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Zopherus Nodulosus Haldemani) Mississippi State University Scholars Junction Theses and Dissertations Theses and Dissertations 1-1-2017 Structure-Property Relations of the Exoskeleton of the Ironclad Beetle (Zopherus Nodulosus Haldemani) Vina Le Nguyen Follow this and additional works at: https://scholarsjunction.msstate.edu/td Recommended Citation Nguyen, Vina Le, "Structure-Property Relations of the Exoskeleton of the Ironclad Beetle (Zopherus Nodulosus Haldemani)" (2017). Theses and Dissertations. 4094. https://scholarsjunction.msstate.edu/td/4094 This Graduate Thesis - Open Access is brought to you for free and open access by the Theses and Dissertations at Scholars Junction. It has been accepted for inclusion in Theses and Dissertations by an authorized administrator of Scholars Junction. For more information, please contact [email protected]. Template C v3.0 (beta): Created by J. Nail 06/2015 Structure-property relations of the exoskeleton of the ironclad beetle (Zopherus nodulosus haldemani) By TITLE PAGE Vina Le Nguyen A Document Type. Submitted to the Faculty of Mississippi State University in Partial Fulfillment of the Requirements for the Degree of Master of Science in Biological Engineering in the Department of Agricultural and Biological Engineering Mississippi State, Mississippi December 2017 Copyright by COPYRIGHT PAGE Vina Le Nguyen 2017 Structure-property relations of the exoskeleton of the ironclad beetle (Zopherus nodulosus haldemani) By APPROVAL PAGE Vina Le Nguyen Approved: ____________________________________ RajKumar Prabhu (Major Advisor) ____________________________________ Lakiesha Williams (Committee Member) ____________________________________ Hongjoo Rhee (Committee Member) ____________________________________ Mark Horstemeyer (Committee Member) ____________________________________ Fei Yu (Graduate Coordinator) ____________________________________ Dean’s Name Dean Bagley College of Engineering Name: Vina Le Nguyen ABSTRACT Date of Degree: December 1, 2017 Institution: Mississippi State University Major Field: Biological Engineering Major Advisor: Dr. Rajkumar Prabhu Title of Study: Structure-property relations of the exoskeleton of the ironclad beetle (Zopherus nodulosus haldemani) Pages in Study: 60 Candidate for Degree of Master of Science In this study, structure-property relationships in the ironclad beetle (Zopherus nodulosus haldemani) exoskeleton are quantified to develop novel bio-inspired impact resistance technologies. The hierarchical structure of this exoskeleton was observed at various length scales for both the ironclad beetle pronotum and elytron. The exocuticle and endocuticle layers provide the bulk of the structural integrity and consist of chitin- fiber planes arranged in a Bouligand structure. The pronotum consists of a layered structure, while elytron consists of an extra layer with “tunnel-like” voids running along the anteroposterior axis along with smaller interconnecting “tunnel-like” voids in the lateral plane. Energy dispersive X-ray diffraction revealed the existence of minerals such as calcium carbonate, iron oxide, zinc oxide, and manganese oxide. We assert that the strength of this exoskeleton could be attributed to its overall thickness, the epicuticle layer thickness, the existence of various minerals embedded in the exoskeleton, and its structural hierarchy. The thickness of the exoskeleton correlates to a higher number of chitin-fiber planes to increase fracture toughness, while the increased thickness of the epicuticle prevents hydration of the chitin-fiber planes. In previous studies, the existence of minerals in the exoskeleton has been shown to create a tougher material compared to non-mineralized exoskeletons. ACKNOWLEDGEMENTS This effort was sponsored by the Engineer Research and Development Center under Cooperative Agreement number W912HZ-15- 2-0004. The views and conclusions contained herein are those of the authors and should not be interpreted as necessarily representing the official policies or endorsements, either expressed or implied, of the Engineer Research and Development Center or the U.S. Government. In addition, thanks to Mississippi State University’s Center for Advanced Vehicular Systems (CAVS), Amanda Lawrence and I-Wei Chu at Institute of Imaging and Analytical Technologies (I2AT), Xanthe Shirley and other students at Texas A&M University’s Department of Entomology, and Brett Williams at Engineer Research and Development Center. iv TABLE OF CONTENTS ACKNOWLEDGEMENTS ............................................................................................... iv LIST OF TABLES ............................................................................................................ vii LIST OF FIGURES ......................................................................................................... viii CHAPTER I. INTRODUCTION .................................................................................................1 1.1 Introduction ...............................................................................................1 1.2 Bio-inspired Design ...................................................................................1 1.3 Arthropod Exoskeletons ............................................................................2 1.3.1 Hierarchical Structure ..........................................................................2 1.3.2 Chitin ...................................................................................................6 1.3.3 Mineralization ......................................................................................7 1.4 Bio-inspired Design Studies Involving Arthropod Exoskeletons .............8 1.4.1 Introduction .........................................................................................8 1.4.2 Crustacean Exoskeletons .....................................................................8 1.4.3 Beetle Exoskeletons ...........................................................................13 1.5 Ironclad Beetle .........................................................................................16 1.5.1 Introduction .......................................................................................16 1.5.2 Anatomy of Ironclad Beetle ..............................................................17 1.6 Study Objectives ......................................................................................18 II. MICROSTRUCTURE OBSERVATION ...........................................................20 2.1 Sample Preparation ..................................................................................20 2.1.1 Obtainment ........................................................................................20 2.1.2 Preparation .........................................................................................21 2.2 Microtomography ....................................................................................21 2.3 Scanning Electron Microscopy and the Electron Diffraction X- Ray Spectroscopy ....................................................................................21 2.4 Image Analysis ........................................................................................22 III. MECHANICAL TESTING .................................................................................23 3.1 Nano-indentation .....................................................................................23 3.1.1 Introduction .......................................................................................23 3.1.2 Surface Indentation ............................................................................25 3.2 Cross Section Indentation ........................................................................27 IV. RESULTS AND DISCUSSION ..........................................................................28 v 4.1 Beetle Length Characterization ...............................................................28 4.2 Surface Analysis of Pronotum and Elytron .............................................29 4.3 Analysis of Cross Section of Exoskeleton ...............................................33 4.4 Chemical Composition ............................................................................37 4.5 Nano-indentation .....................................................................................39 4.6 Structure-Property Relationship ..............................................................42 4.7 Hierarchical Structure ..............................................................................46 V. CONCLUSIONS .................................................................................................48 VI. FUTURE WORKS ..............................................................................................51 REFERENCES ................................................................................................................. 53 vi LIST OF TABLES 3.1 Nano-indentation parameters from previous studies (Sun 2014, Sun 2007, and Sun 2008) .......................................................................................26 4.1 Chemical composition of the pronotum and elytron top and bottom surfaces ...........................................................................................................38 4.2 Chemical composition of the pronotum and elytron top and bottom surfaces ...........................................................................................................39 vii LIST OF FIGURES 1.1 (a) Structure
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