单晶硅表面有机硅烷/Ag2O纳米微粒复合自组装膜的制备和表征

利用分子自组装成膜技术 ,在单晶硅表面制备了有机硅烷 /Ag2 O纳米微粒复合膜 .应用接触角测定仪、原子力显微镜和X射线光电子能谱仪分析表征了薄膜的组成和结构 .结果表明 ,通过硅烷偶联剂 3 氨丙基 三乙氧基硅烷在单晶硅基底表面的成功组装 ,获得了较为均匀的硅烷化表面 ,而Ag2 O纳米微粒可在硅烷化表面成功地进行组装 ,并呈亚单层排布     

Si(111)衬底切偏角对GaN基LED外延膜的影响

利用金属有机化学气相沉积(MOCVD)方法在具有偏角(0°~0.9°)的Si(111)衬底上生长了GaN薄膜。采用高分辨X射线衍射(HRXRD)对Si衬底的偏角进行了精确的测量,利用HRXRD、原子力显微镜(AFM)以及光致发光(PL)对外延薄膜的晶体质量、量子阱中In组分、表面形貌及光学特性进行了研究。结果表明,Si(111)衬底偏角对量子阱中的In组分、 GaN外延膜的表面形貌、晶体质量以及光学性能具有重大影响。为了获得高质量的GaN外延薄膜,衬底偏角必须控制在小于0.5°的范围内。超出该范围,GaN薄膜的晶体质量、表面形貌及光学性能都明显下降。     

Structure and microtribological characteristics of laser-arc deposited TiB2 thin film

TiB2 thin film was deposited by laser-arc deposition method on the surface of single crystalline silicon. The morphology, composition, structure and microtribological properties of the film were studied by using XPS, XRD and atomic force/friction force microscope (AFM/FFM). The results show that TiB2 (100) preferred growth on the Si(100)substrate, TiB2(001) preferred growth on the Si(111) substrate. The TiB2 thin film was composed of TiB2 and a small amount of TiO2. The friction coefficient of TiB2 film on substrates Si (100) and Si(111) in microtribological process were 0.087 and 0.073,respectively. TiB2 thin film displayed distinct ability of anti-scratch and wear-resistance.     

Fabrication of contact electrodes in Si for nanoelectronic devices using ion implantation

We fabricated contact electrodes in Si for nanoelectronic device fabrication using 40 keV As ion implantation. Complete amorphization of the Si surface with contact electrodes using 400 eV Ar ion irradiation at room temperature followed by annealing at 700 °C produced Si surface with negligible SiC crystallites suitable for ultrahigh vacuum scanning tunneling microscope nanolithography. We could locate the implanted and unimplanted regions on Si and fabricate Si dangling bond wires between two contact electrodes, which is the first step for the fabrication of nanoelectronic devices in Si using UHV STM nanolithography.     

Structure and microtribological characteristics of laser-arc deposited TiB2 thin film

TiB2 thin film was deposited by laser-arc deposition method on the surface of single crystalline silicon. The morphology, composition, structure and microtribological properties of the film were studied by using XPS, XRD and atomic force/friction force microscope (AFM/FFM). The results show that TiB2 (100) preferred growth on the Si(100) substrate, TiB2(001) preferred growth on the Si(111) substrate. The TiB2 thin film was composed of TiB2 and a small amount of TiO2. The friction coefficient of TiB2 film on substrates Si (100) and Si(111) in microtribological process were 0.087 and 0.073, respectively. TiB2 thin film displayed distinct ability of anti-scratch and wear-resistance.     

