EN 6041-2018 Aerospace series - Non-metallic materials - Test method - Analysis of non-metallic materials (uncured) 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 - Non-metallic materials - Test method - Analysis of non-metallic materials (uncured) by Differential Scanning Calorimetry (DSC)BS EN 6041:2018EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 6041 J

2、anuary 2018 ICS 49.025.01 English Version Aerospace series - Non-metallic materials - Test method - Analysis of non-metallic materials (uncured) by Differential Scanning Calorimetry (DSC) Srie arospatiale - Matriaux non mtalliques - Mthode dessai - Analyse Enthalpique Diffrentielle (AED) des matriau

3、x non mtalliques (non polymriss) Luft- und Raumfahrt - Nichtmetallische Werkstoffe - Prfverfahren - Analyse von nichtmetallischen Werkstoffen (ungehrtet) mittels dynamischer Differenzkalorimetrie (DSC) This European Standard was approved by CEN on 28 August 2017. CEN members are bound to comply with

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

5、ment 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 its own language and notified to the CEN-CENELEC Management Centre has the same stat

6、us as the 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

7、, Netherlands, 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: Rue de la Science 23, B-1040 Brusse

8、ls 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 6041:2018 ENational forewordThis British Standard is the UK implementation of EN 6041:2018.The UK participation in its preparation was entrusted to Technical Committee ACE/61/

9、-/6, Mechanical Testing of Metallic 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 applic

10、ation. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 98578 2ICS 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 Commit

11、tee on 28 February 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 6041:2018EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 6041 January 2018 ICS 49.025.01 English Version Aerospace series - Non-metallic materials - Test method - Analysis of non-metall

12、ic materials (uncured) by Differential Scanning Calorimetry (DSC) Srie arospatiale - Matriaux non mtalliques - Mthode dessai - Analyse Enthalpique Diffrentielle (AED) des matriaux non mtalliques (non polymriss) Luft- und Raumfahrt - Nichtmetallische Werkstoffe - Prfverfahren - Analyse von nichtmetal

13、lischen Werkstoffen (ungehrtet) mittels dynamischer Differenzkalorimetrie (DSC) This European Standard was approved by CEN on 28 August 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 nat

14、ional 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 Standard exists in three official versions (English, French, German). A ve

15、rsion 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 the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus,

16、 Czech Republic, Denmark, Estonia, 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 Unite

17、d Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No.

18、EN 6041:2018 EBS EN 6041:2018EN 6041:2018 (E) 2 Contents Page European foreword 3 1 Scope 4 2 Normative references 4 3 Symbols and definitions . 4 4 Principle of the method 5 5 Designation of the method . 5 6 Apparatus. 5 7 Test specimens . 6 8 Procedure 8 9 Presentation of the results 8 10 Test rep

19、ort . 8 Annex A (informative) Equipment . 13 A.1 Mettler TA 3000/TA 2100 - DSC 20/DSC 30 13 A.2 DuPont 9900 . 13 A.3 Perkin Elmer DSC 2/DSC 4/DSC 7 . 13 BS EN 6041:2018EN 6041:2018 (E) 3 European foreword This document (EN 6041:2018) has been prepared by the Aerospace and Defence Industries Associat

20、ion of Europe - Standardization (ASD-STAN). After enquiries and votes carried 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 Eu

21、ropean 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 2018, and conflicting national standards shall be withdrawn at the latest by July 2018. Attention is drawn to the possibility that some of the element

22、s 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 standards organisations of the following countries are bound to implement this Europ

23、ean Standard: 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, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovak

24、ia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 6041:2018EN 6041:2018 (E) 4 1 Scope This test method defines the procedure for the determination of the curing-characteristic and glass transition temperature of non-metallic materials (e.g. preimpregnated and neat resin

25、systems, adhesives) for aerospace use by Differential Scanning Calorimetry (DSC). The results obtained by this method may be useful for: derivation of the optimum cure cycle (only together with other test methods e.g. Tg determination) assessment of the condition of the resin assessment of the agein

26、g behavior of the resin This European Standard does not give any directions necessary to meet the health and safety requirements. It is the responsibility of the user of this European Standard to adopt appropriate health and safety precautions. 2 Normative references The following documents, in whol

27、e or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 2331, Aerospace series Textile glass

28、 fibre preimpregnates Test methods for the determination of the resin and fibre content and mass of fibre per unit area EN 2559, Aerospace series Carbon fibre preimpregnates Determination of the resin and fibre content and the mass of fibre per unit area EN 2743, Aerospace series Fibre reinforced pl

