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Synthesis and Characterization of Mixed Bismuth Oxide of Nano-Structured Particles

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Synthesis and Characterization of Mixed Bismuth Oxide of Nano-Structured Particles ARISTOTLE UNIVERSITY OF THESSALONIKI FACULTY OF SCIENCES DEPARTMENT OF PHYSICS POST-GRADUATE PROGRAM “NANOSCIENCES & NANOTECHNOLOGIES” Synthesis and Characterization of Mixed Bismuth Oxide of Nano-structured Particles for Soot Oxidation Catalysis Artemis Tsiaprazi-Stamou Supervisor: Prof. Athanasios G. Konstandopoulos THESSALONIKI 2016 ΑΡΙΣΤΟΤΕΛΕΙΟ ΠΑΝΕΠΙΣΤΗΜΙΟ ΘΕΣΣΑΛΟΝΙΚΗΣ ΣΧΟΛΗ ΘΕΤΙΚΩΝ ΕΠΙΣΤΗΜΩΝ ΤΜΗΜΑ ΦΥΣΙΚΗΣ ΔΠΜΣ “ΝΑΝΟΕΠΙΣΤΗΜΕΣ & ΝΑΝΟΤΕΧΝΟΛΟΓΙΕΣ ” Σύνθεση και Χαρακτηρισμός Μικτών Νανο- δομημένων Σωματιδίων Οξειδίου του Βισμουθίου για Ενεργειακές Εφαρμογές Τσιαπράζη-Στάμου Άρτεμις Επιβλέπων: Καθ. Αθανάσιος Γ. Κωνσταντόπουλος ΘΕΣΣΑΛΟΝΙΚΗ 2016 ACKNOWLEDGMENTS - ΕΥΧΑΡΙΣΤΙΕΣ Η Διπλωματική Εργασία εκπονήθηκε στα πλαίσια του Διατμηματικού Προγράμματος Μεταπτυχιακών Σπουδών «Νανοεπιστήμες & Νανοτεχνολογίες» κατά το χρονικό διάστημα Ιανουαρίου 2016 και Δεκεμβρίου 2016 στο Εργαστήριο ΤΕχνολογίας Σωματιδίων & Αερολυμάτων (Ε.ΤΕ.Σ.Α.) του Ινστιτούτου Χημικών Διεργασιών & Ενεργειακών Πόρων (Ι.Δ.Ε.Π.) στο Εθνικό Κέντρο Έρευνας και Τεχνολογικής Ανάπτυξης (Ε.Κ.Ε.Τ.Α.). Στο σημείο αυτό θα ήθελα, να εκφράσω τις ευχαριστίες μου σε όλους όσους συνέβαλαν στην επιτυχή της ολοκλήρωση. Αρχικά θα ήθελα να ευχαριστήσω τον επιβλέποντά μου, Καθηγητή Αθανάσιο Γ. Κωνσταντόπουλο για την εμπιστοσύνη στην ανάθεση και επίβλεψη της παρούσας εργασίας καθώς και για την βοήθειά του στην ανάλυση και ερμηνεία των αποτελεσμάτων. Θα ήθελα να ευχαριστήσω από καρδιάς την Κυριακή Σακελλαρίου για την υποστήριξη και την καθοδήγησή της, τόσο σε επιστημονικό όσο και σε προσωπικό επίπεδο, καθώς ήταν πάντα παρούσα σε οποιαδήποτε αναποδιά, επιστημονικού και διαδικαστικού επιπέδου. Ευχαριστώ θερμά τη Δρ. Σουζάνα Λορέντζου για την υπομονή της απέναντι στο πλήθος των ερωτήσεών μου αλλά και για την προθυμία της να με εξυπηρετήσει ανά πάσα στιγμή. Ευχαριστώ ειλικρινά την Πένυ Μπαλτζοπούλου, αλλά και όλο το προσωπικό του Ε.ΤΕ.Σ.Α. Θα ήθελα πολύ να τους κατονομάσω όλους, αλλά για να μην δώσω έκταση σε αυτό το μήνυμα τους ευχαριστώ όλους ομαδικά. Ο κύριος λόγος είναι ότι η λέξη «ομάδα-οικογένεια» αρμόζει όσο καμία άλλη για να περιγράψει τους ανθρώπους με τους οποίους είτε συνυπήρξα είτε συνεργάστηκα τους δέκα μήνες που διήρκησε η εκπόνηση αυτής της εργασίας. Σας ευχαριστώ λοιπόν όλους ειλικρινά για την επιστημονική και τεχνική καθοδήγηση και βοήθεια από την πρώτη μέχρι και την τελευταία ημέρα. -i- Ευχαριστώ θερμά τους Δρ. Γιώργο Καραγιαννάκη και Δρ. Χριστόφορο Γαβραλίδη, για την συμμετοχή τους στην εξέταση αυτής της διπλωματικής εργασίας. Πέρα από το προσωπικό του Ε.ΤΕ.Σ.