不同后处理方法对溶胶-凝胶SiO2膜层抗污染能力的影响

 以正硅酸乙酯作为前驱体,利用碱催化方式制备了SiO₂溶胶,采用提拉法在K9基片上镀制SiO₂单层薄膜,分别用热处理、紫外辐射处理、氨水加六甲基二硅胺烷气氛处理和酸碱复合膜4种后处理法对膜层进行处理,采用分光光度计、红外光谱、扫描探针显微镜、静滴接触角测量仪、椭偏仪等分析了薄膜的特性,通过真空环境加速污染实验对处理前后的膜层进行抗污染能力对比,结果表明：在碱性SiO₂膜层上加镀一层酸性SiO₂膜的复合膜层整体透过率仍保持在99%以上,疏水角达到128°,膜层真空抗污染能力大大加强。     

Graft and characterization of 9-vinylcarbazole conjugated molecule on hydrogen-terminated silicon surface

Using wet chemical reaction between N-vinylcarbazole and hydrogen-terminated silicon surface, we present a new and simple route to directly bond π-conjugated organic molecule on silicon surface. The Si can be in the form of single crystal Si including heavily doped p-type Si, intrinsic Si, heavily doped n-type Si, on Si(1 1 1) and Si(1 0 0), and on n-type polycrystalline Si. The covalent bond between 9-vinylcarbazole and silicon surface was confirmed by reflectance FTIR, XPS and contact angle measurement, respectively. A data-encompassing explanation for the mechanism discusses the possible route of the reaction. This simple and low-costly reaction offers an attractive route to attach functional conjugated molecules onto the semiconductor surface which aims to create some unique molecular device in the future.     

Superhydrophobic poly(vinylidene fluoride) film fabricated by alkali treatment enhancing chemical bath deposition

Based on the lotus effect principle, the superhydrophobic poly(vinylidene fluoride) (PVDF) film was successfully prepared by the method of alkali treatment enhancing chemical bath deposition. The surface of PVDF film prepared in this work was constructed by many smooth and regular microreliefs. Oxygen-containing functional groups were introduced in PVDF film by treatment with aqueous NaOH solution. The nano-scale peaks on the top of the microreliefs were implemented by the reaction between dimethyldichlorosilane/methyltrichlorosilane solution and the oxygen-containing functional groups of PVDF film. The micro- and nano-scale structures, similar to the lotus leaf, was clearly observed on PVDF film surface by scanning electronic microscopy (SEM) and atomic force microscope (AFM). The water contact angle and sliding angle on the fabricated lotus-leaf-like PVDF film surface were 157° and 1°, respectively, exhibiting superhydrophobic property and self-cleaning property.     

Effect of deposition condition on residual stress of iron nitride thin films prepared by magnetron sputtering and ion implantation

The surface roughness and residual stress development in Fe-N thin films prepared by compound technology—combining magnetron sputtering with plasma based ion implantation were investigated by means of atomic force microscope and synchrotron radiation. The results indicate that the grain size of the thin film increases with the increasing of nitrogen ion implantation time, and the state of residual stress is related closely to the formation mechanism of thin films. With the nitrogen ion implantation time increasing, the residual stress of the thin film changes into tensile stress from initial compressive stress, and the tensile stress decreases with the further increasing of ion implantation time.     

Wettability and formation mechanism of ZnO micro-spheres composed film

This paper reports that the film composed of flower-like ZnO micro-spheres, which consists of nano-sheets, is fabricated by chemical bath deposition. By adding hydrogen fluoride (HF) into the reaction solution, which contains zinc nitrate hexahydrate and hexamethylenetetramine, the ZnO crystal growth process is changed and the film composed by ZnO micro-spheres is obtained after keeping the reaction solution at 95 oC for 2 h. The morphology, crystal phase and wettability of the sample are characterized by scanning electron microscope, x-ray diffraction and contact angle meter, respectively. The results show that the film has the micro-nano compound structure. After modification with heptadecafluorodecyltrimethoxy-silane, the wettability of the film changed from superhydrophilicity to superhydrophobicity, on which water contact angle and the sliding angle are 154o and less than 5o for 8-μL water droplet, respectively. Additionally, the formation mechanism of the ZnO micro-sphere is also discussed.     

