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Effect of different surface treatments on mechanical properties of CFRP

bonded joints

Conference Paper · March 2011

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EFFECT OF DIFFERENT SURFACE TREATMENTS ON
MECHANICAL PROPERTIES OF CFRP BONDED JOINTS
ALBERTO SÁNCHEZ CEBRIÁN, STEFANO LUCCHINI, DR. MARKUS ZOGG AND
PROF. DR. PAOLO ERMANNI
Centre of Structure Technologies, ETH Zürich, Leonhardstrasse 27, 8092 Zürich,
Switzerland
ABSTRACT
The overall goal of our research, which is carried-on in the frame of the European
project ‘Clean Sky’, is to develop novel, more efficient bonding technologies for
aircraft applications. This contribution is presenting the results of an experimental
program aiming at investigating the influence of different surface treatments on the
mechanical properties of bonded CFRP plates. Considered surface treatments
include different mechanical abrading techniques e.g. manual and electrical sanding
and grit blasting, chemical etching as well as special procedures for surface
treatments of composites e.g. peel ply. Additionally, the influence of release agents
used during the manufacturing process of the CFRP plates has been considered.
Digital microscopy is used for the analysis of the composite surface before bonding,
e.g. to detect potential fiber damage caused by the different techniques, and also for
the characterization of the fracture mode after failure. Bonded samples are
mechanically characterized by shear and double cantilever beam (DCB) tests.
INTRODUCTION
Bonding is a well-suited technique for joining Carbon Fiber Reinforced Polymer
(CFRP) structures. Advantages of adhesive bonding include the possibility to avoid
load peaks, as they often appear in riveted joining systems and to not require drilling
in load carrying structures (ref. 1). Furthermore, bonded joints are weight efficient
and have potential for integration of functions (ref. 2).
Adhesive systems for primary composite structures are available in film form or as a
paste (ref. 3). A major advantage of paste adhesives compared to film adhesives is
the possibility to compensate geometrical tolerances of the bonding partners thus
allowing more simple and cost effective manufacturing routes. Paste adhesives have
successfully been applied for structural bonding in non aerospace field; typical
examples are windows bonded to the vehicle structure. The mixing rate and curing
cycle of these systems depends on the chemical composition and typically is
provided by the supplier.
Previous to this joining process, the CFRP surface presents a flat surface, and it is
treated to increase the roughness thus having a larger surface. In this treatment and
also in the production of adherents, the new parts are affected different sources of
contamination which can affect the strength of the joint, e.g. release agent remaining
after curing or loose particles after a mechanical treatment (ref. 4). Another problem
in the manufacturing process of the CFRP plates is that typically the part of the
composite closer to the bonding area has a higher percentage of resin, while carbon
fibers remain some micrometers under this first layer. This fact affects the shear and
peel strength in the joint, being lower with a thicker resin layer. To avoid these
undesirable effects, some treatments can be applied in order to minimize the amount
of resin (ref. 5).
The studied methods in this research can be divided in three main blocks:
mechanical abrasion, chemical pretreatment and special methods for CFRP.
Mechanical abrasion methods pretend to remove this upper resin layer of the
composite. Some simple methods can be found in literature e.g. sanding, grit
blasting… Chemical pretreatments are commonly used for cleaning after a
mechanical treatment to remove loose particles or after the manufacturing process of
the plates. Finally, other approaches can be found in literature for composite surface
treatment e.g. peel ply (ref. 6). The use of release agents in the manufacturing
process of the CFRP plates is also considered for shear tests, comparing its
performance with release films, typically used in production of CFRP plates, under
laboratory conditions.
The effect of all these methods in the quality of the bonded joint is matter of research
in composite industry, for this reason one of the goals of this study is to compare
results obtained with the existing literature. The current state of the art for surface
treatment in reinforced plastics states the procedure to apply these approaches and
the advantages and disadvantages of each technique. The highlights of today’s state
of the art set abrading methods as common approach for surface treatment.
However, the state of the art prefers the use of peel ply over abrading methods due
to its low cost and reduced human factors (ref 7). Also recommends always a
cleaning, chemical or just manual scoring, after applying any surface treatment. This
research will compare different approaches for surface treatment of CFRP bonded
plates and will confirm the importance of surface treatment before bonding.
MATERIALS AND METHODS
Materials
The commercial aerospace carbon fiber curing epoxy prepreg (CFRP) used in this
investigation is EPO TECH PRFB1264 370/11000 FT 1029. Panels for plates are
made with different thicknesses, depending on the different standards for the
mechanical testing e.g. 1 mm for shear test and 1.5 mm for DCB test. All the panels
are produced using a typical vacuum bag lay-up on a tool that is covered by a
release film (Airtech Advanced Materials WL 3900R).
Processing
The curing of the panels is done in an autoclave following recommendations from the
manufacturer of CFRP (Full vacuum at -0.9 bar, pressure inside the autoclave of 2
bar and a temperature of 100°C for three hours). Then the panels are cut as
requested in standards for mechanical testing and microscope analysis.
The bi-component paste adhesive system used to bond the CFRP plates is LMB
6687-2/LME 10049-4 from Huntsman Advanced Materials, mixed in the
recommended ratio between epoxy and hardener of 100:55.3 (LMB 6687-2: LME
10049-4). Spacers are used to keep the bondline thickness constant while the
adhesive is placed in the overlap area (different for shear and DCB: 12.5x25 mm in
single lap shear and 60x20 mm in DCB as shown in figure 2). Bonded plates cure 4
hours at room temperature until gelling state is reached and then are post-cured at
80 °C for 4 hours in a forced convection oven.

