Page 118 - 《精细化工》2020年第4期

第 37 卷第 4 期 精 细 化 工 Vol.37, No.4
202 0 年 4 月 FINE CHEMICALS Apr. 2020

催化与分离提纯技术
氮气低温等离子体辅助制备 N-TiO 及其光催化活性
2

赵文霞 1,2 ，王 蕊 1,2 ，张 硕 1,2 ，肖滨滨 1,2 ，赵 玉 1,2 ，刘 帅 1,2

（1. 河北科技大学 环境科学与工程学院，河北 石家庄 050018；2. 河北省污染防治生物技术重点实验
室，河北 石家庄 050018）

摘要：以钛酸丁酯为钛源、尿素为氮源，采用溶胶-凝胶法制得 N-TiO 2 中间体。分别经过“N 2 氛围煅烧”、“N 2
等离子体处理+N 2 氛围煅烧”和“N 2 氛围煅烧+N 2 等离子体处理”3 种处理方式制得 N-TiO 2 光催化剂，分别记作
N-TiO 2 (C)、N-TiO 2 (LTP+C)和 N-TiO 2 (C+LTP)。借助 XRD、TEM、EDS、UV-Vis DRS 和 XPS 表征手段，以甲
基橙（MO）溶液为目标污染物，考察了 N-TiO 2 的可见光催化性能。结果表明，经过 N 2 等离子体处理的 N-TiO 2
比单纯煅烧的 N-TiO 2 晶粒尺寸更小，对可见光的响应性更强，且 N 的掺入量更高。可见光照射 240 min 内，3
种 N-TiO 2 对 MO 的光降解性能由高到低依次为 N-TiO 2 (LTP+C)> N-TiO 2 (C+LTP)> N-TiO 2 (C)，其中 MO 的最大
降解率为 90%。3 种 N-TiO 2 对 MO 的光降解性能均符合假一级动力学方程，且 N-TiO 2 (LTP+C)和 N-TiO 2 (C+LTP)
的表观速率常数分别是 N-TiO 2 (C)的 4.5 倍和 1.9 倍。研究得出，在 N-TiO 2 的制备过程中引入 N 2 等离子体处理
工序，有利于改善 N 元素的表面分散性，增加 N 元素的掺入量，能提升 N-TiO 2 可见光催化活性，且“N 2 等离子
体处理+N 2 氛围煅烧”处理方式最佳。
关键词：TiO 2 ；氮掺杂；N 2 等离子体；制备；可见光；光催化活性
中图分类号：X505 文献标识码：A 文章编号：1003-5214 (2020) 04-0752-07

Preparation of N-TiO 2 assisted by low-temperature N 2

plasma and its photocatalytic activity

1,2
1,2
1,2
1,2
1,2
1,2
ZHAO Wenxia , WANG Rui , ZHANG Shuo , XIAO Binbin , ZHAO Yu , LIU Shuai
（1. Environmental Science and Engineering, Hebei University of Science and Technology, Shijiazhuang 050018, Hebei,
China; 2. Key Laboratory of Pollution Prevention and Control Biotechnology of Hebei Province, Hebei University of
Science and Technology, Shijiazhuang 050018, Hebei, China）
Abstract: N-doped TiO 2 (N-TiO 2) intermediate was prepared by sol-gel method using tetrabutyl titanate
and urea as titanium source and nitrogen source, respectively. The N-TiO 2 intermediate was treated by three
process, N 2 atmospheric calcinations, N 2 plasma treatment + N 2 atmospheric calcination and N 2
atmospheric calcination + N 2 plasma treatment, which were noted as N-TiO 2(C), N-TiO 2(LTP+C) and
N-TiO 2(C+LTP), respectively. The samples were characterized by XRD, TEM, EDS, UV-vis DRS and XPS
techniques. The corresponding photocatalytic properties in degradation of methyl orange (MO) were
investigated under visible-light irradiation. The results show that compared with N-TiO 2 (C), N-TiO 2 (LTP+C)
and N-TiO 2(C+LTP) have smaller particle size, and exhibit more responsive to visible- light, and possess
higher N content. Within 240 min of visible-light irradiation, the photodegradation performance of N-TiO 2
to MO was decreased in the sequence of N-TiO 2(LTP+C)>N-TiO 2(C+LTP)> N-TiO 2(C), and the maximum
degradation rate of MO was 90%. The photodegradation of MO on three kinds of N-TiO 2 accorded with the
pseudo first-order kinetic equation. The apparent rate constants of N-TiO 2(LTP+C) and N-TiO 2(C+LTP)
were 4.5 times and 1.9 times that of N-TiO 2, respectively. It is found that the introduction of N 2 plasma
treatment process in the preparation of N-TiO 2 is beneficial to improve the surface dispersibility of N
element, increase the amount of N element, and enhance the visible-light photocatalytic activity of N-TiO 2.

收稿日期：2019-09-26; 定用日期：2019-11-25; DOI: 10.13550/j.jxhg.20190910
基金项目：国家重点研发计划重点专项（2016YFC0207907）
作者简介：赵文霞（1973—），女，博士，教授，E-mail：kd2010zwx@163.com。