Platinum/iridium/carbon: a high-resolution shadowing material for TEM,STM and SEM of biological macromolecular structures

Thin Pt/Ir/C coating films (1.5 nm) show a fine granularity and provide a high structural resolution in the transmission electron microscope (TEM) when applied to freeze-dried biological macromolecules. They keep their structure when exposed to atmospheric conditions, without the need of an additional stabilizing carbon layer, in contrast to conventional high-resolution shadowing materials such as Ta/W and Pt/C. However, the correct ratio of the components has turned out to be crucial. When evaporating Pt/Ir/C from the source electrode in an electron-beam-heated evaporator, the ratio of the three elements changes progressively, and, consequently, the properties of such films depend strongly on the mass that has been pre-evaporated. In this paper we present a quantitative analysis of the composition of Pt/Ir/C films by wavelength-dispersive X-ray analysis (WDX) undertaken in association with TEM experiments. We applied Pt/Ir/C shadowing to two regular biological test specimens, the phage T4 type III polyhead and the HPI-layer of Deinococcus radiodurans. It turns out that Pt/Ir/C films containing at least 25% C are three-dimensionally stable on the freeze-dried macromolecular samples. By the dramatically improved resolution power of the latest scanning electron microscopes (SEM) and the invention of the scanning tunnelling microscope (STM), two new surface-sensitive tools for the investigation of biological macromolecular structures became available. The Pt/Ir/C coating has proved to be well suited for STM and SEM imaging of freeze-dried biological structures because of its good electrical conductivity and its direct three-dimensional stability. We compare STM, SEM and TEM images of freeze-dried and Pt/Ir/C-coated polyheads.     

Improved handling of structural fragile cell-biological specimens during electron microscopic preparation by the exchange method

An exact method of preparation of soft biological specimens for electron microscopic analysis of surface fine structures is described. It allows routine preparations of fragile specimens for SEM and TEM imaging modes. With this procedure physical preparation parameters such as mechanical loads on the specimen surface or changes of temperature are controlled. The wet specimens are premounted in cheap disposable BEEM-containers or glass boats and are constantly kept under liquid in a closed system. The exchange of preparation media is performed continuously and, if necessary, over gradients. For comparative investigations with different EM-modes, at each step of the procedure parts of the specimens may be removed for individual processing. Conventionally prepared critical-point dried specimens are compared to those processed by the exchange technique and preservation of surface fine structures is demonstrated. Shadow-casted clathrin cages and stereo-replicas of virus infected cell cultures are shown in TEM preparations. For SEM, coverslip cell cultures and isolated glomerulus basement membranes are prepared and an additional flat embedding for TEM ultrathin sections is demonstrated.     

Low cycle fatigue of pps polymer injection welds (II) — fiber orientation and fracture mechanism

The polymer composites contain numerous internal boundaries and its structural elements have different responses and different resistances under the same service environment. Fatigue phenomenon is much more complex in composites than homogeneous materials. An understanding of the fracture behavior of polymer composite materials subjected to constant and cyclic loading is necessary for predicting the life time of structures fabricated with polymers. There is a need to acquire a better understanding of the fatigue performance and failure mechanisms of composites under such conditions. Therefore, in this study the analyses of fiber orientation and fracture mechanism for low cycle fatigue crack have been studied by SEM and LM for observing the ultrathin sections.     

Developing a manufacturing technology for the components made of a multiphase perfect material

A component made up of a perfect combination of different materials (most often including homogeneous materials and three different types of heterogeneous materials, i.e., composite materials, functionally graded materials, and heterogeneous materials with a periodic microstructure) in its different portions for a specific application is considered to be a component made of a multiphase perfect material. To design and represent such components, a corresponding computer-aided design method and a CAD modeling method have been developed. Although, there is no existing manufacturing method and facility for such components. Their fabrication entails four steps described in this paper: analysis of the requirements of their manufacture; review of the currently available layered manufacturing, micro-fabrications, and hybrid manufacturing technologies; presentation of a new hybrid layered manufacturing technology (including its manufacturing process and the principle scheme of its corresponding manufacturing facilities); and implementation of the manufacturing simulation by means of virtual manufacturing technology.     

