反溶剂沉淀法合成Fe~(3+)掺杂ZnO纳米结构及其可见光催化性能
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摘要
以氯化胆碱-草酸低共熔溶剂(ChCl-OA DES)为溶剂,ZnO和Fe_2O_3为原料,通过简单的反溶剂沉淀法制备出不同掺杂浓度的Fe~(3+)掺杂ZnO (Fe-ZnO)纳米结构。采用SEM、XRD、拉曼光谱、XPS等手段对所制Fe-ZnO结构与形貌进行了表征。结果表明,Fe-ZnO是由直径为20～30 nm纳米晶组装而成的微米棒。不同掺杂浓度的Fe-ZnO纳米晶均为六方铅锌矿结构,Fe~(3+)很好地进入ZnO晶格。同时考察了所制Fe-ZnO的光吸收特性和光催化活性,发现Fe~(3+)掺杂使其吸收峰红移至可见光范围,有效增强了可见光区域的催化活性。当Fe掺杂量为1.0%(atom)时,样品的光催化活性最好,比ZnO增大了约102倍。这说明Fe~(3+)掺杂可改善ZnO对可见光光子的捕获能力。
Fe~(3+)-doped ZnO(Fe-ZnO) nanostructures with different dopant concentrations were successfully synthesized by a simple antisolvent precipitation method from the choline chloride-oxalic acid deep eutectic solvent(ChCl-OA DES). The structure and morphology of the prepared Fe-ZnO were characterized by SEM, XRD, Raman spectroscopy and XPS. The as-prepared Fe~(3+)-doped ZnO sample was micro-rods that were composed of nanopartiles with diameter of 20-30 nm. All of Fe~(3+)-doped ZnO samples with various Fe~(3+)-doping concentration were hexagonal wurtzite structure and the Fe~(3+) ions were well incorporated into the ZnO crystal lattice. In addition,the optical properties and photocatalytic activities of the samples were investigated based on ultraviolet-visible(UV-Vis) spectra analysis as well as the degradation of Rhodamine B in aqueous solution under visible light.Compared with ZnO catalysts, the threshold wavelength of Fe~(3+)-doped ZnO nanostructure was shifted to the full visible light region(red shift) and their absorption in the visible region increased with increasing of Fe~(3+)-doping concentration from 0 to 5.0%(atom). The content of iron ion was found to be significant to the photocatalytic efficiency of Fe-ZnO nanostructures. The results demonstrated that the most optimal Fe~(3+)-doping concentration was 1.0%(atom), and its photocatalytic activity was increased by 102% compared with ZnO under visible light. The enhanced photoactivity of the Fe~(3+)-doped ZnO nanostructure was mainly due to the improved visible photon harvesting achieved by Fe~(3+) doping.
Fe~(3+)-doped ZnO(Fe-ZnO) nanostructures with different dopant concentrations were successfully synthesized by a simple antisolvent precipitation method from the choline chloride-oxalic acid deep eutectic solvent(ChCl-OA DES). The structure and morphology of the prepared Fe-ZnO were characterized by SEM, XRD, Raman spectroscopy and XPS. The as-prepared Fe~(3+)-doped ZnO sample was micro-rods that were composed of nanopartiles with diameter of 20-30 nm. All of Fe~(3+)-doped ZnO samples with various Fe~(3+)-doping concentration were hexagonal wurtzite structure and the Fe~(3+) ions were well incorporated into the ZnO crystal lattice. In addition,the optical properties and photocatalytic activities of the samples were investigated based on ultraviolet-visible(UV-Vis) spectra analysis as well as the degradation of Rhodamine B in aqueous solution under visible light.Compared with ZnO catalysts, the threshold wavelength of Fe~(3+)-doped ZnO nanostructure was shifted to the full visible light region(red shift) and their absorption in the visible region increased with increasing of Fe~(3+)-doping concentration from 0 to 5.0%(atom). The content of iron ion was found to be significant to the photocatalytic efficiency of Fe-ZnO nanostructures. The results demonstrated that the most optimal Fe~(3+)-doping concentration was 1.0%(atom), and its photocatalytic activity was increased by 102% compared with ZnO under visible light. The enhanced photoactivity of the Fe~(3+)-doped ZnO nanostructure was mainly due to the improved visible photon harvesting achieved by Fe~(3+) doping.
引文
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[33]Maldonado M,Oleksiak M D,Chinta S,et al.Controlling crystal polymorphism in organic-free synthesis of Na-zeolites[J].Journal of the American Chemical Society,2013,135(7):2641-2652.
[34]Liao H G,Jiang Y X,Zhou Z Y,et al.Shape-controlled synthesis of gold nanoparticles in deep eutectic solvents for studies of structure-functionality relationships in electrocatalysis[J].Angewandte Chemie International Edition,2008,47(47):9100-9103.
