射频反应磁控溅射法制备的氟化类金刚石薄膜摩擦特性研究

以高纯石墨做靶,CHF3和Ar气为源气体,采用射频反应磁控溅射法在不同流量比条件下制备了氟化类金刚石(F-DLC)薄膜.利用原子力显微镜、纳米压痕仪、拉曼光谱和红外光谱、摩擦磨损测试仪对薄膜的表面形貌、硬度、键结构以及摩擦性能做了具体分析.表面形貌测试结果表明,制备的薄膜整体均匀致密,表现出了良好的减摩性能.当CHF3与Ar气流量比r为1:6时,所得薄膜的摩擦系数减小至0.42,而纳米压痕结果显示,此时薄膜的硬度也最高.拉曼和红外光谱显示,随着r的增加,薄膜中的F浓度呈上升趋势,薄膜中的芳香环比例减小.研究表明,F原子的键入方式是影响F-DLC薄膜摩擦系数的一个重要因素,CF2反对称伸缩振动强度的减弱和CC中适量碳氢氟键的形成都能导致薄膜具有相对较低的摩擦系数.     

含氮氟化类金刚石(FN-DLC)薄膜的研究：(Ⅲ)疏水性能分析

不同沉积条件下，在单晶硅基底上沉积了含氮氟化类金刚石(FN-DLC)薄膜，用静滴接触角/表面张力测量仪测量了水与FN-DLC膜表面的接触角.用X射线光电子能谱、Raman光谱和傅里叶变换吸收红外光谱(FTIR)分析了薄膜的组分和结构.用原子力显微镜观测了薄膜的表面形貌.结果表明，FN-DLC薄膜疏水性能主要取决于薄膜表面的化学结构、薄膜表面极化强度的强弱、以及薄膜的表面粗糙度的大小.sp³/sp²的比值减小，CF₂基团含量增加，薄膜粗糙度增加，接触角增大；反之，则接触角减小.在工艺上，沉积温度和功率的减小，气体流量比r(r=CF4/［CF₄+CH₄］)的增加，都会使水的浸润性变差，接触角增大. 关键词： 氟化类金刚石膜 疏水性 接触角     

含氮氟化类金刚石(FN-DLC)薄膜的研究：(Ⅱ)射频功率对薄膜光学带隙的影响

以CF₄,CH₄和N₂为源气体，采用射频等离子体增强化学气相沉积法，在不同射频功率下制备了含氮氟化类金刚石薄膜样品.原子力显微形貌显示，低功率下沉积样品表面致密均匀.拉曼及傅里叶变换红外光谱分析显示，随着射频功率的改变，薄膜的结构和组分也随之变化.紫外-可见光透射光谱证明薄膜具有紫外强吸收特性，通过计算得到其光学带隙在1.89—2.29 eV之间.结果表明，射频功率增加，薄膜内sp²C含量增加，或者说C=C交联相对浓度增加、F的相对浓度降低，导致薄膜内π-π^*带边态密度增大，光学带隙减小. 关键词： 含氮氟化类金刚石薄膜 射频功率 光学带隙     

反应磁控溅射法制备的氟化类金刚石薄膜的XPS结构研究

采用射频反应磁控溅射法用高纯石墨作靶、三氟甲烷(CHF₃)和氩气(Ar)作源气体制 备了氟化类金刚石（FDLC）薄膜，通过XPS光谱结合拉曼光谱、红外透射光谱和紫外 可见光光谱研究了源气体流量比等工艺条件对薄膜中键结构、sp2/sp3杂化比以及光学带隙等性能的影响.结果表明在低功率(60W)、高气压(2.0Pa)和适当的流量比(Ar/CHF₃=2∶ 1)下利用射频反应磁控溅射法可制备出氟含量高且具有较宽光学带隙和超低介电常数的FDLC薄膜. 关键词： 反应磁控溅射 氟化类金刚石薄膜 红外透射光谱 XPS光谱     

