1、BRITISH STANDARD BS EN ISO 12114:1997 Fibre-reinforced plastics Thermosetting moulding compounds and prepregs Determination of cure characteristics The European Standard EN ISO 12114:1997 has the status of a British Standard ICS 83.120BSENISO12114:1997 This British Standard, having been prepared und
2、er the directionof the Sector Board forMaterials and Chemicals, waspublished under the authorityof the Standards Boardand comes into effect on 15August 1997 BSI 09-1999 ISBN 0 580 28029 2 National foreword This British Standard is the English language version ofENISO 12114:1997. It is identical with
3、 ISO12114:1997. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries
4、on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is
5、drawn to the fact that CEN and CENELEC standards normally include an annex which lists normative references to international publications with their corresponding European publications. The BritishStandards which implement international or European publications referred to in this document may be fo
6、und in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards
7、are responsible for their correct application. 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, pages i and ii, theEN ISO title page, page 2, the ISO title page, pages ii to iv
8、, pages 1 to 10 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBSENISO12114:1997 BSI 09-1999 i Contents
9、Page National foreword Inside front cover Foreword 2 Foreword iii Text of ISO 12114 1ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 12114 May 1997 ICS 83.120.00 Descriptors: See ISO document English version Fibre-reinforced plastics Thermosetting moulding compounds and prepregs Det
10、ermination of cure characteristics (ISO12114:1997) Plastiques renforcs de fibres Compositions de moulage et primprgns Dtermination des caractristiques de durcissement (ISO12114:1997) Faserverstrkte Kunststoffe Hrtbare Formmassen und Prepregs Bestimmung des Hrtungsverhaltens (ISO 12114:1997) This Eur
11、opean Standard was approved by CEN on 1997-05-10. 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 national standard without any alteration. Up-to-date Lists and bibliographical references conce
12、rning such national standards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist 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 l
13、anguage and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden
14、, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN ALL rights of exploitation in any form and by any means reserved worldwide for CEN national Mem
15、bers. Ref. No. EN ISO 12114:1997 EENISO12114:1997 BSI 09-1999 2 Foreword The text of the International Standard ISO12114:1997 has been prepared by Technical Committee ISO/TC61 “Plastics” in collaboration with Technical Committee CEN/TC249 “Plastics”, the secretariat of which is held by IBN. This Eur
16、opean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November1997, and conflicting national standards shall be withdrawn at the latest by November1997. According to the CEN/CENELEC Internal Regulations, the na
17、tional standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. E
18、ndorsement notice The text of the International Standard ISO12114:1997 was approved by CEN as a European Standard without any modification.ENISO12114:1997 ii BSI 09-1999 Contents Page Foreword iii Introduction 1 1 Scope 1 2 Normative references 1 3 Definitions 1 4 Apparatus 2 5 Sampling 2 6 Conditio
19、ning and test atmospheres 2 7 Test specimens 3 8 Procedure 3 9 Expression of results 4 10 Precision 5 11 Test report 5 Figure 1 Principle of apparatus (4.1.1) 6 Figure 2 Principle of apparatus (4.1.2) 7 Figure 3 Example of apparatus for the preparation of specimens from bulk products 8 Figure 4 Shea
20、r edge mould 9 Figure 5 Typical reactivity curve 10 Figure 6 Typical set of traces obtained by method II 10 Descriptors: Plastics, reinforced plastics, thermosetting resins, moulding materials, ingredients, prepregs, tests, determination, characteristics, hardening, test equipment.ENISO12114:1997 BS
21、I 09-1999 iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject
22、 for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC)
23、on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an InternationalStandard requires approval by at least75% of the member bodiescasting a vote. International Standard IS
24、O12114 was prepared by Technical Committee ISO/TC61, Plastics, Subcommittee SC13, Composites and reinforcement fibres.iv blankENISO12114:1997 BSI 09-1999 1 Introduction The description of the cure characteristics of thermosetting moulding compounds is rather complex. Various parameters and propertie
25、s like reactivity, temperature, pressure and shrinkage are of interest to the end user. Some of these parameters influence each other. For this reason, several test methods are necessary for quality control and to determine the effect of varying the proportion of any particular component in the form
26、ulation. The characteristics determined are selected to enable different moulding compounds and prepregs to be compared and their shelf life assessed. One important characteristic of thermosetting compounds is their reactivity, i.e. their ability to polymerize under the influence of a catalyst and/o
27、r heat. This reactivity can be evaluated by various methods. This International Standard gives two such methods: the first of which is a simple 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 condi