[35]Abbott A P,Capper G,Davies D L,et al.Selective extraction of metals from mixed oxide matrixes using choline-based ionic liquids[J].Inorganic Chemistry,2005,44(19):6497-6499.
[36]Dong J Y,Hsu Y J,Wong D S H,et al.Growth of ZnOnanostructures with controllable morphology using a facile green antisolvent method[J].The Journal of Physical Chemistry C,2010,114(19):8867-8872.
[37]Shakti N,Gupta P S.Structural and optical properties of sol-gel prepared ZnO thin film[J].Applied Physics Research,2010,2(1):19-28.
[38]Bundesmann C,Ashkenov N,Schubert M,et al.Raman scattering in ZnO thin films doped with Fe,Sb,Al,Ga,and Li[J].Applied Physics Letters,2003,83(10):1974-1976.
[39]Wang J B,Huang G J,Zhong X L,et al.Raman scattering and high temperature ferromagnetism of Mn-doped ZnO nanoparticles[J].Applied Physics Letters,2006,88(25):252502.
[40]Singh P,Kaushal A,Kaur D.Mn-doped ZnO nanocrystalline thin films prepared by ultrasonic spray pyrolysis[J].Journal of Alloys and Compounds,2009,471(1/2):11-15.
[41]Karamat S,Rawat R S,Lee P,et al.Structural,elemental,optical and magnetic study of Fe doped ZnO and impurity phase formation[J].Progress in Natural Science:Materials International,2014,24(2):142-149.
[42]Rambu A P,Nica V,Dobromir M.Influence of Fe-doping on the optical and electrical properties of ZnO films[J].Superlattices and Microstructures,2013,59:87-96.
[43]Cui J,Sun J,Liu X,et al.Fabrication of hierarchical flower-like porous ZnO nanostructures from layered ZnC2O4·3Zn(OH)2and gas sensing properties[J].Applied Surface Science,2014,308:17-23.
[44]Raja K,Ramesh P S,Geetha D.Structural,FTIR and photoluminescence studies of Fe doped ZnO nanopowder by coprecipitation method[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2014,131:183-188.
[45]Mitra P,Mondal S.Structural and morphological characterization of ZnO thin films synthesized by SILAR[J].Progress in Theoretical and Applied Physics,2013,1:17-31.
[46]Parra P A,Perales P O,Singhal R,et al.Structural,optical,and magnetic characterization of monodisperse Fe-doped ZnOnanocrystals[J].Journal of Applied Physics,2008,103(7):07D121.
[47]李奡麒,陈玉娟,胡晓宇,等.低共熔溶剂辅助水热法合成分层球状微/纳米ZnO晶体及其光催化性能[J].高等学校化学学报,2015,36(1):165-170.Li W Q,Chen Y J,Hu X Y,et al.Synthesis of layered spherical micro/nano ZnO crystals by hydrothermal solvent-assisted hydrothermal method[J].Chemical Journal of Chinese Universities,2015,36(1):165-170.
[48]Zhang Q,Liu J K,Wang J D,et al.Atmospheric self-induction synthesis and enhanced visible light photocatalytic performance of Fe3+doped Ag-ZnO mesocrystals[J].Ind.Eng.Chem.Res.,2014,53:13236-13246
[2]Saleh R,Djaja N F.UV light photocatalytic degradation of organic dyes with Fe-doped ZnO nanoparticles[J].Superlattices and Microstructures,2014,74:217-233.
[3]Wang Y,Zhao X,Duan L,et al.Structure,luminescence and photocatalytic activity of Mg-doped ZnO nanoparticles prepared by auto combustion method[J].Materials Science in Semiconductor Processing,2015,29:372-379.
[4]丁艳,马歌,李良超,等.M2+(M=Cu,Cd,Ag,Fe)掺杂氧化锌纳米粉晶的抗菌性能[J].无机化学学报,2014,30(2):293-302.Ding Y,Ma G,Li L C,et al.Antibacterial activities of doped ZnOnano-powder with M2+(M=Cu,Cd,Ag and Fe)[J].Chinese Journal of Inorganic Chemistry,2014,30(2):293-302.
[5]Kumar R,Umar A,Kumar G,et al.Ce-doped ZnO nanoparticles for efficient photocatalytic degradation of direct red-23 dye[J].Ceramics International,2015,41(6):7773-7782.
[6]Shukla S K,Agorku E S,Mittal H,et al.Synthesis,characterization and photoluminescence properties of Ce3+-doped ZnO-nanophosphors[J].Chemical Papers,2014,68(2):217-222.
