衬底温度对PLD制备的Mo薄膜结构及表面形貌的影响

运用脉冲激光沉积(PLD)技术在Si(100)基片上沉积了金属Mo薄膜。在激光重复频率2 Hz,能量密度5.2 J/cm2,本底真空10－6 Pa的条件下,研究Mo薄膜的结构和表面形貌,讨论了衬底温度对薄膜形貌与结构的影响。原子力显微镜(AFM)图像和X射线小角衍射(XRD)分析表明,薄膜表面平整、光滑,均方根粗糙度小于2 nm。沉积温度对Mo薄膜结构和表面形貌影响较大,在373~573 K范围内随着温度升高,薄膜粗糙度变小,结晶程度变好。     

NaF薄膜的脉冲激光沉积法制备与结构研究

 采用脉冲激光沉积(PLD)方法在Si(100)衬底上制备了NaF薄膜。在激光重复频率2 Hz,能量密度3 J/cm²,本底真空度5×10^-5 Pa的条件下,研究衬底温度对薄膜沉积速率及结构的影响。台阶仪分析表明：薄膜的沉积速率随衬底温度增加呈指数函数增加,算出NaF薄膜的反应激活能为48.67 kJ/mol。原子力显微镜分析表明：薄膜致密而光滑,均方根粗糙度为0.553 nm。扫描电镜截面微观形貌分析表明：薄膜呈现柱状结构。X射线衍射分析表明：NaF薄膜为面心立方晶体结构,并具有显著的择优取向;当衬底温度约为400 ℃时,平均晶粒尺寸最大(129.6 nm),晶格微应变最小(0.225%)。     

氩离子轰击对四面体非晶碳膜内应力和摩擦系数影响的研究

利用磁过滤真空阴极电弧技术制备了sp³键大于80%的四面体非晶碳(ta-C)薄膜, 通过冷阴极离子源产生keV能量的氩离子轰击ta-C薄膜,研究了氩离子轰击能量对ta-C薄膜结构, 内应力以及耐磨性的影响.通过X射线光电子能谱和原子力显微镜研究了氩离子轰击对薄膜结构 与表面形貌的改性,研究表明,氩离子轰击诱导了ta-C薄膜中sp³键向sp²键的转化, 并且随着氩离子轰击能量的增大,薄膜中sp²键的含量逐渐增多, 薄膜内应力随着氩离子轰击能量的增大逐渐减小.氩离子轰击对薄膜的表面形貌有较大影响, 在薄膜表面形成刻蚀坑,并且改变了薄膜的表面粗糙度,随着氩离子轰击能量的增大, 薄膜的表面粗糙度也会逐渐增大.通过摩擦磨损仪的测试结果,氩离子轰击对薄膜的初始摩擦系数影响较大, 但是对薄膜的稳定摩擦系数影响较小,经过氩离子轰击前后的ta-C薄膜的摩擦系数为0.1左右, 并且具有优异的耐磨性.     

Ho3+掺杂对ZnO薄膜的微观结构和磁性的影响

研究Ho³⁺掺杂对氧化锌半导体材料的微结构和磁学性质影响. 利用热蒸发技术制备了一系列沉积在Si(100)衬底的Zn_1-xHo_xO(x=0.0、0.04、0.05）薄膜. X射线光谱、表面形貌以及磁性的实验结果表明,Ho³⁺掺杂对ZnO薄膜材料的性能影响很大. X射线衍射图显示峰位出现高角度转变并且趋向于(101)取向,在ZnO晶格显示Ho³⁺置换. 扫描电子显微镜和能谱仪对薄膜的表面形貌以及化学     

