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.