自支撑金刚石膜的生长特征对断裂强度的影响

研究了自支撑今刚石膜的生长取向特征、表面形貌和质量对断裂强度的影响。X射线衍射和断裂强度的结果表明,随着衍射强度比值I(111)/I(220)的增大,断裂强度呈下降趋势。堆积在晶粒间界处的二次形核生长的小晶粒,覆盖晶粒间界的缝隙,在柱状晶粒间形成类似的搭桥效应,增强柱状晶之间的相互作用能,提高柱状晶结构的抗破断能力,金刚石膜中出现的非金刚石相将降低金刚石厚膜的断裂强度。     

不同靶基距下凹槽表面HIPIMS法制备钒膜的微观结构及膜厚均匀性

目的研究不同靶基距对高功率脉冲磁控溅射(HIPIMS)在凹槽表面制备钒膜微观结构和膜厚均匀性的影响,实现凹槽表面高膜层致密性和均匀性的钒膜制备。方法采用HIPIMS方法制备钒膜,在其他工艺参数不变的前提下,探讨不同靶基距对凹槽表面钒膜相结构、表面形貌及表面粗糙度、膜层厚度均匀性的影响。采用XRD、AFM及SEM等观测钒膜的表面形貌及生长特征。结果随着靶基距的增加,V(111)晶面衍射峰强度逐渐降低。当靶基距为12 cm时,钒膜膜层表面粗糙度最小,为0.434nm。相比直流磁控溅射(DCMS),采用HIPIMS制备的钒膜呈现出致密的膜层结构且柱状晶晶界不清晰。采用HIPIMS和DCMS方法制备钒膜时的沉积速率均随靶基距的增加而减少。当靶基距为8 cm时,采用HIPIMS方法在凹槽表面制备的钒膜均匀性最佳。结论采用HIPIMS方法凹槽表面钒膜生长的择优取向、表面形貌、沉积速率及膜厚均匀性均有影响。在相同的靶基距下,采用HIPIMS获得的钒膜膜厚均匀性优于DCMS方法。     

铝在高温水蒸气中表面氧化膜的性能

采用X射线衍射法(XRD)和扫描电镜(SEM)研究了纯铝在高温水蒸气中表面氧化膜的相组成及形貌特征.结果表明,本次实验条件下,在高温水蒸气中铝表面生成的是由一水软铝石AlO(OH)相组成的氧化膜,延长氧化时间氧化膜的相组成不发生改变,氧化膜表面的微观形态由微米数量级大小的颗粒构成,在一定临界值内,随着氧化时间延长,氧化膜厚度增加.     

磁控溅射法制备二氧化钒薄膜及其性能表征

采用射频反应磁控溅射法在镀有SiO2膜的钠钙硅玻璃基片上沉积了二氧化钒(VO2)薄膜.研究了在300℃沉积温度下,不同溅射时间(5～35min)对VO2薄膜结构和性能的影响.用X射线衍射、扫描电镜、自制电阻测量装置、紫外-可见光谱仪、双光束红外分光光度计对薄膜结构、形貌、电学及光学性能进行了表征.结果表明:薄膜在低温半导体相主要以四方相畸变金红石结构存在,在(011)方向出现明显择优取向生长,随着溅射时间的延长,晶粒生长趋于完整,晶粒尺寸增大;对溅射时间为35 min的薄膜热处理,发现从室温到90℃范围内,薄膜方块电阻的变化接近3个数量级;由于本征吸收,薄膜在可见光范围透过率较低,且随膜厚的增加而逐渐降低;在1500～4000 cm-1波数范围内,原位测量薄膜样品加热前后(20和80℃)的红外反射率,发现反射率的变化幅度随着膜厚增加而提高,最高可达59%.     

Preparation and Properties of GaN Micro-Ribbons on Ga-Diffused Si （111） Substrates

用射频磁控溅射工艺在室温扩镓硅衬底上沉积Ga2O3膜,然后在氨气气氛下氮化Ga2O3膜得到GaN微米带,用X射线衍射(XRD)、扫描电镜(SEM)、选区电子衍射(SAED)、X射线光电子能谱(XPS)及光致发光谱(PL)对薄膜样品进行了结构、表面形貌、组分及发光特性分析.SEM图像显示直径约为100 nm～300 nm微米带随机分布在GaN薄膜表面.XRD、XPS及SAED分析表明GaN微米带呈六方闪锌矿多晶结构,择优沿[001]方向生长.P1显示了可能由量子限制效应引起的发光峰,其相对于报道的GaN晶体发光峰有显著蓝移.     

