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Frontiers of Chemical Science and Engineering

ISSN 2095-0179

ISSN 2095-0187(Online)

CN 11-5981/TQ

Postal Subscription Code 80-969

2018 Impact Factor: 2.809

Front Chem Sci Eng    2012, Vol. 6 Issue (4) : 371-380    https://doi.org/10.1007/s11705-012-1215-3
RESEARCH ARTICLE
Comparison of the morphology and structure of WO3 nanomaterials synthesized by a sol-gel method followed by calcination or hydrothermal treatment
Diah Susanti1(), Stefanus Haryo N1, Hasnan Nisfu1, Eko Prasetio Nugroho1, Hariyati Purwaningsih1, George Endri Kusuma2, Shao-Ju Shih3
1. Materials and Metallurgical Engineering Department, Faculty of Industrial Technology, Sepuluh Nopember Institute of Technology (ITS), Surabaya 60111, Indonesia; 2. Mechanical Engineering Department, Surabaya State Shipbuilding Polytechnic, Surabaya 60111, Indonesia; 3. Materials Science and Engineering Department, Taiwan Tech (NTUST), Taipei 106, China
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Abstract

Tungsten (VI) oxide (WO3) nanomaterials were synthesized by a sol-gel method using WCl6 and C2H5OH as precursors followed by calcination or hydrothermal treatment. X-Ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM) equipped with energy dispersive X-ray spectroscopy (EDX) were used to characterize the structure and morphology of the materials. There were significant differences between the WO3 materials that were calcinated and those that were subjected to a hydrothermal process. The XRD results revealed that calcination temperatures of 300°C and 400°C gave hexagonal structures and temperatures of 500°C and 600°C gave monoclinic structures. The SEM images showed that an increase in calcination temperature led to a decrease in the WO3 powder particle size. The TEM analysis showed that several nanoparticles agglomerated to form bigger clusters. The hydrothermal process produced hexagonal structures for holding times of 12, 16, and 20 h and monoclinic structures for a holding time of 24 h. The SEM results showed transparent rectangular particles which according to the TEM results originated from the aggregation of several nanotubes.

