微波水熱法快速合成氧化鋅納米棒及其光催化性能

李蕊; 夏仡; 許磊; 劉建華; 剛瑞奇; 羅銅

doi:10.13374/j.issn2095-9389.2019.05.25.003

微波水熱法快速合成氧化鋅納米棒及其光催化性能

doi: 10.13374/j.issn2095-9389.2019.05.25.003

李蕊¹,
夏仡²,
許磊^{1, 3, ,},
劉建華³,
剛瑞奇^{1, 3},
羅銅^{1, 3}

1.
昆明理工大學冶金與能源工程學院，昆明 650093
2.
昆明理工大學分析測試中心，昆明 650093
3.
云南省部共建復雜有色金屬資源清潔利用國家重點實驗室，昆明 650093

基金項目: 國家自然科學基金資助項目（51864030）；云南省科技人才計劃資助項目(2019HB003)；云南省萬人計劃青年拔尖人才；云南省重大科技專項項目（2018ZE027）；昆明理工大學自然科學基金項目（KKSY201732033）

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通訊作者:
E-mail: xulei_kmust@aliyun.com

中圖分類號: O643.36；TN304.2
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出版歷程
- 收稿日期: 2019-05-25
- 刊出日期: 2020-01-01

Study of rapidly synthesis of ZnO nanorods by microwave hydrothermal method and photocatalytic performance

LI Rui¹,
XIA Yi²,
XU Lei^{1, 3
, ,},
LIU Jian-hua³,
GANG Rui-qi^{1, 3},
LUO Tong^{1, 3}

1.
Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming 650093, China
2.
Analysis and Testing Center, Kunming University of Science and Technology, Kunming 650093, China
3.
State Key Laboratory for Clean and Utilization of Complex Nonferrous Metal Resources in Yunnan Province, Kunming 650093, China

More Information

Corresponding author: E-mail: xulei_kmust@aliyun.com

摘要

摘要: 以硫酸鋅、醋酸鋅和氫氧化鋅為原料，制備出氫氧化鋅前驅體和氧化鋅晶種，在微波水熱條件下快速合成了氧化鋅納米棒。通過X射線衍射（XRD）、掃描電鏡（SEM）、透射電鏡（TEM）和紫外?可見分光光度計（UV-vis）對氧化鋅納米棒的形貌、結構和光學性質等進行了表征，并通過降解羅丹明B（RhB）測試了樣品的光催化性能，探討了微波輻射作用對產物的催化活性的影響。實驗結果表明，氫氧化鋅作為前驅體在微波作用下30 min，生成為基于氧化鋅納米棒自組裝的三維籠狀結構，與常規方法制備的氧化鋅納米棒相比，微波輻射作用下生成的樣品結晶度更高。紫外?可見分光光度計結果表明微波輻射會導致合成的氧化鋅納米棒吸收邊紅移，縮小帶隙能量，從而提升氧化鋅納米棒的催化活性。光催化測試表明微波輔助合成的氧化鋅納米棒具有更好的可見光吸收特性，在紫外和可見光照射下，對羅丹明B都具有較好的降解效率，在紫外光照射下80 min內羅丹明B的降解率可達到98.5%。這種微波輔助的合成方法能夠在短時間內合成大量的氧化鋅納米材料，具有高效批量制備、清潔環保等優點。
- 氧化鋅納米棒 /
- 微波 /
- 水熱 /
- 光催化 /
- 羅丹明B
Abstract: Nano-zinc oxide materials have been widely studied and applied due to their excellent photocatalytic properties. In this study, ZnO nanorods were rapidly synthesized via a microwave-assisted hydrothermal method, using Zn(OH)₂ precursor and ZnO seeds that were prepared by zinc sulfate, zinc acetate, and zinc hydroxide as raw materials. The morphology, nanostructure, and optical properties of ZnO nanorods were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-vis spectroscopy. To investigate the effect of microwave irradiation on the photocatalytic activity of the ZnO nanorods, the photocatalytic properties of the samples were tested by degrading rhodamine B (RhB) under ultraviolet and visible light for about 80 min. The experimental results indicate that Zn(OH)₂ precursor and ZnO seeds can be successfully converted into a three-dimensional cage structure based on the self-assembly of ZnO nanorods in 30 min with microwave irradiation reaction. Compared with the conventional method of synthesizing ZnO nanorods, the samples under microwave irradiation featured a better crystallinity performance. The UV-vis results show that microwave radiation can cause a red shift of the absorption edge of synthesized ZnO nanorods and reduce the band gap energy, thereby enhancing the photocatalytic activity and efficiency of the ZnO nanorods. The photocatalytic test results indicate that ZnO nanorods synthesized by the microwave-assisted hydrothermal method have a better efficiency of light absorption; the samples have a better degradation rate of rhodamine B under the ultraviolet and visible light irradiation. The degradation efficiency of rhodamine B by ZnO nanorods could reach 98.5% within 80 min under ultraviolet light irradiation. The microwave-assisted synthesis method can allow to synthesize a large amount of ZnO nanorods materials in a short time, and it has the advantages of high-efficiency batch preparation and environmental friendliness.
- ZnO nanorods /
- microwave /
- hydrothermal /
- photocatalysis /
- rhodamine B

