The Effect of Mode-Mixity and Constraint in Adhesively Bonded Composite Joints

The Effect of Mode-Mixity and Constraint in Adhesively Bonded Composite Joints
Final Year Project Report Neville Lawless 06523587
UCD SCHOOL OF ELECTRICAL, ELECTRONIC AND MECHANICAL ENGINEERING BE Mechanical Engineering University College Dublin 22 Apr 2010
Head of School: Dr D. Fitzpatrick
Project Supervisor: Dr. Neal Murphy
Abstract
In this investigation the effects of mode mixity and constraint in adhesively bonded composites laminates were tested using mode I double cantilever beam (DCB), mode II end-loaded split (ELS) and mixed mode I/II asymmetric double cantilever beam testing methods. The test specimens were manufactured in-house in UCD labs from Hexcel Hexply 8552 composite material with a Henkel Hysol EA 9895 peel ply and bonded using a two part experimental Epoxy adhesive, Hysol EA9830.05.
In attempts to attain cohesive failure, to characterize the adhesive properties, differing surface preparation techniques were tested. These being the use of a peel ply, abrasive blasting and plasma treatment. An investigation was also carried out on the effects obtained from the use of a scrim cloth used for bondline thickness control. It was shown conclusively that scrim cloths give an average increase of 94% on the value of fracture toughness GIC. This was only displayed in DCB tests and cannot be proved for other mode mixities. Also shown was that although certain levels of grit blasting increase fracture toughness, this cannot be repeated to any acceptable standard. Finally for mode I DCB specimens it has been demonstrated that the use of a plasma treatment in nearly all cases resulted in a minimum doubling effect on the mean G IC values. All these results were compared with a control batch prepared using only a peel ply. From this it is shown that the incorporation of the peel ply sets a high level of repeatability for all tests carried out, however, along with this it sets a lower bound on toughness levels attained.
Following this, the investigation into differing mode mixities provides a good insight into the effect each loading mode has on fracture toughness. An increase of phase angles from 18 o40o63o achieved by varying adherent thicknesses resulted in a significant decrease in mean toughness values for each batch. Finally, data was generated from mode I, mode II, and mode I/II from 3 similarly prepared batches and the dramatic rise in fracture toughness mode II demonstrates over the others was displayed. The effects of the contribution of each loading mode are made apparent for mixed mode loading conditions with the use of a failure envelope being constructed.
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Table of Contents
Abstract ...................................................................................................................................... ii Project Specification ................................................................................................................ vii 1. 2. Introduction ........................................................................................................................1 Modes of Failure .................................................................................................................3 2.1 2.2 2.3 3. 4. Mode I .........................................................................................................................3 Mode II ........................................................................................................................7 Mixed Mode (I/II) ...................................................................................................... 10
The effect of constraint on fracture toughness ............................................................... 14 Failure of Adhesive joints ................................................................................................ 15 4.1 4.2 4.3 Cohesive fracture ....................................................................................................... 15 Interfacial fracture...................................................................................................... 15 Other types of fracture ............................................................................................... 16
5.
Specimen Manufacture .................................................................................................... 18 5.1 5.2 5.2.1 5.2.2 5.2.3 5.2.4 5.2.5 5.2.6 5.3 5.3.1 5.3.2 5.3.3 5.3.4 5.4 5.4.1 5.4.2 Materials .................................................................................................................... 18 Composite Specimen production ............................................................................... 19 Pre-Preg Composite Layup: ................................................................................... 19 Press-clave build-up and de-bulking: ..................................................................... 19 Peel-Ply addition: .................................................................................................. 21 Press Clave build-up: ............................................................................................. 21 Curing: ................................................................................................................... 22 Machining .............................................................................................................. 25 Surface Treatments .................................................................................................... 27 Peel Ply .................................................................................................................. 27 Abrasive Blasting .................................................................................................. 28 Plasma Treatment .................................................................................................. 29 Scrim Cloth............................................................................................................ 29 Preparation of DCB specimens .................................................................................. 30 Bonding specimens: ............................................................................................... 30 Finishing: ............................................................................................................... 33
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6.
ELS test rig manufacture ................................................................................................. 35 6.1 6.2 CAD Drawings .......................................................................................................... 35 Rig manufacture ......................................................................................................... 37
7.
Experimental procedures ................................................................................................. 40 7.1 7.2 7.2.1 7.2.2 Test methodology ...................................................................................................... 40 Testing approach ........................................................................................................ 44 Mode I DCB tests. ................................................................................................. 44 Mixed mode tests. .................................................................................................. 46
8.
Beam theory analysis ........................................................................................................ 47 8.1 8.2 8.3 8.4 Mode I DCB tests ...................................................................................................... 49 Mode II ELS test ........................................................................................................ 49 Mixed mode ADCB test............................................................................................. 50 Correction factors ...................................................................................................... 50
9.
Results & Discussion ........................................................................................................ 52 9.1 9.2 9.3 9.3.1 9.3.2 Loaddisplacement behaviour ................................................................................... 52 Crack initiation values of G IC .................................................................................... 53 Mean crack propagation values of G IC ...................................................................... 54 Mode I Results. ...................................................................................................... 55 Mode-mixity results ............................................................................................... 65
10. Conclusion ......................................................................................................................... 70 11. Appendix ........................................................................................................................... 73 11.1 11.2 11.3 Mode I GIC Initiation values ....................................................................................... 73 Mode I GIC Mean propagation values ........................................................................ 76 Mixed mode GIC mean propagation values. ............................................................... 77
12. Acknowledgments ............................................................................................................. 81 13. References ......................................................................................................................... 82
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Table of figures
Figure 1: Schematic of the double cantilever beam specimen used for mode I testing, load blocks can be used for the load introduction [] .......................................................... 4 Figure 2: DCB experimental setup..................................................................................... 5 Figure 3: Indication of mode II (In-plane) fracture............................................................ 7 Figure 4: Schematic diagram of various mode II delamination test methods [12]. ........... 8 Figure 5: The mode II ELS delamination specimen held in the clamping fixture. ............ 9 Figure 6: Schematic of MMB test configuration. [20] ..................................................... 10 Figure 7: Illustration of the mixed-mode end loaded split test specimen: (a) for short crack lengths and (b) for long crack lengths [25]. ........................................................... 12 Figure 8: Alternative MMELS test rigs with sliding clamped end and fixed load point [25]. .................................................................................................................................. 13 Figure 9: Crack tip stress fields constrained by adherents. .............................................. 14 Figure 10: Cohesive fracture. ........................................................................................... 15 Figure 11: Interfacial failure ............................................................................................ 15 Figure 12: Interfacial fracture surface. Adhesive remains fully bonded on top beam. .... 16 Figure 13: Fracture with crack jumping present. ............................................................. 16 Figure 14: Crack jumping from one interface to another................................................. 17 Figure 15: Press clave with breather fabric showing vacuum holes. ............................... 19 Figure 16: Bagging film and Debulking tape. .................................................................. 20 Figure 17: Vacuum generator........................................................................................... 20 Figure 18: Press clave layup. ........................................................................................... 21 Figure 19: Hydraulic press. .............................................................................................. 22 Figure 20: Air compressor ............................................................................................... 23 Figure 21: Thermocouples in place in the hydraulic press. ............................................. 24 Figure 22: Temperature control system. .......................................................................... 24 Figure 23: Temperature control settings for curing composites. ..................................... 25 Figure 24: Tile Cutter. ...................................................................................................... 26 Figure 25: Respiratory facemask. .................................................................................... 26 Figure 26: Wet peel ply EA 9895 used over the course of this investigation. ................. 27 Figure 27: Grit blaster in UCD labs with close up of nozzle. .......................................... 28 Figure 28: Scrim Cloth. .................................................................................................... 29 Figure 29: Dispensing gun with mixing nozzle. .............................................................. 30 Figure 30: Specimens secured in bonding jig. ................................................................ 32 Figure 31: Bonding Jig after curing with lid still attached............................................... 32 Figure 32: 2 part adhesive dispenser for bonding loading blocks to specimens. ............. 33 Figure 33: Finished DCB specimen. ................................................................................ 34 Figure 34: Callipers (top) & Micrometer (bottom) .......................................................... 34 Figure 35: Test piece clamp. ............................................................................................ 36 Figure 36: Construction drawings. ................................................................................... 36 Figure 37: Finished model with selected material finishes. ............................................ 37 Figure 38: Vertical-turret-3-axis-milling-machine .......................................................... 38 Figure 39: Completed ELS test rig................................................................................... 39 Figure 40: Macro to record crack propagation values. .................................................... 41
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Figure 41: Macro which generates values for time corresponding to force and displacement..................................................................................................................... 41 Figure 42: Excel spreadsheet used for GIC calculations. .................................................. 42 Figure 43: Test area setup. ............................................................................................... 43 Figure 44: Delamination under general loading []. ......................................................... 47 Figure 45: A typical loaddisplacement trace for a DCB joint. ...................................... 52 Figure 46: Initiation values indicated on P vs. d graph. ................................................... 53 Figure 47: Mean GIC propagation values for 3 methods of analysis. ............................... 54 Figure 48: Effect of scrim cloth on load displacement diagram. ..................................... 56 Figure 49: Visible tearing of scrim cloth after testing. .................................................... 56 Figure 50: Effect of scrim on various surface treatments. ............................................... 57 Figure 51: Micro voids seen with scanning electron microscope. ................................... 59 Figure 52: Effect of scrim with Heavy grit blast.............................................................. 60 Figure 53: Effect of scrim with light grit blast. ................................................................ 60 Figure 54: Effect of scrim with plasma treatment. ........................................................... 61 Figure 55: Effect of scrim with no peel ply. .................................................................... 63 Figure 56: Mean fracture toughness values for differing bondline thicknesses............... 64 Figure 57: Mean Fracture toughness values..................................................................... 66 Figure 58: Fracture surfaces for differ mode mixity ........................................................ 68 Figure 59: Mode I and Mode II fractions of mean fracture toughness versus Mode Mix ratio. ................................................................................................................................. 68 Figure 60: Failure envelope for the effects of scrim cloth on fracture toughness............ 69 Figure 61: Control batch J09 with peel ply. ..................................................................... 76
