钴掺杂对二氧化钛晶粒尺寸及相变的影响
|
摘要
通过溶胶凝胶法制备了纯Ti O_2与不同Co浓度掺杂的Ti O_2纳米粉体,并对样品进行了450、550、650℃保温2 h的热处理.采用X射线衍射仪对制得的纳米粉体进行了晶体结构表征,研究了热处理温度以及Co掺杂浓度对Ti O_2晶粒尺寸以及锐钛矿金红石相变的影响.结果表明:纯Ti O_2与Co-Ti O_2在450℃时为单一的锐钛矿;550℃时,纯Ti O_2有微量金红石生成,Co-Ti O_2仍然全部为锐钛矿;650℃时纯Ti O_2大部分转变为金红石,当Co掺杂量较低时,Co能促进锐钛矿相向金红石相的转变,而当掺杂浓度为8%时,Co抑制锐钛矿相向金红石相的转变;热处理温度升高以及Co掺杂浓度增加有利于Co Ti O_3相的生成,相同温度下,Co掺杂后Ti O_2晶粒尺寸减小.
The pure Ti O_2and Ti O_2nanopowder with different Co-doped concentrations are synthesized via a sol-gel method and the nanopowders are annealed at the temperature of 450℃,550℃and 650℃for 2 hours.The crystal structure of the obtained samples is characterized by XRD.The effects of heat treatment temperature and Co doping content on the crystallite size and phase transition from anatase to rutile are investigated.The results show that both pure Ti O_2and Co-Ti O_2are pure anatase at the temperature of 450℃.Pure Ti O_2forms a little rutile and Co-Ti O_2is still anatase at 550℃.Most of the pure Ti O_2forms rutile at 650℃.The phase transition from anatase to rutile is promoted when Co doping content is at a low level and is inhibited when Co doping concentration is 8%.The enhancement of heat treatment temperature and higher Co doping content are beneficial for the formation of Co Ti O_3.The grain size of Ti O_2decreases after Co doping at the same temperature.
The pure Ti O_2and Ti O_2nanopowder with different Co-doped concentrations are synthesized via a sol-gel method and the nanopowders are annealed at the temperature of 450℃,550℃and 650℃for 2 hours.The crystal structure of the obtained samples is characterized by XRD.The effects of heat treatment temperature and Co doping content on the crystallite size and phase transition from anatase to rutile are investigated.The results show that both pure Ti O_2and Co-Ti O_2are pure anatase at the temperature of 450℃.Pure Ti O_2forms a little rutile and Co-Ti O_2is still anatase at 550℃.Most of the pure Ti O_2forms rutile at 650℃.The phase transition from anatase to rutile is promoted when Co doping content is at a low level and is inhibited when Co doping concentration is 8%.The enhancement of heat treatment temperature and higher Co doping content are beneficial for the formation of Co Ti O_3.The grain size of Ti O_2decreases after Co doping at the same temperature.
引文
[1]Motegh M,Van Ommen J R,Appel P W,et al.Scale-up study of a multiphase photocatalytic reactor-degradation of cyanide in water over Ti O2[J].Environ Sci Technol,2014,48(3):1574-1581.
[2]朱晓东,朱然苒,徐洪燕,等.二氧化钛的表征及其光降解研究[J].成都大学学报(自然科学版),2017,36(2):201-203.
[3]Li H,Hao Y B,Lu H Q,et al.A systematic study on visiblelight N-doped Ti O2photocatalyst obtained from ethylenediamine by sol-gel method[J].Appl Surf Sci,2015,344(1):112-118.
[4]Wojcieszak D,Mazur M,Kaczmarek D,et al.Influence of Nd dopant amount on microstructure and photoluminescence of Ti O2:Nd thin films[J].Opt Mater,2015,48(2):172-178.
[5]刘昭麟,崔作林,张志火昆.Cr3+掺杂纳米Ti O2结构相变及光谱特征[J].功能材料,2005,36(9):1404-1408.
[6]朱晓东,李浩宇,易倩,等.Zn掺杂Ti O2的制备与形貌研究[J].成都大学学报(自然科学版),2016,35(3):275-277.
[7]朱燕峰,杜荣归,李静,等.水热法制备Ti O2纳米线薄膜的光生阴极保护性能[J].物理化学学报,2010,26(9):2349-2353.
[8]李洪义,冉津,王金淑,等.液相沉积法制备Ti O2薄膜及其对304不锈钢的光生阴极防护[J].北京工业大学学报,2009,35(9):102-106.
[9]Dubey R S.Temperature-dependent phase transformation of Ti O2nanoparticles synthesized by sol-gel method[J].Mater lett,2018,215:312-317.
[10]Uvarov V,Popov I.Metrological characterization of X-ray diffraction methods for determination of crystallite size in nano-scale materials[J].Mater Charact,2007,58(10):883-891.
[11]Spurr R A,Myers H.Quantitative analysis of anatase-rutile mixtures with an X-ray diffractometer[J].Anal Chem,1957,29(5):760-762.
[12]顾建军,刘鹏飞,韩金荣,等.Fe掺杂量和退火氛围对Ti O2薄膜晶体结构和磁性能的影响[J].材料工程,2014,59(10):101-105.
[2]朱晓东,朱然苒,徐洪燕,等.二氧化钛的表征及其光降解研究[J].成都大学学报(自然科学版),2017,36(2):201-203.
[3]Li H,Hao Y B,Lu H Q,et al.A systematic study on visiblelight N-doped Ti O2photocatalyst obtained from ethylenediamine by sol-gel method[J].Appl Surf Sci,2015,344(1):112-118.
[4]Wojcieszak D,Mazur M,Kaczmarek D,et al.Influence of Nd dopant amount on microstructure and photoluminescence of Ti O2:Nd thin films[J].Opt Mater,2015,48(2):172-178.
[5]刘昭麟,崔作林,张志火昆.Cr3+掺杂纳米Ti O2结构相变及光谱特征[J].功能材料,2005,36(9):1404-1408.
[6]朱晓东,李浩宇,易倩,等.Zn掺杂Ti O2的制备与形貌研究[J].成都大学学报(自然科学版),2016,35(3):275-277.
[7]朱燕峰,杜荣归,李静,等.水热法制备Ti O2纳米线薄膜的光生阴极保护性能[J].物理化学学报,2010,26(9):2349-2353.
[8]李洪义,冉津,王金淑,等.液相沉积法制备Ti O2薄膜及其对304不锈钢的光生阴极防护[J].北京工业大学学报,2009,35(9):102-106.
[9]Dubey R S.Temperature-dependent phase transformation of Ti O2nanoparticles synthesized by sol-gel method[J].Mater lett,2018,215:312-317.
[10]Uvarov V,Popov I.Metrological characterization of X-ray diffraction methods for determination of crystallite size in nano-scale materials[J].Mater Charact,2007,58(10):883-891.
[11]Spurr R A,Myers H.Quantitative analysis of anatase-rutile mixtures with an X-ray diffractometer[J].Anal Chem,1957,29(5):760-762.
[12]顾建军,刘鹏飞,韩金荣,等.Fe掺杂量和退火氛围对Ti O2薄膜晶体结构和磁性能的影响[J].材料工程,2014,59(10):101-105.