ETCHING OF SILICON NITRIDE WITH HIGH TEMPERATURE WATER AND DEUTERIUM OXIDE
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1 ETCHING OF SILICON NITRIDE WITH HIGH TEMPERATURE WATER AND DEUTERIUM OXIDE Joshua Barclay, Jesse Smith, Rick Reidy Department of Materials Science and Engineering University of North Texas, Denton TX (979)
2 Outline Rationale Deuterium oxide Dissociation of water and D 2 O Experimental conditions Results Ellipsometry SEM Molybdate blue UV-Vis (dissolved silica) ATR D 2 O post etch liquid Etch rate comparison Summary Future work
3 Rationale SiN is commonly etched using 160 C (85%) H 3 PO 4 --it is widely believed that the principal etchant is water At this temperature, surface Si-N are protonated followed by water attack creating Si-OH (soluble groups)* Previous work showed high temperature water (HTW) is an effective etchant for SiN Compare HTW and HT deuterium oxide (HTD 2 O) to understand the etching mechanism Because dissociation of D 2 O is 10x less than H 2 O *Martin Knotter, Handbook for Cleaning for Semiconductor Manufacturing: Fundamentals and Applications, Chapter 3, Scrivener, 2011
4 Deuterium Oxide (D2O) H 2 O D 2 O N + + N N N N N + + N N N N g/mol Boiling Point 100 C Vapor Pressure 23.8 torr g/mol Boiling Point C Vapor Pressure 20.6 torr
5 Dissociation pk w H2O D2O D2O estimated Temperature ( C) H 2 O 140 C pk w =11.71 D 2 O 140 C pk w =12.56 H 2 O 160 C pk w =11.53 D 2 O 160 C pk w =12.35 Order of magnitude difference in reactive specie concentration between H 2 O and D 2 O AV Bandura, AN Lvov, J. Phys and Chem Ref Data 35 (1) 15 30, 2006 DW Shoesmith, W Lee, Can J. Chem, 54, , 1976
6 Experimental Conditions 30ml water and D 2 O Heated to 140, 160 C ramp time: 120 mins Hold times of 0,10,20 min at temp 3 samples for each condition P equil, H 2 O (140 C) = 3.5 atm P equil, H 2 O (160 C) = 6.1 atm Reactor is quickly cooled with water Post etch water is collected for characterization 140/160 C SiN
7 Post Etch Thickness (Å) Thickness Losses DI Ellipsometry Results D2O Samples Etch Rate (Å /min ) D 2 O 140 C 24±8 D 2 O 160 C 30±8 DI 140 C 25±12 DI 160 C 45±9 HTW and HTD 2 O remove same amount of material HTW etches slightly faster at 160 C Etching more dependent on temperature than reactive species concentration
8 SEM 140 C D 2 O 140 C 0 min 20 min Di 140 C 0 min 20 min 310nm 275nm 315nm 270nm SEM images of 140 C samples agree with ellipsometry results Given the dissociation behavior, expected HTW to etch more (faster) than D 2 O
9 log Absorbance (%) Thickness Loss vs Dissolved SiO 2 Molybdate Blue UV-Vis C 160C 0 min 10 min 20 min 0 20 min min 10 min Thickness loss (Å) Increasing dissolved silica concentration with increased etching Molybdate blue method did not work in D 2 O need a different method
10 Absorbance a.u. Absorbance a.u. Absorbance a.u. ATR Post 160 C Etch D 2 O N-H O-D 0 min 10 min 20 min D2O D-O-H Wavenumber cm -1 D-O-D D-O-H 1450 Wavenumber cm N-H N-H: Ammonia formed during reaction D-O-H: Exchange of dissociated D 2 O with surface OH Wavenumber cm
11 Etch Rate Comparison Samples Etch Rate (Å /min) Nitride D 2 O 140 C 24±8 Nitride D 2 O 160 C 30±8 Nitride DI 140 C 25±12 Nitride DI 160 C 45±9 TOX DI 140 C 18±3 TOX DI 160 C 45±6 Etch rates of silicon nitride and TOX are equivalent under the similar conditions Poor selectivity between TOX and SiN without spiking
12 Summary SiN HTW and HT D 2 O etch rates are similar SiN Etching more dependent on temperature than reactive species concentration Follows SiN etching behavior in 85%H 3 PO 4 phosphoric increases [H + ] but does not show increased etch rates over HTW HTW is a viable etchant for silicon nitride However with poor selectivity over silica without spiking HTW is potentially more environmentally friendly and cost effective SiN etchant than hot phosphoric
13 Future Work Dilute hot phosphoric under the same conditions Substitute HT DI water with ultra pure water (UPW) to determine if other ions impact etch rates. Determine concentration and identity dissolved siliceus species in post etch water Silica spiking and other methods to gain selectivity between SiN and SiO 2 Investigate etching of bare silicon Significant etching of underlying silicon
14 Acknowledgements University of North Texas UNT Materials Research Facility Qorvo: Nitride Wafers
15 Thank You Questions?
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