Professional Documents
Culture Documents
Bubble Free Resin For Infusion Process: MD Afendi, W.M. Banks, D. Kirkwood
Bubble Free Resin For Infusion Process: MD Afendi, W.M. Banks, D. Kirkwood
www.elsevier.com/locate/compositesa
Abstract
The vacuum infusion process has been found to be very versatile for making large composite structures. During the resin impregnation
process, the vacuum causes the nucleation and formation of air bubbles from gasses dissolved in the resin. One solution to this would be a
degassing process prior to infusion. Recent experiments have shown that a degassing process, conducted in batches with a small quantity of a
bubble nucleation agent (Scotch–Brite) and an air sparging method could reduce void formation in the vacuum infusion process. At 90 mbar,
this method of degassing may remove 40–50% of the dissolved gas. However, despite reducing the level of dissolved gas, some micro-
bubbles remain suspended due to the viscosity of the resin and contribute to void formation. While these results were quite encouraging, there
is a need to design a system to ensure a continuous supply of degassed resin as a better way forward. In a continuous degassing system, it is
necessary to establish the relationship between the degassing process quality and void content reduction from the perspective of strength and
performance, besides signifying the most viable method of degassing.
q 2004 Elsevier Ltd. All rights reserved.
1.4. Vacuum infusion After infusion, voids can also be formed as a result of resin
shrinkage. Labordus and Soderlund [26] suggest that one
Vacuum infusion is one of the manufacturing techniques way to reduce the void content is to use degassed resin.
suitable for large load carrying composite and sandwich Labordus [1] reported that some reinforcement materials
structures. Resin infusion shares many of the characteristics (e.g. Unifiloe) cause more bubble nucleation than other
of vacuum bag moulding and resin transfer moulding materials, and thus result in laminates with a higher void
(RTM). All these techniques reduce emission of volatile content. Labordus reported resin degassing procedures
components into the workplace by wetting out and curing using bubble nucleation material and air sparging showing
the laminate in a closed system. very good results in reducing the void formation during
In comparison with traditional hand lay-up, the infusion vacuum infusion.
process has obvious health and safety advantages, through The aim of the current studies on the process of vacuum
reductions in human contact with liquid resin and in reduced infusion is to fully understand the specific sources of voids
emissions to the environment. Additionally, laminate and to reduce void formation. Even though it is not
mechanical properties are improved by higher fibre content imperative to eliminate all the voids, it is essential to
and lower voidage. In comparison with conventional minimize the void content as well as assuring the
(matched mould) resin transfer moulding, the process can homogeneity of the laminates. Investigations throughout
offer a substantial reduction in tooling cost, especially for the process have been taken to identify the sources of voids
large parts. These processes are most suitable for making in order to control the void formation during production.
large structures as they minimise mould and laminate Lower resin viscosity, achieved by heat treatment can
deformation during the process as the tooling is uniformly improve the degassing process as well as the wetting profile
subjected to external atmospheric pressure. Petrie [14] and infusion rate but this action also shortens the pot life of
strongly emphasized that the vacuum infusion process the resin solution, resulting in limiting the time the process
virtually eliminates styrene emissions, making for a cleaner has to completely infuse. For the infusion of large
and healthier workplace. This process not only improved the structures, the quantities of resin and hardener to be
air quality, but also reduced non-construction solid waste mixed can make the process very vulnerable to exothermic
products significantly. reaction. Therefore, it is preferable for the manufacturer to
The generic form of resin infusion itself can be traced to have a continuous supply of resin to maintain productivity
the use of the Marco method [15] in 1950, where the dry and minimise quality concerns.
reinforcement was placed onto a solid male tool and then Two issues have been given special attention in this
encapsulated by a semi-flexible female tool used for research; one is to seek an appropriate method of degassing
compaction, and vacuum sealing. The use of a silicone suitable for a continuous process and the other the
rubber bag as one of the tool halves can be traced to the production of bubble free resin.
development by Gotch [16] in 1985 in response to the need
for lower styrene emissions. Le Compte [17] extended these
methods to the fabrication of large structural components 2. Experimental
including hulls for surface effect ships up to 50 m length.
