Anatase TiO2 Nanoparticles: Facile Synthesis via Non-aqueous Precipitation and Photocatalytic Property

doi:10.15541/jim20170532

Abstract

Abstract:

A facile strategy for anatase titanium dioxide (TiO₂) nanoparticle preparation was proposed via a non-aqueous precipitation method. With the aid of glacial acetic acid, tetrabutyl titanate underwent non-hydrolytic reaction in solvent ethanol. Glacial acetic acid increased polarity of Ti-O and C-O bonds of tetrabutyl titanate, and promoted non-hydrolytic de-etherization poly condensation reaction to form Ti-O-Ti bond in the solvent. After refluxing at 80℃ for 24 h, the Ti-O-Ti bond was rearranged to form anatase TiO₂ nanoparticles with the particle size of 5 nm-20 nm and specific surface area of 169.4 m²/g, which exhibited good dispersion and excellent photocatalytic activity. The degradation rate against methyl orange under ultraviolet radiation for 2 h reached 99.81%, showing promising prospect in wastewater treatment process.

Key words: TiO₂, non-aqueous precipitation method, photocatalytic property, low temperature synthesis

CLC Number:

TQ174

JIANG Feng, YU Yun, FENG Ai-Hu, YU Yang, MI Le, SONG Li-Xin. Anatase TiO₂ Nanoparticles: Facile Synthesis via Non-aqueous Precipitation and Photocatalytic Property[J]. Journal of Inorganic Materials, 2018, 33(10): 1136-1140.

Figures/Tables 8

Fig. 1 (a, b) TEM, (c) HRTEM images and (d) SAED pattern of the as-prepared TiO2 nanoparticles

Fig. 2 FT-IR spectra of samples at different reaction stages

Table 1 Peak position of samples at different reaction stages (cm-1)

Ti(OBu)₄	Ti(OBu)₄+ AcOH	Precipitate slurry	Precipitate	Attribution	Ref.
3334	-	3334	-	OH	[19]
2958	2958	2958	-	C-H	[20]
2933	2933	2933	-	aromatic C-C	[21]
2873	2873	2873	-	C-H	[20]
2700	-	-	-	C-H	[20]
1460	-	-	-	-CH₂	[22]
1379	1419	-	-	-CH₃	[22]
1124	-	-	-	Ti-O-C	[23]
1096	-	-	-	Ti-O-C	[23]
1039	-	-	-	Ti-O-C-	[23]
611	613	-	-	Ti-O	[24]
-	1724	1735	-	-C==O	[25]
-	1547	-	-	COO-group	[26]
-	1290	-	-	C-O	[27]
-	1070	1074	-	C-O	[28]
-	1028	1045	-	C-O	[29]
-	-	1458	-	CH₂	[30]
-	-	1378	-	Sym COO	[31]
-	-	1189	-	C-O	[32]
-	-	881	-	C-COO	[31]
-	-	438	455	Ti-O-Ti	[33]

Fig. 3 Mechanism of acetic acid coordinated with butyl titanate

Fig. 4 FT-IR spectrum of the non-hydrolytic polycondensation by-product

Fig. 5 Schematic diagram of the proposed mechanism for the formation of TiO2 nanoparticles

Fig. 6 Photodegradation effect of TiO2 nanoparticles(a) UV-Vis absorption spectra of MO solutions after photocatalytic performance test at different time intervals; (b) Photodegradation rate of MO after photocatalysis by TiO2 nanoparticles and commercial P25 powders

Fig. 7 Kinetics of MO photodegradation (linear transform ln(c/c0) vs t in photocatalytic experiments)