HTML全文

圖 1 氧化鋅納米棒制備流程示意圖

Figure 1. Schematic of preparation of ZnO nanorods

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圖 2 氧化鋅納米棒的XRD圖譜

Figure 2. XRD patterns of the ZnO nanorods

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圖 3 氧化鋅納米棒的微觀結構。（a，c，e，f）微波水熱法；（b，d）常規水熱法

Figure 3. Microstructure of the ZnO nanorods: (a, c, e, f) microwave hydrothermal; (b, d) traditional hydrothermal

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圖 4 氧化鋅納米棒的紫外?可見吸收光譜圖（a）和氧化鋅的Tauc圖（b）

Figure 4. Ultraviolet-visible absorption spectra of ZnO nanorods (a) and the Tauc’s plot of ZnO nanorods (b)

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圖 5 氧化鋅納米棒的光催化性能。（a）紫外光下的光催化曲線；（b）紫外光下的降解速率；（c）可見光下的光催化曲線；（d）可見光下的降解速率

Figure 5. Photocatalytic property of ZnO nanorods: (a) photocatalytic curves under ultraviolet light; (b) degradation rate under ultraviolet light; (c) photocatalytic curves under visible light; (d) degradation rate under visible light

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參考文獻(27)

[1]	Fujishima A, Honda K. Electrochemical photolysis of water at a semiconductor electrode. Nature, 1972, 238(5358): 37 doi: 10.1038/238037a0
[2]	Zhang J L, Wu Y M, Xing M Y, et al. Development of modified N doped TiO₂ photocatalyst with metals, nonmetals and metal oxides. Energy Environ Sci, 2010, 3(6): 715 doi: 10.1039/b927575d
[3]	Chen S F, Zhao W, Liu W, et al. Preparation characterization and activity evaluation of p-n junction photocatalyst p-NiO/n-ZnO. J Sol-Gel Sci Technol, 2009, 50(3): 387 doi: 10.1007/s10971-009-1908-3
[4]	Zhang M L, An T C, Hu X H, et al. Preparation and photocatalytic properties of a nanometer ZnO?SnO₂ coupled oxide. Appl Catal A, 2004, 260(2): 215 doi: 10.1016/j.apcata.2003.10.025
[5]	Vinodgopal K, Kmat P V. Enhanced rates of photocatalytic degradation of an azo dye using SnO₂/TiO₂ coupled semiconductor thin films. Environ Sci Technol, 1995, 29(3): 841 doi: 10.1021/es00003a037
[6]	Othman A A, Ali M A, Ibrahim E M M, et al. Influence of Cu doping on structural, morphological, photoluminescence, and electrical properties of ZnO nanostructures synthesized by ice-bath assisted sonochemical method. J Alloys Compd, 2016, 683: 399 doi: 10.1016/j.jallcom.2016.05.131
[7]	Sun Q Q, Wang S M, Wang Z M. Preparation and doping modification of ZnO nanorods by microwave heating. J Mater Sci Eng, 2013, 31(5): 732 doi: 10.3969/j.issn.1673-2812.2013.05.023 孫強強, 王書民, 王正民. 微波法制備納米棒狀氧化鋅及其摻雜改性. 材料科學與工程學報, 2013, 31(5):732 doi: 10.3969/j.issn.1673-2812.2013.05.023
[8]	Thankachan R M, Joy N, Abraham J, et al. Enhanced photocatalytic performance of ZnO nanostructures produced via a quick microwave assisted route for the degradation of rhodamine in aqueous solution. Mater Res Bull, 2017, 85: 131 doi: 10.1016/j.materresbull.2016.09.009
[9]	Mo M, Yu J C, Zhang L, et al. Self-assembly of ZnO nanorods and nanosheets into hollow microhemispheres and microspheres. Adv Mater, 2005, 17(6): 756 doi: 10.1002/adma.200401477
[10]	Qi K Z, Cheng B, Yu J G, et al. Review on the improvement of the photocatalytic and antibacterial activities of ZnO. J Alloys Compd, 2017, 727: 792 doi: 10.1016/j.jallcom.2017.08.142
[11]	Ba-Abbad M M, Kadhum A A H, Mohamad A B, et al. The effect of process parameters on the size of ZnO nanoparticles synthesized via the sol-gel technique. J Alloys Compd, 2013, 550: 63 doi: 10.1016/j.jallcom.2012.09.076