非平衡磁控溅射制备类石墨碳膜及性能研究

利用中频非平衡磁控溅射技术在单晶硅基底上沉积了类石墨碳膜, 采用Raman光谱、高分辨透射电子显微镜、原子力显微镜分析了薄膜微观结构和表面形貌; 采用纳米压痕仪和CSM摩擦磨损试验机测试了碳膜力学性能和摩擦学性能. 结果表明: 利用中频非平衡磁控溅射技术沉积的碳膜是一种以sp²键合碳为主、结构非晶、硬度适中、应力较低、表面粗糙度较大、摩擦性能优异的薄膜. 脉冲占空比对薄膜微观结构和性能有显著影响, 随着脉冲占空比的增大, Raman光谱D峰和G峰的强度比I_D/I_G先减小后增大, 而硬度随脉冲占空比的增大却呈现出相反的变化趋势, 即先增大后减小; 大气氛围中的摩擦性能测试表明, 本实验制备的薄膜具有优异的抗磨性能(～10^-11 cm³/N^-1. m^-1)和承载能力(～2.5 GPa). 随脉冲占空比的增大, 薄膜摩擦系数变化甚微而磨损率却呈现先显著减小后轻微增大的变化趋势. 类石墨碳膜优异的摩擦学性能主要归因于其独特的结构、较低的内应力及良好的结构稳定性.     

CHN薄膜的制备方法与工艺研究

 采用空心阴极等离子化学气相沉积方法，以NH₃/H₂的混合气体及CH4气体为原料反应气体，成功地制备了非晶的CHN薄膜，研究了CHN薄膜的沉积速率与直流电压及反应气体流量的关系。同时用X射线光电子能谱(XPS)确定了不同条件下薄膜中N原子的百分比，用原子力显微镜(AFM)对薄膜的表面粗糙度及表面形貌进行了测量和表征。结果表明：薄膜中N原子的百分比最大为12%，薄膜的表面结构光滑、致密，表面粗糙度小于1 nm。     

物理法和化学法制备的单层ZrO2膜的激光损伤行为差异

 分别采用电子束热蒸发技术和溶胶-凝胶技术在K9基片上镀制了光学厚度相近的ZrO₂单层薄膜,测试了两类薄膜的激光损伤阈值。分别采用透射式光热透镜技术、椭偏仪、原子力显微镜和光学显微镜研究了两类薄膜的热吸收、孔隙率、微观表面形貌、激光辐照前薄膜的杂质和缺陷状况以及激光辐照后薄膜的损伤形貌。实验结果表明：两类薄膜的不同损伤形貌与薄膜的热吸收与微观结构有关， 物理法制备的ZrO₂膜结构致密紧凑，膜层的杂质和缺陷多；化学法制备的ZrO₂膜结构疏松多孔，膜层纯净杂质少，激光损伤阈值达26.9 J/cm²；因物理法制备的ZrO₂膜拥有更大的热吸收(115.10×10^-6)和更小的孔隙率(0.20)，其激光损伤阈值较小(18.8 J/cm²)，损伤主要为溅射和应力破坏，而化学法制备的ZrO₂膜的损伤主要为剥层。理论上对实验结果进行了解释。     

电化学方法制备ZnO纳米颗粒掺杂类金刚石薄膜及其场发射性能研究

采用液相电化学沉积技术制备了ZnO纳米颗粒掺杂的类金刚石(DLC)薄膜, 研究了ZnO纳米颗粒掺杂对DLC薄膜场发射性能的影响. 利用X射线光电子能谱、透射电子显微镜、Raman光谱以及原子力显微镜分别对薄膜的化学组成、 微观结构和表面形貌进行了表征. 结果表明: 薄膜中的ZnO纳米颗粒具有纤锌矿结构, 其含量随着电解液中Zn源的增加而增加. ZnO纳米颗粒掺杂增强了DLC薄膜的石墨化和表面粗糙度. 场发射测试表明, ZnO纳米颗粒掺杂能提高DLC薄膜的场发射性能, 其中Zn与Zn+C的原子比为10.3%的样品在外加电场强度为20.7 V/μm时电流密度达到了1 mA/cm². 薄膜场发射性能的提高归因于ZnO掺杂引起的表面粗糙度和DLC薄膜石墨化程度的增加.     