Table 1: Rig parts list. .............................................................................................................................. 37 Table 2: Rig cutting list. .......................................................................................................................... 38 Table 3: Control batch mean fracture toughness initiation values (M/J2). ................................................. 73 Table 4: Heavy grit blast mean fracture toughness initiation values (M/J2). .............................................. 73 Table 5: Light grit blast mean fracture toughness initiation values (M/J2). ................................................ 74 Table 6: Plasma treated mean fracture toughness initiation values (M/J2). ................................................ 74 Table 7: Samples without peel ply mean fracture toughness initiation values (M/J2). ................................ 75 Table 8: Control batch mean fracture toughness propagation values (M/J2). ............................................. 76 Table 9: Heavy grit blast mean fracture toughness propagation values (M/J2)...........................................76 Table 10: Light grit blast mean fracture toughness propagation values (M/J2). ......................................... 77 Table 11: Plasma treatment mean fracture toughness propagation values (M/J2). ...................................... 77 Table 12: No peel ply mean fracture toughness propagation values (M/J2). .............................................. 77 Table 13: 18o mean fracture toughness propagation values (M/J2). ........................................................... 77 Table 14: 18o with scrim mean fracture toughness propagation values (M/J2)...........................................78 Table 15: 63o mean fracture toughness propagation values (M/J2). ........................................................... 78 Table 16: 63o with scrim mean fracture toughness propagation values (M/J2).......................................... 78 Table 17: 40o with scrim mean fracture toughness propagation values (M/J2). ..........................................79 Table 18: Mode II with scrim mean fracture toughness propagation values (M/J2). .................................. 79 Table 19: Mode I with scrim mean fracture toughness propagation values (M/J2). .................................... 79 Table 20: Fracture toughness values for %GII ......................................................................................... 80 Table 21: Fracture toughness values with no scrim partitioned into each loading mode. ........................... 80 Table 22: Fracture toughness values with scrim partitioned into each loading mode................................. 80
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Project Specification
This project intends to focus on so-called secondary bonded joints, where the composite panels are first cured and cut into specimens of the required size. The adhesive joint is then carefully produced using a state of the art epoxy adhesive, and cured separately. This shall be further discussed later in the review of works. An important prerequisite in the use of these composite joints is an understanding of their fracture properties under mixed-mode loading conditions.
In the context of fracture mechanics, tensile opening of the crack faces is termed Mode I and shear loading is termed Mode II. One of the aims of this project is to examine the effect of mode-mixity (the combination of tensile and shear loading) on the fracture toughness of secondary bonded composite joints.
In addition, ongoing research in the UCD adhesives group has shown that the fracture toughness of epoxy adhesives often varies with the thickness of the bondline itself, so that when a thicker layer of adhesive is used, the fracture toughness appears to increase. The second aim of this project is to investigate this effect for the secondary bonded composite joints.
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1.
Introduction
Research of Adhesively bonded composite laminates has been an area of great interest to the aeronautical sector in recent times. This is primarily due to the importance that weight reduction holds in aircraft design. As a result of this, the replacement of traditional materials such as aluminium with composites is becoming more commonplace. Primarily due to them having high specific strengths whilst also being lightweight. Their growth is more evident in the military area where funding for research and maintenance is more widely available. The use of epoxy adhesives as a method of joining materials has also numerous benefits over other such methods. These include better resistance to fatigue because of the lack of stress concentrators around rivet holes. This is particularly evident in thin sheet metal encountered in aircraft manufacture. As the use of adhesives is still in its infancy in terms of fastening, the primary structural components of aircraft are still bolted and shall remain as so for some time to come.
Nonetheless, the performance of adhesively bonded composites still needs to be rigorously tested before they can be put to use in working conditions. Already, significant investment has been made in the development of standardised test protocols for the determination of the fracture toughness of structural adhesive joints under a variety of loading conditions
It is hoped that this investigation will serve as a guide to understand the methods currently available and under development with regards to adhesively bonded composite testing. With this in mind, the main aspects of the literature review will focus on papers concerned with the experimental testing of the delamination resistance of composites and critically comparing the methods that are currently in practice, whilst avoiding computer modelling techniques where possible.
In the following sections, the different modes of loading that when applied cause delamination and fracture to occur will be reviewed and surmised. These being; tensile opening (Mode I), shear failure (mode II) and the main focus of this work Mode-Mixity (Mode I/II). Also to be included is a review of work done in the area of constraint due to the effect of bond-line thickness.
2.
2.1
Modes of Failure
Mode I
Current international standards for mode I (opening mode) fracture testing of composite materials set in 2001 typically incorporate the Double Cantilever Beam (DCB) specimen geometry [1]. This is, in most regards modelled on the test protocol set out by the American Standards for Testing and Materials (ASTM) [2]. Mode I (opening mode) type failure, of composites is called delamination and can arise from internal defects like cracks or contaminants in the pre-preg layup or inadequate pressure being applied during curing. This can then cause debonding of 2 adjacent plies if subjected to a tensile force. If delamination occurs, the specimens resistance to further loading, damage and fatigue can be drastically affected. By performing Mode I tests on DCB specimens, delamination can be achieved and a linear elastic fracture mechanics (LEFM) approach can be taken to determine results for the delamination resistance or energy release rate GI. In practice this would be considered to be the most common mode of failure and so its understanding is of paramount importance. A review was carried out by Davies et al [3] in 1998 of the methods that were being widely used for testing. This comprehensive review is an indication of the amount of work needed to produce working standards and the difficulties such a challenge creates. The Double Cantilever Beam method was chosen for its relative simplicity, both in testing and analysis. Test specimen manufacturing, which will be further described later in this work, is also of a simpler nature than other methods, although the procedure is still relatively time consuming. The DCB test was initially introduced by Ripling et al. [4] as a means to measure the fracture toughness structural bonds between metallic substrates. From this work, an ASTM standard was published in 1973 [5].
A rotation factor was used to correct for rotation at the built in end and then with further research done, [6] it was adapted to act as a beam on an elastic foundation, and correction factors for load blocks and large displacements introduced.
The double cantilever beam shown in Figure 1, contains a thin film of PTFE, recommended in the standards to be less than 13 microns thick. This is used to give a point for crack initiation. The DCB specimens are fitted with loading blocks as shown below and connected to a tensile testing machine using pin-jointed clevis grips, or piano hinges. This ensures that there is a force acting only in the vertical direction on the loading blocks. A load is applied with the tensile machine to cause crack initiation and once this has propagated to 5mm the load is removed. A travelling microscope is used to monitor crack growth.
Figure 1: Schematic of the double cantilever beam specimen used for mode I testing, load blocks can be used for the load introduction [7]
The test is then carried out at quasi-static cross-head displacement rates of between 1 & 5 mm/min. [8]
Figure 2 below indicates the tensile load being applied.
Figure 2: DCB experimental setup
In recent years, the majority of research and work being carried out in the area of mode I failure has been gathering data on the applicability of the standards to various different material types other than carbon/glass fibre composites that are growing in use and variety. For the scope of this investigation and the extent to which they could be applied to this work it was deemed unnecessary that they be included.
Rather, the aspect of mode I delamination resistance testing here that is more applicable, would be of composites manufactured using multi-directional layups. At the time of writing these are not covered under International standards [1] due to the tests being invalidated because of problems that occur due to crack branching and other factors such as specimens becoming de-laminated away from the adhesive plane. In 1999 Choi et al, [9] carried out an assessment on this and should be referenced to for further background on the matter. Zemck [10] in 2008 concluded that it is reasonable to consider the critical energy-release rate GIC value as the inter-laminar fracture
toughness in the case of the delamination of a composite with transversely oriented fibres. If one is to follow the standards to achieve the delamination resistance by DCB test means on cross-ply laminates it is only allowable for crack initiation values of toughness. De Morais [11] observed that initiation values were found to be higher in his case but the underlying reasons are not fully understood at present. Realistically it would be desirable to use adhesively bonded composites with multidirectional fibres over ones with unidirectional orientations but as of yet, until standards can be established, the use of unidirectional composites can be seen as the lower limit of attainable toughness and strength.
2.2
Mode II
Mode II (In plane shear) fracture (Figure 3.) occurs when a material is subjected to a shear stress. As with Mode I, this causes delamination with composite materials which then leads to failure. Again a fracture mechanics approach can be employed to determine results for fracture toughness GIIC. As has been seen in the previous section, there has been significant progression of the Mode I DCB test method to international standards in 2001. Surprisingly this has not also been the case for Mode II delamination test methods as of yet.
Figure 3: Indication of mode II (In-plane) fracture.
A paper published by Davies et al [12] gives a thorough review of the four methods most widely used for the determination of Mode II fracture toughness. These being the end notched flexure (ENF) test, the stabilised ENF test proposed by the Japanese industrial standards group, the end-loaded split (ELS) test and a variant on a four-point loaded ENF (4-ENF) test proposed by Martin et al [13]. Figure 4 shows simple free body diagrams of all four.
Figure 4: Schematic diagram of various mode II delamination test methods [12].
The reason for Mode II test methods being slow to reach standardised levels is not due to a lack of research, of which there is an extensive level carried out previously [14, 15, 16], but rather to complications that have arose in the testing area. The ENF test makes use of a 3 point bending method which yields unstable crack propagation and so can only be used to achieve crack initiation values. The stabilised ENF is also deemed unfit to be standardised as it is too complex as a test method. The reason being, it requires the input of real time crack shear displacement values to control the loading of the specimen [14]. The remaining methods, ELS and 4-ENF are both stable and they utilize relatively simple apparatus. So it is possible that either could be standardised at some point in the future. For this investigation into mode-mixity an ELS test rig (Figure 5) was manufactured, with the intention that it could be used for both mode II and mixed mode tests.
This method has been used comprehensively by the European Structural Integrity Society (ESIS), Technical Committee 4 (TC4) on polymers and composites in a round robin [14]. The specimen preparation used is the same as that used for Mode I DCBs and shall be discussed in a later section. It has been shown in a publication by A.J. Brunner [17], that on comparing the GIIC initiation values from pre-cracking, the mode I method of precracking gave more conservative fracture toughness values when compared with the mode II method. This suggests that mode I pre-cracking should be considered over the mode II approach. More research is needed in this area as of yet.
Figure 5: The mode II ELS delamination specimen held in the clamping fixture.
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2.3
Mixed Mode (I/II)
The main focus of this review is to investigate the current status of mode mixity delamination testing in adhesively bonded composites. A paper published by Reeder et al [18] gives a comprehensive evaluation of methods used at that time for mode mixture experiments. In this, the reader is also presented with the Mixed mode Bend (MMB) test, shown in figure 6, which upon further modification formed the basis of the 2001 ASTM standard [19] method for the determination of mixed mode I/II interlaminar fracture toughness of unidirectional fibre-reinforced polymermatrix composites.
Figure 6: Schematic of MMB test configuration. [20]
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The modification carried out was a non-linear analysis and redesign of the test to account for non-linearity brought about by the large displacements occurring during bending [20].
The MMB test is a combination of mode I Double cantilever beam and mode II End Notched Flexure tests. The test makes use of a hinge and lever to create the two load components by applying a single load at P. The mode mixture is achieved by varying the dimension of c (figure 6) along the composites span [18].
During the development of the MMB test, Reeder proposed further modifications [21] to provide an improved level of accuracy. Methods for careful checking of fixture alignment were also included as de-lamination is known to occur at the corners of the PTFE inserts. So although necessary, these provide significantly more work to be carried out when performing the tests. A final complication that can arise, which was remedied by Chen et al. [22] is that if the arm applying the load to the specimen approaches over 3% of the specimens weight, this can influence the value of the toughness. This suggests that the design of the MMB test rig can be problematic. So with this and the high level of inaccuracies that can abound, other test configurations have been considered. One such configuration is the mixed-mode end loaded split delamination test setup. As with the Mode I delamination of composites, the applicability of laboratory condition experiments in the MMB test, to in-service situations is limited. This is due to the layup arrangement, specimen thickness, curves or tapers on the component or any combination of complications. These will all contribute to delamination growth (if it is to occur) that can vary with the crack length along the specimen. In this case a variation of the mode mixity will become evident and a test such as the MMB cannot encompass it whilst the MMELS can.
Kinloch et al [23] has contributed a great deal of research towards this test method and would be considered most relevant to this subject matter. The approach taken by
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Kinloch is that of a beam theory one, using an analysis which was formulated by Williams in his famous work [24].
The MMELS test, seen here in figure 7 is similar to the DCB test but only one adherent is put under load.
Figure 7: Illustration of the mixed-mode end loaded split test specimen: (a) for short crack lengths and (b) for long crack lengths [25].
As the crack initiates the deflection of the beam can be seen to change. While the crack length (a) is small, the deflection is the same in both adherents, but as the crack extends, the deflection of the lower beam approaches zero (Unloaded point). As this is occurring, the value of GI/IIC increases until an asymptote value is reached. This model is more pragmatic as to what would occur in real loading situations [25]. This is why for this project, that this approach was taken. By having this model modified as suggested by Kinloch [23], to exclude axial forces when the load is applied as seen in Figure 8, it is believed to be a more appropriate model to incorporate the interlaminar crack propagation of a real composite structure as L- a decreases. [25]
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Figure 8: Alternative MMELS test rigs with sliding clamped end and fixed load point [25].
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3.
The effect of constraint on fracture toughness
The secondary aims of this project were to investigate the effect that constraint has on the fracture toughness of specimens. It has been shown by C. Yan et al [26] with the use of fractography and a fracture mechanics approach into their research that the width and thickness of the adhesive layer effects stress and strain distributions in the adhesive. This is indicated in Figure 9 below.
Figure 9: Crack tip stress fields constrained by adherents.
A change in the adhesive layer thickness can cause a transition from small-scale yielding to fully plastic conditions. Research has shown that a linear proportionality for toughness values is found to exist due to the high level of constraint with small bond thicknesses. This then reaches a critical bond thickness, where it has been found that the toughness decreases resulting in blunting of the crack tip with loading. To fully characterise this phenomena, cohesive failure (Section 5.1) is needed in the adhesive layer. This was not achieved with initial experimental testing, so a variety of surface treatments were employed with a hope that cohesive failure would result. (Section 6.)
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4.
4.1
Failure of Adhesive joints

