Blekinge Institute of Technology Research Report No 2004:05

Fracture Toughness Testing of Non Standard Specimens

Etienne Mfoumou Sharon Kao-Walter

School of Engineering Blekinge Institute of Technology

Fracture Toughness Testing of Non Standard Specimens

MSc Etienne Mfoumou (etienne.mfoumou@bth.se) Tech. Lic. Sharon Kao-Walter (skw@bth.se ) School of Engineering Blekinge Institute of Technology, 371 44 Karlskrona, Sweden Tel.: +46 455 38 55 06 / Fax: +46 455 38 55 07

Abstract The fracture behavior of the main layers used in food packaging material is studied. Investigations include aluminium foil (9m), paper board (100 m) and Low Density Polyethylene (27 m). The plane stress fracture toughness of each layer is derived based on a centered crack panel. Different crack sizes have been tested. A compromise (crack length) was found, at which Strip Yield Model as well as Linear Elastic Fracture Mechanics allow the validation of experimental results. Meanwhile, accurate results are obtained using the Strip Yield Model with a geometric correction. The result is also used to evaluate crack initiation from a notch when all three layers are laminated. 1. Introduction Liquid food packages are often made from packaging material, which consists of several different layers of material for the different requirements of the package, within which alumium foil (Al), Low Density Polyethylene (LDPE), and Carton (PPR). One important task is to secure that every layer keeps its function during the forming, filling and transportation process. Several studies have been done to study the different mechanical properties of these materials [1-5]. The fracture behaviour of Al-foil (about 6-7 m) was investigated in [6], and the fracture toughness was found to be much lower than what is given in standard materials handbooks. However, a fracture mechanical study of such thin materials was suggested. The purpose and aim of this work is to extend the results from [6] through investigation of the fracture behaviour of Al-foil (9 m), paper board (100 m) and LDPE (27 m). The specificity of this continuation study is still the non standard specimen size, particularly the thickness which doesnt satisfy the ASTM standard No E399 [7]. The study uses experimental method and theoretical analysis to determine a reliable modelling method for approximating the thin materials under consideration. Furthermore, the fracture behaviour in the laminated packaging material is still not understood completely. In [S. Kao-Walter, P. Sthle and R. Hgglund], it was observed that the load carrying capacity increases dramatically when a thin aluminium foil is laminated together with a Low Density Polyethylene layer. This experiment is therefore designed to illustrate how strength in the presence of cracks - termed Fracture Toughness - is characterized and measured. The fracture toughness of each layer is investigated using the suggested method.

2. Background Fracture and fracture toughness The crack in a real specimen under load is shown on figure 2 below

Figure 2: Crack in a real specimen under load Let suppose that the load on the specimen in figure 2 (which is half of our geometry, because of symmetry) is increased until it fractures, i.e. the crack grows. The resistance to fracture may be characterized by the stress intensity at fracture K c, called the fracture toughness. The fracture toughness and the manner in which the crack grows are heavily dependent upon the material thickness [8]. Consider a specimen having a thickness t that is small compared to the diameter of the plastic zone ro, figure 3 below. As the crack is pulled apart the plastic zone will undergo Poisson contraction, relieving stresses z acting through the sample in the z direction. This is called plane stress because stresses are only acting in the x-y plane. With y large and z near zero the shear stress on the 45o plane between the y and z axes is at a maximum. The crack therefore tends to orient itself along this plane as it grows. This type of crack growth is usually stable and gradual and is characterized as tearing. This mode of fracture is more or less close to the cases studied here.

Figure 3: Plane stress fracture. Plastic zone diameter ro comparable to or greater than sample thickness. Now consider a specimen having a thickness t that is large compared to ro, figure 4 below. As the crack is pulled apart, the material above and below the plastic zone prevents Poisson contraction from occurring throughout most of the sample. This sets up large z stresses in the plastic zone. This situation is defined as plane strain because material is straining only in the x-y plane. With z comparable to y, the shear stresses are small so the crack tends to orient itself in a plane perpendicular to y as it grows. This type of growth is usually unstable and is characterized as cleavage. Note that even with a thick sample there will be thin regions close to its surfaces where Poisson contraction will take place and failure on 45o planes will occur.