The application of magnetic structural phase analysis for the diagnostics of the State of a 08X18H10T Steel-Ct3 Steel composite material and its components that were subjected to plastic deformation

The use of composite, in particular, multilayer materials, is one way to decrease the specific quantity of metal in an item and to increase its service characteristics. To develop methods for the diagnostic of the state of such composite materials and their components, the effect of cold rolling on the structure, magnetic, and mechanical properties of a two-ply composite material and its separate components was studied; the material was prepared by explosion welding of austenitic corrosion-resistant and low-carbon steels. It was shown that magnetic characteristics can be used for estimating the degree of deformation by rolling, phase composition, and mechanical properties of both two-ply 08X18H10T Steel-C^t3 Steel composite material as a whole and its separate components.     

Multi‐walled carbon nanotubes decorated by platinum catalyst nanoparticles—Examination and microanalysis using scanning and transmission electron microscopies

Carbon nanotubes (CNTs) decorated with platinum (Pt) nanoparticles (NPs) have been characterized using a cold field‐emission scanning electron microscope (SEM) and a high resolution field‐emission transmission electron microscope (TEM). With this particular composite material, the complementary nature of the two instruments was demonstrated. Although the long CNTs were found to be mostly bent and defective in some parts, the nucleation of Pt occurred randomly and uniformly covered the CNTs. The NPs displayed a large variation in size, were sometimes defective with twins and stacking faults, and were found to be faceted with the presence of surface steps. The shape and size of the NPs and the presence of defects may have significant consequences on the activity of the Pt catalyst material. Also, thin layers of platinum oxide were identified on the surface of some NPs.     

直升机复合材料桨叶的疲劳寿命计算

着重说明直升机复合材料桨叶安全寿命的计算方法。首先分析某型直升机的飞行任务剖面、桨叶载荷谱及材料的疲劳特性,然后利用迈勒线性累积损伤理论计算桨叶的安全疲劳寿命,并分析不同飞行状态及载荷变化对疲劳寿命的影响。计算结果证实直升机复合材料桨叶在正常飞行状态下的无限寿命设计理念。该方法可用于在直升机设计阶段对复合材料构件的疲劳寿命进行评估校核。     

Atomic force microscopy of histological sections using a chemical etching method

Physiology and pathology have a big deal on tissue morphology, and the intrinsic spatial resolution of an atomic force microscope (AFM) is able to observe ultrastructural details. In order to investigate cellular and subcellular structures in histological sections with the AFM, we used a new simple method for sample preparation, i.e. chemical etching of semithin sections from epoxy resin-embedded specimens: such treatment appears to melt the upper layers of the embedding resin; thus, removing the superficial roughness caused by the edge of the microtome knife and bringing into high relief the biological structures hidden in the bulk. Consecutive ultrathin sections embedded in epoxy resin were observed with a transmission electron microscope (TEM) to compare the different imaging properties on the same specimen sample. In this paper we report, as an example, our AFM and TEM images of two different tissue specimens, rat pancreas and skeletal muscle fibres, showing that most of the inner details are visible with the AFM. These results suggest that chemical etching of histological sections may be a simple, fast and cost-effective method for AFM imaging with ultrastructural resolution.     

Estimation of residual strength of components of composite constructions after low-speed impact

A methodology of computing the damageability of composite materials at low-speed impact is suggested. The methodology is based on applying a fracture criterion of the monolayer and following computation of material damageability taking the interaction of different damage evolution mechanisms into account. This approach allows us to obtain the distribution of damageability parameters in the surface of the monolayer and the width of material at an arbitrary moment of time until complete destruction of the construction component, computing the degradation of elastic properties, and the position and sizes of delamination regions after the impact. Applying this methodology for estimating residual strength permits the avoidance of excessive conservatism of the projected strength of construction components from composite materials which have incurred impact damage.     

