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9 Supporting Information
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11  Copyright Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, 2018
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Hydrothermal Crystallization of Nano-Titanium Dioxide for
15 Enhanced Photocatalytic Hydrogen Generation
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17 Simanta Kundu and Vivek Polshettiwar*
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Synthesis of DFNT:
DFNS was prepared by our reported procedure with particle size of 390 (± 20)nm (Figure S1) and the
surface area and pore volume are 690 m²/g and 1.01 cm³/g respectively. DFNT was then synthesised by
TiO2 coating via ammonia-assisted solution-phase deposition technique. Briefly, DFNS(1 g)was taken in a
500 mL round bottom flask containing 180 mL of dried ethanol, and sonicated for 15 min followed by
stirring for 5 min at room temperature. To this dispersion, 2 mL of aqueous ammonia (25%) was added
dropwise, with final pH reached to10.8. The Ti-precursor, titanium(IV) butoxide (TBOT), 1.5 or 2.5 or 3.5
or 4.5 or 7.0 mL was then added dropwise to this dispersion at room temperature under stirring and then
further stirred at 45 °C for24 h. The resultant product was isolated by centrifugation, washed with ethanol (4
x 40 mL) and dried at 80 °C in an oven, to yield powder DFNT samples. These samples were named as
DFNT-x (where X is TBOT amount).

Hydrothermal crystallization of DFNT: As-prepared DFNT’s were amorphous and was crystallized by
hydrothermal treatment. In a typical process, as-prepared DFNT (110 mg) was dispersed in 30 mL of solvent
[dry ethanol (EtOH) or a mixture of water and EtOH] by sonication for 10 min. This dispersion was then
transferred to a 50 mL volume Teflon lined autoclave and autoclave was heated 180 oC in oven for 20h. The
autoclave was then cooled to room temperature and the product was collected by centrifugation. Obtained
solid was washed with EtOH and dried at 80 °C in an oven. These samples were named as DFNT-Hy (Hy
for hydrothermal).

Synthesis of trioctylphosphine oxide(TOPO) capped CdSe quantum dots (QDs): CdSe QDs were prepared
using reported method.29 Briefly, CdO (120 mg), oleic acid (2.5 mL) and 1-octadecene (10 mL) was taken in
a 50 mL three necked round bottomed flask and the mixture was heated under the flow of argon (Ar) at 120
o
C till the mixture becomes colourless. Then the mixture was cooled and TOPO (2 g) was added and the
temperature was increased to 280 oC with continuous flow of Ar. Premixed 5 mL clear solution mixture of
Se powder (118 mg), in 1.5 ml trioctylphosphine (TOP) and 1.5 ml 1-octadecene (1-ODE) under Ar was
quickly injected to above mixture at 280 oC. The growth time of the QDs was optimized to prepare different
sizes of the QDs. The reaction mixture was cooled down by addition of p-xylene and the final mixture was
made to a volume of 40 ml to fix QDs particle concentrations.

Attachment of CdSe QDs with DFNT: Solid QDs were isolated from CdSe QDs stock solution (4 mL) by
precipitating with EtOH. The precipitate was re-dissolved in n-hexane and again precipitated by EtOH. The
procedure was repeated one more time and finally QDs were dissolved in 5 ml n-hexane. On the other hand
80 mg of DFNT-Hy sample was dispersed in 5 ml n-hexane by sonication and then above QDs solution was
added drop wise to this dispersion under vigorous stirring. The mixture was stirred for overnight and then
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centrifuged to isolate the solid. It was then washed with n-hexane and EtOH and dried in oven at 80 oC. The
similar procedure was followed for different concentration and different sized QDs. Finally the samples
were annealed at 200 oC under Ar flow of 50 ml/min for 1 hour.

