icwes15 - preparation of mesoporous titania photocatalyst for water treatment application. ...
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Preparation of Mesoporous Titania Photocatalyst for Water Treatment
ApplicationXingdong Wang1, David R.G.Mitchell2, Patrick Hartley1 and Rachel A. Caruso1,3
1 CMSE, CSIRO Material Science and Engineering, 2 Australia Center for Microscopy and Microanalysis, The University of Sydney, 3 PFPC, School of Chemistry, The University of Melbourne
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My background
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Environmental pollution remediation ---principle of photocatalysis
http://www.mchnanosolutions.com/whatis.html
High recombination rate of e-/h+ pairs (~90%) Inactive under visible light (wide band gap---3.2 eV for anatase TiO2)
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Outline of Porous TiO2 Project---Environmental pollution remediation
Enhancing photocatalytic (PC) activity UV light: decrease charge recombination (e-/h+) Visible light: narrow TiO2 band gap
Crystal properties Surface properties Porosity Band gap …
X. D. Wang, R. A. Caruso, J. Mater. Chem. 2011, 21, 20.
Control Material properties
X. Chen, S. S. Mao, Chem. Rev., 2007, 107, 2891.
Composition Crystal phase Morphology
Preparation of TiO2
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Synthesis of porous TiO2 materials
Composition Composition and Crystal phase
Morphology: beads Morphology: fibre
X .D. Wang, G.I. N. Waterhouse, D. R. G. Mitchell, K. Prince, R. A. Caruso, submitted
X. D. Wang, M. Blackford, K. Prince, R. A. Caruso, submitted
X. D. Wang, L. Cao, D.H. Chen, R. A. Caruso, in preparation
Ongoing project: collaboration with J. choi, Y.
B. Truong, and L.Kyratzis
UV light PC increase: Noble metal deposition decrease recombination of e-/h+
Crystal phase & Boron doping: band gap Noble metal deposition: Visible light PC: increased
400 nm
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TiCl3
Hydrolysis & condensation
NaOH
AmorphousTiO2
Washing
Solvothermal: 160°C, 16h
Crystallized TiO2
NaOH (mol) 0.041 0.054 0.059 0.068 0.070 0.073 0.076
Solution pH 0.25 0.56 0.80 7.92 7.98 9.67 11.58
Synthesis scheme
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Surface area
0
50
100
150
200
250
300
0.25 0.56 0.80 7.92 7.98 11.58 P25
pH during the synthesis
Su
rfac
e ar
ea (
m2 g
-1)
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Pore size distribution
0
0.2
0.4
0.6
0.8
1
1.2
1.4
0 20 40 60 80 100 120 140 160Pore diameter (nm)
dV
/dlo
gD
(cm
3/g
) 0.250.567.927.9811.58
-0.1
0.4
0.9
1.4
0 5 10 15 20
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Morphology-SEM
0.25
7.98
11.58
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Morphology and porosity -TEM
0.25 11.587.98
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5 15 25 35 45 55 65 75 85
2 theta (degree)
Inte
ns
ity
(a.
u.)
0.25
0.80
7.92
7.98
9.67
11.58
Crystal phase
Anatase
Rutile
Titanate
Acid condition: rutile phaseNeutral condition: anatase phase (slight brookite)Alkaline condition: titanate phase
8Å
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Surface hydroxyl groups (FT-IR)
0.00
0.01
0.02
0.03
0.04
0.05
0.06
0.07
1000150020002500300035004000
Wavenumber (cm-1)
abs
(a.
u.)
0.250.807.929.6711.58
Ti-OH
Ti…H2O
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Diffuse UV-Vis and band gap
0
10
20
30
40
50
60
70
80
90
100
200 300 400 500 600 700 800
Wavelength (nm)
Ref
lect
ance
(%
)
P25 0.25 7.98 11.58
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Diffuse UV-vis and Band gap
0
1
2
3
4
5
6
7
8
9
10
2.5 3 3.5 4
E (eV)
(F(r
)E)1
/2
11.587.987.929.670.560.25 pH9.67: 3.25 eV
pH11.58: 3.22 eV
pH7.98: 3.15 eV
pH0.56: 2.98 eV
pH7.92: 3.13 eV
pH0.25: 3.00 eV
pH 0.25 0.56 7.92 7.98 9.67 11.58 P25
Bg (eV) 3.00 2.98 3.13 3.15 3.25 3.22 3.10
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Adsorption test
Test conditions: 100 ppmIn the dark: shaking overnight (pH 5.10)
0
10
20
30
40
50
60
70
80
90
100
0.25 0.8 7.92 7.98 9.67 11.58 P25 AC
Ad
sorp
tio
n o
f M
B (
pp
m)
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Set up: 500 Watt Hg(Xe) lamp with band pass visible light filter (420-650 nm) Methylene blue (MB) as a probe molecule RSD< 3%
Photocatalysis reaction
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Photocatalytic activity
Test conditions: 12.5 ppm of MBVisible light: 120 min at pH 5.10
pH
40
50
60
70
80
90
100
0 20 40 60 80 100 120
Degradation time (min)
C/C
0 *
100%
0.250.807.927.989.67P2511.58
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Conclusions
• Solvothermal treatment produced high surface area TiO2.
• The material properties are pH dependant.
• The porous TiO2 prepared at pH 7.98 showed highest adsorption capacity.
• The maximum photocatalytic activity was for the sample prepared at pH 11.58.
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Acknowledgements
• My supervisor (Dr Rachel Caruso) & group members • Internal collaborations (Dr Patrick Hartley and Darryl Wells)• Synchrotron PD teams (Dr Qinfen Gu, Justin Kimpton & Kia
Wallwork )• Dr Nathan Webster for help with synchrotron data analysis
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CSIRO Materials Science and EngineeringDr Xingdong Wang
Ph: +61 3 9545 2689Email: [email protected]: www.csiro.au/cmse
CSIRO Materials Science and EngineeringDr Rachel Caruso OCE Science leader | Advanced Porous Materials Ph: +61 3 9545 7960Email: [email protected]: www.csiro.au/cmse