28、tions usually used in production; the second method is more sophisticated and gives information on the physical behaviour of the compound under simulated moulding conditions. The description of the curing behaviour of a thermosetting compound is not possible by a single value. It is dependent on sev
29、eral parameters, like pressure, temperature and shrinkage, which influence each other. This interdependence must also be described. Such a description 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 cu
30、rves for a particular compound are all shown in the same figure to enable the interdependence of the parameters concerned to be seen at a glance. 1 Scope This International Standard specifies two methods for the determination of the cure characteristics of fibre-reinforced thermosetting moulding com
31、pounds and prepregs. The characteristics measured are the heat generated by the exothermic reaction; the thermal expansion of the compound accompanying the rise in temperature; the shrinkage due to the curing reaction. The methods specified are applicable to all compounds comprising thermosetting ma
32、trices 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. This method examines only the reactive behaviour of the matrix and its sta
33、te of stabilization (one factor affecting the shelf life of the moulding compound). Method II describes a test method which needs more sophisticated equipment, takes more time but provides additional detailed information about the physical behaviour of the compound under simulated practical moulding
34、 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 text, constitute provisions of this International Standard. At the time of publica
35、tion, 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 editions of the standards indicated below. Members of IEC and ISO maintain register
36、s of currently valid International Standards. ISO 472:1988, Plastics Vocabulary. ISO 8605:1989, Textile glass reinforced plastics Sheet moulding compound (SMC) Basis for a specification. ISO 8606:1990, Plastics Prepregs Bulk moulding compound (BMC) and dough moulding compound (DMC) Basis for a speci
37、fication. 3 Definitions For the purposes of this International Standard, the definitions given in ISO472, ISO8605 and ISO8606 apply, plus the following definitions: 3.1 reactivity the reactivity of a thermosetting material is taken, by convention, as the maximum gradient, in degrees Celsius per seco
38、nd, of a plot of the temperature of the thermosetting material as a function of time during curingENISO12114:1997 2 BSI 09-1999 3.2 curing behaviour the behaviour of a thermosetting material when moulded under commonly used moulding conditions, as described by the following set of parameters: cure t
39、ime; 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 3.3 elementary unit the smallest normally commercially available entity of a given product. The d
40、escription (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 NOTEFor a given product, the dimensions, mass or volume of the elementary unit may change, as manufa
41、cturing 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 I 4.1.1 Cylindrical metal mould, with an inside diameter of20mm, equipped with a heater and a temperat
42、ure control system, and with a heated steel punch which fits inside the cylindrical mould (seeFigure 1). 4.1.2 Device for applying a minimum force of 15 daN to the punch (seeFigure 2). 4.1.3 Insulated thermocouple, diameter1mm, located at the centre of the bottom of the mould and rising5mm into the
43、mould cavity. The thermocouple shall be insulated from the heated steel block by insulation having a thickness of2mm. 4.1.4 Suitable recording system, for plotting a curve of temperature versus time. 4.1.5 Device for preparing moulding-compound test specimens (seeFigure 3). 4.1.6 Syringe, for measur
44、ing out paste specimens. 4.1.7 Balance, accurate to the nearest0,1g. 4.1.8 Brass bristle brush, to clean the mould. 4.2 Method II 4.2.1 Suitable press, capable of applying a moulding pressure of 100bar 3%. 4.2.2 Shear edge mould, mounted in the press, with a cavity of surface area not less than200cm
45、 2 , heatable to200 C with an accuracy of1% (seeFigure 4). The mould shall be equipped with a pressure sensor 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 me
46、asure changes in temperature at the surface of the moulding compound with an accuracy of1%. Both sensors 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 about20mm with a resolution of0,01mm. NOTEFor practical reas
47、ons, it is recommended that the sensors be mounted at a maximum distance apart of30mm and equidistant from the axis of symmetry. 4.2.3 Recording equipment, connected to the sensors in the mould, to plot the variation with time of pressure (from 0 to150bar); displacement (from 0 to20mm); temperature
48、(from 0 to200 C). 4.2.4 Calipers, for measuring the thickness of the moulded test specimen. 5 Sampling For a sheet moulding compound, take a laboratory sample over the full width of the roll. Reduce the width by5cm on each side to avoid edge effects. For a bulk moulding compound, take a laboratory s
49、ample from the centre of an elementary unit. When taking 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 prepared (see7.1). 6 Conditioning and test atmospheres 6.1 Conditioning Condition the laboratory sample for a time sufficient to establish tem
