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Novel Geopolymers Incorporating Silicate Waste

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Novel Geopolymers Incorporating Silicate Waste Novel geopolymers incorporating silicate waste Neuartige Geopolymere aus silikatischen Industrieabfällen Der Technischen Fakultät der Friedrich-Alexander-Universität Erlangen-Nürnberg zur Erlangung des Grades DOKTOR-INGENIEUR vorgelegt von Nicoletta Toniolo aus Velo d´Astico, Italy Als Dissertation genehmigt von der Technischen Fakultät der Friedrich-Alexander-Universität Erlangen-Nürnberg Tag der mündlichen Prüfung: 27.07.2018 Vorsitzende des Promotionsorgans: Prof. Dr. –Ing. Reinhard Lerch Gutachter: Prof. Dr.-Ing. habil. Aldo R. Boccaccini Prof. Enrico Bernardo Prof. Cristina Leonelli “Al mio angelo custode” I II Acknowledgements Firstly, I would like to express my sincere gratitude to Prof. Aldo Boccaccini, supervisor and head of the Institute of Biomaterials, who gave me the opportunity to do my PhD research at his Institute. I want to thank him for all the support during the past 3 years, all the suggestions he gave me and for the opportunity to take part to numerous international conferences, which were important for my knowledge and my personal experience. This research project was carried out within the framework of the poject “CoACH”, funded under the Marie Sklodowska-Curie action of the EU funding program for research and innovation “Horizon 2020”. I am grateful for the financial support it gave me. Thanks to the coordinator of the project Monica Ferraris, Milena Salvo and Cristiana Contardi, thanks for being always available, thanks for organizing meetings, training, etc. I really enjoyed everything. A super thanks to my “CoACH” fellows, I really think that it would have been impossible for me to have better project mates: thanks to Fra, for all the time together, for organizing all the meetings together, for supporting me and listening to my presentation 100 times. Thanks to Cava per le mille chiacchierate! Thanks to Acacio, you have been more than a support for me, thanks for all the scientific support, thanks for the thousand laughs in Sasil, thanks for introducing me to Lindy hop and of course for all the beers together. Thanks to Ale e Rocio, thanks for all the gossip and the evening chats, thanks to Giamma per avermi sopportato un mese a Brno, Min, who taught me that I should be proud of my curly hair , Pablo, Cristian, Hassan, Bhuva, Silviu, Francesco, Katarzyna, Thanks a lot Coachitos, I will really miss our time together! I would like to thank all the PhD students of UNIPD that helped me a lot during my secondment in Padova, especially to Elena, Giamma, Alberto. A special thanks to Prof. Enrico Bernardo for encouraging me to do this PhD and for the support throughout the 3 years, grazie veramente. Thanks also to the members of the IPM group, where I spent one intensive month of mechanical characterizations, thanks to Ivo Dlouhy to supervise my experiments there. III I am thankful to Piero Ercole, who took care of my research since the first moment, thanks to Ludovico Ramon, Alessandra La Barbera and all the laboratory staff in Sasil which helped me during the two intensive months I spent in the company. Thanks to my students Philipp Müller and Sebastian Schulte, for helping me with the experiments and for teaching me to be patient. Thanks a lot to the people that helped me with the characterizations: Dr. Judith A. Roether, thanks for your availability and kindness, Harald Rost, Dr. Liliana Liverani, Dr. Yamini Avadhut, Dr. Giulia Zanmarchi and Prof. Jan Dusza. Thanks to all the members of the Biomaterials Institute. Thanks to Julia Will for all the discussions, the important advices and die Deutschunterricht.. Vielen Dank! Thanks to Heinz Maler, always available to solve my problems and to Gerhard Frank, who I disturbed every SEM section. To Frau Bärbel Wust, she was always available to help me with expeditions and travels, moreover thanks for trying to understand my German, Danke. Thanks to Jasmin and Alina for helping me with the lab organization and orders. Thanks to my office colleagues: Valentina, Marfa, Eyerusalem, Ranjot, Diana, thanks for the discussions about geopolymers, thanks for the time together in the lab and of course for the coffee, the cupcakes and all the breaks together, we will start the diet tomorrow ! Thanks to all my colleagues, Barbarita for pushing me all the time towards the goal, Agata, Samira, Lukas, Laura, Marcela, Vera, Florian, Lena, Atiq, Kai, Svenja, Agata, Katharina, Irem, thanks a lot for these three years together, I will never forget you! Thanks to my special friends in Erlangen: Crystel, thanks for trying to improve my English, Andy, Antonina, Sofia, Giacomo, Natascia, thanks for all the adventures, the game evenings, the beers and remember that we are the best to crash party. To