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© Copyright by Prithvi Basu 2013 All Rights Reserved © Copyright by Prithvi Basu 2013 All Rights Reserved Optimization of Reactive Ion Etching to Fabricate Silicon Nitride Stencil Masks in SF6 Plasma A Thesis Presented to the Faculty of the Department of Electrical and Computer Engineering University of Houston In Partial Fulfillment of the Requirements for the Degree Master of Science in Electrical Engineering by Prithvi Basu August 2013 Optimization of Reactive Ion Etching to Fabricate Silicon Nitride Stencil Masks in SF6 Plasma Prithvi Basu Approved: Chair of the Committee Paul Ruchhoeft, Associate Professor Electrical and Computer Engineering Committee Members: Dmitri Litvinov, Professor Electrical and Computer Engineering Richard C. Willson, Professor Chemical and Biomolecular Engineering Suresh K. Khator, Associate Dean Badri Roysam, Professor and Chair Cullen College of Engineering Electrical and Computer Engineering Acknowledgements I would foremost like to thank my advisor, Dr. Paul Ruchhoeft, for all his guidance and support towards the completion of my master’s degree. I would also like to thank Carmen Pascente, Gauri Samel, and David Shakarisaz for being excellent lab mates and their invaluable advice on numerous problems. I would also like to acknowledge Azeem Nasrullah, Tim Sherlock, and Jon Elizalde for all of their training and assistance during the initial stages of my research. Finally, I would like to thank my parents: Bhaskar Basu and Shikha Basu for many years of both emotional and financial support. v Optimization of Reactive Ion Etching to Fabricate Silicon Nitride Stencil Masks in SF6 Plasma An Abstract of a Thesis Presented to the Faculty of the Department of Electrical and Computer Engineering University of Houston In Partial Fulfillment of the Requirements for the Degree Master of Science in Electrical Engineering by Prithvi Basu August 2013 vi Abstract Stencil masks are used to print ultra-high resolution patterns using helium ion/atom beam lithography and are often manufactured from thin, free-standing silicon nitride membranes. The masks have sub-200nm openings etched through the thickness of the membrane using a reactive ion etch (RIE) process that determine the printed pattern. This project deals with the optimization of a sulfur hexafluoride and oxygen RIE. In this process, 0.5µm thick silicon nitride membranes are coated with 20nm of copper (hard mask) and 200nm of poly (methyl methacrylate) (resist). The desired patterns are then formed in the resist by electron beam lithography, and the patterns are transferred through copper by argon milling. A mixture of 0.8 millitorr of sulfur hexafluoride and 0.2 millitorr of oxygen is used in an RIE step at a power of 15 watts to transfer them through the thickness of the membrane. The process allows for the patterning of extremely straight features (anisotropic etch), has excellent selectivity (200) between silicon nitride and copper, suffers from minimal RIE lag, and is generally very robust. The challenges associated with this process lie in etch non-uniformity due to membrane heating and pattern fidelity in the milling step. Solutions to these problems have been explored and stencil masks with sub-200 nm etched openings have been successfully fabricated. vii Table of Contents Acknowledgements .............................................................................................. v Abstract ............................................................................................................ ...vii Table of Contents .............................................................................................. viii List of Figures ..................................................................................................... x List of Tables ...................................................................................................... xiii Chapter 1 Introduction and Background ............................................................. 1 1.1 Ion Beam Proximity Lithography ........................................................ 1 1.2 Scope of the Project .......................................................................... 4 Chapter 2 Plasma Etching and Stencil Masks: Literature Review ...................... 6 2.1 Reactive Ion Etching .......................................................................... 8 2.2 Sputtering .......................................................................................... 12 2.3 Selectivity and Anisotropy .................................................................. 14 2.4 Stencil Masks .................................................................................... 16 Chapter 3 Fabrication Tools ............................................................................... 