Cohesive fracture
Cohesive fracture is the term used when a crack propagates through the bulk of the material. When this type of failure occurs with adhesively bonded composites, the adhesive will be found to remain on both of the adherents. Cohesive fracture can occur at the centre of an adhesive layer or very near the interface. This is referred to as near interface cohesive fracture. Figure 10 gives an indication of this type of failure.
Figure 10: Cohesive fracture.
4.2
Interfacial fracture
This type of fracture occurs when the adhesive debonds from the adherents. On inspection of the failure surface, adhesive should only remain on one of the adherents. Interfacial failure is usually associated with the adhesive having lower fracture toughness. Figure 11 shows this schematically.
Figure 11: Interfacial failure

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Figure 12 indicates the types of interfacial failure experienced after testing was carried out in UCD labs.
Figure 12: Interfacial fracture surface. Adhesive remains fully bonded on top beam.
4.3
Other types of fracture
Mixed fracture types: Occur where the adhesive can be failing cohesively and then jumps to one of interfaces. The alternating crack path type: Occurs if the crack jumps from one interface to the other. Figure 13 gives a schematic of this and Figure 14 shows the occurrence of this after testing.
Figure 13: Fracture with crack jumping present.

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Figure 14: Crack jumping from one interface to another.
It has also been seen that the adhesives fracture toughness can have a much higher value than that of the bonding substrate. This can cause failure of the adherent, termed interlaminar failure and is a highly undesirable form of failure.
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5.
Specimen Manufacture
As this project involves working with adhesively bonded composites, it was a requisite to be able to manufacture carbon fibre composite specimens. This process is a lengthy one with an associated learning curve due to the numerous components involved.
The first step was to produce high quality aero grade composite panels for delamination resistance testing.
5.1
Materials
Composite prepreg sheets:
Hexcel Hexply 8552 /37%/46364/C. Fibre material is Tenax HTA type 3, class 2, style 6k-135-5H. (6k =6000 fibres/tow, 135= cured ply thickness .0135"approx, 5H = 5 harness satin weave).
Peel ply: Henkel Hysol EA 9895 Peel Ply. Adhesive:
Henkel Hysol EA9830.05.
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5.2 Composite Specimen production

5.2.1 Pre-Preg Composite Layup:
Cut to size sheets of the Hexcel pre-preg were layered with weaves on each facing the same directions following removal of the protective film. Five layers in total were used with the top and bottom films being left on till removal was necessary prior to curing.
5.2.2
Press-clave build-up and de-bulking:
PTFE film was placed on the press-clave followed by a release layer to provide a good textured surface which let the layup be removed easily. Next the Composite layup was placed, with a breather layer to cover it. This needed to cover the vacuum holes so that a vacuum can be drawn evenly over the whole surface area.
Figure 15: Press clave with breather fabric showing vacuum holes.
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De-bulking tape was then attached to the periphery of a clear plastic bagging film and adhered to the autoclave.
Figure 16: Bagging film and Debulking tape.
The layup was then attached to a vacuum for 45 Minutes. This gives the layup a uniform thickness over the composite area before curing and also the force involved begins to bond the resin throughout the layers to provide a level of green strength before peel ply addition.
Figure 17: Vacuum generator.

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5.2.3
Peel-Ply addition:
After the layup has been removed, a peel-ply is placed on the bottom layer of the layup after its protective film had been removed. Peel-ply's are used to create a protective film on one side of the composite layup prior to bonding. This will be detailed further in section 5.3.
5.2.4
Press Clave build-up:
On the press-clave, a layer of PTFE, Release layer and PTFE again were placed. The pre-preg layup was then placed. Around this a protective dam was made with sealant tape to prevent epoxy leakage. Another release layer was then placed to provide an aesthetic finish and to prevent damage during curing. A rubber pad was used here to spread the load evenly when the breather layer was laid. The Debulking layer was again used with the sealant tape applied to the bagging film. Finally adhesive tape was also put on the edges of the press-clave so its lid would stick closed when attached and maintain the vacuum.
Figure 18: Press clave layup.
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5.2.5
Curing:
The curing process has 4 components: Hydraulic press Compressor Vacuum Heat control system.
First the vacuum hose was attached to the press-clave and a vacuum drawn. The lid was then attached and the completed layup in the press clave are all placed carefully into the hydraulic press (figure 19). The press is dropped with only its own weight being applied.
Figure 19: Hydraulic press.

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The compressor (figure 20) and thermocouples (figure 21) were then attached. Please refer to user manual for instructions. The press was then set to rise to 30 tonnes or 500 kg, taking all necessary safety precautions. The Compressor was switched on and set to 30 PSI. This keeps the vacuum in place under the bagging film as the pressure is much greater on the compressed side. When the pressure has settled at 30 PSI the vacuum hose is then removed from the vacuum. This needed to be ventilated to the atmosphere to get rid of volatile gases that are released during the curing period. The compressor was then ramped to 80 PSI to promote maximum adhesion between composite layup plies. The temperature control system (figure 22) was then set to run as shown in figure 23 and started. Prior to the press-clave being removed it is let to cool for safety concerns.
Figure 20: Air compressor

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Figure 21: Thermocouples in place in the hydraulic press.
Figure 22: Temperature control system.

