EN ISO 12114-1997 en Fibre-Reinforced Plastics - Thermosetting Moulding Compounds and Prepregs - Determination of Cure Characteristics《纤维增强塑料 热固性模塑化合物和聚酯胶片 固化特性的测定 ISO 12114-1997》.pdf

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1、STD.BSI BS EN IS0 12124-ENGL 1997 Lb24bb9 Ob34270 Tb4 BRITISH STANDARD Fibre-reinforced plastics - Thermosetting moulding compounds and prepregs - Determination of cure characteristics The European Standard EN IS0 12114 : 1997 has the status of a British Standard ICs 83.120 NO COPYING WITHOUT BSI PE

2、RMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN IS0 12114 : 1997 BS EN IS0 12114 : 1997 National foreword This British Standard is the English language version of EN IS0 12114 : 1997. It is identical with IS0 12114 : 1997. The UK participation in its preparation was entrusted to Technid Committe

3、e PW42, Fibre reinforced thermoseing plastics and prepregs, which has the . responsibility to: - aid enquirers to understand the text; - present to the responsible iuropean committee any enquiries on the interpretation, or proposais for change, and keep the UK interests infOrIIled; - monitor related

4、 intedonai and European developments and promulgate themintheUK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC standards nody include an annex which iists nolTllilf;ive reference

5、s to internationai publications with their correponding European pubiications. The British Standards which implement internationai or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled international Standards Correspondence Index

6、, or using the Find facility of the BSI Standards Electronic Catalogue. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the Is

7、0 title page, pages ii to iv, pages 1 to 13, a blank page, an inside back cover and a back cover. This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 Augu

8、st 1997 O BSI 1997 ISBN O 680 28029 2 Amendments issued since publication IDischa Komitee fr Nornuig Central Secretariat: rue de Stmsart,36 B-10M Brrrucli * 1W7 CEN - ALL rights of exploitation in any,form and by iny mans reserved worldwide for CEN nitionil ilenbers. Ref. No. EN IS0 12114:1997 E EN

9、IS0 12114 : 1997 Foreword The text of the International Standard IS0 12114:1997 has been prepared by Technical Committee ISORC 61 “Plastics“ in collaboration with Technid Committee CEN/TC 249 “Plastics“, the secretariat of which is held by IBN. This European Standard shall be given the status of a n

10、ational standard, either by publication of an identical text or by endorsement, at the latest by November 1997, and conflicting national standars shall be withdrawn at the latest by November 1997. According to the CENKENELEC Internal Regulations, the national standards organizations of the following

11、 countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, .Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the Internatio

12、nal Standard IS0 121 14: 1997 was approved by CEN as a European Standard without any modification. STD-BSI BS EN IS0 12114-ENGL 1997 lb24bb7 Ob31r271.i bOT EN IS0 12114 : 1997 INTERNATIONAL STANDARD IS0 12114 First edition 1997-05-1 5 Fibre-reinforced plastics - Thermosetting moulding compounds and

13、prepregs - Determination of cure characteristics Plastiques renforcs de fibres - Compositions de moulage thermodurcissables et primprgns - Dtermination des caractristiques de durcissement Reference number IS0 12114:1997(E) STD-BSI BS EN IS0 121Lq-ENGL 1997 Lb24bbS b34275 54b W EN IS0 12114 : 1997 Co

14、ntents Introduction . 1 2 3 4 5 6 7 8 9 10 11 Scope Normative references Definitions Apparatus Sampling Conditioning and test atmospheres . Test specimens . Procedure Expression of results . Precision Test report . Page iv 1 1 2 2 3 3 4 5 6 7 7 Descriptors: piastics. reinforced plastics. thermosetti

15、ng resins. moulding materials. ingredients. prepregs. tests. determination. chractenstics . hardening. test equipment . i STD-BSI BS EN IS0 12LL4-ENGL 1777 U Lb2qbbS b34276 482 B EN IS0 12114 : 1997 Foreword IS0 (the International Organization for Standardization) is a worldwide federation of nation

16、al standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. Intemation

17、al organizations, governmental and non- governmental, in liaison with SO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Drat International Standards adopted by the technical committees

