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Mulligan, David - Cure Monitoring For Composites and Adhesives-Ismithers Rapra Publishing (2003!01!01)
Mulligan, David - Cure Monitoring For Composites and Adhesives-Ismithers Rapra Publishing (2003!01!01)
D. Mulligan
1. A commissioned expert review, discussing a key topic of current interest, and referring to the References and
Abstracts section. Reference numbers in brackets refer to item numbers from the References and Abstracts
section. Where it has been necessary for completeness to cite sources outside the scope of the Rapra Abstracts
database, these are listed at the end of the review, and cited in the text as a.1, a.2, etc.
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Item 1
Source of
Macromolecules
original article
33, No.6, 21st March 2000, p.2171-83
Title EFFECT OF THERMAL HISTORY ON THE RHEOLOGICAL
BEHAVIOR OF THERMOPLASTIC POLYURETHANES
Authors and
Pil Joong Yoon; Chang Dae Han affiliation
Akron,University
The effect of thermal history on the rheological behaviour of ester- and
ether-based commercial thermoplastic PUs (Estane 5701, 5707 and 5714
from B.F.Goodrich) was investigated. It was found that the injection
moulding temp. used for specimen preparation had a marked effect on the
variations of dynamic storage and loss moduli of specimens with time
observed during isothermal annealing. Analysis of FTIR spectra indicated
that variations in hydrogen bonding with time during isothermal annealing Abstract
very much resembled variations of dynamic storage modulus with time
during isothermal annealing. Isochronal dynamic temp. sweep experiments
indicated that the thermoplastic PUs exhibited a hysteresis effect in the
heating and cooling processes. It was concluded that the microphase
separation transition or order-disorder transition in thermoplastic PUs could
not be determined from the isochronal dynamic temp. sweep experiment.
The plots of log dynamic storage modulus versus log loss modulus varied
with temp. over the entire range of temps. (110-190C) investigated. 57 refs. Companies or
GOODRICH B.F. organisations
Location USA mentioned
Accession no.771897
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Cure Monitoring for Composites
and Adhesives
David R. Mulligan
(Certech)
ISBN 1-85957-393-2
Cure Monitoring for Composites and Adhesives
Contents
1 Introduction .............................................................................................................................................. 3
1.1 Aims and Scope .............................................................................................................................. 3
1.2 Cure of Composites and Adhesives ................................................................................................ 3
1.3 Benefits of Cure Monitoring ........................................................................................................... 4
1
Cure Monitoring for Composites and Adhesives
The views and opinions expressed by authors in Rapra Review Reports do not necessarily reflect those of
Rapra Technology Limited or the editor. The series is published on the basis that no responsibility or
liability of any nature shall attach to Rapra Technology Limited arising out of or in connection with any
utilisation in any form of any material contained therein.
2
Cure Monitoring for Composites and Adhesives
3.2 Acoustic
absorb ultrasonic waves or are highly filled. An 3.3.1 Extrinsic Fabry-Pérot Sensor
example of such a technique follows the change in
resonant frequency as the material cures. This change A schematic of the extrinsic Fabry-Pérot sensor is
can be analysed and interpreted as an increase in the shown in Figure 4. The input fibre is a single-mode
modulus, and therefore degree-of-cure, of the material. fibre, while the reflection fibre is multi-mode.
Typically, these two fibres are inserted into a tight
fitting glass capillary and glued into place with epoxy
3.3 Fibre Optic resin. The gauge length of the sensor is the distance
between the points where the capillary is adhered to
the fibres. The absolute cavity length is measured very
Fibre optic strain sensors have mainly been applied to
accurately using a Fabry-Pérot interferometer and so
composite materials for structural health monitoring.
the strain in the material can be determined with
It is possible to extend their use, so that they provide
accuracy.
information on strain during cure. Since resins
generally shrink during cure, these strains can provide
information on the degree-of-cure of the resin. The sensor arrangement of Liu and co-workers (200)
However, there must be a good bond between the resin was tested for temperature sensitivity for temperatures
and the sensor for the strain to be transferred, which is between 38 °C and 180 °C. In this range, the sensor
unlikely early in cure. It has been shown that for an was found to be insensitive to temperature changes,
epoxy resin adhesive system, most of the shrinkage largely due to the fact that the quartz capillary and
took place during post cure ageing (60), which could optical fibre comprise of essentially the same material.
limit the value of this technique for on-line monitoring So, the difference in coefficient of thermal expansion
and control of cycle times. is negligible. This temperature range will cover most
curing processes, which gives confidence that
temperature sensitivity will not be a major source of
Integration of optical fibres into composite or adhesive
error for these sensors in cure monitoring applications.
parts is far from trivial. There are a number of practical
difficulties that need to be overcome, such as keeping
the fibre straight and finding the ends of the fibre after
processing so that they can be connected. All these
problems must be dealt with in the context of an artefact
that can be regarded as extremely fragile by shop floor
standards.
Extrinsic Fabry-Pérot sensors and fibre Bragg grating In contrast to the extrinsic Fabry-Pérot sensor, the
sensors have been used for cure monitoring in several Bragg grating sensor is very sensitive to changes in
studies and these two types of sensors will be described temperature, as temperature affects both the refractive
and discussed in turn. index and the periodicity of the grating. Hence, it is
ε ∗ = ε ′ − iε ′′
dielectric measurements have been discussed in detail components are often presented against frequency, i.e.,
by Mijovic and co-workers (323). an impedance spectrum. Although the underlying data
is identical, this presentation allows frequency shifts
Pethrick (a.4) has presented a valuable overview of to be identified more readily.
dielectric properties for selected resins during cure.
These results are presented in terms of the dielectric A complete cure monitoring system based on
constant and dielectric loss (proportional to real and impedance measurement has been developed (97). This
imaginary permittivity respectively). Commonly used system is based on the observation that most cure
resins are considered and features identifying processes have a characteristic impedance curve that
meaningful points in the cure are described and their is independent of the details of the process. Hence,
significance discussed. comparison with this curve will indicate where the
reaction has progressed to and the process equipment
Ionic conductivity is often quoted during the early can be controlled accordingly.
stages of cure as it is related to the viscosity of the
resin. It has been shown that viscosity ( η) is There are two studies originating from Renault,
approximately inversely proportional to the ionic concerning dielectric cure monitoring of a glass fibre-
conductivity (σ) (288), so that epoxy in a compression mould. The first of these studies
(212) showed that combining dielectric and
η = A.σ − B temperature information allowed the degree-of-cure to
be calculated. These measurements were supported by
differential scanning calorimetry (DSC) measurements
where A and B are constants that are resin and
to determine the residual cure. A mathematical model
temperature specific. This allows the dielectric
was proposed that allowed the degree-of-cure to be
properties to be related to the physical flow properties
forecast for both isothermal and non-isothermal cases.
of the resin. Consequently, log ion viscosity can be used
Although this model was empirical, it did show
as a measure of cure progression. An example of typical
applicability to other cure studies.
data for a curing reaction is presented in Figure 8. The
reaction is considered to be complete when the log ion
viscosity becomes constant. This work was extended to cover thicker composite
parts that exhibited a cure gradient (167). In this case a
number of interdigitated sensors were embedded within
An alternative approach to the presentation of dielectric
the plies of the composite material, which allowed
data is to present it in terms of the complex impedance
information on the through thickness cure to be
(Z), such that
obtained. Both of these studies (167, 212) were based
on the collection of ionic conductivity data during
Z = Z ′ − iZ ′′ processing.
where Z´ is the real impedance and Z´´ is the imaginary Dielectric measurements have also been applied to
impedance. The logs of the two complex impedance monitoring the quality of glass fibre-polyester
pultrusions (298). Two types of dielectric sensor were
applied to the process, alongside pressure
measurements. An interdigitated sensor was
incorporated in the part and drawn through the
process, so it can only be used once. A second sensor
was a parallel plate sensor in the die. Both sensors
were sensitive to the process conditions, although it
is not possible to compare the outputs as they are
exposed to different volumes of material. For this
application it was suggested that the parallel plate
sensor would be of more benefit as it provided a
constant output.
The reflection sensor is simply a termination of the The two types of optical fibre sensors for monitoring
fibre in the material, as illustrated in Figure 9, and is refractive index have been used to study the same
sometimes called a Fresnel sensor because it is based epoxy-amine resin (193). The sensors behaved
on Fresnel reflection. At the end of the fibre there is an differently during the temperature ramp at the start of
interface between the fibre and the curing material. At cure, but during the isotherm, both were sensitive to
this interface a light pulse is partially reflected, the curing of the material. The signal from the reflection
depending on the refractive index of the curing material sensor was proportional to the refractive index, whereas
(see for example 222). the signal from the stripped cladding sensor was
inversely proportional to the refractive index. Both
The second type of sensor is an evanescent sensor, types of sensor identified the cure as complete at
which is illustrated in Figure 10. This type of sensor approximately the same time. However, the differences
consists of a portion of the optical fibre that has had in response at the start of cure suggest that applying
the cladding removed, so the core is in contact with these sensors for non-isothermal cure would present
the curing material. Typically the unclad portion of the significant additional challenges.
fibre is 15 to 20 cm in length. A light pulse that is
incident on this surface will generate an evanescent
wave in the surrounding material, providing that the
refractive index of the fibre core is greater than that of 5.2 Spectroscopic
thermosetting resins and the TTT diagram is determined problematic. The first step was to develop an algorithm
for isothermal cure of a material. A development from relating the die heater temperature to the degree-of-
the TTT diagram is the continuous-heating- cure profile through the thickness of the material. This
transformation (CHT) diagram (330). As the name algorithm was implemented with a three dimensional
suggests, the CHT diagram is for a situation where treatment by FEA on a pultrusion line to control the
curing material is subject to a linear increase in die heaters. The algorithm was found to be stable and
temperature with time. The CHT diagram allows the produced C-section and hollow pultrusions with the
time that transformations take place to be calculated. desired degree-of-cure, throughout the material.
The use of TTT and CHT diagrams allow optimum
cure programmes to be developed with relative ease. Another issue associated with process modelling is how
It is also possible to use TTT and CHT diagrams to to use the information for controlling processing. A
produce a prediction of the effect of changes in a cure simple, and often perfectly acceptable approach, is to
programme during processing. cure the material until on-line cure monitoring indicates
that the material is sufficiently cured, at which point
There are several more complex models that attempt the material can be removed from the process line. Of
complete treatments for the curing system. A scheme course it is possible to use the information from on-
for such models has been described (190) that takes line monitoring in a more sophisticated way to control,
time, temperature and dielectric data as real-time input for instance, temperatures and pressures. One such
parameters to produce predictions for resin viscosity scheme has been described (35) that uses the output of
and glass transition temperature (T g ). Accurate an evanescent wave optical fibre sensor to provide
predictions of these quantities are highly desirable, but information on the degree-of-cure. This information is
there is inevitably a cost in terms of the complexity then used to control the temperature of the mould to
and detail. In this case, submodels for heat transfer, maintain the rate of increase of degree-of-cure at a
kinetic, structural, chemoviscosity, dielectric relaxation desired value.
and ionic conductivity are all required. A formidable
task, although good progress is being made towards An expert system has been used to control the cure of
this goal. carbon fibre-phenolic material (271). In this case the
role of the expert system was divided into three
A particular problem arises, when thick sections of components:
material are required, as the variation in temperature,
and therefore variation of degree-of-cure, through the 1. the ‘observer’, which receives the signals from the
thickness of the material can be very significant. cure monitoring sensors,
Predictions for such composite materials were
calculated based on measured chemical and physical 2. the ‘thinker’, applies the algorithms and makes
parameters (180). This work was later improved and decisions,
extended (29, 30). The method outlined in these studies
uses data from heat flux sensors external to the material. 3. the ‘stoker’, interprets the current process
It was found that for optimal curing of thick sections parameters and implements changes.
of composite materials, it was necessary to introduce a
cooling stage to the cure cycle, which prevented
There is not a great deal of detail on how these three
overheating in the centre of the component. The
subfunctions are put into practice, but this is an
optimum start and end of this cooling stage was
appealing model for describing how cure monitoring
indicated by the data from the heat flux sensors,
can be applied. It can be seen how various aspects of
although smoothing of this data was critical. This
cure monitoring technology can fit into each of the three
approach worked well and improved the quality of
categories. For successful implementation these three
material produced, although the limitation of using a
components must form an unbroken feedback loop.
one-dimensional heat transfer model meant that cooling
losses at the edge of the component were neglected.
This problem could be addressed by using a three- Taking a step back from the various approaches to
dimensional heat transfer model. process modelling and control it can be seen that there
is no end to the detail and complexity that can be
included. At some point it is necessary to reflect on
A similar problem of ensuring uniform cure of
how the data will be used and critically assess whether
pultrusions has been addressed using finite element
greater accuracy justifies the additional work required.
analysis (FEA) (50). Uneven heating, and therefore
curing, of hollow or uneven pultrusion sections can be
6.2 Off-line Cure Assessment determined. DMA usually offers the greatest sensitivity
to property changes at the Tg. Examples of the studies
Off-line cure assessment has been covered in far greater that use DMA to characterise a curing material are (58,
detail in an earlier Review Report devoted to the subject 91, a.6). DMA has also been used to produce a model
(318). In this review, the subject is considered from for the development of the storage modulus and the
the perspective of using cure assessment to support cure increase in Tg of an epoxy material (a.7).
monitoring and identify issues that impact on-line and
in-line cure monitoring. A particular form of dynamic mechanical test is the
torsional braid analysis (TBA), which is a torsion
There are a variety of techniques that can be used to pendulum consisting of a glass fibre substrate to support
measure degree-of-cure after processing has been the curing material. For the study of curing materials
completed. Generally, off-line measurements allow greater it is usually necessary to enclose the sample within a
control of the testing environment, which makes furnace. Oscillations are induced in the pendulum,
reproducible measurement far more straightforward and which are allowed to proceed freely. The frequency
allows a wider range of techniques to be used. It is worth and damping of the induced oscillations are sensitive
noting that many of these techniques have on-line to the mechanical properties of the curing material. The
analogues, although, the greater flexibility of sample form use of this technique to formulate TTT and CHT
and shape increases the number of possible techniques. diagrams has been described (a.8).
For discussion, the techniques have been classified as
either physical or chemical property measurements. The principles of dielectric analysis (DEA) were
discussed in the context of on-line dielectric methods.
Generally, the only significant difference is that off-
6.2.1 Physical Property Measurements line measurement is far more convenient. The same
range of sensor types and options for interpretation
There are a variety of techniques that assess the physical apply for both on-line and off-line measurements.
properties of a curing material to provide an indirect
measure of the degree-of-cure, such as Deflection temperature under load (DTUL) is a
technique which follows the deflection of a beam of
• mechanical testing, material under fixed stress as the temperature is
increased. The temperature at which the beam deforms
• hardness testing, by a specified strain (0.2% for plastics and 0.1% for
composites) is the DTUL. This technique was previously
known as heat deflection temperature (HDT).
• dynamic mechanical analysis (DMA),
Differential scanning calorimetry (DSC) is a technique used for off-line cure assessment. This technique is
which determines the difference in heat flux into a based on the inelastic scattering of infrared radiation
specimen and a reference. This allows the and, like infrared spectroscopy, can be used to
determination of the enthalpy of a reaction. DSC is determine the degree-of-cure.
often used as the reference technique for evaluating
the degree-of-cure. The degree-of-cure, α, is calculated Nuclear magnetic resonance (NMR) provides structural
from the expression, information on a material through study of the magnetic
properties of the nuclei. Samples must contain
ΔHo − ΔHt particular nuclei and are studied in a strong magnetic
α= field. This technique is certainly a research tool, rather
ΔHo
than an option for routine testing of materials. For
instance, a recent study used NMR as a reference
where ΔHo is the enthalpy of the cure reaction for technique for comparison with results from ultrasonic
uncured resin and ΔHt is the enthalpy of the cure measurements (107).
reaction for test material. The appeal of DSC as a
reference technique is that it is straightforward to
calculate a value for the degree-of-cure from DSC
6.2.3 Comparison of Off-line Techniques
measurements. Examples of recent studies where DSC
has been used to determine the degree-of-cure include
As mentioned earlier in the context of on-line
(47, 58, 74).
spectroscopic techniques, direct measures of the
chemical species are the most meaningful in
DSC has also been used in numerous studies to determining the degree-of-cure. A comparison of
determine cure kinetics, such as (31, 41, 47). A several techniques for cure assessment (114) considered
development of DSC is temperature modulated DSC FTIR, DSC and ultrasonic measurements. In this case,
(TMDSC). A temperature modulation is superimposed it was argued that FTIR was preferable as it produced
on the temperature programme. This modulation results the most accurate data on degree-of-cure through the
in complex heat flow data, which may be resolved into course of the complete reaction.
heat flow components. TMDSC is claimed to offer
improved sensitivity and resolution compared to DSC.
The glass transition temperature (Tg) is often measured
TMDSC may also be used for determining cure
to assess cure. The increase in Tg is a good indication
kinetics. Recently, a general procedure of the
of cure progression and is often specified for materials
determination of cure kinetics by TMDSC was
as proof that the material is cured sufficiently. However,
proposed (a.9) and verified by application to a three
it is not trivial to relate Tg to the degree-of-cure. It is
component epoxy system.
possible to ‘calibrate’ Tg to the degree-of-cure. Such
an approach has been described (71) for an amine-
Thermogravimetric analysis (TGA) follows the weight epoxy curing material. It was found that exponential
change of a sample following a defined temperature equations could be used to relate the degree-of-cure to
programme. This can be used for the study of materials the Tg. Different equations were required for values of
that exhibit a weight loss during cure, such as phenolics. degree-of-cure above or below 0.55. It was thought that
this value of degree-of-cure probably corresponded to
Gas chromatography can measure the quantity of gelation.
unreacted monomer material present in a sample.
However, it can present difficulties to extract the An interlaboratory comparison for measurement of Tg
volatile monomer material from the polymer matrix. for composites and adhesives, showed that DSC and
The principal benefit of the technique is that it is DMA can give significantly different values for Tg of
sensitive to very low levels of a component. the same material (a.10). Although, from a technical
viewpoint this is reasonable, as the two techniques
Infrared spectroscopy is a type of vibrational measure different properties, it can lead to problems
spectroscopy, which can identify and quantify as logically a single value for Tg would be expected.
functional groups. This technique can provide much There can be a similar problem with defining the
information on the progress of the cure reaction and gelation point as it is not universally defined between
can provide degree-of-cure information. A limitation different techniques.
of the technique is that it may not be used with heavily
filled materials that do not allow transmission of the For the measurement of Tg, the preferred technique is
infrared radiation. Raman spectroscopy can also be often DMA, as DSC can have poor sensitivity and DEA
is not commonly adopted for routine testing. A problem This variation in material properties will have a
with measuring glass transition temperature by thermal different effect on different techniques. Some
analysis techniques is that the sample is heated during techniques measure relatively large volumes of
the test. This heating may progress the cure reaction materials, such as ultrasonic methods and parallel plate
during the test, so the reported Tg may be higher and dielectric methods, where properties are averaged
the sample will be changed by the test. through the thickness of the material. Where a result is
averaged across the thickness of the material, it is
essential to have an appreciation of the variation that
is contained within that result.
6.3 Quality Assurance
On the other hand evanescent wave sensors or
Consideration of cure monitoring up to this point has
interdigitated dielectric sensors measure a very small
focussed on the use of results within the processing
volume of material surrounding the sensor. This
environment, or, at most, comparison with post
presents an opportunity to place a number of sensors
processing quality control. There is however, a wider
at different locations within the component, so the
opportunity for cure monitoring to provide assurance
degree-of-cure can be seen at different locations. This
to purchasers and users of the materials or components
is potentially reassuring, although it must be balanced
that have been produced.
against creating vast amounts of data that it is difficult
to use effectively.
A very common aspiration is to demonstrate a good
correlation between on-line results and the performance
It is important that the difference in the meaning of
of the material in quality control tests, and ultimately
results from these two broad classes of sensors are
the performance of the materials in service. Dielectric
appreciated as one class of sensors report data averaged
techniques are the most advanced in their use for quality
across the material, while the other report results for a
control. The application of dielectric analysis for the
particular location within the material. When probing
quality control of sheet moulding compound (SMC)
very locally (e.g., optical fibre techniques) it is possible
and bulk moulding compound has been described
that the material close to the sensor may not be
(282). In this case, critical points from the cure
representative of the bulk. For instance because of
monitoring data were extracted and compared
segregation at the surface or thermal transfer along the
statistically with a population of samples that has
fibre.
previously passed. This allowed swift assessment of
parts against strict limits.
The availability of international standards would be of
great help to the use of cure monitoring for quality
An alternative approach to qualification of
assurance. However, there are currently no international
manufactured materials, which also is based on
standards covering on-line cure monitoring. Although
dielectric measurements, has been described (a.11). The
confirmation of the degree-of-cure has been recognised
processing of material that is the subject of this paper
as critical for quality assessment of composite materials
has traditionally relied on the mechanical testing of
(a.12).
samples after processing has been completed. The
objective was to develop a system of cure monitoring
that could dispense with the sample testing. This was There are standards that are relevant to aspects of cure
achieved by curing a DEA specimen separately using monitoring. These cover generic measurements to
a temperature profile that followed the temperature of assess cure properties, the use of cure assessment
the lagging thermocouple in the autoclave. Hence, methods or guidance on the techniques that are relevant
dielectric data is obtained for the least cured part of to cure assessment. These are listed in Table 1.
the component.
There is a general problem with establishing standard
With the use of any analysis technique, it is always test methods that they can appear either too specific,
necessary to consider how representative, and therefore with a limited scope, or too generic, with procedures
how meaningful, an analysis result is. For a that are too generalised. For technologies such as cure
homogeneous material, the sampling of the material is monitoring there will be a substantial challenge in
less relevant. However for composites and adhesives establishing standardised procedures.
there is a good chance that the material is
inhomogeneous, due to the use of fillers and fibres and
it is possible that the resin itself is inhomogeneous,
with phase separation.
6.4 Comparison of Techniques precedence over the technology. In addition, it has been
noted that the function of the fibres is different in the
two types of techniques (283). For monitoring
6.4.1 Technical Considerations mechanical properties, a very small and delicate sensor
is present on the optical fibre, whereas for spectroscopic
As discussed in Section 1.2, there are several classes monitoring the fibre merely transmits light to and from
of curing materials and numerous formulations for each the material, a less demanding function.
of these classes of materials. In addition, there will be
variations from batch to batch of nominally the same Although there are practical examples of all the
formulation. On the other hand there is also a wide techniques being used to improve processing, ultrasonic
range of processing methods that use curing material. and dielectric techniques can be viewed as being the
The result of this is that it is very difficult to be most established techniques. However, there is little
prescriptive in the choice of cure monitoring technique, similarity between the usage of the two techniques.
i.e., no single technique will be universally applicable Ultrasonic techniques have been used for some time and
to a particular material, or a particular process. they provide information on the modulus of the curing
material. However, ultrasonic techniques are generally
The scope of this review has covered the spectrum of mature and there are unlikely to be major jumps in the
cure monitoring techniques that have been developed. development of ultrasonic techniques. Progress is likely
It should be recognised that this covers a wide range to focus on reduction in cost and improvements in the
of technical disciplines, which presents challenges in quality and reliability of the equipment.
comparing the techniques as the only universal feature
is the curing material that is being monitored. However, On the other hand, dielectric techniques are the focus
this Section will attempt to draw together some of the of substantial development work and are often claimed
studies that have considered cure monitoring by more to be the most promising cure monitoring techniques.
than one technique. Certainly, there are a number of appealing features with
dielectric techniques, as there are a variety of sensors
The use of optical fibre for sensing mechanical and detailed information on the cure progress may be
properties and spectroscopy has been considered obtained. However, the adoption of these techniques
separately in this review, although in many reviews in higher volume processes may not be straightforward
they will be considered together. They have been as there is not a consensus on the best approach to
separated here as they measure unrelated properties of interpretation of the results and the quantities measured
the material, and in this report the application is given can appear abstract.
