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Materials and Design 32 (2011) 3671–3685

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Materials and Design


journal homepage: www.elsevier.com/locate/matdes

Review

A review: Fibre metal laminates, background, bonding types and applied


test methods
Tamer Sinmazçelik a,b,⇑, Egemen Avcu a, Mustafa Özgür Bora a, Onur Çoban a
a
Kocaeli University, Mech. Eng. Dept., Umuttepe Campus, 41380 Izmit, Kocaeli, Turkey
b
TUBITAK-MRC, Materials Institute, P.K. 21, 41470 Gebze, Kocaeli, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: During the past decades, increasing demand in aircraft industry for high-performance, lightweight
Received 28 January 2011 structures have stimulated a strong trend towards the development of refined models for fibre-metal
Accepted 4 March 2011 laminates (FMLs). Fibre metal laminates are hybrid composite materials built up from interlacing lay-
Available online 12 March 2011
ers of thin metals and fibre reinforced adhesives. The most commercially available fibre metal lami-
nates (FMLs) are ARALL (Aramid Reinforced Aluminium Laminate), based on aramid fibres, GLARE
Keywords: (Glass Reinforced Aluminium Laminate), based on high strength glass fibres and CARALL (Carbon Rein-
B. Sandwich structures
forced Aluminium Laminate), based on carbon fibres. Taking advantage of the hybrid nature from
C. Surface treatments
E. Mechanical
their two key constituents: metals (mostly aluminium) and fibre-reinforced laminate, these compos-
ites offer several advantages such as better damage tolerance to fatigue crack growth and impact
damage especially for aircraft applications. Metallic layers and fibre reinforced laminate can be
bonded by classical techniques, i.e. mechanically and adhesively. Adhesively bonded fibre metal lam-
inates have been shown to be far more fatigue resistant than equivalent mechanically bonded
structures.
Ó 2011 Elsevier Ltd. All rights reserved.

1. Introduction effectiveness of the structure. These materials still have their


advantages and disadvantages, like the poor fatigue strength of
Composite materials have been subject of permanent interest of the aluminium alloys and the poor impact and residual strength
various specialists during the last decades. Firstly, military applica- properties of carbon fibre reinforced composites. At the end of
tions in the aircraft industry triggered off the commercial use of the seventies, the idea of using the two materials to form a hybrid
composites after the Second World War. The innovations in the composite structural material to overcome most of the disadvan-
composite area have allowed significant weight reduction in struc- tages of both materials was born [8]. At the Delft University of
tural design. Composites offer many advantages when compared to Technology, it was found that the fatigue crack growth rates in
metallic alloys, especially where high strength and stiffness to adhesive bonded sheet materials can be reduced, if they are built
weigh ratio is concerned. Additionally, they provide excellent fati- up by laminating and adhesively bonding thin sheets of the mate-
gue properties and corrosion resistance in applications [1]. With all rial, instead of using on one thick monolithic sheet [7]. The advan-
these advantages, composite structures have gained widespread tage becomes highly evident if cracks start in one of the sheets of
use in the aerospace industry during the last decades [2–6]. the laminate only, the adhesive layers behaving as crack dividers.
In the fifties, an important goal of aircraft materials develop- Under these circumstances, the sheets that are still uncracked
ment was to improve the crack growth properties of structural reduce the crack growth rate in the cracked sheet. The reduction
materials [7]. Competing materials like advanced aluminium alloys in the crack growth rates persists until a crack is initiated in the
and fibre reinforced composites have potential to increase the cost neighbouring sheet also. Based upon all the research, initial Fibre
Metal Laminates material, ARALL (Aramid Fibre Reinforced
Aluminium Laminate) was introduced at 1978 in the Faculty of
⇑ Corresponding author at: Kocaeli University, Mech. Eng. Dept., Umuttepe
Aerospace Engineering at the Delft University of Technology
Campus, 41380 Izmit, Kocaeli, Turkey. Tel.: +90 262 303 3006; fax: +90 262 303 (DUT) [3]. ARALL consists of alternating thin aluminium alloy
3003. layers (0.2 ± 0.4 mm) and uniaxial or biaxial aramid fibre prepreg,
E-mail address: tamersc@yahoo.com (T. Sinmazçelik). as shown in Fig. 1 [8].

0261-3069/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2011.03.011
3672 T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685

Fig. 1. Schematic presentation of Fibre Metal Laminate (ARALL 2).

Fibre metal laminates (FMLs) are hybrid composite structures minium with aramid and glass fibres, but also can be applied to
based on thin sheets of metal alloys and plies of fibre reinforced other constituents [10]. Fig. 2 gives a classification of FML based
polymeric materials [6]. The fibre/metal composite technology on metal plies. The most commercially available FMLs are ARALL1,
combines the advantages of metallic materials and fibre reinforced based on aramid fibres and GLARE1 based on high strength glass
matrix systems. Metals are for instance isotropic, have a high bear- fibres [8]. These two grades of FMLs are going to be explained in
ing strength and impact resistance and are easy to repair, while full detail Chapter 3.
composites have excellent fatigue characteristics and high strength
and stiffness. The fatigue and corrosion characteristics of metals 1.1. Historical development of fibre metal laminates
and the low bearing strength, impact resistance and reparability
of composites can be overcome by the combination [5,9]. During the last three decades, there has been a search for light-
These material systems are created by bonding composite lam- weight materials that can replace the traditional aluminium alloys
inate plies to metal plies [8]. The concept usually applied to alu- in aerospace structures [11]. For an optimal structural design, a

Fig. 2. Classification of FMLs based on metal plies.


