, and having either an isotropic or an orthotropic structure. The

26、method covers values of the thermal diffusivity, , in the range 1,0 108m2s11 or c(see Annex A or References 1 to 3 for details). Liquid specimens are inserted between backing plates, using a quantity of liquid sufficient to cover an area larger than that of the heater and sensor elements on the back

27、ing plates see Figure 2 b). The thickness shall be kept constant with a spacer, the thickness of which shall be 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 thic

28、kness shall be measured by means of a suitable calibrated instrument, such as a mechanical micrometer or an optical, 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

29、be less than 1 % of the mean thickness or 1 m, whichever is the smaller. 7.3 Specimen-backing plates The thickness of the backing plates used should preferably exceed that of the specimen. It is also desirable that the backing-plate material and specimen have similar thermal properties (i.e. similar

30、 values of the parameter k) in order to obtain a wide linear range in the plot of phase shift versus the square root of the angular frequency of 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

31、air) or a vacuum could be used. 8 Procedure 8.1 Measure the thickness of the specimen. 8.2 In the case of a solid film, sputter a thin metal layer on each of the surfaces of the specimen to form the heater and sensor. Sputter the metal leads and insert the specimen between the backing plates. 8.3 If

32、 the test is performed on a liquid, insert the specimen between backing plates onto which the heater and sensor have already 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 assembled d

33、evice can be used to ensure good electrical contact between the leads and the heater and sensor and good thermal contact between the heater and sensor elements and the specimen. 8.5 Place the assembled device containing the specimen in the constant-temperature enclosure. Connect the heater to the po

34、wer source and the sensor to the phase detector. 8.6 Raise or lower the temperature of the enclosure to the test temperature at not more than 10 K/min. 8.7 Check the specimen temperature. If the resistance of the sensor is not constant throughout the test, this could indicate either that too much po

35、wer is being supplied to the heater or a lack of thermal equilibrium in the enclosure. In such circumstances, repeat the test with less electric power and/or wait longer to allow the enclosure to come to equilibrium. DIN EN ISO 22007-3:2012-04 EN ISO 22007-3:2012 (E) 10 Figure 3 Example of a plot of

36、 phase shift, , versus square root of angular frequency, 1/28.8 Close the measurement circuit, generate an a.c. current 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 the heater element and the

37、wave frequency in order to limit the specimen temperature rise to less than 1 K. 8.9 Measure the phase difference of the temperature wave between the front and rear surfaces of the specimen at a fixed temperature wave angular frequency with a phase detector, such as a lock-in amplifier, using a refe

38、rence signal from the function synthesizer. 8.10 Repeat the procedure described in 8.8 and 8.9 to obtain further measurements of the phase shift at other frequencies. Select at least five frequencies for which the empirical criterion 1 (i.e. c) is satisfied. This criterion is useful to estimate a su

39、itable frequency range when the thermal properties of the specimen are not known (see also Annex D). 8.11 If the test is also performed at one or more higher or lower temperatures, raise or lower the temperature of the constant-temperature enclosure to the next temperature at not more than 10 K/min.

40、 Perform again the procedure specified in 8.7 to 8.10 after the temperature has stabilized, in order to obtain the measurements of the 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 s

41、hift, , versus the square root of the angular frequency, , of the temperature wave1. 9.2 Plotting the phase shift as a function of the square root of the angular frequency should produce a straight-line plot (see Annex A and Figure 3). If this is not the case, it is likely that the angular frequency

42、 used DIN EN ISO 22007-3:2012-04 EN ISO 22007-3:2012 (E) 11 does not fulfil the conditions necessary for this test. In such circumstances, repeat the test over a different frequency range. 9.3 Calculate the specimen thickness at the test temperature, taking into account the change in its thickness d

43、ue to thermal expansion. 9.4 The thermal diffusivity, , in square metres per second, of the material is given (see Annex A) by the equation 222dA = 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

44、 specimen. 9.5 Check that the condition cfor the calculation in 9.4 is fulfilled. If it is not fulfilled, repeat the tests using 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 th

45、e user to perform measurements that are directly traceable to primary SI units without calibration using reference materials. 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

46、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 of at least 0,3 K. 10.1.4 The frequencies of the power supply and the phase-shift measurement device may be calibrated in accordance with the instrument man

47、ufacturers guidelines for the equipment. Check the zero phase shift in the electric circuit itself. 10.2 Verification Verification of the method and the apparatus can be carried out by making measurements on standard reference materials, preferably covering the range of thermal diffusivities of the

48、materials to be tested and the range of temperatures to be used. It is recommended that any deviation detected during verification be less than 5 % of the reference values. If this limit is exceeded, the measurement conditions should be re-examined and/or the various items of apparatus re-calibrated until the verification is successful. NOTE Typical values for thin polyimide film are given in Reference 4 and Annex B. Typical values for Pyrex77401)and poly(methyl methacrylat