Figure 1: Shear and DCB specimens.

Surface treatments
Abrading methods
The abrading methods consist on removing the layer of resin placed at the top of the
composite plate. Different methods following this principle have been applied:
Manual sanding P100 and P150: The election of the size of the sand plays an
important role. With a bigger size, more resin is removed being the process faster
and simpler, but as drawback, the quality of the bond decreases due to fracture of
fibers. Typical sizes recommended for composites in literature are from P80 to P180
for rough sanding (ref. 8).
Electrical sanding: In this case an electrical sander is used with a sand size of P150.
The removal of material is different than with a manual sanding because this
equipment applies the force circumferentially and more homogeneously.
Air-grit blasting: This treatment consists on aluminum particles thrown with a
pressurized air gun. These small aluminum particles (size from 125 to 315 μm)
impact with the surface to be treated removing the resin.
Chemical methods
Acetone cleaning: This methodology does not consist on milling the material to be
bonded but on cleaning the surface for decontaminating it from grease or other
undesirable substances present after the manufacturing process of the plates or after
the mechanical abrasion methods. After the area is cleaned, water is used to remove
the remaining acetone from the surface to be bonded and finally the samples are
dried in a convection oven for 5 minutes at 40°C.
Other approaches
Peel ply: This method consists on applying a peel ply between the composite and the
lower release film in the manufacturing process of the CFRP plates. The material
used in this case is CS Interglass and is cured under the same temperature, vacuum
and pressure conditions. The bonding process is done after the removal of the peel
ply, without any additional cleaning.
Adherents made on a tool that is treated by release agent (RA)
In this case the release film used for covering the tool is replaced by this chemical
product. The agent used in this study is Loctite 770-NC Frekote. It is applied four
times with a brush thoroughly on a steel plate and dried each time in a convection
oven with a temperature about 65°C. Afterwards no release film is needed between
the mold and the composite, but the rest of the vacuum bag is done with typical
configuration, used for all the plates. Samples are produced with and without
cleaning process before bonding.
RESULTS
Surface topography
The microscope Keyence VHX-600 is used to take images of the specimens once
applied the different surface treatments, as shown in figures 2, 3 and 4. Difference in
the topography within the treatments is observed and roughness is measured in
abrading methods and peel ply. Then these values are compared with the value of
diameter of carbon fibers, from 5 to 8 μm approximately, in order to assess the
potential fracture or damage of fibers. Values of roughness higher than the diameter
of carbon fibers will cause the fracture whereas a lower value will cause only
damage.

