金属离子掺杂的纳米氧化锌的制备及性能研究

发布时间：2018-08-19 10:00

【摘要】：本文采用回流法制备纳米Ni_xZn_(1-x)O(x=0.0,0.04,0.08和0.12)、纳米Co_xZn_(1-x)O(x=0,0.04,0.08和0.12)和纳米Fe_xZn_(1-x)O(x=0,0.04,0.08和0.12)。用X射线衍射(XRD),扫描电镜(SEM)和透射电子显微镜(TEM),傅里叶红外光谱(FT-IR)和紫外可见吸收光谱(UV-vis)等方法对其进行了分析。以甲基橙为目标化合物,紫外灯为光源,对纳米氧化锌、掺杂Ni2、Co~(2+)和Fe~(2+)离子的纳米氧化锌的光催化活性进行了研究。结果表明:以二水乙酸锌作为前躯体,乙二醇作为溶剂,柠檬酸三钠为分散剂制备了纳米氧化锌。制得的纳米氧化锌为六方纤锌矿结构。镍掺杂的纳米氧化锌为六方纤锌矿结构;粒子近似为球形,平均粒径在10-20nm之间,粒子分布均匀,粒子间有轻微的团聚现象;随着Ni~(2+)离子含量的增加,粒子平均粒径逐渐减小;紫外光谱分析,随着Ni~(2+)离子的掺杂量的增加,吸收峰位置向小波长方向移动,出现了轻微的红移现象;掺杂Ni~(2+)离子会提高纳米氧化锌材料的光催化活性和抗菌活性,掺杂不同含量的Ni~(2+)离子也会使得纳米氧化锌的光催化性能和抗菌性能不同;在频率2-20GHz范围内,当Ni~(2+)离子掺杂量为x=0.04时,Ni~(2+)离子掺杂氧化锌介电性最好,吸波性能最好。Co~(2+)离子掺杂的纳米氧化锌为六方纤锌矿结构,掺杂的钴单质的形式存在于氧化锌表面,没有破坏氧化锌纳米棒状结构,氧化锌晶粒平均尺寸为150nm;Co~(2+)离子的掺杂明显改变了氧化锌的光催化性能,其中Co~(2+)离子的掺杂量为x=0.08时,表现出最高的光催化性能;随着Co~(2+)离子掺杂量的增加,纳米氧化锌的抗菌性能得到了提高,Co~(2+)离子的掺杂量为x=0.12时,纳米氧化锌体现出最佳的抗菌性能;在Co~(2+)离子掺杂量为x=0.04时,纳米氧化锌显示出最好的介电性和吸波性能。掺杂Fe~(2+)离子后的纳米氧化锌的晶形未发生什么改变,掺杂效果较好,形貌好,颗粒均匀,掺杂的Fe~(2+)离子能够均匀地分散到氧化锌颗粒中,削弱了细小的纳米氧化锌团聚;从红外光谱图看出,制备的样品显示出ZnO的特征吸收峰,未见Fe-O特征吸收峰;掺杂Fe~(2+)离子含量x=0.08的纳米氧化锌的降解率最高,相对于纯纳米氧化锌提高了4.59%;随着Fe~(2+)离子掺杂量的增加,其介电常数实部ε’先增大后减小,并且ε’值在Fe~(2+)离子掺杂含量为x=0.08时到达最大,在测试频率范围内,ε’’和反射损耗的大小受掺杂Fe~(2+)离子的影响比较小。
[Abstract]:In this paper, nanosized NixZn1-x) O (xc0.04 (0.08 and 0.12), nano-CoxZn1- (1-x) O (XPX) 0.04 (0.08 and 0.12) and nano-FexZn1- (1-x) O (xOON0) 0.04 (0.08 and 0.12) have been prepared by refluxing method. X-ray diffraction (XRD) (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) (TEM), Fourier transform infrared spectroscopy (FT-IR) and UV-Vis absorption spectrum (UV-vis) were used to analyze them. The photocatalytic activity of nano-zinc oxide doped with Ni _ 2CO ~ (2) and Fe ~ (2) ions was studied with methyl orange as the target compound and UV lamp as the light source. The results showed that nanometer zinc oxide was prepared by using zinc acetate dihydrate as precursor, ethylene glycol as solvent and sodium citrate as dispersant. The prepared nanometer zinc oxide is hexagonal wurtzite structure. Nickel-doped nano-zinc oxide is hexagonal wurtzite structure, the particle size is approximately spherical, the average particle size is between 10-20nm, the particle distribution is uniform, and there is a slight agglomeration between the particles, and the average particle size decreases with the increase of Ni2 ion content. Ultraviolet spectrum analysis showed that with the increase of doping amount of Ni ~ (2) ions, the position of absorption peak shifted to the direction of small wavelength, and there appeared a slight red-shift phenomenon, and the photocatalytic activity and antibacterial activity of nano-ZnO materials were improved by doping Ni ~ (2) ion. Doping of Ni ~ (2) ions with different content of Ni ~ (2) ions also resulted in different photocatalytic and antibacterial properties of nano-ZnO. In the range of frequency 2-20GHz, when the doping amount of Ni ~ (2) ions was x = 0.04, the dielectric properties of ZnO doped with Ni ~ (2) ions were the best. The nanocrystalline zinc oxide doped by Co ~ (2) ion is hexagonal wurtzite structure, and the doped cobalt element exists on the surface of zinc oxide, and does not destroy the nanorod structure of zinc oxide. The average size of ZnO grain is 150 nm ~ (2) Co ~ (2) ion doping has changed the photocatalytic performance of zinc oxide obviously, and the photocatalytic activity of Co ~ (2) ion is the highest when the doping amount of Co ~ (2) ion is x ~ (0.08), and with the increase of Co ~ (2) ion doping amount, The antibacterial properties of nanometer zinc oxide were obtained when the doping amount of Co ~ (2) ion was increased to be x ~ (2) 0.12, the nanometer zinc oxide showed the best antimicrobial property when the doping amount of Co ~ (2) ion was x = 0.04, and the nanometer zinc oxide showed the best dielectric property and absorbing property when the doping amount of Co ~ (2) ion was x = 0.04. After doping Fe ~ (2) ions, there is no change in the crystal shape of nanometer zinc oxide. The doping effect is good, the morphology is good, the particles are uniform, and the doped Fe ~ (2) ions can be dispersed uniformly into the zinc oxide particles, which weakens the fine nano-ZnO agglomeration. The infrared spectra showed that the prepared samples showed the characteristic absorption peak of ZnO, but no characteristic absorption peak of Fe-O, and the degradation rate of nano-ZnO doped with Fe2 + x0. 08 was the highest. The dielectric constant 蔚 'increases first and then decreases with the increase of Fe ~ (2) ion doping content, and the 蔚' value reaches the maximum when the Fe ~ (2) ion doping content is x ~ (0.08). In the range of measured frequency, the magnitude of 蔚 'and reflection loss is less affected by doped Fe ~ (2) ion.
【学位授予单位】：沈阳理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ132.41;TB383.1

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