[12]	Hirate T, Kimpara T, Nakamura S, et al. Control of diameter of ZnO nanorods grown by chemical vapor deposition with laser ablation of ZnO. Superlattices Microstruct, 2007, 42(1-6): 409 doi: 10.1016/j.spmi.2007.04.011
[13]	Labuayai S, Promarak V, Maensiri S. Synthesis and optical properties of nanocrystalline ZnO powders prepared by a direct thermal decomposition route. Appl Phys A, 2009, 94(4): 755 doi: 10.1007/s00339-008-4984-2
[14]	Zhang B P, Binh N T, Wakatsuki K, et al. Pressure-dependent ZnO nanocrsytal growth in a chemical vapor deposition process. J Phys Chem B, 2004, 108(30): 10899 doi: 10.1021/jp048602i
[15]	Chen N L, Yang S R, Ren Y P, et al. Preparation of rod like oxide of zinc and its photocatalytic performance. J Lanzhou Univ Technol, 2017, 43(2): 76 doi: 10.3969/j.issn.1673-5196.2017.02.015 陳娜麗, 楊樹榮, 任亞鵬, 等. 棒狀氧化鋅的制備及其光催化性能. 蘭州理工大學學報, 2017, 43(2):76 doi: 10.3969/j.issn.1673-5196.2017.02.015
[16]	Polsongkram D, Chamninok P, Pukird S, et al. Effect of synthesis conditions on the growth of ZnO nanorods via hydrothermal method. Physica B, 2008, 403(19-20): 3713 doi: 10.1016/j.physb.2008.06.020
[17]	Chen G, Li L, Tao C Y, et al. Effects of microwave heating on microstructures and structure properties of the manganese ore. J Alloys Compd, 2016, 657: 515 doi: 10.1016/j.jallcom.2015.10.147
[18]	Anas S, Rahul S, Babitha K B, et al. Microwave accelerated synthesis of zinc oxide nanoplates and their enhanced photocatalytic activity under UV and solar illuminations. Appl Surf Sci, 2015, 355: 98 doi: 10.1016/j.apsusc.2015.07.058
[19]	Lavand A B, Malghe Y S. Synthesis, characterization and visible light photocatalytic activity of nitrogen-doped zinc oxide nanospheres. J Asian Ceram Soc, 2015, 3(3): 305 doi: 10.1016/j.jascer.2015.06.002
[20]	Jing X Y, Kuang W W, Liu J Y. One-step preparation of zinc oxide micron-powders by microwave hydrolysis. J Funct Mater, 2008, 39(7): 1186 doi: 10.3321/j.issn:1001-9731.2008.07.038 景曉燕, 匡巍巍, 劉婧媛. 微波水熱法一步合成微米氧化鋅粒子. 功能材料, 2008, 39(7):1186 doi: 10.3321/j.issn:1001-9731.2008.07.038
[21]	Shaporev A S, Ivanov V K, Baranchikov A E, et al. Microwave-assisted hydrothermal synthesis and photocatalytic activity of ZnO. Inorg Mater, 2007, 43(1): 35 doi: 10.1134/S0020168507010098
[22]	Music S, Saric A, Popovic S. Formation of nanosize ZnO particles by thermal decomposition of zinc acetylacetonate monohydrate. Ceram Int, 2010, 36(3): 1117 doi: 10.1016/j.ceramint.2009.12.008
[23]	Mendoza-Mendoza E, Nunez-Briones A G, Garcia-Cerda L A, et al. One-step synthesis of ZnO and Ag/ZnO heterostructures and their photocatalytic activity. Ceram Int, 2018, 44(6): 6176 doi: 10.1016/j.ceramint.2018.01.001
[24]	Huang J F, Xia C K, Cao L Y, et al. Facile microwave hydrothermal synthesis of zinc oxide one-dimensional nanostructure with three-dimensional morphology. Mater Sci Eng B, 2008, 150(3): 187 doi: 10.1016/j.mseb.2008.05.014
[25]	Cao G X, Hong K Q, Wang W D, et al. Fast growth of well-aligned ZnO nanowire arrays by a microwave heating method and their photocatalytic properties. Nanotechnology, 2016, 27(43): 435402 doi: 10.1088/0957-4484/27/43/435402
[26]	Xu A J, Feng S S, Shen S J, et al. Enhanced visible light-responsive photocatalytic properties of Ag/BiPbO₂Cl nanosheet composites. Nanoscale Res Lett, 2018, 13: 292 doi: 10.1186/s11671-018-2706-z
[27]	Baruah S, Dutta J. Hydrothermal growth of ZnO nanostructures. Sci Technol Adv Mater, 2009, 10(1): 013001 doi: 10.1088/1468-6996/10/1/013001