EN ISO 12114:1997
(Main)Fibre-reinforced plastics - Thermosetting moulding compounds and prepregs - Determination of cure characteristics (ISO 12114:1997)
Fibre-reinforced plastics - Thermosetting moulding compounds and prepregs - Determination of cure characteristics (ISO 12114:1997)
Faserverstärkte Kunststoffe - Härtbare Formmassen und Prepregs - Bestimmung des Härtungsverhaltens (ISO 12114:1997)
Diese internationale Norm beschreibt zwei Methoden zur Bestimmung des Härtungsverhaltens von faserverstärkten Formmassen und Prepregs. Die charakteristischen Werte sind: - Wärmeentwicklung durch die exotherme Reaktionstönung; - Wärmeausdehnung der Formmasse während des Temperaturanstiegs; - Schwindung durch die Härtungsreaktion. Die beschriebenen Methoden sind für alle härtbaren Formmassen mit Faserverstärkung anwendbar. Das Hauptanwendungsgebiet sind Formmassen auf der Basis von ungesättigten Polyesterharzen (UP).
Plastiques renforcés de fibres - Compositions de moulage et préimprégnés - Détermination des caractéristiques de durcissement (ISO 12114:1997)
La présente Norme internationale prescrit deux méthodes pour la détermination des caractéristiques de durcissement des compositions de moulage thermodurcissables renforcées de fibres et des préimprégnés. Les caractéristiques mesurées sont -- l'émission de chaleur due à l'exothermie de la réaction; -- la dilatation thermique du produit accompagnant l'augmentation de température; -- le retrait dû à la réaction de durcissement. Les méthodes sont applicables à toutes les compositions à base de matrices thermodurcissables renforcées de fibres. Le principal domaine d'application porte sur les produits à base de résines polyesters insaturés. La méthode I est une méthode d'essai permettant de déterminer la réactivité d'une composition thermodurcissable selon un mode opératoire simple. Cette mesure se rapporte uniquement au comportement réactif de la matrice et à son état de stabilisation (facteur influant sur la durée de vie de la composition de moulage). La méthode II est une méthode d'essai qui nécessite un équipement plus sophistiqué, prend plus de temps mais donne des indicatio 269ns détaillées supplémentaires sur le comportement physique de la composition dans des conditions de moulage habituelles simulées. Il en résulte une plaque qui pourra être utilisée ultérieurement pour déterminer certaines propriétés du produit moulé.
Z vlakni ojačeni polimerni materiali – Duromerne mase za oblikovanje in predimpregniranja – Določevanje poteka zamreženja (ISO 12114:1997)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-maj-1999
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Fibre-reinforced plastics - Thermosetting moulding compounds and prepregs -
Determination of cure characteristics (ISO 12114:1997)
Faserverstärkte Kunststoffe - Härtbare Formmassen und Prepregs - Bestimmung des
Härtungsverhaltens (ISO 12114:1997)
Plastiques renforcés de fibres - Compositions de moulage et préimprégnés -
Détermination des caractéristiques de durcissement (ISO 12114:1997)
Ta slovenski standard je istoveten z: EN ISO 12114:1997
ICS:
83.120 2MDþDQLSROLPHUL Reinforced plastics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
INTERNATIONAL
IS0
STANDARD 12114
First edition
1997-05-I 5
Fibre-reinforced plastics - Thermosetting
moulding compounds and prepregs -
Determination of cure characteristics
Plastiques renforks de fibres - Compositions de moulage
thermodurcissables et pr&mpr4gn& - Dbtermination des caractkristiques
de durcissement
Reference number
IS0 12114:1997(E)
IS0 12114:1997(E)
Page
Contents
iv
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
1 Scope . 1
2 Normative references .
Definitions . 2
4 Apparatus .
5 Sampling .
6 Conditioning and test atmospheres .
7 Test specimens .
8 Procedure .
9 Expression of results .
10 Precision . 7
11 Test report .
0 is0 1997
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ii
0 IS0
IS0 12114:1997(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national 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. International organizations, governmental and non-
governmental, in liaison with ISO, also take part in the work. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) 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 International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard IS0 12114 was prepared by Technical Committee
ISOTTC 61, Plastics, Subcommittee SC 13, Composites and reinforcement
fibres.
IS0 12114:1997(E)
@ IS0
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 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
formulation. 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/or 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 conditions 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 several 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 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 glance.
iV
INTERNATIONAL STANDARD @ Iso IS0 12114:1997(E)
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 characteristics 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;
- the shrinkage due to the curing reaction.
The methods 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.
This method examines only the reactive behaviour of the matrix and its state 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
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 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 editions of the standards indicated below. Members of IEC and IS0 maintain
registers of currently valid International Standards.
IS0 47211988, Plastics - Vocabulary.
Sheet moulding compound (SMC) - Basis for a specification.
IS0 8605: 1989, Textile glass reinforced plastics -
IS0 86063 990, Plastics - Prepregs - Bulk moulding compound (BMC) and dough moulding compound (DMC) -
Basis for a specification.
@ IS0
IS0 12114:1997(E)
3 Definitions
For the purposes of this International Standard, the definitions given in IS0 472, IS0 8605 and IS0 8606 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 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 commonly 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.
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.
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 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 Insulated 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 versus time.
Device for preparing moulding-compound test specimens (see figure 3).
4.1.5
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.
@ IS0 IS0 12114:1997(E)
4.2 Method II
4.2.1 Suitable press, capable of applying a moulding pressure of 100 bar k 3 %.
4.2.2 Shear edge mould, mounted in the press, with a cavity of surface area not less than 200 cm2, heatable
to 200 “C with an accuracy of 1 % (see figure 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 measure changes in temperature at the surface of the
moulding compound with an accuracy of rtl %.
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 about 20 mm with a resolution of 0,Ol mm.
distance apart
NOTE - For practical reasons, it is recommended that the sensors be mounted at a maximum
from the axis of symmetry.
of 30 mm and eq uidistant
4.2.3 Recording equipment, connected to the sensors in the mould, to plot the variation with time of
- pressure (from 0 to 150 bar);
- displacement (from 0 to 20 mm);
- temperature (from 0 to 200 “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 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
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
(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 “C.
J
6.2 Test atmosphere
The atmosphere for testing shall be the same as that used for conditioning.
IS0 12114:1997(E)
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 determination be performed on
unit
additional specimens or at specific places in the ele mentary or laboratory sample.
7.2 Method I
For each test specimen, take 6 cm3 + 0,5 cm3 of moulding material, giving a test specimen height in the range
I,75 cm to 2,lO cm. This quantity can be obtained by direct measurement 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 + 1 mm.
Cut all the pieces from the same sheet at intervals of about IO 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 using the device described in 4.1.5.
7.2.3 Paste specimens
Take 6 cm3 k 0,5 cm3 of the paste or resin with the syringe (4.1.6).
7.3 Method II
The thickness of the moulded test specimen should preferably be the same as the thickness of the production
moulding it is intended to represent. However, the thickness of the moulded specimen depends on the number of
complete layers of the same size of a sheet moulding compound used and their individual thickness or, in the case
a
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