溅射方法和基体材料对氧化钛薄膜微观结构的影响

发布时间：2018-02-04 20:42

本文关键词： 氧化钛薄膜高功率脉冲磁控溅射直流磁控溅射基体晶体结构化学价态　出处：《表面技术》2017年09期 　论文类型：期刊论文

【摘要】：目的研究不同溅射方法和基体材料对沉积氧化钛薄膜的晶体结构、化学价态、表面形貌的影响。方法采用高功率脉冲磁控溅射(HPPMS)和直流磁控溅射(DCMS)在316L不锈钢和硅片表面制备了氧化钛薄膜。采用等离子光发射谱检测了沉积薄膜时的等离子体特征。采用X射线衍射仪(XRD)、X射线光电子能谱(XPS)、原子力显微镜(AFM)和扫描电子显微镜(SEM),分别评价氧化钛薄膜的晶体结构、化学价态、晶粒尺寸和表面粗糙度。结果等离子体特征显示,沉积氧化钛薄膜时,HPPMS比DCMS具有更高的离化率和等离子体密度。XRD结果显示,在相同的平均溅射功率下,采用HPPMS和DCMS方法,均在不锈钢表面制备出纯金红石结构的氧化钛薄膜,而在硅片表面得到的氧化钛薄膜为金红石、锐钛矿混合结构,且采用HPPMS比DCMS技术制备的氧化钛薄膜含有更高的金红石含量。XPS结果显示,两种方法在所有基体表面均制备出了含有氧缺位的氧化钛薄膜。采用HPPMS和DCMS制备氧化钛薄膜时,不锈钢基体沉积的薄膜中,Ti3+/Ti4+比值均高于Si基体上的薄膜。SEM和硬度测试结果显示,HPPMS制备的氧化钛薄膜为等轴晶,晶粒较小,硬度较高。DCMS制备的氧化钛薄膜具有柱状晶的结构,晶粒较大。AFM的结果显示,采用不同溅射方法制备的氧化钛薄膜表面粗糙度没有明显差别。结论不同溅射方法和基体材料导致了薄膜沉积时样品表面离子轰击能量的差异,因此影响了氧化钛薄膜的晶体结构、化学价态和晶粒尺寸。
[Abstract]:Aim to study the crystal structure and chemical valence state of titanium oxide thin films deposited by different sputtering methods and substrate materials. Effect of Surface Morphology. Methods High Power Pulsed Magnetron sputtering (HPPMS) and DC Magnetron sputtering (DC MS). Titanium oxide thin films were prepared on 316L stainless steel and silicon substrates. Plasma characteristics of the deposited films were measured by plasma emission spectroscopy and X-ray diffractometer (XRD). X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and scanning electron microscopy (SEM) were used to evaluate the crystal structure and chemical valence state of titanium oxide films. Results Plasma characteristics showed that HPPMS had higher ionization rate and plasma density than DCMS. Under the same average sputtering power, pure rutile titanium oxide thin films were prepared on stainless steel by HPPMS and DCMS methods, while rutile films were obtained on silicon substrates. The anatase mixed structure and the results of HPPMS show that the titanium oxide films prepared by DCMS have higher rutile content. Titanium oxide thin films with oxygen vacancies were prepared on all substrates by both methods. The thin films deposited on stainless steel substrates were deposited by HPPMS and DCMS. The ratio of Ti3 / Ti _ 4 is higher than that on Si substrate. The results of hardness test show that the titanium oxide films prepared by Ti3 / Ti _ 4 are equiaxed and have smaller grain size. Titanium oxide thin films prepared with higher hardness. DCMS have columnar crystal structure. The results of larger grain size. AFM show that titanium oxide thin films with high hardness have a columnar structure. The surface roughness of titanium oxide films prepared by different sputtering methods has no obvious difference. Conclusion different sputtering methods and substrate materials lead to the difference of surface ion bombardment energy. Therefore, the crystal structure, chemical valence state and grain size of titanium oxide films are affected.
【作者单位】：西南交通大学材料科学与工程学院材料先进技术教育部重点实验室;西南交通大学物理科学与技术学院;
【基金】：国家自然科学基金项目(31300787,U1330113)~~
【分类号】：TB383.2;TQ134.11
【正文快照】： Received:2017-03-23;Revised:2017-05-02氧化钛薄膜具有良好的机械性能、化学稳定性和较好的生物相容性[1-4],可用于血管支架、人工心脏瓣膜等心血管材料的表面改性。氧化钛薄膜有无定形态以及金红石和锐钛矿两种晶体结构[5],金红石型氧化钛相比锐钛矿型氧化钛的热力学更加稳

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