分步法高速沉积微晶硅薄膜

为提高微晶硅薄膜的纵向结晶性能, 在甚高频等离子体增强化学气相沉积技术的基础上, 采用过渡参数缓变和两步法相结合的方法在普通玻璃衬底上高速沉积薄膜. 当功率密度为2.1 W/cm², 硅烷浓度在6%和9.6%之间变化时, 从薄膜方向和玻璃方向测算的Raman晶化率的差异维持在2%以内. 硅烷浓度为9.6%时, 薄膜沉积速率可达3.43 nm/s, 从薄膜方向和玻璃方向测算的Raman晶化率分别为50%和48%, 差异的相对值仅为4.0%. 合理控制过渡阶段的参数变化, 可使两个方向的Raman晶化率差值下降到一个百分点. 表明采用新方法制备薄膜, 不仅可以抑制非晶孵化层的形成, 改善微晶硅薄膜的纵向结构, 还为制备优质薄膜提供了较宽的参数变化空间. 关键词： 微晶硅薄膜 非晶孵化层 高速沉积 甚高频等离子体增强化学气相沉积     

Fabrication of xenogeneic bone-derived hydroxyapatite thin film by aerosol deposition method

Xenogeneic bone-derived hydroxyapatite (HA) was coated on Ti-6Al-4V substrate using aerosol deposition (AD) system. HA precursor powder was derived from bovine bone for the deposition. In aerosol system, submicron particles of HA were mixed with a carrier gas to form an aerosol flow in the aerosol chamber. The aerosol flow was through a tube to a nozzle, and then ejected into a deposition chamber. The effect of the beam incident angle on the HA film formation was investigated. The incident angle of the beam was changed from 0° to 60°. Homogeneous HA film with the thickness of 1-2 μm was fabricated by flattering of particles shape for the incident angle of 60°.     

Amorphous carbon nitride film preparation by plasma-assisted pulsed laser deposition method

Amorphous carbon nitride (aCN_x) films were prepared by pulsed laser ablation of graphite in N₂ RF plasma. The film property was compared with that prepared in N₂ gas. The N₂ plasma was generated by a mesh electrode, which was inserted between a graphite target and a Si substrate. The gas pressure p_N2 was varied from 10 to 100 mTorr. The film deposition rate exponentially decreased with p_N2 for both the plasma and gas environment. X-ray photoelectron spectroscopy analysis showed that the ratio of nitrogen content to the carbon one ([N]/[C]) of the aCN_x film surface deposited in the N₂ plasma was 2 times higher than that obtained in the N₂ gas. The film structure was shown by Raman spectroscopy analysis that sp² clustering was enhanced with increasing the [N]/[C]. The effect of plasma on aCN_x film deposition was discussed. PACS 81.15.Fg; 79.60.-i; 81.05.Uw     

Features of the film-growth conditions by cross-beam pulsed-laser deposition

Spatial and energetic characteristics of the plasma plume by cross-beam pulsed-laser deposition (CBPLD) were investigated. Effective droplets filtering together with high efficiency of material usage are observed by this approach. Time-of-flight (TOF) technique with electrostatic ion collectors (Langmuir probes operating in the ion-collecting mode) were applied to obtain kinetic energy distribution functions of ionized particles and to compare the ionization degrees of the plasma by the CBPLD and by the conventional PLD. The average and maximum kinetic energies of the ions by the CBPLD are found to be 2–3 times lower as compared to the conventional PLD. At the same time, the fraction of ionized species and highly exited neutrals (Rydberg atoms) in the CBPLD plasma is 1.5–2 times larger in comparison to the conventional approach. Re-sputtering of the material of the growing film by fast ions is a considerable effect in both the PLD methods by the chosen experimental conditions. The angular width of the directional pattern of the plasma plume by CBPLD is comparable to that typical for the conventional PLD. Received: 21 December 1998 / Accepted: 28 March 1999 / Published online: 7 July 1999     

Thickness dependent surface microstructure evolution of bismuth thin film prepared by molecular beam deposition method

The evolution of surface microstructure on bismuth thin film deposited by molecular beam deposition method is investigated. Morphological, topographical, structural, and electrical property changes of the film with various thicknesses are studied by means of AFM, XRD, XRR, and 4-point probe. Drastic change of surface grain in shape, which transforms from round shape to polyhedral shape, is detected around 13–18 nm film thickness. Abrupt horizontal profile change of surface grain is verified with power spectral density (PSD) function. At this threshold thickness, the film shows very low roughness value and surface area ratio. Then both increase steeply as the film thickness surpasses the thickness. As the bismuth film is deposited thicker, it has textured structure and high roughness on surface. With increment of the thickness, the electrical sheet resistance of the films is significantly decreased. We explain this surface microstructure evolution on the bismuth film with the evolutionary selection model.     

