本文選題：多孔氧化鋁膜 + 納米線(管)陣列�。� 參考：《沈陽理工大學(xué)》2010年碩士論文

【摘要】： 本論文采用陽極氧化法制備了多孔氧化鋁膜(AAO),再以所制備的AAO為模板,運(yùn)用溶膠/凝膠法制備了鈷鐵氧體納米線/管和鋇鐵氧體納米線。經(jīng)XRD、SEM、VSM等表征手段,研究了AAO的制備影響因素、鐵氧體納米線/管的制備影響因素及磁性能。 AAO制備影響因素研究結(jié)果表明:電壓對AAO納米孔道影響顯著,升高氧化電壓引起孔徑增大且孔排列有序程度增加,但電壓過高會因氧化反應(yīng)過于激烈而不利于納米孔道的形成;二次陽極氧化較一次陽極氧化所得到的孔的空隙率提高,孔間距減小,且孔更接近正六邊形;在一定濃度范圍內(nèi),草酸電解液濃度對陽極氧化過程無明顯影響;適當(dāng)提高擴(kuò)孔溫度和延長擴(kuò)孔時間能增大孔徑;隨著氧化時間延長,膜厚度呈現(xiàn)“先迅速增長、再緩慢增加、然后平穩(wěn)”的變化趨勢;氧化溫度較高易引起酸性電解液對孔洞和阻擋層的腐蝕作用加劇,不利于AAO的制備。 鈷鐵氧體納米線/管制備影響因素研究結(jié)果表明:沉積時間和沉積次數(shù)影響鐵氧體前驅(qū)體在AAO孔道中的填充程度,進(jìn)而影響納米線長度或線狀、管狀形貌的形成;溶膠pH值的減小會引起AAO腐蝕,因而要制備更長的納米線需提高溶膠pH值;延長煅燒時間引起鈷鐵氧體納米線結(jié)晶有序程度提高;升高煅燒溫度不但使鈷鐵氧體納米線的結(jié)晶有序程度顯著提高,且部分Al~(3+)取代了Fe~(3+),進(jìn)而使得鈷鐵氧體晶胞參數(shù)減小。 鈷鐵氧體納米線/管磁性能研究結(jié)果表明:納米線長徑比的提高有利于鈷鐵氧體納米線的飽和磁化強(qiáng)度M_s、剩余磁化強(qiáng)度M_r、矯頑力H_c、矩形比P的增加;直徑相近條件下,鈷鐵氧體納米管的磁性能優(yōu)于納米線;煅燒時間和煅燒溫度對鈷鐵氧體納米線的M_s、M_r、H_c和P也存在明顯影響。延長煅燒時間引起M_s、M_r、H_c和P均有所增加,升高煅燒溫度則使M_s、M_r、H_c和P均顯著增加。這主要?dú)w因于延長煅燒時間或提高煅燒溫度導(dǎo)致鈷鐵氧體納米線的結(jié)晶度提高或顯著提高,且增加煅燒溫度使部分Fe~(3+)被Al~(3+)取代,進(jìn)而提高了鐵氧體納米線的磁性能。前述結(jié)果暗示,當(dāng)磁晶各向異性固定于一定程度時,形狀各向異性對鈷鐵氧體磁性能的影響不容忽視;再者,基于鈷鐵氧體納米線的磁性能與其長徑比、線或管狀形貌及結(jié)晶有序程度的內(nèi)在聯(lián)系,可通過制備條件對鈷鐵氧體納米線的長徑比、線或管狀形貌或結(jié)晶有序程度的影響,實(shí)現(xiàn)對鈷鐵氧體納米線磁性能的控制。
[Abstract]:In this paper, the porous alumina membrane (AAO) was prepared by anodic oxidation, and the prepared AAO was used as a template. The nanowire / tube and barium ferrite nanowires were prepared by the sol / gel method. The influencing factors of preparation of AAO, the influencing factors and magnetic properties of the preparation of ferrite nanowires / tubes were studied by means of XRD, SEM and VSM.
The influence factors of the AAO preparation show that the voltage has a significant effect on the nano channel of AAO, the increase of the oxidation voltage and the increase in the order of the pore arrangement, but the excessive voltage will not help the formation of the nanoscale through the excessive oxidation reaction, and the porosity of the hole obtained by the two anodization is higher than that of the first anodic oxidation. In a certain concentration range, the concentration of oxalic acid has no obvious effect on the anodic oxidation process, and the pore size can be increased by increasing the reaming temperature and prolonging the reaming time. With the prolonged oxidation time, the film thickness presents a "first rapid growth, then slow increase, and then smooth" change trend. The higher temperature causes the corrosion of acidic electrolyte to the pores and barrier layers, which is not conducive to the preparation of AAO.
The study results of cobalt ferrite nanowires / control factors show that deposition time and deposition times affect the filling degree of ferrite precursor in the AAO channel, and then influence the length or line shape of nanowires and the formation of tubular morphology; the decrease of the sol pH value will cause AAO corrosion, because the preparation of longer nanowires needs to increase the sol pH value; The crystallization order of cobalt ferrite nanowires is increased by long calcining time, and the increase of calcining temperature not only improves the crystallization order of the cobalt ferrite nanowires, but also the partial Al~ (3+) is replaced by Fe~ (3+), which makes the co ferrite crystal cell parameters decrease.
The study results of cobalt ferrite nanowires / magnetic properties show that the increase of the length to diameter ratio of nanowire is beneficial to the saturation magnetization of cobalt ferrite nanowires M_s, the residual magnetization M_r, coercive force H_c, and the increase of the rectangular ratio P; the magnetic properties of cobalt ferrite nanotubes are better than the nanowires under the same diameter; calcining time and calcining temperature have a good effect on cobalt iron. The M_s, M_r, H_c and P of the oxygen nanowires also have obvious influence. The prolongation of calcining time increases M_s, M_r, H_c and P. The increase of calcination temperature makes M_s, M_r, H_c and P significantly increase. This is mainly attributed to the prolongation of calcining time or the increase of calcining temperature to increase or significantly increase the crystallinity of cobalt ferrite nanowires, and increase calcination. The temperature makes some Fe~ (3+) replaced by Al~ (3+), and then increases the magnetic properties of the ferrite nanowires. The results suggest that the influence of the shape anisotropy on the magnetic properties of cobalt ferrite can not be ignored when the magnetocrystalline anisotropy is fixed to a certain extent; moreover, the magnetic properties of the cobalt ferrite nanowires are compared with the length to diameter ratio, line or tubular morphology and the shape of the magnetic properties of the cobalt ferrite nanowires. The intrinsic relationship between the degree of crystallization and the degree of crystallization can be used to control the magnetic properties of cobalt ferrite nanowires by the influence of the preparation conditions on the length to diameter ratio, line or tubular morphology or the degree of crystal order of the cobalt ferrite nanowires.

【學(xué)位授予單位】：沈陽理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2010
【分類號】：TB383.1

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