源气体流量比对氟化类金刚石薄膜蛋白吸附能力的影响

用316L不锈钢(SU316L)作基片,以高纯石墨作靶、CHF₃和Ar作源气体,采用反应磁控溅射法在不同流量比R (CHF₃／Ar)下制备了氟化类金刚石(F-DLC)薄膜. 利用双蒸水液滴法、BCA(二喹啉甲酸)法和傅里叶红外光谱(FTIR)探讨了影响薄膜蛋白吸附能力的因素. 结果表明,镀有F-DLC薄膜的SU316L表面的血小板黏附量明显减少,血小板的变形程度显著减轻,相应的白蛋白与纤维蛋白原的吸附比普遍高于未镀膜的SU316L表面的相应值,说明镀上F-DLC薄膜可以改善样品的血液相容性. 流量比为2 ∶1左右时制备出的F-DLC薄膜,其白蛋白与纤维蛋白原的吸附比值达到最大,相应的血液相容性最佳. 对薄膜的接触角和表面能以及FTIR光谱分析研究表明,SU316L表面的F-DLC薄膜的白蛋白与纤维蛋白原的吸附比及血液相容性与薄膜的中的-CF_x键的含量(F/C比)和表面能(疏水性)直接相关,控制源气体流量比可以实现对薄膜的血液相容性的调制. 关键词： 反应磁控溅射 氟化类金刚石薄膜 蛋白吸附     

氟化类金刚石薄膜的拉曼和红外光谱结构研究

关键词：     

含氮氟化类金刚石(FN-DLC)薄膜的研究:(Ⅰ)sp结构与化学键分析

以CF4,CH4和N2为源气体,利用射频等离子体增强化学气相沉积法,在不同功率下制备了含氮氟化类金刚石膜.用俄歇电子能谱、拉曼光谱、X射线光电子能谱和傅里叶变换红外光谱对薄膜的电子结构和化学键进行了表征,并结合高斯分峰拟合方法分析了薄膜中sp2,sp3结构比率.结果表明,制备的薄膜属于类金刚石结构,不同沉积功率下,薄膜内的sp2/sp3值在2.0—9.0之间,随着沉积功率的增加薄膜内sp2的相对含量增加.膜内主要有C—Fx(x=1,2),C—C,CC和CN等化学键.沉积功率增加,C—C基团增加,膜内F的浓度降低,C—F基团减少,薄膜的关联加强,稳定性提高.     

含氮氟化类金刚石(FN-DLC)薄膜的研究：(Ⅰ) sp结构与化学键分析

以CF₄，CH₄和N₂为源气体，利用射频等离子体增强化学气相沉积法，在不同功率下制备了含氮氟化类金刚石膜.用俄歇电子能谱、拉曼光谱、X射线光电子能谱和傅里叶变换红外光谱对薄膜的电子结构和化学键进行了表征，并结合高斯分峰拟合方法分析了薄膜中sp²，sp³结构比率.结果表明，制备的薄膜属于类金刚石结构，不同沉积功率下，薄膜内的sp²/sp³值在2.0—9.0之间，随着沉积功率的增加薄膜内sp²的相对含量增加.膜内主要有C—F_x(x=1，2)，C—C，C=C和C≡N等化学键.沉积功率增加，C—C基团增加，膜内F的浓度降低，C—F基团减少，薄膜的关联加强，稳定性提高. 关键词： 含氮氟化类金刚石膜 sp结构 化学键结构 射频功率     

射频功率对类金刚石薄膜性能的影响

在不同射频功率条件下,实验研究了射频等离子体化学气相沉积类金刚石薄膜的金刚石相分数、光学常数和硬度。利用Raman光谱仪、椭圆偏振仪、数字式显微硬度计分别测试了不同条件下单层类金刚石薄膜的金刚石相分数、光学常数和硬度。实验表明,随着功率的增加,金刚石相的相对分数减少,薄膜的折射率先减小再增加然后减小,射频功率大于910 W时,沉积速率急剧增大。而薄膜的硬度先增加后减小,在射频功率为860 W处获得最大值。     