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Figure 23: Temperature control settings for curing composites.
5.2.6
Machining
Samples were cut with a standard tile cutter (figure 24) to a width of approximately 25 mm. Extreme caution was needed to be taken here as the dust given off is very toxic. A full face respirator safety mask (figure 25) was used along with latex gloves and a lab coat. A generator was used to run a ventilation system to prevent particulates from leaving the lab. The finished specimens were grouped into batches according to where they lay in the initial composite layup because the placement of the vacuum holes on the press clave can affect the specimen thickness. This can be investigated further if problems occur with a batch. The specimens were then wiped clean and stored in a desiccator cabinet until the final DCB specimens were produced to prevent moisture absorption.
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Figure 24: Tile Cutter.
Figure 25: Respiratory facemask.
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5.3
Surface Treatments
Over the course of this investigation cohesive failure has been a major objective that has been strived for. It was initially aimed that having achieved this, a fracture mechanics approach could be taken towards characterizing the properties of the adhesive being employed. Initial DCB tests failed in achieving this (resulting interfacial failure) so a variety of different methods of preparing the surface to increase adhesion and encourage cohesive fracture were investigated. The following sections shall give a brief indication of the methods used. 5.3.1 Peel Ply
Peel plies are woven fabric sheets, usually made from Nylon or polyester. They are heavily used in the area of composite adhesion. They are used to create clean surfaces with a roughened texture, offering a much better surface energy which is left on the composite after its removal. This promotes adhesion and also offers a higher level of repeatability in experimental testing which is a requisite particularly in the aerospace industry.
Figure 26: Wet peel ply EA 9895 used over the course of this investigation.
27
Peel plies come in two forms, wet and dry types. Wet peel plies are referred to as so because they come pre-impregnated with a resin which cures alongside the composite adherents. Dry peel plies use the composites own resin to form the improved adhesive surface. Peel plies are only removed immediately prior to bonding. This removes some but not all of the risk of contamination such as release agents and particulates from machining affecting the adhesive. The level of contamination resulting is set with tighter bounds from the use of the peel plies.
5.3.2
Abrasive Blasting
Abrasive blasting or grit blasting as it is more commonly referred to, is a method of treating surfaces which is widely used in all manner of surface treatment applications. Grit blasting involves supplying compressed air through a nozzle which carries abrasive particulates with it.
Figure 27: Grit blaster in UCD labs with close up of nozzle.
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As grit blasting is not a very controllable method of surface preparation (unless automated), its use is not employed to any great extent in the aerospace industry due to the high level of standards that are in place. 5.3.3 Plasma Treatment
Plasma treatments are used widely in industry to improve the surface properties of all manner of objects. They are used as a means of increasing the surface energy of an object by adding functional groups to the surface of an adherent providing it with a more hydrophilic substrate for bonding. The plasma treatment used was: Helium /Oxygen (He/O2) 10 l/min: 1 l/min @ 1250W 1 pass (25s) 5.3.4 Scrim Cloth
Scrim cloths are thin woven meshes used as a method of controlling bondline thickness. They are used in the aerospace industry as a part of the layup used when joining fuselage skins which are bonded together. It was hoped for the scope of this investigation that they would provide a successful means of achieving cohesive failure in the adhesive media. Below is an SEM image of the scrim after testing. Adhesive can be seen to remain where meshes are woven.
Figure 28: Scrim Cloth.

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5.4
Preparation of DCB specimens
All specimens were dried in a vacuum oven prior to bonding being carried out. This step was taken to prevent the moisture content from affecting the test results and give a more repeatable set of conditions. The samples were placed in the oven which was then sealed and had a vacuum drawn. They were heated for 4 hrs at 40 oC and left to cool overnight with the vacuum held.
5.4.1
Bonding specimens:
Samples were placed ready to be bonded. A 2 part experimental Epoxy adhesive, Hysol EA9830.05, which was provided by Henkel, is measured out by weight. 100 parts A: 53 parts B. For a 6 specimen batch, this consisted 15 grams part A and 7.95 grams part B. This is mixed according to the user guide or is mixed using the nozzle on the dispensing gun (figure 29).
Figure 29: Dispensing gun with mixing nozzle.

30
Moments before adhesive is applied, peel plies are removed. Then a thin layer of epoxy adhesive is then applied to each beam of the specimen using a spatula. Depending on the batch, the bondline thickness can be controlled as required. This entails the use of either thin aluminium spacers or scrim cloth to be added to the adhesive to control the bondline. A non stick Teflon film was placed on one of the specimens to a length of 57.50 mm for the DCB samples or 77.5mm for the mixed mode samples. This acts as a crack initiator prior to pre-cracking. The specimens were then placed into a specially designed bonding jig (figure 30) which holds them in place. Each specimen has a rubber pad and aluminium plate placed on top and below to spread an even load over the two composite substrates. The lid was attached using M8 bolts and a torque wrench tightened these evenly to 4 Nm. This ensures adequate pressure was applied during curing. The specimens were cured at 80oC for 4 hours. The jig was let cool before removal for safety reasons.
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Figure 30: Specimens secured in bonding jig.
Figure 31: Bonding Jig after curing with lid still attached.
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5.4.2
Finishing:
Samples were then sanded using a sanding discs to remove adhesive from the sides. This would otherwise affect crack propagation. Grit blasting was used to give a rough finish to one end of samples and loading blocks so that they could be bonded successfully. Acetone was used to clean the surface of the loading block and methanol used on the composite specimen itself. Acetone can erode the carbon fibres so it was not used on the composite. Loading blocks were added using a 2 part adhesive from Henkel Locktite whish is applied using a spatula (figure 32). A thin layer is all that is necessary. These are left to set following the users guide. A watered down Tipp-ex correction fluid was painted onto one side of the specimen and tick marks were inscribed to produce a scaled ruler so that crack propagation could be followed more easily. This can be seen in figure 33.
Figure 32: 2 part adhesive dispenser for bonding loading blocks to specimens.
33
Figure 33: Finished DCB specimen.
Finally 3 widths and thicknesses were measured using a micrometer and callipers (figure 34) so they could be used during calculations. These are recorded in the joint manufacturing log book.
Figure 34: Callipers (top) & Micrometer (bottom)
34
6.
ELS test rig manufacture
Concurrently whilst learning the procedure of composite specimen production, the ELS test rig was being modelled using a computer aided design package and then manufactured in the school workshop. Prior to this investigation, the school of engineering in U.C.D did not have the means to carry out mode II and mixed mode testing on composite materials, so this needed to be remedied. This test rig concept which has been now been constructed was designed by Joseph Mohan (U.C.D. Postgraduate student 2010). The test rig is intended to be used for both Mode II and Mixed mode tests which are described in section 3.
6.1
CAD Drawings
Having received designs of the ELS test rig the next step was to prepare a computer model so the design could be fully visualised prior to manufacture in a bid to avoid problems when machining each component. This was done using Pro/ENGINEER Wildfire 4.0 cad package. This was done in 3 steps. Rig base Test piece clamp Linear rail & Bearing
The linear rail design in use was available for download off a reputable CAD component website and the other components were designed. These were then all assembled so engineering drawings could be produced following this.
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Figure 35: Test piece clamp.
Figure 36: Construction drawings.
36
Figure 37: Finished model with selected material finishes.
6.2
Rig manufacture
Firstly a parts list was needed to be drawn up so parts could be sourced. It was decided that stainless steel would be the best choice as it is strong, heavy and durable. A strong material was needed so as not to incorporate a high level of compliance into the system during testing. This will be detailed in later sections.
Rig Clamp Flat stainless steel Part A Part B Rig Base Flat stainless steel Part A Part B 80 x 68 x 25mm 80 x 68 x 25mm 250 x 70 x 25mm 160 x 70 x 25mm
Bolts
Rig Clamp
4 x M8 4 x M10
Rig Base Table 1: Rig parts list.
3x M15
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Next a plan for machining the stainless steel parts was formed.
Rig Clamp Flat stainless steel Part A Part A Part B Part A Part B 2 x 10mm channels milled 4 x 6.4 mm through holes drilled 4 x 6.4 mm through holes drilled 4 x 8.4 mm through holes drilled 4 x 14.5 mm holes to 8mm drilled
Rig Base
Flat stainless steel
Part A Part A Part B Part B
1 x 16mm through hole drilled 3 x 14.5mm bore to 8mm drilled 3 x 8.4mm through hole drilled 3 x 8.4mm drilled and tapped
Table 2: Rig cutting list.
Finally the test rig was machined mainly using a vertical turret 3 axis milling machine, similar to that in figure 38 in the school workshop, under the supervision and guidance of the workshop technicians. This was not without its problems as stainless steel is difficult to machine and slower cutting speeds were needed to avoid damage to the cutting tool and the work piece.
Figure 38: Vertical-turret-3-axis-milling-machine

38
The completed ELS test rig can be seen below in figure 39 which has been used to carry out successful mode II and mixed mode delamination tests.
Figure 39: Completed ELS test rig.
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7.
7.1
Experimental procedures
Test methodology
Under the scope of this investigation, all tests (Mode I DCB, Mode II and Mixed mode I/II) tests were carried out using a Hounsfield H50KS tensile testing machine.
A 1 KN load cell was attached by a screw to the cross-head.
Clevis grips which hold the DCB samples were attached on the top and bottom with pins and the sample put into place also held with pins. This ensured that there was only tensile force in the vertical direction acting on the loading blocks.
A travelling microscope and halogen lamp were positioned so that crack propagation could be observed with a higher level of accuracy.
QMAT software was run on the PC to take readings; force (P) and displacement (d), from the Hounsfield machine. Prior to testing the load and displacement were zeroed to prevent errors.
The test was set to run with a displacement controlled rate of between 1mm/s - 5mm/s. As specified in international standards. [1] When the test was initiated, a macro (figure 40) ran simultaneously on Microsoft excel. This was used in a stopwatch manner. As the propagating crack passed each distance on the scale which was previously inscribed on the specimen side, the crack length (a) was entered into the sheet and a time was recorded automatically. Once the pre-crack reached a distance of 5 mm the test was stopped and the specimen was released from tension. The test was then repeated till a crack length of 65mm was achieved. Raw data stored in QMAT was then cleaned up and added into the excel spreadsheet. The crosshead speed was entered and another macro was run (figure 41), this calculated
40
the load for every instance of crack length. This data was used on another excel spreadsheet (figure 41) [277] to produce results for fracture toughness and other data used to characterize the specimens.
Figure 40: Macro to record crack propagation values.
Figure 41: Macro which generates values for time corresponding to force and displacement.
41
Figure 42: Excel spreadsheet used for GIC calculations.