T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685 3673

new material is needed which combines high strength, low density 1. Preparation of tools and materials. During this step, the alumin-
and high elasticity modulus with improved toughness, corrosion ium layer surfaces are pre-treated by chromic acid or phospho-
resistance and fatigue properties. Fibre reinforced composites ric acid, in order to improve the adhesive bonding between
materials almost cover all these demands, except for fracture metallic layer and fibre reinforced laminate (metallic surface
toughness. treatment is explained in detail in Chapter 2).
In 1978, researches were carried out to increase the fatigue per- 2. Material deposition, including cutting, lay-up and debunking.
formance of aluminium alloys at the National Aerospace Labora- 3. Cure preparation, including the tool cleaning and the part trans-
tory and at the Delft University of Technology in Netherland. An ferring in some cases, and the vacuum bag preparation in all
improvement of the fatigue behaviour in laminate sheet materials cases.
was obtained by introducing a high strength aramid fibre into the 4. Cure, including the flow-consolidation process, the chemical
adhesive layers. As a result of all these studies, they introduced curing reactions, as well as the bond between fibre/metal
ARALL, first fibre metal laminate at the Faculty of Aerospace Engi- layers.
neering at the Delft University of Technology in Netherland [3]. In 5. Post stretching, after the hot-curing (200 °C) cycle in the auto-
1984, two international patents were accepted and a pilot produc- clave, the fibre metal laminates carry a residual stress system
tion of four different types of standardized ARALL was started by over the thickness of the material with a small tensile stress
the Alcoa Company after sufficient confidence in this material in the aluminium sheets and compression in the fibres, this sit-
had been gained [7]. The trades ARALL 1 and ARALL 2 were stan- uation adversely effects fatigue resistance of FMLs. Post stretch-
dardized. Arall 1 is a variant with aluminium 7075 layers and Arall ing operation after curing cycle can reverses the residual stress
2 uses aluminium 2024 layers and it was in the as-cured condition system and solves this problem.
[1]. 6. Inspection, usually by ultrasound, X-ray, visual techniques and
Later, a much stiffer ARALL which consists carbon fibres instead mechanical tests [1,7]. Mechanical tests of FMLs are explained
of aramid fibres, the CARALL Laminates, had been investigated in widely in Chapter 4.
DUT [12]. Recent research has shown that CARALL laminates also
have fibre failure occurred during flight-simulation fatigue tests
1.4. Applications
at elevated stress levels, which resulted in poor fatigue perfor-
mance. The limited failure strain of the carbon fibres (0.5–2.0%)
Due to their advantages aforementioned above, FMLs are find-
was thought to be a disadvantage. Thus, it is sensitive to notch
ing great use in most commonly in aerospace applications. A num-
behaviour comparing to monolithic aluminium alloy. Due to the
ber of companies have interest in substitute the traditional
problem of galvanic corrosion between the carbon fibres and the
aluminium components by FML composites [5]. Both ARALL and
aluminium sheet in moisture environment, more research has to
GLARE laminates are now being used as structural materials in air-
be done.
crafts. Fibre Metal Laminates have been successfully introduced
In 1990, another attempt to improve ARALL laminates, adopting
into the Airbus A380 [4]. The Fig. 3 shows FML composite applica-
high strength glass fibre instead of aramid fibres, called GLARE
tions in the Airbus A380 airplane [1,18].
(Glass reinforced, or ARALL with glass fibres) was developed suc-
ARALL has been developed for the lower wing skin panels of the
cessfully [7]. Glass reinforced aluminium (GLARE) is the successor
former Fokker 27 aircraft and the cargo door of the Boeing C-17
of Aramid aluminium laminate (ARALL) [12]. A partnership be-
[8,10]. ARALL 3 material is currently in production and flight test
tween AKZO and ALCOA started to operate in 1991 to produce
on the C-17 cargo doors and GLARE is selected for the Boeing
and commercialize GLARE [1].
777 impact resistant bulk cargo floor.
Finally, a new concept for fibre metal laminates (ARALL &
GLARE), the Spliced Laminates, is launched by the Structural Lam-
inates Company (SLC) in 1992. Spliced laminates are defined as 2. Adhesive bonding
FML in which the aluminium layers are interrupted such that the
dimensions of the spliced sheets depend on the autoclave dimen- Adhesive bonding process has been used in the manufacture of
sions only [7]. aircraft structures and components for 30–40 years [19]. Bonding
techniques are used in an ever-growing number of applications:
electronics (multilayer boards, bounded components), aerospace
1.2. Advantages and disadvantages of fibre metal laminates
and aeronautical industries (F-18 bonded wings), automotive
industries and many more organizations. Bonding structural com-
Fibre metal laminates take advantages of metal and fibre-rein-
ponents with adhesives offers many advantages over conventional
forced composites, providing superior mechanical properties to
mechanical fasteners: lower structural weight, lower fabrication
the conventional lamina consisting only of fibre-reinforced lamina
cost, and improved damage tolerance [20]. Light weight sandwich
or monolithic aluminium alloys [9]. Table 1 summarizes all the
construction and structural bonded joints form a major proportion
advantages of fibre metal laminates depending on previous
of modern aircraft [21]. Modern metallic bonded structures using
studies.
longitudinal lap joints in commercial aircrafts were introduced
The major disadvantage associated with epoxy based fibre
with the advent of the Airbus A300 [19]. As stated in Ref. [19], this
metal laminates is the long processing cycle to cure the polymer
technique is currently migrating from secondary to primary struc-
matrix in the composite plies [6]. This problem increases the cycle
tural applications as one of the most interesting ways to fasten
time of whole production and decreases productivity. This
structural parts with a high level of confidence. For example, struc-
increases labour costs and overall cost of FMLs.
tural adhesive bonding is mainly used for attaching stringers and/
or tear straps to the fuselage and wing skins, to stiffen the struc-
1.3. Production of FMLs tures against buckling. It is also applied to skin-to-core bonding
in metallic honeycomb structures, such as elevators, ailerons,
To produce FMLs, as for polymeric composite materials, the spoilers, and so on [22]. Bonded structures have been shown to
most common process involves autoclave processing. The overall be far more fatigue resistant than equivalent mechanically fas-
generic scenario for production of FMLs involves about five major tened structures and when designed correctly, can sustain higher
activities. load levels than equivalent mechanically fastened joints [21].
3674 T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685

Table 1
Advantages of fibre metal laminates.

Material 1. High fatigue resistance: It is achieved by the intact bridging fibres in the wake of the crack, which restrain crack opening. FMLs have excellent
behaviour fatigue characteristics [5,13]
2. High strength: As mentioned before, FMLs are hybrid structures based on thin sheets of metal alloy and plies of fibre-reinforced polymeric
materials. Combination of metal alloys which have high bearing strength and fibre reinforced composites which have high strength and stiffness.
FMLs are structural materials with high strength [4,5]
3. High fracture toughness: Depending on the studies, FMLs have better fracture toughness than their constituent alloys. Based on this behaviour and
accounting for the lower fatigue crack growth rates presented by these materials, they can be a very attractive option for a wide set of structural
applications [14]
4. High impact resistance: Unlike composites, the damage tolerance behaviour of FML is comparable to conventional aluminium alloys. The same
types of damage and plastic deformation are observed, only at higher impact energy levels. Impact deformation is actually a significant advantage of
FML, especially when compared to composites, because this visible damage significantly increases inspect ability and detect ability. Therefore, the
use of FML allows for repair criteria and techniques [8,15]
5. High energy absorbing capacity: Based upon researches, FMLs are capable of absorbing significant energy through localized fibre fracture and shear
failure in the metal plies [6,16]
Physical 1. Low density: Owing to epoxy based polymer matrix and low density aluminium sheets, FMLs are a weight saving structural material compare to
properties others [7]
Durability 1. Excellent moisture resistance: The moisture absorption in FML composites is slower when compared with polymer composites, even under the
relatively harsh conditions, due to the barrier of the aluminium outer layers [1]. Additionally pregreg layers are able to act as moisture barriers
between the various aluminium layers inside of the FMLs [13]
2. Excellent corrosion resistance: As mentioned above excellent moisture resistance of FMLs and high corrosion resistance of polymer based fibre
laminates ensures FMLs excellent corrosion resistance [7,8,10,13]
3. Lower material degradation: FMLs have excellent moisture and corrosion resistance, FMLs degradation as result of environmental aspects is
significant lower as compared to either metallic structures, or composite structures [5]
Safety 1. Fire resistance: The high melting point of the fibres in FML (for instance, glass fibres in GLARE laminates can withstand 1100 °C) prevents
penetration of the fire to the inner layers. Hence, the fire resistance of FMLs are much better than monolithic aluminium alloys depending on their
fibre melting point. FMLs are being used as fuselage materials in aircrafts. With their good fire resistance, FMLs ensures enough time to passengers
for evacuating the aircraft safely [8,17]
Cost saving 1. FML offer substantial weight savings relative to current metallic structures. Further, the number of parts required to build a component may be
dramatically less than the number of parts needed to construct the same component of metal alloy. This can lead to labour savings. Sometimes
offsetting the higher price of the present materials
2. Owing to fatigue insensitivity of FMLs, less repair and longer maintenance periods are sufficient for FMLs. These advantages reduce maintenance
costs of FMLs [7]

As reported in Ref. [19], early experiences in bonding tech-


niques demonstrated that surface treatment prior to bonding is
the single most critical step which can not be disregarded, even
for tertiary-loaded structures, since it is essential to achieve
long-term service capability [21,23]. A particular surface treatment
tends to modify the substrate surface by delivering the following
features: free from contamination; wettable with either primer
or adhesive; highly roughened; and mechanically and hydrolyti-
cally stable [23]. Surface treatment technologies need to be ex-
plained from the viewpoint of adhesively bonded fibre-metal
laminate research.