Keywords WO3 nanomaterial      sol-gel method      calcination      hydrothermal     
Corresponding Author(s): Susanti Diah,Email:santiche@mat-eng.its.ac.id   
Issue Date: 05 December 2012
 Cite this article:   
Diah Susanti,Stefanus Haryo N,Hasnan Nisfu, et al. Comparison of the morphology and structure of WO3 nanomaterials synthesized by a sol-gel method followed by calcination or hydrothermal treatment[J]. Front Chem Sci Eng, 2012, 6(4): 371-380.
 URL:  
https://academic.hep.com.cn/fcse/EN/10.1007/s11705-012-1215-3
https://academic.hep.com.cn/fcse/EN/Y2012/V6/I4/371
Fig.1  Secondary electron SEM images of WO nanomaterials after calcination at different temperatures (a) 300°C, particle sizes: 277-780 nm, (b) 400°C, particle sizes: 137-550 nm, (c) 500°C, particle sizes: 50-500 nm and (d) 600°C, particle sizes: 25-125 nm. The circles indicate clusters of particles
Fig.1  Secondary electron SEM images of WO nanomaterials after calcination at different temperatures (a) 300°C, particle sizes: 277-780 nm, (b) 400°C, particle sizes: 137-550 nm, (c) 500°C, particle sizes: 50-500 nm and (d) 600°C, particle sizes: 25-125 nm. The circles indicate clusters of particles
Fig.1  Secondary electron SEM images of WO nanomaterials after calcination at different temperatures (a) 300°C, particle sizes: 277-780 nm, (b) 400°C, particle sizes: 137-550 nm, (c) 500°C, particle sizes: 50-500 nm and (d) 600°C, particle sizes: 25-125 nm. The circles indicate clusters of particles
Fig.1  Secondary electron SEM images of WO nanomaterials after calcination at different temperatures (a) 300°C, particle sizes: 277-780 nm, (b) 400°C, particle sizes: 137-550 nm, (c) 500°C, particle sizes: 50-500 nm and (d) 600°C, particle sizes: 25-125 nm. The circles indicate clusters of particles
Fig.1  Secondary electron SEM images of WO nanomaterials after calcination at different temperatures (a) 300°C, particle sizes: 277-780 nm, (b) 400°C, particle sizes: 137-550 nm, (c) 500°C, particle sizes: 50-500 nm and (d) 600°C, particle sizes: 25-125 nm. The circles indicate clusters of particles
Fig.1  Secondary electron SEM images of WO nanomaterials after calcination at different temperatures (a) 300°C, particle sizes: 277-780 nm, (b) 400°C, particle sizes: 137-550 nm, (c) 500°C, particle sizes: 50-500 nm and (d) 600°C, particle sizes: 25-125 nm. The circles indicate clusters of particles
Fig.2  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment at 200°C for holding times of (a) 12 h, (b) 16 h, (c) 20 h and (d) 24 h
Fig.2  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment at 200°C for holding times of (a) 12 h, (b) 16 h, (c) 20 h and (d) 24 h
Fig.2  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment at 200°C for holding times of (a) 12 h, (b) 16 h, (c) 20 h and (d) 24 h
Fig.2  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment at 200°C for holding times of (a) 12 h, (b) 16 h, (c) 20 h and (d) 24 h
Fig.2  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment at 200°C for holding times of (a) 12 h, (b) 16 h, (c) 20 h and (d) 24 h
Fig.2  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment at 200°C for holding times of (a) 12 h, (b) 16 h, (c) 20 h and (d) 24 h
Holding time /h12162024
Particle size /μm0.4-30.4-3.50.5-40.5-4.2
Particle thickness /nm~ 100~ 150~ 200~ 300
Tab.1  WO nanomaterials particle sizes after hydrothermal treatment at 200°C with different holding times
Fig.3  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment with a holding time of 12 h at (a) 160°C, (b) 180°C and (c) 200°C
Fig.3  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment with a holding time of 12 h at (a) 160°C, (b) 180°C and (c) 200°C
Fig.3  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment with a holding time of 12 h at (a) 160°C, (b) 180°C and (c) 200°C
Fig.3  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment with a holding time of 12 h at (a) 160°C, (b) 180°C and (c) 200°C
Fig.3  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment with a holding time of 12 h at (a) 160°C, (b) 180°C and (c) 200°C
Fig.3  Secondary electron SEM images of WO nanomaterials after hydrothermal treatment with a holding time of 12 h at (a) 160°C, (b) 180°C and (c) 200°C
Temperature /°C160180200
Particle size /μm0.4 - 20.4 - 2.20.4 - 3
Particle thickness /nm~ 70~ 90~ 100
Tab.2  Particle sizes of WO nanomaterials after hydrothermal treatment at different temperatures with a holding time of 12 h
Fig.4  XRD patterns of WO nanomaterials after calcination at 300°C, 400°C, 500°C and 600°C
Fig.4  XRD patterns of WO nanomaterials after calcination at 300°C, 400°C, 500°C and 600°C
Fig.4  XRD patterns of WO nanomaterials after calcination at 300°C, 400°C, 500°C and 600°C
Fig.4  XRD patterns of WO nanomaterials after calcination at 300°C, 400°C, 500°C and 600°C
Fig.4  XRD patterns of WO nanomaterials after calcination at 300°C, 400°C, 500°C and 600°C
Fig.4  XRD patterns of WO nanomaterials after calcination at 300°C, 400°C, 500°C and 600°C
Temperature /°C300400500600
Crystallite size /nm7.319.9220.428.36
Tab.3  Crystallite sizes of WO nanomaterial after calcination at different temperatures
Fig.5  XRD patterns of WO nanomaterials after hydrothermal treatment at holding times of 12, 16, 20, and 24 h
Fig.5  XRD patterns of WO nanomaterials after hydrothermal treatment at holding times of 12, 16, 20, and 24 h
Fig.5  XRD patterns of WO nanomaterials after hydrothermal treatment at holding times of 12, 16, 20, and 24 h
Fig.5  XRD patterns of WO nanomaterials after hydrothermal treatment at holding times of 12, 16, 20, and 24 h
Fig.5  XRD patterns of WO nanomaterials after hydrothermal treatment at holding times of 12, 16, 20, and 24 h
Fig.5  XRD patterns of WO nanomaterials after hydrothermal treatment at holding times of 12, 16, 20, and 24 h
Holding time /h12162024
Crystallite size /nm60.651.644.89.6
Tab.4  Crystallite sizes of WO nanomaterials after hydrothermal treatment at 200°C with different holding times
Fig.6  Bright-field TEM images of WO nanomaterials (a) before and (b) after calcination at 600°C, and (c) before and (d) after hydrothermal treatment at 200°C for 12 h
Fig.6  Bright-field TEM images of WO nanomaterials (a) before and (b) after calcination at 600°C, and (c) before and (d) after hydrothermal treatment at 200°C for 12 h
Fig.6  Bright-field TEM images of WO nanomaterials (a) before and (b) after calcination at 600°C, and (c) before and (d) after hydrothermal treatment at 200°C for 12 h
Fig.6  Bright-field TEM images of WO nanomaterials (a) before and (b) after calcination at 600°C, and (c) before and (d) after hydrothermal treatment at 200°C for 12 h
Fig.6  Bright-field TEM images of WO nanomaterials (a) before and (b) after calcination at 600°C, and (c) before and (d) after hydrothermal treatment at 200°C for 12 h
Fig.6  Bright-field TEM images of WO nanomaterials (a) before and (b) after calcination at 600°C, and (c) before and (d) after hydrothermal treatment at 200°C for 12 h
Fig.7  Bright-field TEM images of WO materials calcined at 600°C. (a) a WO cluster, (b) higher magnification of the square region in (a), (c) magnified WO image taken from the square region in (b)
Fig.7  Bright-field TEM images of WO materials calcined at 600°C. (a) a WO cluster, (b) higher magnification of the square region in (a), (c) magnified WO image taken from the square region in (b)
Fig.7  Bright-field TEM images of WO materials calcined at 600°C. (a) a WO cluster, (b) higher magnification of the square region in (a), (c) magnified WO image taken from the square region in (b)
Fig.7  Bright-field TEM images of WO materials calcined at 600°C. (a) a WO cluster, (b) higher magnification of the square region in (a), (c) magnified WO image taken from the square region in (b)
Fig.7  Bright-field TEM images of WO materials calcined at 600°C. (a) a WO cluster, (b) higher magnification of the square region in (a), (c) magnified WO image taken from the square region in (b)
Fig.7  Bright-field TEM images of WO materials calcined at 600°C. (a) a WO cluster, (b) higher magnification of the square region in (a), (c) magnified WO image taken from the square region in (b)
Fig.8  EDX spectra of WO taken from the area in Fig. 7(a)
Fig.8  EDX spectra of WO taken from the area in Fig. 7(a)
Fig.8  EDX spectra of WO taken from the area in Fig. 7(a)
Fig.8  EDX spectra of WO taken from the area in Fig. 7(a)
Fig.8  EDX spectra of WO taken from the area in Fig. 7(a)
Fig.8  EDX spectra of WO taken from the area in Fig. 7(a)
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