42
Figure 43: Test area setup.
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7.2
Testing approach
Due to the large amount of data to be presented, a systematic approach was taken to its organisation. This involves two main groupings:
Mode I DCB tests Mixed mode tests
These were further grouped into batches represented with a J xx format (where xx indicates a numerical order).
It was planned that a comparison between fracture toughness values should be made concurrently with the surface treatments investigation and the effect of scrim cloth used to control bondline thickness. This is used in both the Mode I DCB tests and the mode mixity investigation.
7.2.1
Mode I DCB tests.
As explained previously, this investigation was initially concerned with achieving cohesive failure in specimens whilst varying the bond thickness from batch to batch. Preliminary tests indicated that without a surface treatment, this was not going to occur.
Overleaf shows the different surface preparation methods used on each batch. All batches bar J 09 compare the effect of scrim vs. no scrim cloth.
44
J 09: o
Control batch. No scrim. All peel ply. J 09 A-L 0.15mm Bondline thickness All specimens received no surface treatments
J 12: o o
Heavy grit blast. J 12 A-C 0.15mm Bondline thickness No scrim cloth. J 12 D-F 0.15mm Bondline thickness Scrim cloth.
J 13: o o
Light grit blast. J 12 D-F 0.15mm Bondline thickness No scrim cloth. J 12 A-C 0.15mm Bondline thickness Scrim cloth.
J 15: o o
Plasma treated. J 15 A-C 0.15mm Bondline thickness No scrim cloth. J 15 D-F 0.15mm Bondline thickness Scrim cloth.
J 16: o o
No Peel ply used. J 16 A-C 0.15mm Bondline thickness No scrim cloth. J 16 D-F 0.15mm Bondline thickness Scrim cloth.
J 17: o o
0.25 mm bondline samples J 17 A Scrim cloth No plasma treatment J 17 D Scrim cloth Plasma treated.
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7.2.2
Mixed mode tests.
J 11: 5/9 & 9/5 ply layup. o Lightly grit blasted. 0.15mm bondline thickness. o J 11 A-C
5/9 ply layup No Scrim cloth.
o J 11 D-F
9/5 ply layup No Scrim cloth.
o J 11 G-I
5/9 ply layup Scrim cloth.
o J 11J-L
9/5 ply layup Scrim cloth.
J 14: All with: o 7/7 ply layup. o Lightly grit blasted. o 0.15mm bondline thickness. o Scrim o J 14 A-D o J 14 E-H o J 14 I-L
Mixed Mode Mode II Mode I
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8.
Beam theory analysis
For the determination of inter-laminar fracture toughness (GIC) there were two sets of calculations that were employed. These made use of two theories, Simple beam theory (SBT) and corrected beam theory (CBT). The reasons for this shall be discussed further in this work. All the calculations and explanations surmised here are drawn from a thesis [27] by the authors supervisor which heavily influenced this project. In turn all these are from famous works by Williams on interlaminar fracture toughness [28,29]. Williams work was intended towards the failure of laminated composites; however the theory can be applied directly in calculations to the case of adhesively bonded composites that have small bondline thicknesses.
Figure 44: Delamination under general loading [30].

47
The strain energy release rate (G), was first found in a generalised form:
(1)
B= Specimen Width (m) E= Youngs modulus of substrate (Pa) I = Second moment of area M= Bending moments associated with each adherent = h1/2h I = (Bh3/2h) (2)
This was then partitioned into the separate modes I and II where:
G= G1+G2
(3)
And
(4)
Where:
(5)
Having done this, they can be applied to the separate modes to get critical values for the fracture resistance GC.
48
8.1
Mode I DCB tests
From symmetry in the DCB specimens h1=h; so =1/2. Also M is the moment applied in each arm. Here M1=M2 Where MI = (P a) MII = 0 Applying this to equations 4 yields the Mode I fracture toughness: (load by crack length in a simple beam).
(6)
8.2
Mode II ELS test
The same methodology is applied here. The specimens contain adherents of equal thickness: h1=h; so =1/2. However in this case, the applied load in the positive Y direction is applied to the 2 beams. This gives: M1=-M2= (P *a)/2
Again applying this to equations 4 yields the Mode II fracture toughness:
(7)
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8.3
Mixed mode ADCB test
The details of the ADCB calculations are of a more detailed nature due to the different adherent thicknesses. The reader shall again be referred to the works of Williams for a more fruitful insight. (8)
(9)
With a phase angle of: (10)
8.4
Correction factors
As has been mentioned already, there are two approaches to achieving figures for our delamination results, the Simple Beam Theory and Corrected Beam Theory. In Beam theory it is known that any displacements are considered to be infinitesimal. This is not the case with any of the tests carried out, so corrections need to be applied to the set of equations for GC. The load correction factor F is used to settle the irregularities which occur. Next is the loading block correction factor N. This is necessary because of the shape of the loading block which causes a moment due to the stiffening of the section of beam adhered to the loading block. Ideally a point load should exert the force but this cannot be done practically.
50
The loading block correction factor can also accounts for the root rotation which occurs because the beams are not fully built in. These two correction factors are employed in the CBT analysis but not in the SBT analysis. Along with this, the experimental compliance method (ECM) is used as a means of comparison. The variations between SBT and CBT will become apparent in later sections. For now it is only necessary to note that both these equations are used in the excel spread sheets [27] used for calculation of fracture toughness and so are not approached here due to the level of complexity.
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9.
9.1
Results & Discussion

Loaddisplacement behaviour
Load displacement graphs were generated for every test carried out. These simply plot the applied load against the crosshead displacement during the test. Figure 44 shows both the insert stage (red) where the specimen is being pre-cracked and its unloading line, and also the reloading stage (blue) where crack propagation is observed for the remainder of the test. This region gives the mean fracture toughness values GIC Close inspection of the graph indicates non linearity in the very early stages of loading. The occurrence of this is expected due to the crosshead taking up slack in the specimen prior to it taking up the load. This is remedied by setting a limit on the excel spread sheet within the bounds of the linear region which occurs prior to crack propagation. The slope of this region is calculated and the intercept value used to re-set the initial load to zero.
120 100 80 60 40 20 0 0.000
Force, P [N]
0.002
0.004
0.006
0.008
0.010
0.012
0.014
Crosshead Displacement, d [m]
Figure 45: A typical loaddisplacement trace for a DCB joint.
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9.2
Crack initiation values of G IC
In current ISO standards it is a requirement that the values associated with crack initiation be determined and documented for both the initial pre-cracking from the insert film and also for resulting pre-cracked stage [1]. This is required so that any influence caused by the insert film can be removed prior to analysis of the test data. The initiation values are the non-linear (NL) point, the 5% compliance value (CO 5%) and the maximum load (MAX). These are indicated in figure 46 below. On the insert stage, it is noted that the NL and MAX point coincide. These values are tabulated in the appendix in tables 3 to tables 7.
Figure 46: Initiation values indicated on P vs. d graph.
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9.3
Mean crack propagation values of G IC
Also proposed in the ISO standards [1] is the inclusion of R-curves which are generated by plotting the value of critical strain energy release rate GIC (fracture toughness) against crack length. This is required so a quick visual inspection can detect the presence of irregularities following testing. These are provided in the accompanying excel spread sheets. For a full comparison to be made between numerous batches, the mean GIC values for crack propagation are collated. These are all values arising after the 3 initiation values are determined. They are to be found in tables 8 to table 19 for all specimen batches. In this investigation, 3 methods were employed to achieve these. Simple beam theory (SBT), corrected beam theory (CBM) and the experimental compliance method (ECM). An example of these is seen in figure 47 below. It should be noted that the SBT method of analysis consistently provides values lower than the two other methods which are highly comparable. This holds with the theory mentioned in section 8 in that the lack of correction factors significantly hinders the values of fracture toughness achieved.
Figure 47: Mean GIC propagation values for 3 methods of analysis.