3. Surface treatments for adhesive bonding


Fig. 3. Metal/fibre applications in A380 airplane from Airbus [1].
As shown in Table 2, all the treatments for modification of metal
surfaces can be grouped as:
One of the most important aspect of designing aircraft struc-
tures is to consider skin cracks resulting from fatigue that the 1. Mechanical.
cracks will be discovered within a particular inspection interval 2. Chemical.
prior to their reaching a critical crack length that can lead to cata- 3. Electrochemical.
strophic failure. As noted in Ref. [7], at the Delft University of Tech- 4. Coupling agent.
nology, it was found that the fatigue crack growth rates in adhesive 5. Dry surface treatments.
bonded sheet materials can be reduced. If they are built up by lam-
inating and adhesively bonding thin sheets of the material, instead Solvent degreasing is important, because it removes contami-
of using on one thick monolithic sheet. The advantage becomes nant materials which inhibit the formation of the chemical bonds.
highly evident if cracks start in one of the sheets of the laminate However, solvent degreasing, while providing a clean surface, does
only, the adhesive layers behaving as crack dividers. Under these not promote the formation of acceptable surface conditions for
circumstances the sheets that are still uncracked reduce the crack longer term bond durability [21]. The degreasing stage usually
growth rate in the cracked sheet. The reduction in the crack growth makes use of chlorinated solvents such as trichloroethylene,
rates persists until a crack is initiated in the neighboring sheet also. 1,1,1-trichloroethane, perchloroethylene, or dichloromethane, or
The research on adhesive-bonded sheet metal laminates is then be- alternatively, non-chlorinated solvents including methyl ethyl
came the predecessor of a new class of materials; the fibre-metal ketone, methanol, isobutanol, toluene or acetone [24]. All alumin-
laminates [7]. ium alloy sheets were initially degreased prior to further surface
T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685 3675

Table 2 acid-etch were consistently reported to be out-performed by anod-


All treatments for modification of metal surfaces. ized surfaces so that the inconsistent results made them unsuitable
Treatments Nature of Ref. for stand-alone treatment in primary bonded structures [23].
treatments Chemical acid etches are given in Table 3 with concentration of
Grit-blasting Mechanical [26–29] compounds, used temperature and immersion time.
Chromic–sulphuric acid (CAE) Acid etching [30,33]
Sulfo-ferric acid (P2) Acid etching [31]
Forest Product Laboratory (FPL) Acid etching [32]
3.3. Electrochemical treatment
Alkaline Etching [25,30]
Chromic acid anodizing (CAA) DC-anodizing [46] Good adhesion between the metal and the adhesive could be
Phosphoric acid anodizing (PAA) DC-anodizing [23,34,36] obtained when the aluminium surfaces were degreased in alka-
Sulphiric acid anodizing (SAA) DC-anodizing [36,45]
line solutions or organic solvents and subsequently etched in
Boric-sulphiric acid anodizing (BSAA) DC-anodizing [24]
Phosphoric acid anodizing (AC-PAA) AC-anodizing [36] aqueous chromic–sulphuric acid solutions. However, this surface
Sulphiric acid anodizing (AC-SAA) AC-anodizing [36] pre-treatment was found to be insufficient in certain non-
Silane Coupling/oxidation [28,47,49–52] bonded areas where corrosion occurred. The corrosion suscepti-
Sol–gel Coupling/oxidation [53–57] bility was reduced if the aluminium surface, after chromic–sul-
Excimer laser texturing Mechanical [54,58–62]
Plasma sprayed coating Ablation/oxidation [35,63–67,69]
phuric acid etching, was anodized before bonding [34]. In
Ion beam enchanced deposition Ablation/oxidation [62,68] order to obtain optimum durability of adhesive bonded alumin-
(IBED) ium joints, anodizing processes are extensively used in the aero-
space industry. Anodizing produces a thin oxide film, again with
a high degree of micro-roughness and an oxide form which is
pre-treatment steps. The first step in the fabrication of baseline highly resistant to hydration [21]. Anodic oxidation in solutions
test specimens was methyl ethyl ketone (MEK)-wiping of alumin- of chromic acid anodizing (CAA) or phosphoric acid anodizing
ium substrates with lint-free tissues to degrease the surface [25]. (PAA) is the preferred stabilizing treatment for the structural
Each surface treatment technologies which have been used to adhesive bonding of high-strength aluminium alloys in critical
modify metal surfaces will be explained detail in subtitles of Sec- applications such as aircraft components [35]. Chromic acid
tion 3. anodizing (CAA) was found to give a relatively thin and ductile
oxide layer and was established as an effective pretreatment
for adhesive bonding with good durability properties in service.
3.1. Mechanical treatment
The European aviation industry is still using this method [36].
However, as a result of delamination in the boundary zone and
As a preliminary preparation step in the multi-stage schedules,
corrosion after only a few years of operation, an improvement
mechanical abrasion has been used to produce a macro-roughened
of the usual FPL process was established. Boeing developed the
surface, different roughness levels of the surface textures and to re-
phosphoric acid anodizing (PAA), which led to a clearly better
move an undesirable oxide layer, respectively [19]. This method
joint durability [23,34].
typically involves abrasive scrubbing of the substrate surface with
As stated in Ref. [24], in almost all studies, however, the DC
sand paper. This mechanical treatment would introduce physico-
electrochemical pretreatments give the best levels of initial adhe-
chemical changes which yield a wettable surface and modify the
sion and durability [23,36,40,41]. The three most widely used
surface topography, i.e., a macro-roughened surface [27].
Mechanical treatments include abrasion methods usually com-
bined with degreasing. Pretreatment by blasting using alumina or
Table 3
silica grit or glass beads change the topography and chemical state
Chemical acid etches and their application process.
of an aluminium adherend by the introduction of a ‘‘peak-and-val-
ley’’ type morphology [24]. In general terms, degreasing is the min- Chemical Application process Ref.
etch type
imum pretreatment that is usually carried out prior to bonding.
Grit-blasting or other mechanical abrasion methods are recognized CAE Immersion in a water solution with 330 ml/l chromic– [30]
sulphuric acid (97% v/v) and 50 g/l potassium
as providing a useful increase in initial adhesion levels [24]. Several
dichromate, at 60 oC for 15 min, and rinsed in tap water
researches have highlighted different aspects of grit blasting or Immersion in a water solution with 185 ml/l chromic– [30]
other mechanical abrasion methods for aluminium alloys. Grit- sulphuric acid (97% v/v) and 127 g/l ferric sulphate, at
blasting, which uses alumina grit with clean, dry, propellant air, 65 °C for 8 min, and rinsed in tap water (percentages by
is employed as a logical surface activation step prior to modify weight: 48% H2O, 37% H2SO4 and 15% FeSO4)
Immersion at 15 min in a 65 °C, followed by tap and [33]
the metallic surface for satisfactory bonding results [26–29].
de-ionised water rinsing
P2 Involves treatment of the adherend surface with an [31]
3.2. Chemical treatment aqueous acidic solution containing Fe(III). (1)
immersing the adherend in the P2 solution at 65 °C for
The most commonly applied chemical treatments are based on 8 min, (2) rinsing the specimen in DI water for 2–3 min,
and (3) drying the aluminium bars in an oven at 60 °C
a chromic–sulphuric acid etch [23,37]. This treatment consists of
for 30 min. The P2 solution was prepared by dissolving
immersion of the substrate in a solution of sulphuric acid and 122.5 g Fe2(SO4)3 4H2O and 0.185 l of concentrated
potassium dichromate. Typically, chemical treatment, i.e., acid- sulphuric acid in enough water to make a liter of
etching, is an intermediate production step between degreasing, solution
alkaline cleaning, and electrochemical treatment [19]. Three classi- FPL Treat with optimized FPL for 30 min at 62 + 2 °C. After [32]
cal acid-etching solutions were introduced to modify the metallic treatment in the acid, the aluminium was washed for
20 min in cold running tap water and finally dried in an
surfaces: chromic–sulphuric acid (CAE) [38], Forest Product Labo-
oven at 40 °C for 30 min
ratory (FPL) [25], and sulfo-ferric acid (P2) etches. The most effec-
Alkaline Immersion in 100 g/l NaOH solution, at 60 °C for 1 min, [30]
tive etches incorporate mixed chromic and hydrofluoric acids.
etch and rinsed in tap water
However, non-chromated acid etchants have been demonstrated Immersion in %10 wt. NaOH solution for 2 min at 60 °C [25]
to provide good adhesion results [23,39].The surfaces treated with
3676 T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685