α-C:H膜表面形貌及光学性能的测试分析

 以H₂和反式-2-丁烯（T₂B）为工作气体,利用低压等离子体增强化学气相沉积法制备了α-C:H薄膜。采用原子力显微镜、扫描电镜测试了α-C:H薄膜的表面形貌,分析了实验参数对其形貌的影响。研究表明：固定压强(15 Pa),当T₂B/H₂流量比为4时,薄膜均方根粗糙度可达0.97 nm。保持T2B/H2流量比固定,增加工作气压,薄膜均方根粗糙度减小,表面更平整、致密。利用傅里叶变换红外光谱仪对薄膜价键结构进行分析,结果表明：α-C:H薄膜中主要存在sp3C—H键,氢含量较高;T₂B/H₂流量比越低,薄膜中含有更多的C=C键。应用UV-VIS光谱仪,获得了波长在200～1 100 nm范围内薄膜的光吸收特性,α-C:H薄膜透过率可达98%,计算得到的折射率在1.16～1.40。随工作气压的增加,α-C:H薄膜中sp³杂化键增多,透过率、折射率增大。     

衬底温度对类金刚石薄膜力学性能的影响

 采用脉冲激光沉积方法在不同衬底温度下制备了最高硬度与弹性模量分别达45 GPa和290 GPa,且表面十分光滑的类金刚石薄膜。在相对湿度为80%的条件下,薄膜最低的摩擦系数与磨损率分别为0.045与5.74×10^-10 mm³·N^-1·m^-1。实验结果表明,硬度与弹性模量随衬底温度升高而降低,摩擦系数与磨损率随衬底温度升高而增大。拉曼光谱表明:在室温下制备的薄膜为典型类金刚石结构,sp³含量高达76.8%,而随温度升高,薄膜结构逐渐经无定形碳结构向纳米晶石墨结构方向发展,sp³含量也随之降低,力学性能变差。     

Microstructural and optical properties of nanocrystalline undoped zirconia thin films prepared by pulsed laser deposition

The zirconium oxide (ZrO₂) thin films are deposited on Si (100) and quartz substrates at various substrate temperatures (room temperature–973 K) at an optimized oxygen partial pressure of 3×10^?2 mbar using pulsed laser deposition technique. The effect of substrate temperature on microstructural, optical and mechanical properties of the films is investigated. The X-ray diffraction studies show that the films deposited at temperatures ≤773 K are monoclinic, while the films deposited at temperatures ≥873 K show both monoclinic and tetragonal phases. Tetragonal phase content increases with the increase of substrate temperatures. The surface morphology and roughness are investigated using atomic force microscope in contact mode. The optical properties of the films show that the refractive indices (at 550 nm) are found to increase from 1.84 to 2.35 as the temperature raises from room temperature (RT) to 973 K. Nanoindentation measurements show that the hardness of the films is 11.8 and 13.7 GPa for the films deposited at 300 and 973 K, respectively.     

Structural characterization and optoelectronic properties of GaN thin films on Si(111) substrates using pulsed laser deposition assisted by gas discharge

GaN films have been grown on Si(111) substrates with a thin AlN buffer layer using pulsed laser deposition (PLD) assisted by gas discharge. The crystalline quality, surface morphology and optoelectronic properties of the deposited films were characterized by X-ray diffraction (XRD), atomic force microscopy (AFM), photoluminescence (PL) spectroscopy, and room-temperature Van der Pauw–Hall measurements. The influence of the deposition temperature in the range 637–1037 K on the crystallinity of GaN films, the laser incident energy in the range 150–250 mJ/pulse on the surface morphology and the optoelectronic properties were systematically studied. The XRD analysis shows that the crystalline quality of the GaN films improves with increasing deposition temperature to 937 K, but further increase of the deposition temperature to 1037 K leads to the degradation of the crystalline quality. AFM results show that the surface roughness of the GaN films can be decreased with increasing laser incident energy to 220 mJ/pulse. Further increase of the laser incident energy to 250 mJ/pulse leads to an increase in the surface roughness. The optoelectronic properties of GaN films were also improved by increasing the laser incident energy to 220 mJ/pulse. GaN films which have a n-type carrier concentration of 1.26×10¹⁷ cm^-3 and a mobility of 158.1 cm²/Vs can be deposited at a substrate temperature of 937 K, a deposition pressure of 20 Pa and a laser incident energy of 220 mJ/pulse. Their room-temperature PL spectra exhibit a strong band-edge emission at 365 nm. PACS 81.15.Fg; 81.05.Ea; 78.20.-e; 73.61.Ey; 78.66.Fd     