Hydrogen isotopic replacement and microstructure evolution in zirconium deuteride implanted by 150 keV protons

Zirconium tritiated(ZrT_x) is an alternative target material for deuteron–triton(D-T) reaction neutron generator. The isotopic replacement and microstructure evolution induced by hydrogen isotope implantation could significantly affect the performance of the target film. In this work, the zirconium deuteride film deposited on Mo/Si substrate was implanted by 150 ke V protons with fluence from 1×10~(16) to 1×10~(18) protons/cm~2. After implantation, the depth profiles of retained hydrogen(H) and deuterium(D) in these target films were analyzed by elastic recoil detection analysis(ERDA), and time of flight-secondary ion mass spectrometry(To F-SIMS). Additionally, the microstructure evolution was also observed by x-ray diffraction(XRD) and scanning electron microscope(SEM). The D concentration in the Zr Dx film decreased versus the proton implantation fluence. An analytical model was proposed to describe the hydrogen isotopic trapping and exchange as functions of incident protons fluence. Additionally, the XRD analysis revealed that no new phase was formed after proton implantation. Furthermore, circular flakings were observed on the ZrD_x surface from SEM images at fluence up to 1×10~(18) protons/cm~2, and this surface morphology was considered to associate with the hydrogen atoms congregation in Mo/Si boundary.     

Characterization of the N-polar GaN film grown on C-plane sapphire and misoriented C-plane sapphire substrates by MOCVD

Gallium nitride (GaN) thin film of the nitrogen polarity (N-polar) was grown on C-plane sapphire and misoriented C-plane sapphire substrates respectively by metal-organic chemical vapor deposition (MOCVD). The misorientation angle is off-axis from C-plane toward M-plane of the substrates, and the angle is 2° and 4° respectively. The nitrogen polarity was confirmed by examining the images of the scanning electron microscope before and after the wet etching in potassium hydroxide (KOH) solution. The morphology was studied by the optical microscope and atomic force microscope. The crystalline quality was characterized by the x-ray diffraction. The lateral coherence length, the tilt angle, the vertical coherence length, and the vertical lattice-strain were acquired using the pseudo-Voigt function to fit the x-ray diffraction curves and then calculating with four empirical formulae. The lateral coherence length increases with the misorientation angle, because higher step density and shorter distance between adjacent steps can lead to larger lateral coherence length. The tilt angle increases with the misorientation angle, which means that the misoriented substrate can degrade the identity of crystal orientation of the N-polar GaN film. The vertical lattice-strain decreases with the misorientation angle. The vertical coherence length does not change a lot as the misorientation angle increases and this value of all samples is close to the nominal thickness of the N-polar GaN layer. This study helps to understand the influence of the misorientation angle of misoriented C-plane sapphire on the morphology, the crystalline quality, and the microstructure of N-polar GaN films.     

Measurement of lattice damage caused by ion-implantation doping of semiconductors†

Two new techniques have been used to measure the lattice damage produced in gallium arsenide by the implantation of 60 keV cadmium ions. In one of these methods, optical reflection spectra of the ion-implanted samples were measured in the wavelength range from 2000 to 4600Å. The decrease in reflectivity resulting from ion- implantation was used to determine the relative amount of lattice damage as a function of ion dose. The second technique employed the scanning electron microscope. Patterns very similar in appearance to Kikuchi electron diffraction patterns are obtained when the secondary and/or backscattered electron intensity is displayed in the scanning electron microscope as a function of the angle of incidence of the electron beam on a single crystal surface. The degradation of these ‘Coates-Kikuchi’ patterns resulting from ion implantation was used to obtain a quantitative measure of the lattice damage caused by the implantation process. The results of measurements made by both of the methods described have been compared with each other, and with data obtained by the more established method of measuring lattice damage by Rutherford scattering of 1 MeV helium ions.     