The development of various vacuum bagging materials for 2.1. Degassing dissolved gas
low cost, better compaction, and flow development was
conducted by a number of researchers including Brittles In the case of dissolved gas, it is quite difficult to know
[18], Marcus [19] and Shepheard [20]. the extent to which a solution is effectively degassed. The
The process is often practiced with one of the solid gas concentration at equilibrium, generally increases
mould faces replaced by a polymeric film. This is known by linearly with respect to the absolute pressure (Henry’s
a confusing array of acronyms. In the United Kingdom, it is Law), whereas the gas concentration at absolute vacuum is
commonly referred to as Resin Infusion under Flexible zero. Thus, for manufacturing methods, where the mould is
Tooling (RIFT) [21]. In the United States of America, it is evacuated (vacuum injection, resin transfer moulding, etc.),
known as Vacuum Assisted Resin Transfer Moulding it is likely that the resin will become over-saturated with gas
(VARTM) [22]. The use of a high permeability distribution when exposed to lower absolute pressure.
medium adjacent to the preformed reinforcement has been Dalton’s law states that the total pressure exerted by a
patented and is known as SCRIMPe [23–25]. mixture of gases is equal to the sum of the pressures that
Labordus [1,26] investigated void formation in the would be exerted by each of the gases. For a container filled
vacuum infusion process and verified that voids may be by three gases, the gases together would have a partial
due to local variation in permeability of the reinforcement at pressure of 1 and each alone would have a partial pressure
the resin flow front, leakage, boiling of volatile components relative to its percentage of the whole. For normal air, the
in the resin or gas dissolved in the resin coming out of the partial pressure of each gas would be as shown in Table 1.
solution. In the case of dissolved gas, it is quite difficult to Henry’s law states that the amount of any given gas that
know the extent to which a solution is effectively degassed. will dissolve in a liquid at a given temperature is a function
742 M. Afendi et al. / Composites: Part A 36 (2005) 739–746
Table 1 Table 3
Gas component fraction and partial pressure in normal air Percentage of oxygen content in degassed resin by various methods
Percent of component (%) Partial pressure Epoxy resin mixture Oxygen content (%)
Nitrogen 78.08 0.7808 After mixing 85–96
Oxygen 20.95 0.2095 Fully saturated with air bubble 100
Carbon dioxide 0.03 0.0003 After 15 min degassing with bubble nucleation 53–63
Other 0.94 0.0094 After 60 min degassing with bubble nucleation 50–60
Total 100 1.0000 After 120 min degassing with bubble nucleation 50–60
After 15 min degassing with air sparging 50–60
After 60 min degassing with air sparging 50–60
of the partial pressure of the gas that is in contact with the After 120 min degassing with air sparging 50–60
liquid and of the solubility coefficient of the gas in the Degassing Thin filament through 1 mm orifice 65–75
Degassing thin film through narrow passage 68–78
particular liquid.
(1 mm)
Two epoxy resin systems were used in the experiments Degassing of thin film on spinning disc 55–65
(Table 2). The PRF resin system is very much less viscous (1000 rpm)
than the Vantico system. The PRF resin is about 100 times Degassing of thin film on spinning disc 55–65
more viscous than water, and hence the Vantico resin is (3000 rpm)
around 1000 times more viscous than water. Both resins are
Newtonian fluids. bubbles develop in the mixture. When using bubble
The resin and the hardener were mixed in the proportions nucleation agent, the bubbling activity diminished after
recommended by the respective supplier. Some air bubbles 15 min. A sample was taken and tested with the dissolved
were found to be suspended in the solution. The solution was oxygen meter (Rank Brothers Ltd, Digital Model 10). The
degassed under vacuum at 90 mbar absolute, with a piece of dissolved oxygen meter gives an unstable reading (for
‘Scotch–Brite’ to act as a bubble nucleation agent. Bubble reasons which are not fully understood) resulting in the
nucleation had usually stopped after degassing for 15 min. range of values quoted above. The variation may result from
The viscosity has a very significant effect on the out- non-uniform diffusion of oxygen due to the resin viscosity
gassing process. The PRF resin system took a shorter time and the permeation behavior through the Teflon membrane
for degassing than the Vantico resin system. In the highly of the oxygen meter.
viscous liquid, bubble nucleation was seen to be very slow The oxygen content of the degassed resin dropped from
although detailed timing was not measured. After the the range of 85–96% down to a range of 53–64% after 15 min
degassing process, it was found that the mixture contained a degassing with bubble nucleation agent (Table 3). However,
lot of micro-bubbles in suspension. These micro-bubbles the test equipment does show significant reduction of oxygen
take a long time to travel up to the surface of the resin: about content. The same procedure of testing has been carried out
4 h for the PRF resin mixture and much longer for the on different samples with variation of prolonged exposure to
Vantico resin. vacuum and different methods of degassing.
