用AFM压痕技术定量介观硬度的方法研究

用原子力显微镜(AFM)纳米压痕方法结合扫描力显微镜技术，表征类金刚石(DLC)膜，金块Au，单晶硅Si的纳米硬度。用能量密度理论解释基于AFM压痕技术测定纳米硬度的机理，给出AFM纳米压痕的能量平衡方程。对DLC膜，金块，单晶硅进行纳米压痕试验，表明在同样载荷下，不同材料的压痕深度是不相同的。DLC膜具有较高的抗压性能，Si其次，Au的抗压性能最低。通过曲线拟合技术，定量给出金块的纳米硬度分析模型：H=(2．83／Df) 2．86。     

The microstructure of petroleum vacuum residue films for bituminous concrete: a microscopy approach

Selected carbon-rich refinery residues ('binders') mixed with mineral particles can form composite materials ('bituminous concrete') with bulk mechanical properties comparable to those of cement concrete. The microstructural mechanism underlying the remarkable composite properties has been related to the appearance of a rigid percolating network consisting of asphaltenes and mineral particles [Wilbrink M. et al. (2005) Rigidity percolation in dispersions with a structured visco-elastic matrix. Phys. Rev. E71, 031402]. In this paper, we explore the microstructure of thin binder films of varying thickness with a number of microscopic characterization techniques, and attempt to relate the observed microstructure to the distinctive mechanical behaviour. Two binders, only one of which has been proven to be suitable for bituminous concrete were investigated, and their microstructure compared. Both binders show the formation of asphaltene aggregates. The binder suitable for bituminous concrete is distinguished by the fact that the asphaltenes show a stronger tendency towards such aggregation, due to a higher concentration and less stabilization in the maltene phase. They also show a clear affinity to other species (such as waxes) and may act as nucleation sites for crystals and aggregates of those species.     

超薄类金刚石膜纳米摩擦性能研究

使用原子力显微镜对由微波等离子体电子回旋共振化学气相沉积技术制备的超薄类金刚石薄膜的纳米摩擦性能进行了研究。结果表明：氢化非晶碳膜(a-C：H)的摩擦力和外加载荷基本成线性关系，可以使用修正的Amonton公式进行表征；厚度在64．9nm以下薄膜的微观承载性能和膜厚存在明显的正比例关系。通过分析磨损深度和循环次数之间的关系以及对磨损区域的导电性研究，表明a-C：H膜表层的微观承载性能较其内层相差很大，表面存在着一层软膜。     

In situ study of nano-cracking in multilayered magnetic tapes under monotonic and fatigue loading using an AFM

Atomic force microscopy (AFM) techniques are increasingly used for tribological studies of engineering surfaces on micro- to nano-scales. In situ surface characterization of local deformation of materials and thin coatings helps to develop a better understanding of failure mechanisms. In this study, an AFM-based technique has been developed for in situ monitoring of nano-crack formation and progression under fatigue loading. To conduct monotonic and fatigue loading tests, a tensile stage is used to mount samples on the AFM base and the same area on the sample surface is scanned intermittently during the loading process. Crack growth under monotonic and fatigue loading for multilayered magnetic tapes is studied and a crack growth mechanism for metallic magnetic tapes under monotonic loading is proposed. Fatigue strength for the metallic magnetic tapes is measured and a mathematical model based on theory of elasticity for fatigue life prediction is developed.     

Morphological properties of Ag₂SeTe nano thin films prepared by thermal evaporation

Semiconducting silver selenide telluride (Ag₂SeTe) thin films were prepared with different thicknesses onto glass substrates at room temperature using thermal evaporation technique. The structural properties were determined as a function of thickness by X‐ray diffraction exhibiting no preferential orientation along any plane; however, the films are found to have peaks corresponding to mixed phase. The morphology of these films was studied using scanning electron microscope and atomic force microscopy respectively, and is reported. The morphological properties are found to be very sensitive to the thin film thickness. The composition of the films is also estimated using energy dispersive analysis using X‐rays and are also reported.     

Atomic force microscopy observations of in situ deformed materials: application to single crystals and thin films on substrates

An experimental apparatus which consists of a compression machine interfaced with an atomic force microscope has been realized and allows the in situ observation of a sample surface under compressive stress. Taking advantage of the high resolution offered by this microscopy, the equipment is particularly suited both to analysing the fine slip line structure of deformed single crystals, providing interesting complementary information about plastic mechanisms taking place in the bulk, and to characterizing the mechanical behaviour of thin films on substrates with the investigation of the buckling phenomenon.     

