| 487 | 3 | 85 |
| 下载次数 | 被引频次 | 阅读次数 |
在催化领域，氧化锌纳米棒因其在径向上具有纳米粒子的小尺寸效应、纵向上具有体相材料的宏观特性，而受到越来越多的关注。采用改进的溶剂热法合成 ZnO 纳米棒，采用分步法加入 Zn2+与 Na OH。通过 X 射线衍射，扫描电子显微镜等方法对样品进行表征，探究了聚乙二醇(PEG)辅助 ZnO 纳米棒合成的作用机理以及 Na OH 的加入方式对 ZnO 纳米棒形貌控制规律的影响，研究了不同长/径的 ZnO 纳米棒的脱硫性能。结果表明：PEG 的分子量对 ZnO 纳米棒的形貌有着显著影响，PEG 分子量为 20 000 时，能够在温和的溶剂热条件下，控制合成出长度为 3～4 μm，直径为 250 nm 左右的 ZnO 纳米棒，分步法加入 NaOH 优于一步法加入 Na OH。将合成的 ZnO 纳米棒负载金属氧化镍制成脱硫剂，大长/径的棒状 ZnO 脱硫剂的脱硫率高达 98.2%，同时具有良好的再生性能。
Abstract：In the field of catalysis, ZnO nanorods have attracted much attention because of their small size effect in the radial direction and the macroscopic characteristics of bulk materials in the longitudinal direction. In this paper, ZnO nanorods were synthesized by an improved solvothermal method, and Zn2+ ions and NaOH were added by a step-by-step method. The samples were characterized by X-ray diffraction and scanning electron microscopy. The mechanism of PEG-assisted synthesis of ZnO nanorods and the effect of NaOH addition on the morphology of ZnO nanorods were investigated. The desulfurization performance of ZnO nanorods with different length to diameter ratios was analyzed. The results show that the molecular weight of PEG has a significant effect on the morphology of ZnO nanorods. ZnO nanorods with a length of 3-4 μm and a diameter of approximately 250 nm can be synthesized under mild solvothermal conditions when the molecular weight of PEG is 20000. Also, the step-by-step method of adding Na OH is better than the one-step method of adding NaOH. NiO is loaded on the synthesized ZnO nanorods as a desulfurizer. The desulfurization rate of ZnO nanorods desulfurizer with a large length to diameter ratio can achieve 98.2%, and the desulfurizer has a better regeneration performance.
[1]李苹,陈卫.一维纳米材料在能源电催化中的研究进展[J].催化学报, 2019(1):4-22.LI Ping, CHEN Wei. Chin J Catalys(in Chinese), 2019(1):4–22.
[2] YUE Z, YING Y, et al. Shape controlled synthesis and growth mechanism of one-dimensional zinc oxide nanomaterials[J]. Rarer Met,2004, 11(1):23–29.
[3]孙武,汤政涛,于少明.氨配合法控制合成片状纳米氧化锌[J].人工晶体学报, 2018, 47(6):1171–1176.SUN Wu, TANG Zhengtao, YU Shaoming. J Synth Cryst(in Chinese),2018, 47(6):1171–1176.
[4] Tl A, PSA B, Dn A, et al. Specific Al mole ratio doping aided flake-like ZnO surface morphology nanostructures film for efficient window layer in CuInS2 photovoltaic cells[J]. Sol Energy, 2019, 177:108–117.
[5] NARA V K, CUI Y. Nanostructures for photon management iin solar cells[J]. Nanophotonics, 2013, 2(3):187–210.
[6] ALEXANDER M, SUR S, RAGHU S, et al. Semiconducting material of pure ZnO hollow nanospheres; and their modified electrode used for electrocatalytic reduction of ethanol and hydrogen peroxide[J]. Mater Sci Semicond Process, 2019, 99:62–67.
[7]朱宪安,王泉,石永敬,等.水热法制备的ZnO纳米棒的微结构,光学性质以及光学模型[J].中国有色金属学报(英文版), 2020, 30(1):191–199.ZHU Xian'an, WANG Quan, SHI Yongjing, et al. Trans Nonferrous Metal Soc CH, 2020, 30(1):191–199.
[8] REN Z, GUO X Y, WROBEL G, et al. Three dimensional koosh ball nanoarchitecture with a tunable magnetic core, fluorescent nanowire shell and enhanced photocatalytic property[J]. J Mater Chem, 2012,22(14):6862–6868.
[9] BARRECA D, GASPAROTTO A, Maccato C, et al. Photoinduced superhydrophilicity and photocatalytic properties of ZnO nanoplatelets[J]. Surf Coat Technol, 2009, 203(14):2041–2045.
[10] REN Z, Botu V, WANG S, et al. Monolithically integrated spinel M(x)Co(3-x)O(4)(M=Co, Ni, Zn)nanoarray catalysts:Scalable synthesis and cation manipulation for tunable low-temperature CH(4)and CO oxidation[J]. Angew Chem, 2014, 53(28):7223–7227.
[11]彭德艳.纳米氧化物及其复合纳米结构的制备与应用研究[D].华东:华东师范大学, 2017.PENG Deyan. Synthesis preparation and applying research of nano-oxide and its composite nanostructure(in Chinese, dissertation).East China:East China Normal University, 2017.
