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Post Plasma Etch Residue Removal Using Carbon POST PLASMA ETCH RESIDUE REMOVAL USING CARBON DIOXIDE BASED FLUIDS A Dissertation Presented to The Academic Faculty By Satyanarayana Myneni In Partial Fulfillment Of the Requirements for the Degree Doctor of Philosophy in Chemical Engineering Georgia Institute of Technology December 2004 POST PLASMA ETCH RESIDUE REMOVAL USING CARBON DIOXIDE BASED FLUIDS Approved by: Dr. Dennis W. Hess, Advisor (ChBE) Dr. Charles A. Eckert (ChBE) Dr. Charles L. Liotta (CHEM) Dr. J. Carson Meredith (ChBE) Dr. Amyn S. Teja (ChBE) October 13, 2004 ACKNOWLEDGEMENTS First of all, I would like to thank my advisor Dr. Dennis Hess for his guidance and support during this research. His extensive knowledge of this area and constant encouragement has been invaluable for the successful completion of this project. The best thing I liked about working with Dr. Hess was that he was always available to guide my research while encouraging me to pursue independent ideas. He has always encouraged critical thinking and attention to details of any problem without losing focus of the bigger picture. I also want to thank Dr. Charles Eckert, Dr. Charles Liotta, Dr. Carson Meredith, and Dr. Amyn Teja for serving on my committee and providing valuable suggestions during this work. Funding for this work has been provided by Novellus Systems, Inc., and National Center for Environmental Research STAR program (EPA contract no. R-82955401) and is greatly appreciated. I also want to thank Novellus Systems, Inc. for providing low-k etch residue samples. This work would not have been complete without direct contribution from Dr. Galit Levitin. In addition to performing phase behavior measurements, she has provided experimental assistance and valuable suggestions throughout the project. I am grateful to her for being a great mentor and a friend. I want to thank every member, present and past, of Dr. Hess’s research group for helping me with ideas and making life at graduate school a very enjoyable and memorable experience. In particular, many thanks to Chris Timmons for helping me with setting up equipment and for brainstorming with me, to Jie Diao for help with cleanroom processing and providing the code for ARXPS, and to Sudeep Vaswani for depositing fluorocarbon films in his plasma reactor. iii During this research, I have obtained assistance from several faculty and research groups. I am grateful to Dr. Charles Eckert, Dr. Cliff Henderson, Dr. Paul Kohl, Dr. Amyn Teja, and Dr. Brent Carter (MSE) for allowing me to use the equipment in their labs. I want to thank Dr. David Gidley and his graduate student Huagen Peng at University of Michigan for performing the PALS measurements. I also want to thank the staff at Microelectronics Research Center (in particular Gary Spinner and Scott Fowler) for always willing to help with any equipment related issues. Many thanks also to Linda Perry and Gloria Beale of ChBE for placing countless purchase orders that allowed my work to run smoothly. Jeff Andrews of the ChBE machine shop has fabricated the optical window assembly and the ATR-FTIR cell, which made all my in-situ experiments possible. I want to thank all my friends at Georgia Tech for providing great company and a balance between work and life. In particular, many thanks to Suraj Nair and Rajesh Rajaram for putting up with me for four years as roommates. Finally, I want to thank my family. My parents have made great sacrifices to provide me with the best possible education and family environment. They have always had great faith in me and have supported me during every step of my life. I have received moral support and constant encouragement from every member of my family, including my sister and brother-in-law, which made this research possible. iv TABLE OF CONTENTS ACKNOWLEDGEMENTS iii TABLE OF CONTENTS v LIST OF FIGURES ix LIST OF TABLES xiv SUMMARY xv Chapter 1 1 INTRODUCTION 1 Chapter 2 7 BACKGROUND AND LITERATURE REVIEW 7 2.1 Dual damascene processing 7 2.2 Etch residue formation and characterization 13 2.2.1 Photoresist background 13 2.2.2 Dielectric etch mechanism 16 2.2.3 Line-of-sight residue formation 19 2.2.4 Sidewall residue formation 23 2.2.5 Photoresist residue formation 26 2.3 Etch residue removal 29 2.3.1 Residue removal by plasma ashing and other dry methods 29 2.3.2 Post ash cleaning 32 2.3.3 Residue removal by liquids 33 2.4 CO2 based fluids for etch residue removal 36 2.4.1 CO2 applications in the IC industry 37 v 2.4.2 CO2 for cleaning applications 38 2.4.3 Surfactants for CO2 39 2.5 Organization of the thesis 41 Chapter 3 43 EXPERIMENTAL METHODS AND ANALYTICAL TECHNIQUES 43 3.1 High pressure cleaning system 43 3.2 Titrimetric analysis 46 3.3 X-ray photoelectron spectroscopy 48 3.4 Attenuated total reflection – Fourier