1. Optical Properties and Application of Uranium-based Thin-Films for the Extreme Ultraviolet and Soft X-ray Region Richard L. Sandberg, David D. Allred, Marie K. Urry, Shannon Lunt, R. Steven Turley Thanks to Fellow EUV Members: Jed E. Johnson, Winston Larson, Kristi R. Adamson, Nikki Farnsworth, William R. Evans, and others from EUV Group, Andy Aguila & Eric Gullickson at ALS/CXRO Funding: SPIE Scholarship, BYU Physics Dept. Funding, BYU ORCA Scholarship BYU EUV Optics August 4, 2004

2. Why Extreme Ultraviolet (EUV) and Soft X-Rays? Images from www.schott.com/magazine/english/info99/ and www.lbl.gov/Science-Articles/Archive/xray-inside-cells.html. EUV Lithography (making really small computer chips) Thin Film or Multilayer MirrorsEUV Astronomy The Earth’s magnetosphere in the EUV Soft X-Ray Microscopes BYU EUV Optics August 4, 2004

3. Why Uranium? Pros: high density and many electrons (92) for absorption, high theoretical reflectivity: low absorption and high index of refraction Con: chemically reactive (oxidizes in air to most abundant natural oxide UO 2 at STP) We study different compounds of uranium, such as uranium dioxide (UO 2 ) and uranium mononitride (UN), in search of compounds with the highest reflectance and most chemical stability. Previous Success: IMAGE Satellite Mirror Project—BYU uranium based mirrors (Launched March 25, 2000) BYU EUV Optics August 4, 2004

4. Note: Nickel and its neighboring 3d elements are the nearest to uranium in this area. Delta vs. beta plot for several elements at 4.48 nm 4.48nm BYU EUV Optics August 4, 2004

5. Reflectance computed using the CXRO Website: http://www-cxro.lbl.gov/optical_constants/mirror2.html BYU EUV Optics August 4, 2004

6. Schematic of DC magnetron sputtering system at BYU. Sample Preparation The UO, UN, Ni, and Au samples were deposited on pieces polished silicon test wafers (100 orientation). Quartz crystal monitors were used to measure the sputtering and evaporation rates. U DC Magnetron/RF Sputtering The uranium sputter targets used here were of depleted uranium metal (less than 0.2% U-235). UO 2 deposited in two ways. Reactively sputtered (DC) in oxygen partial pressure (Lunt at oxygen partial pressure of 3x10 -4 torr) or as pure uranium (RF) and then allowed to oxidize in ambient air. Uranium nitride was reactively sputtered (RF) in nitrogen partial pressure of about 10 -5 torr. Ni/Au Resistive Thermal Evaporation Evaporated Ni wire/Au beads from a resistively heated tungsten boat (RD Mathis Co.) in a large, cryopumped, stainless steel “bell jar” coater. Ir Sample Prepared at Goddard Space Flight Center on Glass Slides BYU EUV Optics August 4, 2004

7. XRD Sample Thickness -UO 2 30.0 nm (ρ=10.97 g/cm 3 ) -UN 38.0 nm (ρ=10. g/cm 3 ) -NiO on Ni 49.7 nm (ρ=6.67 g/cm 3 ) -Au 29.5 nm (ρ=19.3 g/cm 3 ) -Ir ?? (ρ=22.42 g/cm 3 ) Thickness Determined by XRD m λ = 2d sin θ BYU EUV Optics August 4, 2004

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9. 5 Studying Our Samples Images courtesy of www.weizmann.ac.il/surflab/peter/afmworks, www.mos.org/sln/SEM/works/ http://volta.byu.edu/adamson03.pdf, and http://www.swt.edu/~wg06/manuals/Gaertner117/ellipsometerHome.htm. Ellipsometry X-ray Photoelectron Spectroscope (XPS) Scanning/Transmission Electron Microscopes (SEM/TEM) Atomic Force Microscopy (AFM) BYU EUV Optics August 4, 2004

10. Inage courtesy of http:// www.lbl.gov / Taking Reflectance Measurements at the ALS (Advance Light Source) Sample of Data from the ALS Beamline 6.3.2 Reflectometer Bright synchrotron radiation 1-24.8 nm range High spectral purity Energy/wavelength or θ-2θ scan capability Small Discrepancies arise from one region to another with the use of different filters. XANES Capability Normalization given by R=(I detector -I dark )/(I beam -I dark ) BYU EUV Optics August 4, 2004

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14. Calculating Optical Properties of Uranium Oxide and Uranium Nitride from Reflectance Lunt and Urry both used Kohn and Parratt’s equations to calculate reflectance from previously published value of δ and β. The values of δ and β were then adjusted until the difference between the measured reflectance and calculated reflectance were minimized. The measured reflectance scans were angle scans from the ALS. Urry studied uranium nitride and Lunt studied uranium oxide. where V.G. Kohn. Phys. Stat. Sol. 185(61), 61-70 (1995), L.G. Parratt. Physical Review 95 (2), 359-369 (1954).

15. Optical Properties of Uranium Oxide and Uranium Nitride δ and β of UOx Top layer obtained from Lunt ALS Measured λ (nm)δ β 4.60.00650.0011 5.60.01030.0016 6.80.01610.0031 8.50.02950.0134 100.03980.0269 12.50.02060.0091 140.03600.0151 15.50.04950.0216 17.50.06390.0338 δ and β of UN from M. Urry λ (nm)  130.011520.0595 140.01380.0416 δ and β of UO2 obtained from S. Lunt’s Thesis ALS Measured CXRO Calculated λ (nm)δ β δ β 4.60.00658.09E-040.01160.0011 5.60.01030.00120.01870.0025 6.80.01730.0040.03020.0065 8.50.02980.01510.04910.0271 100.03440.04580.06740.0693 12.5-0.00380.01290.00570.0399 140.02290.01030.05090.017 15.50.03620.01580.07820.0281 17.50.05470.02460.10580.0464 Lunt found that her samples were mostly UO2 with a top layer of an slightly higher oxidation state.

16. Measured Data compared with CXRO Previously Published Constants Measured reflectance features do not agree with CXRO published constants. More work need to be done on measuring uranium’s optical constants. BYU EUV Optics August 4, 2004

17. XANES (X-Ray Absorption Near Edge Spectroscopy) XANES at ALS show additional absorption resonances not accounted for in Published Data at CXRO. U N VI O IV @ 286.3 eV * *D. R. Lide (ed.), CRC Handbook of Chemistry and Physics, 71st edition, CRC Press, Boca Raton, 1990-91, p.10-256. BYU EUV Optics August 4, 2004

18. Conclusions UO 2 and UN reflect significantly more than Ni, Ir, and Au, the current materials with highest reflectance, between 4 and 9 nm. U reflectance differs from the reflectance predicted by the previously published uranium optical properties. Current preparation of UN is not stable in ambient air (oxidizes to UO 2 ). Need to test oxidation of heated UN sample Goals Determine the optical properties of UO 2 below Shannon’s data (4.5 nm) and fill out UN optical properties data. Work with CXRO to amend the current uranium optical properties. Questions? EUV Group Contact Dr. David Allred allred@byu.edu (801) 422-3489 THANK YOU!! BYU EUV Optics August 4, 2004