化学沉淀法制备硒化铅薄膜

采用化学沉淀的方法沉淀PbSe薄膜,分别加入缓冲剂联氨(方法A)和碘化钾(方法B)。对反应原理进行了分析,对制备过程进行了优化,分别制备出了高质量的PbSe薄膜。采用XRD、SEM、EDS以及红外光谱测试对所制备样品进行了分析。结果表明,两种方法制备均为PbSe多晶薄膜,方法A制备薄膜结晶质量更好,择优生长方向明显;薄膜颗粒度、表面粗糙度都小于方法B;两种薄膜的Pb元素与Se元素比例接近化学计量比,方法B含有少量I元素;两种方法制备样品的吸收边相对带边跃迁都发生蓝移。     

Electrical conductivity of BaTi4O9 film prepared by laser chemical vapor deposition method

A BaTi₄O₉ film was prepared on a Pt/Ti/SiO₂/Si substrate by a laser chemical vapor deposition method and was investigated by impedance spectroscopy over ranges of temperature (300–1073 K) and frequency (10²–10⁷ Hz). Plots between real and imaginary parts of the impedance (Z′ and Z′′) suggest the presence of two relaxation regimes, which were attributed to grain and grain boundary responses. The conduction of both grains and grain boundaries obeys the Arrhenius format with activation energies of respectively 1.45 and 1.24 eV. The close activation energies indicate that the conduction in BaTi₄O₉ film is mainly by oxygen vacancies.     

Grain boundary diffusion of Cu in TiN film by X-ray photoelectron spectroscopy

In this study, the grain boundary diffusion of Cu through a TiN layer with columnar structure was investigated by X-ray photoelectron spectroscopy (XPS). It was observed that Cu atoms diffuse from the Cu layer to the surface along the grain boundaries in the TiN layer at elevated temperature. In order to estimate the grain boundary diffusion constants, we used the surface accumulation method. The diffusivity of Cu through TiN layer with columnar structure from 400 °C to 650 °C is D_b≈6×10⁻¹¹exp(−0.29/(k_BT )) cm²/s. Received: 18 May 1999 / Accepted: 8 September 1999 / Published online: 23 February 2000     

Physical and technological principles of designing layer-gradient multicomponent surfaces by combining the methods of ion-diffusion saturation and magnetron- and vacuum-arc deposition

Using a technological system proposed by the authors, a combined process is developed for formation of stratified-gradient surface layers and multicomponent coatings. It is implemented under the conditions of a combined serial-parallel operation of a hot-cathode gas plasma generator and a duomagnetron with two targets and two electric-arc evaporators. The extended functional potential is ensured by using advanced multi-element and multi-phase cathode targets made of borides, carbides, silicides, and sulfides of metals produced by the SHS-process followed by their immediate compaction. The variations in composition, structure, and physicomechanical properties in the cross-section of the stratified-gradient surface layers and coating is provided by a predetermined alternating replacement of the sputtered cathode targets of the plasma sources, the plasma flow intensity ratios, and variation in the particle energy incident on the substrate, which is determined by the accelerating voltage on the substrate.     

Properties including step coverage of TiN thin films prepared by atomic layer deposition

The physical properties including the step coverage of the TiN films deposited by atomic layer deposition (ALD) technique, using TiCl₄ and NH₃ as the precursors have been investigated. The deposition rate of the TiN film is constant and moderately high (0.6 Å per cycle) under an optimum deposition condition. The film resistivity is appreciably low (200 μΩ cm). The XRD analysis results indicate polycrystalline nature of the TiN films with a (1 1 1) preferred orientation. The XPS and AES analysis results establish that the Cl impurity concentration in the TiN films is lower than 1 at.% and the ratio of Ti and N by atomic concentration in the TiN films is nearly equal to 1:1 AFM analysis reveals that the RMS surface roughness is low. Also it is found by SEM observation that the step coverage of the TiN films with trenches (the aspect ratio being 10:1) is excellent. One hundred percent conformality is observed for both the side/bottom and the side/top sections.     

Kinetic model of thin film growth by vapor deposition

A phenomenological kinetic model is proposed for describing the production of a thin film containing two components, A and B, by chemical and physical vapor deposition. The film was created by the “site-to-site” deposition of components A and B. The equations for the densities of components A and B in the surface layers were formed, and analytical and numerical solutions were obtained. The model includes the probabilities of different elementary processes for the interaction of gas phase components (molecules, radicals, atoms and ions) with those of A and B on the film surface. The deposition and erosion rates, the surface and volume densities of components A and B and the relative volume of micro-cavities inside the film were calculated as a function of the probabilities for the elementary processes of gas (plasma)-surface interactions. The experimental characteristics of a-Si: H thin films prepared by SiH₄ plasma deposition and those of carbon nitride thin films deposited from r.f. — magnetron sputtering and ion beam-assisted processes are compared with model calculations.     