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9.3.1
Mode I Results.
9.3.1.1 The effect of scrim cloths The first comparison that has been made in this investigation is the effect of the scrim cloth addition as a means of controlling bondline thickness.
It has been found conclusively from a comparison of tables 9, 10, 11, and 12 in the appendix that the scrim cloth significantly increases the value of the specimens fracture toughness when used to control the bondline thickness to a better level of repeatability.
It was observed during testing that the scrim cloth acts in a large number of cases in the same manner as the fibres in composite materials when fibre bridging occurs. During testing the scrim appears to branch in a manner not unlike a cobweb when crack jumping occurs. This can be seen from the load displacement diagram (figure 48).
The region which typically falls off with standard DCB P vs. d diagrams once crack propagation begins is seen to hold at a constant value till the fibres snap. The resulting load is then too great to be held by the specimen so a dramatic drop off is encountered. The load then begins to recover towards the region where it would usually be, had scrim cloth effects not taken over. Visual inspection of the specimen (figure 49) following testing shows that the scrim maintains an attachment to one of the adherents until the applied tensile load reaches a level too great for the specimen to maintain. Tearing of the scrim is evident and there appears to be a sense of proportionality in the manner of its tearing with that of the reloading line on the graph until final failure of the specimen is reached. However this plateauing does not occur in every specimen, so one cannot say in all certainty that this is the sole cause.
55
120 100 80 Force, P [N] 60 40 20 0 0.000
0.005
0.010 0.015 Crosshead Displacement,d [m]
0.020
0.025
Figure 48: Effect of scrim cloth on load displacement diagram.
Figure 49: Visible tearing of scrim cloth after testing.
56
Figure 50 below gives a good visual indication of the dramatic effect of the use of scrim cloths on the mean fracture toughness values for crack propagation in the various batches tested. It was calculated that a mean increase of 94% was achieved by the use of a scrim cloth. This alone indicates the use of a scrim as a bondline thickness control has a major secondary benefit. The effects of scrim cloth addition on mode-mixity will be discussed in later sections.
Variation of GIC with treatment type

1000 900 800 700 600 500 400 300 200 100 0
J09 Control J12 Heavy GB J13 Light GB J15 Plasma treatment J16 No peel ply J17 .25mm bond
Fracture toughness GIC (J/M^2)
NO SCRIM
SCRIM
Figure 50: Effect of scrim on various surface treatments.
57
J09 Control Batch

For this initial batch 12 samples were tested which used a peel ply to give accurate repeatable results for the mean GIC crack propagation values. It was found that this was 193 +/- 24 J/M2 having a standard deviation of 12% with this being calculated from the mean of each value (table 8). It can be said that as a control this batch provides a satisfactory means of comparison. 9.3.1.2 The effects of grit blasting as a surface treatment Two methods of grit blasting were employed in this investigation. A heavy grit blaster and light grit blaster with finer grain sizes were used for the purposes. For an unbiased means of comparison all values will be compared to the batch J 09 (table 8). Also the specimens without scrim cloths are the only ones being considered as the use of this would not give satisfactory statistics. Visual inspection of figure 52 and figure 53 suggests that the use of both methods of grit blasting is an unnecessary step, as the results do not to appear to deviate far from the control region. A further inspection of tables 9 & 10 show the mean value for a heavy grit blast (HGB) is 217J/M2 while for the LGB is 141 J/M2. This suggests that the HGB was successful in increasing fracture toughness by increasing the surface energy of the adherent, if even not to a significant level. The interesting finding is the LGB actually decreases the mean GIC value which is surprising. The reasons for this are not yet known, however it is likely that the abrasive nature of the grit blast was sufficient to damage the peel ply interface with the substrate it was bonded to without actually removing the peel ply. Another aspect could be the fine nature of the abrasive particles, which although the sample was cleaned with methanol prior to bonding, could be still present at microscopic levels. By the use of scanning electron microscopy it was found that there were indeed voids and some particulates left in the adhesive following testing. The scope of this investigation did not permit further research but it is felt that the sizes evident in figure
58
51 might be in a range too small to represent abrasive grit. However these voids could play a role in lowering GIC values so a further study might warrant this.
Figure 51: Micro voids seen with scanning electron microscope.
59
Effects of scrim cloth on mean GIC values

700
Fracture toughness (J/M^2)
600 500 400 300 200 100 0 Batch J12

Figure 52: Effect of scrim with Heavy grit blast.
NoScrim Scrim

450
400 350 300 250 200 150 100 50 0 Batch J13

Figure 53: Effect of scrim with light grit blast.
NoScrim Scrim
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9.3.1.3 The effect of plasma treatment as a surface treatment
It has been shown successfully in this work that the use of a plasma treatment gives a significant increase of fracture toughness in all specimens. In nearly all cases there was a minimum doubling effect on the mean GIC values. From table 11 it is clear that even with the lowest mean propagation value being 352+/141 J/M2 this still yields a lower bounding value of 211J/M 2. On comparison again with table 8, (factoring out sample L as this appears to have an irregularly high value) the maximum possible value still falls slightly below the lowest value for plasma treated samples. The maximum fracture toughness reached by specimens without peel ply was 1325 J/M2. In achieving this, most of these failed with interlaminar behaviour. This indicates that the adhesive performs better than the composite substrate to which it was bonded.

1600
1400 1200 1000 800 600 400 200 0 Batch J15 NoScrim Scrim
Figure 54: Effect of scrim with plasma treatment.

61
9.3.1.4 The effect on fracture toughness without use of a peel ply For this stage of the investigation it was again hoped to achieve cohesive failure of the adhesive by performing the mode I DCB tests without the use of a peel ply. Inspecting figure 61 shows that the peel ply does in fact provide a lower bound value for fracture toughness. The average propagation value being found in table 12 for mean toughness values without peel plies is seen to have a value of 433 J/M2. Again this is providing a near doubling compared to that of the control batch.
Repeatability has been mentioned before with regards to peel plies. This investigation shows that there is a high level of associated repeatability in this case. Figure 55 has six mean values all having a sizeable standard deviation from the mean; these values are spread over a range in the region of 300 J/M2. On making a comparison with the peel ply treated samples in figure 61 it can also been seen that deviation from the mean is nowhere near as great, with these falling into a much smaller spread of about 50/60 J/M2.
Finally, it needs also to be mentioned that on further study of the associated tables for this batch it is evident that even with the presence of a scrim cloth; the value for G IC can in some cases be less than that of those with the peel ply. This is a point which needs to be noted as it indicates that errors can occur with samples and that results can deviate from the norm.
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900
800 700 600 500 400 300 200 100 0 Batch J16 NoScrim Scrim
Figure 55: Effect of scrim with no peel ply.
9.3.1.5 The effect of bondline thickness on fracture toughness
Having initially envisaged that cohesive failure would be achieved and a full investigation carried out into bondline thickness effects it has been felt that a section on this point is necessary for finality. Two samples were tested using a bondline thickness of 0.25mm as opposed to the 0.15mm thickness used for all other tests. One of these being grit blasted and the other plasma treated. It was found that the resulting mean fracture toughness values were: J17 A- No plasma: J17 D- Plasma treatment: 394.1+/-44.8 J/m2 966.7+/-392.2 J/m2.
On first inspection of these values, there seems to be no apparent significance held here and the trend, as seen with a plasma treatment before is followed, but on comparison of J17 A with the J12 batch which had identical surface preparations there is an interesting
63
point to be made. There seems to be a decrease in mean fracture toughness for the specimen with a bigger bondline. This would go against other published literature in the area of constraint. Figure 56 shows the mean toughness values for the specimens and the difference is over 100J/M2, a value which is too large to ignore as experimental error. An Inspection of the fracture surfaces once again reveals interfacial failure to have occurred. It can be justifiably argued from this that although the 0.15mm bondline specimen has a greater GIC value, this is not just a characteristic of the adhesive, but of the interface between it and the adherent. It is a known fact that a crack will propagate in the plane of least resistance and consume the least energy, so deducing from this, it can be said that the 0.25mm specimens adhesive layer could still well hold a higher fracture toughness due to constraint effects and so cause crack propagation to jump to the interface sooner than for the 0.15mm because this offers less resistance to fracture. This analogy, it is felt could possibly stand as an explanation for such unexpected behaviour.
Figure 56: Mean fracture toughness values for differing bondline thicknesses.
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9.3.2
Mode-mixity results
The effect of phase angle on fracture toughness of adhesively bonded composite has been shown to have a significant impact on the attainable levels of toughness. The results from the investigation were found to agree with literature on this area [31].
The phase angles of each type of mode mixity were calculated using equation 10 (section 8.3). The 3 mode mixtures were a 5/9 ply layup, a 7/7 ply layup and a 9/5 ply layup (the leading number being the loaded arm). These resulted in phase angles of 18o 40o and 63o respectively. Figure 57 constructed from table 13 to table 19 gives a good visual indication of the mean fracture toughness for each mode mixity. The first notable point to be considered is the effect of the scrim on these mixed loadings is not as drastic when compared with that of the mode I DCB specimens. On inspecting the test specimens after testing, it is seen that the failure type is in nearly all cases primarily interfacial when the scrim cloth is present. Without scrim there is a significant increase in cracks jumping from one interface to the other. This perhaps may be the reason for smaller variations of GI/IIC values for samples with and without scrim cloths. As has been discussed previously, and visible in figure 49, there was a visible tearing or fibre bridging of the scrim cloth in numerous mode I DCB samples, without this tearing or bridging the scrim only serves as a control on the bondline thickness. This observation could be a valuable one, as the presence of shear forces occurring due to the influence of the mode II partition in the mixed mode tests appears to affect this. Mixed mode loading is a more accurate modelling of the forces that can occur in service conditions. For instance, the oscillations of an aircraft wing with a high velocity airflow over them can give rise to mixed mode loading. In these cases, it should be taken into
65
consideration that the use of a scrim not be used to provide any functional increase of mean GIC values. The next results to be discussed are the mean GI/IIC values resulting from the different phase angles discussed above. The mean values achieved for crack propagation (table 13 to table 17) were: 334+/-103 M/J2 without scrim and 389+/-110 M/J2 with scrim for the 18o phase, 221+/-48 M/J2 with scrim for the 40o phase and, 213+/-35M/J2 without scrim and 383+/-79 M/J2 with scrim for the 63o phase. Immediately it is clear that there is an associated trend between the values of fracture toughness attained and the phase angle at which they were achieved. The mean fracture toughness values are seen to decrease with an increasing phase angle from 18-63o. This correlates well with results published from other researchers in this area.
Figure 57: Mean Fracture toughness values