镁合金挤压型材磷酸盐转化膜生长特征

利用磷酸盐溶液在AZ31镁合金挤压型材表面获得转化膜.用扫描电镜(SEM),X射线衍射(XRD)和质量损失检测等试验手段,对膜层生长和形貌特征进行了研究,对其表面膜层的成膜机理进行了探讨.结果表明,膜层生长初期基材腐蚀溶解迅速,质量损失超过整个损失的2/3;磷酸盐呈双膜层结构,底层为鳞片条带状相间分布,具有方向性.由于底层由微结构差异较大膜组成,这种微结构的差异使得两类膜之间结合处出现明显的狭缝, 成为影响底层膜耐蚀性的根本原因之一;基材的微观组织特点和化学状态直接影响底层膜层的生长特征.     

微/纳米复合多层金刚石自支撑膜的制备及应力研究

利用大功率DC Arc Plasma Jet CVD装置,采用Ar-H2-CH4混合气体为气源,通过优化工艺参数,在多晶钼衬底上制备出了多层复合金刚石自支撑膜.利用扫描电镜(SEM)、X射线衍射(XRD)、激光拉曼谱(Raman)对膜体进行表征,结果显示,多层膜体的组织结构体现了微米金刚石与纳米金刚石的典型特征;复合金刚石自支撑膜具有光滑的表面,微米层与纳米层间呈相互嵌套式的界面;此外,利用激光拉曼谱分析了多层膜中的内应力状态,研究发现,多层膜中各层膜体具有不同的内应力状态,内应力沿膜体生长方向有明显变化,呈现出从压应力到拉应力的变化过程.     

纳米金刚石膜真空窗口的制备

使用自制的微波等离子体化学气相沉积装置,以乙醇为碳源在（100）硅表面制备了金刚石膜;然后用浓硝酸和氢氟酸的混合溶液腐蚀硅,制备出金刚石膜窗口。使用场发射扫描电镜（SEM）、X射线衍射、拉曼光谱（Raman）、原子力显微镜（AFM）表征和分析金刚石膜,并以自制的漏气率测量系统测量金刚石膜窗口的漏气率。结果表明:金刚石膜的厚度为15 μm,平均粗糙度值R_a为39.5 nm,晶粒的尺寸大小为30 nm,漏气率为8.8×10-9 Pa·m3/s。      

磁控溅射铱薄膜的表面形态与取向演变的控制优化

目的 研究磁控溅射制备金属Ir膜的过程中溅射参数对Ir膜表面微结构和晶体质量的影响,制备高质量(100)取向的外延Ir膜,为单晶金刚石的异质外延生长奠定重要基础。方法 通过磁控溅射技术在单一改变参数(溅射功率、溅射厚度)的条件下制备金属Ir膜,通过分析原子力显微镜、扫描电子显微镜、X射线衍射、电子背散射衍射等测试结果,研究了各条件对所制备Ir膜粗糙度、表面形貌、晶体结构和取向的影响,并通过摇摆曲线衡量真空退火对薄膜晶体质量的优化效果。结果 在(100)MgO衬底上外延生长的Ir膜具有均匀的微结构,该结构由规则且紧密的矩形颗粒排列而成。薄膜表面微结构特征尺寸随溅射功率升高而逐渐减小;当功率为45 W时,Ir(200)X射线衍射峰强度最大、半高宽最宽;而随着厚度的增大,Ir(200)X射线衍射峰的半高宽及强度均增大。经优化的Ir膜表面光滑(Ra<0.5nm)、薄膜晶体质量高(θ_FWHM<0.5°)。结论 功率、厚度和退火处理都会影响薄膜晶体质量和表面微结构尺寸,合适的功率和厚度结合退火处理能获得具有特定表面微结构的高质量Ir膜。     

纯钛表面纳米化预处理对氧化膜结构的影响

采用快速多重旋转碾压(FMRR)技术对工业纯钛表面进行表面纳米化预处理,再通过微弧氧化技术在处理后的样品表层制备氧化膜。利用X射线衍射仪(XRD)、透射电镜(TEM)及扫描电镜(SEM)研究了FMRR处理后纯钛表层的微观结构及氧化膜的形貌。结果表明:FMRR处理后,纯钛的X射线衍射峰均发生明显的宽化,其主要原因是由于剧烈塑性变形导致晶粒细化及产生了微观应力所引起的;纯钛经过FMRR处理40 min后,最表层的平均晶粒被细化到大约10 nm。纳米化预处理使微弧氧化膜的孔洞减少、致密性提高,同时膜层的厚度也增加;当电流大小为3 A时,纳米纯钛表面制备的氧化膜的厚度达到38μm。     

