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

Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

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Page 1: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Engineering and Development of a Transportable ALD Reactor/ Measuring

Growth of CeO2

Adam KueltzoThornton Fractional North High School

August 2nd, 2012

University of Illinois at ChicagoAdvanced Materials Research Laboratory (AMReL)

Mentors: Sathess Selvaraj, Jorge Rossero, Dr. C.G. Takoudis, and Dr. G. Jursich

Departments of Bioengineering and Chemical Engineering

Page 2: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

PurposeDevelop 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)

Page 3: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:
Page 4: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Experimental Station at APS

Page 5: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

GoalsAssess the current status of the ALD system

in placeVacuum pump

completed …pressure…temperature…Configuration

completed…valves…gaskets…tubing Flow meter control

completed

Other goals to will be met soon

Page 6: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Vacuum PumpWasn’t pumping

down to low enough pressure -30mTorr

Tested at machine shop and singled out problems in lab

Now pumping down to 10 mTorr

Called company and verified parameters

Page 7: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

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

Page 8: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Flow Bubble Test

Mass Flow Meter

From gas cylinder

Soap solution

Page 9: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

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

Page 10: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Precursor Bubbler

Page 11: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Precursor Bubbler- Conflat-lid type

Volume ~ 150 ccT ~ 200 0CP ~ 300 mTorr

Page 12: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Water Bubbler

Page 13: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Water Delivery Line

MKS

P

3-way valve

To reactor

Water bath

Flow meter

From cylinder

Page 14: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Exhaust pipe modification

Page 15: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Proposed modification

Page 16: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

System Schematic

Page 17: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

PurposeVerify 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 (700oC)

Allows for use of more readily available and cheaper materials

Page 18: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Current ALD Status

Page 19: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

ALD Process“One Cycle”PrecursorPurge (N2)

Oxidizer (H2O)

Purge (N2)

http://www.cambridgenanotech.com/

Page 20: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Results

0 50 100 150 200 250 300 350 400 4500

50

100

150

200

250

300

350

400

450

500

f(x) = 1.21617787034626 x − 13.3725337151783

Growth Rate of Cerium Oxide (CeO2)

Cycle number

Th

ickn

ess

(A

ngst

rom

s)

Reactor Temp 250oC

Page 21: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

Current Testing TEM imaging taking place 400 cycle sampleAnnealed 600oC and 800oC As deposited

Page 22: Adam Kueltzo Thornton Fractional North High School August 2nd, 2012 University of Illinois at Chicago Advanced Materials Research Laboratory (AMReL) Mentors:

AcknowledgmentsCBET-NSF Grant #1142255

Mentors - Dr. Takoudis and Dr. Jursich

Doctoral Students - Sathess Selvaraj and Jorge Rossero

Air Liquide