Controlled growth and formation of SAMs investigated by atomic force microscopy

Recently we reported a simple method for obtaining both monolayer thickness and surface patterning using self-assembled monolayers (SAMs). Here we presented a straightforward method for controlling the formation of SAMs over surfaces useful for both chemical and biological applications. Atomic force microscopy (AFM) has been used to investigate the growth mechanism and formation of octadecylsiloxane (ODS) films obtained using a less-reactive silane; octadecyltrimethoxysilane (OTMS). SAMs formation from both OTMS and octadecyltrichlorosilane (ODTS) differ in the hydrolysis step where ODTS results in hydrochloric acid formation, which may affect the delicate features on surfaces. On the other hand, OTMS does not show this behavior. In contrast to monolayer formation from chlorosilane precursors, methoxysilane SAMs have been studied less extensively. Our observations highlight the importance of controlling water content during the formation of ODS monolayers in order to get well-ordered SAMs. We have also seen that, like ODTS, OTMS exhibits monolayer growth through an island expansion process but with a comparatively slow growth rate and different island morphology. The average height of islands, surface coverage, contact angle and root-mean-square (RMS) roughness increase with OTMS adsorption time in a consecutive manner.     

Nanotribological Studies of Chromium Thin Films

Systematic nanotribological studies of Cr thin films using nanoscratch and AFM techniques are presented. Constant and ramped loading scratches were made using a Nano Indenter II system at various loads (1mN, 2.5mN and 5mN). Extensive AFM studies of the scratch wear tracks have been performed after scratching. The dependence of the displacement, residual wear depth, percent elastic recovery, and friction coefficient on load in constant load and ramped load tests is compared. Under the same (maximum) load, constant load tests exhibit higher displacements, residual depths and friction coefficients but lower percent elastic recoveries. Detailed AFM observations of the wear tracks indicate that significant differences in lateral deformation accompany the observed displacement differences.     

Broadband nanodielectric spectroscopy by means of amplitude modulation electrostatic force microscopy (AM-EFM)

In this work we present a new AFM based approach to measure the local dielectric response of polymer films at the nanoscale by means of Amplitude Modulation Electrostatic Force Microscopy (AM-EFM). The proposed experimental method is based on the measurement of the tip-sample force via the detection of the second harmonic component of the photosensor signal by means of a lock-in amplifier. This approach allows reaching unprecedented broad frequency range (2-3×10⁴ Hz) without restrictions on the sample environment. The method was tested on different poly(vinyl acetate) (PVAc) films at several temperatures. Simple analytical models for describing the electric tip-sample interaction semi-quantitatively account for the dependence of the measured local dielectric response on samples with different thicknesses and at several tip-sample distances.     

Amorphous hydrogenated carbon films for tribological applications II. Films deposited on aluminium alloys and steel

This paper describes the methods for the deposition of AHC films on aluminium alloys (2024, 7075 and an additional Al-Si alloy) and AISI 4340 steel. Both unmodified and silicon modified AHC films were deposited. AHC films could be deposited on aluminium alloys without any interlayer. The deposition of AHC films on steel required an interlayer which could be aluminium, silicon or chromium. Thin films (1–2 μm) deposited on aluminium alloys and steel influenced durability of films and friction coefficients in contact with steel. These were believed to be due to plastic deformation of substrates. Deposition of a thicker coating system (interlayer + AHC) reduced friction coefficients and also improved film durability. The durability of films deposited on steel substrates was evaluated under both unlubricated and lubricated conditions for 5.5 million cycles under 4.4 N load and up to 2.5 m/s sliding speed. Although there was wear, the films survived 5.5 million test cycles under unlubricated sliding, but in the presence of two lubricants, the film wear was very small and could not be measured. It was observed that the wear of the steel counterface in contact with silicon-containing AHC films could be higher than that against an uncoated steel in the presence of certain lubricants.     

大型预硬化718塑料模具钢不同区域的抛光性能

用光学显微镜和扫描电镜对截面尺寸为1 360mm×715mm的大型预硬化718塑料模具钢块不同区域的显微组织进行了分析,用原子力显微镜对不同显微组织的表面形貌进行了观察,分析了珠光体/回火贝氏体混合组织区域的抛光去除机制。结果表明:模具钢边部为均匀的回火索氏体组织,边部和心部的中间部位存在带状偏析,组织为回火贝氏体、珠光体以及偏析处形成的索氏体+粒状碳化物,心部为珠光体组织;回火索氏体组织细小,回火碳化物分布均匀,具有良好的抛光性能;回火贝氏体组织由于具有粗大的贝氏体铁素体板条和粗大的不均匀分布的颗粒状碳化物,其抛光性能较差;珠光体以及偏析处形成的异常组织的抛光性能也较差,可观察到橘皮形貌;具有不同组织的表面,其组织间的屈服强度相差越大,则表面抛光性能越差。     

