Solvothermal Synthesis of Mesoporous TiO2 Microspheres with Tailored Pore
Size and Specific Surface Area
Yajing Zhang1,3, Yuan Zhu1, Kangjun Wang1,3*, Fu Ding1,3*, Dan Meng1,
Xiaolei Wang2，Jing Wu1
1
College of Chemical Engineering, Shenyang University of Chemical Technology, Shenyang
110142, PR China
2
School of Science, Shenyang University of Technology, Shenyang 110870, PR China
3
Liaoning Co-innovation Center of Fine Chemical Industry, Shenyang 110142, PR China
To demonstrate the role of calcination, a contrast experiment without calcination
process was carried out.
In brief, 60 mL 0.2 M urea ethanol solution was slowly added into 3 mL TiCl3
(Titanium(III) chloride, 15% in 3% hydrochloric acid) under stirring. The solution
was transferred into a 100 mL teflonlined autoclave. The autoclave was maintained at
150 °C for 15 h before being cooled to room temperature naturally. The precipitate
was rinsed by ethanol for several times, dried at 100 °C for 12 h. And the obtained
sample is referred as T2before.
5000

Intensity(a.u.)
4000

NH4Cl

TiO2
3000
2000
1000




0
10
20
30
40
  

50
60


70
2Theta(degree)
Figure S1 XRD pattern of the T2before
*
Corresponding author. E-mail address: angle_79@163.com (kangjun Wang); dingfu@syuct.edu.cn (Fu Ding).
1
Figure S1 shows the XRD pattern of the sample without calcination process
(T2before). The diffraction peaks appear at 25.17o, 38.23o, 48.09o, 55.05o, 62.83o can be
indexed to TiO2 phase (Anatase, JCPDS 21-1272). And the diffraction peaks appear at
12.30o, 22.94o, 32.60o, 40.25o, 46.81o, 58.18o, 68.42o, and 73.16o can be indexed to
NH4Cl phase (JCPDS 07-0007).
Table 1 Specific surface area, pore volume and pore size of the samples before and
after calcination
Sample
SBET/
(m2g-1)
V/
(cm3g-1)
Dpore/
(nm)
T2 before
71.9
0.10
3.8
T2
106.3
0.29
7.8
2