electrochemical processes used in prebond applications are phos- promotes the hydrolytic stability of the adhesively bonded joint,
phoric acid anodizing (PAA), chromic acid anodizing (CAA) and sul- leading to increased durability in wedge tests.
phuric acid anodizing (SAA). Other electrolytes have been studied Sol–gels are organic–inorganic polymers formed by hydrolysis/
but to a much lesser extent. CAA and PAA are both extensively used condensation reactions of alkoxide precursors, primarily silanes,
in aerospace applications [42,43]. All DC anodizing procedures are which have found applications as electronic, optical and protective
complex multi-stage operations incorporating degreasing, desmut- coatings. These coatings possess important characteristics such as
ting and deoxidizing stages [34]. The boric–sulphuric acid anodiz- chemical stability, physical strength and scratch resistance. The
ing (BSAA) process has advantages associated with both the CAA sol–gel process can be used to form nanostructured inorganic films
and PAA. A BSAA process has been patented by Boeing as a direct (typically 200 nm to 10 lm in overall thickness) that are more
replacement to CAA to meet environmental regulations [44]. AC resistant than metals to oxidation, corrosion, erosion and wear
anodizing is a highly feasible, robust, and environmentally friendly while also possessing good thermal and electrical properties [53].
process, which is free from the hexavalent chromium found in the As noted in Ref. [19], sol–gel which involves the growth of me-
conventional CAA. A distinct difference from DC anodizing is tal–oxo polymers through both hydrolysis and a condensation
hydrogen gas generation on the treated surface during the hot reaction to form inorganic polymer networks in thicknesses rang-
AC anodizing process [19]. Electrochemical treatments which are ing from 50 to 200 nm [54,55]. The Boegel EPII sol–gel agent con-
used for improving the metallic surfaces as an adhesive layer are sists of a dilute aqueous epoxy-silane and zirconium alkoxide. This
shown in Table 4. mixture provides a thin inorganic zirconium oxide film incorpo-
rated with the epoxy-silane that is applied to the metallic surface
[55,56]. In this process, zirconium reacts with the metallic surface
3.4. Coupling agent treatment
to produce a covalent chemical bond, while the epoxy-silane offers
a reactive organic group for bonding with the adhesive [55,57].
There is an ongoing need to develop environmentally friendly
coupling agent techniques, i.e., silane or sol–gel, which can be used
with the current generation of materials, i.e., primer and film adhe- 3.5. Dry surface treatments
sive [19]. Silane based products are becoming an interesting mate-
rial for pre-treatment deposition, because, for the environmental Several dry treatments for aluminium alloy surfaces have been
compatibility, they can be used as substitutes of traditional pre- developed to replace chemical wet treatment process: excimer la-
treatments like chromates [47]. Silane coatings are environmen- ser texturing [54,58–62], plasma-sprayed coating [35,63–67], and
tally sound, multi-metal surface pre-treatments, considered for ion beam enhanced deposition (IBED) [62,68].
use on various metals such as aluminium and its alloys, copper, As reported in Ref. [19], laser texturing was utilized to modify
iron and steel, zinc and magnesium containing alloys [48]. It is an aluminium substrate’s morphology and micro-structure, result-
sufficient to mention that a large number of studies have demon- ing in an increased bond strength and durability [58,59,62]. IBED is
strated the usefulness of silanes such as c-glycidoxypropyltrimeth- a process that cleans and modifies the surface by sputtering with
oxysilane when used as a primer to improve the durability of high energy argon ions under vacuum. This process requires a sur-
structural aluminium bonds. This has been attributed to the forma- face activation step, particularly grit-blasting, prior to IBED. Good
tion of stable, covalent bonds between the metal(oxide) and the initial bond strengths were obtained and the improvements in
silane and the possibility for interphase formation giving a region wedge durability compared with PAA were found [62]. In the aero-
of intermediate modulus between the metal and polymer which nautic industry, a complex and critical process is used in order to
facilitates stress transfer [49,50]. Silanes may be used as stand- enhance both wettability and adhesive properties of aluminium al-
alone processes or part of a more complex pretreatment [28,51]. loy surfaces.
Bis-1,2-(triethoxysilyl)ethane (BTSE) has received much attention Cold plasma treatment represents an alternative to conven-
as it is, after hydrolysis, highly reactive towards (covalent) metal/ tional processes in terms of environmental impact. Plasma is an
film bonding and cross-link formation for the creation of barrier ionized gas containing both charged and neutral particles, such
properties [52]. Fedel et al. [47] examined the effect of water-based as electrons, ions, atoms, molecules and radicals. There are two
silane pre-treatments on galvanized steel. Three different silanes kinds of plasma: cold and hot. The working pressure of a cold plas-
were used for the pre-treatment deposition (glycidoxypropiltri- ma is generally lower than atmospheric pressure which allows the
methoxysilane, tetraethoxysilane and methyltriethoxysilane). The production of chemical reactive species at low temperatures
electrochemical tests showed that the silane layer acts not only (<773 K). Since hot plasma pressure is higher than atmospheric,
as a coupling agent between the inorganic substrate and the organ- the temperature is about 104–105 K [35]. Cold plasma treatment
ic coating, but it also ensures a good barrier effect against water represents an efficient, clean and economic alternative to activate
and oxygen. Rider and Arnott [28] described that the silane layer aluminium surfaces [67]. Plasma spray coatings were also used
as pretreatments prior to adhesive bonding. Davis et al. [63] re-
Table 4
AC and DC Electrochemical Treatment.
ported that a 60Al–Si/40 polyester (by wt.) plasma spray coating
could be engineered for specific applications and was better suited
Pre- Electrolyte Voltage (V) Time Temperature Ref. for the adhesive bonding process of aluminium substrates, by
treatment (wt.%) (min) (°C)
yielding a performance equivalent to that of the PAA treatment
PAA 10 (H3PO4) 10 (DC) 20 25 [36] with some epoxy adhesives in the wedge test. De Iorio et al. [69]
SAA 16 (H2SO4) 1.5 (DC) 20 20 [36]
(current
examined cold plasma treatments to modify the surface properties
density A/dm2) of polymeric materials (polyoxyphenylene–polyammide, polycar-
BSAA 5.0–10.0 15 ± 1 (DC) 18– 26.7 ± 2.2 [24] bonate–ABS) and A1 6061 alloy, with the aim of increasing the sur-
H3BO3/30.0– 22 face adhesion in structural joints.
50.0 H2SO4
SAA 15 (DC) 22 15 [45]
CAA 2.5–3.0 CrO3 40.0 ± 1.0/ 35– 40.0 ± 2.0 [46] 4. Mechanical bonding
50.0 ± 1.0 (DC) 45
PAA-AC 10 (H3PO4) 4 (AC) 30 s 50 [36]
SAA-AC 15 (H2SO4) 10 (AC) 12 s 80 [36] As reported at Ref.[73], the increasing requirements for weight
reduction demand more and more use of composite materials in
T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685 3677