Photocatalytic Test for Hydrogen Generation: Photocatalytic measurements were carried out by taking five
milligrams of the catalyst (optimized by changing the weight of the catalysts), 2.5 mL of ethanol and 50 mL
of water in a 100 mL two-neck quartz round bottom flask (RB). Reaction mixture was sonicated for 10 sec
to disperse the particles and then stirred for a five minutes. An aqueous Pt solution (13 μL, 20 mM K 2PtCl4)
was added to the reaction mixture under continuous stirring. The RB was then sealed and purged with argon
gas for 30 min before irradiating with UV light (250–385 nm; light intensity = 33 mW/cm2), for 2 h. Gas
chromatography (GC) connected with thermal conductivity detector (TCD) was used to quantify hydrogen
evolution with time by injecting 1 mL of gas from the RB headspace into the GC. Detailed experimental set-
up is given in figure S4.Visible light photocatalysis was carried out with ~10 mg catalyst dispersion in 50 ml
aqueous solution of 0.1 M Na2SO3 and 0.05 M Na2S solution in a 50 ml two-neck quartz round bottom flask.
1 wt% Pt was photodeposited in the catalyst by UV-Vis light irradiation and degassed with Ar gas for 30
min before irradiation with Newport solar simulator equipped with filters (400–800 nm; light intensity = 140
mW/cm2).

Table S1. TiO2 loading and Textural properties of different DFNT samples.
Sample Name TBOT Amount TiO2 Loading BET Surface Pore Volume
(mL/gm DFNS) (wt%) Area (m2/g) (cm3/g)

DFNS 0 0 690 1.01

DFNT-1.5 1.5 10.8 624 0.78
DFNT-2.5 2.5 18.3 548 0.52
DFNT-3.5 3.5 25.3 535 0.48
DFNT-4.5 4.5 27.2 511 0.41
DFNT-7.0 7.0 47.7 419 0.27
Standard error in measurements: TiO2 loading ± 1 wt%, surface area ± 4%, pore volume ± 0.01.

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Figure S1. SEM images of DFNT samples prepared by addition of 1.5 ml (a, b), 2.5 ml (c, d), 3.5 ml (e, f),
4.5 ml (g, h) and 7 ml (i, j) of TiO2precursor (TBOT) per gram of DFNS.

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Figure S2. XRD pattern of DFNT-2.5 sample, as prepared (a), after hydrothermal treatment at 180 oC for 20
hour in,30 ml water (b),in water: ethanol mixture of 15:15 (c), 5:25 (d), 1.5:28.5 (e), 0.5:29.5 (f) and 30 ml
ethanol (g).

Table S2. Textural properties of DFNT-2.5 after hydrothermal treatment for 20 h at 180 oC in different
water:ethanol ratios.

Solvent ratio Crystallite size Average TiO2 Surface Pore TiO2

Water: of TiO2from particle size Area Volume (wt%)
EtOH XRD (nm) TEM (nm) (m²/g) (cm³/g)
0:30 8.8 5 400 0.62 19
0.5:29.5 11.5 10.8 367 0.61 21.3
1.5:28.5 12.3 17.5 369 0.59 21.5
5:25 10.6 10.1 362 0.55 23.3
15:15 7.5 9.1 424 0.85 21.4
30:0 8.7 8 602 0.92 23.3
asp - - 548 0.52 18.3
asp- as prepared; Standard error in measurements: TiO2 loading ± 1 wt%, surface area ± 4%, pore volume ± 0.01.

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Figure S3. SEM images of DFNT samples after hydrothermal treatment at 180 oC for 20 hour in30 ml water
(a, b), 15:15 (c, d), 5:25 (e, f), 1.5:28.5 (g, h), 0.5:29.5 (i, j) water: ethanol mixture and 30 ml ethanol (k, l).

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 Figure S4. Set up for typical photocatalytic hydrogen generation experiment.

Figure S5. XRD pattern of the DFNT samples with different hydrothermal treatment time in EtOH at 180
o
C.

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Figure S6.SEM images of the DFNT samples with 2 (a, b); 4 (c, d); 6 (e, f); 9 (g, h); 12 (i, j) and 20 (k, l)
hour of hydrothermal treatment time in EtOH at 180 oC.

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Figure S7. SEM images of hydrothermally treated DFNT-2.5 samples at 150 oC (a, b), 180 oC (c, d) and 210
o
C (e, f)

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Figure S8. PXRD patterns of hydrothermally treated DFNT-2.5 samples at 150, 180 and 210 oC.

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Figure S9. SEM images of hydrothermally treated DFNT samples in ethanol for 12 hour at 180oC obtained
after addition of 1.5 ml (a, b), 2.5 ml (c, d), 3.5 ml (e, f), 4.5 ml (g, h) and 7 ml (i, j) of precursor TBOT.