References 35

[1]	KHAN S U M, AL S M, INGLER W B. Efficient photochemical water splitting by a chemically modifiedn-TiO2. Science, 2002, 297(5590): 2243-2245.
[2]	BACH U, LUPO D, COMTE P,et al. Solid-state dye-sensitized mesoporous TiO2 solar cells with high photon-to-electronconversion efficiencies. Nature, 1998, 395(6702): 583-585.
[3]	GAYA U I, ABDULLAH A H.Heterogeneous photocatalytic degradation of organic contaminants over titanium dioxide: a review of fundamentals, progress and problems.Journal of Photochemistry & Photobiology C Photochemistry Reviews, 2006, 9(1): 1-12.
[4]	JUNG K Y, PARK S B, JANG H D.Phase control and photocatalytic properties of nano-sized titania particles by gas-phase pyrolysis of TiCl4.Catalysis Communications, 2004, 5(9): 491-497.
[5]	LOOK J L, ZUKOSKI C F.Alkoxide-derived titania particles: use of electrolytes to control size and agglomeration levels.Journal of the American Ceramic Society, 2010, 75(6): 1587-1595.
[6]	JIANG H Q, WANG P, GUO X L,et al. Preparation and characterization of low-amount Yb3+-doped TiO2 photocatalyst. Russian Chemical Bulletin, 2006, 55(10): 1743-1747.
[7]	GUO Y G, HU Y S, SIGLE W.Superior electrode performance of nanostructured mesoporous TiO2 (anatase) through efficient hierarchical mixed conducting networks. Advanced Materials, 2007, 19(16): 2087-2091.
[8]	ADDAMO M, AUGUGLIARO V, PAOLA A D,et al. Preparation, characterization, and photoactivity of polycrystalline nanostructured TiO2 catalysts. The Journal of Physical Chemistry A, 2004, 35(21): 3303-3310.
[9]	SUGIMOTO T, ZHOU X, MURAMATSU A.Synthesis of uniform anatase TiO2 nanoparticles by Gel-Sol method 4. Shape control.Journal of Colloid and Interface Science, 2003, 259(1): 53-61.
[10]	SUGIMOTO T, ZHOU X, MURAMATSU A.Synthesis of uniform anatase TiO2 nanoparticles by Gel-Sol method. 3. Formation process and size control.Journal of Colloid and Interface Science, 2003, 259(1): 43-52.
[11]	ZHANG Y X, LI G H, JIN Y X.Hydrothermal synthesis and photoluminescence of TiO2 nanowires.Chemical Physics Letters, 2002, 365(3/4): 300-304.
[12]	HE W, FANG Z, ZHANG K,et al. Continuous synthesis of a co-doped TiO2 photocatalyst and its enhanced visible light catalytic activity using a photocatalysis microreactor. RSC Advances, 2015, 5(68): 54853-54860.
[13]	REYES C D, RODRÍGUEZ G G, ESPINOSA P M E,et al. Phase-pure TiO2 nanoparticles: anatase, brookite and rutile. Nanotechnology, 2008, 19(14): 1-10.
[14]	CHAN S K, KOICHI N, BIN X,et al. A new observation on the phase transformation of TiO2 nanoparticles produced by a CVD method. Aerosol Science & Technology, 2005, 39(2): 104-112.
[15]	FENG Q, WANG T, ZHANG F, et al. Synthesis of TiO2 photocatalytic materials via solid-state reaction and its photodegradation property for methyl orange. Material Research Innovations, 2015, 18(S4): 92-96.
[16]	BANNIER E, DARUT G, SÁNCHEZ E,et al. Microstructure and photocatalytic activity of suspension plasma sprayed TiO2 coatings on steel and glass substrates. Surface & Coatings Technology, 2011, 206(2/3): 378-386.
[17]	ZHU J, BIAN Z F, REN J,et al. An integrated low temperature approach to highly photoactive nanocrystalline mesostructured titania. Catalysis Communications, 2007, 8(7): 971-976.
