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Preparasi Dan Karakterisasi Glassy Ce3+ Dan Mn2+- Doped Caal2o4 Powder Dengan Metode Spray Pyrolysis

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Preparasi Dan Karakterisasi Glassy Ce3+ Dan Mn2+- Doped Caal2o4 Powder Dengan Metode Spray Pyrolysis HALAMAN JUDUL TESIS – TL142501 Preparasi dan karakterisasi glassy Ce3+ dan 2+ Mn - doped CaAl2O4 powder dengan metode spray pyrolysis A MARSHA ALVIANI NRP. 02511650010008 DOSEN PEMBIMBING Dr. Widyastuti., S.Si., M.Si. Dr.Eng. Hosta Ardyananta., ST., M. Sc. Prof. Shao-Ju Shih PROGRAM MAGISTER BIDANG KEAHLIAN MATERIAL INOVATIF DEPARTEMEN TEKNIK MATERIAL FAKULTAS TEKNOLOGI INDUSTRI INSTITUT TEKNOLOGI SEPULUH NOPEMBER SURABAYA 2018 (This page intentionally left blank) THESIS – TL142501 Preparation and characterization of glassy Ce3+ 2+ and Mn -doped CaAl2O4 powder using spray pyrolysis A MARSHA ALVIANI NRP. 02511650010008 ADVISOR Dr. Widyastuti., S.Si., M.Si. Dr.Eng. Hosta Ardyananta., ST., M. Sc. Prof. Shao-Ju Shih MASTER DEGREE PROGRAM MATERIAL INOVATIVE DEPARTEMENT OF MATERIAL ENGINEERING FACULTY OF INDUSTRIAL TECHNOLOGY INSTITUT TEKNOLOGI SEPULUH NOPEMBER SURABAYA 2018 (This page intentionally left blank) i ii ABSTRAK Inorganic luminescence material atau biasa disebut dengan phosphor telah diaplikasikan secara luas seperti security label, emergency signalling, solid state, dan laser light-emitting diodes (LEDs). Saat ini, phosphor sebagai security label dapat ditemukan di uang, paspor, dan beberapa kertas penting. Sebagai tambahan, Shih et al, menerangkan terkait amorfus gehlenite sebagai material phosphor yang memiliki distribusi partikel yang baik. Selain itu untuk membandingkan aplikasi dengan fasa amorfus, glassy phosphor akan diteliti lebih lanjut dalam riset ini. Dalam penelitian ini, calcium aluminate (CaAl2O4) digunakan karena memiliki beberapa karakteristik seperti long after glow time, stabilitas kimia yang baik, tidak beracun, harga murah, dan efisiensi kuantum yang tinggi pada visible 3+ 2+ region. Dalam penelitian ini Ce , Mn doped with CaAl2O4 dibuat menjadi fasa o amorfus. Annealing temperature pada 800 C pada 95%N2/ 5%H2 digunakan untuk mereduksi Ce4+ menjadi Ce3+ dan Mn4+ menjadi Mn2+. Untuk mendapatkan fasa 3+ 2+ CaAl2O4:Ce , Mn , terdapat beberapa karakterisasi yang dilakukan. Seperti, X- ray diffraction (XRD). Untuk mengetahui morfologi permukaan digunakan scanning electron microscopy (SEM). Selain itu untuk mengetahui sifat photoluminescecne menggunakan alat photoluminescence spectra (PL), karakterisasi panjang gelombang yang digunakan pada 273 nm. Maksimum komposisi untuk meningkatkan intensitas dari sinar biru-hijau adalah 0.5%Ce3+ 2+ and 1%Mn in CaAl2O4. Kata kunci : Calcium aluminate, Ce/Mn, luminescence, amorphous iii (This page intentionally left blank) iv ABSTRACT Inorganic luminescent materials (also known as phosphors), have been extensively studied in numerous application such as security label, emergency signalling, solid state, and laser light-emitting diodes (LEDs). Nowadays, phosphor for security labels can be found in money, passport, and other important paper. In addition, Shih et al determined that amorphous gehlenite phosphor material have a good activator particle distribution. Therefore, as compared to the application and amorphous phase superiority, glassy phosphor will be further investigated in this study. In this research calcium aluminate (CaAl2O4) is used because it has special characteristics such as long after glow time, good chemical stability, low toxicity, low cost, and high quantum efficiency in the visible region. 3+ 2+ In this study, Ce , Mn doped with CaAl2O4 were synthesized with amorphous o phase. Annealing temperature at 800 C in 95%N2/ 5%H2 condition was used to 4+ 3+ 4+ 2+ 3+ reduce Ce to Ce and Mn to Mn . The obtained phosphor CaAl2O4:Ce , Mn2+ phase was characterized by X-ray diffraction technique (XRD). The surface morphology was determined by scanning electron microscopy (SEM). Also photoluminescence spectra (PL), characterization were done with excitation at 273 nm. The maximum composition to increase the intensity of the blue-green 3+ 2+ light is 0.5%Ce and 1%Mn in CaAl2O4. Keywords: Calcium aluminate, Ce/Mn, luminescence, amorphous v (This page intentionally left blank) vi ACKNOWLEDGEMENTS There are many people I would like to thank for being part at this work. First of all, I would like to thank to Allah SWT, the greatest God in this world that gives me a lot of favours. Then I would like to thank to my advisor, Prof. Shao-Ju Shih for the opportunity to do a research under his supervision and always supporting me to finish this thesis on time. I would like to say many thanks to my advisor in Indonesia Dr. Widyastuti who supported me to continue for Master Degree and finished this thesis. I would like to thank to NGB lab family, Fetene, Abadi, Bo Jiang, Tim Lin, Fred, Janet, Tim Sun, Henni, Kevin, Stacey, Peggy, Chen Yan, Guang