aerospace applications [70]. There has been a progressive increase multiple layers of thin aluminium alloy sheets. A schematic pre-
in the number of metal parts and structures replaced by composite sentation of ARALL is shown in Fig. 1. Combination of high strength
materials, not only in military, but also in civil aircraft design. For metals (aluminium layers) and strong fibres (aramid layers) gener-
instance, composite materials comprise 22% of the total weight of ates a new composite material with a unique set of properties.
the Airbus A380 [71]. The centre wing box, the tail cone, the pres- ARALL laminates offer many advantages such as high strength
sure bulkheads and the vertical and horizontal tails are only some and excellent fatigue properties. Moreover, they retain the advan-
of numerous parts of this modern aircraft [72] being made of com- tages of aluminium alloys, namely lower cost, easy machining,
posite materials. Structural coupling leads to an increase in struc- forming, and mechanical fastening abilities, as well as substantial
tural complexity and to additional local stress factors, but also to a ductility [1,3,85,86].
considerable reduction in global optimizing possibilities, which, in In the ARALL concept, unidirectional fibre prepregs are used.
turn, decreases the lightweight potential of composite design. This concept is very tolerant of material inconsistencies. The fibre
Thus, the development of advanced joining technologies designed orientation is chosen into the direction of the main load. The lam-
to minimize the weight penalties produced by structural coupling inates are designed such that the fibres do not fail, when fatigue
gains a new meaning in the present situation. This is especially cracks develop. That means they remain intact behind the tip of
true for concentrated load transmissions, as it is the case for the propagating crack in the metallic layers. They hinder the open-
mechanically fastened joints [73]. Mechanical fastening is still ing of the crack, and consequently, the crack tip stress intensity in
one of the main methods currently used for joining composite the aluminium sheet is reduced. Fig. 4 shows the crack bridging
components [70], with the advantage of no special surface prepa- mechanism of the ARALL laminates.
rations, easy disassembly and inspection. The fibres are insensitive to the fatigue loading, which key ben-
Hybrid bolted bonded (HBB) joining technology in lap joints efit of this material regarding crack propagation. The pregreg
combines both classical techniques, i.e. bolting and bonding. The transfers loads over the crack, decreasing the stress intensity at
advantages of HBB joints, compared to bolted joints, could be sum- the crack tip and reducing the crack growth rate. As a result of
merized in two main points: (i) continuous instead of discrete load crack bridging mechanism, the crack growth life of FMLs is signif-
transfer distribution along the overlap and (ii) decrease of load icantly extended compared to monolithic aluminium. Crack bridg-
transferred by fasteners. Furthermore, in terms of security, the ing is related to the crack opening, the loads are initially mainly
existence of fasteners in HBB joints could ensure the functioning transferred through the aluminium sheets until a certain crack
of the structure, even if the adhesive layer failure occurs. In man- opening is reached [7,12,87,88]. This behaviour can lead to
ufacturing industries in which numerous bolted and riveted joints improvement in the crack growth rates by a factor of a hundred
are used, the use of HBB technology could be considered as a po- and even more, as compared to monolithic aluminium alloy sheet.
tential solution, in order to reduce the mass as well as the manu- This improvement also allows for weight savings up to 30% in fati-
facturing cost [74]. gue-critical aircraft components. Comparison of ARALL laminates
As stated at Ref. [73], the mechanical behaviour of composite on a structural level with other aircraft materials show that, ARALL
bolted joints has been extensively studied in the past by means of laminates are very attractive materials, especially for fatigue
experimental, analytical and numerical approaches [75–81], mainly dominated structural parts, such as the lower wing skin and the
focusing on the determination of the load capability, the load and
stress distributions and failure criteria of single- and multi-row
bolted joints under the influence of varying laminate configurations
and joint geometries. One of the most effective ways to improve the
load capacity of composite bolted joints entails the local reinforce-
ment of the composite laminate with high-strength metal layers
[82–84], thus clearly improving its bearing and shear capabilities.
The special feature of this reinforcement technique consists of only
embedding the metal layers into the bolted joining area locally,
which is accomplished either by ply-addition (metallic layers are in-
serted between the composite plies [82]) or ply-substitution tech-
niques (composite plies are replaced by metallic layers [84]).
Hence, the total load capability of this reinforcement approach de-
pends not only directly on the load capability of the bolted joint,
but also on the strength of the transition zone between the pure fi-
bre composite material and the hybridized laminate region.

5. Fibre metal laminates

5.1. Arall

The idea of putting fibre reinforcement in the adhesive bond


lines between aluminium alloys has been researched at many lab-
oratories over the past three decades. These researches made it
possible to develop first fibre metal laminates. Finally in 1978,
ARALL has been developed at the Faculty of Aerospace Engineering
at the Delft University of Technology in Netherland. In 1982 the
first commercial product under the trade name ARALL was
launched by ALCOA.
ARALL laminates are made of high strength aramid fibres
embedded in a structural epoxy adhesive sandwiched between Fig. 4. Crack bridging mechanism of ARALL laminates.
3678 T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685