Deposition of aluminum nitride thin film on Si(1 1 1) by KrF excimer laser and its characterizations

We present the deposition of aluminum nitride (AlN) thin film by KrF excimer laser sputtering and the study of the effects of substrate temperature and laser fluences. Deposition rate of AlN thin film at 0.3 Å/pulse has been achieved with laser fluence of 1500 mJ/cm² and at substrate temperature of 250 K, and this shows the enhancement of the deposition rate at low substrate temperature. Surface morphology of the deposited films is characterized by atomic force microscopy (AFM). In addition, the electrical performance of the MIS devices with AlN thin films prepared in this experiment has been characterized.     

Structural, electrical, and surface characteristics of La0.5Sr0.5CoO3 thin films prepared by pulsed-laser deposition

A parametric study of the growth of La_0.5Sr_0.5CoO₃ (LSCO) thin films on (100) MgO substrates by pulsed-laser deposition (PLD) is reported. Films are grown under a wide range of substrate temperature (450–800 °C), oxygen pressure (0.1–0.9 mbar), and incident laser fluence (0.8–2.6 J/cm²). The optimum ranges of temperature, oxygen pressure, and laser fluence to produce c-axis oriented films with smooth surface morphology and high metallic conductivity are identified. Films deposited at low temperature (500 °C) and post-annealed in situ at higher temperatures (600–800 °C) are also investigated with respect to their structure, surface morphology, and electrical conductivity. Received: 20 November 1998 / Accepted: 6 July 1999 / Published online: 21 October 1999     

Gas sensing properties of nanostructured MoO3 thin films prepared by spray pyrolysis

Thin films of molybdenum trioxide (MoO₃) were deposited on common glass using the chemical spray pyrolysis technique. A (NH₄)₆Mo₇O₂₄4H₂0 solution 0.1 M was used as the precursor one. The influence of substrate temperature on the crystallographic structure, surface morphology and electrical behavior of MoO₃ thin films was studied. MoO₃ can exist in two crystalline forms, the thermodynamically stable orthorhombic α-MoO₃ and the metastable monoclinic β-MoO₃ phase. XRD-spectra showed a growth of α-MoO₃ phase percentage as substrate temperature increases from 420 K up to 670 K. Films deposited in the 500–600 K range have a clearly porous surface structure of nanometer order as can be seen in SEM images. Changes up to six magnitude orders were observed in MoO₃ thin films electrical resistance when films temperature varied from 100 K up to 500 K. The sensing property of these MoO₃ films was also studied. The sensitivity was investigated in the temperature range 160 and 360 K for H₂O and CO gases, respectively. Both of them are of reducing nature. In all studied cases sensitivity decreases slowly as film temperature is raised. At room temperature the sensitivity changes from 12 up to 75% depending on substrate temperature. The sensitivity for CO gas was found to be lower than that of H₂O.     

Radio-frequency assisted pulsed laser deposition of nanostructured WOx films

The synthesis of tungsten oxide films with large surface area is promising for gas sensing applications. Thin WO_x films were obtained by radio-frequency assisted pulsed laser deposition (RF-PLD). A tungsten target was ablated at 700 and 900 Pa in reactive oxygen, or in a 50% mixed oxygen-helium atmosphere at the same total pressure values. Corning glass was used as substrate, at temperatures including 673, 773 and 873 K. Other deposition parameters such as laser fluence (4.5 J cm⁻²), laser wavelength (355 nm), radiofrequency power (150 W), target to substrate distance (4 cm), laser spot area (0.7 mm²), and number of laser shots (12,000) were kept fixed. The sensitivity on the deposition conditions of morphology, nanostructure, bond coordination, and roughness of the obtained films were analyzed by scanning and transmission electron microscopy, micro-Raman spectroscopy, and atomic force microscopy.     