Characterization of titanium nitride films deposited by cathodic arc plasma technique on copper substrates

TiN films were deposited directly on Cu substrates by a cathodic arc plasma deposition technique. The films were then characterized by X-ray diffraction (XRD), grazing incidence X-ray diffraction (GID), (TEM), Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS). The preferred orientation of the film changed from (200) to (111) with increasing film thickness. Analyses of both the XRD and GID results showed that in the highly (111) textured grains, the (111) plane was approximately parallel to the film surface, while in the (200) textured grains, the (200) plane was tilted away from the film surface. Small-elongated crystallites with a large aspect ratio and textured grains were found on the TiN surface. AES, which was employed to examine the concentration depth profile, showed no apparent interdiffusion between Cu and TiN during the growth of the film. XPS results showed that amorphous TiO₂, as well as titanium oxynitride, was present on the TiN surface. The spectra of Ti-2p, N-1s, O-1s and Cu-2p before and after the film being sputter etched through the entire film region were also discussed.     

Si基底磁控溅射制备CrN薄膜的表面形貌与生长机制

在Si基底上采用直流磁控溅射法制备CrN薄膜,利用原子力显微镜(AFM)、扫描电镜(SEM)和X射线衍射仪(XRD)分析薄膜表面形貌和物相成分,探讨薄膜生长的动力学过程.结果表明只有当生长时间足够(1800s)时,才能形成具有CrN相的薄膜.随着CrN薄膜的生长,薄膜表面晶粒由三棱锥发展为三棱锥与胞状共存状,薄膜表面粗糙度逐渐增大,动力学生长指数β=0.50.     

ZnO-TiO_2核壳纳米线结构及其热稳定性研究

采用热还原法和原子层沉积技术制备了ZnO-TiO_2核壳纳米线,研究沉积厚度、沉积温度及退火对于ZnO-TiO_2核壳纳米线晶化和结构的影响。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、高分辨率透射电镜(HRTEM)等手段对退火前后核壳纳米线进行表征。结果表明:沉积厚度和温度的增加有利于TiO_2壳层发生非晶向晶化的转变;500℃退火提高了TiO_2的结晶性,但可能会使细核壳纳米线(ZnO纳米线直径80 nm)产生波浪形变形,使150℃沉积的非晶TiO_2壳层形成凸出晶粒,并导致其界面处ZnO缺失。     

Microstructure and hardness of hollow cathode discharge ion-plated titanium nitride film

Titanium nitride (TiN) films were deposited on 304 stainless steel substrate by hollow cathode discharge (HCD) ion-plating technique. The preferred orientation and microstructure were studied by x-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. Microhardness of the TiN film was measured and correlated to the microstructure and preferred orientation. The results of TEM study showed that the microstructure of TiN film contains grains with nanometer scale. As the film thickness increases, the grain size of TiN increases. The x-ray results show that TiN(111) is the major preferred orientation of the film. The hardness of TiN film is primarily contributed from TiN(111) preferred orientation.     

Analysis of solid-liquid fluid dynamics about the characteristics of electrotyping diamond-nickel composite film

In this paper,super-thin free-standing diamond grains-nickel composite film in large area were prepared by using electrotyping method,which were used to make super-thin cutting blades.Scanning electron microscope(SEM) were used to analyse the characteristics of the film.It was found that the agitation velocity and the place of impeller strongly affected the content and uniformity of diamond grains in deposited composite film when the other parameters were the same.The best film was deposited when agitation velocity was 180-220 r/m and the impeller was placed in the lower part of the solution.The obliquity of cathode strongly affected the content of diamond grains in the film,and the content reached maximum when the obliquity was kept at 45 degree.The hanging orientation of cathode strongly affected the uniformity of the thickness of the film,and uniform films were deposited when cathode was intermissively circumrotated by 90 degree in the plane itself during deposition.The fluid field in solid-liquid stirred electrolytic solution was analysed by using Computational Fluid Dynamics(CFD).And the influences of agitation velocity, the place of impeller and the obliquity of cathode on the content of diamond grains in the film were explained.With Euler-Lagrange model,the just-suspended speed of impeller in solid-liquid stirred electrolytic tank was predicted by using Zwietering formula,the predicted speed was and it was consistent with experimental result.     

