PULSED LASER DEPOSITION OF DLC FILMS OVER LARGE AREA AND IT

利用脉冲激光沉积结合计算机辅助衬底扫描技术制备了 尺寸为70×66mm、均匀性为±5％的类金刚石薄膜,薄膜显微硬度最高为27GPa,薄 膜结合强度达到20000转;在制备大尺寸薄膜的过程中,衬底扫描速度越慢,薄膜的均匀性 越好;在应用传统清洗等方法的基础上,认为增大镀膜粒子的能量对于提高薄膜和衬底的结 合强度是非常重要的.     

直流反应磁控溅射在氮化的蓝宝石衬底上制备AlN薄膜

通过直流磁控反应溅射装置,在蓝宝石(0001)衬底和氮化的蓝宝石(0001)衬底上成功制备了氮化铝(AIN)薄膜。利用X射线衍射仪、原子力学显微镜和双光束扫描分光计,研究了蓝宝石氮化对AIN薄膜结构、应力、晶粒尺寸、形貌和光学性质的影响。X射线衍射研究表明:制备的AIN薄膜具有较强的(0002)择优取向,蓝宝石衬底的氮化不仅能够改善AIN结晶质量,而且还可以减少薄膜的残余应力。但是,原子力学显微镜结果表明:在蓝宝石衬底上制备的AIN薄膜的晶粒大小分布比在氮化的蓝宝石衬底上制备的AIN薄膜的晶粒大小分布更加均匀。我们认为,蓝宝石衬底在氮化的过程中形成的AIN具有过多的位错和缺陷,正是这些位错和缺陷造成了在氮化的蓝宝石衬底上制备的AIN薄膜的晶粒大小分布的不均匀性。吸收光谱显示:蓝宝石衬底的氮化并没有对AIN薄膜的光学性质产生明显的改善。     

YBCO大面积超导薄膜沉积工艺与微结构研究

采用中空柱状阴极直流磁控溅射方法制备了大面积ＹＢＣＯ超导薄膜。应用ＸＲＤ方法,对在３０×３０ｍｍ＾２ＬａＡｌＯ３衬底上沉积的ＹＢＣＯ薄膜进行了结晶完整性、均匀性的测定。对同一样品,使用透射电子显微镜对薄膜和衬底间的界面进行了研究。     

扫描电子显微镜法测定金属衬底上石墨烯薄膜的覆盖度

利用化学气相沉积法生长在金属衬底上的石墨烯薄膜,由于其尺寸的可控性和转移的便利性,被广泛用作各种透明电极.石墨烯薄膜的方块电阻是衡量其品质的重要指标之一,而石墨烯覆盖完全是保证薄膜拥有优良导电性能的基本前提.本文通过研究评估不确定度的分量,提出利用扫描电子显微镜像素计算微区和宏观覆盖度的方法.考虑到石墨烯薄膜覆盖区域与未覆盖区域边界的确定,以及晶畴数目的选取这两个因素对覆盖度测定造成的误差.通过微区有效扫描电子显微镜图像的确定、宏观石墨烯薄膜有效扫描电子显微镜图像的测量数目以及宏观石墨烯薄膜覆盖均匀性的表达,系统研究了化学气相沉积法生长在金属衬底上的石墨烯薄膜的微区覆盖度、宏观覆盖度和覆盖均匀性.该方法通过获得有限次微区扫描电子显微镜图像,不仅可以计算宏观石墨烯薄膜的覆盖度,还可以给出覆盖均匀性,既节省了测量时间,同时也能保证测量有效性.     