A comparison of several techniques for cure monitoring techniques will fare with repeated use in a
(114) considered FTIR and ultrasonic measurements, manufacturing process.
alongside DSC measurements. It was found that FTIR
was most sensitive early in cure, before structure
formed, as it is sensitive to the chemical changes in 6.4.2 Practical Considerations
the material. As cure progresses and mechanical
properties develop the ultrasonic technique became There are a whole range of practical considerations
more sensitive. Degree-of-cure calculation from FTIR before cure monitoring is implemented. Many of these
and DSC showed reasonable, but not exact, agreement will be specific to the individual process, but there are
several generic issues, such as location of sensors and
Results from dielectric and ultrasonic techniques for a cost that will be considered in this Section. In addition,
carbon fibre-epoxy prepreg have been compared (106). it should be remembered that safe operation must also
It was found that there was excellent agreement be considered. With the exception of techniques using
between resistivity, from the dielectric method, and the lasers, the techniques possess little inherent risks.
speed of sound, from the ultrasonic method. Although However, many of the processes will involve elevated
the individual techniques may not be feasible for a temperatures and pressures, and perhaps harmful
specific application, generally the data will be valid chemicals. It is important that any cure monitoring
from either technique. With no significant technical method does not expose people to any of these hazards.
differences, the choice of technique will be largely
driven by practical issues of implementing cure The most fundamental difference between sensors is
monitoring. whether the sensors are permanently housed in a mould,
so are used repeatedly, or are placed within the curing
The use of various types of optical fibre sensors for materials, so are used only once. Where sensors are
cure monitoring of an amine-epoxy has been reported used in the mould, some sensors only require access to
(193). The sensors used were evanescent wave sensors one side of the mould, while others require access to
for refractive index and evanescent wave and both sides. This can influence the choice of technique
transmission sensors for infrared spectroscopy. All where there is only one side to the mould, for instance
methods were sensitive to the cure of the material, hand lay up, as it will not usually be possible to use a
however there were discrepancies in the data reported method which requires access to both sides of the
by different types of sensor. Proposed reasons to material. The common usage of sensors for several of
account for this were interaction between the resin and the cure monitoring techniques is described in Table 2.
the fibre, inaccurate correlation of refractive index with
the degree-of-cure and local variations that had a The presence of cure monitoring sensors in high
significant effect on the evanescent wave sensor. Some performance materials can have a deleterious effect on
of these difficulties are related to sampling of the the properties of the material with decreases in
materials, but significant problems can arise in toughness and strength reported. However, if structural
obtaining accurate technical results from any of the health monitoring is desired, for instance by optical
techniques. fibre sensors, their presence will be desirable. In this
case, the same sensors can be used during processing
An even more wide ranging study of cure monitoring and in service. In fact, their subsequent use for
techniques has been conducted for a carbon fibre- monitoring is the strongest argument for the use of
phenolic composite (271). This study reported on the optical fibre sensors. Otherwise the difficulty of
use of thermal, ultrasonic, interdigitated dielectric and introducing a straight, intact optical fibre to the material
extrinsic Fabry-Pérot sensors. In this case, the will prohibit their use in most applications.
ultrasonic technique was not successful; this was
though to be due to degradation of the couplant. It was Clearly, the location of sensors will have an impact on
also found that the extrinsic Fabry-Pérot sensor the cost of a cure monitoring technique. It will
degraded during cure of the material. However, the obviously be cheaper to reuse the same sensors, than
dielectric technique was used successfully and use a new sensor for each component. However, the
indication of the critical point for mould closure was cost of sensors may only be a relatively small
obtained. However, the final observation from this contribution to the overall cost of implementing cure
study concerns the durability of sensors and their monitoring.
vulnerability in the manufacturing process. For
implementation to be worthwhile the technology must No attempt will be made here to assess the absolute
be right, however it is essential to consider how the costs of implementing cure monitoring, but to highlight
some of the factors that need to be considered. For To a large extent these barriers will be addressed
instance, the ease with which the sensors can be through cure monitoring acquiring a critical mass of
incorporated can affect the cost. For in-mould sensors, adoption. If there is sufficient take up of the technology
there can be a significant initial cost associated with then the costs of equipment will reduce and the
incorporating sensors into the mould, but once in place, expertise will be more readily available. There are a
they should have minimal impact. For in-material number of specific cure monitoring technologies that
sensors, they will need to be incorporated in each new warrant further research. However, for cure monitoring
component. For interdigitated sensors this should not in general, the next major steps will not be in pure
be too demanding, but can present a major challenge research, but through the commercial exploitation of
with optical fibre sensors. cure monitoring technologies by both original
equipment manufacturers and materials processors.
Cure monitoring is an active area of academic research a.1 R. Davidson and N. L. Hancox, Cure monitoring
and industrial development and there are ongoing of resins in fibre composites, AEAT Report
research programmes to produce new techniques and AEAT-CPD4B-R1, Abingdon, UK, 2000.
develop existing techniques. In terms of a.2 I. K. Partridge, Networking in Cure
implementation there have been several notable Monitoring, Materials World, July, 1999,
successes, where cure monitoring has been successfully London, UK.
used in a commercial environment. The benefits are
generally observed in terms of improvements of both a.3 N. Oshima, K. Aoki, S. Umemoto, S. Motogi
efficiency and quality. and T. Fukuda, Journal of the Japan Society
for Composite Materials, 2001, 27, 5, 237.
It would be fair to say that cure monitoring is nowhere
a.4 R.A. Pethrick, Plastics, Rubber and
near fulfilling its potential to improve manufacturing.
Composites Processing and Applications,
Many commercial operations currently rely on either
1998, 27, 6, 257.
temperature monitoring or off-line cure assessment and
there may be a reluctance to tamper with a process that a.5 J.K. Gillham in Encyclopaedia of Polymer
is working successfully. This factor, combined with a Science and Engineering, Volume 4, 2nd
perception of high cost and a requirement for technical Edition, Eds., H.F. Mark, N.M. Bikales, C.G.
expertise has hindered adoption of cure monitoring Overberger and G. Menges, John Wiley &
techniques. Both research and implementation have Sons, New York, USA, 1986, 519.
tended to be in large companies operating high value-
low volume manufacturing processes, where the capital a.6 C. Carfagna, V. Ambrogi, G, Malucelli and M.
and staff initially required to implement cure Giamberini, Journal of Adhesion Science and
monitoring can more easily be found. Technology, 2001, 15, 13, 1635.
CHT continuous-heating-transformation
IR infrared
L longitudinal modulus
PTFE polytetrafluoroethylene
TTT time-temperature-transformation
Vl longitudinal velocity
Z complex impedance
α degree-of-cure
δ phase lag
ε* complex permittivity
ε´ real permittivity
η viscosity
ρ density
σ ionic conductivity
Item 1 Item 3
Handbook of Polymer Blends and Composites. Volume 1. Journal of Applied Polymer Science
Shawbury, Rapra Technology Ltd., 2002, p.501-28 88, No.2, 11th April 2003, p.452-8
COMPOSITES: AT THE TURN OF CENTURY ANALYSIS OF THE CURE REACTION OF
Kulshreshtha A K; Vasile C CARBON NANOTUBES/EPOXY RESIN
Petru Poni,Institute of Macromolecular Chemistry; COMPOSITES THROUGH THERMAL
Indian Petrochemical Corp.Ltd. ANALYSIS AND RAMAN SPECTROSCOPY
Edited by: Vasile C; Kulshreshtha A K Puglia D; Valentini L; Kenny J M
Perugia,University
Trends in composites and emerging technology for the
production of composite products at the turn of the century The effect of incorporating single-walled carbon
are discussed. Attention is paid to smart composites, nanotubes (SWNTs) on the cure reaction of a bisphenol
nanocomposites, resin developments at NASA, A diglycidyl ether epoxy matrix was studied by thermal
micromoulding, rapid prototyping, vacuum assisted resin analysis and Raman spectroscopy. The result showed that
transfer moulding, cure monitoring, wood-filled SWNTs acted as a strong catalyst. A shift of the
thermoplastics, PEEK composites, liquid crystal polymer exothermic reaction peak to lower temperatures was
composites, composite recycling, underwater observed in the presence of SWNTs. The effects occurred
applications, offshore applications, shipbuilding, dental at the lower nanotube concentration analysed (5%) and a
applications, medical applications, polymer concrete, civil further increase in SWNT concentration (to 10%)
engineering and packaging. 26 refs. produced only a slightly increased effect, suggesting a
US,NATIONAL AERONAUTICS & SPACE saturation of the catalysing action at the higher
ADMINISTRATION concentration. The thermal degradation of the epoxy resin/
EASTERN EUROPE; INDIA; RUMANIA SWNT composite was faster than that of cured epoxy
Accession no.886384 resin. Raman spectroscopy showed that the observed
changes in the cure reaction of the composites led to a
different residual strain on the SWNT bundles following
Item 2 a different intercalation of the epoxy matrix. 28 refs.
International Polymer Science and Technology EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
30, No.4, 2003, p.T/25-32 WESTERN EUROPE
PREPREGS WITH LONG SERVICE LIFE. 2. Accession no.883770
RHEOKINETIC SELECTION OF INDUSTRIAL
TYPES OF EPOXY RESINS AND CURING
Item 4
AGENTS
International Journal of Polymeric Materials
Smirnov Y N; Kruzhkova S V; Shatskaia T E;
52, No.3, March 2003, p.175-88
Natrusov V I
CURE CHARACTERISTICS AND MECHANICAL
Russian Academy of Sciences; AOO NPO Stekloplastik
PROPERTIES OF SHORT NYLON FIBER
-NPK Kompozit
REINFORCED ACRYLONITRILE BUTADIENE
A rheokinetic analysis is made of the curing processes RUBBER/RECLAIMED RUBBER BLENDS
for a number of the cheapest industrial grades of epoxy Sreeja T D; Kutty S K N
resins and curing agents produced in large volumes, and Cochin,University of Science & Technology
the selection of them for implementation in various types
The cure characteristics and mechanical properties of
of prepreg technology. Previous methods of selection
short nylon fibre reinforced acrylonitrile-butadiene
using an isothermic calorimeter enable the reactivity of
rubber/reclaimed rubber blends were studied. The
the binder components at prepreg storage temperatures
minimum torque, (maximum-minimum) torque and cure
to be evaluated from the initial rates of the curing process,
rate increased with increasing fibre concentration. Adding
but do not allow the maximum kinetic service life, linked
fibres decreased the scorch time and cure time. The tensile
to the gelation time for the binder at the storage
and tear properties, and the abrasion resistance, were
temperature, to be forecast because the latter also depends
enhanced by the addition of fibres and were higher for
on the functional properties of the components. An
fibres in the longitudinal direction. Heat build up values
analysis is presented of the results of the rheokinetic
increased with fibre concentration and were higher for
studies. 30 refs. (Article translated from Plasticheskie
samples with longitudinally oriented fibres. Resilience
Massy, No.6, 2002,p.18-23).
increased with the introduction of the fibres and the
RUSSIA
compression set was higher for the composites. 18 refs.
Accession no.884928 INDIA
Accession no.883693
Item 9 Item 11
Journal of Applied Polymer Science EURADH 2002. Adhesion 02. Proceedings of a
87, No.9, 28th Feb.2003, p.1493-9 conference held Glasgow, 10th-13th Sept.2002.
CROSSLINKED ACRYLIC PRESSURE- London. IOM Communications Ltd., 2002, Session 7;
SENSITIVE ADHESIVES. I. EFFECT OF THE Chemistry and Rheology, Paper 6, p.129-32, 29cm, 012
CROSSLINKING REACTION ON THE PEEL MOLECULAR MOBILITY IN AN EPOXY
STRENGTH ADHESIVE: DIELECTRIC SPECTRA FOR BULK
Asahara J; Hori N; Takemura A; Ono H AND FOR THIN LAYERS
Tokyo,University Neurohr H; Possart W; Valeske B
Saarlandes,Universitat
The relationship between the crosslinking reaction and
(Institute of Materials)
the peel strength was studied for pressure-sensitive
adhesives(PSAs) based on ethyl acrylate/2-ethylhexyl The molecular dynamics of an epoxy adhesive during
acrylate/2-hydroxyethyl methacrylate copolymer as a base curing and after curing was investigated using dielectric
resin and polyisocyanate as a crosslinking agent. A 90 spectroscopy. The dielectric spectra for thin layer joints
degree peel test of cured PSA films under various storage with aluminium adherends were compared with those for
conditions was carried out. The isocyanate(NCO) thicker adhesive films and the dielectric behaviour of the
consumption in these PSA films was also monitored by cured epoxy system in the glassy state characterised. It
ATR/FTIR spectroscopy. The peel strength of the PSA was found that in layers having a thickness of less than
compounded with the crosslinking agent decreased as the 10 micrometers curing gave rise to earlier vitrification,
NCO groups were consumed. The elevation of the ageing resulting in a less mobile network structure as indicated
temperature promoted the crosslinking reaction and by increased activation energies for secondary relaxations
increased the decrement in the peel strength. The peel in the cured state. 7 refs.
strength of non-crosslinked and crosslinked PSA films EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
increased with the contact time. A high storage UK; WESTERN EUROPE
temperature made the increment in the peel strength Accession no.876570
increase. The addition of the crosslinking agent to the
PSA films reduced the increment in the peel strength.
Item 12
Furthermore, PSA films with residual NCO groups
EURADH 2002. Adhesion 02. Proceedings of a
possessed stronger peel strengths than fully cured films.
conference held Glasgow, 10th-13th Sept.2002.
10 refs.
London. IOM Communications Ltd., 2002, Session 7;
JAPAN
Chemistry and Rheology, Paper 5, p.125-8, 29cm, 012
Accession no.879831 COMBINING IR-ERAS AND SPECTRA
CALCULATION FOR THE STUDY OF THE
Item 10 CURING REACTION IN ULTRA-THIN EPOXY
Polymer Composites FILMS ON METALS
23, No.6, Dec.2002, p.1111-9 Wehlack C; Valeske B; Possart W
SEPARATION OF GELATION FROM Saarlandes,Universitat
VITRIFICATION IN CURING OF A FIBER- (Institute of Materials)
REINFORCED EPOXY COMPOSITE Changes in the chemical structure of spin coated epoxy
Bilyeu B; Brostow W; Menard K P resin adhesive films on aluminium substrates were
North Texas,University; Perkin-Elmer Inc. investigated using a combination of IR spectroscopy and
Temperature-modulated DSC (TMDSC) and DMA were reflection absorption spectroscopy during curing of the
used to characterise prepregs composed of a mixture of adhesive. The spectroscopic degree of epoxy conversion
tetraglycidyl 4,4-diaminodiphenylmethane and 4,4'- during curing of the ultra-thin films was quantitatively
diaminodiphenylsulphone. Separation of the baseline shift analysed and compared with that of bulk adhesive. 2 refs.
of the Tg from the curing isotherm was achieved using EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
TMDSC and step scan DSC temperature scans and UK; WESTERN EUROPE
TMDSC isotherms were utilised to isolate the baseline Accession no.876569
shift in heat capacity due to vitrification. Using the data
obtained, a time-temperature-transformation diagram was Item 13
developed for optimising the curing of the epoxy prepreg. ANTEC 2002. Proceedings of the 60th SPE Annual
17 refs. Technical Conference held San Francisco, Ca., 5th-9th
USA May 2002.
Accession no.876661 Brookfield, Ct., SPE, 2002, Paper 441, Session T41-
Composites. Other Reinforcements in Composites I,
pp.5, CD-ROM, 012
CAPACITIVE SENSING DIELECTROMETERS adhesive was cured with the Electro-Lite BondWand and
FOR NONCONTACT CHARACTERIZATION OF EXFO Novacure light guide devices. 3 refs.
ADHESIVES AND EPOXIES USA
Schlicker D; Sheiretov Y; Washabaugh A; Goldfine N Accession no.875941
Jentek Sensors Inc.
(SPE)
Item 16
Sensors incorporating multiple sensing elements are Journal of Polymer Science: Polymer Chemistry
described which enable the non-contact measurement of Edition
dielectric properties from one side of a sample. The 40, No.23, 1st Dec.2002, p.4236-44
multiple wavelength electrode structures control the ULTRAVIOLET CURING OF ACRYLIC
penetration depth of the electric field, and can SYSTEMS: REAL TIME FOURIER TRANSFORM
accommodate variations in lift-off or air gap. The INFRARED, MECHANICAL, AND
dielectric properties may be correlated with the state of FLUORESCENCE STUDIES
cure, and are suitable for monitoring epoxies and Peinado C; Salvador E F; Alonso A; Corrales T;
adhesives in thick and thin film applications. Baselga J; Catalina F
USA CSIC; Madrid,Universidad Carlos III
Accession no.876531 The UV curing of an acrylic adhesive was studied with
two different initiators (2-benzyl-2-N,N-dimethylamino-
1-(4-morpholinophenyl)-1-butanone (DBMP) or
Item 14
bis(2,4,6-trimethylbenzoyl)phenyl phosphine oxide
Journal of Composite Materials
(TMBAPO)). Real time FTIR was used to measure the
36, No.21, 2002, p.2479-98
acrylate double bond conversion at different irradiation
CURE KINETIC MODEL, HEAT OF REACTION,
times and the changes in fluorescence intensity were also
AND GLASS TRANSITION TEMPERATURE OF
measured in real time. The polymerisation rate depended
AS4/3501-6 GRAPHITE-EPOXY PREPREGS
on the square root of the absorbed light intensity when
Kim J; Moon T J; Howell J R
DMBP was used as the photoinitiator, whereas primary
Texas,University at Austin
radical termination was observed when TMBAPO was
An isothermally-based cure kinetic model for a carbon used. The fluorescence emission changes of different
graphite-epoxy AS4/3501-6 benchmark prepreg system fluorescent probes during UV curing also showed different
containing tetraglycidyl methylenedianiline, alicyclic behaviours which depended on the nature of the
diepoxy carboxylate, epoxy cresol novolac, photoinitiator. The results were discussed. 19 refs.
diaminodiphenyl sulphone and boron trifluoride amine EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
complex is presented. The cure kinetics of the prepreg were WESTERN EUROPE
determined by DSC and the mass fraction of the epoxy Accession no.875050
resin in the prepreg by thermogravimetry. The ultimate heat
of reaction of the resin incorporated within the prepreg was Item 17
measured using dynamic DSC scans at 20C/min. and the Polymer
Tg of the partially-cured and fully cured prepregs 43, No.25, 2002, p.6829-37
determined by differential scanning calorimetry. 35 refs. SMALL ANGLE LIGHT SCATTERING
USA INVESTIGATION OF POLYMER DISPERSED
Accession no.875966 LIQUID CRYSTAL COMPOSITES
Maugey J; Navard P
Paris,Ecole des Mines
Item 15
Adhesives Age The curing of a homogeneous mixture of a nematic liquid
45, No.12, Dec.2002, p.12-4 crystal and an acrylate UV curable prepolymer was
THE RIGHT LIGHT FOR EPOXIES studied using small angle light scattering. The temperature
Dake K and UV intensity during curing were varied. Phase
DSM Desotech separation occurred for all conditions other than elevated
temperatures. The isotropic-to-nematic transition could
Test methods for quantifying the degree of cure of UV be seen as a decrease of the scattering intensity. For all
curing epoxy adhesives and establishing optimum cure the conditions studied, the final morphology was a droplet
conditions are considered. These methods include Shore morphology. At high UV intensity, two scattering peaks
D hardness testing, lap shear testing, fibre pull-out and were observed which were thought to be possibly due to
measurement of changes in functionality via FTIR a double spinodal decomposition. 29 refs
spectroscopy. The results of tests carried out on a UV-
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
curable adhesive subjected to various light exposures WESTERN EUROPE
using the above methods are presented and discussed. This
Accession no.874652
measurements taken during manufacture of a composite are measured in the composite laminates curing using
specimen are presented. The laser ultrasonic cure embedded fibre optic strain sensors and electrical
monitoring system described had the ability to operate in resistance strain gauges. It is found that significant strain
a high temp. and high pressure environment, was small is developed by interference between composite and
enough to be incorporated into moulds and measured the mould during cure, resulting in constraint-induced strain.
cure state at several locations within the composite part. The magnitude of residual stresses is also assessed by
27 refs. measuring the warpage curvature of asymmetric cross ply
USA laminates. The data show that the residual stress is
Accession no.865846 significantly dependent on the cure cycle and the
interference. 13 refs.
USA
Item 26
Polymer Composites Accession no.864818
23, No.4, Aug. 2002, p.479-94
MONITORING THE REACTION PROGRESS OF Item 28
A HIGH-PERFORMANCE PHENYLETHYNYL- Journal of Reinforced Plastics & Composites
TERMINATED POLY(ETHERIMIDE). PART II. 21, No.13, 2002, p.1193-203
ADVANCEMENT OF GLASS TRANSITION THERMAL PROPERTY MEASUREMENTS
TEMPERATURE DURING CURING OF THERMOSET RESINS
Bullions T A; Stoykovich M P; McGrath J E; Loos A C USING STEADY PERIODIC CONDITIONS
Virginia Polytechnic Institute & State University Garnier B; Sommier A
Nantes,Laboratoire de thermocinetique
An attempt was made to identify the cure schedules
maximising Tg by monitoring the progress of the reaction Variation of thermal diffusivity and specific heat of a
through Tg measurements following different cure general-purpose epoxy during curing is investigated
schedules for carbon fibre-reinforced phenylethynyl- experimentally. The thermoset materials are particularly
terminated polyetherimide composites. Towpreg and neat difficult to characterise during their polymerisation on
resin samples were cured in a differential scanning the one hand because of the presence of exothermic
calorimeter, Tgs of all specimens were measured by DSC chemical reactions, and on the other because their
and the Tgs of composites were also measured by dynamic thermophysical properties depend both on the temperature
mechanical thermal analysis. It was found that the Tgs of and on the degree of cure. Due to a method in periodic
the composite and towpreg increased to a plateau with mode associated with very sensitive thermal sensors, it is
increasing cure time and cure temperature and that the possible to separate and measure the variations of thermal
neat resin exhibited an optimal Tg followed by a reduction diffusivity with temperature and degree of cure during
in Tg with increasing cure time and cure temperature. 28 the thermoset polymerisation. In addition, heat capacity
refs. analysis is performed during cure using a temperature
USA modulated calorimeter. Thermal diffusivity measurements
Accession no.865325 show a non-linear increase of more than 100% during the
cure of an epoxy/glass fibre composite while heat capacity
changes are less than 10%. 10 refs.
