纳米金刚石对电沉积镍基复合镀层微观结构及抗磨性能的影响

利用直流电沉积技术制备了纳米和微米镍镀层,以及纳米金刚石增强镍基复合镀层,考察了纳米金刚石颗粒对纳米及微米镍基质的表面形貌、微结构、硬度及磨损性能的影响．结果表明：引入纳米金刚石使得微米镍镀层的硬度和抗磨性能显著提高;但引入纳米金刚石对纳米镍镀层硬度的影响不大,对镀层的抗磨性能则反而产生不利影响．     

微/纳米制造技术的摩擦学挑战

评述了国内外航天、信息和军事等高技术领域中微/纳米制造技术的研究现状和发展趋势,介绍了微/纳米制造技术特征及其关键技术问题,揭示了当器件的尺度由毫米量级减小到微米甚至纳米量级时,微器件材料表面和界面的摩擦学(摩擦磨损及润滑)、力学和化学等及其控制方法是微/纳米制造研究中急需解决的关键技术问题.这些问题的解决对摩擦学研究提出了严峻挑战,新的摩擦学理论和技术的出现将为微/纳米制造技术的发展以及相关问题的解决提供保障.     

真空磁过滤电弧离子镀法制备DLC膜的机械性能

采用真空磁过滤电弧离子镀法分别在9Cr18和40CrNiMo钢上沉积厚约为0.2μm的类金刚石（DLC）膜。为了检测成膜质量，分别使用纳米压痕和纳米划痕技术表征钢基材和DLC/基材的机械性能，对这种亚微米厚的膜，纳米压痕技术和纳米划痕技术能提供丰富的近表面的弹塑性变形，断裂和摩擦等的信息。同DLC/40CrNiMo相比。DLC/9Cr18的硬度高和固体润滑效果显著，9Cr18是较为理想的基体材料。     

影响纳米压入测试结果的因素

纳米硬度计 ,又称深度测量压入仪。该仪器在刚性压针上施加特定载荷 ,同时记录压入试样深度。此技术广泛应用于微纳米尺度力学性能的研究。以MTSNanoIndenter○RXP为测试手段 ,参考试样熔融硅为研究对象 ,进行了不同压入深度的测试。结果显示 ,硬度和模量有随压入深度减小而增大的趋势。分析了接触零点的确定、压针尖端缺陷、试样表面的吸湿和粗糙度、弹塑性转变等因素对测试结果的影响。在压入深度为微米和亚微米量级时 ,上述因素对测试结果无显著影响 ;而在纳米量级时 ,有显著影响。所以 ,当压入深度为几十纳米时 ,纳米压入测试结果的可靠性值得注意     

氮化钛沉积膜的摩擦性能研究

采用等离子电弧沉积法在9Crl8钢表面制备了厚约0．5μm的TiN薄膜，通过显微硬度测试以及纳米压痕和纳米划痕试验，对比考察了9Crl8钢及其表面T|N薄膜的机械和摩擦性能．结果表明，9Crl8钢及其表面T．N沉积膜的纳米硬度分别为8GPa和38GPa，弹性模量分别为250GPa和580GPa，9Crl8、TiN和有机薄膜的摩擦系数分别为0．40、0．12和0．10；TiN沉积膜可显著提高基体钢的承载和耐磨能力．     

亚微米氮化钛膜的纳米压痕和划痕测定

采用等离子电弧沉积的方法，分别在GT35和40CrNiMo钢上沉积厚约为0．5μm的氮化钛(TiN)膜．为了筛选基材，采用纳米压痕和划痕技术，评价膜基界面结合和固体润滑效果．纳米压痕结果，GT35，40CrNiMo和TiN的纳米硬度／弹性模量的典型值分别约为11．5GPa／330GPa，6．0GPa／210GPa，30GPa／450GPa．纳米划痕结果，GT35有较理想的膜基结合能力；GT35，40CrNiMo，TiN及其有机膜的摩擦系数分别约为0．25，0．45，0．i5，0．i0．同40CrNiMo相比，GT35是较为理想的基体材料．纳米压痕和划痕技术能提供丰富的近表面的弹塑性变形、断裂和摩擦等的信息，是评价亚微米薄膜力学性能的有效手段．     

微米/纳米尺度的材料力学性能测试

针对如何定量测定纳米、微米尺度及低维材料的力学性能,叙述了采用当今先进观测手段,结合设备特点和力学分析技术来评价材料的硬度、弹性模量、屈服应力、抗蠕变及抗疲劳性等力学性能的测试方法．     