[7]Ismail I M I,Aslam M,Almeelbi T,et al.Ce3+impregnated ZnO:a highly efficient photocatalyst for sunlight mediated mineralization[J].RSC Advances,2014,4(31):16043-16046.
[8]Sharma D K,Sharma K K,Kumar V,et al.Effect of Ce doping on the structural,optical and magnetic properties of ZnOnanoparticles[J].Journal of Materials Science:Materials in Electronics,2016,27(10):10330-10335.
[9]May J W,Ma J,Badaeva E,et al.Effect of excited-state structural relaxation on midgap excitations in Co2+-doped ZnO quantum dots[J].The Journal of Physical Chemistry C,2014,118(24):13152-13156.
[10]Kumar S,Song T K,Gautam S,et al.Structural,magnetic and electronic structure properties of Co doped ZnO nanoparticles[J].Materials Research Bulletin,2015,66:76-82.
[11]Raza W,Haque M M,Muneer M.Synthesis of visible light driven ZnO:characterization and photocatalytic performance[J].Applied Surface Science,2014,322:215-224.
[12]Kaneva N,Bojinova A,Papazova K,et al.Photocatalytic purification of dye contaminated sea water by lanthanide(La3+,Ce3+,Eu3+)modified ZnO[J].Catalysis Today,2015,252:113-119.
[13]Chen C,Ma W,Zhao J.Semiconductor-mediated photodegradation of pollutants under visible-light irradiation[J].Chem.Soc.Rev.,2010,39:4206-4219.
[14]Baik J M,Kang T W,Lee J L.Effects of N2O plasma treatment on magnetic properties of(Zn,Mn)O nanorods[J].Nanotechnology,2007,18(9):095703.
[15]翟英娇,李金华,陈新影,等.镉掺杂氧化锌纳米花的制备及其光催化活性[J].中国光学,2014,7(1):124-130.Zhai Y J,Li J H,Chen X Y,et al.Preparation and photocatalytic activity of cadmium-doped zinc oxide nanoflowers[J].China Optics,2014,7(1):124-130.
[16]Koleva M E,Atanasov P A,Nedialkov N N,et al.Role of vanadium content in ZnO thin films grown by pulsed laser deposition[J].Applied Surface Science,2007,254(4):1228-1231.
[17]Yimaz S,Parlak M,?zcan?,et al.Structural,optical and magnetic properties of Cr doped ZnO microrods prepared by spray pyrolysis method[J].Applied Surface Science,2011,257(22):9293-9298.
[18]Shinde V R,Gujar T P,Lokhande C D,et al.Mn doped and undoped ZnO films:a comparative structural,optical and electrical properties study[J].Mater.Chem.Phys.,2006,96:326-330.
[19]Shishodia P K.Effect of cobalt doping on ZnO thin films deposited by sol-gel method[J].Thin Solid Films,2016,612:55-60.
[20]Zhao X,Liu E,Ramanujan R V,et al.Effects of rapid thermal annealing on structural,magnetic and optical properties of Nidoped ZnO thin films[J].Current Applied Physics,2012,12(3):834-840.
[21]Hou D L,Ye X J,Meng H J,et al.Magnetic properties of n-type Cu-doped ZnO thin films[J].Applied Physics Letters,2007,90(14):142502.
[22]Srivastava A,Kumar N,Khare S.Enhancement in UV emission and band gap by Fe doping in ZnO thin films[J].Opto-Electronics Review,2014,22(1):68-76.
[23]Yi S S,Cui J B,Li S,et al.Enhanced visible-light photocatalytic activity of Fe/ZnO for Rhodamine B degradation and its photogenerated charge transfer properties[J].Applied Surface Science,2014,319:230-236.
[24]Saleh R,Djaja N F.UV light photocatalytic degradation of organic dyes with Fe-doped ZnO nanoparticles[J].Superlattices and Microstructures,2014,74:217-233.
[25]Lmai F,Moubah R,Amiri E A,et al.Spin wave study and optical properties in Fe-doped ZnO thin films prepared by spray pyrolysis technique[J].Optical Materials,2016,57:28-33.
[26]Wu X,Wei Z,Zhang L,et al.Optical and magnetic properties of Fe doped ZnO nanoparticles obtained by hydrothermal synthesis[J].Journal of Nanomaterials,2014,2014:1-6.
[27]Li X,Hou M,Han B,et al.Solubility of CO2in a choline chloride+urea eutectic mixture[J].Journal of Chemical&Engineering Data,2008,53(2):548-550.
[28]Abbott A P,Cullis P M,Gibson M J,et al.Extraction of glycerol from biodiesel into a eutectic based ionic liquid[J].Green Chemistry,2007,9(8):868-872.