Figure 4: Plane strain fracture. Plastic zone diameter ro much less than sample thickness.

Thicknesses between those that result in plane strain or plane stress are termed mixed, with plane strain occurring in the interior and plane stress some significant distance from the surface. As the sample thickness increases and the form of the stress distribution changes the fracture toughness falls, asymptoting to a constant value for plane strain. Because of its independence of sample thickness this asymptote, termed the plane strain fracture toughness KIc, is considered a material property. Meanwhile, the model developed by Sthle [9], even though corresponding to homogeneous elastic body, is well suited for our material in study. A specimen containing a mode I crack with length 2a is considered (see figure 1). As the stress is applied, decohesive process regions come out ahead of the crack tips. The fracture process takes place in these regions when the stress starts to decrease at increasing displacement. These regions grow symmetrically in the crack plane until the material fails.

3. Theoretical Analysis
The fracture toughness value is in principle computed on the basis of the load corresponding to a well-defined unstable advance of the crack. The relationship between the stress intensity K and the load P applied on a Centered crack panel can be defined as follow [8]:
P( a ) a K( ) = w .f( a ) w B w w

(1)

with
2 4 f( a ) = .a .sec a + 0.06. a ] .a . [ 1 0.025. w 4.w w w 2.w
(2)

where a is half the crack length, w is half the width, and B is the thickness (see figure 7). At onset of crack growth the stress intensity factor, K, equals the fracture toughness Kc. Therefore, the linear elastic fracture mechanics limiting stress is given by:

c = Kc. w (3) 2.w.f( a ) w where c is the stress at crack growth (here peak stress for the given initial crack length), and Kc obtained experiment (based on the reasonable crack length for the purpose).

The Strip Yield Model with the appropriate geometry correction factor f, derived in [6], is expressed as follows 2 2. .K c b (4) = asec exp c 2 .f 2 ( a ) 8.a. b w where is the Yield Strength (here stress at break for a strip specimen). b Analytically, the experimental stress vs. crack length relationship is given by

exp

P(a) 2BW

(5)

The fracture toughness Kc is expressed from (4) as follows: . c Kc = b . f . 8.a . ln sec 2. b

(6)

4. Experiment 4-1. Set up

The objective of this experiment is to determine the plane-stress fracture toughness Kc of the materials of interest. The fracture toughness testing procedures specified in ASTM Standard No. E399 do not fit the materials of interest, thus we attempt the determination of a realistic procedure. Three different nominal thicknesses (for the individual layers) are tested. Each sample contains a hand made crack'. To determine their fracture toughness each of the samples will be pulled apart by applying load to a pair of grips clamping the specimen (figure 5). The load on the specimen P vs. the extension for each crack size is recorded. These data, plus the sample dimensions are then used according to the flow chart in appendix B. The MTS Tensile Test Machine [10], shown in figure 5, is used. This machine has a crosshead a horizontal bar - that can be very accurately traversed up and down under digital control by means of two large jack screws. Specimens are tested by attaching them between the crosshead and the stationary base of the machine and then traversing the crosshead up to place the sample under increasing load. The load on the sample is recorded by a piezo-electric load cell mounted between the sample and the crosshead. A 2.5 kN loadcell is used, the grip separation is set to the specimen length and the test speed is 9.2 mm/min.