To measure how much dissolved gas has been extracted
from a resin solution after being degassed, the resin needs to 2.2. Micro-bubble analysis
be analyzed for its chemical content, especially, the amount
of gas still remaining in the solution. One standard method After degassing using bubble nucleation, it is found that
is the dissolved oxygen meter, normally used for measuring the resin mixture contains a lot of micro-bubbles in
water-based solution. Oxygen is much easier to measure suspension. Degassing (by one of our industrial partners)
than nitrogen and the relationship between the level of air with lower vacuum pressure of 5 mbar gave the same result.
and that of oxygen is well correlated. Therefore, the oxygen Mass-spectral analysis of the bubble showed that the content
content should be able to give an approximate represen-
tation of the effectiveness of dissolved gas removal in any
degassing method.
All degassing processes were done at 90 mbar absolute.
Degassing at lower vacuum pressure should give lower
readings of oxygen content. When degassing starts, a lot of
Table 2
Resins and hardeners: supplier, type and viscosities in mPa s
3. Conclusions
[9] Kurematsu K, Koshi M. Kinetic studies on void formation during [18] Brittles P. New development in RTM. Proceedings of the 19th
liquid epoxy resin impregnation through polyester non-woven fabric. international BPF composite conference, Birmingham 1994 p. 11–26.
Colloid Polym Sci 1985;263:454. [19] Marcus SA. New developments of vacuum bag forming. J Adv Mater
[10] Oliver P, Cottu JP, Ferret B. Effects of cure cycle pressure and voids Process 1987;6:33–9.
on some mechanical properties of carbon/epoxy laminates. Compo- [20] Shepheard G. Embossed vacuum bag, methods for producing said bag
sites 1995;26:509–15. and composite article produced using said bag. World Patent
[11] Wood JR, Bader MG. Void control for polymer matrix composite (1): W092/13695 1992.
theoritical and experimental methods for determining the growth and [21] Williams CD, Summerscales J, Grove SM. Resin infusion under
collapse of gas bubbles. Compos Manuf 1994;5(3). flexible tooling (RIFT): a review Composites Part A. Appl Sci Manuf
[12] Bear J. Dynamic of fluid in porous media.: American Elsevier 1996;27A:517–24.
Publishing Company; 1972. [22] Beckwith SW, Hyland CR. Resin transfer moulding: a decade of
[13] Kiljanski T, Dziubinski M. Centrifugal degassing of highly viscous technology advances. SAMPE J 1998;34:7–19.
Newtonian liquids. Can J Chem Eng 2001;79. [23] Seemann WH. US Patent 4902215, 20 February 1990.
[14] Petrie G. L. Intermarine Savannah’s vacuum infusion process, http:// [24] Seemann WH. US Patent 5052906, 1 October 1991.
powerandmotoryacht.about.com/library/weekly/aa080801b.htm; [25] Seemann WH. US Patent 5316462, 31 May 1994.
2002. [26] Labordus M, Soderlund J. Avoiding voids by creating bubbles,
[15] Marco method. US Patent 2495640, 24 January 1950. degassing of resin for the vacuum injection process. Centre Of Light
[16] Gotch TM. Low investment alternative to hand lay up GRP weight Structures, TUD-TNO, Delft (NL) http://www.clc.tno.nl/
production. Hand off GRP conference.: Plastics And Rubber Institute; Projects/Recent/Voids.Html; 2001.
1985 p. 1–11. [27] Howell PD. The draining of a two-dimensional bubble. J Eng Math
[17] Le Compte. US Patent 4359437, 16 November 1982. 1999;35:251–72.