Item 27 EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Journal of Composite Materials WESTERN EUROPE
36, No.14, 2002, p.1725-43 Accession no.864812
CURE CYCLE EFFECT ON COMPOSITE
STRUCTURES MANUFACTURED BY RESIN
TRANSFER MOULDING Item 29
Kim Y K; Daniel I M Journal of Composite Materials
Georgia,Institute of Technology; Northwestern 36, No.10, 2002, p.1201-31
University THICK-SECTIONED RTM COMPOSITE
MANUFACTURING, PART II. ROBUST CURE
An experimental investigation is conducted of the effect CYCLE OPTIMIZATION AND CONTROL
of curing cycle on the development of material properties, Michaud D J; Beris A N; Dhurjati P S
residual strains and stresses in composite parts during the Delaware,University
resin transfer moulding (RTM) process. The material
investigated consisted of AS4 carbon fibres as the preform The development of a robust optimisation and control
and a three-part epoxy system. Unidirectional indirect and methodology for identifying and implementing optimal
crossply carbon/epoxy laminates are prepared by the RTM curing conditions for the thick-sectioned resin transfer
process in aluminium moulds. Several different curing moulding of composites is described. The requirement
cycles are designed by changing the peak cure temperature of at least one cooling stage in the cure cycle for the
and heat up rate based on a cure kinetic model. Strains manufacture of quality composites in a minimum amount
is cooled to ambient from its elevated processing strength can be increased even further by suitable thermal
temperature. These stresses can be significant enough to post-curing. 5 refs. (Article translated from Gummi Fasern
distort the dimensions and shape of a cured part as well Kunststoffe, No.1, 2001, pp.34)
as initiate damage in off-axis plies, either during EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
fabrication or under the application of relatively low WESTERN EUROPE
mechanical loads. The magnitude of these stresses Accession no.859553
depends on a number of factors including anisotropy,
volume fraction and thermal expansion, ply orientation,
Item 35
process cycle and matrix cure chemistry. Embedded strain
Composites Part A: Applied Science and
gauges are employed to follow, in situ, the build-up of
Manufacturing
residual strains in carbon fibre-reinforced laminates
33A, No.6, 2002, p.841-54
during cure. The data are compared to those from
MODEL-ASSISTED FEEDBACK CONTROL FOR
volumetric dilatometer studies to ascertain the fraction
LIQUID COMPOSITE MOLDING
of resin shrinkage that contribute to residual stress build-
Dunkers J P; Flynn K M; Parnas R S; Sourlas D D
up during cure. Based on earlier studies with single fibre
US,National Inst.of Standards & Technology; Missouri-
model composites, the process cycle in each case is then
Rolla,University
varied to determine if the cycles optimised to minimise
residual stresses for isolated fibres in an infinite matrix A model-assisted feedback control algorithm, a type of
are applicable to the reduction of residual stresses in generic mode control, was used to control cure in resin
conventional multi-fibre composites. The results of these transfer moulding. This control algorithm calculated an
studies are reported. 13 refs. apparent temp. of reaction based on the cure data input
USA from a sensor and this temp. was used to compare the
Accession no.860540 actual rate of reaction with the desired rate and to calculate
the mould set-point temp. The model input into the control
algorithm was an empirical cure model of a pre-ceramic
Item 34 polymer with an Arrhenius temp. dependence from 55 to
International Polymer Science and Technology 95C. The effect of varying control parameters was
29, No.7, 2002, p.T/5-10 evaluated through cure simulations and experiments. The
INVESTIGATION OF ADHESIVE LIGHT- effect of noise on the controller robustness was also
CURING USING THE PRE-ACTIVATION evaluated through simulation and experiment. Control
TECHNIQUE. 2 parameters were evaluated for temps. of 55 and 95C.
Ehrenstein G W 30 refs.
Erlangen,Universitat USA
The pre-activation technique is described as a method of Accession no.858464
speeding up assembly times using UV curing adhesives.
The adhesive is pre-activated by radiation after metering,
Item 36
followed by the application of the constructional element
Elgin, Il., 2001, pp.4. 28cms. 25/4/02
and heat post-treatment. The integration of the pre-
DESOBOND UV-CURABLE ADHESIVES :
activation into the bonding process makes it possible to
DESOBOND 956-104
keep the irradiation preceding the assembly short and
DSM Desotech Inc.
comparatively low-intensity in the first stage of the
process, so that a later post-curing by means of heat A datasheet from DSM Desotech provides details of the
radiation, can be flexibly incorporated without loss of acrylate-urethane adhesive DesoBond 956-104. This
time. The pre-activation technique also permits successive medium Tg, medium viscosity, UV-curable adhesive for
feeding of several adhesive points and additional surface optical fibres has been formulated to provide strong,
curing of the region to be bonded by radiation. With the durable bonding on substrates including glass, metals and
aid of a pot life of the adhesive optimised on the basis of plastics. The adhesive is rigid when cured, yet allows for
the number of equipment elements, the assembly some flexibility. Product benefits are listed and data
operation can thus be carried out using heat-based post- tabulated relating to performance characteristics and
hardening. This permits the possibility of multiple bonds typical properties. Graphs show the degree of cure using
on complex substrates. Using viscosity and DSC FTIR measurement and dynamic mechanical analysis
measurements, it was possible to characterise the curing results. Recommendations for the safe storage and use of
behaviour of the light-curing epoxy adhesive as a function the adhesive are also included. 2 figs.
of the irradiation intensity and time at different USA
temperatures. Compression and shear tests were carried Accession no.858287
out to assess the achievable adhesion strengths, and
showed that durable adhesive joints can be obtained with
suitable irradiation time and intensity, and that their
for further spectroscopic, calorimetric and mechanical UV lamps, and the spectroscopic data confirmed by
evaluation. Interpretation of calorimetric and measurement of the peel strength and shear strength of
spectroscopic analysis revealed a high consumption of the UV cured adhesive. 17 refs.
isocyanate early in cure. Mechanical strength, however, EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
as revealed by lap shear tests, did not develop until late WESTERN EUROPE
in cure. Low lap shear strengths and a plateau in Accession no.850402
conversion rates were detected for samples pressed at 110
and 120C. Several components of the analysis suggested
Item 49
that low temperature cure could result in crystal formation,
Polymer Preprints. Volume 42, number 2. Fall 2001.
leading to diffusion controlled cure. 24 refs.
Proceedings of a conference held Chicago, Il., 26th-
USA
30th August 2001.
Accession no.851472 Washington, D.C., ACS,Div.of Polymer Chemistry,
2001, p.216-7
Item 47 CURE KINETICS OF PHOTOCURABLE
Journal of Applied Polymer Science ADHESIVES
84, No.1, 4th April 2002, p.144-54 Wang Q; Zhu P; Li Z
EQUIVALENT PROCESSING TIME ANALYSIS Southern Mississippi,University; Hebei,University of
OF GLASS TRANSITION DEVELOPMENT IN Technology
EPOXY/CARBON FIBER COMPOSITE (ACS,Div.of Polymer Chemistry)
SYSTEMS The development and application of photocurable
Park I-K; Lee D-S; Nam J-D materials are increasingly gaining interest due to their
Sung Kyun Kwan,University lowered pollution emissions, lowered costs and high
Differential scanning calorimetry was used to examine processing efficiencies compared to their conventional
cure kinetics and glass transition temperature development counterparts. These materials have a wide range of
during the cure of a commercially available epoxy resin/ applications, including printing, coatings, sealants and
carbon fibre prepreg system. Isothermal and dynamic adhesives. In particular, the liquid crystal display device
heating experiments were carried out, and results were can be automatically produced, with higher efficiency,
used to develop a kinetic model describing the degree of due to advancement, in photosensitive sealants and
cure as a function of isothermal curing temperatures. adhesives. Cure behaviour is very important for a
Incorporation of the maximum degree of cure into this photocurable adhesive as it influences the cured film’s
model gave kinetic equations that described both properties. The photocuring kinetics of several UV-
isothermal and dynamic heating behaviour. Glass curable epoxy acrylate adhesives, synthesised based on
transition temperature as a function of degree of cure was the ring-opening reaction of epoxy-resin and acrylic acid,
indicated by the Di Beneditto equation and equivalent are studied by differential photocalorimetry. The effects
processing time was used to evaluate development of glass of several variables are studied including the amount of
transition temperature for different curing conditions photoinitiator, cure temperature, air and nitrogen, active
where internal stress build-up during cure and subsequent diluents. Induction time in air is less than nine seconds,
cooling stages were considered. 38 refs. and the maximum cure rate is reached within twenty
KOREA seconds under 30 deg.C. However, at the same
temperature, but in nitrogen, the induction time is less
Accession no.851110
than four seconds, and the maximum cure rate is reached
within ten seconds. Using nitrogen will increase the speed
Item 48 of the reaction when compared to oxygen, by decreasing
Journal of Coatings Technology the time necessary for induction and decreasing the time
74, No.927, April 2002, p.41-7 necessary for the maximum cure rate to be achieved. By
UV CURING OF A PRESSURE SENSITIVE choosing the appropriate active diluent and the cure
ADHESIVE COATING STUDIED BY REAL- temperature, the photocure rate can be adjusted. 5 refs.
TIME FTIR SPECTROSCOPY AND CHINA; USA
LABORATORY SCALE CURING EXPERIMENTS Accession no.848987
Tauber A; Scherzer T; Weiss I; Mehnert R
Institut fuer Oberflaechenmodifizierung
Item 50
The UV curing behaviour of a hot melt, pressure-sensitive Composites Science & Technology
adhesive composed of an acrylic polymer with a 62, No.3, 2002, p.457-67
photoreactive functional group in the side chain was CURING OPTIMISATION FOR PULTRUDED
investigated using real-time FTIR spectroscopy. UV light COMPOSITE SECTIONS
flash experiments were carried out to simulate production Li J; Joshi S C; Lam Y C
parameters, such as cure velocity and number of required Nanyang,Technological University
A mathematical relationship between the degree of cure An experimental technique was developed for monitoring
profile across the cross-section of a pultruded part and residual stress development throughout the composite
the die-heater temperatures is established. The relationship patch repair curing process. Process-induced strains and
is employed to optimise the die-heating profile such that specimen warpage during a number of different cure
finally a near-uniformly-cured component can be cycles were measured using this technique for a simulated
obtained. The algorithm is implemented using the 3D single-sided composite patch repair of an aluminium
finite element/nodal control volume (FE/NCV) approach substrate. Models for adhesive cure rate and Tg behaviour
for process simulation. The application of the procedure of the patch adhesive resin (FM 300-1K) were combined
is demonstrated by simulating the pultrusion of composite with a simple bimetallic strip model to predict specimen
sections that use a multi-heater die. The effects of the warpage and strain behaviour during cure. Model
element aspect ratio and different initial heater conditions predictions were compared with experimental
are studied. The results of the case studies show that the measurements and were used to assist in the development
developed algorithm is numerically stable and provides of optimised cure cycles. Using these optimised cycles,
optimal die temperatures for producing a uniformly cured it was found that it was possible to achieve significant
pultrudate under the prescribed process conditions. 9 refs. reductions in patch warpage and at the same time
SINGAPORE minimise processing time and obtain a high final adhesive
Accession no.848951 degree of cure. Experimental observations suggested that
an improved patch model incorporating adhesive
viscoelastic behaviour during cure would assist in
Item 51
achieving additional process improvements. 13 refs.
Macromolecular Chemistry & Physics
CANADA; USA
203, No.2, 31st Jan.2002, p.336-45
NEW FLUORESCENT PROBES FOR Accession no.846115
MONITORING POLYMERIZATION
REACTIONS: PHOTOCURING OF ACRYLIC Item 53
ADHESIVES. II. Polymer Composites
Bosch P; Fernandez-Arizpe A; Catalina F; Mateo J L; 23, No.1, Feb. 2002, p.10-20
Peinado C NEW FABRICATION TECHNIQUE UTILISING A
CSIC COMPOSITE MATERIAL APPLIED TO
ORTHOPAEDIC BRACING
The fluorescence of selected amide-based probes was
Morrison B J; Creasy T S; Polliack A A; Fite R
monitored over the entire range of curing of acrylic-based
Southern California,University; California,Center for
adhesives (Loctite 329 and Loctite 312). The changes of
Applied Rehabilitation Technology
fluorescent parameters were continuously measured
during the photocrosslinking process. Real-time FTIR The feasibility of using a fabrication and fitting technique
spectroscopy was used to quantify the conversion at utilising an epoxy resin, which initiates cure at a
different irradiation times. The intensity ratio, maximum temperature of 121C but which cures at 154C, as a rapid
emission wavelength and first moment of fluorescence and cost-effective alternative to a process employing PP
could be used as parameters to determine the conversion. to fabricate orthopaedic braces was investigated. Flexural
Two-slope plots were obtained, which corresponded to tests were carried out on advanced carbon composites with
the different stages of the reaction. The use of the different degrees of cure to determine the effect of
fluorescence technique allowed the mechanism taking adjustment to complete a component on the residual
place and the role of the binder matrix to be understood, mechanical properties of the specimen once fully cured.
depending on the photoinitiator used. 28 refs. The degree of partial cure achieved during each cure cycle
was assessed using DSC. 14 refs.
LOCTITE
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA
WESTERN EUROPE Accession no.845116
Accession no.847537
Item 54
Item 52 Composites Part A: Applied Science and
Composites Part A: Applied Science and Manufacturing
Manufacturing 33A, No.3, 2002, p.385-97
33A, No.2, 2002, p.277-88 LINEAR DIRECT CURRENT SENSING SYSTEM
RESIDUAL STRESS DEVELOPMENT DURING FOR FLOW MONITORING IN LIQUID
THE COMPOSITE PATCH BONDING PROCESS: COMPOSITE MOULDING
MEASUREMENT AND MODELING Luthy T; Ermanni P
Djokic D; Johnston A; Rogers A; Lee-Sullivan P; Mrad N Swiss Federal Institute of Technology
New Brunswick,University; National Research Council Direct current (DC) resistance measurement is a well-
of Canada established technique for monitoring liquid composite
and degree of cure is reported. Experimental results for a paints and coatings to study the cure behaviour of these
glass fibre-reinforced epoxy composite obtained using the materials in the laboratory and in actual processing
equipment are presented and compared with those environments such as ovens, presses, moulds and
obtained utilising the effective conductivity model of autoclaves. Typical applications include study of cure
Hasselman and Benveniste and previously reported data. rates, optimisation of cycle times and the analysis of
11 refs. curing behaviour within a part or mould.
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; HOLOMETRIX MICROMET
WESTERN EUROPE USA
Accession no.837126 Accession no.834730
Item 63
Item 65
Journal of Macromolecular Science B
Composites Part A: Applied Science and
40, No.3-4, 2001, p.429-41
Manufacturing
FLUORESCENCE MONITORING OF CURING
32A, No.11, 2001, p.1561-72
PROCESS AND WATER ACCESSIBILITY AT
PROCESSING OF POLYMER COMPOSITES: AN
GLASS FIBER/EPOXY INTERPHASE ON
OPTICAL FIBRE-BASED SENSOR SYSTEM FOR
COMPOSITE MATERIALS
ON-LINE AMINE MONITORING
Gonzalez-Benito J; Mikes F; Bravo J; Aznar A J;
Liu T; Fernando G F
Baselga J
Cranfield,University
Madrid,Universidad Carlos III
An investigation was carried out into the feasibility of
Modified glass fibres with three different aminosilanes
monitoring the efficiency of mixing and the feasibility of
were labelled with 5-dimethylaminonaphthalene-1-
simultaneously monitoring amine concentration and
sulphonylchloride and the fluorescence was followed as
mixing efficiency in amine/epoxy based composites using
a function of curing time and of water uptake for two
a visible near-infrared monochromator based on a charge
epoxide formulations. It was shown that the fluorescence
coupled device. The influence of mixing efficiency on
response from fluorophores directly attached to the
the enthalpy of curing was examined by means of DSC
coupling region in glass fibre/epoxy resin composites was
and transmission spectra at specified mixing conditions
a suitable method for non-destructive and ‘in-situ’
presented and discussed. 17 refs.
monitoring of any changes that appeared at the interphase
USA
(rigidity and solvent accessibility). Fluorescence from a
dansyl label showed more rigidity when (of the three Accession no.832749
aminosilanes tested) 3-aminopropyldimethylethoxysilane
was used as the coupling agent. This suggested that the Item 66
epoxy chain interdiffusion decreased with increasing Plastics, Rubber and Composites
degree of crosslinking at the coupling region. The water 29, No.8, 2000, p.391-4
uptake process in glass fibre/epoxy resin composites could DIELECTRIC FLOW SENSING IN RESIN
be divided into two steps, the first corresponding to the TRANSFER MOULDING OF CARBON FIBRE
diffusion of water to the coupling region and the second REINFORCED COMPOSITES
to the hydrolysis of siloxane bonds in the interphase. Both Skordos A A; Partridge I K
steps were dependent on the surface treatment of the glass Cranfield,University
fibres. 29 refs. (Europhysics Conference on Structure
Development during Polymer Processing: Physical An in situ dielectric technique for sensing flow is outlined
Aspects, Sept.2000, Minho, Portugal) and shown to be suitable for use in moulding of
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; composites from liquid resins containing continuous
WESTERN EUROPE conducting fibres. This work builds upon the recent
Accession no.836377 development of a sensor for monitoring flow and cure in
thermosetting composites with (non-conductive) glass
reinforcements. The linear relationship between the
Item 64 position of the flow front in the mould and the electrical
Reinforced Plastics admittance of the sensor system, observed in resins with
45, No.11, Nov.2001, p.19 non-conductive reinforcements, is found to extend to
STUDYING CURE RATES OF COMPOSITES resins containing conducting fibres. The performance of
It is briefly reported that the latest product from the sensor in detecting the position of the flow front is
Holometrix Micromet is a laboratory measurement system evaluated by comparison with visual observations. The
for the dielectric analysis of polymers and in-process cure capability of the sensing system to monitor the cure of
monitoring of thermoset resins. The MDE Series 20 is the resin after mould filling is also investigated. The
designed to enable users of thermoset composites, resins, results demonstrate that the sensor can both locate the
MEASUREMENT TECHNIQUE USING A NOVEL to obtain both data on cooling and on heating. It also
INTEGRATED DIELECTRIC, OPTICAL FIBRE depended on the effect of microcracking (which it was
AND PIEZOELECTRIC SENSING ELEMENT assumed is responsible for the hysteresis) could be removed
FOR THE ONLINE CHARACTERISATION OF by heating (healing) near the glass transition and on a single
SMART STRUCTURES specimen providing an internal reference for comparing
Talaie A; Kosaka T; Oshima N; Osaka K; Asano Y; differences in isothermal modulus versus conversion data
Fukuda T at different temperatures. It was also assumed that glass
Osaka,City University transition is a direct measure of conversion. 0 refs.
USA
A simultaneous ion viscosity, strain and impedance (SISI)
system for measurement of the physical and chemical Accession no.817120
properties of composites during cure process described.
The SISI system uses an integrated multi-sensing element, Item 85
entitled DOP, that is comprised of dielectric (D), optical Adhesives Age
fibre (O) and piezoelectric (P) sensors. This system is 44, No.3, Mar.2001, p.24/9
used to measure several data simultaneously in real time ADHESIVE BONDS
and in situ. The results clearly show that there is a direct Hussain A
relationship between the ion viscosity, impedance and Comtech GmbH
strain changes during the curing process. It is found that
In order to understand the adhesion and failure phenomena
dielectric sensor is very sensitive to physical and chemical
of adhesive bonds, characterisation of the substrate
changes of the composite both in the heating and
surface, before applying adhesives, and the cure mode of
crosslinking periods. The piezoelectric proves to be a
adhesives are very important. For studying the surface
useful element during the heating period with a very
roughness in the submicron range, atomic force
sensitive and surprising behaviour during the cooling
microscopy is proving to be increasingly important.
period. The optical fibre also demonstrates a very striking
Depending upon the thickness of surface treatment and/
profile in strain variations during cooling. 14 refs.
or coupling agents, surface analytical techniques like
JAPAN
FTIR, ESCA and/or TOFSIMS are almost indispensable.
Accession no.818042 Results of contact angle measurements can be correlated
with those obtained from these techniques. Contamination
Item 84 is one of the bigger enemies in surface engineering and
ACS Polymeric Materials Science and Engineering. ESCA/TOFSIMS are proving extremely helpful in
Volume 75. Conference Proceedings. detecting and combating tile enemy. After an adhesive is
Orlando, FL., Fall 1996, p.361 applied on the substrate, it is imperative to investigate
EVOLUTION OF PROPERTIES OF A the cure/crosslinking mode of the adhesive - especially
THERMOSETTING ISOCYANATE/EPOXY/ for epoxides and PU adhesives - in an accurate way.
GLASS FIBER MODEL COMPOSITE SYSTEM MDSC, DMTA and DETA/DEA are employed very
WITH INCREASING CURE successfully as analytical tools for following the degree
DeMeuse M T; Gilham J K; Parodi F of cure. 2 refs.
EniChem America Inc.; Princeton,University; EniChem EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
SpA WESTERN EUROPE
(ACS,Div.of Polymeric Materials Science & Engng.) Accession no.815819
Studies were carried out on a methodology for monitoring
Item 86
the evolution of isothermal physical properties of
Adhasion Kleben & Dichten
thermosetting systems with increasing conversion (cure).
42, No.6, 1998, p.36-40
Measurements of modulus versus temperature of a single
German
composite specimen were obtained on repetitive cooling
FAULTY ONLINE CURING ON TRACK (PART I)
and subsequent heating to successively higher
De Wit F; Raeckers B
temperatures: cooling and subsequent heating data often
DASA
showed thermohysteresis. Plots of isothermal modulus
versus conversion (as measured in the same experiment Tests have produced the result that there is no doubt that
by glass transition) were obtained by cross-plotting for a dielectric analysis has made crosslinking procedures
broad range of temperatures (for example, from minus 180 possible with non-destructive consequences during the
degrees Celsius to 380 degrees Celsius) from both the running of a process. This method is demonstrated in a
cooling and the heating data. A measure of toughness of two-part article by using the example of the curing routine
the matrix versus conversion through the extent of for an epoxy resin prepreg.
hysteresis of the data was obtained by comparing the EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
isothermal cooling and heating data. The approach WESTERN EUROPE
depended on the use of a composite specimen and the ability Accession no.814441
Item 91 Item 93
International Journal of Adhesion & Adhesives Natural Polymers and Composites. Conference
21, No.1, 2001, p.35-40 proceedings.
STUDY OF AGEING IN ACRYLIC ADHESIVES Sao Pedro, Brazil, 14th-17th May 2000, p.367-75
Lyons E; Leahy J J; Hayes K CHARACTERISATION OF CASHEW NUT
Limerick,University SHELL LIQUID FOR COMPOSITE
MANUFACTURE
DMTA was used to investigate the effects of ageing on
Mwaikambo L; Ansell M P
the curing behaviour of air-activated acrylic adhesives.
Bath,University
The aim was to establish if the rate of cure of the adhesives
Edited by: Mattoso L H C; Leao A; Frollini E
was retarded on storage at room temp. over a period of
(EMBRAPA; UNESP; USP)
one year. Tubes of adhesives were tested at selected time
intervals and the results were examined using analysis of Differential scanning calorimetry is applied to study the
variance. It was found that, over a twelve month period, change in the glass transition temperature of the oven-
there was no ageing effect on the cure characteristics of cured resin with and without hexamethylene tetramine
air-activated adhesives. 7 refs. (HMTA) in order to monitor the extent of cure. This is a
EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND; new development in the understanding of cashew nut shell
WESTERN EUROPE liquid (CNSL) cure characteristics. The glass transition
Accession no.807266 temperature is found to rise when the alkaline catalysed
resin is subjected to higher curing temperatures regardless
of the concentration of formaldehyde used. The mode of
Item 92
cure of the NaOH-catalysed CNSL-formaldehyde resin
Composites Part A: Applied Science and
is found to be more regular with HMTA hardener. FTIR
Manufacturing
spectroscopy is used to study the neat CNSL and
31A, No.12, 2000, p.1373-81
polymerised CNSL-formaldehyde resin with and without
DEVELOPMENT OF A DIELECTRIC SYSTEM
HMTA. Analysis of the neat and polymerised CNSL
FOR THE ON-LINE CURE MONITORING OF
indicates that reduction of the phenolic hydroxyl groups
THE RESIN TRANSFER MOULDING PROCESS
and that of the side chain vinyl groups occurs as a result
McIlhagger A; Brown D; Hill B
of CNSL reaction with formaldehyde. The use of the DSC
Ulster,University
and FTIR techniques to elucidate the extent of cure of
The aerospace industry has identified the need for an CNSL resins is a valuable step towards the production of
online cure monitoring system for resin transfer moulding commercially successful CNSL-natural fibre composites.
which can determine the through-thickness cure state of 7 refs.
a composite, without affecting the integrity of the finished EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
component. Several techniques have been extensively WESTERN EUROPE
investigated but dielectric analysis (DEA) appears to offer Accession no.802305
the greatest potential. The parallel plate sensor
configuration is appropriate for through-thickness
Item 94
measurements. Using a laboratory dielectric instrument,
Smart Materials & Structures
dielectric properties in fibre (conductive and non-
9, No.6, Dec.2000, p.727-36
conductive) reinforced composite samples are measured
ASSESSMENT OF FLOW AND CURE
during a simulated RTM cure cycle. Particular parameters
MONITORING USING DIRECT CURRENT AND
derived from dielectric measurements are shown to be
ALTERNATING CURRENT SENSING IN
useful in terms of monitoring and optimising the RTM
VACUUM-ASSISTED RESIN TRANSFER
cure cycle. These parameters can be used to identify key
MOLDING
stages in the curing process and to estimate values of the
Vaidya U K; Jadkav N C; Hosur M V; Gillespie J W;
resin properties at these stages. Correlation of key
Fink B K
dielectric events with other thermal data is shown. Sensors
North Dakota State University; Tuskegee,University;
currently are being developed with a view to incorporation
Delaware,University; US,Army Research Laboratory
into the RTM mould. The ultimate aim is the development
of an on-line cure monitoring system for the RTM process The implementation of SMARTweave, a direct-current-
in collaboration with Bombardier Shorts. 43 refs. sensing-based approach, together with the traditional
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; alternating-current-based dielectric sensing, for cure
WESTERN EUROPE monitoring of S2-glass/vinyl ester and epoxy resins in
Accession no.802606 low-cost, liquid moulding vacuum-assisted resin transfer
moulding processing was performed. Through several
parametric studies, including the influence of the resin
type, single and multiple SMARTweave planes, the use
of carbon and insulated copper sensors and the stitching
versus non-stitching of the preform, it was demonstrated curing process based on the actual chemical and physical
that the SMARTweave technique of cure and resin state of the material being cured.
position/flow monitoring had definite advantages, in terms USA
of obtaining global cure information, over traditional Accession no.793612
sensing techniques. 10 refs.
