Zn<sup>2+</sup>和TiO<sub>2</sub>合金化过程中不同成分占比对薄膜结构和光催化性能的影响

肖文悦; 董小硕; 买买提热夏提·买买提; 牛娜娜; 李国栋; 朱泽涛; 毕杰昊

doi:10.7498/aps.73.20240814

摘要

使用溶胶-凝胶法在单晶硅衬底上制备一批不同Zn²⁺成分调节的TiO₂薄膜, 观测Zn²⁺和TiO₂合金化过程中光学和光催化性能的变化. X射线衍射光谱仪用于观测在合金化过程中薄膜的晶体结构变化并追踪ZnTiO₃化合物的形成. 扫描电子显微镜、原子力显微镜用于观测合金化过程中因TiO₂晶格对Zn²⁺溶解度有限而导致薄膜表面出现大量孔洞的现象. X射线光电子能谱和光学带隙用于观测Zn²⁺与TiO₂合金化过程中电子结构层面的变化. 最后, 通过降解亚甲基蓝(MB)溶液, 表明少量Zn²⁺掺杂完全溶解在TiO₂中, 并破坏TiO₂结晶质量. 在Zn²⁺的成分占比继续提高至15%的过程中, XPS峰形拟合结果验证了TiO₂对Zn²⁺的溶解度有限, 导致薄膜出现大量孔洞结构, 薄膜的活性比表面积得以提升, 同时Zn²⁺可以有效地捕获光生e^–/h⁺. 为了继续观察Zn²⁺浓度对TiO₂的影响, 将Zn²⁺的浓度提升至40%, 观察Zn²⁺与TiO₂合金化过程中的现象. 表明化合物ZnTiO₃的出现可以充当e^–/h⁺的复合中心以及TiO₂占比的大幅下降导致合金化之后的薄膜光催化效率逐渐下降.

关键词:

TiO₂ /
Zn²⁺ /
光催化 /
带隙 /
表面

Abstract

A batch of TiO₂ films with different Zn²⁺ compositions are prepared on a single crystal silicon substrate by using sol-gel method to observe the changes in optical and photocatalytic properties in the alloying process of Zn²⁺ and TiO₂. X-ray diffractometer (XRD) is used to observe the changes in the crystal structures of the films in the alloying process and to track the formation of ZnTiO₃ compounds. Scanning electron microscope (SEM) and atomic force microscope (AFM) are used to observe the phenomena of a large number of holes on the surfaces of the films due to the limited solubility of the crystal lattice for Zn²⁺ in the alloying process. X-ray photoelectron spectroscopy (XPS) and optical bandgap are used to observe the changes at a level of the electronic structure of the films in the alloying process of Zn²⁺ with TiO₂. Finally, by degrading the methylene blue solution, it is shown that a small amount of Zn²⁺ doping is completely dissolved in TiO₂, destroying the TiO₂ crystalline quality. As the compositional share of Zn²⁺ continues to increase to 15%, the limited solubility of TiO₂ for Zn²⁺ is verified in the XPS peak fitting, resulting in a large number of hole structures in the film, and the active specific surface area of the film is enhanced, while Zn²⁺ effectively traps the photogenerated e^–/h⁺. In order to continue to observe the effect of Zn²⁺ concentration on TiO₂, we increase the concentration of Zn²⁺ to 40% and observe the phenomenon in the alloying process of Zn²⁺ with TiO₂. It is shown that the appearance of the compound ZnTiO₃ can act as a complex center for e^–/h⁺ and a significant decrease in the percentage of TiO₂ leads to a gradual decrease in the photocatalytic efficiency of the films after alloying.

Keywords:

TiO₂ /
Zn²⁺ /
photocatalysis /
bandgap /
surface

作者及机构信息

1.
新疆大学物理科学与技术学院, 乌鲁木齐　830017

2.
新疆大学材料科学与工程学院, 乌鲁木齐　830017

通信作者: 买买提热夏提·买买提, rxtmmt@xju.edu.cn

基金项目: 新疆大学校级大学生创新训练计划(批准号: XJU-SRT-23114)资助的课题.

