First, I will discuss my objectives, followed by a short introduction on

Printed Electronics, GO and RGO and also printing techniques.

Then I will discuss you my my Methodology and Results,
Lastly, I will give a summary of my presentation
Here is a list of my objectives
To formulate GO and RGO inks
To synthesize GO and RGO
To optimize the jettability of the inks by DOE of JMP
To reduced coffee ring effect by surfactant addition
To Optimize Printing settings of the inks
To visualize printing patterns
Printed electronics is an interdisciplinary discipline which aims to produce
technology which is a key in the engineering of all kinds of electronics.
In fact according to Hoffman the director of Flextech alliance, The market for
flexible, printed, and organic large-area electronics is rapidly growing.
Currently estimated at over $1B, the global market is expected to increase to
a $45B market by 2016. Various printing techniques has been utilized.
But for this reasearch I utilized inkjet printing due to its non-contact method
of printing and versatility
For my methodology, the research is divided into three main parts,
Synthesis of GO and RGO
Ink Optimization
Printing Optimization
For the synthesis or Graphene Oxide, I used the modifed hummers method
which allows better oxidation of the Graphite. Unlike conventional hummers
method, modified hummers method doesnt utilize Sodium nitrate in its
reaction and therefore less toxic to its counterpart.
The process is starts by oxidizing graphite in 100 mL concentrated
Sulfuric acid/Phosphoric acid solution. Then washing it consecutively with the
following liquids
On the other hand, Reduced Graphene Oxide was synthesized by adding a
reducing agent and a series of sonicataion and washing
For the synthesis or Graphene Oxide, I used the modifed hummers method
which allows better oxidation of the Graphite.
The process is starts by oxidizing graphite in 100 mL concentrated
Sulfuric acid/Phosphoric acid solution. Then washing it consecutively with the
following liquids

On the other hand, Reduced Graphene Oxide was synthesized by adding a

reducing agent and a series of sonicataion and washing
To select the best reducing agent and the effect of surfactant to the
reduction of GO, various configuration were tested, one group with an SDS
surfactant and one without. The reducing agents tested for the experiment
are Ascorbic acid, Sodium borohydride, Zn and Glucose.
Ink optimization on the other hand was divided into 4 parts, Design of
experiment, Viscometry, Contact Angle Measurements, Jettability Calculation.
To predict the jettability of the ink which was formulated, a dimensionless
number, Z, the inverse ohnesorge number was calculated using the equation
above which states that the squareroot of the product of the jet diameter,
density and surface tension divided by viscosity should range from 4 to 14 to
be jettable in the printer.
To determine the optimal printable range based on the composition of the
ink,
JMP was used to model the experiment.
Two sets Tables were generated using custom design for GO and RGO
For the GO ink, the two responses were set, Inverse Ohnersorge
number with match target as its goal and Surface tension as to with
minimize as its goal.
Various factors were set
Such as the amount of Graphene Oxide
Water:Glycerol Ratio
Two types of Surfactants SDS and PSS
And the amount of Surfactants
On the other hand for RGO
The responses were identical with GO
The factors however doesnt include any surfactant because terpineol
itself is the surfactant in the solvent.
A random set of parameters were generated through JMP and were tabulated
into a sheet.
To obtain the Z, the jettability of the inks, density, viscosity and surface
tension were obtain using these techniques
To measure the viscosity, four uhbelod viscometer was used for the
research, the standards used for the experiments were, water, ethanol,
isopropanol and glycerol.
Depending on the viscosity of the inks, the flow time of the ink should
be between 10 seconds to 300 seconds to be considered appropriate for the
viscometer.