USA
Accession no.800685 Item 98
SAMPE Journal
35, No.2, March/April 1999, p.39-46
Item 95 RTM EQUIPMENT AND PROCESS
West Conshohocken, PA, 2000, pp.2. NALOAN. AUTOMATION
ASTM D 3532-. TEST METHOD FOR GEL TIME Moore M F; Bland R J
OF CARBON FIBER-EPOXY PREPREG Plastech TT
American Society for Testing & Materials
ASTM D 3532- Methods of achieving improved production rates and cost
benefits in the resin transfer moulding of composites
Version 99. Photocopies and loans of this document are through selection of the most suitable preform, mould
not available from Rapra. manipulation and mould clamping are considered and
USA recent developments in the automation of the RTM
Accession no.796556 process, which are bringing about increasing levels of
production, are highlighted. These developments include
Plastech’s MegaPress range of programmable logic
Item 96
controlled pneumatic presses, Hypaject range of pressure
SAMPE Journal
pot resin injection machines, Megaject meter-mix
35, No.3, May/June 1999, p.64-72
injection machines, Autosprue inlet valve unit, Mold
USE OF PROCESS MODELS TO CONTROL AND
Pressure Guard system, catalyst flow monitoring system
OPTIMIZE PULTRUSION-TYPE PROCESSES
and resin cure monitoring system.
Voorakaranam S; Joseph B; Kardos J L
USA
Washington,University
Accession no.793611
The use of process models to control and optimise
pultrusion-type processes for reinforced plastics materials
is discussed. It is shown that on-line process models can Item 99
be developed and used to overcome the limitations Journal of Composite Materials
imposed by the lack of adequate sensors to monitor key 34, No.22, 2000, p.1926-47
processing variables such as quality and exit cure NEW METHOD TO REDUCE CURE-INDUCED
condition. An additional attraction of the model-predictive STRESSES IN THERMOSET POLYMER
control strategy is the ability it provides for operators to COMPOSITES. III. CORRELATING STRESS
view the forecasted behaviour of the process. 17 refs. HISTORY TO VISCOSITY, DEGREE OF CURE,
USA AND CURE SHRINKAGE
Accession no.795909 Madhukar M S; Genidy M S; Russell J D; Lee A Y
Tennessee,University; US,Air Force Research
Laboratory; Michigan,State University
Item 97
SAMPE Journal Details are given of the effect of different cure cycles on
35, No.2, March/April 1999, p.47-51 residual stress in epoxy resins. The percentage specific
BEYOND THE THERMOCOUPLE volume change during cure cycles was measured by a
Williamson R volumetric dilatometer. The volumetric response was
Signature Control Systems compared with dielectric data, with degree of cure
calculations, and with fibre stress data. 16 refs.
The development of a fully integrated system for Intelligent
USA
Process Control, which uses impedance sensors and
SmartCure expert system software to provide visibility and Accession no.792509
control of the curing process for materials, such as structural
composites, engineering plastics and rubber products, is Item 100
reported. The system includes installation, training, data Journal of Composite Materials
acquisition and control hardware as well as the expert 34, No.22, 2000, p.1905-25
system software and sensors and is capable of optimising NEW METHOD TO REDUCE CURE-INDUCED
cycle times and improving product uniformity. The expert STRESSES IN THERMOSET POLYMER
system software recognises a unique data signature COMPOSITES. II. CLOSED LOOP FEEDBACK
provided by the sensors and automatically controls the CONTROL SYSTEM
Emphasis is placed on fibre optic strain sensing use in the laboratory instrument with the potential for
techniques, which have been demonstrated or potentially incorporation into composite production tooling. 26 refs.
could be used for condition monitoring in AFRCs. The EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
application of fibre optic strain sensors for impact and WESTERN EUROPE
fatigue damage detection in composites is briefly Accession no.790059
discussed. The ability of multiplexing a number of sensors
in one fibre is a unique advantage of fibre optic sensors.
Item 106
Another is the ability to monitor strain distribution along
ICAC 99. Conference proceedings.
the length of the fibre. The basic concept of multiplexed
Bristol, UK, 23rd-24th Sept.1999, p.125-32
and distributed strain sensors and their applications in
COMPARISON OF DIELECTRIC AND
strain and temperature monitoring in composites is
ULTRASONIC CURE MONITORING OF
described. The cross-talk between axial strain and
ADVANCED COMPOSITES
transverse strain as well as temperature interference are
Shepard D D; Smith K R; Thibodeau L H
major issues for the application of fibre optic strain sensors
Holometrix Micromet
in AFRCs. Various approaches have been developed for
(IOM Communications Ltd.; Ulster,University;
simultaneously measuring strain and temperature.
IMechE)
Attempts have also been made to demonstrate
simultaneous measurements of three-axis strain and Dielectric measurements are widely used for the cure
temperature. 74 refs. monitoring of thermosetting resins and composites. The
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; ability to implant disposable dielectric sensors within a
WESTERN EUROPE part or install permanent dielectric sensors in a mould
Accession no.790086 wall or tool makes dielectric cure monitoring a very
versatile in-process cure monitoring technique,
Commercial dielectric cure monitoring systems,
Item 105
comprising of an electronics package, sensors, cabling
ICAC 99. Conference proceedings.
and software are available which enable routine use in
Bristol, UK, 23rd-24th Sept.1999, p.133-43
research, development and production. Measurements of
IDENTIFICATION OF KEY CURE STAGES IN
the ultrasonic sound speed of thermosetting resins and
LIQUID MOULDING PROCESSES BY
composites can also be used for in-process cure
PARALLEL PLATE DIELECTRIC ANALYSIS
monitoring. Previously, use of ultrasonic measurements
McIlhagger A T; Matthews S T; Brown D; Hill B
as a cure monitoring technique had been hindered by poor
Ulster,University
reliability of ultrasonic transducers under typical
(IOM Communications Ltd.; Ulster,University;
processing conditions, especially thermal cycling to
IMechE)
elevated temperatures. A self-contained, in-mould, robust
The aerospace industry has recognised the major benefits ultrasonic sensor is available that is capable of
associated with fibre reinforced composite materials. The withstanding hundreds of thermal cycles up to 260 deg.C.
more popular techniques available for composite This sensor technology enables ultrasonic sound speed
production are the traditional wet lay-up or autoclave and measurements to be routinely made during the processing
resin transfer moulding (RTM). Efforts to further reduce of thermosets. Commercial ultrasonic cure monitoring
processing time and improve part quality have focused systems, comprising of an electronic package, sensors,
on improved process control. To date this has been based cabling and software are also now available. 8 refs.
on off-line techniques. The need for on-line cure EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
monitoring is widely recognised and this will require the WESTERN EUROPE
development of suitable in-mould sensors. The Accession no.790058
Engineering Composites Research Centre (ECKE) has
investigated and concentrated on the specific problems
Item 107
encountered in the aerospace industry. Of the available
Plastics, Rubber and Composites
cure monitoring methods, parallel plate dielectric analysis
29, No.3, 2000, p.109-18
(DEA) appears to offer the greatest potential for
ULTRASONIC MEASUREMENTS RELATED TO
determining the through-thickness cure state of the resin
EVOLUTION OF STRUCTURE IN CURING
during cure. A laboratory dielectric instrument is utilised
EPOXY RESINS
to simulate RTM and autoclave cure cycles for composite
Challis R E; Freemantle R J; Cocker R P; Chacwick D L;
structures containing non-conductive and conductive
Dare D J; Martin C; Mahendrasingam A; Fuller W
fibres and for different resin systems used in the aerospace
Nottingham,University; Keele,University;
industry. Key resin cure stages are identified by an
Manchester,Metropolitan University
appropriate dielectric signal and correlated with data from
other thermal and mechanical techniques. Insulated The tracking of the cure of epoxy adhesives and the
parallel plate dielectric sensors are being developed for assessment of the cure state of adhesive bondlines joining
investigated. The curing kinetics of the epoxy/amine resin THERMAL, AND DYNAMIC-MECHANICAL
is analysed in both the dynamic and the isothermal modes PROPERTIES OF AN EPOXY/ANHYDRIDE
with differential scanning calorimetry. The dynamic SYSTEM
viscosity of the resin at the same temperature as in the Anton J J S; Pradas M M; Ribelles J L G
mould filling process is measured. The curing kinetics of Jaume I,Universitat; Valencia,Polytechnical University
the resin is described by a modified Kamal kinetic model,
Details are given of the curing, thermal and dynamic
for the autocatalytic and the diffusion-control effect. An
mechanical relaxation behaviour of an epoxy-anhydride
empirical model correlated Role resin viscosity with
resin and a Kevlar fibre-reinforced epoxy resin. Curing
temperature and the degree of cure is obtained. Predictions
kinetics were also studied by DSC heating scans. The
of the rate of reaction and the resulting viscosity change
effect of fibre addition on the main dynamic mechanical
by the modified Kamal model and by the empirical model
relaxation was analysed with a simple mechanical model.
agree well with the experimental data, respectively, over
47 refs.
the temperature range 50-80 deg.C and up to the degree
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;
of cure alpha = 0.4, which are suitable for the mould- WESTERN EUROPE
filling stage in the RTM process. 25 refs.
Accession no.782975
TAIWAN
Accession no.784167
Item 114
Polymer Composites
Item 112 21, No.4, Aug.2000, p.605-18
Polymer Composites POLYESTER CURE MONITORING BY MEANS
21, No.3, June 2000, p.436-49 OF DIFFERENT TECHNIQUES
SENSOR PLACEMENT STUDY FOR ONLINE Ton-That M-T; Cole K C; Jen C-K; Franca D R
FLOW MONITORING IN LIQUID COMPOSITE Canada,National Research Council
MOULDING
The cure of a set of unsaturated polyester resins having
Kueh S R M; Advani S G; Parnas R S
different styrene contents was monitored by FTIR, DSC,
Delaware,University; US,National Institute of
rheometry, and ultrasonic measurements. The dependence
Standards & Technology
of viscosity on the degree of curing was investigated at
On-line sensing can play an important part in controlling different shear rates. 25 refs.
the quality of the final product in any manufacturing CANADA
environment, including liquid composite moulding Accession no.782722
(LCM). Having a sensor embedded within the part itself
is often the most effective means of monitoring its
condition at various stages of manufacturing and even Item 115
throughout its useful life. However, given their intrusive Polymer Composites
nature, there are practical limitations imposed upon their 21, No.4, Aug.2000, p.523-30
size, quantity and trajectory within the part. The possibility FIBRE OPTIC THERMOSET CURE
of using a single lineal sensor to monitor the resin flow MONITORING SENSOR
front during the mould filling stage of LCM, and to detect Giordano M; Nicolais L; Calabro A M; Cantoni S;
the onset of void formation and the presence of dry spots Cusano A; Breglio G; Cutolo A
within the mould, is explored. Experiments are conducted CNR; Italian Aerospace Research Centre;
to characterise the response of a fibre optic system Naples,University
previously developed for cure monitoring. Simulations Details are given of the design and development of a fibre
are performed to determine the optimal placement of just optic sensor system to measure the reflection coefficient
one such sensor in a mould to demonstrate that sufficient at the interface between the fibre optic and the resin during
information on the mould filling process could be a curing process. Correlation between the sensor output
obtained. The purpose of the simulation is to learn how and conversion is proposed. Isothermal data from the
to interpret the sensor response and, subsequently, use it sensor were compared with calorimetric analysis of an
to control the LCM process. 48 refs. epoxy resin-based system. 14 refs.
USA EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
Accession no.784121 WESTERN EUROPE
Accession no.782713
Item 113
Polymer Engineering and Science Item 116
40, No.8, Aug.2000, p.1725-35 Kunststoffe Plast Europe
EFFECT OF KEVLAR FIBER 90, No.4, April 2000, p.33-5
REINFORCEMENT ON THE CURING, CROSSLINKING INSTEAD OF GLASS
TRANSITION. DETERMINATION OF DEGREE of the composite structure. Using this temp. information,
OF CURE IN FIBRE-REINFORCED the potential for localised microwave-accelerated cure to
COMPOSITE PARTS reduce the occurrence of material degradation from resin
Stark W; Doering J; Walentowski H-U over-temp. was evaluated. In addition, a theoretical model
was developed that helped to elucidate the influence of
The problem of incomplete curing during the processing
the microwave parameters on the temp. profile. 9 refs.
of fibre-reinforced composites is addressed and methods
USA
of determining the degree of cure are evaluated. The
applicability of DSC and DMTA to the analysis of the Accession no.776370
degree of cure of a vehicle component made from glass
fibre-reinforced epoxy resin and a container produced Item 119
from a glass fibre-reinforced vinyl ester resin for Composite Structures
flammable liquids and the role of the equilibrium Tg in 49, No.3, July 2000, p.331-8
complete curing are discussed. STRAIN MONITORING IN COMPOSITE
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; PATCHED STRUCTURES
WESTERN EUROPE Findik F; Mrad N; Johnston A
Accession no.779482 Sakarya,University; Canada,National Research Council
Strain monitoring was studied in a single-sided patched
Item 117 structure (as used in the aerospace industry). The thermal
International Journal of Adhesion & Adhesives residual strains were defined in graphite/epoxy resin
20, No.3, 2000, p.189-93 composites on Al-2024 T3 substrate. Five samples were
EFFECTS OF SHRINKAGE ON CONDUCTIVITY manufactured and several strain gauges were bonded on
OF ISOTROPIC CONDUCTIVE ADHESIVES the patch Al-substrate. Thermal and thermal residual
Lu D; Wong C P strains were measured after one- and two-step curing at
Georgia,Institute of Technology different temps. and the results were compared for each
step as well as with results from previous studies. 12 refs.
Details are given of changes in properties such as cure
CANADA; TURKEY
shrinkage of an isotropic conductive adhesive during cure
and of the correlation with establishment of conductivity. Accession no.774352
An epoxy resin adhesive was cured and its heat flow,
storage modulus, dimension changes, and electrical Item 120
conductivity were studied using DSC, rheological Composite Structures
measurements, thermomechanical analysis, and the use 49, No.3, July 2000, p.303-12
of an electrical multimeter. Changes in these properties PROCESS INDUCED STRESS FOR WOVEN
with time in the course of an isothermal cure were also FABRIC THICK SECTION COMPOSITE
conducted. 15 refs. STRUCTURES
USA Xiaogang Huang; Gillespie J W; Bogetti T
Accession no.777972 Delaware,University; US,Army Research Laboratory
A semi-numerical model was developed to simulate
processing-induced stress for woven fabric composite
Item 118
material structures. The approach consisted of three main
Polymer Engineering and Science
parts. The first was the simulation of resin chemical kinetic
40, No.5, May 2000, p.1157-64
cure behaviour and micromechanics for cure-dependent
SPATIAL AND TEMPORAL CONTROL OF THE
resin and glass fibre. The second was the analytical
DEGREE OF CURE IN POLYMER COMPOSITE
extension of the TEXCAD woven fabric micromechanics
STRUCTURES
model to the cure-dependent textile unit cell model. The
Shull P J; Hurley D H; Spicer J W M; Spicer J B
last was the introduction of the effective unit cell
Penn State University; Johns Hopkins University
properties to finite element structure modelling. Cure-
Current attempts to apply spatially and temporally dependent material response included thermoset resin
localised microwave processing techniques to ensure hardening and volumetric shrinkage during cure. The
uniformity of material properties in polymer composite approach was incrementally employed whereby the model
materials are described. It is shown that, in large polymer predicted the composite fabric unit cell effective modulus,
composite structures, high temps. caused by exothermic processing-induced strains and stresses (thermal
resin cure can degrade the mechanical properties of the expansion and chemical shrinkage) during cure. Case
composite. Resin cure temp. data were obtained during studies were presented which illustrated the effective
microwave processing from a series of thermocouples modulus and processing stress/strain development during
embedded at various lateral locations relative to the cure for a plain weave S2-glass/vinyl ester composite
microwave source and uniformly through the thickness laminate. An understanding of the complex relationships
between cure, modulus and processing-induced stress/ the case of process-induced strain during the cooling down
strain development represented a significant step towards stage of manufacturing. 8 refs.
optimising processing strategies for thick-section woven CANADA
fabric composite structures. 13 refs. Accession no.771718
USA
Accession no.774349 Item 123
Polymer Composites 99. Conference proceedings.
Item 121 Quebec, Canada, 6th-8th Oct.1999, p.251-63
Polymer Composites 99. Conference proceedings. ULTRASONIC MONITORING OF CURING
Quebec, Canada, 6th-8th Oct.1999, p.379-94 PROCESS OF GRAPHITE/EPOXY COMPOSITES
POLYESTER CURE MONITORING BY MEANS Mrad N; Prevost C; Johnston A; Jen C-K
OF DIFFERENT TECHNIQUES National Research Council of Canada
Ton-That M-T; Cole K C; Jen C-K; Franca D R (SPE; National Research Council of Canada)
National Research Council of Canada
Any system for automatic process monitoring and control
(SPE; National Research Council of Canada)
must possess the ability to effectively determine at any
The cure of a set of polyester resin samples having point in time the state of the process being controlled.
different styrene contents is monitored by means of Thus, in situ sensors capable of monitoring physical and
Fourier transform infrared (FTIR) spectroscopy, chemical changes are an essential component of such
differential scanning calorimetry (DSC), rheometry and systems. In this work, an in situ ultrasonic monitoring
ultrasonic measurements. FTIR and DSC experimental system is investigated for the curing process of graphite/
data are used to calculate the cure kinetics using a free- epoxy composites in a mid-sized autoclave. The non-
radical polymerisation model (multiple steps) and also intrusive and non-destructive ultrasonic monitoring
an empirical model that considers the curing to involve system enables monitoring of part temperature variation,
only a single step. The dependence of viscosity on the development of resin rich and resin poor regions due to
degree of curing is investigated at different shear rates. non-uniform compaction, point of gelation and part cure
Finally, correlations among the results from the different state. This unique system is expected to find application
techniques are established and discussed in terms of the in composites process development and systems for online
curing mechanism. 25 refs. process monitoring and control. 13 refs.
CANADA CANADA
Accession no.771724 Accession no.771714
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; process. Finally, using a plot of the variation of the shear
WESTERN EUROPE modulus of the epoxy with time during cure, approximate
Accession no.771713 formulae for estimating the residual stress caused by
shrinkage are given. 4 refs.
Item 125 EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Polymer Composites 99. Conference proceedings.
Quebec, Canada, 6th-8th Oct.1999, p.223-34 Accession no.769439
MONITORING AND HEAT TRANSFER
MODELLING OF THE CURE OF THERMOSET
Item 127
COMPOSITES PROCESSED BY RESIN
Polymer Engineering and Science
TRANSFER MOULDING
40, No.3, March 2000, p.656-64
Skordos A A; Partridge I K
NON-DESTRUCTIVE AND IN-SITU
Cranfield,University
MONITORING OF MECHANICAL PROPERTY
(SPE; National Research Council of Canada)
BUILDUP IN EPOXY ADHESIVES FOR CIVIL
Experimental studies demonstrate the existence of APPLICATIONS BY PROPAGATION OF
significant thermal gradients during the cure stage of resin ULTRASONIC WAVES
transfer moulding (RTM). The presence of such thermal Frigione M; Maffezzoli A; Acierno D; Luprano V A M;
gradients can affect the final degree-of-cure distribution Montagna G
and cause the development of residual stresses, leading Lecce,Universita; Naples,University; PASTIS-CNRSM
to deterioration of the final composite component
The progress of cure of an epoxy adhesive during
properties. Therefore the incorporation of heat transfer
polymerisation at ambient temperature was investigated
modelling in the general context of RTM modelling and
using ultrasonic wave propagation. Data were obtained
monitoring of the process is necessary. Emphasis is placed
under isothermal conditions for the neat epoxy resin and
on the application of combined monitoring and heat
a concrete-epoxy resin-concrete system. The Young’s
transfer modelling to the process. A finite element heat
modulus and shear modulus were calculated from
transfer model incorporating resin cure kinetics is
measurements of longitudinal and shear velocity. The
developed and tested. An inverse solution of the heat
results obtained indicated that the method of ultrasonic
diffusion model is implemented in order to extend the
wave propagation is suitable for analysing such slow cure
local measurements given by in situ monitoring to global
reactions. 22 refs.
information about the temperature distribution and the
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
degree-of-cure distribution during the cure. 22 refs. WESTERN EUROPE
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Accession no.768226
Accession no.771712
Item 128
Item 126 Journal of Applied Polymer Science
Epoxy Technologies for Ambient Cure Protective 75, No.11, 14th March 2000, p.1345-9
Coatings. Conference proceedings. GLASS FIBRE-REINFORCED COMPOSITES OF
Brussels, 12th-14th May 1998, paper 6 DIGLYCIDYL ETHER OF 2,7-DIHYDROXY
CURE SHRINKAGE IN EPOXY ADHESIVES NAPHTHALENE
Adams R; Hua Y U; Karachalios V F Patel K J; Amin K G; Patel R G
Bristol,University Gujarat,Sardar Patel University
(Paint Research Association)
The curing reactions of the diglycidyl ether of 2,7-
The build-up of shrinkage over time during curing and dihydroxynaphthalene (DGEDHN) with different
on cooling of an epoxy adhesive is investigated. A new aliphatic and aromatic amines were studied using DSC.
device, designed and built inhouse, is used to measure The thermal stability of the cured products was also
the shrinkage of the epoxy during cure at room and studied using thermogravimetric analysis and was found
elevated temperatures. The cure of two epoxy systems to be affected by the structure of the amine used as a curing
which consists of one part adhesive ESP110 and a two- agent. The curing of DGEDHN in the presence of a
part adhesive is successfully monitored using this device conventional epoxy resin (diglycidyl ether of bisphenol
and through the way of measurement of shrinkage change A, DGEBA) in the ratio 20:80 was also studied. Glass
with time. By careful monitoring of the shrinkage, it is fibre-reinforced composites of DGEDHN and DGEBA
shown that the cure contraction at room temperature is of (ratio 20:80) were prepared using diethyltriamine,
the order of 3.75% by volume and 1.24% expansion, triethyltetramine, p,p’-diaminodiphenylmethane and p,p’-
3.45% contraction at 60 deg.C for the two-part adhesive. diaminodiphenylsulphone as curing agents. The
It is also shown how the overall volume change caused mechanical properties of the composites were greatly
by expansion and shrinkage is distributed during the cure affected by the curing agent used. All the composites had
good electrical insulation properties. Their chemical formulations in comparison with standard 120C and 175C
resistance was also studied. 10 refs. DCDA cured systems. 7 refs.