Upper crosshead Load cell Upper clamp

Lower clamp Handset

Figure 5: The MTS machine

Measurements will be recorded using a computer with MTS TestWorks software [10]. Data are then exported to MATLAB for calculations and analysis.
4-2. Determining the sample dimensions

Measure the half height h and width (to crack centers) w of each of the samples using the ruler. Measure the thickness t of each sample using the micrometer. The length of the initial crack, measured from the crack center could also be needed, but is assumed to be zero.
4-3. Preparing the sample for test

For each material composition, at least 10 pieces of 230x95 size specimens (taken from cross direction) are cut using a paper cutter. The pre-crack is hand made with a knife and a ruler. Meanwhile, to realize the pre-crack on aluminium foil is much difficult. Therefore, aluminium specimen is placed between a paper (below) and PET (above) and the pre-crack is realized from the upper layer (PET). Since LDPE layer has been produced by extruding melted LDPE on a PET layer with a table extruder, it is first pre-peeled (in one corner) from PET before the precrack is realized on both layers. Finally the 2 layers are separated carefully by hands, making sure that the peeling process in the crack region goes along the crack (widths direction). The pre-crack process is realized on a plastic glass plate. A centered crack panel specimen is ready to be used as shown on figure 1.
4-4. Mounting the specimen in the testing machine

Load is applied to the specimen through the crosshead, connected to a load cell. The pair of grips that match the specimen under test is chosen (figure 6), and the 2,5kN load cell is installed. One grip is mounted to the base of the testing machine and one to the crosshead using the dowel pins provided. The flat side of both grips is parallel to the crosshead. The grips are equipped with needles facilitating a correct positioning of the specimen. The specimen is placed in the slot in the upper grip and secured with locking nuts provided. The same process is performed in the slot

in the lower grip. It is important to make sure that the specimen sits well in the grips before running the test, otherwise adjustment must be made.

Figure 6: The clamping arragement 4-5. Running the test

The MTS-software Test Works 4.07 is launched and the input configuration introduced to record the data. The Testing Machine controller is set to raise the crosshead at a speed of 9.2 mm/min, the grip separation being 230mm (specimen length). The thickness and the width of the specimen are also introduced, and the needed output parameters set on. The specimen is not pre-loaded. As the test begins (by pressing the play button), the drawing of the load/displacement diagram is continuously displayed. It appears initially as a straight diagonal line showing the initial elastic deformation of the specimen. The specimen configuration is as presented in figure 7 below

2a

2W Figure 7: Specimen configuration with a centered crack of length 2a 7

As the load on the specimen increases, its surface dimples around the crack. This dimpling is produced by Poisson contraction (still difficult to observe here because of thin material) of the material in the plastic zone. As the specimen begins to fracture different situations could happen depending on its thickness [Anderson et al.] The sample may fail suddenly, or it may tear. In the latter case a popping sound may be heard. This is the sound of the crack intermittently growing. An acoustic emission method is therefore ongoing in order to analyze this sound for a laminated material, in order to assess which layer breaks first. The test continues until the material breaks totally. The plotter then displays the load vs. extension curve. Output results are given, mainly peak load and extension at break. The process is performed for at least five specimens, and a least square method is used to select the resulting parameters for each crack length. Data are exported to MATLAB [11] for analysis. The different load-displacement curves obtained are shown in appendix A.
4-6. Experimental data analysis

4-6-1. Examination of the specimen The crack should propagate from the two tips to the edges for a successful test. Looking over the fracture surfaces, the initial crack is not obviously seen, making it impossible to measure its length. Therefore, the standard method is not appropriate for the current case. 4-6-2. Identifying the load at fracture Four types of load-displacement behavior are shown on figures 7 and 8 below.