Figure 2: Acetone cleaning (Ra=3.30 μm) and manual sanding P100 (Ra=9.5 μm).
Figure 3: Manual sanding P150 (Ra=3.85 μm) and electrical sanding (Ra=4.38 μm).

Figure 4: Grit Blasting (Ra=10.12 μm) and peel ply (Ra=75 μm).
In the images the damage on the fibers produced by the abrading methods can be
observed. The most aggressive approach is grit blasting, where fracture of fibers is
produced and the roughness is higher than any other abrading method. Manual
sanding P100, which has a slightly smaller roughness than grit blasting, causes also
fracture and the scratches are deeper than other sanding methods due to the bigger
diameter of the abrasive particles. Additionally, manual and electrical sanding with
P150 show similar results, showing a measured roughness lower than the diameter
of carbon fibers. Peel ply creates a characteristic print, having peaks of resins on top
of the fibers.
Mechanical testing
For all the mechanical experiments carried out, three samples of each treatment are
tested in a standard test machine (Zwick 1474). In shear stress, the peak before
failure (maximum shear force) is measured and maximum shear stress calculated,
according to EN 2243-1. DCB shows typical cracking behavior, and the fracture
toughness is calculated according to ISO 15024.
Shear test
Results of the average of maximum shear force for each treatment are summarized
in table 1.
 Method Max. Force Average [N] Max. Shear stress [Mpa]
1 No treatment 3734 ± 1629 11.8 ± 5.2
2 Acetone 8513 ± 160 26.1 ± 0.6
3 P100 6961 ± 549 22.6 ± 2.1
4 P150 7374 ± 487 23.2 ± 2.4
5 Electric P150 7378 ± 316 22.3 ± 1.2
6 Grit blasting 7309 ± 589 21.2 ± 1.9
7 Peel ply 6808 ± 589 20.1 ± 1.9
8 RA No treatment 3627 ± 2285 11.6 ± 9.5
9 RA acetone 6849 ± 149 21.4 ± 0.7
Table1: Summary of shear tests according to EN 2243-1.

DCB test
Averages of the medium force for each treatment are summarized in table 2.

Method Fracture thoughness [J/m^2]

1 No treatment 683 ± 166
2 Acetone cleaning 2740 ± 254
3 P100 2297 ± 511
4 P150 2270 ± 719
5 Electric P150 24367 ± 50
6 Grit blasting 1893 ± 488
7 Peel ply 2723 ± 387
Table 2: Summary of DCB tests according to ISO 15024.

Fracture modes
Finally, all broken samples are analyzed for adhesive type failure characterization. In
adhesive bonding, three main types of failure can be observed depending on the
location of the failure. The fracture is adherent if adhesive is not affected. If the failure
is in the center of the bonding, dividing the specimen by the middle of the bondline,
then is called cohesive failure and if the fracture is located in one side of the
adhesive, having most of the bondline in one of the sides, then is called adhesive
failure. This last type of bond failure is not desirable meaning problems of adhesion
between the adhesive and adherent (ref. 9). All the samples after mechanical testing
are studied and summarized in table 3.
Most of the samples present an adherent failure, meaning that the mechanical
performance of the adhesive under shear and DCB is higher than the CFRP. The
adhesive is well bonded to the adherent in most of the samples excepting the non-
treated specimens, which show a lower performance than the rest of the approaches.
Adherent
surface Surface treatment Single lap Shear DCB
Release film No treatment 100% Adhesive 100% Adhesive
60%Adherent,
Release film Acetone cleaning 40% Cohesive 100% Cohesive
Manual sanding 80% Adherent,
Release film P100 100% Adherent 20% Cohesive
Manual sanding 80% Adherent,
Release film P150 100% Adherent 20% Cohesive
Electrical sanding 80% Adherent,
Release film P150 100% Adherent 20% Cohesive
Release film Grit blasting 100% Adherent 100% Adherent
50% Adhesive, 80% Adherent,
Release film Peel ply 50% Adherent 20% Adhesive
Release agent No treatment 100% Adhesive -
80% Adherent,
Release agent Acetone cleaning 20% Cohesive -
Table 3: Fracture types.

