Brigham Young University. Infiltration of CNT-M Microstructures using CVD and ALD Presented by: Collin Brown, Jason Kyle Anderson
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1 Infiltration of CNT-M Microstructures using CVD and ALD Presented by: Collin Brown, Jason Kyle Anderson October 31st, 2013
2 Acknowledgments Jason Kyle Anderson for his help in getting the system to work Dr's David Allred, Richard Vanfleet, and Robert Davis for their help and direction in this project BYU Environment for Mentoring Grant (MEG) Richard Hansen for his work on CNT-M David McKenna for constructing the CVD system
3 Outline Purpose of Deposition Techniques Overview of CNT-M Theory of Deposition Chemical Vapor Deposition (CVD) Atomic Layer Deposition (ALD) Conversion of CVD system to ALD Initial Results Initial Characterization with SEM, TEM, and XEDS
4 Purpose Create mechanical and electrical components on a micro scale - NEMS/MEMS
5 Why does this matter? High sensitivity inertial sensors X-ray collimator (1) (2 ) wii-sports-bowling.php
6 Traditional Fabrication Method Etching- Chemically or mechanically removing selective parts of a solid metal (3)
7 Limitations of Chemical Etching Limited selection of materials - Tungsten, Gold, Silicon, Aluminum Poor aspect ratio (height to width) (~5:1) aspect ratio due to gas transportation limits (4 )
8 New Method for NEMS/MEMS Carbon Nanotube Templated Micro-fabrication M) (CNT- Easily Controlled High Aspect Ratio (200:1) features >500 microns tall by 2-3 microns across Electrically conductive
9 CNT-M Process Hot Ethylene Mask Photoresist Silicon Wafer
10 Chemical Vapor Deposition (CVD) When used to infiltrate a CNT, called Chemical Vapor Infiltration (CVI) Flow reactants into chamber constantly, usually at high temperature Heat the solid precursor so it will volatilize Flow an inert gas to carry the precursor to the sample Problems Uneven Infiltration Capping
11 Before infiltration After infiltration (6) Forest - 1% Carbon Carbon Nanotube Forest Infiltrated with Mo(CO)6 by Richard Hansen
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16 Atomic Layer Deposition (ALD) Propose to try with Tungsten in nanotube forests, so Atomic Layer Infiltration (AFI) Self-limiting layer by layer Hope to achieve: uniform material properties eliminate crusts
17 Tungsten ALD with WF6 Gaseous form of WF6 self-limits deposition Flow H2, monatomic Hydrogen from Plasma, or Silane ( SiH4 ) H reduces WF6 leaving a layer of W HF gas molecules created HF Vacuum Chamber WF6 W Sample H2 Ar WF6
18 Converting the System Modified from CVD Hooked in gas lines for WF6 Seal cabinet,install cabinet exhaust system, and insert sensors and filters for HF. Automate Labview TM program to cycle valves for ALD
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20 Initial Results Brigham Young University
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22 Plasma - RF generated
23 Latest Deposition - Pseudo ALD Constant H (40 sccm) - from a Hydrogen Plasma 5 seconds of WF6 ( l at 5 psi, about 2.0 x 10-4 mole) 120 cycles 235 degrees C - sample temperature Ozone treated 1 of the samples for 20 min, for better nucleation
24 Ozone treatment vs No Ozone treatment 7 Ozone Treatment No Ozone Treatment
25 Top of Sample Side of Sample
26 Top of Sample - Break in Lower Left Image of Fresh Surface from Break
27 No obvious difference between chemical makeup of small or large stuff
28 scattered peaks have a lattice spacing too large for BCC tungsten may be an A15 compound, something like Beta-Tungsten
29 Future Plans Optimize procedure (Intervals, flow rates, etc.) Silane vs. Hydrogen Ozone treatment vs. No Ozone treatment vs. In Situ Ozone treatment Annealing Characterization by SEM & TEM cross sectioning, Also X-ray characterization at ALS, FIB Capping Grain size uniformity Electrical conductivity Mechanical Properties
30 Sources Johnson, R. Colin. MEMS finds niche in space exploration. EE Times, Sep < Oxford Instruments. Plasma Technology. Accessed March 7, < 5. Kellen Moulton, Nicholas B. Morrill, Adam M. Konneker, Brian D. Jensen, Richard R. Vanfleet, David D. Allred, and Robert C. Davis. Effect of Iron Catalyst Thickness on Vertically Aligned Carbon Nanotube Forest Straightness for CNT-MEMS. Journal of Micromechanics and Microengineering 22 (5) May 2012 and references cited therein. 6. Hansen, Richard Scott. "Mechanical and Electrical Properties of Carbon-Nanotube-Templated Metallic Microstructures." Senior Thesis. June 2012.
Developing Atomic Layer Deposition Techniques of Tungsten on. Carbon Nanotube Microstructures. Jason Kyle Anderson
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