碳纳米管原子力显微镜针尖的制作研究

研究在光学显微镜下，运用两个独立的三维工作台分别控制针尖和碳纳米管的位置，将碳纳米管吸附在传统的原子力显微镜针尖上。首先将碳纳米管粘附在导电的胶带上，然后用涂胶的针尖与其接触将碳纳米管粘附到针尖上，最后运用电蚀的方法优化碳纳米管针尖的长度，以达到高分辨率的要求。运用制作的碳纳米管针尖对硅表面的深槽进行成像，获得了传统针尖无法得到的信息。     

钢的(M+B)复相热处理技术研究

指出目前理论界初步认为(M B)两相组织对同时提高钢强韧性方面的贡献.主要是适量的先析贝氏体分割了奥氏体晶粒,细化了有效晶粒,减小了随着转变形成的马氏体领域条片尺寸,缩短了单位裂纹长度,降低了脆性转变温度.但这些理论均存在着局限性,值得进一步研究、探讨.     

纳米操纵机器人及其自动化设计

在纳米技术和纳米材料领域,纳米操纵机器人已经成为一种用于分析和制作原型纳米器件的使能技术.这类纳米操纵机器人拾放操作灵活,可将单个纳米器件集成到现有的微器件中来提高微器件的总体性能和灵敏度.如今这种被称作微纳米集成装配的自动化装置不再局限于实验室使用,还需要应用于工业领域.本文综述了纳米微操作机器人的产生、集成装配和自动化等方面的基础技术,同时探讨了不同种类原子力显微镜超级探针的装配方案.     

Thin Metal Films Deposited on Dendrimer Monolayers

Chemical interactions and the evolution of surface morphology resulting from deposition of Cr and Co onto dendrimer monolayers have been investigated by XPS, RAIRS, and AFM. Evidence is presented for formation of metal nitrides and mediation of film morphology as a function of the metal and generation number of the dendrimer comprising the monolayer.     

Lateral force microscopy study of Langmuir–Blodgett films of a macrocyclic compound

Langmuir–Blodgett films of 4-phenyl-4-sulfide-11-(1-oxodecyl)-1,7-dithia-11-aza-4-phosphacyclotetradecane, a thiomacrocyclic compound used as a Cu(II) ions sensor, were extracted over mica at several surface pressure values from two subphases: pure water and a 0.01 M Cu(II) aqueous solution. Atomic Force Microscopy and Force Spectroscopy (Lateral Force Microscopy) were used to study both the morphology and the nanomechanical response of Langmuir–Blodgett films. A correlation between extraction pressure and monolayer mechanical properties was observed, so an increase in the extraction pressure of the monolayers corresponds with an increase in the vertical force at which the monolayer breaks while doing lateral force experiments. Experimental data proves that Langmuir–Blodgett extraction technique truly obtains monolayers with different nanotribological properties as a function of the extraction surface pressure. The formation of islands on top of the monolayers was studied and a model mechanism of formation is proposed. A higher friction value was measured on the islands than on the monolayer and friction asymmetry was observed in the latest stage of island formation.     

Effect of lateral morphology formation of polymer blend towards patterning silane-based SAMs using selective dissolution method

A number of strategies have been developed including soft lithography and photolithography for patterning various surfaces. Here we have discussed a customized strategy for surface patterning of nanosized, silane-based SAMs and monolayer thickness measurement investigated using atomic force microscope (AFM). We have utilized the versatile morphology of a binary polymer blend to generate patterned SAMs over silicon substrate by employing a selective dissolution procedure. This method was confirmed with different organosilanes with varying number of C-atoms and to other polymer blend. The samples were imaged both in tapping mode and pulsed force mode AFM.     

Studies on ZDDP Thermal Film Formation by XANES Spectroscopy, Atomic Force Microscopy, FIB/SEM and 31P NMR

X-ray absorption near edge structure (XANES) spectroscopy has been used to characterize the chemistry of thermal films on steel samples, which were generated from a mineral base oil containing a zinc dialkyl dithiophosphate (ZDDP) additive. These films were formed at 150 °C by immersing steel coupons in ZDDP oil solutions. The phosphorus L-edge XANES spectra show that these films are composed of polyphosphates, unreacted ZDDP and other thiophosphate intermediates. Phosphorus K-edge FY XANES was used to monitor the thickness of these films, and the data are consistent with thickness derived by focussed ion beam (FIB) milling and SEM imaging. The sulphur K-edge TEY and FY XANES spectra show that these films are composed of different sulphur components, which depend upon the formation times. The surface morphology of these films was investigated using atomic force microscopy (AFM). These images show that the surface morphology of the thermal films changes with the formation time. 31P NMR spectra show that both primary and secondary ZDDP decomposes gradually at 150 °C.