模板法制备一维铁氧体纳米线（管）及其磁性能研究
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摘要
本论文采用阳极氧化法制备了多孔氧化铝膜(AAO),再以所制备的AAO为模板,运用溶胶/凝胶法制备了钴铁氧体纳米线/管和钡铁氧体纳米线。经XRD、SEM、VSM等表征手段,研究了AAO的制备影响因素、铁氧体纳米线/管的制备影响因素及磁性能。
AAO制备影响因素研究结果表明:电压对AAO纳米孔道影响显著,升高氧化电压引起孔径增大且孔排列有序程度增加,但电压过高会因氧化反应过于激烈而不利于纳米孔道的形成;二次阳极氧化较一次阳极氧化所得到的孔的空隙率提高,孔间距减小,且孔更接近正六边形;在一定浓度范围内,草酸电解液浓度对阳极氧化过程无明显影响;适当提高扩孔温度和延长扩孔时间能增大孔径;随着氧化时间延长,膜厚度呈现“先迅速增长、再缓慢增加、然后平稳”的变化趋势;氧化温度较高易引起酸性电解液对孔洞和阻挡层的腐蚀作用加剧,不利于AAO的制备。
钴铁氧体纳米线/管制备影响因素研究结果表明:沉积时间和沉积次数影响铁氧体前驱体在AAO孔道中的填充程度,进而影响纳米线长度或线状、管状形貌的形成;溶胶pH值的减小会引起AAO腐蚀,因而要制备更长的纳米线需提高溶胶pH值;延长煅烧时间引起钴铁氧体纳米线结晶有序程度提高;升高煅烧温度不但使钴铁氧体纳米线的结晶有序程度显著提高,且部分Al~(3+)取代了Fe~(3+),进而使得钴铁氧体晶胞参数减小。
钴铁氧体纳米线/管磁性能研究结果表明:纳米线长径比的提高有利于钴铁氧体纳米线的饱和磁化强度M_s、剩余磁化强度M_r、矫顽力H_c、矩形比P的增加;直径相近条件下,钴铁氧体纳米管的磁性能优于纳米线;煅烧时间和煅烧温度对钴铁氧体纳米线的M_s、M_r、H_c和P也存在明显影响。延长煅烧时间引起M_s、M_r、H_c和P均有所增加,升高煅烧温度则使M_s、M_r、H_c和P均显著增加。这主要归因于延长煅烧时间或提高煅烧温度导致钴铁氧体纳米线的结晶度提高或显著提高,且增加煅烧温度使部分Fe~(3+)被Al~(3+)取代,进而提高了铁氧体纳米线的磁性能。前述结果暗示,当磁晶各向异性固定于一定程度时,形状各向异性对钴铁氧体磁性能的影响不容忽视;再者,基于钴铁氧体纳米线的磁性能与其长径比、线或管状形貌及结晶有序程度的内在联系,可通过制备条件对钴铁氧体纳米线的长径比、线或管状形貌或结晶有序程度的影响,实现对钴铁氧体纳米线磁性能的控制。
In this paper, Co ferrite nanowires(nanotubes)/Ba ferrite nanowires were prepared by sol-gel method using porous anodic alumina oxide(AAO) membrane as template. The factors ofpreparation of the AAO,ferrite nanowires/tubes and magnetic properties were studyied by XRD,SEM,VSM methods.
The factors of preparation of the AAO show:voltage on the nano-pores have a significant effect,with the oxidation voltage is increased,the pore size is even greater, nano-holes arranged more orderly,but the voltage is too high oxidation reaction would be too intense,is not conducive to the formation of nano-pore.The hole markedly improved,pore spacing significantly decreases,and the hole is more regular hexagon by two steps oxidation compared to an anodic oxidation;The oxalic acid electrolyte concentration has little effect on the anodic oxidation process in the context of a certain concentration;Appropriate opening temperature and time can be increased to extend the bore hole;With the extension of oxidation time,the membrane thickness showed”rapid growth in the first,then slowly increasing,and then smooth”changes in trends;The corrosive effec of nano-holes and barriers was intensified in high temperature,it is not conducive to the formation of AAO.
The results of preparation of Co ferrite nanowires(nanotubes)showed that: deposition time and frequency that primarily affects the pore filling degree of ferrite precursor in the AAO template, thereby affecting nanowire length or formation of wires, tubes shape.Sol pH need to improve in oder to preparate longer nanowires.Co ferrite nanowire crystallinity degree increased by extension of calcining time;Higher calcination temperature not only make the cobalt ferrite nanowire crystallinity significantly increased,and part of the Al~(3+) replaces Fe~(3+),thus makes the cobalt ferrite lattice parameters decrease.
Cobalt ferrite nanowires/tubes magnetic properties results show that:With the increasing of aspect ratio,cobalt ferrite nanowires saturation magnetization,residual magnetization,coercivity,squareness ratio were increased;The same diameter of cobalt ferrite magnetic properties of nanotubes is superior to a considerable diameter nanowires;calcination time and calcination temperature have significant effect on the Ms, Mr, Hc,and P of cobalt ferrite nanowires.To extend the calcining time caused by Ms,Mr, Hc,and P have increased,and higher calcination temperature makes Ms,Mr,Hc,and P both increased significantly.This is mainly due to extended time or improve the calcination temperature calcination of cobalt ferrite nanowires leading to the degree of crystallinity increased or significantly increased,and the increase of calcination temperature to make part of the Fe~(3+) has been replaced by Al~(3+),thereby increasing the ferrite magnetic properties of nanowires.The results suggest that,when the magnetic anisotropy fixed at a certain degree,the shape anisotropy of the magnetic properties of cobalt ferrite can not be ignored;Moreover,based on of Co ferrite nanowires magnetic properties have internal relations with aspect ratio,wires or tubes,morphology and crystallinity degree,we can control the magnetic properties of Co ferrite nano-wires by change the conditions of preparation of Co ferrite nano-wires.