Nano-WC/PTFE-Ni复合电刷镀层的磨损性能研究

采用电刷镀技术在Q235钢基材上制备含纳米WC和PTFE的镍基复合镀层,采用S-2700型扫描电子显微镜观察镀层表面形貌及其显微组织,采用HX-1型显微硬度计测定镀层的显微硬度,采用WS-2005型涂层附着力自动划痕仪测定镀层与基体的结合强度,采用HT-500型销-盘高温摩擦磨损试验机测量镀层的滑动磨损性能.结果表明:镀液中同时加入纳米WC和PTFE可以得到表面形貌平整、纳米粒子分布均匀的纳米复合镍镀层;复合镀层的硬度随WC含量的增加而增大,随PTFE含量的增加而减小;含有2种纳米粒子的复合镍镀层的耐磨性比镍镀层和含单一WC或PTFE的镍镀层的耐磨性优良;当镀液中WC和PTFE含量分别为3.0 g/L和7.5 mL/L时,复合镍镀层的显微硬度较镍镀层提高约30%,耐磨性较镍镀层提高7倍.     

堆焊熔敷层表面纳米晶层摩擦磨损性能研究

用预压力滚压技术在堆焊修复层表面制备纳米晶层.利用TEM、SEM分析技术研究表面纳米晶层微观结构,利用CETR-3型多功能摩擦磨损试验机考察在干摩擦条件下堆焊层表面纳米晶层的摩擦磨损性能.结果表明堆焊修复层表面经表面纳米化处理后,表面形成厚度约为10μm(晶粒尺寸小于100 nm)的纳米晶层,最表面层平均晶粒尺寸约为10 nm.纳米压痕试验表明纳米晶层的硬度提高,最表面纳米晶层的硬度约为原始堆焊层硬度的3倍.与原始堆焊试样相比,表面纳米化试样的摩擦系数降低了10%,磨损体积降低了25%~30%左右.表面纳米化样品的磨损机制由原始堆焊层的磨粒磨损和黏着磨损转变为磨粒磨损,分析表明晶粒细化导致的高硬度、低塑性是摩擦磨损性能改善和磨损机制改变的主要原因.     

电刷镀Ni-PTFE纳米复合镀层的摩擦特性研究

利用电刷镀技术在A3钢基底上制备了Ni-PTFE纳米复合镀层;采用S-2700型扫描电子显微镜观察纳米复合镀层经抛光腐蚀后的表面形貌;采用HX-1000型显微硬度计测量复合镀层的显微硬度;采用MXTX S/X 20-0186型划痕试验仪测量纳米复合镀层的表面粗糙度和定载荷及变载荷作用下镀层的摩擦系数.结果表明:PTFE可以使复合镀层的组织致密,降低复合镀层的硬度和表面粗糙度;在室温、较小载荷及干摩擦条件下,PTFE可以降低复合镀层的摩擦系数(最低降至0.046);复合镀层和普通镀层的摩擦系数均随载荷的增加而增大;在较低载荷作用下,复合镀层的摩擦系数小于普通镀层的摩擦系数.     

Anisotropic Mechanical Properties of SAC Solder Joints in Microelectronic Packaging and Prediction of Uniaxial Creep Using Nanoindentation Creep

In this paper, the mechanical properties and creep behavior of lead-free solder joints has been characterized by nano-mechanical testing of single grain SAC305 solder joints extracted from plastic ball grid array (PBGA) assemblies. The anisotropic mechanical properties characterized include the elastic modulus, hardness, and yield stress. An approach is suggested to predict tensile creep strain rates for low stress levels using nanoindentation creep data measured at very high compressive stress levels. The uniaxial creep rate measured on similarly prepared bulk (large) specimens was found to be of the same order-of-magnitude as the creep rate observed in single-grain BGA joints, with chararacteristically (slightly) higher creep strains measured during nanoindentation. This suggests that the same creep mechanism operates in both size domains. Electron backscattered diffraction (EBSD) and nanoindentation testing further showed that the modulus, hardness, and creep properties of solder joints are highly dependent on the crystal orientation.     