[29]Phadtare S B,Shankarling G S.Halogenation reactions in biodegradable solvent:efficient bromination of substituted 1-aminoanthra-9,10-quinone in deep eutectic solvent(choline chloride:urea)[J].Green Chemistry,2010,12(3):458-462.
[30]Harishkumar H N,Mahadevan K M,Masagalli J N,et al.Synthesis and fluorescence study of phenylcoumarin/cyanophenylbenzocoumarin-3-carboxylates[J].Organic Communications,2012,5(4):196-208.
[31]Pawa P M,Jarag K J,Shankarling G S.Environmentally benign and energy efficient methodology for condensation:an interesting facet to the classical Perkin reaction[J].Green Chemistry,2011,13(8):2130-2134.
[32]Sutrisno A,Liu L,Dong J,et al.Solid-state 91Zr NMRcharacterization of layered and three-dimensional framework zirconium phosphates[J].The Journal of Physical Chemistry C,2012,116(32):17070-17081.
[33]Maldonado M,Oleksiak M D,Chinta S,et al.Controlling crystal polymorphism in organic-free synthesis of Na-zeolites[J].Journal of the American Chemical Society,2013,135(7):2641-2652.
[34]Liao H G,Jiang Y X,Zhou Z Y,et al.Shape-controlled synthesis of gold nanoparticles in deep eutectic solvents for studies of structure-functionality relationships in electrocatalysis[J].Angewandte Chemie International Edition,2008,47(47):9100-9103.
[35]Abbott A P,Capper G,Davies D L,et al.Selective extraction of metals from mixed oxide matrixes using choline-based ionic liquids[J].Inorganic Chemistry,2005,44(19):6497-6499.
[36]Dong J Y,Hsu Y J,Wong D S H,et al.Growth of ZnOnanostructures with controllable morphology using a facile green antisolvent method[J].The Journal of Physical Chemistry C,2010,114(19):8867-8872.
[37]Shakti N,Gupta P S.Structural and optical properties of sol-gel prepared ZnO thin film[J].Applied Physics Research,2010,2(1):19-28.
[38]Bundesmann C,Ashkenov N,Schubert M,et al.Raman scattering in ZnO thin films doped with Fe,Sb,Al,Ga,and Li[J].Applied Physics Letters,2003,83(10):1974-1976.
[39]Wang J B,Huang G J,Zhong X L,et al.Raman scattering and high temperature ferromagnetism of Mn-doped ZnO nanoparticles[J].Applied Physics Letters,2006,88(25):252502.
[40]Singh P,Kaushal A,Kaur D.Mn-doped ZnO nanocrystalline thin films prepared by ultrasonic spray pyrolysis[J].Journal of Alloys and Compounds,2009,471(1/2):11-15.
[41]Karamat S,Rawat R S,Lee P,et al.Structural,elemental,optical and magnetic study of Fe doped ZnO and impurity phase formation[J].Progress in Natural Science:Materials International,2014,24(2):142-149.
[42]Rambu A P,Nica V,Dobromir M.Influence of Fe-doping on the optical and electrical properties of ZnO films[J].Superlattices and Microstructures,2013,59:87-96.
[43]Cui J,Sun J,Liu X,et al.Fabrication of hierarchical flower-like porous ZnO nanostructures from layered ZnC2O4·3Zn(OH)2and gas sensing properties[J].Applied Surface Science,2014,308:17-23.
[44]Raja K,Ramesh P S,Geetha D.Structural,FTIR and photoluminescence studies of Fe doped ZnO nanopowder by coprecipitation method[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2014,131:183-188.
[45]Mitra P,Mondal S.Structural and morphological characterization of ZnO thin films synthesized by SILAR[J].Progress in Theoretical and Applied Physics,2013,1:17-31.
[46]Parra P A,Perales P O,Singhal R,et al.Structural,optical,and magnetic characterization of monodisperse Fe-doped ZnOnanocrystals[J].Journal of Applied Physics,2008,103(7):07D121.
[47]李奡麒,陈玉娟,胡晓宇,等.低共熔溶剂辅助水热法合成分层球状微/纳米ZnO晶体及其光催化性能[J].高等学校化学学报,2015,36(1):165-170.Li W Q,Chen Y J,Hu X Y,et al.Synthesis of layered spherical micro/nano ZnO crystals by hydrothermal solvent-assisted hydrothermal method[J].Chemical Journal of Chinese Universities,2015,36(1):165-170.
[48]Zhang Q,Liu J K,Wang J D,et al.Atmospheric self-induction synthesis and enhanced visible light photocatalytic performance of Fe3+doped Ag-ZnO mesocrystals[J].Ind.Eng.Chem.Res.,2014,53:13236-13246