热处理对铁掺杂TiO_2锐钛矿-金红石相变的影响
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摘要
采用溶胶-凝胶法制备了纯TiO_2和不同浓度Fe掺杂TiO_2纳米粉末,并对各样品进行了350℃、500℃、650℃的热处理。通过SEM、XRD、EDS、XPS等测试方法对其表面形貌、晶体结构及成分组成进行了表征,研究了热处理温度对Fe掺杂TiO_2相变的影响。实验结果表明:纯TiO_2与Fe-TiO_2在350℃、500℃时均为单一的锐钛矿,650℃时大部分转变为金红石;热处理温度升高有利于锐钛矿向金红石的转变;Fe掺杂后以+3价的形式存在,Fe离子掺杂能够明显减小TiO_2的晶粒尺寸,高浓度的Fe掺杂对锐钛矿-金红石相变有微弱的促进作用。
The pure and Fe-doped TiO_(2 )with different concentrations nanopowders were synthesized by sol-gel method and annealed at the temperature of 350℃,500℃and 650℃.The surface morphology,crystal structure and elemental composition were characterized by SEM,XRD,EDS and XPS.The influence of heat treatment temperature on the phase transformation of Fe-doped TiO_(2 )was studied.Experimental results showed that both the pure and Fe-doped TiO_(2 )were anatase at the temperature of 350℃and 500℃,respectively.The phase structure of pure and Fe-doped TiO_2were almost all rutile at the temperature of 650℃,which indicated that higher heat treatment temperature promoted the phase transformation of anatase and rutile.Fe element exsited in the form of+3valence.The incorporation of Fe into TiO_2lattices decreased the crystallite size of TiO_2.Fe doping with high dopant level had a slight promotion effect on the phase transition from anatase to rutile.
The pure and Fe-doped TiO_(2 )with different concentrations nanopowders were synthesized by sol-gel method and annealed at the temperature of 350℃,500℃and 650℃.The surface morphology,crystal structure and elemental composition were characterized by SEM,XRD,EDS and XPS.The influence of heat treatment temperature on the phase transformation of Fe-doped TiO_(2 )was studied.Experimental results showed that both the pure and Fe-doped TiO_(2 )were anatase at the temperature of 350℃and 500℃,respectively.The phase structure of pure and Fe-doped TiO_2were almost all rutile at the temperature of 650℃,which indicated that higher heat treatment temperature promoted the phase transformation of anatase and rutile.Fe element exsited in the form of+3valence.The incorporation of Fe into TiO_2lattices decreased the crystallite size of TiO_2.Fe doping with high dopant level had a slight promotion effect on the phase transition from anatase to rutile.
引文
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[2]杨志广,王筠,吴亚楠,等.TiO2纳米管的制备及其抑菌性能研究[J].化工新型材料,2015,43(7):60-62.
[3]张鹏会,李艳春,胡浩斌,等.B、N和Ce共掺杂TiO2光催化降解染料废水研究[J].化工新型材料,2016,44(3):229-231.
[4]Dubey R S.Temperature-dependent phase transformation of TiO2nanoparticles synthesized by sol-gel method[J].Materials Letters,2018,215:312-317.
[5]Abd El-Lateef H M,Khalaf M M.Corrosion resistance of ZrO2-TiO2 nanocomposite multilayer thin films coated on carbon steel in hydrochloric acid solution[J].Materials Characterization,2015,108:29-41.
[6]Bhangea P D,Awate S V,Gholap R S.et al.Photocatalytic degradation of methylene blue on Sn-doped titania nanoparticles synthesized by solution combustion route[J].Materials Research Bulletin,2016,76:264-272.
[7]Bokare A,Pai M,Athawale A A.Surface modified Nd doped TiO2nanoparticles as photocatalysts[J].Solar Energy,2013,91(8):111-119.
[8]Huang D G,Liao S J,Zhou W B,et al.Synthesis of samariumand nitrogen-co-doped TiO2by modified hydrothermal method and its photocatalytic performance for the degradation of4-chlorophenol[J].Journal of Physics and Chemistry of Solids,2009,7(5):853-859.
[9]孟丹,王和义,刘秀华,等.Fe掺杂对纳米TiO2薄膜的结构与光催化性能的影响[J].应用化学,2011,28(12):1379-1386.
[10]Wei N,Cui H,Song Q,et al.Ag2O nanoparticle/TiO2nanobelt heterostructures with remarkable photo-response and photocatalytic properties under UV,visible and near-infrared irradiation[J].Applied Catalysis B:Environmental,2016,198:83-90.
[11]Uvarov V,Popov I.Metrological characterization of X-ray diffraction methods for determination of crystallite size in nanoscale materials[J].Materials Characterization,2007,58(10):883-891.
[12]陈桂华,葛昌华,潘富友,等.化学沉淀法制备纳米Fe/TiO2及其光催化活性的研究[J].人工晶体学报,2010,39(2):433-439.
[13]Spurr R A,Myers H.Quantitative analysis of anatase-rutile mixtures with an X-Ray diffractometer[J].Analytical Chemistry,1957,29(5):760-762.
[14]Tripathi A K,Mathpal M C,Kumar P,et al.Structural,optical and photoconductivity of Sn and Mn doped TiO2nanoparticles[J].Journal of Alloys and Compounds,2015,622:37-47.
[15]顾建军,刘鹏飞,韩金荣,等.Fe掺杂量和退火氛围对TiO2薄膜晶体结构和磁性能的影响[J].材料工程,2014(10):101-105.