Fracture Analysis of Glass Microsphere Filled Epoxy Resin Syntactic Foam
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SCHOOL OF AEROSPACE, CIVIL AND MECHANICAL ENGINEERING UNIVERSITY COLLEGE UNIVERSITY OF NEW SOUTH WALES AUSTRALIAN DEFENCE FORCE ACADEMY FRACTURE ANALYSIS OF GLASS MICROSPHERE FILLED EPOXY RESIN SYNTACTIC FOAM MAJOR PETER YOUNG A thesis submitted for the degree of Masters of Engineering AMEC – 2691 AUGUST 2007 Thesis Supervisor: Dr Krishna Shankar Co - Supervisor: Dr Andrew Neely i ABSTRACT Hollow glass microspheres have been used extensively in the automotive and marine industries as an additive for reducing weight and saving material costs. They are also added to paints and other materials for their reflective properties. They have shown promise for weight critical applications, but have thus far resulted in materials with low fracture toughness and impact resistance when combined with thermosetting resins in syntactic foam. The advent of commercially available microspheres with a wide range of crushing strengths, densities and adhesive properties has given new impetus to research into syntactic foam with better fracture behaviour. Current research suggests that the beneficial effects on fracture and impact resistance gained by the addition of solid reinforcements such as rubber and ceramic particles are not seen with the addition of hollow glass microspheres. The research presented in this paper has examined the mechanisms for fracture resistance in glass microsphere filled epoxy (GMFE) syntactic foams, as well as determined the effect microsphere crushing strength and adhesion strength has on the material’s fracture toughness. The flexural properties of various GMFE have also been determined. GMFE were manufactured with varying microsphere volume fraction up to 50%, and with variances in microsphere crushing strength and adhesion. The specimens were tested for Mode I fracture toughness in a three point single edge notched bending setup as described in ASTM D5045 as well as a three point flexural setup as described in ASTM D790-3. Fracture surfaces were inspected using scanning electron microscope imaging to identify the fracture mechanisms in the presence of microspheres. Results indicate a positive effect on fracture toughness resulting from new fracture areas created as tails in the wake of the microspheres in the fracture plane. Results also indicate a negative effect on fracture toughness resulting from weak microspheres or from interfacial disbonding at the fracture plane. These two effects combine to show an increase in GMFE fracture toughness as the volume fraction of microspheres is increased to between 10 – 20% volume fraction (where the positive effect dominates), with a reduction in fracture toughness as microspheres are added further (where the negative effect dominates). ii ACKNOWLEDGEMENTS I would like to start by acknowledging the support and facilities provided by the School of Aerospace Civil and Mechanical Engineering, without which this thesis would not have been possible. In that regard I thank the Heads of School Dr Warren Smith and Associate Professor Joseph Lai for their ongoing support of both my research and the visiting military fellowship scheme within the school. Further acknowledgement goes to my thesis supervisor Dr Krishna Shankar who has enabled me to undertake something that was to be with me for nearly four years. Not only did Krishna provide the early guidance and advice for this research, he more importantly enabled me to learn as I went. So often in the early stages did I feel that my knowledge was lacking, only to have Krishna guide me in my understanding. It was this well timed instruction that so often enabled the work to continue. His frankness was a weapon used at exactly the right moments, and his criticisms tempered with the right amount of encouragement. His willingness to spend time supporting my work has been greatly appreciated, and I hope others continue to seek out Krishna as a fine supervisor within the School. Dr Shankar also personally undertook testing of the 2003 Japan tests as part of this work. Dr Andrew Neely’s enthusiasm is matched only by his eagerness to see others achieve. His assistance with this work included the encouragement to undertake translucency testing of the uncut specimen sheets, the writing of the MatlabTM scripts used in analysing the translucency results, and a thorough provision of feedback on a draft thesis. Andrew has also taken the time to involve as many postgraduates in a healthy dose of social activities, and I thank him for all the support he has shown me. Other staff who have contributed significantly to the success of this research are Pat Nolan, Bob Clark, Evan Hawke and Bill Doren. Pat for his expertise on the test equipment, Bob for his help with the microscopy and imaging equipment, Evan for painstakingly setting up the data measurement programs, and Bill for assistance in the Materials Lab. I would also like to thank the electron Microscopy Unit of the Australian National University for the kind access to the Cambridge Instruments Scanning Electron iii Microscope. In particular I would like to thank Dr Sally Stowe and Dr Roger Heady for their assistance. Thanks also go to my brother Dr John Young for his advice and support throughout. John also wrote the MatlabTM scripts used in the analysis of the strain energy release rate results. Finally I would like to express my gratitude to my partner Judi who has dealt with my angst throughout the past four years. iv DISCLAIMER This thesis has been written in fulfilment of the requirements for the degree of Masters of Mechanical Engineering. It is the result of a period of research and analysis by the author while a student of the University of New South Wales at the Australian Defence Force Academy. Views expressed throughout this thesis do not represent the views of the University College, the University, the Australian Defence Force Academy or the Australian Defence Force or its agencies. v CONTENTS CHAPTER 1 – INTRODUCTION............................................................................. 1 1.1 BACKGROUND.................................................................................................. 1 1.2 AIM ................................................................................................................. 2 1.2.1 Reason for This Research ............................................................................ 2 1.2.2 Specific Aims ............................................................................................... 2 1.3 METHOD .......................................................................................................... 2 1.3.1 Microsphere Selection ................................................................................. 2 1.3.2 Testing Regime ............................................................................................ 3 1.4 PRESENTATION OF WORK ................................................................................. 4 CHAPTER 2 – BACKGROUND INFORMATION.................................................. 5 2.1 GLASS MICROSPHERES ..................................................................................... 5 2.1.1 Hollow Glass Microsphere Specifications.................................................... 5 2.1.2 Manufacture of Glass Microspheres ............................................................ 7 2.1.3 The Use of Glass Microspheres.................................................................... 9 2.2 SYNTACTIC FOAM .......................................................................................... 10 2.2.1 Manufacture of Syntactic Foam ................................................................. 12 2.2.2 The History of Research into Syntactic Foam............................................. 13 2.2.3 Compressive Response of Syntactic Foam.................................................. 13 2.2.4 Tensile and Flexural Response of Syntactic Foam...................................... 14 2.2.5 Temperature Effect on Syntactic Foam ...................................................... 14 2.2.6 Moisture Absorption in Syntactic Foam ..................................................... 15 2.2.7 Syntactic Foam in Sandwich Panels........................................................... 15 2.2.8 Fibre Reinforced Syntactic Foams ............................................................. 15 2.2.9 Effect of Microsphere Properties on Syntactic Foam ................................. 16 2.2.10 Fracture Behaviour of Syntactic Foam ...................................................... 17 2.2.11 Syntactic Foam - Summary ........................................................................ 19 2.3 TESTING OF COMPOSITES/PLASTICS ................................................................ 20 2.3.1 ASTM Standard D5045.............................................................................. 20 2.3.2 ASTM Standard D790-3............................................................................. 21 CHAPTER 3 – MANUFACTURE OF THE GMFE SYNTACTIC FOAM SPECIMENS............................................................................................................. 23 vi 3.1 MATERIAL SELECTION.................................................................................... 23 3.1.1 Epoxy resin................................................................................................ 23 3.2 SPECIMEN PREPARATION ................................................................................ 26 3.2.1 Specimen Mixing ......................................................................................