Authors and contacts

1.
School of Physics and Technology, Xinjiang University, Urumqi 830017, China

2.
School of Materials Science and Engineering, Xinjiang University, Urumqi 830017, China

Corresponding author: Mamatrishat Mamat, rxtmmt@xju.edu.cn

Funds: Project supported by the Students Innovative-Research Training Program of Xinjiang University, China (Grant No. XJU-SRT-23114).

文章全文 : translate this paragraph

参考文献

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[20]	Yoon Y H, Lee S Y, Gwon J, Cho H J, Wu Q, Kim Y H, Lee W H 2018 Ceram. Int. 44 16647 Google Scholar
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施引文献

图 1 不同Zn²⁺成分占比的薄膜的 XRD 图样

Fig. 1. XRD patterns of thin films with different Zn²⁺ compositions.

下载: 全尺寸图片幻灯片

图 2 不同Zn²⁺成分占比的薄膜的SEM图样

Fig. 2. SEM patterns of thin films with different Zn²⁺ compositions.

下载: 全尺寸图片幻灯片

图 3 (a)纯TiO₂以及(b)—(d) 3%, 15%和40% Zn²⁺成分占比的薄膜的二维和三维AFM图像

Fig. 3. 2D and 3D AFM images of thin films with (a) pure TiO₂ and (b)–(d) 3%, 15% and 40% Zn²⁺ composition.

下载: 全尺寸图片幻灯片

图 4 纯TiO₂以及3%, 15% 和 40%Zn²⁺成分占比的薄膜的XPS光谱

Fig. 4. XPS spectra of pure TiO₂ and thin films with 3%, 15% and 40% Zn²⁺ compositions.

下载: 全尺寸图片幻灯片

图 5 不同Zn²⁺成分占比的薄膜的(a)吸收光谱和(b) 光带隙能

Fig. 5. (a) Absorption spectra and (b) optical band gap energy of films with different Zn²⁺ composition.

下载: 全尺寸图片幻灯片

图 6 (a) 不同Zn²⁺成分占比的薄膜的吸收阈值波长和光带隙能; (b) 纯TiO₂和Zn²⁺成分占比为3%, 15% 和 40%的薄膜的价带

Fig. 6. (a) Absorption threshold wavelengths and optical band gap energies of films with different Zn²⁺ compositions; (b) valence bands of pure TiO₂ and films with 3%, 15% and 40% Zn²⁺ compositions.

下载: 全尺寸图片幻灯片

图 7 不同Zn²⁺成分占比的薄膜的能带位置示意图

Fig. 7. Schematic representation of the energy band positions of films with different Zn²⁺ compositions.

下载: 全尺寸图片幻灯片

图 8 降解亚甲基蓝的光催化活性　(a) 随时间变化的降解量; (b) 相应的降解反应速率常数图

Fig. 8. Photocatalytic activity for degradation of methylene blue: (a) Degradation amount with time; (b) corresponding degradation rate constant plots.

下载: 全尺寸图片幻灯片

图 9 光催化反应速率(η)与光催化反应常数(K_app)的关系图

Fig. 9. Plot of photocatalytic reaction rate (η) versus photocatalytic reaction constant (K_app).

下载: 全尺寸图片幻灯片

表 1 从 XRD 图谱获得的结构参数

Table 1. Structural parameters obtained from XRD spectra.

Samples	(h k l )	FWHM β/(°)	D/nm
TiO₂	(1 0 1)	0.177	8.384
3% Zn-TiO₂	(1 0 1)	0.161	9.217
5% Zn-TiO₂	(1 0 1)	0.197	7.533
10% Zn-TiO₂	(1 0 1)	0.180	8.244
15% Zn-TiO₂	(1 0 1)	0.259	5.730
20% Zn-TiO₂	(1 0 1)	0.152	9.762
40% Zn-TiO₂	(1 0 1)	0.227	6.537

下载: 导出CSV

表 2 从AFM获得的粗糙度参数(R_a为算数平均粗糙度, R_MS为均方根粗糙度, R_Sk为粗糙度斜率, R_Ku为粗糙度峰度)

Table 2. Roughness parameters obtained from AFM (R_a, R_MS, R_Sk, R_Ku are the average, root- mean-square, Skewness, and Kurtosis values of surface roughness, respectively).

