EN 6064-2017 en Aerospace series - Analysis of non-metallic materials (cured) for the determination of the extent of cure by Differential Scanning Calorimetry (DSC).pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Aerospace series - Analysis of non-metallic materials (cured) for the determination of the extent of cure by Differential Scanning Calorimetry (DSC)BS EN 6064:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 606

2、4 December 2017 ICS 49.025.01 English Version Aerospace series - Analysis of non-metallic materials (cured) for the determination of the extent of cure by Differential Scanning Calorimetry (DSC) Srie arospatiale - Analyse Enthalpique Diffrentielle (AED) des matriaux non mtalliques (polymriss) pour l

3、a dtermination du degr de polymrisation Luft- und Raumfahrt - Analyse von nichtmetallischen Werkstoffen (gehrtet) zur Bestimmung des Vernetzungsgrades durch dynamische Differenzkalorimetrie (DSC) This European Standard was approved by CEN on 26 July 2017. CEN members are bound to comply with the CEN

4、/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 concerning such national standards may be obtained on application to the CEN-CENELEC Management Cen

5、tre 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 its own language and notified to the CEN-CENELEC Management Centre has the same status as th

6、e official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nether

7、lands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN

8、All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 6064:2017 ENational forewordThis British Standard is the UK implementation of EN 6064:2017.The UK participation in its preparation was entrusted to Technical Committee ACE/65, Non-metalli

9、c materials for aerospace purposes.A list of organizations represented 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 Insti

10、tution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 98311 5ICS 49.025.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 2018.Amendments/

11、corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 6064:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 6064 December 2017 ICS 49.025.01 English Version Aerospace series - Analysis of non-metallic materials (cured) for the determination of the extent of cure by Diffe

12、rential Scanning Calorimetry (DSC) Srie arospatiale - Analyse Enthalpique Diffrentielle (AED) des matriaux non mtalliques (polymriss) pour la dtermination du degr de polymrisation Luft- und Raumfahrt - Analyse von nichtmetallischen Werkstoffen (gehrtet) zur Bestimmung des Vernetzungsgrades durch dyn

13、amische Differenzkalorimetrie (DSC) This European Standard was approved by CEN on 26 July 2017. 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-d

14、ate 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 Standard exists in three official versions (English, French, German). A version in any other language made by translatio

15、n 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 the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Fo

16、rmer Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZAT

17、ION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 6064:2017 EBS EN 6064:2017EN 6064:2017 (E) 2 Co

18、ntents Page European foreword 3 Scope 4 Normative references 4 Symbols and definitions . 4 Principle of the method 4 Designation of the method . 5 Apparatus. 5 Test specimens . 6 Procedure 7 Presentation of the results 8 Test report . 8 Annex A (informative) Equipment . 11 A.1 Mettler TA 3000/TA 210

19、0 - DSC 20/DSC 30 11 A.2 DuPont 9900 . 11 A.3 Perkin Elmer DSC 2/DSC 4/DSC 7 . 11 BS EN 6064:2017EN 6064:2017 (E) 3 European foreword This document (EN 6064:2017) has been prepared by the Aerospace and Defence Industries Association of Europe - Standardization (ASD-STAN). After enquiries and votes c

20、arried out in accordance with the rules of this Association, this Standard has received the approval of the National Associations and the Official Services of the member countries of ASD, prior to its presentation to CEN. This European Standard shall be given the status of a national standard, eithe

21、r by publication of an identical text or by endorsement, at the latest by June 2018 and conflicting national standards shall be withdrawn at the latest by June 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be

22、 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, Croatia, Cyprus, Czech Republic, Denmark, Est

23、onia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 6064:201

24、7EN 6064:2017 (E) 4 Scope This test method defines the procedure for the estimation of the extent of cure of certain non-metallic materials (e.g. preimpregnated and neat resin systems, adhesives) for aerospace use. The extent of cure is estimated by Differential Scanning Calorimetry (DSC) measuremen

25、ts of uncured (reference) and cured materials. Additional evidence on the extent of cure may be gained by combining results from this method with those obtained by other techniques. This standard does not give any directions necessary to meet the health and safety requirements. It is the responsibil

26、ity of the user of this standard to adopt appropriate health and safety precautions. Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For und

27、ated references, the latest edition of the referenced document (including any amendments) applies. EN 2331, Aerospace series Textile glass fibre preimpregnates Test method for the determination of the resin and fibre content and mass of fibre per unit area EN 2559, Aerospace series Carbon fibre prei

28、mpregnates Determination of the resin and fibre content and the mass of fibre per unit area EN 2743, Aerospace series Fibre reinforced plastics Standard procedures for conditioning prior to testing unaged materials Symbols and definitions For the purposes of this document, the following symbols and

29、definitions apply. The determination of these parameters shall be agreed upon between manufacturer and purchaser in case of non-ideal curves or different instrument types. 3.1 curing reaction (see Figure 1) is the heating rate, in degrees Celsius or Kelvin by minutes; H is the reaction enthalpy, in

30、Joules by grams; H100is the reaction enthalpy corrected to 100 % resin content, in Joules by grams; A-curve is the reference reaction curve for uncured material; B-curve is the reaction curve for an already (semi-) cured sample. 3.2 calibration (see 6.6) Tmis the melting temperature, in degrees Cels