INDIA EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
Accession no.768153
Accession no.761645
Item 129
Brookfield, Ct., 1999, pp.480. $100.00. 28cms. 5/4/00 Item 132
POLYMER COMPOSITES ’99. PROCEEDINGS Adhesion 99. Conference Proceedings.
OF A CONFERENCE HELD QUEBEC, CANADA, Cambridge, UK, 15th-17th Sept.1999, p.99-104
6TH-8TH OCT. 1999 APPLICATION OF DIELECTRIC TECHNIQUES
SPE; National Research Council of Canada TO THE CHARACTERISATION OF ADHESIVE
BONDED STRUCTURES
This international symposium focuses on polymer Pethrick R A; Affrossman S; Comrie R; Li Z C;
composites science and technology and includes keynote Armstrong G; Ivanova K; Halliday S; Hayward D;
lectures and poster sessions. Papers include inspection of Banks W M
composite materials by laser ultrasonics, stamping of Strathclyde,University
continuous fibre thermoplastic composites, (IOM Communications Ltd.)
thermorheology of in-situ organic composites, fibre optic
thermoset curing monitoring sensor, and chains The use of dielectric measurements for the non-destructive
restrictions in filler-polymer composites. characterisation of aluminium and carbon fibre-reinforced
plastics joints bonded with structural adhesives is
Accession no.766769
discussed. Applications of dielectric methods to the
detection of water absorption and the study of ageing
Item 130 processes in bonded structures are examined. 21 refs.
Adhesion 99. Conference Proceedings. EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Cambridge, UK, 15th-17th Sept.1999, p.387 WESTERN EUROPE
STRUCTURAL ADHESIVE CURE KINETICS Accession no.761630
USING DYNAMIC MECHANICAL ANALYSIS
Kavanagh G; Tod D A
DERA Item 133
(IOM Communications Ltd.) Adhesion 99. Conference Proceedings.
Cambridge, UK, 15th-17th Sept.1999, p.93-8
The use of dynamic mechanical analysis in studying the NON-DESTRUCTIVE EVALUATION AND
cure kinetics of structural adhesives is discussed. A multi- INSPECTION OF ADHESIVELY BONDED
frequency approach is used to relate small-scale properties ALUMINIUM JOINTS
to the rate dependence of the adhesive in lap shear tests. Weitzenbock J R; Niese F; Hubschen G
Cure characteristics are reported together with the Det Norske Veritas; Fraunhofer-Institut fuer
expected changes due to ageing and batch variability. (An Zerstorungsfreie Prufverfahren
abstract only is presented). (IOM Communications Ltd.)
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE A number of non-destructive testing techniques were
applied to the detection of bond line defects, including
Accession no.765329
porosity, air inclusions, incomplete cure, thickness
variations and zones of weak or no adhesion, in aluminium
Item 131 joints bonded with an epoxy resin adhesive. Test methods
Adhesion 99. Conference Proceedings. used included the thickness resonance technique, guided
Cambridge, UK, 15th-17th Sept.1999, p.187-92 ultrasonic waves, high frequency ultrasonic pulse echo
STRUCTURE/ACTIVITY CORRELATIONS IN immersion, non-linear ultrasonics and thermography. It
IMIDAZOLES FOR EPOXY CURE was shown that no single method could detect all the
Browne T J; Cawse J L defects in the specimens. The most promising methods
Hexcel Composite Materials for practical application were thickness resonance and
(IOM Communications Ltd.) guided ultrasonic waves. 10 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
A number of imidazoles were examined as potential NORWAY; SCANDINAVIA; UK; WESTERN EUROPE
alternatives to dicyandiamide (DCDA) in the curing of
Accession no.761629
epoxy resin adhesive formulations. The imidazole curing
agents were evaluated by DSC, gel time experiments in
DGEBA, molecular modelling and lap shear and peel tests Item 134
on bonded aluminium joints. Comparable lap shear values Composite Structures
but inferior peel values were observed for the trial 48, Nos.1-3, Jan.-Mar.2000, p.99-106
either specified temperature or convection. The code is different temperatures. The curing kinetics were studied
designed to be modular so the flow problem can be solved using isothermal calorimetry. The initial curing rates with
alone or coupled with the thermal problem. The problems the carbon prepregs above 140C could not obey the
are solved sequentially in a quasi-steady state fashion. Non- Arrhenius law, whereas the rates with the glass fibre
isothermal experiments with a reactive resin are conducted material did. This phenomenon was investigated using
to verify the thermal module and the resin model. A two pulsed NMR. It was concluded that during impregnation
blade stiffened panel, fitted with sensors, is manufactured of the carbon fibres, selective sorption of the components
using the RFI process. Thermocouples are used to measure of the binder by the porous fibres occurred, leading to
the temperatures, and FDEM (dielectric) sensors and component separation, which retarded the curing rate and
pressure transducers are used to monitor the flow front the degree of curing. 17 refs. Translation of Plasticheskie
progression. Model predictions and experimental results Massy, No.7, 1998, p.14.
are found to be in close agreement for the temperatures RUSSIA
and flow progression. The predicted and measured Accession no.756156
infiltration times match to within 12%, and the temperatures
to within 5%. 7 refs.
Item 140
USA
Journal of Materials Science. Materials in Medicine
Accession no.760235 10, No.4, April 1999, p.205-13
FORMATION OF HYDROXYAPATITE-
Item 138 CALCIUM POLYACRYLATE COMPOSITES
International Composites Expo 99. Conference Watson K E; Tenhuisen K S; Brown P W
proceedings. Penn State University
Cincinnati, Oh., 10th-12th May 1999, session 22-D
Factor influencing the workability (working time) and
STRUCTURAL INTEGRITY MONITORING
properties of dental cements prepared from tetracalcium
USING SMART MAGNETOSTRICTIVE
phosphate and polyacrylic acid were investigated.
COMPOSITES
Prehydrating the tetracalcium phosphate to form surface
Trovillion J; Kamphaus J; Quattrone R; Berman J
layers of hydroxyapatite on the tetracalcium phosphate
US,Army Construction Engineering Research Lab.
particles improved workability. The effects of the
(SPI,Composites Institute)
proportions of tetracalcium phosphate and polyacrylic
15 wt% of a commercial magnetostrictive alloy powder acid, with and without hydroxyapatite as filler were
was added to polyester resin, and glass fibre-reinforced examined. Extents of reactions were studied by X-ray
polyester resin, at the mixing stage. Following curing, diffraction analysis. Microstructures were examined by
the composites were loaded in uniaxial tension. The SEM. Neutralisation was studied by FTIR. Pore structures
magnetic flux density, measured using Hall effect devices, were determined by mercury intrusion porosimetry.
increased with increasing axial load, and exposing the Compressive strengths were determined. Strength and
samples to a magnetic field prior to testing increased the porosity depended on liquid/solid ratio. Hydroxyapatite
response by aligning the magnetic dipoles. The composite filler reduced compressive strength. 24 refs.
could also be magnetically annealed under load, re-setting USA
the magnetic characteristics of the structure. It was Accession no.754789
concluded that magnetostrictive composites were suited
as self-monitoring structural materials, as only modest
magnet generation and detection equipment was needed. Item 141
9 refs. Adhasion Kleben & Dichten
USA
41, Nos.7-8, 1997, p.31/5
German
Accession no.759527
HIDDEN GLASS TRANSITIONS MADE VISIBLE
Haessler R
Item 139 Dresden,Institut fuer Polymerforschung
International Polymer Science and Technology
Modulated dynamic differential calorimetry (MDDC)
26, No.3, 1999, p.34-7
makes it possible to record weak transitions and to
EFFECT OF GLASS AND CARBON FABRIC
separate complex transitions through simultaneous
FILLERS ON THE CURING OF AN EPOXY-
measurement of heat capacity and heat flow in only one
PHENOL BINDER
experiment. Here the advantages of this modified method
Smirnov Yu N; Tarasov V P; Dzhamaeva N M
of measurement are examined within the context of
Russian Academy of Sciences; Dagestan,State
manufacturing, processing and testing adhesives.
Pedagogical University
Temperature reactions are analysed during MDDC
Prepregs of carbon and glass fibre were impregnated with measurements as well as glass transition temperatures
an epoxy-novolac binder and cured under pressure at alongside enthalpic relaxation, melting and aftercuring.
MDDC graphs are produced for epoxide resin adhesives, Item 144
which are partially cured, hardened at room temperature Journal of Reinforced Plastics & Composites
during thermal crosslinking and hot cured during thermal 18, No.11, 1999, p.979-84
aftercuring. 6 refs. IN SITU MONITORING OF THE CURE
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY; PROCESS OF FIBERGLASS/POLYESTER
WESTERN EUROPE COMPOSITES
Accession no.754462 Cameron J; Yongping Zhang
Kingston,Queen’s University; Bell Helicopter Textron
Canada
Item 142
Polymer Composites A theoretical relationship between the extent of cure and
20, No.4, Aug.1999, p.581-93 the temp. obtained in thermoset polyester resins was
USE OF A SIMPLE, INEXPENSIVE PRESSURE derived. The curing behaviour of resins in the presence
SENSOR TO MEASURE HYDROSTATIC RESIN of reinforcing phases was also investigated using a
PRESSURE DURING PROCESSING OF computer-assisted thermal analysis system. The
COMPOSITE LAMINATES relationship found between the cure time and temp.
Lynch K; Hubert P; Poursartip A readings on the specimens could be used to assess the
British Columbia,University extent of cure. 5 refs.
CANADA
Inexpensive, reusable pressure sensors were developed to
monitor the hydrostatic resin pressure inside a curing Accession no.749040
composite laminate. The tube sensor assemblies were non-
hysteretic, absolute devices that produced reproducible, Item 145
linear results that were stable with time and temp. If a sensor Journal of Applied Polymer Science
tube became sealed, it would no longer measure pressure, 73, No.10, 6th Sept.1999, p.1969-77
but would be primarily sensitive to temp. changes. The CURE MONITORING OF EPOXY MATRICES
sensors were tested in two flat laminates under bleed FOR COMPOSITES BY ULTRASONIC WAVE
conditions. The resin pressure within a laminate increased PROPAGATION
with the applied pressure until flow began, at which time Maffezzoli A; Quarta E; Luprano V A M; Montagna G;
the resin pressure decreased progressively through the Nicolais L
laminate thickness, from the top surface to the toolplate. A Lecce,Universita; PASTIS-CNRSM; Napoli,Universita
resin pressure gradient existed across the entire laminate Federico II
thickness until full compaction occurred or the applied
pressure was released. The flow module implemented in a A complete characterisation of the cure of a model epoxy
finite element processing model, with appropriate material matrix for composites was carried out by comparing
parameters and boundary conditions, could produce a isothermal and non-isothermal data. The propagation of
reasonable estimate of the resin pressure throughout a ultrasonic waves acting as a dynamic mechanical
laminate during cure and of the final laminate fibre volume deformation at high frequencies was used to calculate
fraction. 18 refs. complex longitudinal bulk moduli during the curing
process. The evolution of attenuation and velocity during
CANADA
the reaction was related to the strong physical changes
Accession no.750343 occurring during the curing process. A comparison
between the degree of reaction measured by DSC and the
Item 143 ultrasonic results was presented. The ultrasonic velocity
Reinforced Plastics (or the bulk longitudinal modulus) was regarded as the
43, No.10, Oct.1999, p.23 most interesting parameter for cure monitoring because
SMC CURE MONITOR it followed the development of the mechanical properties
of the epoxy resin during cure. The results indicated that
The ICAM-1500 Cure Analyzer is designed to monitor
the measurement of the longitudinal velocity could be
the curing of thermosetting resin systems such as SMC,
used for on-line measurement of post-gel properties. A
BMC and UV light curing materials, it is briefly reported.
correlation was proposed between the gel time and the
The system measures changes in dielectric properties to
end of cure and ultrasonic data. 40 refs.
monitor changes in viscosity, cure rate and cure time of
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;
thermosetting resin systems. WESTERN EUROPE
HOLOMETRIX Accession no.747639
USA
Accession no.749254
the resin transfer moulding (RTM) infiltration and cure Details are given of a method for monitoring the real-
process. A science based multi-dimensional model of time curing dynamics of composite monomers, exploiting
RTM is developed which can successfully predict the site specific information provided by high resolution
infiltration behaviour, as well as viscosity and degree of NMR. Data using polyvinylpyrrolidone,
cure as the resin flows in and cures in a dry textile preform. polyhydroxyethyl methacrylate and
Mould filling experiments are conducted at NASA polybutylhydroxycyclohexyl methacrylate are compared
Langley with a reactive epoxy resin and carbon fabric with results from a computer simulation based on a
preforms. Good agreement between model predicted and multicomponent kinetic model. 7 refs.
sensor measured infiltration patterns, viscosity and degree EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;
of cure throughout the infiltration and cure process is WESTERN EUROPE
observed. Use of the sensor model system for closed-loop Accession no.716161
automated intelligent control is also discussed. 5 refs.
USA
Item 158
Accession no.724998 Materiaux & Techniques
Dec.Special, 1998, p.29-32
Item 156 MONITORING THE CYCLE OF LIFE OF
ACS Polymeric Materials Science & Engineering, POLYMER BASED COMPOSITE BY AN
Spring Meeting 1998. Volume 78. Conference EMBEDDED PIEZOELECTRIC ELEMENT
proceedings. Jayet Y; Baboux J C
Dallas, Tx., Spring 1998, p.232. 012 INSA
EVALUATION OF THE CURING PROCESS IN A
An original method was developed to monitor the
REINFORCED EPOXY BY DYNAMIC DSC AND
viscoelastic properties of a composite through
DMA
measurements of the piezoelectric impedance of a
Bilyeu B W; Brostow W K; Menard K P
piezoelectric ceramic inserted in the composite structure.
North Texas,University
This method is a good indicator to follow the different
(ACS,Div.of Polymeric Materials Science & Engng.)
curing phases of the polymerisation process; it is able to
Optimisation of industrial processing of fibre reinforced detect the modifications of the mechanical properties
epoxy prepregs requires knowledge of the relationship induced by water immersion of the structure. The results
between time and temperature, and how the two affect were validated by other classical ultrasonic measurements
the curing reaction. This is usually presented by means and by rheological tests. 12 refs.
of a time-temperature-transformation (TTT) diagram. EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Construction of a TTT diagram requires determination WESTERN EUROPE
of the rate of chemical conversion as a function of time Accession no.715968
and temperature, including vitrification, where the rate
changes from kinetic to diffusion controlled. Also, for
Item 159
industrial processing the gel point curve is very important,
Plastiques Modernes et Elastomeres
since viscosity is very important in both preprocessing
50, No.3, April 1998, p.22-5
and processing, especially concerning workability and
French
adhesion between parts. Chemical conversion (exothermic
SIMULATION OF MOULD FILLING IN RTM
heat or Tg shift), as well as vitrification is being studied
El Hadj M; Burg S
by dynamic DSC (DDSC). Gelation, which cannot be
Rheo Technology Consulting
detected by calorimetry, is studied by the tangent Delta
signal in DMA in parallel plate mode. This abstract The application of the C-MOLD Reactive Molding
includes all the information contained in the original software to the simulation of mould filling in the resin
article. transfer moulding of composites is described.
USA EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
WESTERN EUROPE
Accession no.718749
Accession no.715835
Item 157
Macromolecular Rapid Communications Item 160
20, No.2, Feb. 1999, p.95-7 Journal of Materials Science.Materials in Medicine
CURING OF MONOMER COMPOSITES. II. USE 9, No.12, Dec.1998, p.835-8
OF NMR TO MONITOR REAL TIME CURING COMPARISON BETWEEN THE
DYNAMICS POLYMERISATION BEHAVIOUR OF A NEW
Martin S J; McBrierty V J; Dowling J; Douglass D C BONE CEMENT AND A COMMERCIAL ONE:
Dublin,Trinity College; Bausch & Lomb Inc. MODELLING AND IN-VITRO ANALYSIS
Borzacchiello A; Ambrosio L; Nicolais L; Harper E J; The curing of an unsaturated polyester DMC is followed
Tanner K E; Bonfield W during a commercial compression moulding operation
Naples,University; Queen Mary & Westfield College using a novel ultrasonic measurement technique.
Measurements are carried out using an instrumented three-
Polymerisation behaviour of a new bone cement based
component compression moulding tool enabling the
on poly(ethylmethacrylate), hydroxyapatite powder and
production of 192 mm diameter DMC discs of varying
n-butylmethacrylate monomer and a commercial cement
thickness. The measurement technique uses standard 2.25
was studied. Polymerisation kinetics were analysed by
MHz wide bandwidth NDT ultrasonic flaw detection
DSC; DSC data were used to evaluate a phenomenological
probes combined with a narrow band pass filter. The filter
model describing the cure kinetics of this new bone
is used to remove errors due to preferential absorption of
cement. The kinetic model coupled with the energy
the high frequency components of the ultrasonic pulse
balance was then used to obtain temperature and degree
during cure. Changes in the velocity and attenuation of
of conversion profiles in the bone-cement-prosthesis
the transmitted ultrasonic pulse are monitored throughout
system, under non-isothermal conditions, as a function
cure using a custom-made computer controlled ultrasonic
of initial temperature and thickness of the cement.
analyser. The effect of temperature and part thickness on
Material properties, boundary and initial conditions and
the rate of cure during moulding is investigated. The
the kinetic behaviour were the input data for the
potential of ultrasonic cure measurements for use as a
numerically solved heat transfer model. The modelling
process control aid is also assessed. It is concluded that
results were compared with in-vitro results. 11 refs.
ultrasonic measurements are ideal for following the cure
EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; UK;
WESTERN EUROPE
during processing. Further developed this ultrasonic
measurement technique could be used as a feedback
Accession no.711129
control for thermoset processing equipment. 4 refs.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Item 161 WESTERN EUROPE
High Performance Polymers Accession no.709062
10, No.4, Dec.1998, p.331-40
DMTA STUDIES OF THE EFFECT OF STORAGE Item 163
TIME ON THE CURING PROCESS OF SHEET Structural Adhesives in Engineering V. Conference
MOULDING COMPOUND(SMC) proceedings.
Hamdan S; Hashim D M A; Fong S W Bristol, 1st-3rd April 1998, p.237-42. 6A1
Malaysia,University AN IMPROVED DILATOMETER FOR THE
DMTA was used to study the effect of storage time on MEASUREMENT OF ADHESIVE SHRINKAGE
the curing process of SMC (unsaturated polyester/glass Yu H; Adams R D
fibre). Emphasis was placed on following the curing by Bristol,University
the study of storage modulus and loss tangent with storage (Institute of Materials)
time. Changes in the storage time showed an increase in The volume cure shrinkage of three epoxy resins, used as
the storage modulus during a room-temp. cure. The loss adhesives, is investigated using two different
tangent damping peak occurred as the system was driven measurements. An in-house designed and built dilatometer
into the glassy state by the crosslinking reaction. The SMC is used for measuring adhesives shrinkage with time at
displayed a room temp. storage modulus of 8.5 Pa which different cure temperatures. By careful monitoring of the
increased to about 9 Pa in the subsequent scan in the shrinkage, the volume change of three adhesives,
DMTA. 5 refs. including thermal expansion, polymerisation shrinkage,
MALAYSIA and cooling contraction, is measured automatically and
Accession no.711010 continuously by this new device during the curing and
cooling processes. The shrinkage of two-part adhesive
measured by new device is compared with the shrinkage
Item 162 found from the linear method and density measurement.
Designed for Life: Composites 94. Publication It is also shown how the overall volume change caused
No.293/8. Conference proceedings. by expansion and shrinkage is distributed during the cure
Birmingham, 22nd-23rd Nov.1994, p.7-16. 627 process. The effect of temperature on shrinkage is
ULTRASONIC CURE MEASUREMENTS investigated. Varying the cure temperature produces
DURING THE PROCESSING OF AN changes of cure behaviour, which result in different
UNSATURATED POLYESTER DOUGH shrinkage. The results obtained may be used to calculate
MOULDING COMPOUND the complete stress state of adhesive in the joints. 12 refs.
Gibbs P A J EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
UK,National Physical Laboratory WESTERN EUROPE
(BPF) Accession no.705809
ANALYSIS. II. ON-LINE REAL-TIME achieve cure control. A general high-level controller is
DIELECTRIC MEASUREMENTS DURING A under development to optimise the process under a wide
COMPRESSION MOLDING PROCESS range of operating conditions. 10 refs.
Stephan F; Duteurtre X; Fit A USA
Renault; Auxiribat Accession no.698316
The curing of a glass fibre-epoxy composite based on the
diglycidyl ether of bisphenol A with dicyandiamide as
Item 169
the curing agent and imidazole as the catalyst was
Enercomp 95 International Conference on Composite
analysed using microdielectrometry. The curing behaviour
Materials and Energy. Conference proceedings.
of thick epoxy resin composite parts was examined in a
Montreal, Canada, 8th-10th May 1995, p.11-8. 627-
production environment for the compression moulding
63Ene
process. Particular attention was paid to the method used
MONITORING THE HYDROLYTIC
to collect one-line real-time conversion measurements
DEGRADATION OF POLYESTER-BASED
during an epoxy/glass fibre composite cure. For this
COMPOSITES BY A PIEZOELECTRIC
purpose, temp. and ionic conductivity profiles during
METHOD
industrial moulding of a thick epoxy resin part were
Saint-Pierre N; Perrissin I; Jayet Y; Tatibouet J
recorded. Corresponding conversion profiles were
Lyon,Institut National des Sciences Appliquees
deduced from a previous empirically-established
(Canadian Association for Composite Structures &
correlation and discussed in terms of cure gradients as a
Materials)
function of the through-the-thickness location and of the
cure cycle time. 13 refs. Theoretical considerations show that the electric
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; impedance of a piezoelectric element depends on the
WESTERN EUROPE physical and geometrical properties of the element and
Accession no.699103 also on the viscoelastic characteristics of the different
media surrounding it. According to a dynamic model, an
original technique is developed by inserting a
Item 168
piezoelectric ceramic in the composite structure when
Enercomp 95 International Conference on Composite
processed. The electric signal, after signal processing and
Materials and Energy. Conference proceedings.
numerical treatments, gives access to the viscoelastic
Montreal, Canada, 8th-10th May 1995, p.334-41. 627-
properties of the external medium. This method is an
63Ene
excellent indicator to display the polymerisation kinetics
THE USE OF EVANESCENT WAVE
of the resin as well as the post-curing phase of the
FLUORESCENCE SPECTROSCOPY IN
composite structure process. Moreover, a further
PROCESS CONTROL OF THE LIQUID
application of this non-destructive method is the
MOULDING PROCESS
monitoring of the hydrolytic degradation of the composite
Parnas R S; Woerdeman D L
structure. The evolution of the electric impedance of the
US,National Institute of Standards & Technology;
piezoelectric sensor is presented as a function of water
Johns Hopkins University
exposition time for a polyester-based composite. 4 refs.