transform infrared spectroscopy 53 3.5 Dissolution rate monitor 58 3.6 Variable angle spectroscopic ellipsometry 64 3.7 Positronium annihilation lifetime spectroscopy 67 Chapter 4 71 FORMATION AND CHARACTERIZATION OF TEST SAMPLES AND MODEL FILMS 71 4.1 Description of the test samples 71 4.2 Etch residue sample characterization 73 4.2.1 X-ray photoelectron spectroscopy 73 4.2.2 Fourier transform infrared spectroscopy 75 4.2.3 Estimation of the fluorocarbon residue thickness 80 4.3 Deposition of model films 85 4.3.1 Photoresist thin films 85 4.3.2 Model photoresist residues 86 4.3.3 Model fluorocarbon residues 92 vi Chapter 5 95 FORMULATION OF CO2 BASED CLEANING MIXTURES FOR RESIDUE REMOVAL 95 5.1 Introduction 95 5.2 Initial beaker studies 95 5.2.1 Correlation between XPS and SEM 95 5.2.2 Photoresist dissolution mechanism 98 5.2.3 Organic solvents 99 5.2.4 Residue removal using bases 102 5.3 Reactions between CO2 and TMAH 107 5.4 High pressure cleaning experiments 111 5.5 Conclusions 113 Chapter 6 114 ETCH RESIDUE REMOVAL USING CO2-TMAHCO3-METHANOL MIXTURES 114 6.1 Introduction 114 6.2 Phase behavior of CO2-TMAHCO3-methanol mixtures 116 6.3 High pressure cleaning studies 120 6.3.1 Determination of minimum co-solvent flow rate 120 6.3.2 Effect of temperature 121 6.3.3 Comparison of single phase and two phase mixtures 122 6.4 Post treatment rinsing 127 6.5 Conclusions 130 Chapter 7 132 MECHANISTIC STUDIES 132 7.1 Introduction 132 vii 7.2 Dissolution of the soft photoresist 135 7.3 Chemical attack of the fluorocarbon residue 138 7.4 Undercut of the residues 142 7.5 Role of CO2 144 7.5.1 Angle-resolved XPS 145 7.5.2 Attenuated total reflection - Fourier transform infrared spectroscopy 148 7.6 Role of TMAHCO3 152 7.7 Analysis of the crust 156 7.8 Conclusions 160 Chapter 8 162 EVALUATING THE COMPATIBILITY OF CO2-TMAHCO3-METHANOL MIXTURES WITH A POROUS LOW DIELECTRIC FILM 162 8.1 Introduction 162 8.2 Experimental 166 8.3 Results and discussion 167 8.3.1 Samples without capping layer 168 8.3.2 Samples with capping layer 173 8.3.3 Porosity from variable angle spectroscopic ellipsometry 175 8.4 Conclusions 177 Chapter 9 179 SUMMARY AND RECOMMENDATIONS FOR FUTURE WORK 179 9.1 Summary 179 9.2 Recommendations for future work 185 REFERENCES 191 VITA 204 viii LIST OF FIGURES Figure 1.1. Progression of technology node and number of transistors in Intel’s microprocessors [3]. ............................................................................2 Figure 1.2. Illustration of lithography process used to pattern planar layers in IC fabrication [8].............................................................................................4 Figure 2.1. Illustration of the multi-layered interconnect structure in an integrated circuit (IC) device [16]...................................................................8 Figure 2.2. Via first dual damascene processing sequence [21]: a) film stack deposition, via lithography b) via etch c) etch residue removal d) trench lithography e) trench etch f) etch residue removal g) etch stop barrier breakthrough, metal contact clean h) copper diffusion barrier, copper seed layer deposition i) copper electroplating j) chemical mechanical polishing. The cleaning steps are enclosed in boxes. ..........................................................................11 Figure 2.3. Chemical structures of some of the low dielectric permittivity materials pursued as intermetal and interlevel dielectrics [23].....................12 Figure 2.4. Chemical amplification mechanism in a 248 nm photoresist [26]..................14 Figure 2.5. Mechanism of photoresist hardening by DUV-Bake prior to plasma etching [30].......................................................................................15 Figure 2.6. Surface processes leading to residue formation during plasma etching of a via or a line [36]........................................................................17 Figure 2.7. Etch rate dependence on DC bias (ion energy) for SiO2 etching in an ICP reactor [35]........................................................................................20 Figure 2.8. Schematic of fluxes of species that are incident on and outgoing from (a) Si, (b) Si3N4, and (c) SiO2 during plasma etching. Also shown are the relative thicknesses of fluorocarbon films deposited during the etching process [45]. ...................................................22 Figure 2.9. Cross-sectional SEM image of a plasma etched via with sidewall polymer [52]..................................................................................................25 Figure 2.10. Cross-sectional SEM image showing post plasma etch photoresist residue [60]. ..................................................................................................27 Figure
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