Α. θα ήθελα να ευχαριστήσω με όλη μου την καρδιά την οικογένεια μου για την υπομονή και την υλική και ηθική στήριξη στην μέχρι τώρα πορεία μου. ABSTRACT According to an analysis, held by the European Environment Agency (EEA), it is estimated that “air pollution causes 100 million sick days and 350,000 premature deaths in Europe”. Over the last few years, several exhaust gases after treatment technologies have been developed to reduce engine-out emissions. The latter are sources of the main outdoor air pollutants, that is, nitrogen oxides (NOx), volatile organic compounds (VOCs) and particulate matter (PM), which is comprised of solid carbon (soot) and unburned carbonaceous compounds. PM is a major constituent of air pollution and is associated with respiratory and cardiovascular diseases as well as skin cell alterations. In 1976 Ford Motor Company used for the first time CeO2 in their vehicles and since then it is an irreplaceable material for TWC (three way catalysts). The oxidation activity of soot oxidation catalysts is a result of the combination of two different parameters: 1) the oxygen storage capacity (OSC) of the catalyst and 2) its redox properties. The unique ability of CeO2 to shift between Ce4+ and Ce3+ and the ensuing effect in the creation of oxygen vacancy defects are found to be key factors for its application in heterogeneous catalysis. In literature the doping -ii- of CeO2 with ZrO2 is widely studied, as it empowers the catalytic properties of the product. In this study, the goal was the synthesis of nanostructured mixed Bismuth/Cerium oxides via the LPSHS method and their catalytic evaluation as soot oxidation catalysts. The ultimate goal was the replacement of Zr with Bi, as the latter is twice as cheap as the former. In the case of LPSHS method the parameters that were investigated were the calcination treatment, the calcination rate and the (%w/w) quantity of the Bi- doping agent. XRD, SEM, TEM and BET analysis were performed to study the morphology, phase composition and crystallization of the materials. All matrials were evaluated as for their catalytic activity in soot oxidation reaction. Thermogravimetric (TG) Analysis occurred during this study and the results have been analyzed with the aid of a multi-population kinetics model, where soot is found to consist of three fractions reacting with different activation energies, namely 120, 180, and 240 kJ/mol. The occurrence of these three fractions is attributed to the formation of distinct families of surface oxygen complexes (SOCs) on the carbon surface which are subsequently gasified and hence cause soot oxidation, in agreement with accepted mechanisms of soot oxidation in the literature. For further study of the Bi metal, Bi2O3 and BiFeO3 perovskites were synthesized via a variety of synthesis methods, i.e. LPSHS, ASP and Sol-Gel. Their catalytic activity was poor, so they were not considered as promising candidates for the specific application. However, the replacement of Zr with Bi in a defined composition, lead to the synthesis of a catalyst that had similar if not improved catalytic activity. As the price of Zr is twice as higher as the one of Bi it is believed that further economic research should be done in order to investigate the introduction of Bi in the industry of soot oxidation catalysts. -iii- ΠΕΡΙΛΗΨΗ Σε μια από τις τελευταίες αναλύσεις της Ευρωπαϊκής Περιβαλλοντικής Υπηρεσίας, προέκυψε ότι η ατμοσφαιρική ρύπανση προκαλεί περίπου 350,000 θανάτους στην Ευρώπη. Οι ατμοσφαιρικοί ρύποι περιλαμβάνουν οξείδια του αζώτου (ΝΟx), πτητικές οργανικές ενώσεις και σωματιδιακή ύλη, η οποία αποτελείται από στερεό άνθρακα και άκαυστους υδρογονάνθρακες, δηλαδή αιθάλη. Η σωματιδιακή ύλη είναι ο μεγαλύτερος παράγοντας της ρύπανσης του αέρα και