[18]	ZHU J, YANG J, BIAN Z F,et al. Nanocrystalline anatase TiO2 photocatalysts prepared via a facile low temperature nonhydrolytic Sol-Gel reaction of TiCl4 and benzyl alcohol. Applied Catalysis B Environmental, 2007, 76(1): 82-91.
[19]	PIRES D C, STOCKLERPINTO D V B, SCIAMARELI J,et al. Synthesis and characterization by infrared spectroscopy of hydantoin-based bonding agents, used in composite propellants. Journal of Aerospace Technology & Management, 2009, 1(2): 177-184.
[20]	MAX J J, DANEAULT S, CHAPADOS C.1-Propanol hydrate by IR spectroscopy.Canadian Journal of Chemistry, 2002, 80(1): 113-123.
[21]	JULKAPLI N M, AHMAD Z, AKIL H M.Preparation and characterization of 1,2,4,5-benzenetetra carboxylic-chitosan. E-Polymers, 2010, 10(1): 841-857.
[22]	ENESCU D, FRACHE A.Effects of sterically hindered N-alkoxyamines on photooxidative stability of reinforced polypropylene. E-Polymers, 2013, 12(1): 949-959.
[23]	VELASCO M J, RUBIO F, RUBIO J.Hydrolysis of titanium tetrabutoxide. study by FT-IR spectroscopy.Spectroscopy Letters, 1999, 32(2): 289-304.
[24]	HWANG J D, CHOU C H.On the origin of leakage current reduction in TiO2 passivated porosus silicon Schottky-barrier diode. Applied Physics Letters, 2010, 96(6): 063501-063503.
[25]	URBAN M W, KOENIG J L, SHIH L B,et al. Structure of styrene/acrylic acid copolymer in aqueous solution determined by Fourier transform infrared spectroscopy. Applied Spectroscopy, 1987, 41(4): 590-596.
[26]	FUGU M B, NDAHI N P, PAUL B B,et al. Synthesis, characterization, and antimicrobial studies of some vanillin schiff base metal (ii) complexes. Journal of Chemical & Pharmaceutical Research, 2013, 5(1): 22-28.
[27]	ZHANG W, ZHANG H, XIAO J,et al. Carbon nanotube catalyst for oxidative desulfurization of a model diesel fuel using molecular oxygen. Green Chemistry, 2013, 16(1): 211-220.
[28]	GEIGER C, ZELENKA C, WEIGL M,et al. Synthesis of bicyclic sigma receptor ligands with cytotoxic activity. Journal of Medicinal Chemistry, 2007, 50(24): 6144-6153.
[29]	SUN S L, WEN J L, MA M G,et al. Successive alkali extraction and structural characterization of hemicelluloses from sweet sorghum stem. Carbohydr. Polym., 2013, 92(2): 2224-2231.
[30]	NIKODEM K, GRAŻYNA S G, LIDIA O,et al. A study on the synthesis and properties of substituted EHBG-Fe(iii) complexes as potential MRI contrast agents. Journal of Organometallic Chemistry, 2014, 769(1): 100-105.
[31]	CHOE J I, KIM G H.Ab initio study of vibrational spectra of p-tert-butylcalix[4]aryl ester complexed with alkali metal cation. Journal of the Korean Chemical Society, 2006, 50(1): 7-13.
[32]	SUGIHARTO A B, JOHNSON C M, DUNLOP I E,et al. Delocalized surface modes reveal three-dimensional structures of complex biomolecules. Journal of Physical Chemistry C, 2008, 112(20): 7531-7534.
[33]	LI Z, HOU B, XU Y,et al. Comparative study of Sol-Gel- hydrothermal and Sol-Gel synthesis of titania-silica composite nanoparticles. Journal of Solid State Chemistry, 2005, 178(5): 1395-1405.
[34]	LIANG C Y, KRIMM S.Infrared spectra of high polymers: Part IX. Polyethylene terephthalate.Journal of Molecular Spectroscopy, 1959, 3(1-6): 554-574.
[35]	ZHANG L, LI H, LIU Y,et al. Adsorption-photocatalytic degradation of methyl orange over a facile one-step hydrothermally synthesized TiO2/ZnO-NH2-RGO nanocomposite. RSC Advances, 2014, 4(89): 48703-48711.