18、 are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 YO of the member bodies casting a vote. International Standard IS0 121 14 was prepared by Technical Committee ISORC 61, Plastics, Subcommittee SC 13, Composites and reinforcemen

19、t fibres. iii Introduction The description of the cure characteristics of thermosetting moulding compounds is rather complex. Various parameters and properties like reactivity, temperature, pressure and shrinkage are of interest to the end user. Some of these parameters influence each other. For thi

20、s reason, several test methods are necessary for quality control and to determine the effect of varying the proportion of any particular component in the formulation. The characteristics determined are selected to enable different moulding compounds and prepregs to be compared and their shelf life a

21、ssessed. One important characteristic of thermosetting compounds is their reactivity, .e. their ability to polymerize under the influence of a catalyst and/or heat. This reactivity can be evaluated by various methods. This International Standard gives two such methods: - the first of which is a simp

22、le procedure which is limited to the determination of reactivity and shelf life by measuring the variation of temperature as a function of time under the conditions usually umd in production; - the second method is more sophisticated and gives information on the physical behaviour of the compound un

23、der simulated moulding conditions. The description of the curing behaviour of a thermosetting compound is not possible by a single value. It is dependent on several parameters, like pressure, temperature and shrinkage, which influence each other. This interdependence must also be described. Such a d

24、escription can be given by mathematical functions or expressed in terms of a set of curves for the various parameters, as in this International Standard. The curves for a particular compound are all shown in the same figure to enable the interdependence of the parameters concerned to be seen at a gl

25、ance. iv STD-BSI BS EN IS0 LZLLq-ENGL 1777 Lb2Libb9 0b3ii278 255 EN IS0 12114 : 1997 Fibre-reinforced plastics - Thermosetting moulding compounds and prepregs - Determination of cure characteristics 1 Scope This International Standard specifies two methods for the determination of the cure character

26、istics of fibre- reinforced thermosetting moulding compounds and prepregs. The characteristics measured are - the heat generated by the exothermic reaction; - the thermal expansion of the compound accompanying the rise in temperature; a - the shrinkage due to the curing reaction. - = II - The method

27、s specified are applicable to all compounds comprising thermosetting matrices reinforced with fibres. The major field of application is compounds based on unsaturated polyester resins. Method I describes a test method to determine the reactivity of a thermosetting compound by a simple procedure. Thi

28、s method examines only the reactive behaviour of the matrix and its state of stabilization (one factor affecting the shelf life of the moulding compound). = rn * * Method II describes a test method which needs more sophisticated equipment, takes more time but provides additional detailed information

29、 about the physical behaviour of the compound under simulated practical moulding conditions. It produces a plate which can be used for further testing to determine properties of the moulded article. 2 Normative references The following standards contain provisions which, through reference in this te

30、xt, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edi

31、tions of the standards indicated below. Members of IEC and IS0 maintain registers of currentiy valid International Standards. IS0 472:1988, Plastics - Vocabulary. IS0 8605:1989, Textile glass reinforced plastics - Sheet moulding compound (SMC) - Basis for a specification. IS0 8606:199, Plastics - Pr

32、epregs - Bulk moulding compound (BMC) and dough moulding compound (DMC) - Basis for a specification. 1 EN IS0 12114 : 1997 3 Definitions For the purposes of this Intemational Standard, the definitions given in IS0 472, IS0 8605 and IS0 8606 apply, plus the following definitions: 3.1 reactivity: The

33、reactivity of a thermosetting material is taken, by convention, as the maximum gradient, in degrees Celsius per second, of a plot of the temperature of the thermosetting material as a function of time during curing. 3.2 curing behaviour: The behaviour of a thermosetting material when moulded under c

34、ommonly used moulding conditions, as described by the following set of parameters: - cure time; - thermal expansion; - shrinkage due to the curing reaction; - net shrinkage (reaction shrinkage less thermal expansion). The values of these parameters will depend on the actual moulding conditions used.

35、 3.3 elementary unit: The smallest normally commercially available entity of a given product. The description (form, dimensions, mass, etc.) of the elementary unit will normally be defined in the product specification. Elementary units may be supplied in the form of rolls or packages, for instance.