Synthesis by pulsed laser ablation in Ar and SERS activity of silver thin films with controlled nanostructure

Thin silver films were deposited by pulsed laser ablation in a controlled Ar atmosphere and their SERS activity was investigated. The samples were grown at Ar pressures between 10 and 70 Pa and at different laser pulse numbers. Other deposition parameters such as laser fluence, target to substrate distance and substrate temperature were kept fixed at 2.0 J/cm², 35 mm and 297 K. Film morphologies were investigated by scanning and transmission electron microscopies (SEM, TEM). Surface features range from isolated nearly spherical nanoparticles to larger islands with smoothed edges. Cluster growth is favored by plume confinement induced by background gas. After landing on the substrate clusters start to aggregate giving rise to larger structures as long as the deposition goes on. Such a path of film growth allows controlling the surface morphology as a function of laser pulse number and Ar pressure. These two easy-to-manage process parameters control the number density and the average size of the as-deposited nanoparticles. We investigated the influence of substrate morphologies on their surface enhanced Raman scattering properties. Raman measurements were performed after soaking the samples in rhodamine 6G aqueous solutions over the concentration range between 1.0 × 10⁻⁴ and 5.0 × 10⁻⁸ M. The sensitivity of the film SERS activity on the surface features is put into evidence.     

Crystalline and photoluminescence characteristics of YVO4:Sm thin films grown by pulsed laser deposition under oxygen pressure

YVO₄:Sm³⁺ films were deposited on Al₂O₃ (0 0 0 1) substrates at various oxygen pressures changing from 13.3 to 46.6 Pa by using the pulsed laser deposition method. The crystallinity and surface morphology of these films were investigated by means of X-ray diffraction (XRD) and atomic force microscopy (AFM), respectively. The XRD pattern confirmed that YVO₄:Sm³⁺ film has zircon structure and the AFM study revealed that the films consist of homogeneous grains ranging from 100 to 400 nm. The room temperature photoluminescence (PL) spectra showed that the emitted radiation was dominated by a reddish-orange emission peak at 602 nm radiating from the transition of (⁴G_5/2→⁶H_7/2). The crystallinity, surface morphology, and photoluminescence spectra of thin-film phosphors were highly dependent on the deposition conditions, in particular, the substrate temperature. The surface roughness and photoluminescence intensity of these films showed similar behavior as a function of oxygen pressure.     

Characterization on electron beam evaporated α-MoO3 thin films by the influence of substrate temperature

Electrochromic molybdenum oxide (MoO₃) thin films were prepared by electron beam evaporation technique using the dry MoO₃ pellets. The films were deposited on glass and fluorine doped tin oxide (SnO₂:F or FTO) coated glass substrates at different substrate temperatures like room temperature (RT, 30 °C), 100 °C and 200 °C. The influence of substrate temperature on the structural, surface morphological and optical properties of the films has been studied. The X-ray diffraction analysis showed that the films are having orthorhombic phase MoO₃ (α-MoO₃) with 〈1 1 0〉 preferred orientation. The laser Raman scattering spectrum shows the polycrystalline nature of MoO₃ films deposited at 200 °C. The Raman-active band at 993 cm⁻¹ is corresponding to Mo–O stretching mode that is associated with the unique character of the layered structure of orthorhombic MoO₃. Needle—like morphology was observed from the SEM analysis. The energy band gap of MoO₃ films was evaluated which lies between 2.8 and 2.3 eV depending on the substrate temperature and substrates. The decrease in band gap value with increasing substrate temperature is owing to the oxygen-ion vacancies. The absorption edge shift shows the coloration effect on the films.