A comparative study of nanocrystalline Cu film deposited using anodic vacuum arc and dc magnetron sputtering

A comparative study of structural, electrical and thermoelectric properties of nanocrystalline copper thin films deposited using anodic vacuum arc plasma deposition technique and dc-magnetron sputtering is presented. The crystallographic texture and structural evolution of these films are investigated as a function of thickness within a range of 30 to 230 nm using XRD and SEM. AVA deposited Cu films possess smaller grains with a lesser degree of crystallinity than dc-sputtered ones. Electrical resistivity, temperature coefficient of resistance and thermoelectric power of both as-deposited and annealed Cu films of AVA and dc-magnetron sputtering is measured and their dependence on the film thickness is investigated. AVA deposited Cu films having thickness less than 100 nm show much higher resistivity than dc-sputtered ones. AVA deposited Cu films possess lower temperature coefficient of resistance values than dc-sputtered ones. The observed thickness dependence of thermoelectric power is larger in AVA deposited Cu films than in dc-sputtered ones. These electrical measurements reveal that AVA deposited Cu films possess more vacancies than dc-sputtered ones.     

Growth of Free-standing Diamond Films on Graphite Substrates with Ti Interlayers

DIAMOND has many remarkable chemical andphysical properties,such as extreme hardness,highthermal conductivity,high electrical resistively andexcellent optical transparency and so on.For diamond,approximately5.5ev is required to excite an electronfrom the valence band to the conduction band,compared with1.1ev for Si and0.7ev for Ge m.Therefore,Diamond is a wide band gap material.Furthermore,due to the high vibration energy of carbonatoms in diamond,the frequency of infrared absorptionis abn…     

共溅射氧化法制备掺钼VO_2及其相变特性

采用共溅射氧化法,在普通玻璃衬底上室温直流溅射沉积钒钼金属薄膜,再在大气环境下经热氧化处理获得掺钼VO2薄膜。通过XRD、SEM、热致相变电学特性等分析,研究制备工艺及掺杂改性对掺钼VO2薄膜的微结构、形貌、热滞回线和相变温度的影响。实验与分析结果表明,与相同厚度的纯VO2薄膜相比,钼掺杂显著改变了VO2薄膜的表面形貌特征,掺钼VO2薄膜呈多晶态且沿VO2(002)择优取向生长,结晶性和取向性明显提高,薄膜的相变温度降低至38℃,热滞回线宽度收窄约至8℃。低温共溅射氧化法制备的掺钼VO2薄膜的热阻效应明显,薄膜的金属-半导体相变特性良好。     

阴极弧径向不同位置膜层性能分布规律

利用阴极弧沉积的方法在201不锈钢基体上制备了TiN薄膜,研究了阴极弧径向不同位置大颗粒、膜厚以及膜层性能的分布规律.分别采用X射线衍射(XRD)和扫描电子显微镜(SEM)分析了膜层的相结构、膜层的表面形貌和截面形貌.研究了镀膜试样和基体在3.5%(质量分数)NaCl溶液中的腐蚀行为,并利用电化学方法分析其抗腐蚀性能,并采用球-盘式摩擦磨损、划痕测试以及微小压痕等方法测试了径向不同位置沉积的TiN薄膜摩擦磨损性能、膜基结合力以及硬度.结果表明,靠近靶材中心的位置,膜层的硬度、厚度最大,电化学腐蚀电位最高,在径向夹角20°处的膜层厚度、硬度最小.在靠近出气位置侧沉积的TiN薄膜大颗粒数目较多,造成表面缺陷增加,TiN薄膜的抗腐蚀性能下降.靠近弧源中心位置沉积的膜层摩擦磨损系数较大,两侧处的膜层摩擦系数较小,膜基结合力与表面形貌和膜层厚度有很大关系.     

Al2O3和Cr过渡层对Ag膜光学性质及其附着力的影响

研究了在玻璃基底上镀制Al2O3和Cr过渡层对Ag膜反射率及附着力的影响.分光光度计测试了Ag膜的反射率,结果表明,与Cr过渡层相比,Al2O3过渡层对Ag膜反射率的降低相对较小;而且,随着Al2O3厚度的增加,Ag膜的反射率先增大后减小.XRD与AES测试表明,引入Al2O3或Cr可明显细化Ag晶粒,减弱Ag膜(111)织构;Al2O3作过渡层时,Al原子向Ag层中扩散显著;而Cr作过渡层时,只有少量Cr原子扩散进入Ag层.因此,Al2O3作过渡层能显著增强薄膜与玻璃基体之间的附着力.