36、NOTE - For a given product, the dimensions, mass or volume of the elementary unit may change, as manufacturing techniques evolve. without necessarily causing any modification in the properties of the product or the way in which these properties vary within the elementary unit. 4 Apparatus 4.1 Method

37、 I 4.1.1 Cylindrical metal mould, with an inside diameter of 20 mm, equipped with a heater and a temperature control system, and with a heated steel punch which fits inside the cylindrical mould (see figure 1). 4.1.2 Device for applying a minimum force of 15 daN to the punch (see figure 2). 4.1.3 In

38、sulated thermocouple, diameter 1 mm, located at the centre of the bottom of the mould and rising 5 mm into the mould cavity. The thermocouple shall be insulated from the heated steel block by insulation having a thickness of 2 mm. 4.1.4 Suitable recording system, for plotting a curve of temperature

39、versus time. 4.1.5 Device for preparing moulding-compound test specimens (see figure 3). 4.1.6 Syringe, for measuring out paste specimens. 4.1.7 Balance, accurate to the nearest 0,l g. 4.1.8 Brass bristle brush, to clean the mould. 2 STD-BSI BS EN IS0 12114-ENGL 1997 1624bb7 Ob34280 703 EN IS0 12114

40、 : 1997 4.2 Method II 4.2.1 Suitable press, capable of applying a moulding pressure of 100 barf 3 %. 4.2.2 Shear edge mould, mounted in the press, with a cavity of surface area not less than 20cm2, heatable to 200C with an accuracy of 1 % (see figure4). The mould shall be equipped with a pressure se

41、nsor and temperature sensor, mounted in the centre of the mould. For pressure measurements, piezoelectric sensors are normally used. The temperature sensor shall be insulated from the mould to measure changes in temperature at the surface of the moulding compound with an accuracy of fl %. Both senso

42、rs shall be flush with the surface of the mould cavity. A displacement sensor shall be fitted to the mould to measure mould lid travel of about 20 mm with a resolution of 0,Ol mm. NOTE - For practical reasons, it is recommended that the sensors be mounted at a maximum distance apart of 30 mm and equ

43、idistant from the axis of symmetty. 4.2.3 Recording equipment, connected to the sensors in the mould, to plot the variation with time of - pressure (from O to 150 bar); - displacement (from O to 20 mm); - temperature (from O to 200 OC). _. I 4.2.4 Calipers, for measuring the thickness of the moulded

44、 test specimen. = e - - I = 5 Sampling * * m For a sheet moulding compound, take a laboratory sample over the full width of the roll. Reduce the width by 5 cm on each side to avoid edge effects. For a bulk moulding compound, take a laboratory sample from the centre of an elementary unit. When taking

45、 the laboratory sample, do not remove any protective sheet, and place the sample, immediately after taking it, in a suitable bag to avoid loss of volatile matter or absorption of moisture. The laboratory sample shall be of a size sufficient to enable the required number of test specimens to be prepa

46、red (see 7.1). 6 Conditioning and test atmospheres 6.1 Conditioning Condition the laboratory sample for a time. sufficient to establish temperature equilibrium. The temperature of the laboratory sample immediately before the test specimens are taken shall not be less than 18 OC. 6.2 Test atmosphere

47、The atmosphere for testing shall be the same as that used for conditioning. 3 EN IS0 12114 : 1997 7 Test specimens 7.1 General For both methods, take three specimens from the conditioned laboratory sample. NOTE - The product specification or the person ordering the analyses may require that the dete

48、rmination be performed on additional specimens or at specific places in the elementary unit or laboratory sample. 7.2 Method I For each test specimen, take 6 cm3 f 0,5 cm3 of moulding material, giving a test specimen height in the range 1,75 cm to 2,lO cm. This quantity can be obtained by direct mea

49、surement of a given volume in the case of pastes and resins. For other moulding compounds, it is easier to weigh out a given mass, calculated from the density of the moulding compound. 7.2.1 Sheet moulding compound specimens Stamp the required number of pieces of moulding compound with a blanking die punch of diameter 19 mm I 1 mm. Cut all the pieces from the same sheet at intervals of about 10 cm. Remove the protective sheets and stack the pieces together to form test specimens. 7.2.2 Bulk moulding compound specimens Shape the moulding compound usin

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