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2.1. Synthesis of PPMSGF-50
A flowchart for the preparation of PPMSGF-50 is shown in
Fig. 1. This procedure is similar to that published previously by
Balasubramanian et al. Commercial ultra pure titanium
isopropoxide (TTIP, Aldrich), isopropanol (i-PrOH, Fisher Sci-
entific), diethanolamine (DEA, Fisher Scientific) and nanophase
TiO2 Degussa P-25 powder (50m2/g; 15¨C30% rutile + 85¨C70%
anatase, mean diameter of 30 nm) were used for the preparation
of the modified sol. A 0.5M solution of TTIP in i-PrOH
was prepared and a calculated amount of DEA was added to
the solution. A molar ratio of DEA/TTIP of 4 was used. The
solution was stirred at room temperature for approximately 2 h.
Subsequently, water was added drop-wise under vigorous stirring
conditions. A molar ratio of H2O/TTIP of 2 was used. A
clear and stable alkoxide solwas obtained using this process. The
titania modified solwas prepared by adding 50 g/L Degussa P-25
TiO2 powder into the alkoxide sol. The powderwas added slowly
under vigorous stirring to prevent the formation of agglomerates.
A thick, white, viscous suspension was obtained. This modified
sol was being stirred rapidly to prevent precipitation in storage
between experiments.
The uncoated 304 stainless steel substrates were cleaned with
ethanol and methyl ethyl ketone (99.8%, Fisher Scientific). The
clean substrates were dried at 125 ◦C for 24 h. A dip coating
apparatus equipped with a velocity-control adjustable motor
was used to dip in and pull out the substrate at a preset constant
velocity. A withdrawal velocity of 12.3¡À0.5 cm/min was
used in this study. After the dip coating procedure was completed,
the coatings were dried at room temperature for 24 h,
and then placed into a multi-segment programmable high temperature
furnace (Paragon Model HT-22-D, Thermcraft Inc.,
Winston-Salem, NC) for calcination. The furnace temperature
was incremented at a ramp rate of 3.0 ◦C/min until 100 ◦C was
reached and this temperature was held for 1 h. The temperature
of the oven was increased at a rate of 3.0 ◦C/min to a final
temperature (400¨C700 ◦C) and again held for 1 h. Finally, the
coatings were cooled naturally to room temperature (approximately
a 15 h cooling period).

                                      TTIP/2-propanol
                                               |
                                               |
                                    DEA--        --H2O
                                               |
                                            plain sol
                                               |
                                                 ---- P25 TiO2
                                               |
                                           Modified sol
                                               |
                                          Dip coating
                                               |
                                            Drying
                                               |
                                           Calcination
                                               |
                                             TiO2 film
9Â¥2008-08-28 18:37:49
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