(Canadian Association for Composite Structures &
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Materials) WESTERN EUROPE
Fluorescence has been demonstrated to be an accurate Accession no.698277
measurement of resin cure and has been used in liquid
moulding as distal-end fibre optic sensors. Evanescent
Item 170
wave fibre optic sensors offer the additional advantage
Materials Challenge - Diversification and the Future.
of sensing the cure deep within the preform and very close
Volume 40: Book 1. Symposium proceedings.
to the fibre surface. An economical optical fibre sensor is
Anaheim, Ca., 8th-11th May 1995, p.696-710. 627
developed with a refractive index in excess of 1.6,
CONSIDERATIONS IN THE DIELECTRIC
permitting evanescent wave monitoring of most typical
ANALYSIS OF COMPOSITES
liquid moulding resins. A hierarchical control strategy is
Buczek M B; Lee C W
developed for liquid moulding processes that use the cure
GE Aircraft Engines; Dayton,University
measurement provided by the evanescent wave
(SAMPE)
fluorescence sensor. Single input/single output control
loops are implemented at the base level to regulate the Dielectric analysis has become a popular method for
mould temperature, the vacuum pressure in the mould monitoring the resin state in composites during cure for
either the inlet flow or pressure during injection, and the control purposes. To effectively use this technique it is
final mould pressure. A model-based feedback controller important to understand the electrical measurements that
is implemented to control the chemical cure and are made as well as their relationship to a material’s
manipulates the setpoint of the temperature controller to rheological properties. A description of the theoretical basis
and assumptions from which the dielectric parameters are in polymers and composites is described. The first
obtained is provided. Experimental data obtained from three approach discussed is the route of the extrinsic reactive
dielectric measurement systems with three different types fluorophoric sensors, added in small amounts either to
of sensors are presented and compared. Comparisons are mimic the curing agent or the monomer. The second
based on measurements on epoxy and polyimide (PMR- approach to be described is the exploration of intrinsic
15) composites, as well as simple RC circuits. Comparisons fluorescence and UV signals for cure characterisation of
of dielectric data and Rheometrics Dynamic Spectrometer polymers and composites such as diamine cured epoxy,
data are also presented. The results show that the polyimide, PU, PMMA and PS. For in situ characterisation
measurements of RC-circuit responses made by these three during actual processing, the development of optic fibre
dielectric systems are identical; sensor response, which is fluorescence or UV reflection attachments is described.
influenced by temperature, can confound the test material 12 refs.
response; and different types of sensors have different USA
temperature characteristics. The information presented may Accession no.698104
serve as a guide to making dielectric equipment choices
and interpreting dielectric measurements on new composite
materials. 16 refs. Item 173
USA Materials Challenge - Diversification and the Future.
Accession no.698161 Volume 40: Book 1. Symposium proceedings.
Anaheim, Ca., 8th-11th May 1995, p.42-50. 627
OPTICAL FIBRE EXTRINSIC FABRY-PEROT
Item 171 INTERFEROMERIC SENSOR FOR POLYMER
Materials Challenge - Diversification and the Future. MATRIX COMPOSITE EVALUATION
Volume 40: Book 1. Symposium proceedings. Bhatia V; Sen M B; May R G; Murphy K A; Claus R O;
Anaheim, Ca., 8th-11th May 1995, p.645-53. 627 Greene J A; Tran T A
REAL TIME PROCESS MONITORING FOR Virginia,Polytechnic Institute & State University; Fiber
CURE OF COMPOSITES USING & Sensor Technologies Inc.
DIELECTROMETRY (SAMPE)
Corley T J
Westinghouse Power Generation BU Recent progress in the development of extrinsic Fabry-
(SAMPE) Perot interferometric (EFPI) sensors is reported. Novel
techniques for polymer composite cure monitoring and
Generator stator coil groundwall insulation systems are subsequent non-destructive evaluation are described.
composites of either A- or B-stage materials with fillers Polymer adhesives are evaluated for the construction of
such as glass and mica tapes. These materials, when the EFPI sensor. New construction techniques result in a
appropriately formulated and processed, give the sensor that can survive over 10,000,000 cycles under
groundwall its unique properties. These properties include fatigue loading when attached to or embedded within
long-term dielectric strength, low electrical loss, high polymer matrix composites (PMC). Fibre sensors have
insulation resistance, excellent thermoelectric endurance found numerous industrial, military and civil applications
as well as mechanical and thermomechanical properties. in the last decade. These sensors are small in size and
Dielectrometry is presented as a means of continuous highly sensitive, are immune to electromagnetic
monitoring of the cure of high voltage stator coil interference and can easily be modified for distributed or
groundwall insulation and hence the composite system multi-parameter measurement. The EFPI sensor possesses
in real time. 4 refs. all these advantages but still has a few limitations which
USA have prevented its large-scale commercialisation as an
Accession no.698155 effective, multi-purpose sensor. These limitations are
discussed and the development of techniques which have
allowed these shortcomings to be surmounted, in terms
Item 172
of both sensor fabrication and sensor operation, are
Materials Challenge - Diversification and the Future.
reported. 4 refs.
Volume 40: Book 1. Symposium proceedings.
USA
Anaheim, Ca., 8th-11th May 1995, p.51-8. 627
UV AND FLUORESCENCE TECHNIQUES FOR Accession no.698103
CHARACTERISATION OF CURE PROCESSES
IN POLYMERS AND COMPOSITES
Item 174
Sung C S P; Sung N H
Materials Challenge - Diversification and the Future.
Connecticut,University; Tufts University
Volume 40: Book 2. Symposium proceedings.
(SAMPE)
Anaheim, Ca., 8th-11th May 1995, p.1466-77. 627
Research on the development and application of sensitive IN SITU FDEMS SENSING FOR INTELLIGENT
optical techniques for characterisation of cure processes AUTOMATED CURE IN RESIN TRANSFER
techniques, and suggest that the cure may be divided into are described. The use of a finite difference simulation to
distinct phases. It is suggested that an initial liquid stage predict the curing of the composites based on
where short polymer chains are formed is followed by a experimentally-determined physical and chemical
second stage where longer molecules develop. The later parameters is discussed. The modifications required for
stages of cure are characterised by the solidification of the the kinetic models within the simulation accurately to
adhesive and the development of the final crosslinked predict cure behaviour at the temps. required for thick-
network. The results obtained are consistent with sectioned parts are considered. The improved version of
established reaction mechanisms and cure times predicted the simulation is compared with experimental results and
by mechanical and other techniques. 7 refs. the dramatic effect of the presence of fibres on the kinetic
EUROPEAN COMMUNITY; EUROPEAN UNION; UK; behaviour of the resin is demonstrated. 21 refs.
WESTERN EUROPE USA
Accession no.694778 Accession no.691384
atmosphere and temp. were compared. The mechanical distributions are quantified for two specific resin types.
resistances of the metallic substrate/adhesive pairs were The reduction in interlaminar shear strength, resulting
evaluated by performing a mechanical test, the three-point from the presence of the embedded dielectric sensors, was
flexure test. The surface properties (adherence) were then shown to be 15% for a brittle resin system and 5% for a
characterised. Finally, the influence of curing kinetics on tough resin system. 14 refs.
mass (cohesion) was examined. It was found that metallic EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
catalysis by transition metals clearly increased the curing WESTERN EUROPE
kinetics and, in some cases, its effect on reactivity was Accession no.682765
more significant than the anaerobic or temp. parameters.
It appeared that the three parameters, when studied
Item 191
simultaneously, had a synergistic effect which did not
Materials World
necessarily give appropriate mechanical properties, as
6, No.6, June 1998, p.340-2
shown by the mechanical test results. 16 refs.
MAKING LIGHT WORK OF MATERIALS
LOCTITE CORP. SENSORS
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;
Fernando G
WESTERN EUROPE
Cranfield,University
Accession no.684537
The use of optical fibre-based sensor systems for cost-
effective solutions for in-situ process and health
Item 189
monitoring of composite materials and engineering
Applied Spectroscopy
materials and structures, is discussed. Advantages of
52, No.4, April 1998, p.552-6
optical fibres in sensing applications are examined,
FOURIER TRANSFORM NEAR-IR
together with details of mechanisms by which they
MONITORING OF REACTING RESINS USING
operate, namely: internal selection, evanescence and
AN EVANESCENT WAVE HIGH-INDEX FIBRE-
interference. Details are given of three main approaches
OPTIC SENSOR
to monitoring fibre reinforced composites: embedding
Dunkers J P; Flynn K M; Huang M T; McDonough W G
optical fibres into the composite, the use of an optical
US,National Institute of Standards & Technology
fibre-based sensor system such as the fibre Bragg grating
A high-index silica-based fibre-optic mini-bundle sensor or extrinsic Fabry-Perot interferometric sensor, and a third
was constructed and implemented with a Fourier optical fibre-based sensing system which converts
transform near-IR spectrometer. Reactions of a reinforcing fibres into light guides.
polyisocyanurate and an epoxy resin were monitored and EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
peak assignments were made and discussed with respect WESTERN EUROPE
to their potential for use in real-time analysis. Cure Accession no.681259
monitoring was also demonstrated in a resin transfer
moulded glass fibre-reinforced epoxy resin part. 24 refs.
Item 192
USA
Materials World
Accession no.682964 6, No.6, June 1998, p.337-8
ON-LINE NDE AND MONITORING OF
COMPOSITES MANUFACTURING
Item 190
Steiner K
Composites Part B: Engineering
Delaware,University
29B, No.3, 1998, p.245-50
MONITORING AUTOCLAVE CURE IN Research work carried out at the Centre for Composite
COMMERCIAL CARBON FIBRE/EPOXY Materials at the University of Delaware, is described, with
COMPOSITES reference to non-destructive sensing and monitoring
Maistros G M; Partridge I K techniques used in composite manufacturing. Such
Cranfield,University techniques are claimed will enable composites to be used
in broader areas of applications, and to reduce costs, while
Embedded dielectric sensors and thermocouples were
improving quality and manufacturability.
used to monitor the state of cure, in real time, for a range
of current commercial epoxy resin/carbon fibre-reinforced USA
composites. The methodology and data analyses involved Accession no.681258
in the monitoring procedure are summarised and specific
examples of the results obtained are given. The generic Item 193
rules governing the relationships between dielectric Smart Materials & Structures
properties and material transformations for epoxy-based 7, No.2, April 1998, p.145-58
resins are stated. The problem of reaction exotherms in IN SITU PROCESS AND CONDITION
thick sections and the resulting uneven temp. and property MONITORING OF ADVANCED FIBRE-
composite. A mini-bundle of high index optical fibres is The inherent effect of dramatically increasing stiffness and
placed in the centre of the reinforcement thickness. Spectra strength with elevated temperature post-curing is also
are collected using evanescent wave Fourier transform near detected. This implies that thermal conductivity may be a
infrared spectroscopy as the composite is curing. Peaks valuable parameter for assessing the amount of
representing amine consumption are identified as good crosslinking, as long as the changes are within the resolution
candidates for real-time monitoring and control of the epoxy limits of the measuring equipment. 16 refs.
cure. A cure control algorithm based on model assisted CANADA
feedback control is presented. 11 refs. Accession no.637312
USA
Accession no.638411 Item 210
Rubber World
Item 208 216, No.1, April 1997, p.45
Antec 97. Volume I. Conference proceedings. CURE MONITORING
Toronto, 27th April-2nd May 1997, p.774-81. 012
The capabilities are briefly outlined of dielectric and
ANALYSIS OF CURE BEHAVIOUR OF SMC
ultrasonic cure monitoring instrumentation, software and
DURING COMPRESSION MOULDING
sensors from Micromet Instruments for composite cure
Hamada H; Futamata K; Naito H
characterisation. The instrumentation is designed for use
Kyoto,Institute of Technology; Sekisui Chemical
in research and process development, quality control, and
Co.Ltd.
production control.
(SPE)
MICROMET INSTRUMENTS INC.
The cure behaviour of SMC during compression moulding USA
is rather complicated due to heat generation in cure process Accession no.636861
and heterogeneous material properties. Differential
scanning calorimetry may be an effective and powerful
method for measuring cure behaviour of various materials Item 211
but not useful for practical products, because the Polymer Composites
dimensions of DSC specimens are much smaller than that 18, No.1, Feb.1997, p.133-50
of practical products. A numerical analysis method for CURE MONITORING OF THE LIQUID
measuring the cure behaviour of SMC is described. COMPOSITE MOULDING PROCESS USING
Combining temperature measurement of SMC and three- FIBRE OPTIC SENSORS
dimensional thermal conductivity analysis, taking into Woerdeman D L; Spoerre J K; Flynn K M; Parnas R S
account heat generation due to chemical diffusion, the heat Johns Hopkins University; Southern Illinois,University;
generation is determined by both data and consequently is US,National Inst.of Standards & Technology
defined as a function of temperature of SMC. The obtained Cure monitoring during liquid composite moulding of
heat generation function is again used in thermal unidirectional glass fabric/epoxy resin composites was
conductivity analysis. It is thus possible to obtain heat carried out by evanescent wave fluorescence measurement
generation curves and curing profiles. 7 refs. using a fibre optic sensor embedded in the fibre preform.
JAPAN The fluorescence wavelength shift during cure was
Accession no.637316 correlated with monomer conversion as determined by
IR spectroscopy. Glass fabrics with 40-60% volume
fractions were injected with resin at a variety of driving
Item 209
pressures and cured at several temperatures. Several
Antec 97. Volume I. Conference proceedings.
composite parts were fabricated to test the effects of
Toronto, 27th April-2nd May 1997, p.747-51. 012
vacuum pressure, injection rate, curing temperature and
RESIN CURE MONITORING USING THERMAL
fibre fraction on the performance of the sensor, and the
CONDUCTIVITY MEASUREMENTS
sensitivity of the sensor to the condition of the resin
Mathis N; Pytel J; Lee-Sullivan P
system was also examined. 45 refs.
Mathis Instruments Ltd.; New Brunswick,University
USA
(SPE)
Accession no.632375
The use of thermal conductivity measurements as a non-
destructive technique for monitoring the extent of curing
in a room temperature curing epoxy resin is investigated. Item 212
Three-point bending tests are performed immediately after Polymer Engineering and Science
thermal conductivity measurements to evaluate the degree 37, No.2, Feb.1997, p.436-49
of cure or crosslinking. The thermal conductivity values IN-PROCESS CONTROL OF EPOXY COMPOSITE
closely follow the increase and subsequent levelling off in BY MICRODIELECTROMETRIC ANALYSIS
flexural modulus and strength as vitrification progresses. Stephan F; Fit A; Duteurtre X
systematic FTIR spectroscopy and DSC for 1-14h PROCESS DEFINITION WITH COGNITIVE
isothermal exposures in the 130-300C range. The reaction COMPUTER
mechanisms were discussed with reference to their effects Price H L
on the glass transition temperature and mechanical Wilkes University
properties of the composite matrices. 20 refs. (SPI,Composites Institute)
USA
Processing instrument technology is reported to enable a
Accession no.623493 computer to sense and interpret changes taking place
during the cure of prepreg or moulding compound. P/I
Item 222 technology has been used to make estimates of gel time
Journal of Composite Materials and cure time, thermal diffusivity measurements and
31, No.1, 1997, p.87-102 transition temperature measurements. Control and sensing
FIBER OPTIC SENSOR DEVELOPMENT FOR software is comparatively straightforward. The
REAL-TIME IN-SITU EPOXY CURE interpretation of results with appropriate software is under
MONITORING development. 5 refs.
Liu Y M; Ganesh C; Steele J P H; Jones J E USA
Colorado,School of Mines Accession no.621961
A fibre optic sensor system based on the principle of Fresnel
reflection, for monitoring the cure process in composite Item 225
manufacturing, is described. The main advantage of the Journal of Advanced Materials
sensor is that it is of low cost and can be embedded in the 28, No. 1, Oct.1996, p.42-47
material to provide in-situ, real-time information on degree PHOTO DYNAMIC MECHANICAL ANALYSIS
of cure. The experimental work is discussed with reference FOR CURE MONITORING OF FIBER
to the experimental set-up, DSC calibration, sensor REINFORCED PHOTORESIN COMPOSITES
response for dynamic cure, sensor response for isothermal Renault T; Ogale A A
cure and sensor calibration. 17 refs. Clemson,University
USA
The use of photo dynamic mechanical analysis (photo
Accession no.622482 DMA) for cure monitoring of fibre reinforced photoresin
composites is discussed and compared with existing
Item 223 techniques for such measurements. The influence of glass,
Journal of Composite Materials quartz, and carbon fibres on the photocure of polyacrylate
31, No.1, 1997, p.22-51 resins was determined by the photo DMA technique. Glass
INTELLIGENT CURING OF THICK and quartz fibres were found to have no detectable effect
COMPOSITES USING A KNOWLEDGE-BASED on the cure kinetics of photoresins, but carbon fibres were
SYSTEM found to inhibit the cure significantly. A static and
Pillai V; Beris A N; Dhurjati P dynamic FEA were used to calculate the modulus of the
Delaware,University cured composite from the results. 24 refs.
USA
The model-based optimisation of and the optimal
Accession no.620020
operation of the autoclave curing of thick fibre-reinforced
thermosetting matrix composites were investigated. A
flexible heuristic optimisation method coupled with a Item 226
good simulation of the process was used to determine Kunststoffe Plast Europe
how the process should proceed, given specific objectives 86, No.11, Nov.1996, p.17-8
to be realised. A trend analysis technique was used to DETERMINING THE DEGREE OF CURE OF
create a knowledge base for a knowledge-based system REACTIVE RESINS
which implemented event-based control of the autoclave. Pflaum K
The objective of the real time control was to guide the
The quality of fibre-reinforced polyester and vinyl ester
process through a desired trajectory. 39 refs.
resins depends heavily on the resin matrix. Consequently,
USA
the degree of cure and the properties of the resin make a
Accession no.622480 decisive contribution to the thermal resistance, mechanical
properties and the chemical resistance of the fibre-matrix
Item 224 laminate. The degree of cure, in turn, is dependent on the
SPI Composite Institute 51st Annual Conference. curing conditions and the progress of the curing reaction,
Conference proceedings. and may also be influenced by the duration of post-curing
Cincinnati, Oh., 5th-7th Feb.1996. Paper 21-D. 627 at elevated temperatures. Different methods are employed
PROCESSING INSTRUMENT TECHNOLOGY: in practice to determine the degree of cure, each of which
(pentaerythritol tetrakis(2-mercaptoacetate)) with the in thin, shell-like cavities with three-dimensional shapes
same allyl monomer. Fourier transform mechanical and features. The numerical algorithm for solving the
spectroscopy, in conjunction with specially designed transport model is based on the use of the control volume
quartz plates, provided an in situ method to elucidate the finite element method, providing a simple scheme for flow
effects of temperature and monomer functionality on the front tracking during mould filling. An example is
photoinitiated polymerisation of these systems. The presented to illustrate the use of this approach in modelling
tetrafunctional thiol system crosslinked faster than the mould filling and in-situ cure in the structural reaction
trifunctional thiol system and the rate of crosslinking injection moulding of a glass fibre-reinforced composite.
increased with temperature. The Winter-Chambon 11 refs.
criterion was applied to determine the gel point and the USA
two parameters which characterise the material at its gel Accession no.606420
point, the gel stiffness and the relaxation exponent. From
the temperature dependence of the gel times, apparent
activation energies of 6.6 and 14 kcal/mol were calculated Item 234
for the tri- and tetrafunctional thiol systems, respectively. Journal of Reinforced Plastics & Composites
Possible relevance to adhesives for optical bonding and 15, No.9, Sept.1996, p.922-43
conformal coatings is suggested. 22 refs. USE OF EVANESCENT WAVE FLUORESCENCE
SPECTROSCOPY FOR CONTROL OF THE
USA
LIQUID MOULDING PROCESS
Accession no.607252 Woerdeman D L; Flynn K M; Dunkers J P; Parnas R S
Johns Hopkins University; US,National Inst.of
Item 232 Standards & Technology
Antec 96. Volume II. Conference proceedings.
A cure monitoring sensor for liquid composite moulding
Indianapolis, 5th-10th May 1996, p.2484-8. 012
was developed on the basis of an evanescent wave
NEUROCLAVE: NEURAL NETWORK BASED
fluorescence measurement performed with an optical fibre
INTELLIGENT CONTROL OF THE
embedded in the preform. The optical fibre was similar
AUTOCLAVE CURE PROCESS
in cost to standard glass optical fibre, but the addition of
Albin D C; Coulter J P; Li X; Altan M C
a small amount of lead oxide raised the refractive index
Lehigh University; Oklahoma,University
above that of the resins, permitting evanescent wave
(SPE)
sensing. Evanescent wave sensing allowed the
A real-time intelligent controller for the autoclave cure measurement to be obtained within an approximately 1
process was developed utilising the rapid predicting micrometer radius of the fibre surface, providing a
capabilities of artificial neural networks. The controller measurement of resin cure that was most appropriate for
compensates for unexpected occurrences and prepreg predicting final part properties. The moulding system used
variation, leading to higher final part quality than from to make the parts with the embedded optical fibre was
cure cycles determined off-line. The present controller designed to permit the use of the fluorescence signal in a
improves upon previous real-time controllers by making hierarchical control strategy. The control scheme was
fewer assumptions about the autoclave cure process, and designed to regulate the chemical cure cycle by using the
utilising the more descriptive parameters of degree of cure, cure sensor and a cure model to supervise the base-level
degree of compaction, and viscosity, measurable through temp. control loop. 36 refs.
ultrasonic techniques. 8 refs. USA
USA Accession no.605737
Accession no.606552
Item 235
Item 233 Journal of Composite Materials
Antec 96. Vol.I. Conference Proceedings. 30, No.13, 1996, p.1436-57
Indianapolis, 5th-10th May 1996, p.792-6. 012 MEASUREMENT OF THE DEGREE OF CURE
UNIFIED APPROACH TO MODELLING FLOW OF CARBON FIBRE-EPOXY COMPOSITE
AND HEAT TRANSFER IN MOULD CAVITIES MATERIALS
Chan A W; Morgan R J Jin Soo Kim; Dai Gil Lee
Michigan,State University Korea,Advanced Institute of Science & Technology
(SPE)
A dielectric cure monitoring system which consisted of an
A unified approach is proposed for modelling flow and electric circuit, a sensor and a personal computer was
heat transfer in mould cavities in thermoplastic injection developed to monitor on-line the dielectric properties of
moulding and liquid composite moulding. The transport carbon fibre-epoxy composite materials. A kinetic model
equations for both processes share important similarities of carbon fibre-epoxy composite materials was also
in terms of the computational approach for mould filling developed, involving curve fitting of the DSC data. The
start and end points of cure and the relationship between fluorinated and had a lower refractive index than the silica
the dissipation factor and the degree of cure were obtained fibre. The lower refractive index of the epoxy resin
by comparing the dissipation factor from the dielectric allowed the silica optical fibre to be used as a waveguide
properties with the degree of cure from the DSC data. The for the internal reflection of the near-IR light. The epoxy
relationship between the dissipation factor and the degree resin curing was determined as a function of time and
of cure was tested under various temp. profiles. 18 refs. temp. by analysis of the near-IR spectrum from the epoxy
KOREA adjacent to the fibre obtained by the interaction of the
Accession no.605719 evanescent wave that occurred at each internal reflection
with the low refractive index epoxy resin. The results
obtained showed that epoxy ring-opening and crosslinking
Item 236 reactions could be followed in real time. Treatment of
Smart Materials & Structures the fibre with a silane coupling agent had no observable
5, No.4, Aug.1996, p.415-28 effect on the curing reaction of the epoxy resin. 27 refs.
IN SITU CURE MONITORING OF EPOXY
USA
RESINS USING OPTICAL FIBRE SENSORS
Crosby P A; Powell G R; Fernando G F; France C M; Accession no.600870
Spooncer R C; Waters D N
Brunel University Item 239
Composites Plastiques Renforces Fibres de Verre
A comparative study is presented of in situ cure
Textile
monitoring of epoxy resins by evanescent wave
No.8, March/April 1995, p.104-13
spectroscopy, refractive index change and near-IR
French; German
spectroscopy. Results obtained from the optical fibre
QUALITY CONTROL AND ADVANCED
sensor experiments were used to model cure kinetics of
DIAGNOSTICS FOR PRESSES AND
the resin system. 28 refs.
AUTOMATED LINES FOR THE PROCESSING
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
WESTERN EUROPE
OF REINFORCED THERMOPLASTICS AND
SMC MOULDING
Accession no.605146
Ernst H; Therolf D
Dieffenbacher GmbH & Co.
Item 237
A completely automatic line for the moulding of glass
Biomaterials
mat reinforced thermoplastics is described, with particular
17, No.16, 1996, p.1615-9
reference to its quality control and fault diagnosis
IN SITU ANALYSIS OF THE DEGREE OF
capabilities.
