1、AECIA PREN*bOLi3 95 LOL23LL 0010055 230 AECMA STANDARD prEN 6043 NORME AECMA Edition PI AECMA NORM November 1995 PUBLISHED BY THE EUROPEAN ASSOCIATION OF AEROSPACE INDUSTRIES (AECMA) Gulledelle 94 - B-1200 BRUXELLES - Tel. 132) 2 775 81 10 - Fax. (32) 2 775 81 11 ICs : Descriptors : ENGLISH VERSION
2、Aerospace series Thermosetting resin systems Test method Determination of gel time and viscosity Srie arospatiale Systmes thermodurcissables Mthode dessai Luft- und Raumfahrt Duromere Harzsysteme Prf verf ahren Dtermination du temps de gel et de la .SCOS- Bestimmung von Gelierzeit und .,ositt This “
3、Aerospace Series Prestandard has been drawn up under the responsibility 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 b
4、y the Member countries. 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-identification of the standard. After examination and signature of the AECMA Standard Checkin
5、g Centre INPSI and formal agreement of the Official Services of the Member countries it will be submitted as a draft European Standard to CEN (European Committee for Standardization) for formal vote. Nota - Extra copies can be supplied by B.N.A.E. - Technopolis 54 - 199, rue Jean-Jacques Rousseau -
6、921 38 ISSY-LES-MOULINEAUX CEDEX Comments should be sent within six months after the date of publication to I Edition approved for publication 1995-1 1-30 AECMA Gulledelle 94 B-1200 BRUXELLES AIB/TFG Chairman Mr K. Schneider AECMA PRENab043 95 1012311 00100.56 177 D Page 2 prEN 6043 : 1995 Contents
7、list 1 Scope 2 Normative references 3 Definitions 4 Principle of the method 5 Designation of the method 6 Apparatus 7 Test specimen 8 Procedure 9 Presentation of the results 10 Test report Annex A Equipments AECMA PREN*b043 95 1012311 OOL0057 003 Page 3 prEN 6043 : 1995 1 Scope This test standard de
8、fines the procedure for the determination of the viscosity and gel time of thermosetting resin systems by using several experimental techniques (see Table 1). The results obtained under dynamic and/or isothermal conditions, may be used to control the processing of resin systems during the cure cycle
9、. This standard does not give any directions necessary to meet the health and safety requirements. It is the responsibility of the user of this standard to adopt appropriate health and safety precautions. 2 Normative references This European Standard incorporates by dated or undated reference, provi
10、sions 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 Standard only when incorporated in it b
11、y amendment or revision. For undated references the latest edition of the publication referred to applies. EN 6041 Aerospace Series Non-metallic materials Test method for the analysis of non-metallic materials (uncured) by Differential Scanning Calorimetry (DSC). 3 Definitions 3.1 viscosity The resi
12、stance of a fluid to shear forces, and hence to flow. 3.2 Neat resin (or resin system or resin mix) A material compounded basically of resin + filler(s1 + (additive or catalytic system or hardener or accelerator) + thinner. 3.3 Gelation Irreversible transformation of thermosets from a viscous liquid
13、 to an elastic gel. 4 Principle of the method The characterisation of the curing phenomena of thermosetting resin systems can be carried out by several techniques, see table 1 : 4.1 Rheometry Measures the resin viscosity as a function of time and/or temperature. ) Published as AECMA Prestandard at t
14、he date of publication of this standard - AECMA PREN*b043 95 W 10L2311 0010058 T4T W Page 4 prEN 6043 : 1995 4.2 FisherJohns apparatus Allows the monitoring of changes in resin mobility as a function of time under isothermal conditions. 4.3 Differential scanning calorimetry (DSC) Measures the heat f
15、low associated with the curing reaction of thermosets as a function of time and/or temperature. 4.4 Thermomechanical analysis (TMA) Measures the sample deformation under an alternating load as a function of time and/or temperature. It may be used to indicate relative viscosity from the amount of mov
16、ement permitted. 5 Designation of the method The designation of the method used shall be drawn up according to the following example: Description block I Identity block Determination of gel time and viscosity I EN 6043 A IT Number of this standard I Method of test (see table 1) 6 Apparatus The perti
17、nent apparatus and its calibration is described in the methods presented in paragraph 8. If the test equipment and/or test methods used by the supplier and the customer are different, a cross-check for comparison of the test results is necessary. 7 Test specimens 7.1 Conditioning 7.1.1 Material stor
18、ed 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 at (23 k 2)OC and (50 -c 51% relative humidity for a minimum of 2h and a maximum of 6h, unless otherwise specified