衬底温度对Al/Zn_3N_2薄膜制备的影响

运用等离子体发射光谱,分析衬底温度对氮化锌薄膜制备过程中各等离子体活性基团的影响,随着温度升高,N*2第一正系B3Πg→A3Σ+u,N*2第二正系C3Πu→B3Πg,N+*2第一负系B2Σ+u→X2Σ+g,Zn*以及Zn+*活性基团等离子体发射光谱特征谱线强度逐渐增强;由于衬底温度升高,腔室中各离子动能增加,使得碰撞电离加剧,导致N*2,N+*2,Zn*以及Zn+*活性基团的等离子体离子密度增加;等离子体发射光谱分析结果表明衬底温度在一定范围内升高有利于氮化锌薄膜生长。采用离子源辅助磁控溅射技术在Al薄膜上制备Zn3N2薄膜;X射线衍射图谱(XRD)分析结果表明:室温下,反应生长出单一择优取向面(321)氮化锌薄膜;随着温度的升高,在Al膜上反应生长的氮化锌薄膜择优取向面逐渐丰富,出现(222),(400),(600),(411),(332),(431)以及(622)择优取向面,体现出随着衬底温度的升高,薄膜的结晶度逐渐增加。XP-1台阶仪分析的结果表明,随着衬底温度的升高,氮化锌薄膜的沉积率逐渐增大。场效应扫描电子显微镜(SEM)图表明氮化锌薄膜晶粒尺寸随着衬底温度的升高逐渐变小,表面结构更加致密,晶粒排列更加有序;SEM断面扫描显示Al膜和氮化锌薄膜结合非常紧密。衬底温度影响薄膜性能实验分析结果与等离子体发射光谱分析的结果基本一致,体现出等离子体发射光谱了解等离子体内在特性的有效、快捷性。     

衬底温度对ZnMgO薄膜结构和光致发光性能的影响

利用超声喷雾热解方法以不同的沉积温度(450～550 ℃)在石英衬底上制备出一系列ZnMgO薄膜。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和光致发光谱(PL)表征了样品的晶体结构、表面形貌和光学性能。结果表明衬底温度对薄膜结构性能和光学特性影响显著。所有薄膜都呈六角纤锌矿多晶结构,其中在530 ℃条件下制备的样品C轴择优最明显,晶粒尺寸均匀,表面形貌平整,结晶质量最好。薄膜的光致发光谱显示随着温度的升高深能级跃迁范围逐渐减小,近紫外带边发光峰逐步出现。衬底温度为530 ℃时在374.5 nm处出现了明显的近紫外发光峰,且几乎没有明显的深能级跃迁出现。     

用磁控溅射法制备Cu薄膜的研究

采用磁控溅射法在玻璃衬底上制备了Cu薄膜 ,应用台阶仪测量Cu膜的厚度 ,研究了薄膜的沉积速率与溅射功率的关系 ;用X射线衍射 (XRD)和扫描电镜Cu对薄膜进行了表征 ,研究了溅射功率对所制备薄膜的影响。制备出致密性和均匀性较好的Cu薄膜。     

衬底温度对磁控溅射制备掺铝氧化锌薄膜的结构和光电性能的影响

利用射频磁控溅射在石英基片上沉积掺铝氧化锌薄膜,研究了衬底温度对薄膜结构和光电性能的影响.当给衬底加热时,X射线衍射观测(002)峰相对强度明显增强.在衬底温度250℃下制备的薄膜的晶粒尺寸最大,为24.9nm,表面粗糙度最小,为8.1nm,表明在衬底温度250℃下制备的薄膜的结晶效果最好.衬底温度从30℃升高到250℃,薄膜的电阻率相应地从14.35×10-4Ω·cm降低到7.18×10-4Ω·cm,随着衬底温度的升高,电阻率反而增大.所有样品在可见光区的平均光学透射率都大于85%.引入品质因子分析薄膜的光电性能,当衬底温度为250℃时,品质因子最大为16.15×10-3Ω-1,其光电性能最好.     

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利用微波电子回旋共振等离子体增强型化学气相沉积(ECR-PECVD)采用一步法直接在K9玻璃上低温沉积制备了多晶硅薄膜.研究了不同实验参数对薄膜沉积的影响,采用X射线衍射(XRD)、拉曼光谱、扫描电子显微镜(SEM)等实验分析方法对不同条件下制备的样品进行了晶体结构和表面形貌分析,并讨论了多晶硅薄膜沉积的最佳条件.实验结果表明,玻璃衬底上多晶硅薄膜呈柱状生长,并有一定厚度的非晶孵化层;较高氢气比例和衬底温度有利于结晶,薄膜的结晶率达到了62％;晶粒团簇的最大尺寸约为500nm.     

