Summer 2015 Research Experience for Undergraduates

AcknowledgementsThis material is based upon work primarily supported by the Engineering Research Center Program of the National Science

Foundation and the Office of Energy Efficiency and Renewable Energy of the Department of Energy under NSF Cooperative

Agreement No. EEC‐1041895. Any opinions, findings and conclusions or recommendations expressed in this material are

those of the author(s) and do not necessarily reflect those of the National Science Foundation or Department of Energy.

DESIGN, MODIFICATION, AND PERFORMANCE ENHANCEMENT OF

NANOPARTICLE SYNTHESIS AND DEPOSITION MACHINES

Ethan Bendau1, William Firth2, and Zachary Holman3.1The City College of New York, New York, NY, 2Rice University, Houston,TX, 3Arizona State University,Tempe, AZ

Deppy Improvements

Deppy

• Nozzle Pressure Feedback Control System

• Pressure P-Controller in RxN

Chamber

• Interface Integration

• Modification to Nozzle

• Adjustable bearing blocks

• Forced parallel bearing

guides

• Modification to Universal Sample Holder

• Allows for fabric samples

and microscope slides

• Thickness doubled to

decrease distance from

Raman Probe

• Reversible

• Modification to Shower Head

• Improved Symmetry• Baratron probe hole removed

• Reaction Chamber Electrode Cooling System

• Stainless steel piping system

• Cuts electrode and RxN

chamber temperature in half

• Redesign Of Deposition Chamber Lid

• Added window for camera

access

Figure 6: Nozzle motor Figure 7: Deppy Interface

Figure 8: Bearing block Figure 9: Bearing guides

Figure 10: Universal sample holder

Figure 11: New and

old showerheads

Figure 12: Old

showerhead

Figure 13: New

showerhead

Figure 14: Rxn chamber

and electrode with piping Figure 15: Cooling system

Figure 16: Deppy Lid

Figure 1: Deppy [1]

• Synthesizes and deposits broad range of nanoparticles on an even broader range of substrates [1]

Figure 2: Reaction ChamberFigure 3: Inside of Deposition Chamber

• Deposits material via hypersonic impaction

• Two chamber process

• Allows energetic separation of the synthesis and deposition

processes while still performing as a continuous flow reactor

• Allows for easily removable and swappable reaction chamber [1]

• Uses compressible fluids and the Venturi effect to accelerate particles in order to impact and

adhere to the substrate.

• Surface chemistry only plays small role. [1]

Figure 4: choked flow [1] Figure 5: Nozzle

Anny

• Synthesis and analysis of small-scale (1cm) silicon nanoparticle depositions

• In-situ Fourier Transform Infrared Spectroscopy and Residual Gas Analysis (RGA) capabilities

• Turbo-molecular pump backed by roughing pump for pressure down to 10-7 torr range

• Inficon Transpector 2 Residual Gas Analyzer

• Uses silane (SiH4) as precursor gas to generate nanoparticles in the plasma chamber

• Upstream-downstream pressure ratio accelerates nanoparticles to supersonic speeds, adhering to

substrate on impact

• Samples transferred to loadlocked N2 glovebox for loading, unloading, and further analysis

Figure 17: Anny

Anny Improvements

heater

• Goal: Build controller for molybdenum substrate heater

• Learned principles of circuits, electrical wiring

• Controller uses Eurotherm thyristor and Watlow temperature controller

• Heating element reaches >900⁰C for temperature-controlled desorption

• In Progress: Motorized arm improvements

• Under vacuum, motor

vibrates noisily, disturbing

sample holder

• In Progress: Redesign of forked sample

holder

• Current chamber tolerances too small

heater

• Goal: Bring RGA capabilities back on-line

• Learned principles of vacuum systems, RGA operation

• Determined sensor was malfunctioning, replaced with unit from local reseller

• RGA used for analysis of nanoparticle depositions, plasma analysis, in-situ leak detector

Figure 20: Working in the gloveboxFigure 19: Adjusting electrodesFigure 18: Anny [2]

Figure 24: RGA sensor head

Figure 23: Inside the FTIRFigure 22: Attaching the RGAFigure 21: Turbomolecular pump

Figure 25: Analyzing data in FabGuard Explorer

Figure 24: Recycling salvaged parts Figure 25: Lab workbenchFigure 26: Finished heater controller

Figure 27: Motorized arm and controller Figure 28: Sample holder and heating element

References

[1] Firth, P. (2015) “Substrate Independent Nanomaterial Deposition via hypersonic Impaction.” Masters of Science Thesis: 1-69

[2] Holman, Z. (2104) “SNM: A Nanoparticle Spray Technology for Roll-to-Roll Manufacturing of Functional Porous Coatings.” Project Description: 2