射频功率对类金刚石薄膜性能的影响

在不同射频功率条件下,实验研究了射频等离子体化学气相沉积类金刚石薄膜的金刚石相分数、光学常数和硬度。利用Raman光谱仪、椭圆偏振仪、数字式显微硬度计分别测试了不同条件下单层类金刚石薄膜的金刚石相分数、光学常数和硬度。实验表明,随着功率的增加,金刚石相的相对分数减少,薄膜的折射率先减小再增加然后减小,射频功率大于910 W时,沉积速率急剧增大。而薄膜的硬度先增加后减小,在射频功率为860 W处获得最大值。     

Al和Sb共掺对ZnO有序阵列薄膜的结构和光学性能的影响

采用水热合成法在预先生长的ZnO种子层的玻璃衬底上制备出Al和Sb共掺ZnO纳米棒有序阵列薄膜. 通过X射线衍射、扫描电镜、透射电镜和选区电子衍射分析表明:所制备的薄膜由垂直于ZnO种子层的纳米棒组成, 呈单晶六角纤锌矿ZnO结构, 且沿[001]方向择优生长, 纳米棒的平均直径和长度分别为27.8 nm和1.02 μm. Al和Sb共掺ZnO纳米棒有序阵列薄膜的拉曼散射分析表明:相对于未掺杂ZnO薄膜的拉曼振动峰(580 cm^-1), Al和Sb共掺ZnO阵列薄膜的E₁(LO)振动模式存在拉曼位移. 当Al和Sb的掺杂量为3.0at%,4.0at%,5.0at%,6.0at%时, Al和Sb共掺ZnO阵列薄膜的拉曼振动峰的位移量分别为3,10,14,12 cm^-1. E₁ (LO) 振动模式位移是由Al和Sb掺杂ZnO产生的缺陷引起的. 室温光致发光结果表明:掺杂Al和Sb后, ZnO薄膜在545 nm处的发光强度减小,在414 nm处的发光强度增加. 这是由于掺杂Al和Sb后, ZnO薄膜中Zn_i缺陷增加, O_i缺陷减少引起的. 关键词： Al和Sb共掺ZnO薄膜 纳米棒有序阵列 结构表征 拉曼散射     

Si(001)基片上反应射频磁控溅射ZnO薄膜的两步生长方法

利用反应射频磁控溅射技术，采用两步生长方法制备了ZnO薄膜，探讨了基片刻蚀时间和低温过渡层沉积时间对ZnO薄膜生长行为的影响.研究结果表明，低温ZnO过渡层的沉积时间所导致的薄膜表面形貌的变化与过渡层在Si(001)表面的覆盖度有关.当低温过渡层尚未完全覆盖基片表面时，ZnO薄膜的表面岛尺度较小、表面粗糙度较大，薄膜应力较大；当低温过渡层完全覆盖Si(001)基片后，ZnO薄膜的表面岛尺度较大、表面粗糙度较小，薄膜应力较小.基片刻蚀时间对薄膜表面形貌的影响与低温过渡层的成核密度有关.随着刻蚀时间的增加，ZnO薄膜的表面粗糙度逐渐下降，表面形貌自仿射结构的关联长度逐渐减小. 关键词： ZnO薄膜 反应射频磁控溅射 两步生长 形貌分析     

Ferromagnetism in Eu-doped ZnO films deposited by radio-frequency magnetic sputtering

This paper reports that Eu-doped ZnO films were successfully deposited on silicon (100) by radio-frequency magnetic sputtering. The x-ray diffraction patterns indicate that Eu substitutes for Zn in the lattice. Ferromagnetic loops were obtained by using superconducting quantum interference device at 10 K and room temperature. No discontinuous change was found in both of the zero-field-cooled and field-cooled curves. The observed ferromagnetism in Eu-doped ZnO can be attributed to a single magnetic phase. The saturation magnetisation decreased remarkably for the Eu-doped ZnO prepared by introducing 5% of oxygen in the sputtering gas or by the post annealing in O2, suggesting that the defects play key roles in the development of ferromagnetism in Eu-doped ZnO films.     