συνδέεται με ασθένειες του αναπνευστικού και του καρδιαγγειακού συστήματος, καθώς επίσης και με περιπτώσεις καρκίνου του δέρματος. Η ολοένα και αυξανόμενη ρύπανση του περιβάλλοντος αλλά και οι ενεργειακές απαιτήσεις της σύγχρονης κοινωνίας έχουν μετατοπίσει το ερευνητικό ενδιαφέρον στην ανάπτυξη νέων τεχνολογιών ελέγχου εκπομπής καυσαερίων. Το 1976 η Ford Motor Company εισήγαγε στα οχήματα της τη Ceria (CeO2), το διοξείδιο του δημητρίου, και από τότε είναι ένα ευρέως χρησιμοποιούμενο οξείδιο στη δημιουργία καταλυτών που προκαλούν την οξείδωση της αιθάλης. Οι μοναδικές οξειδοαναγωγικές ικανότητες του δημητρίου, η ικανότητά του δηλαδή να εναλλάσσεται μεταξύ των δύο οξειδωτικών του καταστάσεων Ce+3/Ce+4, και η πολύ καλή θερμική του σταθερότητα, καθιστούν τη Ceria ένα πολύ καλό υλικό για την καταλυτική οξειδωτική καύση της αιθάλης. Το επιστημονικό ερευνητικό ενδιαφέρον εστιάζει στην υποκατάσταση ιόντων δημητρίου στο πλέγμα του CeO2 με ιόντα ζιρκονίου (Zr), καθώς το μικτό οξείδιο των δύο αυτών μετάλλων έχει καλύτερες ιδιότητες. Στόχος της παρούσας εργασίας είναι η σύνθεση νανο-δομημένων υλικών βισμουθίου μέσω αυτοπροωθούμενης αντίδρασης υψηλών θερμοκρασιών στην υγρή φάση (Liquid Phase Self-propagating High-temperature Synthesis, LPSHS) για εφαρμογή σε καταλύτες οξείδωσης της αιθάλης. Το βισμούθιο αναμένεται να λειτουργήσει ως υποκαταστάτης στο πλέγμα του διοξειδίου του δημητρίου/ζιρκονίου για να προσδώσει καλύτερες ιδιότητες στο υλικό. Τελικός στόχος της εργασίας είναι η αντικατάσταση του ζιρκονίου με το βισμούθιο, λόγω του γεγονότος ότι το βισμούθιο είναι κατά πολύ φθηνότερο του ζιρκονίου. Έτσι, -iv- σε πιθανές μελλοντικές εφαρμογές η αντικατάσταση του εν λόγω μετάλλου θα μπορούσε να μειώσει το συνολικό κόστος του προϊόντος του καταλύτη. Στην περίπτωση της μεθόδου LPSHS, οι παράμετροι που εξετάστηκαν ήταν η θερμοκρασία έψησης (calcination), ο ρυθμός έψησης και η ποσότητα (%w/w) του μέσου υποκατάστασης (Bi, «dopant. Τα προκύπτοντα από την αντίδραση προϊόντα χαρακτηρίστηκαν με την μέθοδο της Περιθλασιμετρίας Ακτίνων-Χ (X- Ray Diffraction, XRD), με Ηλεκτρονική Μικροσκοπία Σάρωσης (Scanning Electron Microscopy, SEM) και Διέλευσης (Transmission Electron Microscopy, TEM) για την μελέτη της μορφολογίας, της σύστασης και της κρυσταλλικότητάς τους. Περαιτέρω μελέτη αναφορικά με την καταλυτική τους δράση στην οξειδωτική κατάλυση της αιθάλης πραγματοποιήθηκε στα υλικά μέσω Θερμοσταθμικής Ανάλυσης (Thermogravimetric Analysis). Η ανάλυση των αποτελεσμάτων της Θερμοσταθμικής Ανάλυσης ως προς την εκτίμηση της καταλυτικής ιδιότητας των υλικών έγιναν μέσω ενός κινητικού μοντέλου που λαμβάνει ως παραδοχή την ύπαρξη τριών ειδών πληθυσμών σωματιδιακής αιθάλης, για την οξείδωση καθενός από τα οποία απαιτείται διαφορετική ενέργεια ενεργοποίησης 120, 180 και 240 kJ/mol αντίστοιχα. Η ύπαρξη των τριών αυτών πληθυσμών εκφράζεται μέσω ενός κλάσματος φi και συνδέεται με την ύπαρξη διαφορετικών ομάδων επιφανειακών ενώσεων του οξυγόνου που ενώνονται με την αιθάλη, μέσω απλών, διπλών ή και τριπλών δεσμών. Για την πλήρη αξιολόγηση των αποτελεσμάτων της Θερμοσταθμικής Ανάλυσης, πραγματοποιήθηκε σύνθεση του οξειδίου του βισμουθίου. Για τη σύνθεσή του έλαβαν χώρα και άλλες μέθοδοι σύνθεσης όπως η μέθοδος Πυρόλυσης Νέφους Αερολύματος,
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