19、. 7.1.2 Material stored below ambient temperature For material stored at temperatures lower than ambient temperature, the material (suitably packed in an airtight and solvent resistant bag to prevent moisture pick-up) shall be allowed to reach ambient temperature over a period of time according to t
20、he mass of the package. When the material has reached the ambient temperature, the amount of material (together with the relc film on it) required for testing shall be sampled and conditioned at (23 k 2)OC and (50 k 51% rela humidity for a minimum of 2h and a maximum of 6h, unless otherwise specifie
21、d. Page 5 prEN 6043 : 1995 8 Procedure Several experimental techniques are used and, therefore, different procedures can be applied. The methods) to be applied will be given by the material specification. 8.1 Viscosity profile of thermosetting resin systems (method A) 8.1.1 Apparatus The test shall
22、be performed on a parallel plate dynamic spectrometer capable of operating within the limits laid down in the test procedure. Instruments are given in the Annex A of this standard. 8.1.2 Calibration 8.1.2.1 Viscosity calibration Viscosity calibration shall be carried out by using standard fluids wit
23、h viscosities in the range of expected minimum viscosity (q min) or by applying a known torque using calibrated weights, following the manufacturers instructions. 8.1.2.2 Temperature calibration Temperature calibration shall be performed by using high purity metal standards or by using calibrated re
24、ference thermocouples. Correction factors may be required when calibration is carried out in a dynamic mode and the equipment is operated in an isothermal mode. 8.1.3 Sample preparation 8.1.3.1 Neat resin and unsupported adhesives No sample preparation is required. 8.1.3.2 Prepregs and supported adh
25、esive samples (adhesive + carrier) Unless otherwise agreed, circular specimens (25 mm ) shall be cut with a die to avoid rough edges and wrinkles in the material. 8.1.3.3 Supported adhesive resin It may be prepared by buckling at low temperature (liquid nitrogen). 8.1.4 Procedure 8.1.4.1 Preparation
26、 Pre-heat the plates at the required starting temperature and place the sample on the lower plate of the apparatus. The amount of sample or number of circular specimens to be piled shall be such that a gap of approximately 0,5 mm is attained. AECMA PREN*b043 95 = LOL23LL 00L00b0 bTB Page 6 prEN 6043
27、 : 1995 8.1.4.2 Equipment setting -shear rate : 10 rad/s - strain 10% 8.1.4.3 Test conditions Temperature range : Heating rate : 2OC/min standard, unless otherwise specified. From 5OoC to Tgel + 10C. Combination of dynamic and isothermal conditions is also possible. 8.1.4.4 Recording A continuous re
28、cord, or sufficient readings, shall be obtained to plot the viscosity versus the whole range of temperatures (see figure 2). 8.2 Gel time by monitoring the viscosity profile of thermosetting resin systems (method B) 8.2.1 Apparatus (see 8.1.1 .) 8.2.2 Calibration (see 8.1.2.) 8.2.3 Sample preparatio
29、n Prepregs and supported adhesives shall be prepared by cutting circular specimens (25 mm 9) with a die, unless otherwise agreed. 8.2.4 Procedure 8.2.4.1 Isothermal procedure 8.2.4.1.1 Preparation Pre-heat the plates at the required test temperature (see 8.2.4.1.3) and place the sample on the lower
30、plate of the apparatus. The number of circular specimens to be piled shall be such that a plate to plate gap of approximately 0,5 mm is attained. 8.2.4.1.2 Equipment setting - shear rate : 10 rad/s - strain 10% 8.2.4.1.3 Test conditions The test temperature shall be selected in order to preferably o
31、btain gel times in the range of 15-30 minutes. This temperature has to be agreed by the supplier and the customer before the commencement of the testing programme. Recommended testing temperatures are 160OC for 18OOC cure materials and 1 10C for 12OOC cure materials. AECMA PRENxbOLi3 95 9 1012311 00
32、100bL 53Y = Page 7 prEN 6043 : 1995 8.2.4.2 Dynamic procedure Follow the procedure described in paragraph 8.1.4. Note that the monitoring of the viscosity profile and the determination of the gel time under dynamic conditions, only differ in the evaluation of the results. 8.2.4.3 Recording A continu
33、ous record, or sufficient readings, shall be obtained to plot the viscosity versus time or temperature (see figures 3a and 3b). 8.3 Gel time of thermosetting resin systems : FisherJohns technique (method Cl 8.3.1 Apparatus Fisher-Johns melting point measuring device or equivalent. 8.3.2 Calibration
34、Calibration shall be performed by using high purity metal standards, according to the manufacturers instructions. 8.3.3 Sample preparation 8.3.3.1 Neat resin and unsupported adhesives No sample preparation is required. 8.3.3.2 Prepregs and supported adhesive samples (adhesive + carrier) (6 x 6) mm s