Samples	Roughness R_a/nm	Roughness R_MS/nm	Skewness R_Sk	Kurtosis R_Ku
TiO₂	3.515	4.359	–0.492	0.276
3%Zn-TiO₂	2.230	2.851	–0.077	0.089
15%Zn-TiO₂	5.590	6.990	–0.313	0.819
40%Zn-TiO₂	6.115	8.703	–1.079	3.318

下载: 导出CSV

map

[1]	Lukong V T, Ukoba K, Jen T C 2022 Int. J. Adv. Manuf. Technol. 122 3525 Google Scholar
[2]	李冬冬, 王丽莉 2012 61 034212 Google Scholar Li D D, Wang L L 2012 Acta Phys. Sin. 61 034212 Google Scholar
[3]	Chinnarani M, Suresh S, Prabu K M, Kandasamy M, Pugazhenthiran N 2024 Inorg. Chim. Acta 560 121842 Google Scholar
[4]	Sanattalab E, Gürdağ G, Sığırcı B D 2023 Biomater. Adv. 148 213365 Google Scholar
[5]	Ziental D, Goslinska B C, Mlynarczyk D T, Sobotta A G, Stanisz B, Goslinski T L 2020 Nanomaterials 10 387 Google Scholar
[6]	Zhu Z W, Chen S F, Zhang Y, Wang W 2022 Prog. Org. Coat. 173 107226 Google Scholar
[7]	Alrowaili Z A, Alsohaimi I H, Betiha M A, Essawy A A, Mousa A A, Alruwaili S F, Hassan H M A 2020 Mater. Chem. Phys. 241 122403 Google Scholar
[8]	Ike P O, Ezugwu S, Chikwenze R, Nwanya A C, Ezugwu A E, Madiba I G, Ezekoye B A, Ahmed M S, Maaza M, Ezema F I 2019 Optik 191 1 Google Scholar
[9]	Aruna S T, Vismaya A, Balaji N 2021 Mater. Manuf. Processes 36 868 Google Scholar
[10]	Mittireddi R T, Makani N H, Prajapati D, Raj A, Banerjee R, Panda E 2023 Mater. Charact. 199 112818 Google Scholar
[11]	Sun N R, Wang J W, Yao J Z, Chen H M, Deng C H 2019 Microchim. Acta 186 159 Google Scholar
[12]	Zhang Q, Li C Y 2020 Nanomaterials 10 911 Google Scholar
[13]	Kusior A, Banas J, Zajac A T, Zubrzycka P, Ilnicka A M, Radecka M 2018 J. Mol. Struct. 1157 327 Google Scholar
[14]	Al-Tayeb M A-A, Khan M Y, Drmosh Q A, Hossain M K, Asim M, Dafalla H, Khan A 2023 Inorg. Chim. Acta 556 121611 Google Scholar
[15]	Ma Q, Qiu T, Liu S J, Weng L Q, Dong W Y 2010 Appl. Phys. A 104 365 Google Scholar
[16]	Liu Y, Peng Q, Zhou Z P, Yang G 2018 Chin. Phys. Lett. 35 048101 Google Scholar
[17]	Resende P D, Maria R, Silva J D, Azevedo I, Santos L A, Tadeu V 2020 J. Mater. Res. Technol. 9 10121 Google Scholar
[18]	Chen C C, Hu S H, Fu Y P 2015 J. Alloys Compd. 632 326 Google Scholar
[19]	Ahadi S, Moalej N S, Sheibani S 2019 Solid State Sci. 96 105975 Google Scholar
[20]	Yoon Y H, Lee S Y, Gwon J, Cho H J, Wu Q, Kim Y H, Lee W H 2018 Ceram. Int. 44 16647 Google Scholar
[21]	Qu X, Lin J B, Wei Q, Chen C T, Sun D P 2022 Chemosphere 308 136239 Google Scholar