pressurized fuselage cabin of an aircraft. In this way a new hybrid As mentioned before; ARALL has been developed for the lower
material ARALL has been obtained. In 1984 two international pat- wing skin panels of the former Fokker 27 aircraft and the cargo
ents were accepted and a pilot production of four different types of door of the Boeing C-17. Later with new developments, ARALL
standardized ARALL was started by the Alcoa Company after suffi- has been used in wide range of fields and applications. They were
cient confidence in this material had been gained [7]. Commercial- used in fuselage and wing structures in aerospace applications and
ized ARALL laminates are given in Table 5 [89]. used as a ballistic material in military applications. However, they
All four standard ARALL products employ a thermoset adhesive are mostly used as a structural material in cargo doors of aircrafts
system impregnated with unidirectional aramid fibres in a fibre to [8,10,90].
resin weight ratio of 50:50. The fibres are oriented parallel to the
aluminium sheet rolling direction. ARALL laminates are produced 5.2. Glare
under very rigid quality control standards. The aluminium sheets
are anodized and primed according to existing aerospace industry GLARE laminates belong to fibre metal laminates family, they
specifications. Both chromic acid anodizing and phosphoric acid consist of alternating layers of unidirectional glass fibre reinforced
anodizing treatments are used. The outer aluminium surfaces can pregregs and high strength aluminium alloy sheets. At first, they
be left bare for later processing after an ARALL part has been were developed for aeronautical applications as an improvement
formed. Table 6 summarizes production parameters of ARALL of ARALL with advanced glass fibre and introduced at the Technical
laminates. University of Delft in Netherlands in 1990. Later, a partnership be-
ARALL panels are laid up and cured under the appropriate times tween AKZO and ALCOA started to operate in 1991 to produce and
and temperatures either in mechanical press or an autoclave. After commercialize GLARE [1,7,91,92]. Fig. 5 schematically illustrates a
curing, the aluminium layers are in a slight tensile residual stress cross-ply GLARE laminate.
state and the pregreg layers in a compensating compressive resid- The biggest differentiation of GLARE compared to ARALL is that
ual stress state. The ARALL 1 and 3 laminates are given a postcure GLARE consists of glass fibres instead of aramid fibres. This diver-
0.4% nominal stretch to reverse these residual stress signs. The sity gives superior properties to GLARE laminates. Table 7 high-
ARALL 2 and 4 laminates are not postcured stretched as a standard lights the advantages and disadvantages of various fibres for FMLs.
practice, although they can be supplied that way [86]. The specific stiffness and strength in the fibre direction of
GLARE are enhanced over the high strength aluminium alloy used
for the metal layers, which significantly contributes to weight sav-
ings in the designs of tension-dominated structural components.
Table 5 Aforementioned fibre bridging mechanism impedes the growth
Commercially available ARALL laminates [89]. and propagation of cracks in the aluminium-alloy layers under ten-
Metal type Metal Fibre Fibre Characteristics sile fatigue loading conditions [91].
thickness layer direction GLARE has a better adhesion between the glass fibres compared
(mm) (mm) (°) to ARALL. Moreover, glass fibres are much more resistant to com-
ARALL 1 7075-T6 0.3 0.22 0/0 Fatigue, pression loading. As a consequence, fibre failure in the glass fibres
strength has rarely been observed during in fatigue load. Other advantages
ARALL 2 2024-T3 0.3 0.22 0/0 Fatigue,
of GLARE over ARALL are its higher tensile and compressive
formability
ARALL 3 7475-T76 0.3 0.22 0/0 Fatigue, strength, better impact behaviour and better residual strength.
strength, Better adhesion between glass fibre and resin makes GLARE lami-
exfoliation nates with fibres build up in two directions is possible. This being
ARALL 4 2024-T8 0.3 0.22 0/0 Fatigue, is much more suitable for some constructions where biaxial stres-
elevated
temperature
ses occur. These properties seem to make GLARE has a wider range
of potential application [7].
Nowadays, GLARE materials are commercialized in six different
standard grades (Table 8). They are all based on unidirectional
glass fibres embedded with epoxy adhesive resulting in prepregs
Table 6 with a nominal fibre volume fraction of 60%. During fabrication
Production parameters of ARALL laminates [86]. of composites the prepregs are laid-up in different fibre orienta-
Metal Cure Cure Stretching Characteristics
tions between aluminium alloy sheets, resulting in different stan-
type resin temp. dard GLARE grades. For the GLARE 1, GLARE 2, GLARE 4 and
ARALL 7075- AF- 120 °C 0.4% permanent Superior fatigue
GLARE 5 the composite laminate, i.e. the fibre/resin layer, are
1 T6 163-2 stretch resistance stacked symmetrically. In the case of GLARE 3 composite, the com-
High strength posite laminate have a cross-ply fibre layer stacked to the nearest
ARALL 2024- AF- 120 °C With or without Excellent fatigue outer aluminium layer of the laminate, in relation to the rolling
2 T3 163-2 0.4% stretch resistance direction of the aluminium. For the GLARE 6 composite, the com-
Increased posite layers are stacked at +45° and 45°. Table 8 shows these
formability
grades, including the most important material advantages [1].
Damage tolerant
GLARE is produced with a standard bonding technology. After the
ARALL 7475- AF- 120 °C 0.4% permanent Superior fatigue
hot-curing (120 °C) cycle in the autoclave, the fibre-metal lami-
3 T76 163-2 stretch resistance
Controlled nates carry a residual stress system over the thickness of the mate-
toughness rial, with a small tensile stress in the Al-sheets and compression in
ARALL 2024- AF- 175 °C With or without Excellent fatigue the fibres: this is not favourable for fatigue behaviour. A post-
4 T8 191 0.4% stretch resistance stretching operation after the curing cycle can reverses the residual
Increased stress system and solve the problem, thus a tension stress occurs in
elevated fibres and compression in the Al-sheets. But post-stretching causes
Temperature
properties
extra production cost and it is practically impossible for wide pan-
els [7]. Due to unique combination of properties, GLARE can be ap-
T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685 3679

Fig. 5. Schematic illustration of a cross-ply GLARE laminates.

concept utilizing the high strength glass fibres with strain rate ef-
Table 7
Identified advantages and disadvantages of various fibres for FMLs [93].
fect [9,10,86,87]. With excellent impact characteristics, GLARE is
being evaluated for use as cockpit crown, forward bulkheads, the
Fibre Advantage Disadvantage Conventional
leading edge and the flame-resistant capability of GLARE makes
FML
it suitable for flame sensitive areas such as; fire walls, cargo-liners,
Aramid Outstanding toughness Weak in bending, etc. in aerospace applications [7].
buckling, compression
loading and transverse
tension
Excellent fatigue Absorb moisture ARALL
5.3. Carall
resistance in both-
tensile and flexural Fibre metal laminates consist of alternating layers of aluminium
fatigue loading alloy and adhesive impregnated fibres pregregs. Their superior
High Young’s modulus Do not form strong
properties depend strongly on the type of reinforcing fibres used
bonds with other
materials such as in pregregs. Each type has its advantages and limitations. As men-
composite matrices tioned before ARALL laminates are based on aramid fibres. Aramid
Low weight fibres provide good specific strength and modulus, high impact
Glass High tensile strength High weight resistance and outstanding toughness to ARALL laminates. How-
High failure strain GLARE ever, the poor compressive strength is a major limitation for these
Do not absorb moisture Low stiffness hybrid composites. In this point of view, CARALL laminates has
developed as an improvement of ARALL laminates. They contain
different amount of carbon/epoxy pregregs instead of aramid/
epoxy pregregs [93–95]. A schematic illustration of CARALL lami-
plied to wide range of applications. Manufacturers are giving lots nates is shown in Fig. 6.
of attention on GLARE. However, it has been mostly used in aero- Compared with aramid/epoxy, carbon/epoxy composites pos-
space applications so far. Recently, GLARE is used in the main fuse- sess higher specific modulus, but relatively low values of specific
lage skin and the leading edges of the horizontal and vertical tail strength, strain to failure and impact resistance. In terms of fatigue,
planes of new, high capacity Airbus A380. The latter application it was recognized that aramid fibre composites have better low cy-
is a consequence of the excellent impact resistance of the FML cle fatigue performance but worse high cycle fatigue performance

Table 8
Commercially available GLARE grades [1,89].

Grade Sub Metal Type Metal Thickness (mm) Fibre Layer (mm) Pregreg orientation in each fibre layer (°) Characteristics
GLARE 1 – 7475-T761 0.3–0.4 0.266 0/0 Fatigue, strength, yield stress
GLARE 2 GLARE 2A 2024-T3 0.2–0.5 0.266 0/0 Fatigue, strength
GLARE 2B 2024-T3 0.2–0.5 0.266 90/90 Fatigue, strength
GLARE 3 – 2024-T3 0.2–0.5 0.266 0/90 Fatigue, impact
GLARE 4 GLARE 4A 2024-T3 0.2–0.5 0.266 0/90/0 Fatigue, strength, in 0° direction
GLARE 4B 2024-T3 0.2–0.5 0.266 90/0/90 Fatigue, strength, in 90° direction
GLARE 5 – 2024-T3 0.2–0.5 0.266 0/90/90/0 Impact, Shear, off-axis properties
GLARE 6 GLARE 6A 2024-T3 0.2–0.5 0.266 +45/-45 Shear, off-axis properties
GLARE 6B 2024-T3 0.2–0.5 0.266 -45/+45 Shear, off-axis properties
3680 T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685

Fig. 6. A schematic illustration of CARALL laminates.

than carbon fibre composites. Moreover, the high stiffness of car-


bon fibres allows for extremely efficient crack bridging and there-
fore very low crack growth rates [90,96]. CARALL is produced
similar to ARALL and GLARE laminates. Before the curing process,
aluminium surfaces are treated for an optimal adhesion between
aluminium alloy and epoxy resin. Then, they are cured in hot press.
The combination of high stiffness and strength with good impact
properties gives CARALL laminates a great advantage for space
applications. Other applications for this laminate are impact
absorbers for helicopter struts and aircraft seats [96].

