ASD-STAN PREN 6032-1995 Aerospace Series Fibre Reinforced Plastics Test Method Determination of the Glass Transition Temperatures (Edition P1)《航空航天系列 纤维增强塑料的试验方法 玻璃态转化温度的测定 第P1版》.pdf

1、 AECMA PRENub032 95 LOLE!3LL 0009984 597 Edition approved for publication 1995-1 1-30 AECMA STANDARD NORME AECMA AECMA NORM Comments should be sent within six months after the date of publication to AECMA Gulledelle 94 AIB/TF6 Chairman Mr K. Schneider E-1 200 BRUXELLES prEN 6032 Edition PI November

2、1995 PUBLISHED BY THE EUROPEAN ASSOCIATION OF AEROSPACE INDUSTRIES AECMA) Gulledelle 94 - 13-1 200 BRUXELLES - Tel. (32) 2 775 81 10 - Fax. (32) 2 775 81 11 ICs : Descriptors : ENGLISH VERSION Aerospace series Fibre reinforced plastics Test method Determination of the glass transition temperatures S

3、rie arospatiale Matires plastiques renforces de fibres Mthode dessai Dtermination de la temprature de transition vitreuse Luft- und Raumfahrt Faserverstrkte Kunststoffe Prf verf ahren Bestimmung der Glasbergangstemperatur This “Aerospace Series“ Prestandard has been drawn up under the responsibility

4、 of AECMA (The European Association of Aerospace Industries). It is published on green paper for the needs of AECMA-Members. It has been technically approved by the experts of the concerned Technical Committee following comment by the Member countries. Subsequent to the publication of this Prestanda

5、rd, the technical content shall not be changed to an extent that interchangeability is affected, physically or functionally, without re-identification of the standard. After examination and signature of the AECMA Standard Checking Centre (NPS) and formal agreement of the Official Services of the Mem

6、ber countries it will be submitted as a draft European Standard to CEN (European Committee for Standardization) for formal vote. - AECNA PREN*b032 95 W I10123LL 0009985 423 Page 2 prEN 6032 : 1995 Contents list 1 2 3 4 5 6 7 8 9 10 Scope Normative references Definitions Principle of the method Desig

7、nation of the method Apparatus Test specimen Procedure Presentation of the results Test report Annex A Equipment Page 3 prEN 6032 : 1995 1 Scope This standard specifies a method to determine the apparent glass transition temperatures of non metallic materials. This standard is applicable to unidirec

8、tional tape and woven fabric reinforced plastic or plastic materials like adhesive or neat resin for comparison of the influence on the glass transition temperature resulting from processing-parameters of non metallic parts, for compatibility tests for checking Co-curing effects of different prepreg

9、 types or with adhesive This standard does not give any directions necessary to meet health and safety requirements. It is the responsibility of the user of this standard to consult and establish appropriate health and safety precautions. 2 Normative references This European Standard incorporates by

10、 dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Stand

11、ard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. EN 2374 Aerospace Series Glass fibre reinforced mouldings and sandwich composites Production of test panels EN 2565 Aerospace Series Preparation of carbon fibr

12、e reinforced resin panels for test purposes. ) EN 2743 Aerospace Series Reinforced Plastics Standard procedures for conditioning prior to testing.4) EN 2823 Aerospace Series Fibre Reinforced Plastics Test method for determination of the effect of exposure to humid atmospheres on physical and mechani

13、cal characteristics. ) 3 Definitions 3.1 Glass Transition Temperature ( Tg 1 The glass transition temperature is defined for this sta dard as th temperature where th sample exhibits a dramatic change in mechanical and damping behaviour with increasing temperature when subjected to an oscillating dis

14、placement. The Tg values are determined by measuring sample stiffness (storage modulus) and damping (loss modulus/ tan 6) with increasing temperature using a recommended Dynamic Mechanical Analysis (DMA) instrument and evaluating the plots against temperature (see figure 1). I Published as AECMA Pre

15、standard at the date of publication of this standard Page 4 prEN 6032 : 1995 3.1 .l Tg-onset The Tg-onset is defined as the temperature intersection of extrapolated tangents drawn from points on the storage modulus curve before and after the onset of the glass transition event. 3.1.2 Tg-loss The Tg-

