Engineering and Development of a Transportable ALD Reactor

Engineering and Development of a Transportable ALD Reactor/ Measuring Growth of Ce. O 2 Adam Kueltzo Thornton Fractional North High School August 2 nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMRe. L) Mentors: Sathess Selvaraj, Jorge Rossero, Dr. C. G. Takoudis, and Dr. G. Jursich Departments of Bioengineering and Chemical Engineering

Purpose �Develop a plan for construction of an transportable atomic layer deposition (ALD) reactor �ALD reactor will be transported to Argonne National Laboratory �In-situ X-ray analysis at the Advanced Photon Source (APS)

Experimental Station at APS

Goals �Assess the current status of the ALD system in place �Vacuum pump completed …pressure…temperature… �Configuration completed…valves…gaskets…tubing � Flow meter control completed Other goals to will be met soon

Vacuum Pump �Wasn’t pumping down to low enough pressure -30 m. Torr �Tested at machine shop and singled out problems in lab �Now pumping down to 10 m. Torr �Called company and verified parameters

Mass-flow meter calibration � Found that the flow rate measured was double that found on flowmeter controller. � Compared controller to bubble test. �Flowmeter 1 – 144 -148 cc/min �Flowmeter 2 – 148 -156 cc/min �Flowmeter 3 – 180 -190 cc/min

Flow Bubble Test

Work still in progress �Must be designed for transportation Precursor and water bubbler design � Metal framing for reactor � Exhaust pipe modification � Module and solenoid placement � Movable reactor � Finalize water delivery �

Precursor Bubbler

Precursor Bubbler- Conflat-lid type Volume ~ 150 cc T ~ 200 0 C P ~ 300 m. Torr

Water Bubbler

Water Delivery Line From cylinder P MKS Flow meter To reactor Water bath 3 -way valve

Exhaust pipe modification

Proposed modification

System Schematic

Purpose �Verify growth rate of Cerium Oxide using precursor. Tris(i-propylcyclopentadienyl)cerium �Possible use as electrolyte when Yttrium doped in Solid Oxide Fuel Cells (SOFC) �High ionic conductivity and lower operating temperature (700 o. C) �Allows for use of more readily available and cheaper materials

Current ALD Status

ALD Process �“One Cycle” �Precursor �Purge (N 2) �Oxidizer (H 2 O) �Purge (N 2) http: //www. cambridgenanotech. com/

Results Growth Rate of Cerium Oxide (Ce. O 2) 500 450 400 Thickness (Angstroms) 350 300 250 200 Reactor Temp 250 o. C 150 100 50 0 0 50 100 150 200 250 Cycle number 300 350 400 450

Current Testing �TEM imaging taking place � 400 cycle sample �Annealed 600 o. C and 800 o. C �As deposited

Acknowledgments �CBET-NSF Grant #1142255 �Mentors - Dr. Takoudis and Dr. Jursich �Doctoral Students - Sathess Selvaraj and Jorge Rossero �Air Liquide