[22]	Jaimy K B, Safeena V P, Ghosh S, Hebalkar N, Warrier K 2012 Dalton Trans. 41 4824 Google Scholar
[23]	Chen K T, Hsu C H, Jiang S C, Liang L S, Gao P, Qiu Y, Wu W Y, Zhang S, Zhu W Z, Lien S Y 2022 IEEE Trans. Electron Devices 69 1149 Google Scholar
[24]	Nair P K, Mizukami F, Nair J, Salou M, Oosawa Y, Izutsu H, Maeda K, Okubo T 1998 Mater. Res. Bull. 33 1495 Google Scholar
[25]	Chen P C, Chen C C, Chen S H 2017 Curr. Nanosci. 13 373 Google Scholar
[26]	Ren T Z, Yuan Z Y, Su B L 2004 Colloids Surf., A 241 67 Google Scholar
[27]	Lang J, Takahashi K, Kubo M, Shimada M 2022 Catalysts 12 365 Google Scholar
[28]	Mercado C C, Seeley Z M, Bandyopadhyay A, Bose S, McHale J L 2011 ACS Appl. Mater. Interfaces 3 2281 Google Scholar
[29]	Henderson M 2002 Surf. Sci. Rep. 46 1 Google Scholar
[30]	Dikici T, Yılmaz O, Akalin A S, Demirci S, Gültekin S, Yıldırım S, Yurddaşkal M 2022 J. Aust. Ceram. Soc. 58 1415 Google Scholar
[31]	Xu W, Li X J, Zhang S J, Wang J G, Xu Z K 2005 Trans. Nonferrous Met. Soc. China 15 119 Google Scholar
[32]	Wang C T, Lin H S, Wang W P 2019 Mater. Sci. Semicond. Process. 99 85 Google Scholar
[33]	Liao C Z, Li Y C, Tjong S C 2020 Nanomaterials 10 124 Google Scholar
[34]	Ismael M 2020 Sol. Energy 211 522 Google Scholar
[35]	Matsumoto Y, Katayama M, Abe T, Ohsawa T, Ohkubo I, Kumigashira H, Oshima M, Koinuma H 2010 J. Ceram. Soc. Jpn. 118 993 Google Scholar
[36]	Ribao P, Rivero M J, Ortiz I 2017 Environ. Sci. Pollut. Res. 24 12628 Google Scholar
[37]	Tang T, Wang T, Gao Y, Xiao H, Xu J H 2019 J. Mater. Sci. -Mater. Electron. 30 8471 Google Scholar
[38]	Xavier A M, Jacob I D, Surender S, Saravana kumaar M S S, Elangovan P 2022 Inorg. Chem. Commun. 146 110168 Google Scholar
[39]	Pecherskaya M D, Butanov K T, Ruzimuradov O N, Mamatkulov S I, Parpiev O 2022 Glass Phys. Chem. 48 327 Google Scholar
[40]	Heiba Z K, Mohamed M B, Badawi A, Abdellatief M 2022 J. Mater. Sci. -Mater. Electron. 33 10399 Google Scholar
[41]	Castellón E, Zayat M, Lévy D 2017 Adv. Funct. Mater. 28 04717 Google Scholar
[42]	Chu J Y, Sun Y C, Han X J, Zhang B, Du Y C, Song B, Xu P 2019 ACS Appl. Mater. Interfaces 11 18475 Google Scholar
[43]	Maleki K, Abdizadeh H, Golobostanfard M R, Adelfar R 2017 Appl. Surf. Sci. 394 37 Google Scholar

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Zn²⁺和TiO₂合金化过程中不同成分占比对薄膜结构和光催化性能的影响