66
This decreasing toughness can be partly answered with the increasing stiffness of the adherent being loaded. The type of failure in the adhesive bond tends to change with different layups. Figure 58 gives a good indication of this. The 5/9 ply layup tended to result in an alternating crack propagation whilst the 9/5 ply layup resulted in purely interfacial failure in nearly all instances. The energy required to cause crack jumping appears to give rise to increased fracture toughness in this case
The results obtained were then consolidated into their associated GI and GII partitions. These values and their standard deviations, over the range of mode mixities developed and also the mode II ELS and mode I DCB batch are presented in tables 20, 21 and 22. Figure 59 indicates the mode I and mode II fractions as a function of mode mix ratio. Again here, the dominance of fracture toughness obtained from the use of a scrim cloth is very much apparent. It is clear to be seen that the Mode II specimens result in G IIC values well above those obtained by all other test methods. This shall be discussed in more detail. Figure 59 displays the failure envelope constructed from the mode I and mode II partitions. The failure envelope encompasses the region outside which failure of the specimen shall occur. Values of fracture toughness reached which fall below the arrest values dictated by the lower bounding standard deviations from the mean will experience no crack propagation. Once these values are reached, propagation shall occur in a stable manner and then failure occurs once the limit of the envelope is reached.
67
Figure 58: Fracture surfaces for differ mode mixity
Figure 59: Mode I and Mode II fractions of mean fracture toughness versus Mode Mix ratio.
68
Figure 60: Failure envelope for the effects of scrim cloth on fracture toughness.
It has been said by thouless et al. [32] that the energy release rates associated with crack propagation in uniaxial loading are not affected by the bonding interfaces. But with the incorporation of shear forces, the effects of different mechanisms which hinder crack propagation become more evident. For this investigation this is immediately seen in figure 57 again. The mode II fracture toughness is of a significantly higher value for all tests carried out. It was found that the fracture toughness in this case reaches a value of 2026.6+/-866.2M/J2 which is an increase of over 3.5 times when compared with mode I and mixed mode tests for the same specimen layup. This can arise from any number of reasons. The main one being felt is due to mechanical interlocking between the interfaces. The maximum stress for materials in shear occurs at an angle of 45o to the surface which shear is acting along. This results in the crack attempting to propagate in this direction. It can be seen during testing with the use of a microscope that crack propagation (or branching of crack tips) tend to occur at an angle close to this before the main crack jumps forward again. This could indicate why, in figure 60 that the mode II toughness values seem to be a lot higher than would be expected if a trend line is followed from the other results.
69
10. Conclusion
On completion of this investigation into the effects of constraint and mode mixity in adhesively bonded composites joints, there have been a number of interesting findings which have been reported. Initially the effects of constraint were to be investigated but initial testing proved fruitless in achieving cohesive failure to characterize adhesive bondline properties. Various surface treatments and methods were decided upon to attain cohesive failure, but again these did not provide the results required. However, in this process a number of findings were made on the effects of these treatments on the composite specimens fracture toughness values.
The first of which was the significant impact obtained from the usage of a scrim cloth as a means of controlling bondline thickness. It was found that the fracture toughness GIC in the majority of cases for DCB specimens attained a value much higher (an average 94% increase) than that of a specimen which received the same surface preparation but without a scrim cloth being used. In the case of this comparison being made with asymmetric double cantilever beams and loading modes II and mode mixity (I/II), this increase of GI/IIC was not encountered to the same significant level. It was observed that the shear component of these modes takes away from the contribution that the scrim cloth provides to fracture toughness in pure tensile loading. As components in service conditions undergo various modes of loading, this means of bondline control is an area that further research into could benefit greatly.
A plasma treatment was then applied to increase the surface energy and wettability of the bonding substrate to improve performance. This was achieved with a dramatic increase of fracture toughness being found. Interlaminar failure was the resulting trend, leading to an outperformance of the tested adhesive over the composite specimens.
70
As a means of comparison, samples were tested initially using only peel plies as a control batch. It has been shown that these provide a high level of repeatability over large numbers of samples. This provided the platform against which all other specimens were compared against. For completeness, other samples were compared with these having no peel ply and just a roughened surface. These were shown to have a much higher mean toughness value but a much higher standard deviation and unrepeatable results. Having established the use of peel plies as a positive method of control, it would be highly recommended that further work is done on improving the adhesion mechanisms employed by these. The motive is that the peel ply sets the lower limit of fracture toughness for the components being bonded. If this lower bound can be raised then designers can be safe in the knowledge that this improvement can positively affect the fracture toughness and life of such components in service.
The final conclusion to be drawn from mode I DCB tests carried out is that there is unsubstantial evidence for the necessity of abrasive blasting to promote adhesion from scope of this investigation. It has been seen that the use of a heavy grit blast on peel ply surfaces increases the mean fracture toughness by minimal amounts and the resulting values were seen to deviate greatly from the mean. This highly suggests that this method of surface treatment is unsuitable in applications as highly controlled as the military and aerospace. Also a light grit blast was performed on peel ply surfaces to again promote adhesion. It was found from testing that this caused a decrease in mean fracture toughness below the level achieved from using peel plies alone. This suggests to the author that there was enough considerable exposure to the abrasive as to cause damage to the peel ply, but not remove it totally, as may have been achieved with the heavy grit blast. This could be the primary means of causing it to fail prematurely at a GIC value less than that of the control batch.
Finally the effects of differing mode mixities on the fracture toughness of composite specimens were studied using the asymmetric DCB and ELS method. Although the
71
ADCB method is not preferred over the mixed mode bend test as this has reached an international status, it was found that the results were in a range which was predictable and the standard deviation from the mean was small. Following this, tests were carried out on the mode II fracture toughness of similar specimens and again these resulted in values being entirely greater than those from mode I and mixed mode, as has been documented in other literature. The mean toughness values were found to lie a lot higher than anticipated and it is believed that various mechanisms including mechanical interlocking are the cause. Failure envelopes for the range of mode mixities were then established which characterize the attainable fracture toughness values for the type of specimens in question. Having achieved these successful results from all mode mixities it can be finally concluded that the design and construction of the ELS rig documented in this work was a success and can be employed for further testing in the future.
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11. Appendix
11.1 Mode I GIC Initiation values
Table 3: Control batch mean fracture toughness initiation values (M/J2).
Table 4: Heavy grit blast mean fracture toughness initiation values (M/J2).
73
Table 5: Light grit blast mean fracture toughness initiation values (M/J2).
Table 6: Plasma treated mean fracture toughness initiation values (M/J2).
74
Table 7: Samples without peel ply mean fracture toughness initiation values (M/J2).
75
11.2 Mode I GIC Mean propagation values

Control batch with peel ply
450 400 350
Mean GIC values (J/M^2)
300 250 200 150 100 50 0
Figure 61: Control batch J09 with peel ply.
Table 8: Control batch mean fracture toughness propagation values (M/J2).
Table 9: Heavy grit blast mean fracture toughness propagation values (M/J2).
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Table 10: Light grit blast mean fracture toughness propagation values (M/J2).
Table 11: Plasma treatment mean fracture toughness propagation values (M/J2).
Table 12: No peel ply mean fracture toughness propagation values (M/J2).
11.3 Mixed mode GIC mean propagation values.
NO SCRIM 5/9 ply J11 .15mm Bondline A

GIC (CBT) GIIC (CBT) GI/IIC (CBT)
18o Phase
B
C
Totals
MEAN SD CoV
369 111 30
41 13 31
410 124 30
229 62 27
25 7 28
255 69 27
307 25 8
34 3 8
341 28 8
300 93 31
33 10 31
334 103 31
Table 13: 18o mean fracture toughness propagation values (M/J2).
77
SCRIM 5/9 ply J11 .15mm Bondline A

18o Phase
B
C
Totals
MEAN SD CoV
186 26 14
20 3 14
207 29 14
292 70 24
32 8 23
324 77 24
421 44 10
47 5 11
468 49 11
351 99 28
39 11 28
389 110 28
Table 14: 18o with scrim mean fracture toughness propagation values (M/J2).
J11 .15mm Bondline A

GIC CBT GIIC (CBT)
NO SCRIM 9/5 ply 63o Phase
B
GI/IIC (CBT) GIC (CBT) GIIC (CBT) GI/IIC (CBT)
C
Totals
MEAN SD CoV
44 5 12
166 20 12
210 26 12
47 11 24
175 43 25
221 54 24
44 5 12
166 21 12
210 26 12
45 7 16
168 28 16
213 35 16
Table 15: 63o mean fracture toughness propagation values (M/J2).
J11 .15mm Bondline A

