發(fā)布時(shí)間：2018-12-15 00:29

【摘要】：具有結(jié)構(gòu)色的氧化物薄膜,由于其顏色鮮亮、飽和度高,環(huán)境友好和波長容易調(diào)控等特點(diǎn),在防偽、裝飾和傳感器等領(lǐng)域具有廣泛的應(yīng)用前景。其中,使用陽極氧化法制備該類氧化物薄膜具有制備工藝操作簡單、條件可控以及實(shí)際應(yīng)用范圍廣泛等突出的優(yōu)勢。例如陽極氧化鋁(PAA)薄膜,不僅具有可控的結(jié)構(gòu)色,還具有規(guī)則的六角密堆積狀孔洞分布,從而出現(xiàn)除結(jié)構(gòu)色之外的許多其他物性(如鐵磁性、阻變特性等)。研究發(fā)現(xiàn)這些特性與多孔結(jié)構(gòu)密切相關(guān),基于此,本文通過陽極氧化法制備出了具有有序多孔結(jié)構(gòu)的氧化鈮薄膜以及氧化鉭薄膜,并采用一系列測試表征手段對薄膜的結(jié)構(gòu)和物理性能進(jìn)行了研究。具體結(jié)果如下:(1)對預(yù)處理后的鈮金屬箔片,在室溫條件下經(jīng)由一次陽極氧化制備出了具有結(jié)構(gòu)色的氧化鈮薄膜,發(fā)現(xiàn)通過改變氧化電壓可以調(diào)控氧化鈮薄膜的飽和度和波長范圍,相同時(shí)間內(nèi),薄膜的厚度隨著氧化電壓的升高而增加。結(jié)合實(shí)驗(yàn)測試結(jié)果,對氧化鈮薄膜的顏色產(chǎn)生機(jī)理進(jìn)行了分析,發(fā)現(xiàn)當(dāng)薄膜的厚度小于150nm時(shí),結(jié)構(gòu)色由光的散射引起,符合補(bǔ)色原理;而當(dāng)薄膜的厚度大于150nm的時(shí)候,結(jié)構(gòu)色由光的干涉產(chǎn)生,滿足布拉格公式。(2)對一次陽極氧化法制備出的氧化鈮薄膜進(jìn)行二次陽極氧化,得到了有序多孔氧化鈮薄膜。實(shí)驗(yàn)發(fā)現(xiàn)在相同的時(shí)間內(nèi),隨著氧化電壓升高,孔的深度也隨之增加,同時(shí),薄膜的表面出現(xiàn)溝狀相連的現(xiàn)象。磁性測試結(jié)果發(fā)現(xiàn)不同條件下的多孔氧化鈮薄膜均表現(xiàn)為室溫鐵磁性,且其磁化強(qiáng)度均表現(xiàn)為M_⊥M_∥;空氣退火后,薄膜的磁化強(qiáng)度變化滿足M_(制備態(tài))M_(空氣退火2h)M_(空氣退火3h),這些現(xiàn)象表明了磁化強(qiáng)度的變化與薄膜中的氧空位有很大的關(guān)系。(3)室溫下采用二次陽極氧化法制備得到了一系列多孔氧化鉭薄膜,并對薄膜的結(jié)構(gòu)和性能進(jìn)行了表征。從表征結(jié)果發(fā)現(xiàn),多孔氧化鉭薄膜均表現(xiàn)為室溫鐵磁性,且薄膜的磁化強(qiáng)度都是M_⊥M_∥,不同氣氛下退火后,發(fā)現(xiàn)薄膜的磁化強(qiáng)度變化為M_(真空退火)M_(制備態(tài))M_空氣退火)。延長退火時(shí)間時(shí),薄膜的磁化強(qiáng)度滿足M_(制備態(tài))M_(空氣退火2h)M_(空氣退火4h),這些現(xiàn)象表明氧化鉭薄膜具有室溫鐵磁性,進(jìn)一步證明了薄膜的磁性與氧空位濃度有關(guān)。
[Abstract]:Because of its bright color, high saturation, friendly environment and easy wavelength control, oxide film with structural color has a wide application prospect in the field of anti-counterfeiting, decoration and sensor. Among them, the anodic oxidation method has the advantages of simple preparation process, controllable conditions and wide range of practical application. For example, the anodic alumina (PAA) film not only has controllable structure color, but also has regular hexagonal dense stacked pore distribution, which results in many other physical properties (such as ferromagnetism, resistive property, etc.) besides the structural color. It is found that these properties are closely related to porous structure. In this paper, niobium oxide and tantalum oxide thin films with ordered porous structure were prepared by anodizing method. The structure and physical properties of the films were studied by a series of measurement and characterization methods. The results are as follows: (1) niobium oxide films with structure color were prepared by one anodization at room temperature for the niobium foil. It is found that the saturation and wavelength range of niobium oxide films can be regulated by changing the oxidation voltage, and the thickness of niobium oxide films increases with the increase of oxidation voltage at the same time. Based on the experimental results, the color generation mechanism of niobium oxide film is analyzed. It is found that when the thickness of niobium oxide film is less than 150nm, the structure color is caused by light scattering, which conforms to the principle of complementary color. When the thickness of the film is larger than 150nm, the structure color is produced by interference of light, which satisfies the Bragg formula. (2) the ordered porous niobium oxide film is obtained by the secondary anodization of the niobium oxide film prepared by the primary anodizing method. It is found that the depth of the pore increases with the increase of the oxidation voltage at the same time, and the surface of the film is connected in a trench shape. The results of magnetic measurement show that the porous niobium oxide films exhibit ferromagnetism at room temperature under different conditions, and the magnetization of the films is M _ Karabakh M _ /; After air annealing, the magnetization changes of the films meet the requirements of M _ (prepared) M _ (air) annealing for 2h and M _ (air) annealing for 3 h. These phenomena indicate that the variation of magnetization is closely related to the oxygen vacancies in the films. (3) A series of porous tantalum oxide films have been prepared by secondary anodization at room temperature, and the structure and properties of the films have been characterized. The results show that the porous tantalum oxide films are ferromagnetic at room temperature, and the magnetization of the films is M _ 螕 M _ /. After annealing in different atmosphere, It is found that the magnetization of the films varies from M _ (vacuum annealing) M _ (prepared state to M _ air annealing). When the annealing time is prolonged, the magnetization of the film can meet the requirement of M _ (prepared state) M _ (air annealing for 2h) and M _ (air) annealing for 4h. These phenomena indicate that tantalum oxide films have ferromagnetic properties at room temperature. It is further proved that the magnetic properties of the films are related to the oxygen vacancy concentration.
【學(xué)位授予單位】：河北師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O484.1

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