6. Test methods of fibre metal laminate composites Fig. 7. Schematic view of compression loading on FML DNS specimen.

Kyowa CDV-700A measuring amplifier. The compressive stress is


6.1. Bending tests
calculated using the cross section of the specimen. To calculate
the applied interlaminar shear stress the effective area of the shear
Mechanical properties of composite materials are governed by
plane was used.
the adhesion between fibre and matrix. Beside this, same proper-
The other test methods applied for ILSS investigation of FMLs
ties of FMLs are governed by the interface bond between compos-
are three and five-point bending tests (Fig. 8).
ite ply and metal ply. Determination of this adhesion is not an easy
Lawcock et al. determined the ILSS of FMLs by three and five-
task therefore various test methods have been proposed in the lit-
point bending tests with a span of 10 mm at a crosshead speed
erature for this purpose: interlaminar shear and interfacial fracture
of 1.3 mm/min [99]. The authors calculated the ILSS by Eq. (1) for
tests. These methods give quality control information and are not
three-point bending and five-point bending:
suitable for design specifications.
Interlaminar shear tests have been used to determine the inter- ILSS ¼ ð33Pc Þ=ð64WtÞ ð1Þ
laminar shear strength (ILSS) of FMLs for a long time [97–105].
According to the literature survey, there are three kinds of test where ‘‘Pc’’ is the initial load for interlaminar failure and ‘‘W’’ and ‘‘t’’
methods according to the interlaminar shear loading types: I. Com- are the width and thickness of the specimens, respectively. In an-
pression loading [97], II. Three and five-point bending [98– other work; Lawcock et al. calculated ILSS of FMLs from three-point
101,103,105] and III. Short beam shear loading [102,104]. These and five-point bending tests as follows [101]:
tests will be explained individually. —Three-point bending : ILSS ¼ ð3Pmax Þ=4Wt ð2Þ
Hinz et al. [97] investigated interlaminar shear properties of
FMLs by means of a double-notch shear test (DNS) according to —Five-point bending : ILSS ¼ ð33Pmax Þ=ð64WtÞ ð3Þ
ASTM D3846 at room temperature. The interlaminar shear load be-
tween the notches was primarily applied by compression on both where ‘‘Pmax’’ is the failure load and ‘‘W’’ and ‘‘t’’ are the width and
ends of the DNS specimen as illustrated schematically in Fig. 7. thickness of the specimens, respectively.
According to author’s advice; for controlled deflection, a linear Reyes and Cantwell also reported their investigation about ILSS
guided sliding carriage should be used. In this work a step motor of FMLs by means of three-point bending test [103]. These tests
applied the compression load with a constant carriage speed were undertaken at crosshead displacement rates between 0.1
0.06 mm/min. It is reported that the load was measured using a and 3 m/s and were stopped once a visible crack had propagated
load cell with 500 N load capacities and recorded by means of a from one of the starter defects. In all these studies; the authors
T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685 3681

Fig. 8. Schematic view of three and five-point bending.

were not mentioned about test standards. However; Khalili et al. conducted according to the ASTM standards. The shape and dimen-
[105] reported that three-point bending tests were carried out on sions of specimens for fatigue testing were based on ASTM D3479;
Zwick 1484 by using specifications of ASTM D790 M-93. the specimen length L = 200 mm, the gauge length LG = 100 mm,
The last test method for investigating ILSS of FMLs is short beam the specimen width W = 25 mm [9,91,108]. Beside this Reyes and
shear test. Park et al. performed ILSS tests to evaluate the extent of Kanga were conducted ASTM E466 test standard for analyzing fati-
hygrothermal degradations as a function of water absorption and gue behaviour of FML [109]. Except these papers there are many
thermal cycles [102]. ILSS of FMLs was evaluated by the ASTM studies that fatigue performance of FMLs was not investigated
D2344 standard specimen through a short beam shear test. They according to these standards [8,87,89,96,106,110–119]. In these
reported that tests were carried out with a crosshead speed of papers specimens were prepared as notched or cracked for the ini-
1.3 mm/min. Botelho et al. [104] also used the same test standard tiation of crack. For fatigue tests; servo hydraulic test machines
(ASTM D2344) for investigating the ILSS of FMLs. Authors reported with approximately a load capacity of 5, 10 and 25 metric tons
that the tests were performed with Instron mechanical testing ma- were used. All constant amplitude fatigue tests were conducted
chine using a test speed of 1.3 mm/min. in tension–tension or tension–compression loading at a frequency
The next test method group for investigating the interface of 10 Hz in lab-air at room temperature [9,87,89,91,108,106,
bonding between composite and metal plies is as mentioned above 117,118]. Beside this in some papers fatigue tests were conducted
the interfacial fracture tests. In these tests, the degree of adhesion with sinusoidal waves of frequency 5 Hz [113,114]. During tests;
between the composite and metal plies was investigated using the the fatigue cracks were observed by various ways; charge coupled
single cantilever beam (SCB) geometry [103,106,107]. This geome- device (CCD) camera [110,115], visual observation [111], digital
try yields mixed-mode I/II loading (tension/shear) conditions at the camera [112], clip gage [114], travelling optical microscope
crack tip in the sample. It is reported in these papers that SCB spec- [106,116,119].
imens with dimensions of 20 mm  200 mm were removed from
the moulded plates. The SCB specimens were clamped in the test 6.3. Tensile tests
fixture shown in Fig. 9 and tested at crosshead displacement rate
of 2 mm/min. The tensile behaviour of FMLs was generally investigated
According to these studies the interfacial fracture energy was according to ASTM D3039 [93,99,105,107,120–126]. Beside this
determined using an experimental compliance method where the Kawai and Arai [123] were benefit from JIS K7073 standard for con-
interfacial fracture energy, ‘‘Gc’’ is given by: ducting tensile testing of FMLs. In all papers dealt with tensile
2
Gc ¼ ð3P 2 ka Þ=2B ð4Þ properties of FMLs, the test specimen shapes and dimensions are
different. Some of them used rectangular tensile specimens
where ‘‘P’’ is the applied force, ‘‘B’’ the specimen width, ‘‘C’’ the [6,106,121] and some of them used dog bone shape tensile speci-
specimen compliance and ‘‘a’’ the crack length. Also it is mentioned mens [101,109,118,124]. Beside this; there are a few papers that
that the specimen compliance was determined as a function of tensile test specimen dimensions were prepared according to the
crack length and a curve fit of the following form applied: standards. In these papers; the authors were not referenced their
3 tensile specimen dimensions. For tensile tests; universal and servo
C ¼ C 0 þ ka ð5Þ hydraulic testing machines were used: Instron tensile testing ma-
where ‘‘C0’’ and ‘‘k’’ are constants for a given specimen. Here, it is chines (4469, 1195, 8502, 4204, 1125, 1251) [96,105,107,109,120–
told that the parameter ‘‘k’’ was determined by measuring the gra- 122,127], MTS tensile testing machines (810, RT/50) [99,121,123–
dient of the plot of the compliance ‘‘C’’ versus the cube of the crack 126] and Shimadzu tensile testing machine [121]. Tensile tests
length ‘‘a3’’ whereas it was not necessary to determine the values of were performed at room temperature at various crosshead speeds
‘‘C0’’. of 0,1 mm/min [124], 0,5 mm/min [96], 1 mm/min [103,93,109,
120,121,123,127], 1,27 mm/min [126], 2 mm/min [6,106,125,36],
6.2. Fatigue tests 5 mm/min [105]. However; in Carrillo and Cantwell’s studies ten-
sile behaviour of FMLs were investigated at a constant strain rate
The fatigue properties of fibre metal laminates have been eval- of 0.04 min1 on an Instron 4204 universal test machine according
uated in numerous test programs. Generally fatigue tests were to the ASTM D3039 test standard [107,122]. It is worthy to say that
during tensile tests the Young’s modulus of each specimen was
recorded using a clip-on extensometer which was incapable of
measuring the complete stress–strain curve.