23 3.1 Thermal Evaporator ........................................................................... 26 3.2 Reactive Ion Etcher ............................................................................ 29 Chapter 4 Stencil Mask Fabrication .................................................................... 31 4.1 Membrane Formation ........................................................................ 31 viii 4.2 Wet Etch Process .............................................................................. 32 4.2.1 Process Flow of Wet Etch Fabrication .................................. 33 4.2.2 Results and Discussion ........................................................ 34 4.2.3 Annealing at PMMA Glass Transition Temperature .............. 35 4.2.4 Conclusion ............................................................................ 37 4.3 Dry Etching Technique ...................................................................... 38 4.3.1 Process Flow of Dry Etch Fabrication ................................... 40 4.3.2 Etching of Silicon Nitride Membrane ..................................... 41 4.3.3 Membrane Etching With Metal at the Back ........................... 45 4.3.4 Uniformity in Membrane Etching ........................................... 51 4.3.5 Conclusion ............................................................................ 56 Chapter 5 Variation of Etch Rates and Selectivity with Power ............................ 57 Chapter 6 Summary ........................................................................................... 61 References ......................................................................................................... 62 ix List of Figures Figure 1.1 Schematic diagram of how ion beam proximity lithography works ...... 3 Figure 2.1 Schematic diagram of plasma etch reactor ........................................ 7 Figure 2.2 Simple diagram of RIE process ......................................................... 11 Figure 2.3 Diagram showing collision cascade in sputtering .............................. 13 Figure 2.4 Diagram showing principle of magnetron sputtering .......................... 14 Figure 2.5 Example of selective etching between resist, film and oxide ............. 15 Figure 2.6 Diagram explaining the degree of anisotropy in anisotropic etch ...... 16 Figure 2.7 Schematic diagram of a stencil mask, taken from ref. [3] .................. 18 Figure 2.8 Mask fabrication process flow using palladium and PMMA ............... 20 Figure 2.9 Diagram of a grid support stencil mask, taken from ref. [2] ............... 22 Figure 2.10 Fabrication of a grid support stencil mask, taken from ref. [2] ......... 23 Figure 2.11 Scattering effect of ions in a stencil mask with (a) mask thickness similar to ion range and (b) a thicker mask, taken from ref. [4] ................... 25 Figure 3.1 Schematic diagram of the thermal evaporator ................................... 27 Figure 3.2 Schematic diagram of the reactive ion etcher .................................... 30 Figure 4.1 Process flow diagram of the wet etch process of mask fabrication using 10nm of copper and 70nm of PMMA .............................................. 33 Figure 4.2 Image of silicon nitride wafer after 18 seconds of wet etch in citric acid .................................................................................................. 34 Figure 4.3 Image of silicon nitride wafer after 5 minutes of wet etch in citric acid after annealing PMMA at its glass transition temperature ............... 36 x Figure 4.4 Images of silicon nitride wafer after RIE in SF6 and oxygen for 30 minutes .......................................................................................... 36 Figure 4.5 Undercutting leading to mask failure due to isotropic etch ................ 38 Figure 4.6 Process flow diagram for mask fabrication using dry etch technique using 20nm of copper as hard mask and 200nm of PMMA as photoresist ............................................................................................... 41 Figure 4.7 SEM images of front side of a silicon nitride membrane of (a) 5µm (b) 700nm (c) 500nm (d) 300nm (e) 200nm (f) 100nm features etched through in SF6 and oxygen for an hour..................................................... 43 Figure 4.8 SEM images of back side of a silicon nitride membrane of (a) 700nm (b) 300nm (c) 200nm (d) 100nm features etched through in SF6 for an hour ..................................................................................... 44 Figure 4.9 Silicon nitride membranes with (a) no metal and (b) metal at back ... 45 Figure 4.10 SEM images of front side of a silicon nitride membrane of (a) 5µm (b) 500nm features etched through in SF6 and oxygen for an hour with 100nm gold at
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