[12] KENNEDY O W, WHITE E R, SHAFFER. Vapour-liquid-solid growth of ZnO-ZnMgO core-shell nanowires by gold-catalysed molecular beam epitaxy[J]. Nanotechnology, 2019, 30(19):1-5.
[13] ZHANG Y, YANG Y, HAN H, et al. Ultra-deep desulfurization via reactive adsorption on Ni/ZnO:The effect of ZnO particle size on the adsorption performance[J]. Appl Catal, B, 2012, 119–120:13–19.
[14] BEHL M, YEOM J, LINEBERRY Q, et al. A regenerable oxide-based H2S adsorbent with nanofibrous morphology[J]. Nat nanotechnol, 2012,7(12):810–815.
[15] GHARBI B, TAABOUCHE A, BRELLA M, et al. Spray pyrolysis synthesized and ZnO-NiO nanostructured thin films analysis with their nanocomposites for waveguiding applications[J]. Semiconductors,2021, 55(1):37–43.
[16] SENDA T, BRADTR C, CERVAH, et al. Grain growth in sintering ZnO and ZnO Bi2O3 ceramics[J]. J Am Ceram Soc, 1990, 73(1):106–114.
[17] Gunay V, Gelecek-Sulan O, Ozkan O T. Microstructure and crystal structure ofgrain growth kinetics in x CoO-6%Bi2O3-(94x)ZnO(x=0, 2,4)ceramic system[J]. Ceram Int, 2004, 30:105–110.
[18]王久亮.纳米氧化锌晶体生长宏观动力学研究[J].硅酸盐通报,2007, 26(2):268–272.WANG Jiuliang. Bull Chin Cera Soc(in Chinese). 2007, 26(2):268–272.
[19]周明飞,宋学萍,孙兆奇.基底温度对磁控溅射制备ZnO薄膜性能的影响[J].材料科学与工程学报, 2007, 25(4):598–601.ZHOU Mingfei, SONG Xueping, SUN Zhaoqi. J Mater Sci Eng(in Chinese), 2007, 25(4):598–601.
[20]孔凡志.纳米碳管和氧化物一维功能纳米材料的制备与表征[D].浙江:浙江大学, 2003.KONG Fanzhi. Preparation and characterzation of carbon nanotubes and one-dimensional oxide nanomaterials(in Chinese, dissertation).Zhejiang:Zhejiang University, 2003.
[21]谢娟,李平,魏雨,等.低温陈化法制备ZnO微晶及其形貌控制[J].功能材料, 2008, 39(12):2061–2064.XIE Juan, LI Ping, WEI Yu, et al. J Funct Anal Mater(in Chinese),2008, 39(12):2061–2064.
[22]刘耀鹏.溶剂热合成一维ZnO纳米棒及其光学性质[J].化学与生物工程, 2012, 29(9):59–60.LIU Yaopeng. Chem Bioengin(in Chinese), 2012, 29(9):59–60.
[23] DELOBEL B, LARCHER D, BLACH J F, et al. One-step precipitation of nanometric LiMO2 powders(M=Co, Fe)in alcoholic media[J]. Solid State Ionics, 2010, 181(13/14):623–630.
[24] YAO Q, WANG C, FAN B, et al. One-step solvothermal deposition of ZnO nanorod arrays on a wood surface for robust superamphiphobic performance and superior ultraviolet resistance[J]. Sci Rep, 2016, 6:35505.
[25] TONTO P, MEKA O, PHATA S, et al. Preparation of ZnO nanorod by solvothermal reaction of zinc acetate in various alcohols[J]. Ceram Inter, 2008, 34(1):57–62.
[26] BABICH I V, MOULIJN J A. Science and technology of novel processes for deep desulfurization of oil refinery streams:A review[J].Fuel, 2003, 82(6):607–631.
[27] SIRIWARDANE R, V, GARDNER T, POSTON J A, et al.Spectroscopic characterization of nickel containing desulfurization sorbents[J]. Ind Eng Chem Res, 2000, 39(4):1106–1110.
[28]邹亢,徐广通,盖金祥,等.脱硫吸附剂物相快速定量分析技术及其应用[J].石油炼制与化工, 2014, 45(10):98–104.ZOU Kang, XU Guangtong, GAI Jinxiang, et al. Pet Process PE(in Chinese), 2014, 45(10):98–104.
[29] SUN Y F, GAO S, LEI F C, et al. Atomically-thin two-dimensional sheets for understanding active sites in catalysis[J]. Chem Soc Rev,2014, 44(3):623–636.
[30]胡磊.金属纳米棒材料的合成及其在催化领域的应用[D].苏州大学, 2012.HU Lei. Synthesis of Metal Nanowire Materials and Aapplication in Catalysis(in Chinese, dissertation). Suzhou:Soochow Univ, 2012.
基本信息:
DOI：10.14062/j.issn.0454-5648.20220161
中图分类号:TQ132.41;TB383.1;TE624.5
引用信息:
[1]康蕾,卞延琨,邰伟卫,等.ZnO纳米棒的形貌控制规律及脱硫性能[J].硅酸盐学报,2022,50(10):2630-2637.DOI:10.14062/j.issn.0454-5648.20220161.
基金信息:
辽宁省教育厅科学研究项目(L2020013/L2020014); 辽宁石油化工大学引进人才科研启动基金资助(2021XJJL-020)
2022-03-04
2022
2022-08-23
2022-08-19
2022
1
2022-08-26
2022-08-26
2022-08-26