31、ius or Kelvin Hmis the enthalpy of fusion, in Joules by grams Principle of the method Differential Scanning Calorimetry (DSC) measures the temperatures and the heat flow associated with transitions in materials as a function of time and temperature. BS EN 6064:2017EN 6064:2017 (E) 5 Designation of t

32、he method The designation of the method used shall be drawn up according to the following example: Description block ANALYSIS OF NON-METALLIC MATERIALS DETERMINATION OF THE EXTENT OF CURE BY DIFFERENTIAL SCANNING CALORIMETRY (DSC) Identity block EN6064 Number of this standard Apparatus 6.1 The test

33、shall be performed in a Differential Scanning alorimeter (DSC) capable of operating within the limits laid down in the test procedure. Instruments are given in the Annex A of this standard. If the DSC-apparatus of the manufacturer and the purchaser are different, a cross-check for comparison of the

34、test results is necessary. 6.2 Balance with an accuracy of 0,01 mg. 6.3 Ancillary items such as sharp cutting knife and tweezers. 6.4 Nitrogen (dry, min. 99,99 % purity). 6.5 Hollow punch with a diameter 1 mm the diameter of the sample pan to cut out the required discs of adhesive, prepreg or lamina

35、te. 6.6 Calibration The equipment shall be controlled using a pure indium sample to maintain a temperature accuracy to 0,5 C and a calorimetric precision within 1 % during test. Periodically the temperature and cell constant shall be calibrated using pure samples of the materials specified in Table

36、1 (type and values according to DSC manufacturer recommendations). Temperature calibration shall be performed using two or preferably three materials over the temperature range of interest. The heating rate for calibration shall be the same as used in the subsequent experiments i.e. 10 C/min for sta

37、ndard operation (see Clause 8). The instrument calibration shall be performed using the same sample pan type, purge/purge rate and equivalent thermal mass samples as will be used in subsequent experiments. The base line and the cell shall be checked periodically (interval to be agreed between the pa

38、rties). The base line drift for a pair of empty pans or pans containing an inert substance shall not exceed 1,0 mW over the range 50 C to 300 C. BS EN 6064:2017EN 6064:2017 (E) 6 Test specimens 7.1 Preparation 7.1.1 General Test specimens shall be selected in accordance with the sampling procedure d

39、efined in the Material Specification. For the A-curve uncured samples, for the B-curve (semi-) cured samples shall be taken. Each sample shall comprise approximately the equivalent of 7 mg to 10 mg of neat resin (for example 20 mg of prepreg). In case of extreme enthalpy of reaction the sample size

40、of the material may be adjusted to achieve acceptable curves in the diagram. The sample mass shall be determined to 0,01 mg (see 6.2). For quantitative measurements it is necessary to correct the H to 100 % resin content (H100), the resin content shall be determined using the test methods of 7.1.2 o

41、r 7.1.3. A minimum of two test specimens shall be used for standard operations (e.g. release testing). For determination of standard deviations a minimum of six specimens are necessary (e.g. qualification programs). 7.1.2 Determination of actual fibre/resin content Carbon composite : according to EN

42、 2559; Glass composite : according to EN 2331; Aramid composite : according to EN 2559 but using HNO3/DMSO. If an insoluble filler (such as SiO2) is present, it shall be determined separately (after the removal of the fibre) by centrifuging and its mass added to the reinforcement content. 7.1.3 Dete

43、rmination of actual carrier/resin content for adhesives (uncured) Usual extraction technique: use ultrasonic bath and appropriate solvent such as DMF, DMSO, NMP. Determine the carrier weight after twice flushing with solvents such as Acetone or MEK and thorough drying. If an insoluble filler is pres

44、ent, it shall be determined separately (after the removal of the carrier) by centrifuging and its mass added to the reinforcement content. Actual resin content: mresin= madhesive mcarrier. 7.2 Conditioning 7.2.1 Conditioning of material stored at ambient temperature For material stored at ambient te

45、mperature, the amount of material required for testing shall be sampled and conditioned in the standard atmosphere (defined in EN 2743) for a minimum of 2 h, unless otherwise specified. BS EN 6064:2017EN 6064:2017 (E) 7 7.2.2 Conditioning of material stored below ambient temperature For material sto

46、red at temperatures lower than ambient temperature, the material, suitably packed in an airtight bag (containing a suitable desiccant) to prevent moisture pick-up, shall be allowed to reach ambient temperature over a period of time according to the mass of the package. The actual time shall be recor

47、ded in the report. When the material has reached ambient temperature, the amount (together with the release film on it) required for testing shall be sampled and conditioned in the standard atmosphere (defined in EN 2743) for a minimum of 2 h, unless otherwise specified. 7.2.3 Standard atmosphere fo

48、r testing The test equipment shall be at (23 2) C and (50 5) % relative humidity (EN 2743 B conditions). The actual test environment is controlled inside the equipment. 7.2.4 Time interval between conditioning and testing After conditioning, the test shall be carried out within 6 h, unless otherwise

49、 specified, the specimen being kept in the standard atmosphere until the test is carried out. Procedure 8.1 A-curve The sample shall be placed in a sample pan ensuring that it is in good thermal contact with the pan. The lid shall be firmly crimped on but not hermetically sealed to avoid pressure increase. Place the two pans containing the sample and the reference into the DSC cell (see 6.1 ), close the system and purge with pure dry nitrogen (preferred flow 20 ml/min to 30 ml/min). The following test conditions shall a