29、astics Standard procedures for conditioning prior to testing unaged materials 3 Symbols and definitions For the purposes of this document, the following symbols and definitions apply. The determination of these parameters shall be agreed upon between manufacturer and purchaser in case of non-ideal c

30、urves or different instrument types. BS EN 6041:2018EN 6041:2018 (E) 5 3.1 curing reaction (see Figure 3) is the heating rate, in C /min or K /min; Tos is the onset temperature, in C or K; Tp is the peak maximum temperature, in C or K; H is the reaction enthalpy, in J/g; H100is the reaction enthalpy

31、 corrected to 100 % resin content, in J/g. 3.2 calibration (see 6.5) Tmis the melting temperature, in C or K; Hmis the enthalpy of fusion, in J/g. 3.3 glass transition (see Figure 2) Tgosis the onset temperature of transition, in C or K; Tgeis the end temperature of transition, in degrees C or K; Tg

32、 is the glass transition temperature, in degrees C or K. 4 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. 5 Designation of the method The designation of the me

33、thod used shall be drawn up according to the following example: Description block ANALYSIS OF NON-METALLIC MATERIALS (UNCURED) BY DIFFERENTIAL SCANNING CALORIMETRY (DSC) Identity block EN6041 Number of this standard 6 Apparatus 6.1 The test shall be performed in a Differential Scanning Calorimeter (

34、DSC) capable of operating within the limits laid down in the test procedure. Instruments are given in the Annex A of this European Standard. If the DSC-apparatus of the manufacturer and the purchaser are different, a cross-check for comparison of the test results is necessary. 6.2 Balance with an ac

35、curacy of 0,01 mg. BS EN 6041:2018EN 6041:2018 (E) 6 6.3 Ancillary items such as sharp cutting knife and tweezers. 6.4 Nitrogen (dry, min. 99,99 % purity). 6.5 Calibration. The equipment shall be controlled using a pure indium sample to maintain a temperature accuracy to 0,5 C and a calorimetric pre

36、cision within 1 % during test. Periodically the temperature and cell constant shall be calibrated using pure samples of the materials specified in Table 1 (type and values according to DSC manufacturer recommendations). Temperature calibration shall be performed using two or preferably three materia

37、ls over the temperature range of interest. Sub-ambient temperature operation shall be achieved by the application of sub-ambient accessories specifically designed for use with the particular instrument being used (see Clause 8). For sub-ambient operations ice (H2O or cyclohexane) shall also be used

38、for calibration (the starting temperature shall be below 40 C). The heating rate for calibration shall be the same as used in the subsequent experiments i.e. 10 C/min for standard operation (see Clause 8). The instrument calibration shall be performed using the same sample pan type, purge/purge rate

39、 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 parties). The base line drift for a pair of empty pans or pans containing an inert substance shall not exceed 1,0 mW over the ra

40、nge 50 C to 300 C. 7 Test specimens 7.1 Preparation 7.1.1 General Test specimens shall be selected in accordance with the sampling procedure defined in the material specification. Each sample shall comprise approximately the equivalent of 7 mg to 10 mg of neat resin (for example 20 mg of prepreg). I

41、n case of extreme enthalpy of reaction the sample size 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 conten

42、t shall be determined using the test methods of 7.1.2 or 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 (i.e. qualification programs). BS EN 6041:2018EN 6041:2018 (

43、E) 7 7.1.2 Determination of actual fibre/resin content Carbon composite : according to EN 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

44、of the fibre) by centrifuging and its mass added to the reinforcement content. 7.1.3 Determination of actual carrier/resin content for adhesives Usual extraction technique: use ultrasonic bath and appropriate solvent such as DMF, DMSO, NMP. Determine the carrier weight after twice flushing with solv

45、ents such as acetone or MEK and thorough drying. If an insoluble filler is present, 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 mcarrier7.2 Conditioning 7.2.1 Conditionin

46、g of material stored at ambient temperature For material stored at ambient temperature, the amount of material (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

47、. 7.2.2 Conditioning of material stored below ambient temperature For material stored 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 p

48、eriod of time according to the mass of the package. The actual time shall be recorded 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 27

49、43) for a minimum of 2 h, unless otherwise specified. 7.2.3 Standard atmosphere for 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 specified, the specimen being kept in the standard atmosphere until the test is carried out. BS EN 6041:2018EN 604