Influence of sulfidation treatment on the structure and tribological properties of nitrogen-doped diamond-like carbon films

The nitrogen-doped diamond-like carbon (DLC) films were deposited on high speed steel (HSS) substrates in the direct current unbalanced magnetron sputtering system. Sulphurized layer was formed on the surface of DLC films by means of liquid sulfidation in the intermixture of urea and thiourea solution in order to improve the tribological properties of DLC films. The influence of sulfidation treatment on the structure and tribological properties of DLC films was investigated in this work. The structure and wear surface morphology of DLC films were analyzed by Raman spectroscopy, XPS and SEM, respectively. It reveals that the treated films are smooth and uniform; and sulfur atoms are bonded chemically. The treated films have broader distribution of Raman spectra in the range of 1000-1800 cm⁻¹ and higher I_D/I_G ratio than the untreated films as a result of the appearance of the crystalline graphite structure after the sulfidation treatment. It is showed that the sp² relative content increase in the treated films from the XPS measurement. The Raman results are consistent with the XPS results. The tribological properties of DLC films were investigated using a ball-on-disk rotating friction and wear tester under dry friction conditions. It is found that the sulfidation concentration plays an important part in the tribological properties of the treated DLC films. The results showed the treated films with low sulfidation concentration have a lower friction coefficient (0.1) than the treated films with high sulfidation concentration (0.26) and the untreated films (0.27) under the same friction testing conditions, which can be attributed to both the presence of sulfur-containing materials and the forming of the mechanical alloyed layer on the wear surface. Adding the dry nitrogen to the sliding surface in the testing system helps the friction coefficient of the treated films with low sulfidation concentration to decrease to 0.04 further in this work. On the basis of the experimental results, it is indicated that the liquid sulfidation technique, which is low-cost, non-polluting and convenience, would be an appropriate method for the surface treatment of DLC films.     

Effect of substrate temperature on microstructure and optical properties of single-phased Ag20 film deposited by using radio-frequency reactive magnetron sputtering method

Using a radio-frequency reactive magnetron sputtering technique, a series of the single-phased Ag20 films are deposited in a mixture of oxygen and argon gas with a flow ratio of 2：3 by changing substrate temperature （Ts）. Effects of the Ts on the microstructure and optical properties of the films are investigated by using X-ray diffractometry, scanning electron microscopy and spectrophotometry. The single-phased Ag20 films deposited at values of Ts below 200℃ are （111） preferentially oriented, which may be due to the smallest free energy of the （111） crystalline face. The film crystallization becomes poor as the value of Ts increases from 100℃ to 225℃. In particular, the Ag20 film deposited at Ts=225℃ loses the （111） preferential orientation. Correspondingly, the film surface morphology obviously evolves from a uniform and compact surface structure to a loose and gullied surface structure. With the increase of Ts value, the transmissivity and the reflectivity of the films in the transparent region are gradually reduced, while the absorptivity gradually increases, which may be attributed to an evolution of the crystalline structure and the surface morphology of the films.     

蓝宝石基片的处理方法对ZnO薄膜生长行为的影响

采用反应射频磁控溅射方法，在经过不同方法处理的蓝宝石基片上，在同一条件下沉积了ZnO薄膜.利用原子力显微镜、X射线衍射、反射式高能电子衍射等分析技术，对基片和薄膜的结构、表面形貌进行了系统表征.研究结果显示，不同退火条件下的蓝宝石基片表面结构之间没有本质的差异，均为α-Al₂O₃ (001)晶面，但基片表面形貌的变化较大.在不同方法处理的蓝宝石基片上生长的ZnO薄膜均具有高c轴取向的织构特征，但薄膜的表面形貌差异较大.基片经真空退火处