石英衬底上Au缓冲层对ZnO薄膜微结构的影响

采用单源化学气相沉积(SSCVD)法,在石英衬底上以Au为缓冲层,Zn4(OH)2(O2CCH3)6.2H2O为固相源制备ZnO薄膜。SEM和XRD测试ZnO薄膜的微结构,结果表明:相对于SiO2衬底上生长的ZnO薄膜,Au/SiO2衬底上生长的ZnO薄膜具有较好的结晶质量和表面平整度;对制备ZnO薄膜的衬底温度进行了工艺优化,结果表明:500℃时制备的ZnO薄膜颗粒大小均匀,结晶质量较好;通过荧光光谱仪对Au/SiO2衬底上的ZnO薄膜进行光致发光(PL)谱测试,ZnO薄膜在400nm出现紫光发射峰,而没有出现与缺陷相关的深能级发射峰,表明ZnO薄膜具有较好的结晶质量。     

Pulsed laser deposition and characterization of multilayer metal-carbon thin films

Cobalt-DLC multilayer films were deposited with increasing content of cobalt, keeping carbon content constant by pulsed laser deposition technique. A cobalt free carbon film was also deposited for comparison. Excimer laser was employed to ablate the materials onto silicon substrate, kept at 250 °C, while post-deposition annealing at 400 °C was also performed in situ. The formation of cobalt grains within the carbon matrix in Co-DLC films can be seen through scanning electron and atomic force micrographs while no grains on the surface of the cobalt-free DLC film were observed. Raman spectra of all the films show D- and G-bands, which is a confirmation that the films are DLC in nature. According to Vibrating sample magnetometer (VSM) measurements, the DLC films with cobalt revealed ferromagnetic behaviour whereas the cobalt free DLC film exhibited diamagnetic behaviour. The pure DLC film also shows ferromagnetic nature when diamagnetic background is subtracted. Spectroscopic Ellipsometry (SE) analysis showed that the optical band gaps, refractive indices and extinction coefficients of Co-DLC films can be effectively tuned with increasing content of cobalt.     

飞秒激光制备硅窗口增透保护类金刚石膜

采用飞秒激光(800 nm,120 fs,3 W,1 000 Hz)制备类金刚石膜,研究了不同偏压、生长温度和氧气氛等辅助手段对激光沉积类金刚石膜的影响,实验发现在室温(25℃)、无偏压和低气压氧气氛(2 Pa)条件下沉积的类金刚石膜性能最优。在单面预镀普通增透膜的硅红外窗口材料上镀制出了无氢类金刚石膜,3~5μm波段平均透过率达到90%以上,纳米硬度高达40 GPa,用压力为9.8 N的橡皮磨头,摩擦105次,膜层未见磨损,并且通过了军标规定的高温、低温、湿热、盐雾等环境试验,所制类金刚石膜可对红外窗口起到较好的增透保护作用。     

Effect of substrate morphology on the roughness evolution of ultra thin DLC films

The effect of substrate roughness on growth of ultra thin diamond-like carbon (DLC) films has been studied. The ultra thin DLC films have been deposited on silicon substrates with initial surface roughness of 0.15, 0.46 and 1.08 nm using a filted cathodic vacuum arc (FCVA) system. The films were characterized by Raman spectroscope, transmission electron microscope (TEM) and atomic force microscopy (AFM) to investigate the evolution of the surface roughness as a function of the film thickness. The experimental results show that the evolution of the surface morphology in an atomic scale depends on the initial surface morphology of the silicon substrate. For smooth silicon substrate (initial surface roughness of 0.15 nm), the surface roughness decreased with DLC thickness. However, for silicon substrate with initial surface roughness of 0.46 and 1.08 nm, the film surface roughness decreased first and then increased to a maximum and subsequently decreased again. The preferred growth of the valley and the island growth of DLC were employed to interpret the influence of substrate morphology on the evolution of DLC film roughness.     

激光制备类金刚石膜技术研究

现有技术制备的类金刚石(DLC)膜由于含氢、硬度低、内应力大、附着力差等特点,严重限制了其光学工程应用.激光法是近年发展的一种制备DLC膜的新方法,相比其他制备方法具有诸多优点.综合分析了激光制备DLC膜过程中,激光波长、脉宽、功率密度、衬底温度和偏压等因素对薄膜质量的影响规律.采用氧气氛辅助沉积、元素掺杂和双波长激光...     

脉冲偏压电弧离子镀C-N-V薄膜的成分、结构与性能

用脉冲偏压电弧离子镀方法在硬质合金基体上制备了一系列不同成分的C-N-V薄膜.用X射线光电子能谱、激光Raman光谱、 X射线衍射(XRD)、透射电子显微镜(TEM)和纳米压痕等方法分别研究了薄膜的成分、结构与性能.Raman光谱,XRD和TEM结果表明,所制备的薄膜为在类金刚石(DLC)非晶基体上匹配有VN晶体的碳基复合薄膜.随V和N含量的增加,薄膜硬度与弹性模量先增加后下降,在N含量为204%,V含量为218%时薄膜硬度与弹性模量具有最大值,分别为368和5697 GPa,高于相同条件下制备的 关键词： C-N-V薄膜 类金刚石薄膜 纳米复合薄膜 电弧离子镀     

