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金屬離子摻雜的納米氧化鋅的制備及性能研究

發(fā)布時(shí)間:2018-08-19 10:00
【摘要】:本文采用回流法制備納米Ni_xZn_(1-x)O(x=0.0,0.04,0.08和0.12)、納米Co_xZn_(1-x)O(x=0,0.04,0.08和0.12)和納米Fe_xZn_(1-x)O(x=0,0.04,0.08和0.12)。用X射線(xiàn)衍射(XRD),掃描電鏡(SEM)和透射電子顯微鏡(TEM),傅里葉紅外光譜(FT-IR)和紫外可見(jiàn)吸收光譜(UV-vis)等方法對(duì)其進(jìn)行了分析。以甲基橙為目標(biāo)化合物,紫外燈為光源,對(duì)納米氧化鋅、摻雜Ni2、Co~(2+)和Fe~(2+)離子的納米氧化鋅的光催化活性進(jìn)行了研究。結(jié)果表明:以二水乙酸鋅作為前軀體,乙二醇作為溶劑,檸檬酸三鈉為分散劑制備了納米氧化鋅。制得的納米氧化鋅為六方纖鋅礦結(jié)構(gòu)。鎳摻雜的納米氧化鋅為六方纖鋅礦結(jié)構(gòu);粒子近似為球形,平均粒徑在10-20nm之間,粒子分布均勻,粒子間有輕微的團(tuán)聚現(xiàn)象;隨著Ni~(2+)離子含量的增加,粒子平均粒徑逐漸減小;紫外光譜分析,隨著Ni~(2+)離子的摻雜量的增加,吸收峰位置向小波長(zhǎng)方向移動(dòng),出現(xiàn)了輕微的紅移現(xiàn)象;摻雜Ni~(2+)離子會(huì)提高納米氧化鋅材料的光催化活性和抗菌活性,摻雜不同含量的Ni~(2+)離子也會(huì)使得納米氧化鋅的光催化性能和抗菌性能不同;在頻率2-20GHz范圍內(nèi),當(dāng)Ni~(2+)離子摻雜量為x=0.04時(shí),Ni~(2+)離子摻雜氧化鋅介電性最好,吸波性能最好。Co~(2+)離子摻雜的納米氧化鋅為六方纖鋅礦結(jié)構(gòu),摻雜的鈷單質(zhì)的形式存在于氧化鋅表面,沒(méi)有破壞氧化鋅納米棒狀結(jié)構(gòu),氧化鋅晶粒平均尺寸為150nm;Co~(2+)離子的摻雜明顯改變了氧化鋅的光催化性能,其中Co~(2+)離子的摻雜量為x=0.08時(shí),表現(xiàn)出最高的光催化性能;隨著Co~(2+)離子摻雜量的增加,納米氧化鋅的抗菌性能得到了提高,Co~(2+)離子的摻雜量為x=0.12時(shí),納米氧化鋅體現(xiàn)出最佳的抗菌性能;在Co~(2+)離子摻雜量為x=0.04時(shí),納米氧化鋅顯示出最好的介電性和吸波性能。摻雜Fe~(2+)離子后的納米氧化鋅的晶形未發(fā)生什么改變,摻雜效果較好,形貌好,顆粒均勻,摻雜的Fe~(2+)離子能夠均勻地分散到氧化鋅顆粒中,削弱了細(xì)小的納米氧化鋅團(tuán)聚;從紅外光譜圖看出,制備的樣品顯示出ZnO的特征吸收峰,未見(jiàn)Fe-O特征吸收峰;摻雜Fe~(2+)離子含量x=0.08的納米氧化鋅的降解率最高,相對(duì)于純納米氧化鋅提高了4.59%;隨著Fe~(2+)離子摻雜量的增加,其介電常數(shù)實(shí)部ε’先增大后減小,并且ε’值在Fe~(2+)離子摻雜含量為x=0.08時(shí)到達(dá)最大,在測(cè)試頻率范圍內(nèi),ε’’和反射損耗的大小受摻雜Fe~(2+)離子的影響比較小。
[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.
【學(xué)位授予單位】:沈陽(yáng)理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類(lèi)號(hào)】:TQ132.41;TB383.1

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