Figure 7: Three types of load displacement behavior and the identification of the critical load (ASTM stds., No. E399, Vol. 03.01). Type I - tearing (plane stress fracture). Type 2 mixed. Type 3 - cleavage (plane strain fracture)

Figure 8: Load-displacement curve for an invalid fracture toughness test, where ultimate failure happens well beyond PQ

Comparing the load-extension diagram with the samples shown in figures 7 and 8, its obvious that our materials correspond to the one for an invalid fracture toughness test. As a result, the load-displacement curve displays considerable plastic deformation prior to failure. This is type I curve [8]. Initially the load-extension diagram is linear because the specimen deforms elastically, but the corresponding region is very small here. At fracture the crack will have grown changing the material stiffness and causing the load-extension diagram to depart from a straight line. How this departure occurs depends on how the specimen fractures. A mixture of fracture mechanisms could also be applied here because the curves produced are smooth and punctuated by discontinuities of unstable crack growth (observation of the curves in a small step scale). These discontinuities may be understood as 'pop in' since they could produce the audible popping sound. This report concentrates on the identification according to T.L. Anderson [8] and thus, consider our samples to have a type-I behavior shown in figure 7.

5. Results and discussion

Critical stresses for different crack length (up to 50 mm) were derived for experiment, LEFM as well as SYM. Equation (3), (4), and (5) are normalized and the stress vs. crack length curves (experiment, LEFM and SYM all together) are plotted for each material. The results as critical normalized stress versus normalized crack length are shown on figures 9 to 11.

Figure 9: Normalized stress vs crack length (Al foil)

Figure 10: Normalized stress vs crack length (LDPE)

Figure 11: Normalized stress vs crack length (Paper) Confirming the result from [6] for the materials under investigation in this report, good agreement in found between the measured results and the analytical results both with LEFM and SYM for crack lengths larger than 2a = 20 mm. Meanwhile, for crack lengths less than 20 mm, SYM shows a better correlation with the measured values, whereas LEFM fails to describe the experimental result for such short crack lengths. The computed stress intensity factor can be obtained using the measured loads, and equations (1) and (2). Assuming several values of Kc for analytical calculations, and oriented by the

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appearance on figures 9 to 11 for each crack size, as well as the accuracy of the fit (see table 1), a compromise is found at 2a = 45 mm. Thus, the fracture toughness is analytical calculated using equation (6) and given in table 2. Table 1: Correlation
Correlation Experiment / LEFM Material Al foil LDPE PPR Al foil LDPE PPR /exp [%] (*) 0.0008 0.0038 0.0004 1.6290 4.2207 1.5061

Experiment / SYM
(*)

: Relative difference on experimental value.

Table 2: Calculated Kc values

Material Al foil LDPE PPR Kc [MPa.m1/2] 5.0963 1.2267 3.1204

However, Kc is stiffness dependent; the higher stiffness the higher Kc value. When the layers are laminated together, the strain value will be the same before the delamination or crack propagation happens. Since the strain is proportional to Kc/E, this value was calculated and indicated in table 3 below Table 3: b [MPa] Kc [MPa.m1/2] Kc/E Al 58.4 5 0.000429 PPR 37.2 3.12 0.0024 LDPE 8.7 1.22 0.0124

From the above result and under displacement control condition, we can conclude that if all layers are placed together without glue, Al-foil will break first, then PPR, and finally LDPE.

6. Conclusion and further work

An experimental investigation was performed for the determination of plane stress fracture toughness for non standard materials. Three individual layers from a laminated liquid food packaging material were tested (Al, LDPE and PPR).The modified strip yield model developed in [6] was found to suit these materials. From the normalized stress vs. crack length curves, an acceptable region for approximation of experiment to LEFM or SY-model was defined. A compromise was found at crack length

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2a=45mm, from which the fracture toughness was calculated. It was also found that outside of the acceptable region, SY-model is well suited for Kc estimation. All three layers laminated and loaded under displacement control, the crack seems to start propagating on Al foil, then on PPR and finally on LDPE. Further work could therefore investigate this assessment based on real time test of the laminate together with an acoustic emission method.
Acknowledgement

This work was supported by the School of Engineering at Blekinge Institute of Technology and Department of Mechanical Engineering at University of Douala, Cameroon (ENSET). The authors would like to thank Prof Oleg Rudenko for reviewing the report.