Extraction of Mechanical Properties with Second Harmonic Detection for Dynamic Nanoindentation Testing

In this article, a new method based on the detection of the second harmonic of the displacement signal to determine mechanical properties of materials from dynamic nanoindentation testing, is presented. With this technique, the Young’s modulus and hardness of homogeneous materials can be obtained at small penetration depths from the measurement of the second harmonic amplitude. With this innovative method, the measurement of the normal displacement is indirectly used, avoiding the need for very precise contact detection. Moreover, the influence of the tip defect and thermal drift on the measurements are reduced. This method was used for dynamic nanoindentation tests performed on fused silica and on an amorphous polymer (PMMA) because these materials are supposed not to exhibit an indentation size effect at small penetration depths. The amplitude of the second harmonic of the displacement signal was correctly measured at small depths, allowing to calculate the Young’s modulus and the hardness of the tested materials. The mechanical properties calculated with this method are in good agreement with values obtained from classical nanoindentation tests.     

Hierarchical structure observation and nanoindentation size effect characterization for a limnetic shell

In the present research, hierarchical structure observation and mechanical property characterization for a type of biomaterial are carried out. The investigated biomaterial is Hyriopsis cumingii, a typical limnetic shell, which consists of two different structural layers, a prismatic "pillar"structure and a nacreous "brick and mortar" structure. The prismatic layer looks like a "pillar forest" with variationsection pillars sized on the order of several tens of microns.The nacreous material looks like a "brick wall" with bricks sized on the order of several microns. Both pillars and bricks are composed of nanoparticles. The mechanical properties of the hierarchical biomaterial are measured by using the nanoindentation test. Hardness and modulus are measured for both the nacre layer and the prismatic layer, respectively.The nanoindentation size effects for the hierarchical structural materials are investigated experimentally. The results show that the prismatic nanostructured material has a higher stiffness and hardness than the nacre nanostructured material.In addition, the nanoindentation size effects for the hierarchical structural materials are described theoretically, by using the trans-scale mechanics theory considering both strain gradient effect and the surface/interface effect. The modeling results are consistent with experimental ones.     

Nanomechanical Property and Nanowear Measurements for Sub-10-nm Thick Films in Magnetic Storage

In the magnetic storage industry, thin film carbon overcoats play a critical role in reducing magnetic and physical spacing between the recording slider and the rotating disk so that the information stored per unit area is maximized. Thin film carbon overcoats have been improved such that they exhibit higher hardness with lower thickness of few nanometers and still being able to perform reliably. In this paper, nanoindentation and nanoscratch techniques to measure nanomechanical properties, namely hardness, elastic modulus and shear strength of thin solid films were presented along with a recently developed high resolution force transducer. Nanowear behavior characterization techniques were also examined and were applied to commercially available magnetic disks to characterize their wear behavior. It was shown that the properties and wear behavior of sub-10-nm thick film carbon overcoats were reliably measured. These techniques could be applied to different thin solid films on substrates, and they are not restricted to magnetic storage systems.     

不锈钢表面等离子合金化渗铜层的纳米力学性能研究

为了研究不锈钢渗铜层的纳米力学性能,本文采用等离子表面合金化技术在304不锈钢表面制备了渗铜层。利用纳米压入硬度仪,采用连续刚度测试法,对渗铜层以及不锈钢基体的表面和横截面的纳米力学性能进行了测试,得到了纳米压入过程的载荷-压入深度曲线,发现渗铜层抵抗外载荷的能力低于不锈钢基体。并得到了渗铜层和不锈钢基体的表面、横截面方向的硬度以及杨氏模量,经对比得到渗铜层的杨氏模量和硬度都要比不锈钢基体的低,并且渗铜层的力学性能表现出各向异性。对纳米压入的数据进行分析,发现渗铜层在小尺度压入时硬度和杨氏模量表现出明显的"尺度效应"。     

Determination of elastic and plastic mechanical properties of dentin based on experimental and numerical studies

The aim of this study is to investigate the change of mechanical properties of human dentin due to aging and spatial variation. Sections of coronal dentin are made from human molars in three groups: young, mid-aged, and old patients. A nanoindentation test is conducted from regions near the pulp to the dentin-enamel junction (DEJ) to evaluate the load-depth indentation response and determine Young's modulus and hardness. Based on the loading and unloading load-displacement curves in nanoindentation, a numerical model of plastic damage is used to study the plastic and the damage behaviors and the contribution to the degradation in the unloading stiffness. The experimental results show that Young's modulus of the inner dentin is significantly lower than that of outer dentin in each age group. Compared with the young dentin, the old dentin has greater hardness and Young's modulus with similar spatial variations. The magnitudes of the yield strength and the damage variable are also affected by aging and vary with spatial locations. In the same age group, the yield strength in inner dentin is lower than those in middle and outer dentin, more damage occurs with similar spatial variations, and the yield strength of young dentin is generally lower and causes more damage compared with those in both the mid-aged and old groups.     

