1、BRITISH STANDARD BS EN 61006:2004 Electrical insulating materials Methods of test for the determination of the glass transition temperature The European Standard EN 61006:2004 has the status of a British Standard ICS 17.220.99; 29.035.01 BS EN 61006:2004 This British Standard was published under the
2、 authority of the Standards Policy and Strategy Committee on 28 May 2004 BSI 28 May 2004 ISBN 0 580 43811 2 National foreword This British Standard is the official English language version of EN 61006:2004. It is identical with IEC 61006:2004. It supersedes BS EN 61006:1993 which is withdrawn. The U
3、K participation in its preparation was entrusted by Technical Committee GEL/15, Insulating material, to Subcommittee GEL/15/5, Methods of test, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The
4、British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards
5、 Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the resp
6、onsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front co
7、ver, the EN title page, pages 2 to 23 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEAN STANDARD EN 61006 NORME EUROPENNE EUROPISCHE NORM April 2004 CENELEC European Co
8、mmittee for Electrotechnical Standardization Comit Europen de Normalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung Central Secretariat: rue de Stassart 35, B - 1050 Brussels 2004 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENEL
9、EC members. Ref. No. EN 61006:2004 E ICS 17.220.99; 29.035.01 Supersedes EN 61006:1993English version Electrical insulating materials Methods of test for the determination of the glass transition temperature (IEC 61006:2004) Matriaux isolants lectriques Mthodes dessai pour la dtermination de la temp
10、rature de transition vitreuse (CEI 61006:2004) Elektroisolierstoffe Prfverfahren zur Bestimmung der Glasbergangstemperatur (IEC 61006:2004) This European Standard was approved by CENELEC on 2004-03-01. CENELEC members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the
11、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 Central Secretariat or to any CENELEC member. This European Standard exists
12、in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CENELEC member into its own language and notified to the Central Secretariat has the same status as the official versions. CENELEC members are the national electrot
13、echnical committees of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Forew
14、ord The text of document 15E/222/FDIS, future edition 2 of IEC 61006, prepared by SC 15E, Methods of test, of IEC TC 15, Insulating materials, was submitted to the IEC-CENELEC parallel vote and was approved by CENELEC as EN 61006 on 2004-03-01. This European Standard supersedes EN 61006:1993 Changes
15、 from EN 61006:1993 are as follows: the standard has been completely revised from an editorial point of view and adapted to the state of the art; a figure to demonstrate the dynamic mechanical analysis has been introduced. The following dates were fixed: latest date by which the EN has to be impleme
16、nted at national level by publication of an identical national standard or by endorsement (dop) 2004-12-01 latest date by which the national standards conflicting with the EN have to be withdrawn (dow) 2007-03-01 _ Endorsement notice The text of the International Standard IEC 61006:2004 was approved
17、 by CENELEC as a European Standard without any modification. _ Page2 EN61006:2004CONTENTS 1 Scope.5 2 Terms and definitions .5 3 Significance of a method 7 4 Test methods.7 5 Method A: By differential scanning calorimetry (DSC) or differential thermal analysis (DTA)8 5.1 General.8 5.2 Interferences.
18、8 5.3 Apparatus8 5.4 Calibration.9 5.5 Precautions.9 5.6 Test specimens .9 5.7 Procedure.10 5.8 Test report10 6 Method B: By thermomechanical analysis (TMA) 11 6.1 General.11 6.2 Apparatus11 6.3 Calibration.12 6.4 Precautions .13 6.5 Test specimens .13 6.6 Procedure.13 6.7 Calculations 14 6.8 Test r
19、eport14 7 Method C: By dynamic mechanical analysis (DMA).14 7.1 General.14 7.2 Interferences.15 7.3 Methods and apparatus.15 7.3.1 Apparatus15 7.3.2 Methods15 7.3.3 Composition of the apparatus 15 7.4 Calibration.16 7.4.1 Temperature16 7.4.2 Other parameters16 7.5 Precautions .16 7.6 Test specimens
20、.16 7.7 Procedure.16 7.8 Calculations 17 7.9 Test report18 Annex A (informative) Graphical evaluation .22 Bibliography23 Page3 EN61006:2004Figure 1 Differential scanning calometry (DSC): characteristic transition points associated with glass transition.19 Figure 2 Thermomechanical analysis (TMA) (Ex
21、pansion mode): determination of glass transition temperature T g .19 Figure 3 Thermomechanical analysis (TMA) (Penetration mode): determination of the glass transition temperature T g .20 Figure 4 Thermomechanical analysis (TMA) (Expansion mode): determination of the glass transition temperature (se
22、cond run) .20 Figure 5 Typical mechanical dissipation factor profile 21 Figure 6 Dynamic mechanical analysis (DMA): determination of the glass transition temperature T g 21 Page4 EN61006:2004 ELECTRICAL INSULATING MATERIALS METHODS OF TEST FOR THE DETERMINATION OF THE GLASS TRANSITION TEMPERATURE 1
23、Scope This International Standard specifies procedures for test methods for the determination of the glass transition temperature of solid electrical insulating materials. They are applicable to amorphous materials or to partially crystalline materials containing amorphous regions which are stable a
24、nd do not undergo decomposition or sublimation in the glass transition region. 2 Terms and definitions For the purposes of this document, the following terms and definitions apply. 2.1 glass transition physical change in an amorphous material or in amorphous regions of a partially crystalline materi
25、al from (or to) a viscous or rubbery condition to (or from) a hard one NOTE The glass transition generally occurs over a relatively narrow temperature region and is similar to the solidification of a liquid to a glass state; it is not a first order transition. Not only do hardness and brittleness un
26、dergo rapid changes in this temperature region, but other properties such as thermal expansion and heat capacity also change rapidly. This phenomenon is also referred to as a second order transition, rubber transition or rubbery transition. Where more than one amorphous transition occurs in a materi
27、al, the one associated with changes in the segmental motions of the molecular backbone or accompanied by the largest change in properties is usually considered to be the glass transition. Blends of amorphous materials may have more than one glass transition, each associated with a separate component