all my friends in Italy, for the infinite vocal messages, and in particular for being always ready to party everytime I went back to Italy: Marta, Erica, Roby, Obe, Marta, Grazie ragazze!!! Thanks to my family, for supporting always my choices also when they were not easy to support, a special thanks to my nephews whose video fills my heart. Thanks to Alex, grazie per tutto il supporto, per la pazienza che hai avuto e che avrai, grazie perche´al tuo fianco mi sento una persona migliore! IV Abstract Increasing global warming has raised concerns on the extensive use of Portland cement due to the high amount of carbon dioxide gas associated with its production. For this reason the construction industry is increasingly turning to the use of environmentally friendly materials in order to meet the sustainability targets required for modern infrastructures. Geopolymers are a new class of construction materials developed primarily as an ecofriendly and sustainable alternative to conventional cement-based construction materials. Although research into geopolymers is significantly increasing, most studies have used raw virgin materials or chemical reagents such as metakaolin or sodium silicate, which then raises issues of sustainability and environmental responsibility. To compete with the inexpensive nature of cement and to ameliorate the buildup of waste materials, thus decreasing the strain on landfill space, this study has investigated the use of industrial by-products such as fly ash, waste glass and red mud, in place of virgin raw materials for production of a new family of geopolymers. Initially, fly ash-based geopolymers were developed and the incorporation of red mud or waste glass in the matrix was investigated. The results show that the mechanical properties decrease as the amount of waste glass in the geopolymer increases; on the other hand, the addition of red mud seems to improve the mechanical behavior. Leaching tests were carried out to confirm the capacity of the geopolymer materials to incorporate and stabilize pollutants inside the network. In order to improve the economic and environmental value of geopolymers, the possibility of partially replacing traditional alkaline activators such as sodium silicate, also called waterglass, with urban waste glass was extensively evaluated. Fly ash-based geopolymers and red-mud based geopolymers were developed using waste glass as the silica supplier and sodium hydroxide as the alkaline solution, avoiding altogether the use of waterglass. The incorporation of soda lime glass waste instead of waterglass represents an innovation in geopolymer research. The influence of the addition of waste glass as well as the molarity of the sodium hydroxide solution was investigated for both the microstructure and mechanical strength of the geopolymers. The results suggested that it is possible to incorporate V up to a 60 wt.% of waste glass while still achieving comparable strength to Portland cement. This strength is also attained within a relatively short setting time of circa 7 days. The formation of a geopolymer gel was confirmed by XRD and MAS-NMR analyses. In addition, the XRD technique confirmed the formation of crystalline zeolite phases. Red mud-based geopolymers achieved relatively high compressive strength, 45 MPa, which is extremely interesting given the significant amount of red mud incorporated (60wt.%). Moreover, these geopolymers were developed through an economic process that does not require high temperatures or foaming agents. The light-weight geopolymers, synthesized with the same formulation of the dense materials, have high porosity and acceptable mechanical properties (1 MPa), though, the chemical stability should be improved through future research. In order to expand the range of possible applications, wear resistance and a thermal shock test were carried out obtaining satisfactory results for applications where material degradation in wear and under a sudden temperature change is required. 3D printing and mechanical machining of the developed samples were additionally carried out. The geopolymers were successfully extruded with a 3D printing machine and drilled and worked on the lathe achieving complex shapes and components with accurate surface finish, interesting for expanding the applications of the geopolymers in other industrial sectors beyond constructions. Overall, the outcomes of this study highlight geopolymers as a promising candidate not only for building and construction applications but also for other engineering applications. In particular in areas where specific and accurate shapes are required. The present research has contributed new insights and generated knowledge in the geopolymers field. Geopolymer materials represent an innovative solution for the reuse of waste materials while achieving sound mechanical
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