Preparation of superhydrophobic films on titanium as effective corrosion barriers

Stable superhydrophobic films were prepared on the electrochemical oxidized titania/titanium substrate by a simple immersion technique into a methanol solution of hydrolyzed 1H,1H,2H,2H-perfluorooctyltriethoxysilane [CF₃(CF₂)₅(CH₂)₂Si(OCH₂CH₃)₃, PTES] for 1 h at room temperature followed by a short annealing at 140 °C in air for 1 h. The surface morphologies and chemical composition of the film were characterized by means of water contact angle (CA), field emission scanning electron microscopy (FESEM), atomic force microscope (AFM) and X-ray photoelectron spectroscopy (XPS). The water contact angle on the surface of this film was measured to be as high as 160°. SEM images showed that the resulting surfaces exhibited special hierarchical structure. The special hierarchical structure along with the low surface energy leads to the high surface superhydrophobicity. The corrosion resistance ability and durance property of the superhydrophobic film in 3.5 wt.% NaCl solution was evaluated by the electrochemical impedance spectroscopy (EIS). The anticorrosion properties of the superhydrophobic film are compared to those of unmodified pure titanium and titania/titanium substrates. The results showed that the superhydrophobic film provides an effective corrosion resistant coating for the titanium metal even with immersion periods up to 90 d in the 3.5 wt.% NaCl solution, pointing to promising future applications.     

Friction,adhesion and wear durability of an ultra-thin perfluoropolyether-coated 3-glycidoxypropyltrimethoxy silane self-assembled monolayer on a Si surface

The tribological properties, such as coefficient of friction, adhesion and wear durability of an ultra-thin (<10?nm) dual-layer film on a silicon surface were investigated. The dual-layer film was prepared by dip-coating perfluoropolyether (PFPE), a liquid polymer lubricant, as the top layer onto a 3-glycidoxypropyltrimethoxy silane self-assembled monolayer (epoxy SAM)-coated Si substrate. PFPE contains hydroxyl groups at both ends of its backbone chain, while the SAM surface contains epoxy groups, which terminate at the surface. A combination of tests involving contact angle measurements, ellipsometry, atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) was used to study the physical and chemical properties of the film. The coefficient of friction and wear durability of the film were investigated using a ball-on-disk tribometer (4?mm diameter Si₃N₄ ball as the counterface at a nominal contact pressure of ～330?MPa). AFM was used to investigate the adhesion forces between a sharp Si₃N₄ tip and the film. This dual-layer film had a very low coefficient of friction, adhesion and wear when compared to epoxy SAM-coated Si only or bare Si surface. The reasons for the improved tribological performance are explained in terms of the lubrication characteristics of PFPE molecules, low surface energy of PFPE, covalent bonding between PFPE and epoxy SAM coupled with reduced mobile PFPE. The low adhesion forces coupled with high wear durability show that the film has applications as a wear resistant and anti-stiction film for microcomponents made from Si.     

沉积温度对钛硅共掺杂类金刚石薄膜生长、结构和力学性能的影响

采用中频磁控溅射Ti80Si20复合靶在单晶硅表面制备了共掺杂的类金刚石薄膜.研究了沉积温度对薄膜生长速率、化学成分、结构、表面性质和力学性能的影响.结果表明:随沉积温度升高,薄膜生长速率降低,薄膜Ti和Si原子浓度增加,C原子浓度降低;在高温下沉积的薄膜具有低sp3C含量、低表面接触角、低内应力和高的硬度与弹性模量.基于亚表层注入生长模型分析了沉积温度对薄膜生长和键合结构的影响,从薄膜生长机制和微观结构解释了表面性质和力学性能的变化.     

Surface modification of porous poly(tetrafluoroethylene) film via cold plasma treatment

In this study, cold plasma technology was applied for the surface modification of porous polytetrafluoroethylene (PTFE) film to improve the hydrophilicity. The surface properties of PTFE, modified by air, helium (He) or acrylic acid (AAc), were investigated with scanning electron microscopy (SEM), scanning probe microscope (SPM), in situ X-ray photoelectron spectroscopy (XPS) and water contact angle measurements. The changes of the surface property before and after plasma treatment were discussed. According to SEM and SPM measurements, the surface roughness increased at different levels after plasma treatment. Compared to air and AAc plasma treatment, the He plasma treatment introduced large amounts of oxygen into the surface, as known from XPS results. Contact angle measurements revealed that the hydrophilicity of the PTFE film surface was greatly improved due to the surface roughness and changes of chemical elements on the PTFE surface.     