Characterization of gadolinium oxide film by pulse laser deposition

In this work, Gd-oxide dielectric films were deposited on Si by pulse laser deposition method (PLD), moreover, the micro-structures and electrical properties were reported. High-resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) indicated that Gd-oxide was polycrystalline Gd₂O₃ structure, and no Gd metal phase was detected. In addition, both interface at Si and Ni fully silicide (FUSI) gate were smooth without the formation of Si-oxide. X-ray photoelectron spectroscopy (XPS) confirmed the formation of Gd₂O₃ and gave an atom ratio of 1:1 for Gd:O, indicating O vacancies existed in Gd₂O₃ polycrystal matrix even at O₂ partial pressure of 20 mTorr. Electrical measurements indicated that the dielectric constant of Gd-oxide film was 6 and the leakage current was 0.1 A/cm² at gate bias of 1 V.     

利用多层膜生长技术制备纳米印章模板

在纳米印章技术中，为克服电子束刻蚀制备50nm以下线条的技术难点，利用等离子增强化学 气相沉积技术制备了a-Si/SiN_x多层膜，再利用选择性湿法腐蚀或干法腐蚀在横 截面上制备出浮雕型一维纳米级模板. 多层膜子层之间界面清晰陡峭，可以在纳米量级对子 层厚度进行控制，得到了侧壁在纳米尺度上平滑的模板. 通过控制多层膜子层的生长时间， 制备出线条宽度和槽状宽度均为20nm的等间距模板，品质优于电子束刻蚀技术制备的模板. 关键词： 纳米印章模板 多层膜生长技术     

Ultraviolet emission of ZnO film prepared by electrophoretic deposition

We deposited high quality ZnO film by electrophoretic deposition (EPD) using high quality ZnO powder prepared by solid-state pyrolytic reaction. X-ray photoelectron spectroscopy (XPS) and the infrared (IR) absorption spectrum clearly indicate that the ZnO phase powder has been prepared. Transmission electron microscope (TEM) imaging and x-ray diffraction (XRD) show that the average grain size of the powder is about 20nm. XRD and selected-area electron diffraction (SAED) reveal that the ZnO film has a polycrystalline hexagonal wurtzite structure. Only a strong ultraviolet emission peak at 390nm can be observed at room temperature.     

Formation of Ti and TiN ultra-thin films on Si by ion beam sputter deposition

Ultra-thin titanium and titanium nitride films on silicon substrate were obtained by ion beam sputtering of titanium target in vacuum and nitrogen atmosphere, using argon ions with energy of 5 keV and 15 μA target current. Elemental composition and chemical state of obtained films were investigated by X-ray photoelectron spectroscopy with using Mg-Kα X-ray radiation (photon energy 1253.6 eV). It was shown that it is possible to form both ultra-thin titanium films (sputtering in vacuum) and ultra-thin titanium nitride films (sputtering in nitrogen atmosphere) in the same temperature conditions. Photoelectron spectra of samples surface, obtained in different steps of films synthesis, detailed spectra of photoelectron emission from Si 2p, Ti 2p, N 1s core levels and also X-ray photoelectron spectra of Auger electrons emission are presented.     

Features of the structure of TiN films after irradiation with nitrogen

In this work, we study the structure of submicron titanium-nitride films after surface treatment with a nitrogen-ion beam. It is ascertained that nitrogen-ion beams affect two-phase TiN-Ti films thus transforming them into single-phase TiN.     

Kinetic roughening in polymer film growth by vapor deposition

The growth front roughness of linear poly( p-xylylene) films grown by vapor deposition polymerization has been investigated using atomic force microscopy. The interface width w increases as a power law of film thickness d, w approximately d(beta), with beta = 0. 25+/-0.03, and the lateral correlation length xi grows as xi approximately d(1/z), with 1/z = 0.31+/-0.02. This novel scaling behavior is interpreted as the result of monomer bulk diffusion, and belongs to a new universality class that has not been discussed previously.     

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%)。     

脉冲激光气相沉积法制备钴纳米薄膜实验研究

 采用脉冲激光沉积技术制备了钴纳米薄膜，分析和讨论了不同背景气压和脉冲频率对钴纳米薄膜表面形貌的影响及纳米微粒的形成机理。实验结果表明：在低背景气压下，等离子体羽辉自身粒子之间的碰撞占主导作用，容易形成液滴；在较高背景气压下，等离子体羽辉边缘粒子和背景气体粒子之间的碰撞占主导作用，容易形成小岛并凝聚成微颗粒；在4Hz的脉冲重复频率和5Pa背景气压下生长出单分散性良好的钴纳米颗粒。     

Electrical conductivity of YSZ film grown by pulsed laser deposition

Yttria-stabilized zirconia (YSZ) thin films, 0.6–1.5 μm, were deposited on Pt and sapphire substrates by a pulsed laser deposition (PLD) method. Their structural and transport properties have been studied by means of X-ray diffraction and electrical conductivity measurements. The in-plane and the perpendicular-to-plane conductivities (hereafter, “across-plane” conductivity) of thin films were measured and compared to that of bulk sample. X-ray diffraction and electron microscopy results showed that the films on Pt and sapphire were polycrystalline cubic with a columnar structure. Both the across-plane and the in-plane conductivities of YSZ thin film were close to that of bulk specimens. Thus no conductivity enhancement was found for the present nano-crystalline YSZ films (grain or column size, 60∼100 nm).