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TIO2 Nanoparticle Coated Hollow Glass Microspheres; Fabrication and Analysis

The primary goal of this research is to establish the relationships

between the microstructural properties of titanium dioxide (TiO2)

coatings applied to hollow glass microspheres (HGMs). In order to

do this, the following specific objectives needed to be

accomplished:

Develop a reliable, controllable technique for coating

microparticles with TiO2 nanoparticulates.

Analyze basic coating microstructural properties such as

thickness, mechanical stability, and pore structure.

- Establish key relationships which can be used for future

coating optimization

ABSTRACT

William Ricci, Dr. Paul Fuierer1, Dr Gary Gladysz2

1. Associate Professor- New Mexico Institute of Mining and Technology, 2. Trelleborg Offshore U.S. Inc.

400oC 500oC 600oC

59.4 nm 49 nm 78.35 nm

Thin

184 nm 237.2 nm 188.03 nm

Thi

ck

MATERIALS AND METHODS

ANALYTICAL METHODS

FABRICATION FILM MICROSTRUCTURAL ANALYSIS The use of titanium dioxide (TiO2) nanoparticles has gained

increased interest due to their unique photocatalytic capabilities.

The immobilization of nanoparticulate TiO2 on engineered

microparticles such as hollow glass microspheres (HGMs) can

create a new material combination which offers the unique

abilities of nanoscale materials in a safe and scalable form for use

in real world applications.

Many of the nanoparticle film applications (particularly

photocatalysis) are linked to coating morphological properties such

as surface area through the requirement that a gas or liquid media

have easy ability to flow in and out of the coatings pore structures

in order to access the high surface area.

The unique challenges of depositing nanoparticle surface films on

microparticles have limited the ability of researchers to optimize

the coating morphology to application. This work utilizes a novel

sol-gel nanoparticle formation and deposition technique, which

produced a controlled alteration of coating thickness which has

secondary effects on surface area, porosity, and coating

mechanical stability.

The final coating thickness targets which were attained for thin

and thick coatings were 62.25 ± 14.88 nm and 203.08 ± 29.62nm

respectively. Particularly strong relationships are established

between coating thickness and coating pore volume. Relationships

are also defined between the thermal treatment utilized to

crystallize the thin film coatings and both surface area or average

pore size.

RESULTS

REFERENCES

CONCLUSIONS

The HGMs coating procedure outlined was able to produce a

system of thinly and thickly microparticles. Although, the

deviation in coating thicknesses was large ranging from 14.8% to

33.2% (on a microsphere-to-microsphere basis), the process did

deliver good differentiation between thin and thick coatings. The

thickly coated samples showed 2 – 3 times the thickness of the

thinner coatings.

The ability to produce a nanoparticulate coating on a

microparticle in a safe scalable batch system and reliably target

coating thicknesses to within ~20 nm (thin coatings 60±15nm,

thick coatings 200nm ± 20) is unique. Furthermore, the equipment

and chemicals utilized to fabricate the coated HGMs are readily

available in most laboratories and at low cost.

Several coating microstructural properties have been and analyzed

and strong morphological relationships established.

The average pore size and surface area generated by the

application of the nanoparticulate coating appears to show a very

regular growth with the application of increasing thermal

treatments, but no relationship to coating thickness. Conversely

the total pore volume appears to be sensitive only to coating

thickness.

The ability to manipulate one or two of the coating

microstructural properties while having only minor impacts on the

others makes these materials ideal for optimization.

Thickness measurements were taken by fracturing the HGMs and

imaging the coating cross-sections. HGMS were fractured by

placing them upon carbon tape adhered to a SEM sample stub. A

second stub was then brought into contact in a parallel plate

scenario and twisted several times.

Smart-Tiff® software was used to make estimates of 20

microsphere coating thicknesses.

Several common processing parameters necessary to control coating thickness have

been researched and utilized to produce a cross-section of samples having a variety

of coating thicknesses.

2 coating thickness targets were chosen and thermally treated at 3 temperatures,

for a total of 6 individual coating procedures. The film fabrication parameters for

all 3 samples within each target thickness domain were identical with the exception

of thermal treatment.