References

[1]. S. Kao-Walter, P. Sthle and R. Hgglund , Fracture Toughness of a Laminated Composite, in: Fracture of Polymers, Composites and Adhesives II, Elsevier, Oxford, UK, ISBN: 0-08-044195-5, 2002 [2]. Kao-Walter, S., Dahlstrm, J. Karlsson,T. and Magnusson, A. (2002) A study of relation between mechanical properties and adhesion level in a laminated packaging material, Mechanics of Composite Materials, Vol. 40, No. 1, 2004. [3]. Lau,C.C. (1993) A Fracture Mechanics Approach to the Adhesion of Packaging Laminates, Doc. Thesis, Imperial College of Science, UK. [4]. Tryding, J. (1996) In Plane Fracture of Paper, Division of Structural Mechanics, Lund Institute of Technology. [5]. Kao-Walter, S. and Sthle, P.(2001) Mechanical and Fracture Properties of Thin Alfoil, Research report, Blekinge Inst. of Tech., 2001:09. [6]. Kao-Walter, S. and Sthle, P. Fracture Behaviour of Thin Al-foil Measuring and Modelling of the Fracture Processes, Submitted to Theoretical and Applied Fracture Mechanics Fracture Mechanics Technology, 2004. [7]. ASTM E399, http://www.me.fau.edu/~salivar/ASTM399.html [8]. T.L. Anderson Fracture Mechanics, Fundamentals and Applications, Second Edition, 1995 [9]. P. Sthle On The Small Crack Fracture Mechanics, Int. Journ. Of Fracture 22 (1983) 203216 [10]. MTS Systems Corporation, www.mts.com, c 2002 [11]. The Math Works Inc., 2000 MATLAB, The Language of Technical Computing. Natick, MA USA

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Appendix A: Load-displacement data

Table 1: Aluminium foil

Crack length 2a [mm] Peak Load [N] Strain at break Peak stress [MPa] 5 29.1 0.005 48.3 10 26.6 0.005 44.1 15 23.9 0.004 39.6 20 19.1 0.005 31.7 25 22.6 0.003 37.5 30 18.7 0.003 31.1 35 17.1 0.003 28.4 40 12.4 0.004 20.6 45 14.0 0.003 23.3 50 9.4 0.004 15.6

Table 2: LDPE
Crack length 2a [mm] Peak Load [N] Strain at break Peak stress [MPa] 5 17.5 0.244 7.4 10 16.2 0.246 6.8 15 14.7 0.195 6.2 20 13.2 0.189 5.6 25 12.5 0.176 5.3 30 11.0 0.158 4.6 35 10.8 0.155 4.5 40 9.8 0.137 4.1 45 9.4 0.135 4.0 50 8.3 0.121 3.5

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Table 3. Paper
Crack length 2a [mm] Peak Load [N] Strain at break Peak stress [MPa] 5 264.4 29.3 10 237.6 26.3 15 187.0 20.7 20 165.7 18.3 25 141.9 19.7 30 134.5 14.9 35 118.7 13.1 40 112.7 12.5 45 95.8 10.6 50 85.6 9.4

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Appendix B: Flow chart summarizing the approach

BEGIN

Display the load-extension curve for the material

Identify the type of loaddisplacement behavior

Case of fig.8 ? yes

No

Identify load at fracture (assumed peak load)

Determine stress intensity for each crack size

Assume KIc for the material (LEFM)

Calculate & correlate stress vs. Crack length curves (Experiment, LEFM, and SYM)

No

Good fit ? Yes

Determine Kc SYM and compare with LEFM

Not suited for this sudy

END

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Fracture Toughness Testing of Non Standard Specimens Etienne Mfoumou and Sharon Kao-Walter ISSN 1103-1581 ISRN BTH-RES--05/04--SE Copyright 2004 by individual authors All rights reserved Printed by Kaserntryckeriet AB, Karlskrona 2004