Ge, Peter, Hana, Emma, Candy, and Shun, who always helped and supported me to conduct this thesis. I would like to say thank to NGB lab alumni, Andy, Cho Wei, Dimas, and Parindra, who helped me to solve a lot of problem. I would like to thank to all of my family in Indonesia especially my mom, my father, my brother, my grandmother, my aunt, and my uncle who have encouraged me every time to finish my study. I would like to say my gratitude to my all of my friends especially my roommates, Frizka, Isabel, Yimen, Sirima Keang, and Ery. I would like to say my gratitude to Indonesian student in Material Science and Engineering Department, who always helped me, especially Bang Noto. I would like to say my gratitude to UNIMIG Taiwan, Salimah family, and all Indonesian organization in Taiwan who always supported and gave me their love. I would like to say my gratitude to ITS Career Centre team, the best partner, who always supported me. I would like to say my gratitude to Al Khansa family. I would like to say so many thanks to post crossing member, who gave me a lot of suggestion by their postcard, it made me cheerful again when I got the postcard. I also would like to say thank you for all my friends that I could not mention. vii (This page intentionally left blank) viii CONTENT APPROVAL SHEET ............................................. Error! Bookmark not defined. ABSTRAK ............................................................................................................. iii ABSTRACT ............................................................................................................ v ACKNOWLEDGEMENTS .................................................................................. vii CONTENT ............................................................................................................. ix LIST OF TABLES ............................................................................................... xiii LIST OF FIGURES............................................................................................... xv CHAPTER 1 INTRODUCTION ............................................................................ 1 1.1 Background............................................................................................... 1 1.2 Objective................................................................................................... 2 CHAPTER 2 LITERATURE REVIEW ................................................................. 3 2.1. Luminescence material ............................................................................. 3 2.1.1 Afterglow duration ............................................................................ 3 2.1.2 Light source mechanism ................................................................... 5 2.2 Luminescence mechanism ........................................................................ 9 2.3 Luminescent security label application .................................................. 12 2.4 CaAl2O4 characteristics .......................................................................... 13 2.5 Activator characteristics ......................................................................... 16 2.5.1 Cerium ............................................................................................. 16 2.5.2 Manganese....................................................................................... 16 2.6 Spray pyrolysis method .......................................................................... 19 CHAPTER 3EXPERIMENTAL METHOD ......................................................... 21 3.1 Chemicals ............................................................................................... 21 3.2 Experimental procedure.......................................................................... 21 3.3 Material preparation ............................................................................... 22 3.3.1 Adjusting annealing temperature .................................................... 22 3.3.2 Adjusting atmospheric gases condition ........................................... 25 3.3.3 Variation of cerium and manganese composition ........................... 28 3.4 Materials characterization ...................................................................... 30 3.4.1 X-ray diffraction.............................................................................. 30 3.4.2 Scanning electron microscope......................................................... 30 ix 3.4.3 Spectrofluorometer .......................................................................... 30 CHAPTER 4 RESULTS ........................................................................................ 33 4.1 Adjusting temperature ............................................................................. 33 4.1.1 Phases analysis ...............................................................................
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