UBMS技术制备DLC薄膜的光学常数椭偏分析

采用宽光谱变角度椭圆偏振仪对非平衡磁控溅射（UBMS）技术沉积的类金刚石（DLC）薄膜的光学常数进行了测量与分析。在建立模型时,根据DLC薄膜成膜特性,分析和调整了模型结构;综合考虑了表面粗糙度、薄膜与基底表面及界面因素对测试结果的影响,将表面层和界面层分离出来,并采用有效介质方法对它们的影响作了近似处理。结果表明：硅基底上采用UBMS技术制备DLC薄膜的椭偏数据,经该模型拟合后均方误差（MSE值）从37.39下降到4.061,提高了测量精度。     

激光加速实验超薄类金刚石碳靶的制备

采用过滤阴极真空弧法,制备了满足激光稳相加速机制要求的超薄自支撑类金刚石碳靶。室温下沉积,基片偏压为-32 V,薄膜沉积速率约为每脉冲0.002 nm。选取NaCl膜作脱膜剂,采用漂浮法进行脱膜。打捞板孔径为1 mm时,自支撑厚度范围为5~50 nm,自支撑成功率约为70%。利用拉曼光谱仪及原子力显微镜等仪器,测量了薄膜的结构、表面粗糙度等关键参数。     

The protective properties of ultra-thin diamond like carbon films for high density magnetic storage devices

With the increase of magnetic storage density, the thickness of the protective diamond like carbon (DLC) film on the surfaces of head and disk is required as thin as possible. In this paper, the structure, mechanical properties and corrosion and oxidation resistance of ultra-thin DLC films are investigated. The ultra-thin DLC films were deposited by using filtered cathodic vacuum arc (FCVA) technique. The exact thickness of the ultra-thin DLC film was determined by high resolution transmission electron microscope (HRTEM). Raman analysis indicates that the ultra-thin DLC film presents ta-C structure with high sp³ fraction. In the wear test, a diamond tip was used to simulate a single-asperity contact with the film surface and the wear marks were produced on the film surface. The wear depths decrease with film thickness increasing. If the film thickness was 1.4 nm or above, the wear depth was much lower than that of Si substrate. This indicates that the ultra-thin DLC film with thickness of 1.4 nm shows excellent wear resistance. Corrosion tests in water and oxidation tests in air were carried out to investigate the diffusion barrier effect of the ultra-thin DLC films. The results show that the DLC film with thickness of 1.4 nm provides adequate coverage on the substrate and has good corrosion and oxidation resistance.     

Tribological properties of diamond-like carbon films deposited by pulsed laser arc deposition

A novel method, pulsed laser arc deposition combining the advantages of pulsed laser deposition and cathode vacuum arc techniques, was used to deposit the diamond-like carbon (DLC) nanofilms with different thicknesses. Spectroscopic ellipsometer, Auger electron spectroscopy, x-ray photoelectron spectroscopy, Raman spectroscopy, atomic force microscopy, scanning electron microscopy and multi-functional friction and wear tester were employed to investigate the physical and tribological properties of the deposited films. The results show that the deposited films are amorphous and the sp$^{2}$, sp$^{3}$ and C--O bonds at the top surface of the films are identified. The Raman peak intensity and surface roughness increase with increasing film thickness. Friction coefficients are about 0.1, 0.15, 0.18, when the film thicknesses are in the range of 17--21~nm, 30--57~nm, 67--123~nm, respectively. This is attributed to the united effects of substrate and surface roughness. The wear mechanism of DLC films is mainly abrasive wear when film thickness is in the range of 17--41~nm, while it transforms to abrasive and adhesive wear, when the film thickness lies between 72 and 123~nm.     

Transmission electron microscopy study of epitaxial La0.8MnO3 thin films on SrTiO3

The structure and microstructure of La_0.8MnO₃ thin films on SrTiO₃ substrates, fabricated by pulsed laser deposition at substrate temperatures of 873?K and 1073?K, have been studied by transmission electron microscopy. In both films, columnar growth morphology has been observed. The columnar grain size is found to increase with increasing substrate temperature. In the film deposited at a substrate temperature of 1073?K, there is only one rhombohedral phase. However, two phases, a rhombohedral one and an orthorhombic one, have been observed in the film deposited at 873?K.