POLYMERISATION OF BONE CEMENT BY
USING FT-RAMAN SPECTROSCOPY INSTITUT FUER VERBUNDWERKSTOFFE GMBH
EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;
Rehmann I; Harper E J; Bonfield W WESTERN EUROPE
London,University
Accession no.595305
A method is described for the in situ analysis of the degree
of polymerisation of bone cement. Fourier transform
Raman spectroscopy was used to investigate the degree Item 240
of polymerisation of a novel polyethyl methacrylate-based High Performance Polymers
bone cement in situ, and the results compared with thermal 8, No.2, June 1996, p.301-5
profiles obtained for polymerisation. 12 refs. NOVEL EPOXY RESIN. II.
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Patel K D
WESTERN EUROPE VP & RPTP Science College
Accession no.602613 A novel epoxy resin, namely diglycidyl ether of
dihydroxyacetophenone was prepared and characterised.
Item 238 Curing was studied kinetically by DSC and characterised
Applied Spectroscopy by IR spectroscopy and TGA. Glass fibre-reinforced
50, No.7, July 1996, p.900-5 composites were also prepared and characterised. 6 refs.
IN SITU NEAR-IR CURE MONITORING OF A INDIA
MODEL EPOXY MATRIX COMPOSITE Accession no.594026
Cossins S; Connell M; Cross B; Winter R; Kellar J
South Dakota,School of Mines & Technology
Item 241
The curing of an epoxy resin adjacent to an embedded International Journal of Adhesion & Adhesives
silica optical fibre was monitored in situ by evanescent 16, No.3, 1996, p.165-72
wave spectroscopy. The epoxy resin was partially ACOUSTIC MONITORING OF COLD-SETTING
Item 251 resins. The sensor signal correlates well with resin
Applied Spectroscopy viscosity. Other applications of the sensor are further
50, No.3, March 1996, p.382-7 discussed. 16 refs.
NOVEL IN-SITU PROBE FOR MONITORING USA
POLYMER CURING Accession no.582954
Aust J F; Booksh K S; Myrick M L
South Carolina,University
Item 254
A novel probe design for in-situ fibre optic Raman
ICAC 95. 4th International Conference on Automated
spectroscopy was tested and used for real-time monitoring
Composites: Volume 1. Conference proceedings.
of an epoxy resin curing system consisting of diglycidyl
Nottingham, 6th-7th Sept.1995, p.79-86. 627
ether of bisphenol A and polyoxypropylenetriamine. The
MONITORING CURE IN COMPOSITE
probe consists of a single fibre optic and a small section
STRUCTURES
of Teflon tubing. The tube acts as a waveguide and sample
Maistros G M; Antonsen G A; Partridge I K;
holder. 20 refs.
Cranfield,University; Short Bros.plc
USA
(Institute of Materials; Institution of Mechanical
Accession no.584713 Engineers; Nottingham,University; SAMPE,European
Chapter)
Item 252 The initial results of a study of temperature distributions
Advanced Materials Newsletter and cure rate variations in mini-demonstrator thermoset
18, No.5, 11th March 1996, p.1 matrix composite structures during the course of autoclave
FIBRE OPTIC SENSOR TECHNOLOGY TAKES cure are reported. The temperature profiles are mapped
THE LABORATORY TO THE PROCESS out using multiple thermocouples and the state of resin
cure is followed by dynamic dielectrical analysis (DDA).
A “smart” process control system, developed at the
By using embedded microelectrodes connected to an
Southwest Research Institute, could eliminate the need for
impedance analyser and a microprocessor, it is possible
transferring samples manually from the ongoing process
to identify the crucial stages of maximum resin flow, resin
to the laboratory for analysis. The group has developed
gelation and to predict resin vitrification in real time. The
useful models that capture the key aspects of the chemistry
results can thus be used to compare the rates of cure
and physics of the polymer’s transformation. A laser fibre-
between different matrix resins, under given cure
optic light scattering device was employed to perform
conditions, or between different regions in one composite
remote, in situ physico-chemical analysis of PMR-15
structure. The practical problems associated with the
polyimide resin under actual cure conditions. Under
transfer of this monitoring technology from the laboratory
artificial intelligence control, the model is run in real time
to the production line are addressed. 8 refs.
in a way that enables it to predict the degree of imidisation
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
as a function of temperature and time.
WESTERN EUROPE
SOUTHWEST RESEARCH INSTITUTE Accession no.582902
USA
Accession no.584470
Item 255
Advanced Materials Newsletter
Item 253 18, No.4, 26th Feb.1996,p.2/5
SPI Composite Institute 50th Annual Conference. MICROMET EXTENDS ITS LINE OF PROCESS
Conference Proceedings. MONITORING SYSTEMS
Cincinnati, Oh., 30th Jan-1st Feb.1995, paper 7E. 627
INTENSITY-BASED FIBRE OPTIC SENSOR FOR Several new products have been introduced by Micromet
IN-SITU CURE MONITORING Instruments for use in characterising resin and composite
Klosterman D A; Saliba T E cure conditions and diffusion properties of coatings and
Dayton,University films. Brief product descriptions are given of the MS-25
(SPI,Composites Institute) dielectric sensor for use in high temperature processes
for monitoring the cure process; the MS-05, designed use
The development of an embeddable fibre optic sensor for with thin, 5 micron thick or thicker layers at operating
process monitoring in polymer composites is presented. temperatures of 150-200C, and an ultrasonic cure
Changes in the total transmitted intensity of the optical monitoring system the UCMS-200.
signal were used to follow changes in the resin refractive
MICROMET INSTRUMENTS INC.
index. For the cure of a common epoxy resin (Hercules
USA
3501-6) the resin refractive index was related to the degree
of cure and resin temperature. The results demonstrate Accession no.582230
the utility of the sensor for monitoring cure in thermoset
58, No.10, 5th Dec.1995, p.1689-700 The determination of thermoset moulding compound
DIFFERENTIAL SCANNING AND DYNAMIC variability by the dielectric cure analysis system (CDCA)
MECHANICAL ANALYSIS OF AMINE- is discussed in some detail in this paper. A comparison is
MODIFIED UREA-FORMALDEHYDE made between the CDCA tests and conventional quality
ADHESIVE control tests. 6 refs.
Ebewele R O USA
Ahmadu Bello,University Accession no.564540
The object of this study was to clarify the physical and
morphological factors responsible for the improved Item 264
performance with modified adhesives using DSC to Polymer International
determine relative cure reaction rates and dynamic 38, No.2, Oct.1995, p.183-9
mechanical analysis to determine changes in storage and CURING OF NOVOLAC-LIGNOCELLULOSIC
loss moduli during cure. 21 refs. COMPOSITES
NIGERIA Simitzis J; Karagiannis K; Zoumpoulakis L
Accession no.568015 Athens,National Technical University
Novolac resin with hexamethylenetetramine was cured
Item 262 with biomass or Kraft lignin or hydroxymethylated Kraft
Journal of Adhesion lignin or cellulose. The agricultural/industrial by-product
52, Nos.1-4, 1995, p.149-66 of olive stones was used as biomass. Kraft lignin,
EFFECT OF ADHERENDS ON THE CURING OF hydroxymethylated Kraft lignin and cellulose were
AN EPOXY ADHESIVE isolated from the biomass. The cure was followed by DSC
Chu F D J; Robertson R E and IR spectroscopy. Generally, the cure of all materials
Michigan,University was a first order reaction, indicating that the cure
mechanism of novolac remains the same. 42 refs.
The effect of E-glass, cured vinyl ester resin and silica
EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;
gel on the curing of an epoxy-anhydride adhesive was
WESTERN EUROPE
examined using calorimetry in both isothermal and
scanning modes and FTIR spectroscopy in the ATR mode. Accession no.564204
Isothermal calorimetry was used to obtain the exotherm,
conversion rate and curing kinetic parameters and Item 265
scanning calorimetry was used to obtain the Tg. ATR- Plastics News(USA)
FTIR was used to study the curing kinetics and chemistry 7, No.26, 28th Aug.1995, p.8
of the adhesive. The results suggested either the DIELECTRIC MONITORS FIND FAVOUR IN
immobilisation of a layer of the epoxy adhesive adjacent AEROSPACE
to inert solid surfaces or selective adsorption of the Renstrom R
accelerator or both, each of which suppressed the cure
Developments in the use of dielectric monitors to shorten
reaction. This was reversed by the presence of adsorbed
the resin cure cycles and reduce autoclave, press and oven
water. At least for the epoxy-anhydride system studied,
processing costs, are reviewed, with particular emphasis
adsorbed water seemed to have the beneficial effect of
on the use of the technique in the processing of advanced
increasing the crosslink density in the interfacial region
composites for aerospace applications.
between the adhesive and adherend. Water also seemed
USA
to change the overall cure reaction, causing more ether
formation and less ester formation than without water. Accession no.564098
38 refs.
USA Item 266
Accession no.564603 Applied Spectroscopy
49, No.9, Sept.1995, p.1225-31
NON-DESTRUCTIVE INSPECTION OF
Item 263
GRAPHITE-EPOXY COMPOSITES FOR HEAT
Thermoset Technology 95. Retec Proceedings.
DAMAGE USING LASER-INDUCED
Research Triangle Park, NC, 13th-15th March 1995,
FLUORESCENCE
paper 6, pp.21. 012
Fisher W G; Storey J M E; Sharp S L; Janke C J;
USE OF DIELECTRIC CURE TECHNIQUES TO
Wachter E A
DETERMINE THERMOSET MOULDING
Oak Ridge National Laboratory
COMPOUND VARIABILITY
Horn S W Laser-induced fluorescence was applied to the non-
CYTEC Industries Inc. destructive inspection of graphite fibre-reinforced polymer-
(SPE,Piedmont Coastal Section; SPE,Thermoset Div.) matrix composites. On curing, the epoxy resin in these
investigated as potential candidates to monitor and and vitrification) to be assigned to particular features
subsequently control the manufacturing process of a observed in the dielectric response of the resin during
composite material. 11 refs. cure at 140, 150, 160 and 180C. With this information, it
USA was then possible to use in situ dielectric measurements
Accession no.554143 in a composite curing at 150C to identify both the time at
which the resin matrix underwent gelation, and to predict
the vitrification time whilst the cure was proceeding. A
Item 272 theoretical model was used to extract the dipolar
Macromolecular Symposia relaxation data from the overall signal which, in this type
Vol.94, May 1995, p.273-82 of complex commercial system, was dominated by ionic
APPLICATION OF FTIR SPECTROSCOPY TO conduction. 13 refs.
THE STUDY OF CURING OF GLASS
CIBA
REINFORCED POLYESTER COMPOSITES
EUROPEAN COMMUNITY; EUROPEAN UNION; UK;
Matias M C; Larena A; de la Orden M U; Urreaga J M WESTERN EUROPE
Madrid,Universidad Politecnica Accession no.553744
The effect of glass fibre reinforcements on the curing
behaviour of unsaturated polyester resins was investigated Item 275
by FTIR. Some additional complications found in the IR Journal of Composite Materials
analysis of curing are also discussed. 20 refs. 29, No.8, 1995, p.1000-24
EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; MODEL BASED CONTROL OF VOIDS AND
WESTERN EUROPE
PRODUCT THICKNESS DURING AUTOCLAVE
Accession no.554098 CURING OF CARBON/EPOXY COMPOSITE
LAMINATES
Item 273 Joseph B; Hanratty F W; Kardos J L
Macromolecular Symposia St.Louis,Washington University
Vol.94, May 1995, p.145-58 A novel feedback control strategy is presented for the
EPOXY RESIN AND EPOXY BLENDS STUDIED autoclave curing of carbon fibre-reinforced epoxy resin
BY NEAR IR SPECTROSCOPY laminates. The strategy uses an on-line model of the
Chabert B; Lachenal G; Tung C V process to control the quality by adjusting the cure cycle.
Lyon,Universite 17 refs.
Near IR spectroscopy was used to study the cure reactions USA
of various epoxy resins cured with amine hardener. Accession no.552039
Results are presented concerning hydrogen bonding
between epoxy and amine hardener before curing, epoxy Item 276
resins, glass fibre-reinforced epoxy resin composites, and Journal of Reinforced Plastics & Composites
epoxy resin/polyether sulphone blends. 76 refs. 14, No.5, May 1995, p.495-512
EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE; THREE-DIMENSIONAL CHARACTERISATION
WESTERN EUROPE
OF PULTRUDED FIBREGLASS-EPOXY
Accession no.554087 COMPOSITE MATERIALS
Chachad Y R; Roux J A; Vaughan J G; Arafat E
Mississippi,University; Rust College
Item 274
Composites Science & Technology This research involves a three-dimensional examination
53, No.4, 1995, p.355-9 of the temperature and thermochemical aspects for the
DIELECTRIC MONITORING OF CURE IN A manufacturing of cartesian fibreglass-epoxy composite
COMMERCIAL CARBON FIBRE COMPOSITE materials. Comparison of the computer-generated
Maistros G M; Partridge I K predictions were made with experimentally measured
Cranfield,University temperature profiles and the degree of cure obtained using
DSC. A numerical model employing Patankar’s control
The cure of CIBA’s Fibredux 924, based on carbon fibre
volume based finite difference technique was used for
and a formulated epoxy resin matrix, was studied by
solving the governing energy and species equations used
means of dynamic dielectric analysis with embedded
to model the entire heating (moving and non-moving)
sensors. Rheological measurements and independent
sections of the pultruder. 10 refs.
characterisation of the kinetics of cure were first carried
out on the unreinforced matrix resin. These data enabled USA
the main physical transformations in the resin (gelation Accession no.551545
Item 278
Journal of Applied Polymer Science Item 280
56, No.6, 9th May 1995, p.667-75 SAMPE Journal
MONITORING OF LAMINATION PROCESSES 31, No.2, March/April 1995, p.35-40
IN AN AUTOCLAVE WITH FIBRE-OPTIC MOULD ENGINEERING AND MATERIALS. I.
INFRARED SPECTROSCOPY Morena J J
Zhengfang Ge; Brown C W; Brown M American Composites Manufacturing Learning Center
Rhode Island,University; Digital Equipment Corp. A fundamental analysis approach is presented to the
Curing reactions of certain laminates involve a series of engineering, materials and processes involved in advanced
chemical structure changes which occur with increasing composite mould and tool fabrication. Methods for
temperature and/or pressure. This paper describes the use extending tool life are discussed, together with
of a mid-IR chalcogenide fibre to monitor the lamination determination of cure cycle and relative benefits of five
of polymer prepregs in an autoclave. The fibre optic was cure monitoring methods. Relative benefits of different
used both as a wave guide and as a sensing element for mouldmaking materials are compared, with emphasis on
acquiring evanescent wave spectra. The spectra were moulds made with an epoxy matrix that is reinforced with
measured by embedding the fibre optic in a polymer glass or carbon fibre and which may include a honeycomb
prepreg package. The polymer prepregs studied include panel substructure. 1 ref.
epoxy, polyimide, and bismaleimide triazine resins. The USA
degree of cure and an understanding of the kinetic Accession no.549043
Loos resin transfer model are used to monitor and control eighths of an inch or more, a thermal wave started at the
the processing properties of the epoxy resin during resin surface and built in velocity and amplitude until it reached
transfer moulding impregnation and cure of an advanced the part centre. Measurements of material properties at
fibre architecture stitched preform. 13 refs. the part centre were possible using tool mounted ceramic
USA sensors designed to electrically couple to the opposing
Accession no.529876 mould wall. 13 refs.
USA
imaginary parts of the complex permittivity as a function PROPERTIES AND ULTRAVIOLET (UV) DOSE
of the cure time are reported. These adhesives are designed Rakas M A
to exhibit heterogeneous cure which is initiated by the Loctite Corp.
surfaces of two substrates on either side of a bondline. (SPE)
This situation is referred to as low cure through volume
Changes in tensile properties with UV dose in the curing
(CTV) or heterogeneous cure. Three stages in the cure
of acrylate and norbornene end-capped polydimethyl
process are identified and discussed. A physical model
siloxane prepolymers were investigated. Brief reference
based on the Maxwell-Wagner interfacial polarisation
is made to the use of these materials in adhesives. 14 refs.
effect is given which satisfactorily explains the changes
USA
in the complex permittivity which occur due to the surface
initiated redox cure of an anaerobic adhesive. The physical Accession no.524619
model is modified to explain the cure of another model
anaerobic adhesive which is deliberately tailored to Item 309
exhibit a much more homogeneous cure or high CTV. Polymer Engineering and Science
The model is found to fit the experimental data on 34, No.12, June 1994, p.1025-32
complex permittivity for frequencies up to 10 kHz. The FIBRE OPTIC INTRINSIC FLUORESCENCE
adhesive formulations’ ingredients included 10phr FOR IN-SITU CURE MONITORING OF AMINE
hydroxypropyl methacrylate, 10 phr acrylic acid and 75 CURED EPOXY AND COMPOSITES
phr resin base. 47 refs. Hyung-Joon Paik; Nak-Ho Sung
EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND; Tufts University
WESTERN EUROPE
The cure reactions of epoxy-diamine and its composites
Accession no.526163
are monitored in-situ using the intrinsic fluorescence of
the aromatic diamine, diaminodiphenyl sulphone (DDS).
Item 307 With a fibre optic fluorimeter, in-situ cure monitoring was
Antec 93. Conference Proceedings. performed via a single fibre, distal-end probe, in neat
New Orleans, La., 9th-13th May 1993, Vol.III, p.2352- epoxy as well as in commercial grade prepregs containing
5. 012 graphite fibres and DDS curing agent. The prepregs were
INFLUENCE OF REINFORCEMENTS ON investigated during multi-ply lamination in an oven. The
PHOTOCURING: PHOTODYNAMIC fluorescence excitation spectra were obtained by emitting
MECHANICAL ANALYSIS at 420 nm with a scan range of 320-400 nm, and the DDS
Renault T; Ogale A A; Drews M J peak position was determined as a function of cure time
Clemson,University and temperature. 20 refs.
(SPE)
USA
Photodynamic mechanical analysis, a new technique Accession no.521565
combining the advantages of dynamic mechanical
analysis and photocalorimetry, was used to determine the
influence of glass, quartz and carbon fibre reinforcements Item 310
on the UV curing of polyacrylate resins used in Antec 93. Conference Proceedings.
stereolithography. Liquid resin was dispensed on a New Orleans, La., 9th-13th May 1993, Vol.II, p.1660-5.
polyester braided elastic support and exposed to UV light. 012
The increase of the sample modulus due to curing of the ANALYTICAL TOOLS FOR ADHESIVE
matrix was monitored as a function of time. It was found PROCESS DEVELOPMENT
that glass and quartz fibres did not influence the cure, but MacNeal K A
carbon fibres significantly blocked the UV light and Digital Equipment Corp.
retarded the cure. A shear lag model was developed to (SPE)
derive the modulus of the resins from experimental data. DSC, TGA and DMA were used to evaluate cure
15 refs. schedules for three thermally conductive thermoset
USA adhesives for use in attaching an aluminium heat sink to
Accession no.524621 a ceramic integrated circuit package. Information was
obtained on weight loss, outgassing and void formation
during cure, shelf and pot life and viscosity changes as a
Item 308 function of time.
Antec 93. Conference Proceedings.
USA
New Orleans, La., 9th-13th May 1993, Vol.III, p.2344-
6. 012 Accession no.516975
CHARACTERISATION OF CURE IN
PHOTOCROSSLINKING POLYMERS: THE
RELATIONSHIP BETWEEN TENSILE
Item 330
Journal of Applied Polymer Science
42,No.9,5th March 1991,p.2453-63
CONTINUOUS HEATING TRANSFORMATION
CURE DIAGRAM OF AN AROMATIC AMINE/
EPOXY SYSTEM AT CONSTANT HEATING
RATES
Wisanrakkit G;Gillham J K
PRINCETON,UNIVERSITY
A mathematical expression for the overall reaction
kinetics obtained previously for the reaction of a
difunctional epoxy (bisphenol A diglycidyl ether) with a
tetrafunctional aromatic diamine (trimethylene glycol di-
p-aminobenzoate), together with the unique one-to-one
relationship between Tg and chemical conversion, is used
to calculate the materials Tg vs time under heating at
constant rates. Calculated results correlate well with
experimental results obtained by torsional braid analysis.
22 refs.