The standards used for the experiment, were water, ethanol,

isopropanol and glycerol.
On the other hand, the surface tension of the ink was measured using
contact angle measurement by sessile drop method.
For this technique one microlit droplet was deposited on three clean
surfaces with known surface energy and its components.
The surfaces used for the experiment was teflon, PMMA and
Glass.
Using a digital sony camera, under green light, the image of droplet
was captured and analyzed by ImageJ and dropsnake to obtain its contact
angles.
The contact angles then can be used with the known surface energies to
determine the surface tension using an equation derived from the Lifshitz
Vander wals/acid-base approach.
The same technique was used to RGO and based on the contact angles, we
can observe that GO in glycerol:water exhibits a higher contact angle and
surface tension compared with RGO in cyclohexanone.
After optimizing the ink, the ink was filtered and tested using a high precision
printer with a 60 micron head.
To optimize the ink, various parameters will have to be obtained
through trial and error.
There parameters include,
Rise time, dwell time, fall time, echo time rise time
For the results and discussion, this part is divided into IR and UV-VIS
spectroscopy,
The results for the ink optimization
Coffee Ring Visualization
Printing Optimization
and Pattern Characterizations
The products were analyzed using IR spectrocopy to determine the extend of
oxidation.
Based on the IR spec of GO, there is a significant, increase in the
degree in the oxidation of graphite after the modified hummers method.
After the reduction using Zn, there is a significant decrease in OH and
CO peaks.
The UV-VIS spectra below show that Zn is the most efficient reducing agent
among the solution and exhibited the largest change in wettability after
reduction. You can see the change in peak from GO to RGO the 225 nm range
For the these series of slides I will present you data analyzed by JMP based
on the DOE.

Here is a prediction for the GO, as you can see the error bars are huge which
makes corresponds to high degree of deviation of the results.
Based on the result, only the concentration of Water:glycerol has
a huge effect on the jettability of the ink.
The concentration of GO only becomes significant at high
concentration
The amount of surfactant on the other hand has some very
questionable result due to the presence of a peak.
On the type of surfactant, we can tell that SDS is more efficient
than PSS.
To give you a more clearer view, here is a surface profile for GO. The same
holds true based on the results seen above.
To obtain our target for ink formulation, the surface profile for the type of
surfactant and the solvent ratio was zoom in to reveal the areas of jettability.
On the image on the right are the areas of with jettable ink.
A surface profile was also constructed for RGO. Unlike GO results, the results
for RGO are more precise and has lower error bars. We also have hear a
zoom it image which contains all the jetable range for RGO.
Using the modeled equations, 4 ink formulations were generated.
For GO with surfactant, 5mg/mL 40% Glycerol and 3mg/mL
For GO without surfactant, 5mg/mL, 40% Glycerol and 3mg/mL
For RGO 3mg/mL in pure cyclohexanone
For RGO 3mg/mL in 85:15 cyclohexanone:Terpineol Mixture.
Here are some parameters measured for the ink. Among the inks, RGO is
jettable.
For the printing optimization, the obtained values through trial and error as
follows.
All the three inks are jettable, however, GO w/SDS exhibited a very
erratic behavior. Possible explanation could be the formation of concentration
gradient due to waiting time.
GO without surfactant on the other hand, is stable however, drying
time took so much time.
For the RGO, the ink was completely stable.
Here are some images of the printed patterns,
On the left is a wet GO series of droplets
On the left are droplets of RGO. The optimal droplet spacing is found to
be 60m foe GO to produce a straight droplet.
Unlike GO, the RGO dries quickly over air.

Here is an AFM image of RGO, we can see based the images that the flakes
are discontinuous which makes it non-conductive. The average thickness
also indicate an average of 93.6 nm which is approximately 90 sheets.
Summary
Graphene Oxide was synthesized using Modified Hummers Method
Zn is the most efficient reducing agents among Ascorbic acid, LiBH4
and Glucose.
Four different inks were formulated GO, GO w/SDS, RGO in
cyclohexanone and RGO in cyclohexanone:Terpineol
The jettabilities of the inks were optimized by JMP DOE.
The presence of a surfactant reduces the coffee ring effect on the dried
droplets.
RGO was successfully printed on SiO2 however, the Graphene flakes
were found to be discontinuous.