纳米压痕仪接触投影面积标定方法的研究

基于Oliver与Pharr方法的纳米压痕实验以其简单方便获得广泛的应用，但众多因素对压 痕实验结果的影响范围并无明确的结论. 其中压痕接触面积的确定是一个重要环节，该因素 对实验结果，特别是小深度下的实验结果具有重要影响. 仔细分析了Oliver与Pharr 方法并进行了几种材料的纳米压痕实验，针对该方法在接触深度确定、不同深度范围下方法 的适用性进行了说明. 分析结果表明，对所有的材料使用统一的面积公式，只有在大压痕深 度时才是适用的，而在小压痕深度时可能带来较大的误差. 因此，应慎重使用由Oliver与 Pharr方法得到的小压痕深度的硬度数据.     

Influence of Vickers tip imperfection on depth sensing indentation tests

In the last decade, the development of depth sensing indentation equipment has permitted two of the most conventional mechanical properties of materials to be easily determined: hardness and Young’s modulus. Some care is needed to accurate results from the experimental determination of the aforementioned mechanical properties. In this study, numerical simulations were performed on two well-known materials (Bk7 glass, AISI M2 steel) and on fictitious materials with a wide range of mechanical properties, using Vickers indenters with different sizes of tip imperfections. The purpose is to estimate the influence of the size of the defect on the hardness and Young’s modulus results obtained by ultramicro and nanoindentation tests.     

Development of High Temperature Nanoindentation Methodology and its Application in the Nanoindentation of Polycrystalline Tungsten in Vacuum to 950 °C

The capability for high temperature nanoindentation measurements to 950 °C in high vacuum has been demonstrated on polycrystalline tungsten, a material of great importance for nuclear fusion and spallation applications and as a potential high temperature nanomechanics reference sample. It was possible to produce measurements with minimal thermal drift (typically ~0.05 nm/s at 750–950 °C) and no visible oxidative damage. The temperature dependence of the hardness, elastic modulus, plasticity index, creep, creep strain, and creep recovery were investigated over the temperature range, testing at 25, 750, 800, 850, 900 and 950 °C. The nanoindentation hardness measurements were found to be consistent with previous determinations by hot microhardness. Above 800 °C the hardness changes relatively little but more pronounced time-dependent deformation and plasticity were observed from 850 °C. Plasticity index, indentation creep and creep recovery all increase with temperature. The importance of increased time-dependent deformation and pile-up on the accuracy of the elastic modulus measurements are discussed. Elastic modulus measurements determined from elastic analysis of the unloading curves at 750–800 °C are close to literature bulk values (to within ~11 %). The high temperature modulus measurements deviate more from bulk values determined taking account of the high temperature properties of the indenter material at the point (850 °C) at which more significant time-dependent deformation is observed. This is thought to be due to the dual influence of increased time-dependency and pile-up that are not being accounted for in the elastic unloading analysis. Accounting for this time-dependency by applying a viscoelastic compliance correction developed by G. Feng and A.H.W. Ngan (J. Mater. Res. (2002) 17:660–668) greatly reduces the values of the elastic modulus, so they are agree to within 6 % of literature values at 950 °C.     

Nonlinearly Viscoelastic Nanoindentation of PMMA Under a Spherical Tip

The Oliver-Pharr method has been well established to measure Young’s modulus and hardness of materials without time-dependent behavior in nanoindentation. The method, however, is not appropriate for measuring the viscoelastic properties of materials with pronounced viscoelastic effects. One well-known phenomenon is the formation of unloading “nose” or negative stiffness during unloading that often occurs during slow loading-unloading in nanoindentation on a viscoelastic material. Most methods in literature have only considered the loading curve for analysis of viscoelastic nanoindentation data while the unloading portion is not analyzed adequately to determine the nonlinearly viscoelastic properties. In this paper, nonlinearly viscoelastic effects are considered and modeled using the nonlinear Burgers model. Nanoindentation was conducted on poly-methylmethacrylate (PMMA) using a spherical indenter tip. An inverse problem solving approach is used to allow the finite element simulation results to agree with the nanoindentation load–displacement curve during the entire loading and unloading stage. This approach has allowed the determination of the nonlinearly viscoelastic behavior of PMMA at submicron scale. In addition, the nanoindentation unloading “nose” has been captured by simulation, indicating that the negative stiffness in the viscoelastic material is the result of memory effect in time-dependent materials.