28、 of the blend. 2.2 glass transition temperature T gmidpoint of a temperature range over which the glass transition takes place NOTE 1 The glass transition temperature can be determined readily only by observing the temperature range in which a significant change takes place in some specific electric
29、al, mechanical, thermal, or other physical property. Moreover, the observed temperature can vary significantly depending on the property chosen for observation and on details of the experimental technique (e.g., heating rate, frequency of test). Therefore, the observed T gshould be considered only a
30、n approximate value, valid only for that particular technique and test conditions. NOTE 2 For the purpose of test method C (see Clause 7), the temperature of the peak of the mechanical dissipation factor curve accompanying the glass transition is taken to be the glass transition temperature. 2.3 dif
31、ferential scanning calorimetry DSC technique in which the difference in heat flow energy inputs into a tested material and a reference material is measured as a function of temperature while the tested material and the reference material are subjected to a controlled temperature programme NOTE The r
32、ecord is the differential scanning calorimetric or DSC curve. Page5 EN61006:20042.4 differential thermal analysis DTA technique in which the temperature difference between a tested material and a reference material is measured as a function of temperature while the common environment of the tested m
33、aterial and the reference material is subjected to a controlled temperature programme NOTE 1 The record is the differential thermal analysis or DTA curve. NOTE 2 There are four characteristic transition points associated with a glass transition (see Figure 1). Extrapolated onset temperature (T f ) i
34、n C The point of intersection of the tangent drawn at the point of greatest slope on the transition curve with the extrapolated baseline prior to the transition. Extrapolated endset temperature (T e ) in C The point of intersection of the tangent drawn at the point of greatest slope on the transitio
35、n curve with the extrapolated baseline following the transition. Midpoint temperature (T m ) in C The point on the thermal curve corresponding to half the heat flow difference between the extrapolated onset and extrapolated endset. Inflection temperature (T i ) in C The point on the thermal curve co
36、rresponding to the peak of the first derivative (with respect to temperature) of the parent thermal curve. This point corresponds to the inflection point of the parent thermal curve. Two additional transition points are sometimes identified and are defined. Temperature of first deviation (T o ) in C
37、 The point of first detectable deviation from the extrapolated baseline prior to the transition. Temperature of return-to-baseline (T r ) in C The point of last deviation from the extrapolated baseline beyond transition. For the purpose of this standard T mwill be taken as the glass transition tempe
38、rature T gwhich usually corresponds more closely to the transition determined by the dilatometric and other methods. NOTE 3 Other temperatures than those previously defined can be used for specification purposes as established by individual contract. 2.5 thermodilatometry technique in which a dimens
39、ion of a test specimen under negligible load is measured as a function of temperature whilst the substance is subjected to a controlled temperature programme 2.6 thermomechanical analysis TMA technique in which a deformation of a test specimen under non-oscillatory load is measured as a function of
40、temperature whilst the test specimen is subjected to a controlled temperature programme 2.7 dynamic mechanical analysis DMA technique in which either the storage elastic or loss modulus, or both, of a substance under oscillatory load or deformation is measured as a function of temperature, frequency
41、 or time, or combination thereof 2.8 complex storage modulus complex quantity equal to the ratio of mechanical stress to mechanical strain under sinusoidal conditions Page6 EN61006:20042.9 elastic (storage) modulus the mathematically real part of the complex storage modulus. A quantitative measureme
42、nt of elastic properties defined as the ratio of the stress in-phase with oscillating strain to the magnitude of the strain 2.10 loss modulus the mathematically imaginary part of the complex storage modulus. A quantitative measure of energy dissipation defined as the ratio of stress 90 out of phase
43、with oscillating strain to the magnitude of the strain 2.11 mechanical dissipation factor the ratio of the loss modulus to the storage elastic modulus NOTE If, for instance, a material is subjected to forced, sinusoidally oscillating, linear strain of constant amplitude, then the mechanical stress i
44、n the material is determined by = = ( + i ) where is the complex storage modulus; is the storage modulus (in this case the elastic modulus); is the loss modulus; i is the square root of negative one. The mechanical dissipation factor is equal to /. 3 Significance of a method The glass transition tem
45、perature is highly dependent on the thermal history of the material structure to be tested. For amorphous and semi-crystalline materials the determination of the glass transition temperature may provide important information about their thermal history, processing conditions, stability, progress of
46、chemical reactions, and mechanical and electrical behaviour. The glass transition temperature may be used, for example, as an indication of the degree of cure of thermoset materials. The glass transition temperature of thermoset materials normally increases with increasing cure. Its determination is
47、 useful for quality assurance, specification compliance and research. 4 Test methods This standard describes three methods for the determination of the glass transition temperature. They are based on commercially available instruments, capable to operate in a typical temperature range of 100 C to +5
48、00 C. One method may be more effective in the delineation of the transition than the others depending on the specific material composition, structure and physical state, etc. Selection of the method should therefore be made according to practical criteria. NOTE The glass transition takes place over
49、a temperature range and is known to be affected by time dependent phenomena, such as the rate of heating (cooling). For these reasons only data gathered at the same heating rate should be compared. Page7 EN61006:2004Care should be taken in comparing the glass transition temperature reported by one technique with that of another. 5 Method A: By differential scanning calorimetry (