6.4. Low and High velocity impact and blast loading tests

Due to the importance of understanding the dynamic loading


effect on the FMLs, low and high velocity and also blast loading
tests should be performed. According to the literature survey, it
is well understood that there are many studies dealt with these
Fig. 9. Schematic illustration of SCB geometry. test methods applied to the FMLs. Among these papers some of
3682 T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685

them explain low velocity impact behaviour of FMLs a blast; the swing of the pendulum could be used to calculate
[103,106,13,128,129], some of them dealt with high velocity im- the impulse applied to the panel by detonating the explosive.
pact performance of FMLs [13,128–131] and the others explain
the blast loading effect on the FMLs [132–137].
7. Conclusions
6.4.1. Low velocity impact tests
First of all; the low velocity impact studies shall be mentioned. In this paper, historical development, advantages, disadvan-
In these studies it is seen that all the low velocity impact tests were tages, production and applications of FMLs were presented by
performed by drop weight impact tester. Tests were carried out examining recent studies. In 1978 initial FMLs, ARALL laminates
using drop hammers that have various masses: 2000 g [103,106], which consist alternating thin aluminium layers and aramid fibre
1160 g [128] and 575 g [13,129]. In addition to this, indenter types pregreg were introduced. Later GLARE laminates based on high
were chosen as similar (hemispherical) but the diameters are dif- strength glass fibres and CARALL laminates based on carbon fibres
fering from each other as following: 5 mm [107], 10 mm [106], were developed. GLARE laminates are the successor of ARALL lam-
12.7 mm [128], 15 mm [13,129]. For the investigation of low veloc- inates and commercially production of GLARE laminates were
ity impact performance; square FML samples were generally pre- started in 1991. ARALL, GLARE and CARALL laminates are now
pared as 75 mm  75 mm, 100 mm  100 mm, 125 mm  being used as structural materials in aircrafts. Yet, it can be said
125 mm and clamped between two square or circular frames. that GLARE laminates found more use than ARALL and CARALL
Square frames have 75 mm  75mm or 100 mm  100 mm inter- laminates in aircraft applications. Both laminates production in-
nal openings [106,128]. Beside this circular frames have internal volves five major activities; (i) surface treatment of metallic sur-
diameters of 70 mm [107], 75 mm [103] and 80 mm [13]. The im- face in order to improve bonding between metallic layer and
pact tests are instrumented as the contact force is measured with a fibre reinforced pregreg, (ii) material deposition, (iii) cure prepara-
load cell in the nose of the impactor and the strain in the specimen tion, (iv) cure process, (v) post stretching for reserving residual
is measured with a strain gauge. After an impact, the carriage was stress of FML which caused by curing process. FMLs provides supe-
caught in order to avoid secondary impacts. rior mechanical properties compared to fibre reinforced compos-
ites and aluminium alloys. High strength, high elasticity modulus
6.4.2. High velocity impact tests with improved toughness and excellent fatigue properties can be
After an explanation about low velocity impact tests, in this sec- said as major advantages of FMLs. ARALL, GLARE and CARALL lam-
tion high velocity impact tests applied to FMLs shall be explained inates explained and compared with each other in following
in detail. According to literature survey, it is very clear that gener- chapters.
ally a gas gun consisted of a pressure vessel was used for high In addition to the importance of reinforcement and matrix in
velocity impact tests [13,128–131]. Generally square plates were polymer composites, the bonding between the composite laminae
clamped in a steel support square aperture so that the impactor and the metallic layer is a key issue for the overall metal–fibre lam-
can hit the centre of the test specimen. In this test method; after inate performance. An adequate surface treatment of the metallic
burning through a membrane of the gas gun, the expanding gas layer is required to assure a good mechanical and adhesive bond
or air accelerates a projectile or a steel ball bearing to the velocities between the composite laminates and metal surfaces. In this paper
ranging between 25 and 100 m/s. The velocity of impactor prior to the effects of surface treatments which are improved the metallic
impact can be measured as it exited the barrel by the interruption surface morphology for a better bonding with composite laminates
of two laser beams a known distance apart by using light emitting are investigated. Surface treatment methods, such as mechanical,
diode photovoltaic cell pairs. chemical, electrochemical, coupling agents and dry surface treat-
The ballistic limit is defined as the lowest velocity for complete ments are introduced and showed comparable performance to im-
penetration or perforation. Impact testing should be conducted prove fibre metal laminates.
over a range of impact energies until complete perforation of the Mechanical properties of FMLs are being enhanced by the inter-
FML target was achieved. The resulting perforation energy was face bond between composite and metal plies. This enhancement
then could be used to calculate the specific perforation energy of could be controlled by various test methods. This control reports
the target by normalizing the measured perforation energy by give quality information and are suitable for design specifications.
the areal density of the target [131]. After testing, the specimens In this review; test methods of bending, fatigue, tensile, low and
could be sectioned, polished and then viewed under an optical high velocity impact and blast loading tests for determining the
microscope in order to elucidate the failure mechanisms during mechanical properties of FMLs and research studies utilized from
impact. these test methods were explained in detail.

6.4.3. Blast loading tests


Numerous studies [132,134–138] have investigated the local- 8. Developments for the future
ized blast loading of FMLs. Blast loading was created using a plastic
explosive (PE4) shaped into a circular disc and positioned at the FMLs consist of metallic alloy and fibre reinforced prepreg.
centre of the plate, on top of a polystyrene foam (12–14 mm) Mostly commercially avaible GLARE, ARALL and CARALL consist
pad to attenuate the blast. PE4 consists of 88% RDX and 12% lith- various aluminium alloys. Many researches have been trying to
ium grease, has a detonation velocity of 8200 m/s and a TNT equiv- use possible metallic alloys such as magnesium, titanium, etc. in-
alency of 1.3 [132]. The detonator should be attached to the centre stead of aluminium alloys. It is expected that this diversity gives
of the disc using 1 g of explosive, referred to as a ‘leader’. The im- optimum mechanical properties. Same efforts have been examined
pulse could be varied by varying the diameter of the explosive for engineering polymeric materials to replace fibre reinforced
strips. The FML panels 300 mm  300 mm [136], 400 mm  prepreg.
400 mm [134,138] were clamped between two steel frames leav- Long processing cycle to cure the polymer matrix in the com-
ing an exposed area of 200mm  200 mm [132,136], 300 mm  posite plies increases the cycle time of whole production and de-
300mm [134,135,138]. The frames were mounted onto a ballistic creases productivity. New processing methods are investigated
pendulum. Each FML panel should be weighted and the thickness for improving the productivity of curing process and decreasing
should be measured at four different points before testing. After the labour costs of FMLs. These improvements will make FMLs very
T. Sinmazçelik et al. / Materials and Design 32 (2011) 3671–3685 3683

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