Total coating pore volume and coating

thickness

o The volume percentage of the coating

made up by its pore structure is

decreases as thickness increases.

Average pore size and annealing

temperature

o The average pore size show a very

regular growth with increasing thermal

treatments, but no relationship to

coating thickness.

Surface area and annealing

temperature

o The surface area loss with increased

annealing temperature appears to be

accelerative with increased coating

thickness.

The gas adsorption isotherms show the expected shape for nanoparticulate materials

with hysteresis loops indicating gas condensation inside the pore structure. However,

there are notable differences in shape between the thinly and thickly coated

samples.

The thickly coated samples show an apparent lifting (from a horizontal to vertical

orientation) and narrowing of the hysteresis loop with increased annealing

temperature. These curves show highly organized meso and microporosity which are

common to agglomerates of spherical particles (G.Leofantia,1998).

The 400 and 500oC thinly coated samples show a long horizontal hysteresis indicating

a high level of disorganization in pore geometry and size. The 600oC thinly coated

sample appears to be in a much clearer transition to a more regular mesoporous

structure.

RESULTS

Gas adsorption data was collected on a Micrometerics Gemini 2375 V5.01 gas

adsorption unit with Nitrogen as the adsorbate

• Total Surface Area (m2/g)- BET monolayer method

• Average Pore Size (nm) – Volume adsorption method

• Specific Pore Volume (cm3/g)- Total gas volume adsorbed

TiO2 coating content and process yield were calculated using thickness

measurements under a concentric sphere coating assumption with specific

pore volume measurements used to normalize for the coating pore content.

Crystallite phase and size measurements were taken on an Scintag XDS 2000

with a CuK source.

OBJECTIVES

The process yielded samples with a clear distinction between the thin and thick

coatings.

XRD analysis was performed on the thickly coated samples only. The large volume of

the low density hollow particle catalyst support results in a large amount of sample

volume with a comparatively low TiO2 content. As a result the thinly coated samples

produce results with insufficient intensity to be properly analyzed. The x-ray results

show that the anatase crystal phase is found in all samples regardless of thermal

treatment.

FILM THICKNESS, AND CRYSTAL PHASE

Immediately obvious is the growth of long thin fissures approximately 50 - 200 nm

wide and extending all the way through the coating to the glass substrate. In these

more thinly coated samples there does not seem to be any obvious impacts on the

films adherence to the substrate.

The thickly coated samples which were annealed to 500 and 600oC show severe

fissuring. The fissures have grown to several microns in width and are

interconnected, typically running all the way around the circumference of the

microspheres. The coating delamination seems to be localized around the crack

edges, and triple points. There is little evidence of large scale coating loss. The

film seems to have simply pulled away and retracted revealing the substrate below

FILM QUALITY

600oC

500oC 500oC

600oC

59.4 nm 49 nm 78.3 nm

184 nm 237 nm 188 nm

400oC 500oC 600oC

CONTACT

G. Leofantia M. Padovanb, G. Tozzolac, B. Venturellic; Surface area and pore texture of catalysts : Catalysis Today, 1998. - 1-3 : Vol. 41.

This work utilizes Trelleborg Offshore Boston “SI 200”

grade borosilicate HGMs. The SI 200 HGMs has a mean

particle size of approximately 50 microns with a density

of 0.2 g/cc.

There are several microstructural relationships which appear to have significant

linear correlations to either coating thickness or thermal treatment:

William Ricci – Trelleborg Offshore US 290 Forbes Blvd. Mansfield MA 02048 (774) 444-1400 Will.ricci@trelleborg.com Dr. Paul Fuierer – Associate Professor, NMT, Department of Materials and Metallurgical Engineering 801 Leroy Place. Socorro, NM 87801 (Office: 23 Jones Hall) (575) 835-5497 Fuierer@nmt.edu Gary Gladysz– Trelleborg Offshore US 290 Forbes Blvd. Mansfield MA 02048 (774) 444-1400 Gary.gladysz@trelleborg.com