TiN薄膜在纳米压痕和纳米划痕下的断裂行为

利用磁控溅射方法在Si(111)衬底上制备了具有(111)和(222)择优取向的TiN薄膜. 用纳米压痕和纳米划痕方法研究了该薄膜的变形和断裂行为. 用扫描电子显微镜、纳米压痕原位原子力显微镜及原位光学显微镜并结合加-卸载 曲线及划痕曲线获得了薄膜发生变形和断裂的微观信息. 在压痕试验中, TiN薄膜在压入深度为200 nm时表现为塑性变形及压痕周围的局部断裂, 随着压入深度的增大, 塑性变形和局部断裂变得越显著, 当最大压入深度达到临界值1000 nm时, 薄膜和衬底间发生了界面断裂. 在划痕实验中, 100 mN及200 mN的最大载荷均可以引起界面断裂. 最大为200 mN的载荷使得薄膜发生界面断裂的位置比用100 mN载荷时的位置提前, 但其临界断裂载荷和100 mN时及压痕实验时的临界界面断裂载荷基本相同. 关键词： TiN薄膜 纳米压痕 纳米划痕 界面断裂     

Effects of cold rolling deformation on microstructure,hardness, and creep behavior of high nitrogen austenitic stainless steel

Effects of cold rolling deformation on the microstructure, hardness, and creep behavior of high nitrogen austenitic stainless steel （HNASS） are investigated. Microstructure characterization shows that 70% cold rolling deformation results in significant refinement of the microstructure of this steel, with its average twin thickness reducing from 6.4 μm to 14 nm. Nanoindentation tests at different strain rates demonstrate that the hardness of the steel with nano-scale twins （nt-HNASS） is about 2 times as high as that of steel with micro-scale twins （mt-HNASS）. The hardness of nt-HNASS exhibits a pronounced strain rate dependence with a strain rate sensitivity （m value） of 0.0319, which is far higher than that of mt-HNASS （m = 0.0029）. nt-HNASS shows more significant load plateaus and a higher creep rate than mt-HNASS. Analysis reveals that higher hardness and larger m value of nt-HNASS arise from stronger strain hardening role, which is caused by the higher storage rate of dislocations and the interactions between dislocations and high density twins. The more significant load plateaus and higher creep rates of nt-HNASS are due to the rapid relaxation of the dislocation structures generated during loading.     

血红细胞力学性能的纳米压痕实验和有限元模拟

采用纳米压痕技术和有限元方法研究了血红细胞的生物力学性能. 进行了血红细胞的纳米压痕实验, 得到了血红细胞的材料参数和变形形貌; 在实验基础上, 建立了血红细胞的三维有限元模型, 模拟了血红细胞的压痕载荷-位移曲线, 并考虑了参数效应. 数值模拟结果和实验数据符合很好. 通过改变压头与材料之间的摩擦系数和压头曲率半径等参数, 比较了载荷-位移曲线的变化情况. 研究表明摩擦系数对压痕载荷-位移曲线和应力分布影响很小, 而压头曲率对载荷-位移曲线的影响明显.     

Ti、TiN、TiO2改性层的纳米力学性能测试与分析

采用等离子表面合金化技术,分别在316L不锈钢表面制备出渗Ti改性层、渗TiN改性层和TiO2改性层薄膜.使用连续刚度法,从截面方向和表面方向对改性层进行纳米压痕实验,研究改性层的纳米力学性能.实验测得材料在压痕过程中的载荷—位移曲线以及硬度和模量随压入深度的连续变化值.结果表明,改性层纳米力学特性表现为各向异性;TiN改性层的力学性能表现良好.TiO2改性层由渗Ti改性层经氧化制成,二者的弹性模量和硬度在截面方向上变化规律相似,在表面方向上数值相近.     

Influence of graphene nanoscrolls on the crystallization behavior and nano‐mechanical properties of polylactic acid

Graphene nanoscrolls (GNS), one‐dimensional carbon‐based nanomaterials, have been predicted to possess extraordinary characteristics due to their unique open topology with scrolled graphene monolayers. In this study, the conversion of planar 2‐D graphene nanoplatelets (GNPs) to tubular and scrolled 1‐D GNSs is described. The effects of GNS as a nucleating agent to modulate the morphology, crystallization, and nano‐mechanical properties of polylactic acid (PLA) were studied. The nucleating effect of GNS and its unique topological characteristics proves to influence the crystallization of PLA. Fourier transform infrared (FTIR) spectroscopy indicated nonpreferential interactions of PLA chains around GNS due to the bulky and helical PLA macromolecular chains. Superior interfacial interactions and strain in GNS provide better load transfer between GNS and PLA matrices, resulting in higher modulus and hardness. This study is the first detailed analysis to elucidate the role of unique GNS to favorably modulate the properties of a polymer.     

