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Updates of Iowa State University. S. Dumpala , S. Broderick and K. Rajan May – 14 - 2013. Summary of Previous Results. Atom probe experimentation Atomic scale measurement of gas-solid reactions of Al and Oxygen and Si and O systems Compound formation Study of Interfacial chemistry
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Updates of Iowa State University S. Dumpala, S. Broderick and K. Rajan May – 14 - 2013
Summary of Previous Results • Atom probe experimentation • Atomic scale measurement of gas-solid reactions of Al and Oxygen and Si and O systems • Compound formation • Study of Interfacial chemistry • Environmental chamber for in-situ gas reactions – Unique features and capabilities • Collaborations: • Maryland – Sample prepared by Maryland by reacting Si microtips; analysis of samples by ISU • Van Duin group – Use of atom probe results for experimental inputs into ReaxFF simulations
Progress • Atom probe experimentation • Refinements in Environmental chamber set up for in-situ gas reactions • - Oxidation studies of Al using new set up of E-cell • Study of Si tips from Maryland using APT
E-Cell : Modifications/Improvements Cooling water lines were installed for turbo pump Burst disk valve is added (prevent any accidental excess pressure build up of the chamber) Mass flow controller and pressure regulator is added with flow sensor bypassed with pressure sensor to be able to regulate the flow with desired pressure set point very close to the main reaction cell (small chamber) Prssures as low as 0.1 millitorr can be regulated with the new setup. Digital reader/regulator of the pressure is included. Base pressures is as low as 1 x 10-5torr
Al – Oxidation with New set up of E-cell • 4 tip holder was used. • All the four tips were cleaned using laser atom probe runs prior to oxidation reaction to remove the contamination and native oxide layer • Oxidation was done using the E-cell at 450 C (sample temperature), 20 millitorr for 30 min • Laser atom probe ( 0.5 nj) was used to study the oxidized needles.
Study of Interfaces Al- Iso surface 82.39% Diffusion Profiles - APT
Si Tips from Maryland : Sample 2 (Anode Voltage: 250 V, 50 monolayers of Argon exposure) – Tip 1 Laser Atom probe was employed Laser energy – 1 nj
Sample 2 (Anode Voltage: 250 V, 50 monolayers of Argon exposure) – Tip 2
Sample 2 (Anode Voltage: 250 V, 50 monolayers of Argon exposure) – Tip 7 No SEM done Was able to collect 2.8 million data Thick oxide layer at the very tip and higher Argon content observed here
Bare Si tip No SEM done Lower oxide content
Mass Spectra Comparison Base Si tip After exposed to Ar beam More background noise Detection of Argon Higher hydrogen content
Future • More experiments as function of temperature and pressures • Testing the Si tips from Maryland using FIM • Check other condition tips (Different beam currents) • Different deposition thickness of monolayers • FIM studies