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Development of a Controllable Polymer System Using Interpenetrating Networks University of Nebraska - Lincoln DigitalCommons@University of Nebraska - Lincoln Mechanical (and Materials) Engineering -- Mechanical & Materials Engineering, Dissertations, Theses, and Student Research Department of 8-2013 Development of a controllable polymer system using interpenetrating networks Emilie Bobo University of Nebraska-Lincoln, [email protected] Follow this and additional works at: https://digitalcommons.unl.edu/mechengdiss Part of the Applied Mechanics Commons Bobo, Emilie, "Development of a controllable polymer system using interpenetrating networks" (2013). Mechanical (and Materials) Engineering -- Dissertations, Theses, and Student Research. 53. https://digitalcommons.unl.edu/mechengdiss/53 This Article is brought to you for free and open access by the Mechanical & Materials Engineering, Department of at DigitalCommons@University of Nebraska - Lincoln. It has been accepted for inclusion in Mechanical (and Materials) Engineering -- Dissertations, Theses, and Student Research by an authorized administrator of DigitalCommons@University of Nebraska - Lincoln. DEVELOPMENT OF A CONTROLLABLE POLYMER SYSTEM USING INTERPENETRATING NETWORKS By Emilie Bobo A THESIS Presented to the Faculty of The Graduate College at the University of Nebraska In Partial Fulfillment of the Requirements For the Degree of Master of Science Major: Mechanical & Materials Engineering Under the Supervision of Professors Mehrdad Negahban and Li Tan Lincoln, Nebraska August, 2013 Development of a controllable polymer system using interpenetrating networks Emilie Bobo, M.S. University of Nebraska, 2013 Advisers: Mehrdad Negahban and Li Tan My research partners and I have studied the possibility of building a material system with controllable properties using two interpenetrating polymer networks (IPNs). This study is part of a project to build a rapid prototyping system that allows for the printing of objects with predefined spatial distribution of properties, with the goal that property distributions are controlled though interactions at the molecular level. One can change the properties of an IPN by adjusting the ratio of interpenetrating networks present in a given cured mixture. This is similar to how one obtains different shades of the color green by gradually changing the ratio of blue and yellow pigments when mixing paint. In much the same way as one can use mixing to change colors along the surface of a painting, one may change the properties of a body along a direction in space by changing the ratio of networks in the IPN. To achieve this, we studied how to make an IPN and how to control it in a way that will allow controlled grading of material properties in space. An IPN is constructed by curing two polymer networks in the same space. Unlike separated systems, the IPN shows behavior and properties that result from the close interaction of the networks, a feature that inhibits the expression of the individual network properties in favor of a property resulting from the close interaction of the networks. The properties of a given IPN system change based on the ratio of the networks present in the system and the order and kinetics of the curing process. At first, we studied and demonstrated the construction of an IPN using two networks that are both photo-cured in the same space. Most IPNs are constructed using a combination of rapid photo-curing of one network and then slow thermal curing of the second network, which is constructed from molecules that are trapped in the first network. The ability to photo-cure both networks speeds up the curing process, a point deemed desirable for rapid prototyping. Once constructed, Fourier-Transform Infra-Red spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), and Atomic Force Microscopy (AFM) were used to show that the resulting system is a true IPN and we used Thermal Gravimetric Analysis (TGA), AFM, Dynamic Mechanical Analysis (DMA), and tensile testing to further characterize its properties. Next, we studied how to control the ratio of the two networks in the IPN by selectively controlling the extent of curing of each network and then removing the uncured components. This provided a path based on using selective photo-initiation to control the system properties. To achieve this, we studied the curing kinetics of the two selected systems and the possibility to selectively initiate each system. In the process, we identified photo-initiators that could be more selective than the ones initially used and also studied alternate paths to property control in curing polymer systems. iv Acknowledgments I would like to thank the people who trusted me, encouraged me and helped me during this year. First, I want to thank Dr. Negahban, my advisor, for his precious advice, his supervision and his support. Dr. Tan, my co-advisor, for his explanations about the chemistry and the interpretation of the results, I learned a lot working with him. I would like to thank Dr. Saiter for his expertise and his guidance. Dr. Delpouve, his two visits here were very helpful and I want to thank him too for his guidance. Also, I want to again thank Dr. Saiter and Dr. Negahban who allowed me to participate in this exchange program. Second, I would like to thank my teammates. I have very much appreciated working with them, and they have all helped me improve my English. Next, I would like to thank my friends and my family in France, who have encouraged me this year and my new friends in the USA, with whom I have enjoyed my American life. Finally, I want to especially thank my friends Etienne, Benjamin, and Quentin with whom I have shared this experience, and I would never have done this without their support. Thanks a lot. This thesis was possible with the help of collaborative program between the University of Nebraska-Lincoln, in the United States, and the University of Rouen, in France. v Table of Contents Acknowledgments ................................................................................................................. iv List of figures ....................................................................................................................... vii List of tables .......................................................................................................................... xi Chapter 1: Introduction .............................................................................................................. 1 1.1. Interpenetrating Polymer Networks (IPNs) ................................................................. 2 1.2. IPN observation and detection ..................................................................................... 6 1.3. IPN for constructing spatially graded properties ......................................................... 8 1.4. UV photo-curing .......................................................................................................... 9 Chapter 2: Strategy for IPN design and process characterization ............................................ 12 2.1. General design considerations for IPN construction ................................................. 12 2.2. Issues related to radical and cationic polymerization ................................................ 14 2.3. Selected chemicals ..................................................................................................... 15 2.4. Curing procedure ....................................................................................................... 20 2.5. Curing mechanism ..................................................................................................... 21 2.5.1 Cationic and radical initiators used and their role in the reactions .................... 21 2.5.2 Polymerization reaction for the resins ................................................................ 23 2.6. Post-curing reaction ................................................................................................... 26 2.7. Study of reaction kinetics by Fourier Transformed Infrared Spectroscopy (FTIR) .. 31 Chapter 3: Evidence of the IPN development .......................................................................... 42 vi 3.1. Samples and sample preparation ................................................................................ 42 3.2. AFM microscopy to identify phase separation .......................................................... 43 3.3. Infrared spectroscopy to identify possible chemical interactions between networks 50 3.4. DSC analysis showing the well mixing of resins ...................................................... 55 3.5. Mechanical tests show the effect of composition ratio on tensile properties ............ 58 Chapter 4: From controllable IPN to gradient material ............................................................ 60 4.1. Conversion ratio control ............................................................................................ 63 4.1.1 Problem of photo-initiator selectivity ................................................................ 63 4.1.2 Study of curing kinetics ...................................................................................... 65 4.2. Controlling properties by partial curing followed by removing uncured resins using a solvent ........................................................................................................................ 69 4.3. Other techniques proposed to construct a gradient material ...................................... 76 4.3.1 Selectable photo-initiators
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