CVD金刚石中的氮对等离子体刻蚀的影响

采用非对称磁镜场电子回旋共振等离子体分别对沉积过程中掺氮和未掺氮的化学气相沉积金刚石膜进行了刻蚀研究, 结果表明: 掺氮制备的金刚石膜的刻蚀主要集中在晶棱处, 经过4h刻蚀后其表面粗糙度由刻蚀前的4.761 μm下降至3.701 μm, 刻蚀对金刚石膜的表面粗糙度的影响较小; 而未掺氮制备的金刚石膜的刻蚀表现为晶面的均匀刻蚀, 晶粒坍塌,刻蚀4h后其表面粗糙度由刻蚀前的3.061 μm下降至1.083 μm. 刻蚀导致表面粗糙度显著降低. 上述差别的主要原因在于金刚石膜沉积过程中掺氮导致氮缺陷在金刚石晶棱处富集, 晶棱处电子发射加强, 引导离子向晶棱运动并产生刻蚀, 从而加剧晶棱的刻蚀. 而未掺氮金刚石膜,其缺陷相对较少且分布较均匀 ,刻蚀时整体呈现为 (111) 晶面被均匀刻蚀继而晶粒坍塌的现象. 关键词： 掺氮 金刚石膜 刻蚀 非对称磁镜场     

不同氮流量制备Mn3CuNx薄膜及其电、磁输运性质的研究

采用对靶磁控溅射方法在单晶Si(100)基片上制备了反钙钛矿结构的Mn₃CuN_x薄膜.通过控制制备过程中的反应气体氮气(N₂) 流量(N₂/Ar+N₂), 研究了氮含量对Mn₃CuN_x薄膜结构及物理性能的影响.分别利用X射线衍射仪、俄歇电子能谱、 原子力显微镜、X射线光电子能谱、物理性能测试系统和超导量子干涉仪, 对所制备薄膜的晶体结构、成分、表面形貌和电、磁输运性质进行了测试.结果表明:制备的薄膜均为反钙钛矿立方结构,且沿 (200) 晶面择优生长.随着氮含量的增大,薄膜表面粗糙度和颗粒度尺寸逐渐增大, 导致电阻率增加.氮含量对薄膜的电输运性质没有影响,所有薄膜电阻率均随着温度的降低逐渐增大, 呈现半导体型导电行为,这与对应的块体材料结果相反.Mn₃CuN_x薄膜随着测试温度的增大发生了 亚铁磁到顺磁的磁转变,且N含量的增大降低了磁有序转变温度,主要是由于N缺陷对Mn₆N八面体结构中 磁交换作用的影响所致.     

Fabrication of superhydrophobic wood surface by a sol-gel process

The superhydrophobic wood surface was fabricated via a sol-gel process followed by a fluorination treatment of 1H, 1H, 2H, 2H- perfluoroalkyltriethoxysilanes (POTS) reagent. The crystallization type of silica nanoparticles on wood surface was characterized using X-ray diffraction (XRD), the microstructure and chemical composition of the superhydrophobic wood surface were described by scanning electron microscope (SEM) and energy dispersive spectrometer (EDS), the bonding force between the silica nanoparticles and POTS reagent was analyzed by Fourier transform infrared spectroscopy (FT-IR) and the superhydrophobic property of the treated sample was measured by contact angle (CA) measurements. An analytical characterization revealed that nanoscale silica spheres stacked uniformly over the wood surface, and with the combination of the high surface roughness of silica nanoparticles and the low surface free energy film of POTS on wood surface, the wood surface has turned its wetting property from hydrophilic into superhydrophobic with a water contact angle of 164° and sliding angle less than 3°.