16、loss is defined as the temperature where the diagram loss modulus versus temperature has its maximum. 3.1.3 Tg-peak The Tg-peak is defined as the temperature where the diagram tan 6 (damping) versus temperature has its maximum. 3.2 Slope angle B is the angle of the slope of the storage modulus repre

17、sented by tangent A. (see figure 1 I 4 Principle of the method Using specially designed equipment of the DMA type the storage modulus , loss modulus and the tan delta (damping) of a flat plastic sample is automatically measured and plotted while the temperature of the specimen is raised, at a define

18、d heating rate. Plots of moduli against temperature are evaluated according to the prescribed procedures to determine Tg-onset, Tg-loss and Tg-peak which give an indication of the maximum service temperature of the material tested. The slope angle of the storage modulus estimates the drop of mechani

19、cal properties due to temperature effects. 4.1 Method A The equipment is set to fixed frequency mode at 1 Hz. 4.2 Method B The equipment is set ot resonant frequency mode, initial frequency shall be 20 - 50 Hz. 4.3 Method C Freely damped torsion pendulum. 5 Designation of the method The designation

20、of the method used shall be drawn up according to the following example Description block I Identity block Non metallic materials Glass Transition Temperature (Tg) Number of the standard f Method (see chapter 4.1 - 4.3) AECMA PREN*b032 95 = LOL23Ll 0009988 L32 Page 5 prEN 6032 : 1995 It should be st

21、ated that moduli measured by this method shall not be used for design purposes. The results obtained by this method vary due to the equipment used. For comparing results the involved parties shall agree on the equipment used, correlation factors to compare results of different equipment and the spec

22、ific material requirements. A list of recommended equipment is given in annex A of this standard. When this method is involved in a material specification, with material requirements the relevant test equipment according to annex A shall be stated. 6 Apparatus 6.1 Equipment of the dynamic mechanical

23、 analysis type with bending and/or torsional/shear loading of the specimen, capable of testing and recording frequency, storage modulus, loss modulus, tan delta and temperature in the ranges used. Recommended instruments are given in annex A of this standard. 6.2 Micrometer with 6 mm flat faces and

24、accurate to the nearest 0,Ol mm. 6.3 Vernier caliper accurate to the nearest 0,l mm. 7 Test specimen 7.1 Test specimen description The test specimen can consist of either unidirectional tape, woven fabric or adhesiveheat resin. The fibre orientation is O* for tape and warp for fabric. Dimensions: Th

25、ickness: Width and length of the specimen shall be chosen in accordance with the requirements of the test equipment used. 2 -t 0,2 mm (if not otherwise specified) or the nearest ply if fabric material is used 7.2 Test specimen preparation The specimens are cut out of plates. The coefficient of varia

26、tion in thickness measurements shall be e 2 % per plate. Where relevant the reinforced plates shall be manufactured in accordance with EN 2565 (CFRP) or EN 2374 (GFRP). The process parameters shall be in accordance with the applicable Technical Specification. Precautions shall be taken to avoid notc

27、hes, undercuts, rough or eneven surfaces after machining. 7.3 Number of test specimens Three specimens shall be tested per test condition, except when otherwise specified in the applicable Technical Specification. If tests are carried out after ageing or at a temperature different from room tempera-

28、 ture, care should be taken to ensure that room temperature/dry reference specimens which have been machined from the same plate as the specimen under investigation are also tested. AECMA PREN*b032 95 W LOL23LL 0009989 079 Page 6 prEN 6032 : 1995 7.4 Ageing of specimen In case of tests after exposur

29、e to humid atmosphere, the conditioning shall be according to EN 2823. 8 Procedure 8.1 Conditioning Prior to test cured specimens shall be stored at (23 f 2) OC and (50 f 5) % relative humidity in accordance with EN 2743. Aged specimens shall be tested directly after the ageing procedure (a maximum

