ASD-STAN PREN 2564-2017 Aerospace series Carbon fibre laminates Determination of the fibre resin and void contents (Edition P 2).pdf

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1、ASD-STAN STANDARD NORME ASD-STAN ASD-STAN NORM ASD-STAN prEN 2564 Edition P 2 May 2017 PUBLISHED BY THE AEROSPACE AND DEFENCE INDUSTRIES ASSOCIATION OF EUROPE - STANDARDIZATION Rue Montoyer 10 - 1000 Brussels - Tel. + 32 2 775 8126 - Fax. + 32 2 775 8131 - www.asd-stan.orgICS: Supersedes edition P 1

2、 of October 1988 and Will supersede EN 2564:1998 Descriptors: ENGLISH VERSION Aerospace series Carbon fibre laminates Determination of the fibre, resin and void contents Luft- und Raumfahrt Kohlenstofffaser-Laminate Bestimmung der Faser-, Harz- und Porenanteile Srie arospatiale Stratifis de fibres d

3、e carbone Dtermination de la teneur en fibres, en rsine et du taux de porosit This “Aerospace Series“ Prestandard has been drawn up under the responsibility of ASD-STAN (The AeroSpace and Defence Industries Association of Europe - Standardization). It is published for the needs of the European Aeros

4、pace Industry. It has been technically approved by the experts of the concerned Domain following member comments. Subsequent to the publication of this Prestandard, the technical content shall not be changed to an extent that interchangeability is affected, physically or functionally, without re-ide

5、ntification of the standard. After examination and review by users and formal agreement of ASD-STAN, the ASD-STAN prEN will be submitted as a draft European Standard (prEN) to CEN (European Committee for Standardization) for formal vote and transformation to full European Standard (EN). The CEN nati

6、onal members have then to implement the EN at national level by giving the EN the status of a national standard and by withdrawing any national standards conflicting with the EN. ASD-STAN Technical Committee approves that: “This document is published by ASD-STAN for the needs of the European Aerospa

7、ce Industry. The use of this standard is entirely voluntary, and its applicability and suitability for any particular use, including any patent infringement arising therefrom, is the sole responsibility of the user.” ASD-STAN reviews each standard and technical report at least every five years at wh

8、ich time it may be revised, reaffirmed, stabilized or cancelled. ASD-STAN invites you to send your written comments or any suggestions that may arise. All rights reserved. No parts of this publication may be reproduced, stored in a retrieval system or transmitted, in any form or by any means, electr

9、onic, mechanical, photocopying, recording, or otherwise, without prior written permission of ASD-STAN. Order details: E-mail: salesasd-stan.org Web address: http:/www.asd-stan.org/ Edition approved for publication 1stMay 2017 Comments should be sent within six months after the date of publication to

10、 ASD-STAN Material Domain Copyright 2017 ASD-STAN prEN 2564:2017 (E) 2 Contents Page Foreword 2 1 Scope 3 2 Normative references 3 3 Principle . 3 4 Apparatus and reagents 3 5 Specimens 4 6 Health, safety and environmental aspects . 4 7 Atmosphere for testing . 4 8 Procedure 4 9 Expression of result

11、s 7 10 Designation . 8 11 Test report . 9 Annex A (informative) Standard evolution form 10 Foreword This standard was reviewed by the Domain Technical Coordinator of ASD-STANs Material Domain. After inquiries and votes carried out in accordance with the rules of ASD-STAN defined in ASD-STANs General

12、 Process Manual, this standard has received approval for Publication. prEN 2564:2017 (E) 3 1 Scope This standard specifies the methods for determining the fibre content by volume and mass and, by correlation, the resin content by volume and mass and void content by volume, of carbon fibre laminates,

13、 for aerospace applications. 2 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 undated references, the latest edition of the referenced

14、document (including any amendments) applies. EN 2743, Aerospace series Fibre reinforced plastics Standard procedures for conditioning prior to testing unaged materials ISO 1183, Plastics Methods for determining the density and relative density of non-cellular plastics ISO 10119, Carbon fibre Determi

15、nation of density 3 Principle Determination of the difference in mass of specimens before and after extraction of the resin by sulphuric acid digestion. Two methods are applicable: Method A is the reference method, Method B is a simplified method. 4 Apparatus and reagents 4.1 Balance accurate to 0,1

16、 mg. 4.2 Tweezers. 4.3 Cutting device, such as a diamond blade saw or any other suitable apparatus. 4.4 250 ml double necked pear-shaped flask equipped with 50 ml dropping funnel, air inlet and a water pump. 4.5 Beakers of various capacities, including 400 ml. 4.6 20 ml sintered glass crucible (n 2

17、porosity) and suitable filtration assembly. 4.7 Desiccator containing a suitable drying agent (for example silica gel, calcium chloride or phosphorus pentoxide). 4.8 Concentrated sulphuric acid (specific gravity: 1,84 to 1,89). 4.9 Hydrogen peroxide solution (300 g/l to 500 g/l). 4.10 Acetone (propa

18、none). prEN 2564:2017 (E) 4 4.11 Distilled water 4.12 Heat source with suitable temperature control. 4.13 Fume cupboard (for method B, see 8.2). 4.14 Thermometer capable of measuring 300C. 4.15 Sand bath or equal (for method B, see 8.2). 4.16 Electric oven capable of maintaining a temperature of (12

19、0 5) C. 4.17 Protective clothing, including rubber gloves, for handling hydrogen peroxide and sulphuric acid solutions. 4.18 Safety screen. 5 Specimens 5.1 Shape and dimensions The samples size shall be adjusted to reach minimum 1 5 g sample weight. Specimens of different dimensions may be used, sub