New Nanoindentation and Nanoscratching Parameters of Thermoplastics

Summary: The determination of hardness and modulus values from unloading curves in nanoindentations is particularly troublesome with thermoplastic polymers and the values can strongly depend on the maximal normal force. Quantitative analysis of the loading curves provides reliable nanoindentation coefficients k (µN nm^−3/2) as the slopes of linear plots that reliably characterize the pristine polymers and are potent interpolation tools. Kinks in the linear plots (here not observed with isotactic polypropylene (PP-it)) indicate plastic-viscoelastic transformations and separate the characterization of the degraded polymer with the smaller nanoindentation coefficients from the pristine polymer. The quantitative analysis of the correct relation between lateral and normal force in nanoscratching reveals the coefficient K (µN^−1/2) as a basic extrapolation tool with direct and quantitative access to scratch resistance as a measure for wear that replaces the unfounded and never constant so-called “friction coefficient F_L/F_N”. The linear plots of the correct relation between lateral and normal force reveal the occurrence of plastic-viscoelastic transformations most distinctly by a kink and two linear ranges.     

High‐Throughput Method for Determining Modulus of Polymer Blends

Summary: A method for rapidly determining the modulus of polymer blends was developed. A polymer blend gradient library of poly(L ‐lactic acid) (PLLA) and poly(D ,L ‐lactic acid) (PDLLA) was created in the form of a strip‐shaped film and characterized with FTIR microspectroscopy. Nanoindentation measurements were made along the gradients to obtain modulus data over a wide range of PLLA‐PDLLA blend compositions. This novel, high‐throughput approach to material characterization provides engineers with a technique to accelerate the development of materials.

Deposition of the polymer composition gradient.     

On the extreme depth dependence of the hardness of PDMS rubber: A problem of false surface detection

There is significant interest in nanoindentation of materials yet mixed results for material properties have been reported, including modest depth dependence of the surface stiffness in metals and other crystalline materials and polymer glasses, as well as stiffening of several orders of magnitude in some studies of soft materials such as poly(dimethylsiloxane) (PDMS) rubber. At the same time, there are reports that suggest that the observed extreme stiffening in soft materials might be an artifact, and that such materials at most exhibit only mild stiffening. Unfortunately, a quantitative model of potential artifacts has not been provided. In the present work, we examine the problem of one potential artifact in the testing of soft materials, that of the difficulty of detecting the surface or “true zero” in the indentation test. We provide a quantitative estimate of the effect of error in surface detection on the measured force–displacement curves for the Berkovich tip geometry and find that the observed apparent stiffening is in agreement with our analysis. The significance of the results for testing of soft materials by nanoindentation is discussed. It is also shown that for hard/stiff materials the induced errors are smaller, but may still be significant in some circumstances. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2017 , 55, 30–38     

Effect of annealing temperature on interrelation between the microstructural evolution and plastic deformation in polymers

The mechanical loading induced flow of glassy polymers is triggered by the nucleation of shear transformation units, and strongly depends on the initial microstructural state of the material. Therefore, investigation of the possible relationship between the microstructural state variables and plastic deformation is required for a better understanding of the macroscopic response of this class of materials during large deformation. In this study, free volume content is considered as a state variable and thermal treatment is selected as a process through which the accelerated and forced evolution of the free volume can be imposed. For two well‐known glassy polymers, poly(methyl methacrylate) and polycarbonate, the free volume content alteration upon annealing is monitored via positron annihilation spectroscopy, and the changes of the micro‐ and macromechanical properties are also obtained by utilizing nanoindentation technique and employing the homogeneous amorphous flow theory. The correlation between the microstructural state variable, that is, free volume, and the micromechanical state variable, that is, shear activation volume, is then investigated. The results reveal opposite direction of alterations of free volume and shear activation volume with annealing temperature. Accordingly, the possibility of the existence of an interrelation between these two state variables is critically discussed. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2017 , 55, 1286–1297     

Efficient Cu(I) acetate‐catalyzed cycloaddition of multifunctional alkynes and azides: From solution to bulk polymerization

“Click” chemistry is an effective and commonly used technique in polymer chemistry for the synthesis and modification of polymers. In this study, the bulk polymerization of multifunctional alkynes and azides was achieved by the copper(I)‐catalyzed alkyne–azide 1,3‐dipolar cycloaddition. The influence of different catalyst systems on the polymerization kinetics of the “click”reaction were evaluated by differential scanning calorimetry. Surprisingly, Cu(I) acetate showed the most efficient catalytic behavior among the applied Cu(I) salts. The polymerization kinetics in solution were investigated by 1H NMR spectroscopy and size exclusion chromatography. According to the 1H NMR investigation the copper(I)‐catalyzed cycloaddition follows a second‐order kinetics with external catalysis. Additionally, the mechanical properties of the resulting polymers were investigated by depth sensing indentation. Thereby the polymerizations of the alkyne tripropargylamine with the azides 1,3‐bis(azidomethyl)benzene and 1,4‐bis(azidomethyl)benzene resulted in mechanical hard materials. Furthermore, the combination of the alkynes tripropargylamine and di(prop‐2‐yn‐1‐yl) isophorone dicarbamate and polymerization with 1,2‐bis(2‐azidoethoxy)ethane resulted in high indentation moduli. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 239–247