Figure S10. H2 generation with respect to catalyst (DFNT-4.5-Hy) amount. Panel (a) shows the amount of
total hydrogen per hour and panel (b) shows the amount of hydrogen per gm of catalyst per hour.

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Figure S11. Hydrogen generation activity with variation of the co-catalyst (Pt) amount using DFNT-4.5-Hy.

Figure S12. Recyclability and long term irradiation stability test of the DFNT-4.5-Hy.

Figure S13. SEM image of the DFNT-4.5-Hy catalyst after photocatalysis under UV light.

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Figure S14. TEM image of the DFNT-4.5-Hy catalyst after photocatalysis under UV light. Arrow marked
dark contrast particles are the photo-deposited Pt nanoparticles as co-catalyst.

Figure S15. Schematic representation of DFNT/CdSe heterostructure preparation.

Figure S16. (a) Absorption spectra of DFNT-4.5-Hy/CdSe heterostructures with different concentration of
552 nm absorption maxima CdSe QDs, (b) hydrogen evolution plot for DFNT/CdSe hybrids with different
loading of CdSe QDs (552 nm absorption maxima) and heated at 200 oC using 1 wt% photodeposited Pt as
cocatalyst.
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Figure S17.TEM images of the DFNT-4.5-Hy/CdSe (4 ml, 552 nm) hetero-structures before annealing,
where no outside particles were observed.

Figure S18. (a) Absorption spectra of DFNT-4.5-Hy/CdSe heterostructures with three different CdSe QDs
with absorption maxima at 518 nm, 552 nm and 618nm; (b)hydrogen evolution plot for of DFNT-4.5-
Hy/CdSe hybrids with 4 ml loading of different sized (denoted as absorption maxima) CdSe QDs and heated
at 200 oC with 1 wt% photodeposited Pt as cocatalyst.

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Table S3. Comparison of DFNT with various TiO2based photo-catalysts.
S.N. Catalyst Irradiation Conditions Reaction Conditions H2 yield Reference
(μmolh-1
g-1TiO2)
1 DFNT-4.5-Hy/Pt 300 W Xe lamp, 1.6 mg of catalyst, 2.5 mL of 81204 This work
33 mW/cm2 ethanol, 50 mL of H2O
2 CoOx/TiO2/Pt 300 W Xe lamp, 35 mg of catalyst, 200 mL 15 7882 1
35 mW/cm2 vol.% methanol- water
3 TiO2 (P25)/Cu 300 W Xe lamp, 50 mg of catalyst, 100 mL 30 9500 2
600 mW/cm2 vol.% methanol- water
4 Black TiO2/Pd UV-B lamp with λmax 50 mg of catalyst, 2000 mL 50 9300 3
~ 312, 8000 mW/cm2 vol.% ethanol- water
5 TiO2 (P25)/Pt 500 W Xe lamp 50 mg catalyst, 100 mL 20 vol.% 15600 4
methanol- water, 0.05 mol/L
AgNO3
6 Anatase TiO2/Pt 500 W Xe lamp 50 mg catalyst, 100 mL 20 vol.% 12000 4
methanol- water, 0.05 mol/L
AgNO3
7 Rutile TiO2/Pt 500 W Xe lamp 50 mg catalyst, 100 mL 20 vol.% 14400 4
methanol- water, 0.05 mol/L
AgNO3
8 TiO2/MoS2/graphene 350 W Xe lamp, 80 mg catalyst, 80 mL 25 vol.% 2066 5
composite 20 mW/cm2 ethanol- water
9 TiO2 (P25)/Ni1Pd10 400 W Mercury arc 50 mg of catalyst, 35 mL 50 vol.% 4100 6
lamp methanol- water
10 TiO2/SiO2 500W Xe lamp 2.0 mg of catalyst, 1.6 mL of H2O, 12750 7
(Ti-MCM-48-1-200.) 0.4 mL of methanol
11 TiO2/MCM-48-im-200 300 W Xe lamp 2.0 mg of catalyst, 1.6 mL of 3830 8
equipped with an water, 0.4 mL ofmethanol
optical cut-off filter
(230 nm < λ < 380 nm).
12 2 wt % Pt/F-TiO2 350 W Xe arc lamp, 20 mg of catalyst, 16675 9
UV-visible, 20mW/cm2 20 mL of ethanol, 60 mL of water
13 TiO2:Eu 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 13200 10
(50:1), 0.3 wt % Pt as cocatalyst
14 SiO2-TiO2 300 W Xe lamp 0.1 g of catalyst, water:CH3OH 12487 11
(80:20), 0.5 % Pt
15 TiO2:Gd 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 10800 10
(50:1), 0.3 wt % Pt as cocatalyst.
16 TiO2:Ho 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 10200 10
(50:1), 0.3 wt % Pt as cocatalyst
17 TiO2:Yb 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 8400 10
(50:1), 0.3 wt % Pt as cocatalyst
18 TiO2:Y 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 7800 10
(50:1), 0.3 wt % Pt as cocatalyst
19 TiO2:La 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 7680 10
(50:1), 0.3 wt % Pt as cocatalyst
20 Pt/TiO2 300 W Xe lamp glycerol (20 vol % aq) 7280 12

