氧化铌（钽）薄膜的制备及表征
发布时间：2018-12-15 00:29
【摘要】：具有结构色的氧化物薄膜,由于其颜色鲜亮、饱和度高,环境友好和波长容易调控等特点,在防伪、装饰和传感器等领域具有广泛的应用前景。其中,使用阳极氧化法制备该类氧化物薄膜具有制备工艺操作简单、条件可控以及实际应用范围广泛等突出的优势。例如阳极氧化铝(PAA)薄膜,不仅具有可控的结构色,还具有规则的六角密堆积状孔洞分布,从而出现除结构色之外的许多其他物性(如铁磁性、阻变特性等)。研究发现这些特性与多孔结构密切相关,基于此,本文通过阳极氧化法制备出了具有有序多孔结构的氧化铌薄膜以及氧化钽薄膜,并采用一系列测试表征手段对薄膜的结构和物理性能进行了研究。具体结果如下:(1)对预处理后的铌金属箔片,在室温条件下经由一次阳极氧化制备出了具有结构色的氧化铌薄膜,发现通过改变氧化电压可以调控氧化铌薄膜的饱和度和波长范围,相同时间内,薄膜的厚度随着氧化电压的升高而增加。结合实验测试结果,对氧化铌薄膜的颜色产生机理进行了分析,发现当薄膜的厚度小于150nm时,结构色由光的散射引起,符合补色原理;而当薄膜的厚度大于150nm的时候,结构色由光的干涉产生,满足布拉格公式。(2)对一次阳极氧化法制备出的氧化铌薄膜进行二次阳极氧化,得到了有序多孔氧化铌薄膜。实验发现在相同的时间内,随着氧化电压升高,孔的深度也随之增加,同时,薄膜的表面出现沟状相连的现象。磁性测试结果发现不同条件下的多孔氧化铌薄膜均表现为室温铁磁性,且其磁化强度均表现为M_⊥M_∥;空气退火后,薄膜的磁化强度变化满足M_(制备态)M_(空气退火2h)M_(空气退火3h),这些现象表明了磁化强度的变化与薄膜中的氧空位有很大的关系。(3)室温下采用二次阳极氧化法制备得到了一系列多孔氧化钽薄膜,并对薄膜的结构和性能进行了表征。从表征结果发现,多孔氧化钽薄膜均表现为室温铁磁性,且薄膜的磁化强度都是M_⊥M_∥,不同气氛下退火后,发现薄膜的磁化强度变化为M_(真空退火)M_(制备态)M_空气退火)。延长退火时间时,薄膜的磁化强度满足M_(制备态)M_(空气退火2h)M_(空气退火4h),这些现象表明氧化钽薄膜具有室温铁磁性,进一步证明了薄膜的磁性与氧空位浓度有关。
[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.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O484.1
[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.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O484.1
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