Atomic Layer Deposition of Hafnium Oxide at Temperatures below 100ºC. K. C. Kragh

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1 Atomic Layer Deposition of Hafnium Oxide at Temperatures below 100ºC K. C. Kragh Dept. of Physics and Optical Engineering, Rose-Hulman Institute of Technology REU Student in the Advanced Materials Research Laboratory, University of Illinois Chicago Mentors: Dr. G. Jursich and Dr. C. G. Takoudis

2 Objectives To examine low temperature Atomic Layer Deposition (ALD) growth of HfO 2 on Si To verify the composition of low temperature HfO 2 films To deposit HfO 2 on polymer fibers for creating nanotubes

3 Thin film layers compose the structures of micro-scale technology. International Nomenclature MEMS: Micro Electro Mechanical Systems MST: Micro Systems Technology Applications to every scientific field SiO 2 Al Ti

4 Nanoscale thickness of layers requires a separate deposition technique Atomic Layer Deposition (ALD) Hf(N(C 2 H 5 ) 2 ) 4 Precursor Oxidizer H 2 O One Atomic Layer

5 Process Overview Control Parameters Substrate Preparation & Insertion Lower the Reactor Pressure Reaction Raise the Reactor Pressure Removal of Substrate Analysis

6 ALD Reactor

7 Analysis of Film Thickness Spectral Ellipsometer Material Model Calibrated Reflection Sample Preserved Low Temperature Results Nonuniformity Variation in values

8 Average Thickness after 50 cycles for a 5s Pulse Time with various Reactor Temperatures 250 Average Thickness (Å) Reactor Temperature (ºC)

9 X-ray Photoelectron Spectroscopy (XPS) identifies elements by binding energy. Source: ev Al Kα The photon (hf) must overcome Work Function (φ) Binding Energy (B.E.) Resulting Data from: B.E. = hf K.E. φ Sample Destroyed By Photoemissive Electrons Image: Simon Garrett

10 Examine the Complete Survey XPS Survey across HfO 2 deposited on Silicon at 60ºC 531 ev O 1s 213 ev and 224 ev Hf 4d 5/2 and 4d 3/2 17eV Hf 4f 381 ev Hf 4p 3/2 439 ev Hf 4p 1/2 282 ev C 1 s Binding Energy (ev) 200 0

11 Examine the Hf 4f Doublet Reactor at 60ºC for 5s pulses XPS Hf 4f scan after sputtering Intensity (a.u.) 19.3 ev 17.6 ev Binding Energy (ev)

12 Confirm HfO 2 Films at Low Temperatures Intensity (a.u.) 30ºC 40ºC 60ºC 70ºC 80ºC Peaks are in place 15.8 ev Bulge is Hf-N Bonding Binding Energy (ev) 16 14

13 Inorganic nanotubes are the focus of PCL Fibers (Poly- Caprolactone) Hafnia tubes by ALD Applications: Electrical Chemical Mechanical increasing research. PCL Fibers from Dr. A. Yarin Top Image: Berserker79 Right Image: Dr. Alan W. Nicholls & K. C. Kragh

14 Cautions & Considerations for Polymer Fibers Temperature Operation Careful Loading Rigid Support Slowly Dropping Pressure Heating Strip Caution

15 Problems & Concerns Melting Temperature ~ 60ºC Aldrich Polycaprolactone (PCL) Beads Worrisome deposition Drop to sub-60ºc runs Time Per Run Quality of Fibers

16 Pressure Variations Worried about Blowing out Fibers Tried Lengthen the Distance Tube Temperature Concerns Deposition Rate Concerns Tried Grating Possibilities Solution: Steel Envelope

17 Examination of HfO 2 Coated Fibers Scanning Electron Microscope (SEM) Scattered Electrons High Magnification Composition found by Energy Dispersive X-ray (EDX) Back-Scattering for relative Atomic Number

18 Uncoated and Coated PCL Packets

19 Hafnium Oxide on PCL Fibers by Back-Scattering

20 EDX Composition of HfO 2 PCL Fibers

21 Conclusions and Future Work ALD growth of HfO 2 films will occur down to room temperature of 30ºC on Si & PCL ALD could be used to create hafnia nanotubes with polymer heating Future Work: Heat out the PCL to create the actual nanotubes and evaluate their properties

22 Photo References Garrett, Simon J Special Topic in Analytical Chemistry (CEM 924) Resource Page. Accessed 2008 June 16. Berserker79 All SEM photos captured on the Hitachi S-3000 N Scanning Electron Microscope operated by Dr. Alan W. Nicholls, Director of Research Service Facility and Electron Microcopy for University of Illinois at Chicago All other figures and graphs from K. C. Kragh

23 Acknowledgements National Science Foundation (NSF) Department of Defense (DoD) Grants: NSF-EEC & NSF-CMS Professor G. Jursich Professor C. G. Takoudis Professor A. Yarin Dr. Alan W. Nicholls Adam Kueltzo Qian Tao Manish Singh Suman Sinha Ray Lin Jiang

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