Anatase TiO₂ Nanoparticles: Facile Synthesis via Non-aqueous Precipitation and Photocatalytic Property

RichHTML

PDF (PC)

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 8

References 35

Related Articles 15

Recommended Articles

Metrics

Comments

[1]	AN Lin, WU Hao, HAN Xin, LI Yaogang, WANG Hongzhi, ZHANG Qinghong. Non-precious Metals Co_5.47N/Nitrogen-doped rGO Co-catalyst Enhanced Photocatalytic Hydrogen Evolution Performance of TiO₂ [J]. Journal of Inorganic Materials, 2022, 37(5): 534-540.
[2]	LÜ Qingyang, ZHANG Yuting, GU Xuehong. Fabrication of Hollow Fiber Supported TiO₂ Ultrafiltration Membranes via Ultrasound-assisted Sol-Gel Method [J]. Journal of Inorganic Materials, 2022, 37(10): 1051-1057.
[3]	XIAO Xiang, GUO Shaoke, DING Cheng, ZHANG Zhijie, HUANG Hairui, XU Jiayue. CsPbBr₃@TiO₂ Core-shell Structure Nanocomposite as Water Stable and Efficient Visible-light-driven Photocatalyst [J]. Journal of Inorganic Materials, 2021, 36(5): 507-512.
[4]	XI Wen, LI Haibo. Preparation of TiO₂/Ti₃C₂T_x Composite for Hybrid Capacitive Deionization [J]. Journal of Inorganic Materials, 2021, 36(3): 283-291.
[5]	LIU Cai, LIU Fang, HUANG Fang, WANG Xiaojuan. Preparation and Photocatalytic Properties of Alga-based CDs-Cu-TiO₂ Composite Material [J]. Journal of Inorganic Materials, 2021, 36(11): 1154-1162.
[6]	Li Cuixia, SUN Huizhen, JIN Haize, SHI Xiao, LI Wensheng, KONG Wenhui. Construction and Photocatalytic Performance of 3D Hierarchical Pore rGO/TiO₂ Composites [J]. Journal of Inorganic Materials, 2021, 36(10): 1039-1046.
[7]	WANG Ping,LI Xinyu,SHI Zhanling,LI Haitao. Synergistic Effect of Ag and Ag₂O on Photocatalytic H₂-evolution Performance of TiO₂ [J]. Journal of Inorganic Materials, 2020, 35(7): 781-788.
[8]	JI Bang, ZHAO Wenfeng, DUAN Jieli, MA Lizhe, FU Lanhui, YANG Zhou. Synthesis of TiO₂/WO₃ on Nickel Foam for the Photocatalytic Degradation of Ethylene [J]. Journal of Inorganic Materials, 2020, 35(5): 581-588.
[9]	HUANG Xieyi,WANG Peng,YIN Guoheng,ZHANG Shaoning,ZHAO Wei,WANG Dong,BI Qingyuan,HUANG Fuqiang. Removal of Volatile Organic Compounds Driven by Platinum Supported on Amorphous Phosphated Titanium Oxide [J]. Journal of Inorganic Materials, 2020, 35(4): 482-490.
[10]	WANG Xucong, DENG Hao, JIANG Zhongyi, YUAN Liyong. Photocatalytic Reduction of Re (VII) on Amorphous TiO₂/g-C₃N₄ Derived from Different N Sources [J]. Journal of Inorganic Materials, 2020, 35(12): 1340-1348.
[11]	LIU Jinyun, ZHANG Yuting, HONG Zhou, LIU Hua, WANG Shengxian, GU Xuehong. Fabrication of Dual-layer Hollow Fiber Ceramic Composite Membranes by Co-extrusion [J]. Journal of Inorganic Materials, 2020, 35(12): 1333-1339.
[12]	CHEN Haoyu, ZHANG Yiwen, WU Zhong, QIN Zhenbo, WU Shanshan, HU Wenbin. Room Temperature Magnetoresistance Property of Co-TiO₂ Nanocomposite Film Prepared by Strong Magnetic Target Co-sputtering [J]. Journal of Inorganic Materials, 2020, 35(11): 1263-1267.
[13]	ZHANG Ya-Ping, DING Wen-Ming, ZHU Hai-Feng, HUANG Cheng-Xing, YU Lian-Qing, WANG Yong-Qiang, LI Zhe, XU Fei. Photoelectrochemical Properties of MoSe₂ Modified TiO₂ Nanotube Arrays [J]. Journal of Inorganic Materials, 2019, 34(8): 797-802.
[14]	JIAO Si-Yi, GE Wan-Yin, YIN Li-Xiong, XU Mei-Mei, CHANG Zhe, ZHANG Li. Controllable Synthesis and Growth Mechanism of Two-dimensional TiSe₂ Nanosheets [J]. Journal of Inorganic Materials, 2019, 34(8): 834-838.
[15]	Xi-Qing LÜ, Huan-Yu ZHANG, Rui LI, Mei ZHANG, Min GUO. Nb₂O₅ Coating on the Performance of Flexible Dye Sensitized Solar Cell Based on TiO₂ Nanoarrays/Upconversion Luminescence Composite Structure [J]. Journal of Inorganic Materials, 2019, 34(6): 590-598.