CONCLUSIONS
1. Surface treatment improves the mechanical performance in shear (about 100%
better) and DCB (about 60% better), compared with non-treated samples. There
is a clear negative influence of dust and contamination in the performance of the
bonded joint.
2. The best method performing on shear stress is acetone cleaning and the best
methods in DCB test are acetone cleaning and peel ply for samples under
laboratory conditions.
3. Optical microscopy determines fracture of the fibers in all abrading methods,
explaining the decrease of mechanical performance in shear and DCB tests
comparing with chemical cleaning and peel ply.
4. Abrading treatments are difficult to control due to de dependence on the operator
and his ability with the abrading tools. This can result in the destruction of a high
percentage of fibers, as it happened with grit blasted samples, meaning a
decrease of mechanical properties.
5. Peel ply has a high performance in DCB due to a larger bonding area and a low
performance in shear due to load concentration in the resin peaks that appear
with this method despite no applying a cleaning method before bonding, which
can increase the mechanical performance.
6. Adherents made on a tool that was treated with release agent decrease the
mechanical performance in shear stress compared with samples made on a tool
covered by a release film. The reason of the low performance of samples
produced with release agent is the difficulty to remove rests of the liquid from the
samples even with the use of acetone, meaning another source of contamination
of the samples.
 7. Adhesive failure appears only in non-treated samples, explaining the low results
in the mechanical tests.
Comparing the conclusions of this research with today’s state of the art, few
differences can be found. Most of the results accomplish the expectations and the
importance of surface treatments is proved, accomplishing the main goal of this
study.
Looking at the results more in detail some differences can be found between this
study and literature. It can be stated that the used peel ply gives better results than
abrading methods in DCB test, as said in the state of the art. By the contrary, results
in shear stress show similar results for both approaches, having a lower performance
on peel ply than expected. This probably is because peel ply samples in this study
are not cleaned before bonding, decreasing the mechanical performance.
Considering this effect, peel ply has higher values for shear and peel stress than non
cleaned samples.
Another difference can be found in the comparison between grit blasting and
sanding. Both are said to have a similar performance, as proved in this study, but
literature states grit blasting to provide a slightly better mechanical performance than
manual sanding. In this study, it is measured the contrary, a higher value of manual
sanding versus grit blasting in both shear and DSB test. This fact can be due to an
excess of grit blasting in the samples. This treatment is very aggressive and is very
difficult to control, depending on the ability of the operator. In this study, it can be
observed that there is an excess of fiber fractures in specimens where this technique
is applied, decreasing the values in the tests carried out.
REFERENCES
[1] M. C. Y. Niu, Composite Airframe Structure, Hong Kong Conmilit Press Ltd., Hong
Kong, 1992, p. 330.
[2] I. J. van Straalen, Development of Design Rules for Structural Adhesive Bonded
Joints. A Systematic Approach, Technische Universeteit Delft, Delft, 2001, pp. 3-4.
[3] A. Baker, S. Dutton and D. Kelly, Composite Materials for Aircraft Structures,
American Institute of Aeronautics and Astronautics Inc., Blacksburg, 2004, p. 321.
[4] S. Ebnesajjad, Surface Treatment of Materials for Adhesion Bonding, William
Andrew Publishing, Norwich, 2006, p. 5
[5] E. M. Petrie, Handbook of Adhesives and Sealants, Mc Graw-Hill, New York,
2000, p. 661.
[6] Q. Bérnard, M. Fois and M. Grisel, Composites: Part A, 36 (2005) 1563.
[7] V. Flinn, B. Clark, J. Satterwhite and P. Van Voast, in SAMPE Conf., Baltimore,
June, 2007, p. 1.
[8] K. B. Armstrong, W. Cole and G. Bevan, Care and Repair of Advanced
Composites, Society of Automotive Engineers Inc., Warrendale, 2005, p. 280.
[9] S. Ebnesajjad, Adhesives Technology Handbook, 2nd Edition, William Andrew
Publishing, Norwich, 2008, p. 17.

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