GIC CBT GIIC (CBT) GI/IIC (CBT)
SCRIM 9/5 ply 63o Phase
B
C
Totals
MEAN SD CoV
90 13 14
o
340 51 15
429 64 15
77 7 10
292 28 10
370 36 10
80 19 24
300 73 24
380 92 24
2
80 16 20
303 63 21
383 79 21
Table 16: 63 with scrim mean fracture toughness propagation values (M/J ).
78
Table 17: 40o with scrim mean fracture toughness propagation values (M/J2).
Table 18: Mode II with scrim mean fracture toughness propagation values (M/J2).
Table 19: Mode I with scrim mean fracture toughness propagation values (M/J2).
79
%GII 0 11 43 80 100
Scrim 521.865776 389.342455 221.284934 382.623025 2026.63292
SD 77.5403366 109.580374 48.2697603 79.2700826 866.268184
No scrim 196.563563 333.632255 213.132171
SD 40.371801 103.109248 34.6275973
Table 20: Fracture toughness values for %GII
No scrim
GI 196.563563 300.450412 44.7907093
GII 0 33.1818427 168.341461
SD GI 40.371801 92.6817408 7.12394516
SD GII 0 10.4301994 27.5082529
Table 21: Fracture toughness values with no scrim partitioned into each loading mode.
Scrim
GI 521.865776 350.604035 130.142416 80.1177998 0
GII 0 38.7384196 91.142518 302.505225 2026.63292
SD GI 77.5403366 98.6181348 28.4994726 16.3435207 0
SD GII 0 10.9672152 19.7788703 62.9327573 866.268184
Table 22: Fracture toughness values with scrim partitioned into each loading mode.
80
12. Acknowledgments
I would sincerely like to thank Mr Joe Mohan for his continual help and patience over the course of this project. Without his advice and guidance this investigation could not have happened. I would furthermore like to thank Dr Neal Murphy for all his help and time put into making the final year projects a success. Big thanks are also necessary to all the technicians in the UCD workshop who worked with me giving me good practical experience in the workshop and help in other design areas where needed. Finally I would like to thank all my family and friends who have supported me over the course of the final year.
Cheers, Neville.
81
13. References
1 Fibre-reinforced plastic composites determination of mode I interlaminar fracture toughness, G IC for unidirectionally reinforced materials, 15024, International Organisation for Standardisation, ISO; 2001. 2 Standard test method for mode I interlaminar fracture toughness of unidirectional fibrereinforced polymermatrix composites, D5528, American Society for Testing and Materials International, ASTM; 1994. 3 Davies P, Blackman BRK, Brunner AJ. Standard test methods for delamination resistance of composite materials: current status .Appl Compos Mater 1998; 5(6):34564. 4 Ripling EJ, Mostovoy S, Patrick RL, Measuring fracture toughness of adhesive joints. Materials research and Standards. ASTM, vol. 4, March 1964. 5 ASTM D3433, in Annual Book of ASTM standards. Adhesives section 15 Philadelphia, PA: ASTM; 1990. 6 Olsson R. A simplified improved beam analysis of the DCB specimen. Comput Sci Technol 1992; 43:329. 7 A.J. Brunner, B.R.K. Blackman, P. Davies. A status report on delamination resistance testing of polymermatrix composites. Engineering Fracture Mechanics 75 (2008) 27792794 8 Determination of the mode I adhesive fracture energy, GIC, of structural adhesives using the double cantilever beam (DCB) and tapered double cantilever beam (TDCB) specimens. British standards BS 7991:2001 9 Choi NS, Kinloch. AJ. Williams. JG. Delamination fracture of multidirectional carbon-ber/epoxy composites under mode I, mode II and mixed mode I/II loading. J Compos Mater 1999;33(1):73100 10 Zemck, Robert, and Vladislav Las. Materials and technology. Numerical and experimental analyses of the delamination of cross-ply laminates. 42 (2008): 171-174. 11 De Morais AB, de Moura MF, Marques AT, de Castro PT. Mode-I interlaminar fracture of carbon/epoxy cross-ply composites. Compos Sci Technol 2002; 62(5):67986.
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12 Davies P, Sims GD, Blackman BRK, Brunner AJ, Kageyama K, Hojo M, et al. Comparison of test configurations for determination of mode II interlaminar fracture toughness results, from
international collaborative test programme. Plast Rubber Compos1999;28(9):4327. 13 Martin RH, Davidson BD. Mode II fracture toughness evaluation using a four point bend end notched flexure test. In: Fourth International conference on deformation and fracture of composites, Manchester, 1997. 14 Blackman, B.R.K., Brunner, A.J., Williams, J.G. Mode II fracture testing of composites: a new look at an old problem (2006). Engineering Fracture Mechanics, 73 (16), pp. 2443-2455. 15 Blackman BRK, Brunner AJ, Cartier DDR. Determination of apparent Mode II interlaminar fracture toughness, GIIC, for unidirectionally reinforced composite laminates. In: ESIS TC4 Protocol, 2006. 16 Blackman BRK, Kinloch AJ, Paraschi M. The determination of the mode II adhesive fracture energy, GIIC, of structural adhesive joints: an effective crack length approach. Engng Fracture Mech 2005; 72:87797. 17 Brunner AJ. Experimental aspects of mode I and mode II fracture toughness testing of fibre-reinforced polymer-matrix composites. Comput Meth Appl Mech Engng 2000; 185:16172. 18 Reeder J. Crews J. Mixed-Mode Bending Method for Delamination Testing. AIAA Journal, 28(7), 1270-1276. (1990) 19 Standard test method for mixed mode I-mode II interlaminar fracture toughness of unidirectional fibrereinforced polymermatrix composites, D6671/D6671M. American Society for Testing and Materials, 2006. 20 Reeder JR, Crews Jr. Non-linear analysis and redesign of the mixed mode bending delamination test. NASA Technical Memorandum 102777; 1991. 21 Reeder JR. Renements to the mixed mode bending test for delamination toughness. J Compos Technol Res 2003;25(4):1915. 22 Chen JH, Sernow R, Schulz E, Hinrichsen G. A modication of the mixed-mode bending test apparatus. Compos Part A: Appl Sci 1999;30(7):8717.
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23 Kinloch AJ, Wang Y, Williams JG, Yayla P.
The mixed-mode delamination of fibre
composite materials. Compos Sci Technol 1993;47(3):22537. 24 Williams JG. On the calculation of energy release rates for cracked laminates. Int J Fract 1988;36:10119. 25 Blanco. N and M. Gamstedt. Analysis of the mixed-mode end load split delamination test. Composite Structures 76 (2006): 14-20. 26 Yan, Cheng; Mai, Yiu-Wing; Ye, Lin. Effect of Bond Thickness on Fracture Behaviour in Adhesive Joints. The Journal of Adhesion 75.1 (2001). 14 Apr. 2010 27 J. Mohan, An investigation into composite to composite adhesive bonding. PhD thesis, University College Dublin, 2010. 28 S. Hashemi, A. J. Kinloch, and J. G. Williams. The analysis of interlaminar fracture in uniaxial fibrepolymer composites. Proceedings of the Royal Society of London, 427:173199, 1990.
29 J. G. Williams. The fracture mechanics of delamination tests. Journal of strain analysis, 24(4):207214,
1989.
30 Villaverde, Norbert. Variable Mixed Mode Delamination in Composite Laminates under Fatigue
conditions: Testing and Analysis. PhD thesis, Universitat De Girona, 2004. Web. 10 May 2010. <http://www.tdr.cesca.es/TESIS_UdG/AVAILABLE/TDX-0207105-122952//tnbv.pdf>.
31 Fei Xiao, Chung-Yuen Hui, Junichiro Washiyama, Edward J. Kramer. Phase Angle Effects on Fracture
Toughness of Polymer Interfaces Reinforced with Block Copolymers Macromolecules, 1994, 27 (15), pp 43824390.
32 J. P. Parmigiani and M. D. Thouless, The Effects of Cohesive Strength and Toughness on Mixed-mode
Delamination of Beam-Like Geometries. Engineering Fracture Mechanics, 74, 2675-2699 (2007).
84

The Effect of Mode-Mixity and Constraint in Adhesively Bonded Composite Joints

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The Effect of Mode-Mixity and Constraint in Adhesively Bonded Composite Joints

Final Year Project Report Neville Lawless 06523587

Head of School: Dr D. Fitzpatrick

Project Supervisor: Dr. Neal Murphy

12. Acknowledgments ............................................................................................................. 81 13. References ......................................................................................................................... 82

Figure 2 below indicates the tensile load being applied.

Figure 2: DCB experimental setup

Figure 3: Indication of mode II (In-plane) fracture.

Figure 4: Schematic diagram of various mode II delamination test methods [12].

Mixed Mode (I/II)

Figure 6: Schematic of MMB test configuration. [20]

The effect of constraint on fracture toughness

Figure 9: Crack tip stress fields constrained by adherents.

Failure of Adhesive joints

Figure 10: Cohesive fracture.

Figure 11: Interfacial failure

Other types of fracture

Figure 13: Fracture with crack jumping present.

Figure 14: Crack jumping from one interface to another.

Composite prepreg sheets:

Peel ply: Henkel Hysol EA 9895 Peel Ply. Adhesive:

Henkel Hysol EA9830.05.

5.2 Composite Specimen production

Press-clave build-up and de-bulking:

Figure 16: Bagging film and Debulking tape.

Figure 17: Vacuum generator.

Press Clave build-up:

Figure 18: Press clave layup.

Figure 19: Hydraulic press.

Figure 20: Air compressor

Figure 21: Thermocouples in place in the hydraulic press.

Figure 22: Temperature control system.

Figure 23: Temperature control settings for curing composites.

Figure 24: Tile Cutter.

Figure 25: Respiratory facemask.

Figure 27: Grit blaster in UCD labs with close up of nozzle.

Figure 28: Scrim Cloth.

Preparation of DCB specimens

Figure 29: Dispensing gun with mixing nozzle.

Figure 30: Specimens secured in bonding jig.

Figure 33: Finished DCB specimen.

Figure 34: Callipers (top) & Micrometer (bottom)

ELS test rig manufacture

Figure 35: Test piece clamp.

Figure 36: Construction drawings.

Figure 37: Finished model with selected material finishes.

Rig Base Table 1: Rig parts list.

Flat stainless steel

Part A Part A Part B Part B

Table 2: Rig cutting list.

Figure 38: Vertical-turret-3-axis-milling-machine

Figure 39: Completed ELS test rig.

A 1 KN load cell was attached by a screw to the cross-head.

Figure 40: Macro to record crack propagation values.

Figure 42: Excel spreadsheet used for GIC calculations.

Figure 43: Test area setup.

Mode I DCB tests Mixed mode tests

Mode I DCB tests.

Mixed mode tests.

5/9 ply layup No Scrim cloth.

9/5 ply layup No Scrim cloth.

5/9 ply layup Scrim cloth.

9/5 ply layup Scrim cloth.