35、pecimens shall be cut. 8.3.3.3 Supported adhesive resin It may be prepared by buckling at low temperature (liquid nitrogen). 8.3.4 Procedure (isothermal) Preset the equipment to the required test temperature. Subsequently, insert a small amount of resin or a (6 x 6) mm specimen between two cover gla
36、sses (thickness: O, 15 - 0,30 mm) and place on the heated platform of the apparatus. The test temperature shall be selected in order to preferably obtain gel times in the range of 15-30 minutes. This temperature has to be agreed by the supplier and the customer before the commencement of the testing
37、 programme. Recommended testing temperature are 16OOC for 18OOC cure materials and 1 10C for 12OOC cure materials. Immediately after placing the sample on the heated platform of the apparatus, start a stopwatch or timer and begin to probe on the top of the cover glass with a toothpick or a fine glas
38、s rod until no resin movement is observed. AECMA PRENUbO43 95 = LOL23LL 00L00b2 470 Page 8 prEN 6043 : 1995 8.4 Gel time of thermosetting resin systems : DSC technique (Method DI The applicability of this method to specific resin systems, has to be shown by preliminary correlation studies with Metho
39、ds B or C. 8.4.1 Apparatus (See EN 6041 1. 8.4.2 Sample preparation 8.4.2.1 Neat resin, prepregs, unsupported adhesives and supported adhesive samples (adhesive + carrier) No sample preparation is required. 8.4.2.2 Supported adhesive resin It may be prepared by buckling at low temperature (liquid ni
40、trogen). 8.4.3 Test specimens (See EN 6041) 8.4.4 Procedure 8.4.4.1 Isothermal procedure Follow the procedure described in EN 6041, except for: 8.4.4.1.1 Temperature range The test temperature shall be selected in order to preferably obtain gel times in the range of 15-30 minutes. This temperature s
41、hall to be agreed by the supplier and the customer before the commencement of thc testing programme. Recommended testing temperatures are 1 6OoC for 1 8OoC cure materials and 1 1 OC fo 1 2OoC cure materials. 8.4.4.1 -2 Heating rate The heating rate shall be as fast as possible until the selected tem
42、perature is reached. 8.4.4.2 Dynamic procedure Follow the procedure described in EN 6041, except for: Temperature range : Heating rate : 2OClmin standard, unless otherwise specified. from 5OoC to Tgel + IOOC. 8.4.4.3 Recording A record of heat flow versus time or temperature shall be obtained, and t
43、he derivative curve shall b determined (see figures 4a and 4b). AECMA PRENub043 95 m LOL2311 OOLOOb3 307 m Page 9 prEN 6043 : 1995 8.5 Gel time of thermosetting resin systems : TMA technique (Method E) 8.5.1 Apparatus The test shall be performed using a thermomechanical analyser capable of applying
44、an alternating load with time. Instruments are given in the Annex A of this standard. 8.5.2 Calibration Calibrate the instrument in accordance with the manufacturers instructions. Verify that the temperature indicated in the isothermal mode is correct by scanning slowly (1 OC/min) over the temperatu
45、re of interest and checking the melting point of a suitable high purity reference material such as indium (MP 156,6OC) or benzoic acid (MP 122,4OC) Note : It is also preferable to determine the time taken for the sample to attain the set temperature after insertion into the TMA, again by using the s
46、ame reference materials. For example, if it is assumed that the time delay between the sample attaining 1 6OoC and 156,6OC was negligible, then the time taken for a small sample of indium to melt would be equivalent to that taken by the sample to attain the set temperature. This should be subtracted
47、 from the total gel time determined. 8.5.3 Sample preparation 8.5.3.1 Prepreg and supported adhesives Cut out (5 x 5) mm specimens, remove the backing film, sandwich between two alumina discs (nominally 6 mm diameter x 0,6 mm thick) and press together firmly. 8.5.3.2 Neat resin and unsupported adhes
48、ives Proceed as described in 8.5.3.1. but also insert 1 or 2 layers of pre-cleaned glass cloth. 8.5.4 Procedure 8.5.4.1 Isothermal procedure Preheat the furnace to the desired temperature (see 8.5.4.1.2). Select a run time and load appropriate to the sample under test. Insert the sample into the app
49、aratus (see figure I), lower the probe and furnace, and start the run immediately. The test temperature shall be selected in order to preferably obtain gel times in the range of 15-30 minutes. This temperature has to be agreed by te supplier and the customer before the commencement of the testing programme. Recommended testing temperatures are 1 6OoC for 1 8OoC cure materials and 1 1 OC for 1 2OoC cure materials. 8.5.4.2 Dynamic procedure Insert the sample into the apparatus (see figure 11, lower the probe and furnace and start the run under t
