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COLLEGE OF ENGINEERING Chemical, Biological & Environmental Engineering
ResultsMetal Organic FrameworksMetal-organic frameworks (MOFs) are
crystalline hybrid organic-inorganic solids
constructed with metal ions. Crystals are
typically synthesized using solvothermal
methods, which require long growth times,
use of harsh solutions, high temperatures
and pressures, and lead to poor adhesive
properties when deposited on substrate.
Layer-by-layer growth improves adhesion
due to direct chemical bonding to substrate,
allows for versatility in thin film properties,
and provides precise control of layer
thickness. Uses for MOFs include gas
storage, separation, sensing, and catalysis.
MOF Properties• Large internal surface area
• High porosity
• High thermal stability
• Ability to tailor framework properties
Opportunity: Improve an existing
automation system to perform layer-by-
layer thin film deposition that will produce
repeatable and uniform film growth for
more efficient testing of film properties.
Project Objectives• Improve LabVIEW code and automation
control
• Facilitate deposition of different
substrate geometries
• Achieve thin film uniformity
• Improve deposition reproducibility
• Determine precursor dip times for film
uniformity
AUTOMATION OF LAYER BY LAYER
THIN FILM METAL ORGANIC FRAMEWORKSAnthony Beovich, Brenton Groves, Trey Smith
Future Work• Implement rinse station pump to provide
fresh ethanol for every rinse sequence
• Investigate cycle count relationship to
film thickness and uniformity
• Investigate the affect of different
substrate geometries on system
performance
• Improve LabVIEW code to allow nitrogen
drying flowrate input
AcknowledgmentsThank You:
• Dr. Chih-Hung Chang for support and funding.
• Yujing Zhang for assistance in lab and dedicated time
to guide the project.
• Joe Bergevin for AFM training and assistance.
• Dr. Phil Harding for project feedback and organizing
CBEE 416 design course.
• Oregon State University, HP, and ATAMI for facilities
use.
Two D Image View Analysis of '1x1_256_1Hz_wafer1A.SIG_TM_PHASE_FRW.flt'
Page 1 of 1
Capture File Date: April 21, 2017 Image Note:
0.0 1.0 µm
4.2 V
-7.0 V
Channel 1 Scan Size 1.00 µm Scan Rate 2.00 µm/s Samples/Line 256 Lines 256 Line Direction FORWARD Data Type Tapping Phase Scan Line Main Date Apr/21/2017 1:23:04 PM Tip Serial Number Aspect Ratio 1.00 Capture Direction Unknown Amplitude Setpoint 1799.14 mV Drive Amplitude 0.00 mV Figure 1 Chemical bonding of copper to an oxide layer provides strong
adhesive properties and allows for BTC to attach and form crystalline MOF
structures. The Cu-BTC crystals shown above were grown using 12 cycles
with 30 min. Cu2+, 60 min. BTC, and 10 min. ethanol wash dip times.
Ethanol Rinse
Station 4
Organic Linker
(H3BTC)
Station 3
Metal Precursor
(Cu(II) acetate)
Station 1
Nitrogen Drying
Ethanol Rinse
Station 2
Figure 2 Atomic force microscope
analysis scan locations on the Cu-BTC
thin film to determine uniformity.
https://doi.org/10.1016/j.ccr.2016.11.008
Rotary Motor
EtOH
Cu-BTC
A: 1 min. wash, horizontal drying
Figure 3 20μm x 20μm atomic force microscope scans at the center of wafers with Cu-BTC grown using the automation system.
All three wafers were exposed to 12 cycles with 30 min. Cu2+ and 60 min. BTC dip times. A) A Non-uniform film developed when
exposed to 1 min. EtOH wash times. B) A uniform film developed using 10 min. EtOH wash times and horizontal drying. C) A
uniform film developed using 10 min. EtOH wash times and vertical drying.
B: 10 min. wash, horizontal drying C: 10 min. wash, vertical drying
1 min. wash
Horizontal drying10 min. wash
Horizontal drying
10 min. wash
Vertical drying
Figure 4 Average surface roughness results from AFM
analysis using 12 cycles with 30 min. Cu2+, 60 min. BTC dip
times to grow Cu-BTC thin films. In both horizontal and
vertical drying configurations, the 10 min. wash time
showed the best uniformity results with a lower surface
roughness.
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