AAO制备影响因素研究结果表明:电压对AAO纳米孔道影响显著,升高氧化电压引起孔径增大且孔排列有序程度增加,但电压过高会因氧化反应过于激烈而不利于纳米孔道的形成;二次阳极氧化较一次阳极氧化所得到的孔的空隙率提高,孔间距减小,且孔更接近正六边形;在一定浓度范围内,草酸电解液浓度对阳极氧化过程无明显影响;适当提高扩孔温度和延长扩孔时间能增大孔径;随着氧化时间延长,膜厚度呈现“先迅速增长、再缓慢增加、然后平稳”的变化趋势;氧化温度较高易引起酸性电解液对孔洞和阻挡层的腐蚀作用加剧,不利于AAO的制备。
钴铁氧体纳米线/管制备影响因素研究结果表明:沉积时间和沉积次数影响铁氧体前驱体在AAO孔道中的填充程度,进而影响纳米线长度或线状、管状形貌的形成;溶胶pH值的减小会引起AAO腐蚀,因而要制备更长的纳米线需提高溶胶pH值;延长煅烧时间引起钴铁氧体纳米线结晶有序程度提高;升高煅烧温度不但使钴铁氧体纳米线的结晶有序程度显著提高,且部分Al~(3+)取代了Fe~(3+),进而使得钴铁氧体晶胞参数减小。
钴铁氧体纳米线/管磁性能研究结果表明:纳米线长径比的提高有利于钴铁氧体纳米线的饱和磁化强度M_s、剩余磁化强度M_r、矫顽力H_c、矩形比P的增加;直径相近条件下,钴铁氧体纳米管的磁性能优于纳米线;煅烧时间和煅烧温度对钴铁氧体纳米线的M_s、M_r、H_c和P也存在明显影响。延长煅烧时间引起M_s、M_r、H_c和P均有所增加,升高煅烧温度则使M_s、M_r、H_c和P均显著增加。这主要归因于延长煅烧时间或提高煅烧温度导致钴铁氧体纳米线的结晶度提高或显著提高,且增加煅烧温度使部分Fe~(3+)被Al~(3+)取代,进而提高了铁氧体纳米线的磁性能。前述结果暗示,当磁晶各向异性固定于一定程度时,形状各向异性对钴铁氧体磁性能的影响不容忽视;再者,基于钴铁氧体纳米线的磁性能与其长径比、线或管状形貌及结晶有序程度的内在联系,可通过制备条件对钴铁氧体纳米线的长径比、线或管状形貌或结晶有序程度的影响,实现对钴铁氧体纳米线磁性能的控制。
In this paper, Co ferrite nanowires(nanotubes)/Ba ferrite nanowires were prepared by sol-gel method using porous anodic alumina oxide(AAO) membrane as template. The factors ofpreparation of the AAO,ferrite nanowires/tubes and magnetic properties were studyied by XRD,SEM,VSM methods.
The factors of preparation of the AAO show:voltage on the nano-pores have a significant effect,with the oxidation voltage is increased,the pore size is even greater, nano-holes arranged more orderly,but the voltage is too high oxidation reaction would be too intense,is not conducive to the formation of nano-pore.The hole markedly improved,pore spacing significantly decreases,and the hole is more regular hexagon by two steps oxidation compared to an anodic oxidation;The oxalic acid electrolyte concentration has little effect on the anodic oxidation process in the context of a certain concentration;Appropriate opening temperature and time can be increased to extend the bore hole;With the extension of oxidation time,the membrane thickness showed”rapid growth in the first,then slowly increasing,and then smooth”changes in trends;The corrosive effec of nano-holes and barriers was intensified in high temperature,it is not conducive to the formation of AAO.
The results of preparation of Co ferrite nanowires(nanotubes)showed that: deposition time and frequency that primarily affects the pore filling degree of ferrite precursor in the AAO template, thereby affecting nanowire length or formation of wires, tubes shape.Sol pH need to improve in oder to preparate longer nanowires.Co ferrite nanowire crystallinity degree increased by extension of calcining time;Higher calcination temperature not only make the cobalt ferrite nanowire crystallinity significantly increased,and part of the Al~(3+) replaces Fe~(3+),thus makes the cobalt ferrite lattice parameters decrease.
Cobalt ferrite nanowires/tubes magnetic properties results show that:With the increasing of aspect ratio,cobalt ferrite nanowires saturation magnetization,residual magnetization,coercivity,squareness ratio were increased;The same diameter of cobalt ferrite magnetic properties of nanotubes is superior to a considerable diameter nanowires;calcination time and calcination temperature have significant effect on the Ms, Mr, Hc,and P of cobalt ferrite nanowires.To extend the calcining time caused by Ms,Mr, Hc,and P have increased,and higher calcination temperature makes Ms,Mr,Hc,and P both increased significantly.This is mainly due to extended time or improve the calcination temperature calcination of cobalt ferrite nanowires leading to the degree of crystallinity increased or significantly increased,and the increase of calcination temperature to make part of the Fe~(3+) has been replaced by Al~(3+),thereby increasing the ferrite magnetic properties of nanowires.The results suggest that,when the magnetic anisotropy fixed at a certain degree,the shape anisotropy of the magnetic properties of cobalt ferrite can not be ignored;Moreover,based on of Co ferrite nanowires magnetic properties have internal relations with aspect ratio,wires or tubes,morphology and crystallinity degree,we can control the magnetic properties of Co ferrite nano-wires by change the conditions of preparation of Co ferrite nano-wires.
引文
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