USA
Accession no.423867
Subject Index
A ALUMINIUM, 11 12 52 119 131 BONDING, 7 34 52 67 75 85 131
132 133 147 188 205 250 303 133 192 241 250 278
ACCELERATOR, 5 18 131 152 310 312 BONE CEMENT, 160 183 195 237
204 212 ALUMINIUM OXIDE, 227 259 BOUNDARY CONDITION, 159
ACETONE-FORMALDEHYDE AMINE, 14 56 65 128 132 152 164 160 233 279 302 303
POLYMER, 206 178 211 257 259 261 269 270 BRAGG GRATING, 60
ACOUSTIC EMISSION, 19 129 309 315 BRAKE, 250
241 AMINOSILANE, 63 307 BRITTLE, 82 190 213
ACOUSTIC MICROSCOPY, 182 ANAEROBIC ADHESIVE, 188 BUILDING APPLICATION, 177
ACOUSTIC PROPERTIES, 158 205 295 306 313 BULK MOULDING
227 ARAMID FIBRE, 198 298 COMPOUND, 143 245 246 260
ACOUSTIC WAVE SENSOR, 227 ARAMID FIBRE-REINFORCED 263 282
ACRYLATE POLYMER, 17 24 38 PLASTIC, 291 304 BUS, 198
39 51 250 308 ARMOUR, 80
ACRYLIC ACID COPOLYMER, ARMOURED VEHICLE, 198
306 ARRHENIUS’S LAW, 35 88 139
C
ACRYLIC ACID POLYMER, 140 146 303 CALIBRATION, 54 153 214 222
ACRYLIC COPOLYMER, 9 ASSEMBLY, 34 192 218 250 298 317
ACRYLIC ESTER POLYMER, 24 ATOMIC FORCE MICROSCOPY, CALORIMETRY, 2 28 46 124 139
38 39 51 85 192 262 292 323
ACRYLIC POLYMER, 16 38 48 ATTENUATED TOTAL CAPILLARY RHEOMETER, 285
51 67 69 91 152 188 227 295 REFLECTION CAR, 152 239
306 313 314 329 SPECTROSCOPY, 9 262 307 CARBON FABRIC, 279
ACTIVATION ENERGY, 5 11 22 AUTOCATALYSIS, 88 CARBON FIBRE, 40 47 57 81 139
82 88 108 128 132 150 195 230 AUTOCATALYTIC, 22 31 315 217 225 307
231 258 304 315 AUTOCLAVE, 6 33 123 137 146 CARBON FIBRE-REINFORCED
ADDITION CURING, 82 190 202 223 232 255 265 275 PLASTIC, 6 14 19 22 25 27 33
ADDITIVE, 5 9 18 56 63 131 132 278 283 317 327 42 43 53 56 61 66 71 73 76 90
133 152 164 166 167 204 211 AUTOCLAVE MOULDING, 229 95 100 101 108 119 123 132
212 213 219 227 256 257 259 AUTOMATION, 54 97 98 155 174 135 136 139 146 147 155 159
262 270 279 302 307 308 310 192 199 224 239 290 301 172 182 185 190 193 200 217
313 315 321 AUTOMOTIVE APPLICATION, 7 225 229 230 235 244 258 271
ADHESION, 7 34 36 79 85 131 60 89 116 152 153 199 239 246 274 275 279 280 285 286 289
132 133 146 188 250 295 310 250 291 296 298 301 302 307 321
312 324
ADHESIVE, 7 9 11 12 13 15 16 21
23 34 36 37 39 41 46 48 49 51
B CASHEW NUT RESIN, 93
CATALYST, 3 78 98 167 188 199
52 55 58 60 67 68 69 72 75 77 BALLISTIC, 80 218
79 85 88 89 91 102 107 117 126 BANK CARD, 250 CAVITY PRESSURE, 228 233
127 130 131 132 133 141 149 BISMALEIMIDE POLYMER, 100 CELLULAR MATERIAL, 152 159
151 163 164 177 183 188 205 199 221 219 227
218 219 231 241 250 261 262 BISPHENOL A, 164 251 CELLULOSE, 264
287 295 308 310 311 312 313 BISPHENOL A CYANURATE, 81 CERAMIC, 158 270 303 310
314 325 329 BISPHENOL A DIGLYCIDYL CHARACTERISATION, 34 70 82
ADVANCED COMPOSITE, 252 ETHER, 3 128 131 145 211 212 85 145 149 150 182 192 202
265 302 320 213 259 315 210 217 221 255 269 276 286
AEROSPACE APPLICATION, 92 BISPHENOL A DIGLYCIDYL 297 311 313 321 325
119 146 148 199 230 265 292 ETHER DIMETHACRYLATE, CHEMICAL MODIFICATION, 56
320 67 57 131 213 221 261
AGEING, 4 36 91 130 132 161 270 BLEND, 4 17 229 244 273 288 315 CHEMICAL STRUCTURE, 12 16
282 289 304 315 325 321 41 45 57 76 82 89 90 109 128
AIR ENTRAPMENT, 133 159 BLOWING AGENT, 133 227 131 196 206 212 221 278
AIRCRAFT, 56 119 146 199 252 BOND STRENGTH, 67 79 132 CIVIL ENGINEERING, 1 127 148
320 133 306 CLOSED LOOP, 155 174 245 282
301
212 247 248 255 321 SENSING, 155 279 302 315 EXTRUSION, 227 285
DIGLYCIDYL ETHER, 240 251 ELECTRON PARAMAGNETIC
269 RESONANCE
DIGLYCIDYL ETHER SPECTROSCOPY, 203
F
BISPHENOL A, 5 ELECTRON SCANNING FABRIC, 21 57 120 307
DILATOMETER, 163 MICROSCOPY, 124 FABRIC REINFORCED, 211
DILATOMETRY, 99 ELECTRONIC APPLICATION, 78 FABRICATION, 7 128 252 324
DIMETHACRYLATE POLYMER, 287 310 325
205 ELEMENTAL ANALYSIS, 206 FABRY-PEROT
DIPHENYLMETHANE EMISSION SPECTRA, 257 259 INTERFEROMETRY, 173
DIISOCYANATE, 46 213 EMISSION SPECTROSCOPY, FAILURE, 56 82 132 181 192 308
DIPOLE RELAXATION, 132 212 217 FAST FOURIER TRANSFORM,
274 288 304 315 322 ENGINEERING APPLICATION, 133
DOUGH MOULDING 97 FATIGUE, 129 153 173
COMPOUND, 162 285 ENTHALPY, 56 65 131 141 212 FAULT DIAGNOSIS, 133 239
DYE, 211 249 257 259 302 EPICHLOROHYDRIN, 164 FIBRE, 4 82 148 150 192 225 278
DYNAMIC DIELECTRIC EPOXIDE RESIN, 2 3 5 6 7 10 11 297 309
ANALYSIS, 254 274 12 13 14 15 19 21 22 25 27 28 FIBRE CONTENT, 142 204 211
DYNAMIC DIFFERENTIAL 33 34 41 42 43 44 45 47 53 55 220 258 270 279 298 302
CALORIMETRY, 141 56 58 60 61 62 63 65 70 71 73 FIBRE DIAMETER, 192 198 259
DYNAMIC MECHANICAL 74 77 78 79 81 84 86 90 94 95 FIBRE GLASS, 21 57 84 139 150
ANALYSIS, 10 36 56 57 69 70 99 100 101 103 107 108 109 217 225
82 87 92 105 110 130 145 182 110 113 115 116 117 119 123 FIBRE OPTIC, 25 56 172 211 214
226 261 289 307 310 325 328 124 126 127 128 131 132 133 222 246 251 252 253 268 271
DYNAMIC MECHANICAL 135 136 139 141 145 147 149 278 283 309
PROPERTIES, 32 57 113 130 150 151 152 154 155 156 163 FIBRE-REINFORCED PLASTIC,
145 213 226 304 307 330 164 167 170 171 172 176 178 6 14 27 43 53 56 57 61 66 71
DYNAMIC MECHANICAL 179 181 182 184 185 186 187 76 87 90 93 100 113 132 135
THERMAL ANALYSIS, 19 26 189 190 193 196 199 200 202 138 146 147 150 155 159 185
70 85 91 116 161 181 229 304 204 211 212 213 214 215 217 190 193 200 217 225 246 249
DYNAMIC PROPERTIES, 32 57 222 227 230 235 236 238 240 291
113 130 145 213 226 241 243 249 250 251 253 256 FILAMENT WINDING, 193 289
257 259 262 266 268 269 270 FILLER, 1 7 32 40 58 66 78 81 131
273 274 275 276 278 279 280
E 283 288 289 290 291 292 296
132 138 140 150 152 195 227
310
E-GLASS, 21 31 262 302 297 298 301 302 303 304 305 FILM, 11 12 13 21 131 153 154
E-MODULUS, 27 121 127 145 183 309 312 315 320 321 230 247 248 255 256
ELASTIC MODULUS, 27 121 127 EPOXY ACRYLATE POLYMER, FINITE DIFFERENCE
145 181 182 183 225 49 225 ANALYSIS, 159 180 233 276
ELASTIC PROPERTIES, 19 158 EPOXY-CRESOL RESIN, 14 303 316
177 182 225 EPOXY CYANATE RESIN, 81 FINITE ELEMENT ANALYSIS,
ELASTOMER, 4 7 19 21 36 75 85 EPOXY-ISOCYANURATE 44 50 120 142 147 159 185 194
97 129 130 131 132 177 219 RESIN, 213 208 225 233 279 302
227 287 293 295 307 308 311 ESR SPECTROSCOPY, 203 FLEXURAL PROPERTIES, 53 82
318 ETHYLENE GLYCOL 104 128 145 181 188 219 226
ELECTRIC FIELD, 132 212 257 DIMETHACRYLATE, 195 229 271 285 289 304 318
304 ETHYLENE GLYCOL FLOW, 40 54 66 80 94 98 112 137
ELECTRICAL CONDUCTIVITY, DIMETHACRYLATE 146 159 201 204 227 233 239
40 58 64 73 74 117 132 167 198 COPOLYMER, 277 279 302
212 291 304 306 315 322 EVANESCENCE, 191 259 320 FLOW FRONT, 159 198
ELECTRICAL PROPERTIES, 40 EVANESCENT WAVE FLOW METER, 242
45 64 73 74 128 132 158 171 SPECTROSCOPY, 176 211 234 FLOW RATE, 159 199 201 233
181 196 197 212 215 240 245 238 243 249 257 259 278 320 239 242 279 285
265 270 279 282 288 303 304 EXOTHERM, 131 190 258 262 FLOW VISUALISATION, 54 302
315 303 310 315 FLUORESCENCE, 16 51 69 184
ELECTRICAL RESISTIVITY, 64 EXOTHERMIC, 3 118 152 159 211 217 234 243 249 257 259
73 212 215 292 304 304 266 268 309
ELECTROMAGNETIC EXPANSION, 100 120 FLUORESCENCE
NON-DESTRUCTIVE SENSING, PHENOL-FORMALDEHYDE 164 167 170 171 172 176 178
192 RESIN, 75 139 179 181 182 184 185 186 187
NON-DESTRUCTIVE TESTING, PHENOLIC RESIN, 82 87 199 250 189 190 193 196 199 200 202
40 63 86 103 104 123 127 129 271 298 319 204 211 212 213 214 215 217
132 133 154 166 169 177 178 PHENYLMALEIMIDE, 87 222 227 249
192 209 266 270 PHOTOCALORIMETRY, 307 POLYEPOXY ACRYLATE, 49 225
NOVOLAC RESIN, 75 82 264 PHOTOCURING, 49 51 225 231 250 307
NUCLEAR MAGNETIC 307 308 329 POLYESTER ACRYLATE, 250
RESONANCE, 72 139 157 164 PHOTODETECTOR, 257 POLYESTER RESIN, 59 138 144
178 221 277 297 312 318 PHOTODYNAMIC 152 161 282
MECHANICAL ANALYSIS, POLYESTER-URETHANE, 311
225 307 POLYETHER ACRYLATE, 250
O PHOTOINITIATOR, 16 24 49 308 POLYETHER-URETHANE, 311
OFFSHORE APPLICATION, 1 329 POLYETHERIMIDE, 26
148 PHOTOLITHOGRAPHY, 225 POLYETHYL METHACRYLATE,
ON-LINE CONTROL SYSTEM, 8 PHOTOMICROGRAPHY, 202 160 237
ON-LINE MEASUREMENT, 20 PHOTOPOLYMERISATION, 16 POLYHYDROXYETHYL
167 192 212 235 284 285 315 17 24 51 67 69 72 329 METHACRYLATE, 157 195
327 PHYSICAL PROPERTIES, 36 84 POLYIMIDE, 57 76 170 181 187
ONE-COMPONENT, 152 218 310 89 196 261 286 247 248 249 252 255 256 278
OPTIC FIBRE, 6 25 36 56 65 83 PICTURE FRAME, 301 324
104 122 124 136 148 172 176 PIEZOELECTRIC, 133 158 169 POLYISOCYANATE, 9 46 84 88
184 189 191 193 200 207 211 197 270 POLYISOCYANURATE, 166 189
214 222 234 236 238 243 246 PIPE, 21 149 231
249 251 252 253 256 257 259 PLAQUE, 181 211 227 POLYMER CONCRETE, 1
267 268 271 278 283 309 320 PLASTICISATION, 56 132 239 POLYMER DISPERSED LIQUID
324 PLASTICISER, 183 CRYSTAL, 17
OPTICAL ANALYSIS, 65 257 POLYACRYLATE, 17 24 38 39 51 POLYMERISATION, 16 17 24 32
OPTICAL PROPERTIES, 16 36 51 250 307 329 51 67 69 72 82 127 158 160
69 152 176 184 211 217 236 POLYACRYLIC, 183 252 318
243 256 257 259 266 273 281 POLYACRYLIC ACID, 140 POLYMERISATION KINETICS,
298 305 308 320 POLYAMIC ACID, 256 16 24 37 47 160 237 329
OPTICAL SENSOR, 256 257 POLYBISMALEIMIDE, 221 229 POLYMETHACRYLATE, 72 188
OPTIMISATION, 10 15 29 50 52 321 205 250 313
96 120 134 149 169 175 179 POLYBISMALEIMIDE POLYMETHYL
223 244 270 TRIAZINE, 278 METHACRYLATE, 32 172 183
ORTHOPAEDIC APPLICATION, POLYBUTYLHYDROXYCYCLOHEXYL 270
53 183 METHACRYLATE, 157 POLYTRIACRYLATE, 39
ORTHOPHTHALIC POLYESTER POLYCYANATE, 229 POLYTRIAZINE, 315
RESIN, 152 POLYCYANATE ESTER, 258 POLYUREA, 46
POLYCYCLOPENTADIENE, 286 POLYURETHANE, 21 23 24 37
POLYDICYANATE, 244 152 166 172 184 219 268 291
P POLYDIMETHACRYLATE, 205 298 311
277 313 POLYURETHANE ACRYLATE,
PACKAGING, 1 7
POLYDIMETHYLSILOXANE, 250 307
PAINT, 89 216
308 POLYURETHANE
PANEL, 147
POLYDIPHENYLMETHANE- DIACRYLATE, 24
PAPER-REINFORCED PLASTIC,
DIISOCYANATE, 88 POLYVINYL ESTER, 7 18 31 59
319
POLYEPOXIDE, 2 3 5 6 7 10 11 61 94 120 226 262 270 291 298
PEEL STRENGTH, 9 39 48 131
12 13 14 15 19 21 22 25 27 28 POROSITY, 133 140 159 192 233
250
33 34 41 42 43 44 45 47 53 55 279 328
PERMEABILITY, 54 159 211 233
56 58 60 61 62 63 65 70 71 73 POST CURING, 34 270 304 329
279 302
74 77 78 79 81 84 86 90 94 95 POT LIFE, 34 204 310
PERMITTIVITY, 64 132 181 212
99 100 101 103 107 108 109 PREFORM, 21 94 98 137 152 155
255 279 288 304 306 315 322
110 113 115 116 117 119 123 159 166 198 199 211 233 234
328
124 126 127 128 131 132 133 243 257 279 301 302
PHARMACEUTICAL
135 136 139 141 145 147 149 PREPOLYMER, 17 37 81 212 229
APPLICATION, 102
150 151 152 154 155 156 163 308
SMALL ANGLE LIGHT 35 62 139 146 149 194 212 231 285 300 302 303 316
SCATTERING, 17 279 292 303 304 315 THICKNESS GAUGE, 317
SMART FIBRE, 148 TEMPERATURE THIN FILM, 11 12 13 153 256
SMART MATERIAL, 1 200 290 DISTRIBUTION, 149 159 190 TIME TEMPERATURE
320 279 302 SUPERPOSITION
SOFTWARE, 64 102 143 159 198 TEMPERATURE GRADIENT, PRINCIPLE, 132
210 224 239 247 287 328 279 303 TIME TEMPERATURE
SOUND ATTENUATION, 270 TEMPERATURE MODULATED TRANSFORMATION, 10 68
SOUND VELOCITY, 227 DIFFERENTIAL SCANNING 70
SPECTROMETER, 102 187 217 CALORIMETRY, 10 TORSIONAL BRAID ANALYSIS,
SPECTROSCOPY, 3 9 11 12 15 16 TEMPERATURE PROBE, 200 70 213 330
37 46 48 56 63 82 168 170 172 TEMPERATURE PROFILE, 276 TOTAL INTERNAL
176 187 191 203 205 211 214 303 310 REFLECTION, 253
217 221 249 265 297 313 318 TENSILE PROPERTIES, 4 21 36 TOUGHENING, 131 244 321
325 41 138 200 226 304 307 308 TOUGHNESS, 76 79 84 131 190
SPRAY-UP, 267 325 213 229
SPRAYING, 246 TEST EQUIPMENT, 6 32 105 106 TOW, 233
STABILITY, 36 82 87 128 147 112 154 182 187 216 219 251 TRACER, 259 302
STANDARD, 95 285 293 304 309 328 TRANSDUCER, 106 133 211 227
STIFFNESS, 104 145 181 271 285 TEST METHOD, 19 21 23 34 95 228 285
289 304 133 138 141 177 192 218 285 TRANSFER MOULD, 290
STORAGE MODULUS, 23 27 145 TEST SPECIMEN, 16 19 183 289 TRANSFER MOULDING, 8 21 25
161 261 304 307 TEXTILE-REINFORCED, 279 27 29 30 35 66 80 92 94 98 105
STORAGE STABILITY, 91 215 302 111 125 129 189
310 THERMAL ANALYSIS, 3 10 26 TRANSMISSION ELECTRON
STRAIN, 6 27 33 60 83 104 119 28 53 56 65 85 92 93 105 110 MICROSCOPY, 124
122 146 173 191 200 205 325 111 116 121 124 125 131 135 TRIACRYLATE POLYMER, 39
STRAIN GAUGE, 33 119 144 146 149 156 181 212 226 TRIALLYL ISOCYANURATE,
STRAIN RATE, 80 146 148 258 279 287 304 310 315 321 231
STRAIN SENSOR, 148 THERMAL CONDUCTIVITY, 62 TRIETHYLENE GLYCOL
STRESS, 27 33 52 99 120 126 134 133 149 159 194 208 209 276 DIMETHACRYLATE, 67
213 304 307 308 298 310 TRIETHYLENE GLYCOL
STRESS-STRAIN PROPERTIES, THERMAL CYCLING, 132 199 DIMETHACRYLATE
27 42 43 52 60 99 100 101 119 289 COPOLYMER, 277
120 193 200 308 THERMAL DEGRADATION, 3 TUBING, 251
STRUCTURAL ADHESIVE, 60 87 118 196 213 218 233 258 TWO-COMPONENT, 228 250 310
107 130 131 132 250 266 TWO-STAGE, 310 315
STRUCTURAL COMPOSITE, 97 THERMAL PROPERTIES, 14 26
289 302 28 56 58 76 113 119 131 132
STRUCTURAL PART, 31 133 149 151 159 179 181 182
U
STYRENE, 59 121 152 246 183 194 195 209 212 213 220 ULTRASONIC, 114 129 158 182
SULFORHODAMINE, 259 233 237 240 258 269 276 289 248 249 271
SURFACE MOUNT DEVICE, 34 300 303 304 308 310 315 321 ULTRASONIC CURING, 210
SURFACE PROPERTIES, 188 311 327 ULTRASONIC HEATING, 77
SURGICAL ADHESIVE, 140 THERMAL STABILITY, 76 82 87 ULTRASONIC PROPERTIES, 55
SURGICAL APPLICATION, 183 128 204 218 229 247 286 80
SYNTHETIC FIBRE- THERMOCOUPLE, 20 97 190 271 ULTRASONIC SCANNING, 133
REINFORCED PLASTIC, 113 279 298 227 247
291 304 THERMOGRAM, 56 82 128 321 ULTRASONIC TEST, 8 19 25 106
THERMOGRAVIMETRIC 107 123 127 133 136 162 164
ANALYSIS, 3 14 41 75 76 128
T 196 206 240 269 310
270 285 318
ULTRASONIC VELOCITY, 227
TAN DELTA, 128 213 304 THERMOMECHANICAL 270
TANNIN, 68 ANALYSIS, 68 ULTRASONIC WAVE, 55 133 145
TAPE, 95 229 THICKNESS, 11 29 30 120 132 ULTRASOUND ANALYSIS, 227
TEMPERATURE CONTROL, 29 133 147 153 160 167 180 182 UNCURED, 131 227 258 289 312
30 35 228 233 234 281 194 202 220 223 227 233 239 UNDERCURE, 133 303
TEMPERATURE DEPENDENCE, 247 255 267 270 275 279 282 UNDERGROUND PIPE, 21
UNDERWATER APPLICATION, 1 W
UNSATURATED POLYESTER,
20 21 59 109 114 121 138 144 WARPAGE, 52 153 228
152 161 162 169 199 226 245 WATER, 63 67 128 181 227 262
270 272 282 285 291 298 300 270
303 304 316 WAVEGUIDE, 132 238 251 257
UREA-FORMALDEHYDE 278 324
RESIN, 261 WAVELENGTH, 133 211 227 256
URETHANE DIACRYLATE, 39 257 259 266
UV CURING, 15 16 17 24 34 36 WETTING, 21 173 199 294
38 39 48 49 69 102 143 225 WOOD, 1 46 68 88
250 293 307 308 WOVEN FIBRE, 120
UV SPECTROSCOPY, 172 256
X
V
X-RAY DIFFRACTION, 90 107
VACUUM, 21 80 211 246 140
VACUUM BAG, 153
VACUUM CASTING, 242
VACUUM-ASSISTED Y
TRANSFER MOULDING, 94 YOUNG’S MODULUS, 27 121
VEHICLE, 198 127 145 181 182 183 225
VEHICLE SHELL, 116
VEHICLE SUSPENSION, 199
VIBRATING NEEDLE
CUREMETER, 219
VIBRATION, 77 191 270
VIBRATIONAL
SPECTROSCOPY, 3 12 24 56
69 75 187 211 214 283
VINYL ESTER RESIN, 7 18 59 94
120 262 270
VISCOELASTIC PROPERTIES,
19 52 158 177 270
VISCOSITY, 20 23 34 36 45 69
111 114 121 143 146 151 152
155 159 181 187 194 197 199
204 210 212 213 218 221 227
232 233 247 248 250 253 255
259 263 270 279 285 288 289
290 291 292 294 298 301 302
303 304 308 310 315 324 328
VITRIFICATION, 10 11 60 66 68
146 181 209 212 213 215 259
274 288 304
Company Index
3M CORP., 227 BRUNEL UNIVERSITY, 176 193 D
200 236
BUEHNEN H.,KG, 294 DAGESTAN,STATE
A BULK MOLDING COMPOUNDS PEDAGOGICAL
AALBORG,UNIVERSITY, 5 INC., 228 UNIVERSITY, 139
ADVANCED FUEL RESEARCH DASA, 86
DAYTON,UNIVERSITY, 33 170
INC., 187 C 253 317 327
AEA TECHNOLOGY, 324
AEROSPATIALE SA, 146 CALIFORNIA,CENTER FOR DEK DYNE INC., 302
AGUSTA SPA, 110 APPLIED REHABILITATION DELAWARE,UNIVERSITY, 18 29
AHMADU BELLO,UNIVERSITY, TECHNOLOGY, 53 30 94 112 120 180 186 192 201
261 CALIFORNIA,UNIVERSITY, 31 223
AKZO NOBEL CHEMICALS SA, 61 108 241 DERA, 130
152 CANADA,NATIONAL DET NORSKE VERITAS, 133
AMERICAN COMPOSITES RESEARCH COUNCIL, 114 DHC ANALYSIS, 293
MANUFACTURING 119 136 182 DIEFFENBACHER GMBH &
LEARNING CENTER, 280 CASA, 56 CO., 239
AMERICAN SOCIETY FOR CASE WESTERN RESERVE DIGITAL EQUIPMENT CORP.,
TESTING & MATERIALS, 95 UNIVERSITY, 297 312 278 310
AOO NPO STEKLOPLASTIK - CATANIA,UNIVERSITY, 292 DRESDEN,INSTITUT FUER
NPK KOMPOZIT, 2 CHIBA,UNIVERSITY, 41 POLYMERFORSCHUNG, 141
APPLIED COMPUTING CIBA, 274 DSM DESOTECH, 15 36 38
TECHNOLOGY INC., 102 CIBA POLYMERS, 250 DUBLIN,TRINITY COLLEGE,
ARGENTINA,NATIONAL CIRA ITALIAN CENTRE FOR 157 306
RESEARCH COUNCIL, 183 AEROSPACE RESEARCH, DUBLIN,UNIVERSITY, 295 314
ATHENS,NATIONAL 124
TECHNICAL UNIVERSITY, CLEMSON,UNIVERSITY, 225 E
264 307
AUBURN INTERNATIONAL CNR, 115 ECOLE NATIONALE
INC., 300 COCHIN,UNIVERSITY OF SUPERIEURE DE CHIMIE DE
AUXIRIBAT, 167 SCIENCE & TECHNOLOGY, MULHOUSE, 24
4 ECOLE POLYTECHNIQUE DE
COLORADO,SCHOOL OF MONTREAL, 311
B MINES, 222 ENICHEM AMERICA INC., 84
COMTECH GMBH, 85 213
BAM, 8
CONCORDIA UNIVERSITY, 122 ENICHEM SPA, 84 213
BATH,UNIVERSITY, 93
136 182 ENSAM, 71
BAUSCH & LOMB INC., 157
CONNECTICUT,UNIVERSITY, ERLANGEN,UNIVERSITAT, 34
BELARUS ACADEMY OF
172 175 187 217 268
SCIENCES, 81
COOPERATIVE RESEARCH
BELGRADE,UNIVERSITY, 322
CENTRE FOR ADVANCED F
BELL HELICOPTER TEXTRON
COMPOSITE STRUCTURES FIBER & SENSOR
CANADA, 144
LTD, 19 147 TECHNOLOGIES INC., 173
BP CHEMICALS LTD., 315
CRANFIELD INSTITUTE OF FIRENZE,UNIVERSITA, 58
BPD DIFESA E SPAZIO, 289
TECHNOLOGY, 288 FRAUNHOFER-INSTITUT FUER
BRIGHAM YOUNG
CRANFIELD,UNIVERSITY, 43 ZERSTORUNGSFREIE
UNIVERSITY, 215
60 65 66 104 125 176 181 190 PRUFVERFAHREN, 133
BRIGHT R.F.,ENTERPRISES
191 254 274 FREUDENBERG-NOK, 75
LTD., 242
CSIC, 16 51
BRISTOL,UNIVERSITY, 126 163
CSIR,MININGTEK, 134
BRITISH
COLUMBIA,UNIVERSITY,
CSIRO, 154 G
CYTEC INDUSTRIES INC., 263
142 GE AIRCRAFT ENGINES, 170
BROOKLYN,POLYTECHNIC GEORGIA,INSTITUTE OF
UNIVERSITY, 322 TECHNOLOGY, 27 117
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