30、delay of 8 hours at (23 f 2) OC is allowed). 8.2 Determination of dimensions Before ageing and mechanical testing measure and record the thickness and width at 3 points in the non- gripping area of the specimen. Use for the thickness the micrometer (see 6.2) and for the width the vernier caliper (se

31、e 6.3) or the micrometer (see 6.2). 8.3 Calibration The equipment shall be calibrated according to the manufacturers instructions. The temperature calibration shall be carried out using Tg-loss peaks of agreed grades of, Polycarbonate Tg-loss, 153 I 1 OC Polyethersulphone - Tg-losS, 221 I l0C 8.4 Te

32、sting The relevant test parameters shall be used: Temperature Heating rate Room temperature to, at least, 20 OC higher than point L or M, see Figure 1. 5 I 0,2 OC/min (3 OC/min optional) - Specimen dimensions : Actual Clamp the specimen firmly in the sample holder of the equipment used according to

33、the manufacturers instructions. Perform the test according to the manufacturers instructions. 9 Presentation of the results , 9.1 Diagram The test results shall be plotted in a diagram according to figure 1, showing storage modulus, loss modulus and tan delta (optional) versus temperature. 9.2 Deter

34、mination of Tg-onset The Tg-onset shall be determined by introducing two tangents into the diagram of the storage modulus curve, see figure 1. AECMA PRENub032 95 LOL23LL 0009990 890 Page 7 prEN 6032 : 1995 The first one (tangent A) representing the linear area of the curve from the start temperature

35、 up to the beginning of the dramatic slope of the curve. The second one (tangent BI shall be the tangent left of the point of inflection (= tg loss) on the decreasing part of the curve (see typical diagram figure 1 I. Both tangents shall be extended to intersect in point C. The temperature related t

36、o point C shall be the Tg-onset. 9.3 Determination of Tg-loss Tg-loss is the temperature which corresponds to the maximum of the loss modulus curve (point L in figure 1) 9.4 Determination of Tg-peak (optional) Tg-peak is the temperature which corresponds to the maximum tan-6 (point M in figure 1). 9

37、.5 Determination of the slope angle (optional) Evaluate the slope of the storage modulus curve which is represented by tangent A according to 9.2 (see figure 1 ). Determine by the given formula: = arc tan AEIAT 9.6 Quantitative check Tg results should be within f 2,O OC of their mean. If greater, th

38、e results should be scrutinized to see if they are acceptable. 10 Test report The test report shall refer to this standard and include the following: 10.1 Complete identification of the material tested, including at least: material designation, supplier, batch number, roll number, fibre areal weight

39、, filament count, processing details, stacking sequence, test orientation. 10.2 All details regarding specimen preparation including cure parameters 10.3 The measured specimen dimensions 10.4 Ageing and/or exposure condition prior to the test 10.5 Date of test, facility and identification of individ

40、uals performing the tests. 10.6 Equipment, method and test parameters used including: Displacement amplitude, strain fequency, strain rate 10.7 Plot of storage modulus, loss modulus and tan delta (optional) versus temperature, the tangents A and B and the points C, L and M according to figure 1. 10.

41、8 Individual test results of Tg-onset, Tg-loss, Tg-peak (optional) and (optional). 10.9 Any incident which may have affected the results and any deviation from this standard. AECMA PRENJb032 95 3032333 O009993 727 Page 8 prEN 6032 : 1995 i c O a cp m AECMA PRENrb032 95 LOL23LL O009992 bb3 = Page 9 p

42、rEN 6032 : 1995 Annex A : Equipment The following equipment may be used to determine Glass Transition Temperature A. 1 A.2 A.3 A.4 A.5 PL-DMTA dynamic Mechanical Thermal Analyer The Technology Centre Epinal Way Loughborough LE 11 OQE U.K. 981 /982/983 DMA Dynamic Mechanical Analyser TA Instruments Silver Side Road Wiimington, U.S.A. A.T.M. 3 torsion Pendulum, Myrenne GmbH 5 106 Roetgen Federal Republic of Germany Torsiomatic torsion Pendulum, Zwick GmbH + Co. 7900 Ulm Federal Republic of Germany RDS 7700 Rheometrics inc. 2438 US Hwg 22 Union NJ O7083 USA