ELECTROSPINNING SPACIALLY ORIENTED SUB-MICRON METAL OXIDE FIBERSELECTROSPINNING SPACIALLY ORIENTED, SUB-MICRON METAL OXIDE FIBERSJ R S ti (BChE) E Philli (BME) J D it lJ. R. Santiago (BChE), E. Phillips (BME), J. Deitzelg ( ) ( )

f C f C f CUniversity of Delaware . Center for Composite Materials . Department of Chemical EngineeringUniversity of Delaware . Center for Composite Materials . Department of Chemical Engineering

MOTIVATIONS AND OBJECTIVES DRUM SPEED AND SOLVENT VOLATILITYSET-UPMOTIVATIONS AND OBJECTIVES DRUM SPEED AND SOLVENT VOLATILITY AFFECTS ON FIBER ORIENTATION AND SIZE

SET UPAFFECTS ON FIBER ORIENTATION AND SIZE

Electrospin various solutions to obtain wider view of

pthe electrospinning process including metal oxides The volatilities of the electrospinning process, including metal oxides. trichloroethane and Submicron Metal Oxide fiber applications in chloroform are 3 Submicron Metal Oxide fiber applications in electronics

Solvents: and 26.2 kPa @ electronics 25°C, respectively.

Supercapacitors Fiber diameter SupercapacitorsN i

size is independent Nanowires

pof solvent volatility

Nanoelectronicsy

Collection is done Nanoelectronics Collection is done on a 6” diameter by

Gas Sensorson a 6 diameter by 12” aluminum drum.Gas Sensors

L12 aluminum drum.

Lasers Electrospinning uses an electrostatically

Solar Cells Electrospinning uses an electrostatically

S l C ll Solar Cells driven polymer jet and a collection plate, Solar Cell

Research Goal: Formation of spacially orientedp y j p ,

usually aluminum foil on a rotating drum Research Goal: Formation of spacially oriented metal oxide fibers through use of electrostatcially Difference in orientation based on drum speed is shown to

usually aluminum foil, on a rotating drum.metal oxide fibers through use of electrostatcially p

the left in SEM images taken using the TM-1000 Tabletop Highly oriented sub-micron diameter driven jets. Microscope. Both are PEO/Trichloroethane fibers spun at 9

kV potential and 0 5 mL/hr feed rate On the top the drum

g ypolymer fibers are achieved by spinningj kV potential and 0.5 mL/hr feed rate. On the top the drum

speed is 72 RPM or 0 6 m/s face velocity and the bottom ispolymer fibers are achieved by spinning f l t ith l di l t i t t speed is 72 RPM or 0.6 m/s face velocity and the bottom is

1963RPM or 16 m/s face velocity.from solvents with low dielectric constants. y

METAL OXIDE SOLUTIONS CONCLUSIONS FUTURE WORKELECTROSPUN METAL OXIDEMETAL OXIDE SOLUTIONS CONCLUSIONS FUTURE WORKELECTROSPUN METAL OXIDE SOLUTIONS Observe parameters for electrospinningAND CALCINATION PROCESS SOLUTIONS The volatility of solvents does not appear to

Observe parameters for electrospinning b d d ti it f l ti

C C O OC SS800x Magnification SEM Images:

The volatility of solvents does not appear to have much of an effect on the electrospinning

based on conductivity of solution. g g have much of an effect on the electrospinning Precursor solutions were made by creating Improve calcination process through TGAprocess.y g

solutions containing 3wt% PEO in 1:1 ratioImprove calcination process through TGA experiments and use of with lower degradation

Fiber orientation and fiber diameter size aresolutions containing 3wt% PEO in 1:1 ratio with metal organic salt and trichloroethane

experiments and use of with lower degradation t t (PVA Et ) Fiber orientation and fiber diameter size are

proportional to draw ratiowith metal organic salt and trichloroethanewith any additional solvents when necessary

temperatures (PVA, Etc….)proportional to draw ratio. C l i ti i t tl ti l

with any additional solvents when necessary. Use the opposite charge instead of grounding Calcination process is not currently optimal. Calcination process for electrospun

pp g g gthe rotating drum to dampen wind effect on

PEO Degradation temperature is too highp p

precursors was from 300-550°C by intervalsthe rotating drum to dampen wind effect on needle at high drum speed

Electrospun 3wt% Iron(III) Electrospun 3wt% Copper(III) and g p g

Metal salt loading is too lowprecursors was from 300 550 C by intervals of 50°C per hour in industrial oven

needle at high drum speed.

ACKNOWLEDGEMENTSp ( )

and PEO in Trichloroethane PEO in Trichloroethane, Chloroform, d T i th l i

Metal salt loading is too low. Need to introduce more heating steps

of 50 C per hour in industrial oven.ACKNOWLEDGEMENTSand Triethylamine

M l O id fib f I O id Need to introduce more heating steps

This work is supported by the Army Research Metal Oxide precursor fibers for Iron Oxide This work is supported by the Army Research Laboratory through the Composite Materialsand Copper Oxide had average diameters of Laboratory through the Composite Materials

Research programpp g

1 11 and 0 8 micrometers respectively and Research program.1.11 and 0.8 micrometers respectively and had standard deviations of 0 26 and 0 25 Special Thanks to:had standard deviations of 0.26 and 0.25.

Spec a a s toJeff Knopf Both fiber collections were done at about 8 Jeff Knopf

Denis Kissounkom/s face velocity or 1000 RPM. Iron Oxide Copper OxideVulcan A 550 Oven used for calcination Denis Kissounkoy Iron Oxide Copper OxideVulcan A-550 Oven used for calcination.

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