21 mesoporous  TiO2 300 W Hg lamp 0.8 g of catalyst, 800 mL of water, 160 13
80 mL of CH3OH, Pt as cocatalyst
22 rutile/anatase TiO2 450 W Xe lamp 0.2 g of catalyst, 160 mL of water, 6700 14
40 mL of CH3OH, 0.3 wt % Pt as
cocatalyst

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23 F-TiO2 sphere with 300W Xe arc lamp 0.1 g of catalyst, 80 mL of water , 5841 15
45% {001} facets 20 mL of methanol, 1 wt % Pt
24 2.2% W/C on TiO2 500W Hg lamp MeOH (50 vol % aq sol.) 5350 16
25 TiO2:Tb 300 W Hg lamp 0.1 g of catalyst, water:CH3OH 4800 10
(50:1), 0.3 wt % Pt as cocatalyst
26 0.5 wt % Pt/TiO2 1000 W Xe lamp, 0.0375 g of catalyst, 75 mL of 4266 17
UGI-black filter aqueous methanol solution
27 colloid TiO2 450 W Hg lamp 0.025 g of catalyst, HCl, Pt−RuO2 4000 18
as cocatalyst
28 (5 wt %) Ag/TiO2 NT Hg or Xe lamp MeOH (5 vol % aq) 3200 19

29 Mesoporous TiO2-SiO2 300 W Xe lamp 0.1 g of catalyst, 10 mL of water 3108 20

and 5 mL of CH3OH, 1% Pt
30 1.2 wt % Pt/TiO2 350 W Hg lamp 0.1 g of catalyst, 54 mL of water 2700 21
and 6 mL of CH3OH
31 0.5% Pt/TiO2/KIT-6- 300 W Xe Lamp 100 mg of catalyst, 270 mL of a 2179 22
1.75 20% methanol aqueous solution
32 Pt/TiO2/ Carrageenan Hg Lamp 740 mW cm-2 MeOH (50 vol % aq) 1950 23

33 TiO2 (anatase, 78%), 400 W Hg Lamp 0.3 g of catalyst, 350 mL of aq. 1893 24

P25 TiO2 Na2CO3 solution pH 11, 3 wt % Pt
34 10 wt % NaOH coated 500 W Hg Lamp 0.3 g of catalyst, water vapour, Rh 1497 25
Rh/TiO2 (anatase) 250−400 nm
35 1 wt % Pt/TiO2 Not mentioned 0.1 g of catalyst, 300 mL of 10 vol 800 26
% methanol solution
36 1 wt % Pt/TiO2 Not mentioned 0.1 g of catalyst, 300 mL of 10 vol 500-600 26
% methanol aqueous solution
37 1 wt % Pt/B-TiO2 Not mentioned 0.1 g of catalyst, 300 mL of 10 vol 200 26
% methanol aqueous solution
38 0.4 wt % Pt-C/TiO2 500 W Xe lamp 0.065 g of catalyst, 80 mL of 26.2 27
water, 20 mL of methanol
39 3 wt % Pt/TiO2 pulp 400 W Hg Lamp Ethanol-water solution 7.7 28

Note: Several reports did not mention actual light intensity falling on the reactor; hence only total lamp
power is given for those entries in the above table.

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