20、ject to agreement between the user and manufacturer. 5.2 Number and distribution If not other specified a minimum of three specimens shall be used. These shall be evenly distributed in the laminate and cut at least 10 mm from its edges. 6 Health, safety and environmental aspects This standard may in

21、volve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory

22、limitations prior to use. 7 Atmosphere for testing According to EN 2743 B. 8 Procedure Use protective clothing and rubber gloves for handling hydrogen peroxide and sulphuric acid solutions. Alternatively other acids can be agreed by the user and manufacturer, for example nitric acid. Appropriate hea

23、lth and safety measures including modifications to the procedures below will need assessing and documenting by the test-house associated with the different solution. The reactions shall be carried out behind the safety screen for eye protection. prEN 2564:2017 (E) 5 8.1 Method A 8.1.1 Dry the specim

24、ens to constant mass in the desiccator that is until the difference in mass of two successive weighing is less than 2 mg. Record m1. 8.1.2 Determine the density (c) of each specimen in accordance with ISO 1183, method A. 8.1.3 Drop the specimen into the double necked, pear-shaped flask and carefully

25、 pour 20 ml of concentrated sulphuric acid into the flask. Fit the dropping funnel to one neck and the water pump to the other. 8.1.4 Pour a suitable amount of the hydrogen peroxide solution (e.g. 20 ml of 500 g/l concentration or 40 ml of 300 g/l concentration) into the dropping funnel and heat the

26、 flask . Depending of the material it is recommended to use following temperatures: Resin systems cured at 5 g. 8.2.4 Place each beaker on the sand bath or equal and start the heating. The temperature of disaggregation has to be adjusted depending of the material. It is recommended to use following

27、temperatures: Resin systems cured at 5 g The solution becomes clear and the fibres rise to the surface. Start heating until the evolution of gas ceases and white fumes of sulphur trioxide re-appear. If the solution becomes dark again, repeat the operation. 8.2.6 When the solution remains clear, remo

28、ve the beakers from the sand bath and allow them to cool down to ambient temperature. 8.2.7 Pour the contents of each beaker into a 400 ml beaker containing 100 ml of distilled water; wash with distilled water any fibres adhering to the first beaker into the second. prEN 2564:2017 (E) 7 8.2.8 Filter

29、 the contents of each beaker through a sintered glass crucible, previously dried and weighed (m2), washing the beaker and contents of the crucible with distilled water until the washings are free from acid, then wash with 10 ml of acetone or ethanol. After washing a visual check has to be performed.

30、 The fibres must be free of resin or adhesive. The fibres must be free of tack. If not repeat the steps 8.2.4 to 8.2.8. 8.2.9 Dry the crucible and contents at 120 C for at least 45 min, cool down to standard atmosphere in a desiccator and weigh (m3) to 1 mg. 9 Expression of results 9.1 Fibre content

31、 by mass (Wf) 1 23f )(100 m mmW where Wf is the fibre content as a percentage of the initial mass; m1 is the initial mass of the specimen, in grams; m2 is the mass of the sintered glass crucible, in grams; m3 is the final total mass of the sintered glass crucible and the residue after acid digestion

32、, in grams. 9.2 Fibre content by volume (Vf) fcff WVwhere Vf is the fibre content as a percentage of the initial volume; Wf is the fibre content as a percentage of the initial mass; c is the specimen density, in grams per cubic centimetre; f is the fibre density, in grams per cubic centimetre, deter

33、mined to ISO 10119 or given the suppliers release report. 9.3 Resin content by mass (Wr) Wr 100 Wf where Wr is the resin content as a percentage of the initial mass; - prEN 2564:2017 (E) 8 Wf is the fibre content as a percentage of the initial mass. 9.4 Resin content by volume (Vr) rcfr )100( WVwher

34、e Vr is the resin content as a percentage of the initial volume; Wf is the fibre content as a percentage of the initial mass; c is the specimen density expressed, in grams per cubic centimetre; r is the density of the cured resin, in grams per cubic centimetre, determined to ISO 1183 (method A) on a

35、 cured resin specimen or given in the suppliers report. 9.5 Void content by volume (Vo) rcffcfo )100(100 WWV where Vo is the void content as a percentage of the initial volume; Wf is the fibre content as a percentage of the initial mass; c is the specimen density, in grams per cubic centimetre; f is

36、 the fibre density, in grams per cubic centimetre, determined to ISO 10119 or given in the suppliers release report; r is the density of the cured resin, in grams per cubic centimetre, determined to ISO 1183 (method A) on a cured resin specimen or given in the suppliers release report. NOTE The abso

37、lute error in the determination of void content is estimated to be 1 %, due to uncertainties accumulated in the densities. 10 Designation EXAMPLE EN 2564 A Number of this standard Test method (see 3) prEN 2564:2017 (E) 9 11 Test report It shall include the following: designation (see 10); all data e

38、nsuring the traceability of the material (trade mark, identification marking, date of receipt, batch number, etc.); all information regarding the sampling procedure; specimen dimensions if these differ from 5.1; the fibre and resin contents by volume and mass and the void content by volume; individu

39、al values and arithmetic means; any incident which may have affected the results; agreed deviations to the method quoted. prEN 2564:2017 (E) 10 Annex A (informative) Standard evolution form The main changes with respect to the previous edition are listed in Table A.1. Table A.1 Main changes to previ

40、ous edition prEN/EN Number Edition Publication Date Modification Reason and validation prEN 2564 P1 1/08/1998 4.14 scale of the thermometer To control the higher temperature of the disaggregation another scale of the thermometer is requested. 5.1 sample size A specific sample dimension is needed. A sample size by mass is more efficient. 8.2 modification of - quantity of solvent - temperature of disaggregation