颗粒增强复合材料弹性结构的双尺度有限元分析

颗粒增强方法是实现材料高性能化的重要手段。预测颗粒增强复合材料的细观结构与力学性能的关系是实现材料增强增韧的基础。为更好地分析、设计和优化复合材料,需要引入多尺度计算模型来考察细观结构对宏观力学性能的影响。基于均匀化理论,采用Voronoi有限元法对颗粒增强复合材料进行细观数值模拟,从而预测材料的宏观等效弹性常数,并直接得到材料的细观应力场。在细观尺度,首先假设满足平衡条件的应力场,采用Voronoi应力单元建立余能泛函并得到细观控制方程,最终形成可直接求解的线性代数方程组,从而求得应力系数并得到细观应力场。在宏观尺度,利用商业有限元软件ANSYS来进行宏观结构分析。通过均匀化方法求得弹性模量的宏观平均值,将其输入ANSYS系统即可进行计算,由此把宏细观两个尺度耦合起来,可以对颗粒增强复合材料构成的结构体进行有效的力学分析。     

Microwave-assisted rapid plant sample preparation for transmission electron microscopy

The preparation of plant leaf material for transmission electron microscopical investigations can be a very time- and labour-consuming task as the reagents infiltrate the samples quite slowly and as usually most steps have to be performed manually. Fixation, buffer washes, dehydration, resin infiltration and polymerization of the resin-infiltrated leaf samples can take several days before the specimen can be cut ultrathin and used for ultrastructural investigations. In this study, we present a microwave-assisted automated sample preparation procedure that reduces preparation time from at least 3 days to about 5 h – with only a few steps that have to be performed manually – until the plant sample can be ultrathin sectioned and observed with the transmission electron microscope. For studying the efficiency of this method we have compared the ultrastructure of different leaf material ( Arabidopsis thaliana , Nicotiana tabacum and Picea abies ) which was prepared with a conventional, well-established chemical fixation and embedding protocol and a commercially available automated microwave tissue processor. Despite the massive reduction in sample preparation time no negative effects on cutting properties of the blocks, stability of the sections in the electron beam, contrast and ultrastructure of the cells were observed under the transmission electron microscope when samples were prepared with the microwave-assisted protocol. Additionally, no negative effects were detected on the dimensions of fine structures of grana stacks (including membranes, inter- and intrathylakoidal spaces), the nuclear envelope and the plasma membrane as the diameter of these structural components did not differ between leaf samples (of the same species) that were processed with the automated microwave tissue processor or by conventional fixation and embedding at room temperature.     

基于空耦超声共振法的复合材料测厚技术研究

为解决当前传统超声检测技术对复合材料的检测耦合剂污染和检测效率低等问题,提出空气耦合超声共振法来检测复合材料薄板的厚度,从而确定缺陷的大小。利用 COMSOL 有限元仿真软件对复合材料进行建模,设置不同厚度及不同大小缺陷的物理模型来对比实验,后处理求解并进行快速傅里叶变换,提取谐振频率计算出复合材料的厚度。结果表明,超声共振法可对复合材料进行定性、定量检测;当复合材料的厚度越薄时,超声信号产生的谐振频率越大,则复合材料中所含缺陷范围越广,分层现象越严重;其检测精度可达 0.1 mm 左右,相对误差范围分布在 5% 以下。实验证明了该测厚技术的可靠性,为超薄复合材料板缺陷厚度的测量提供一定的参考和借鉴。     

DC potential drop method for evaluating material degradation

The remaining life estimation for the aged components in power plants as well as chemical plants are very important because mechanical properties of the components are degraded with in-service exposure time in high temperatures. Since it is difficult to take specimens from the operating components to evaluate mechanical properties of components, nondestructive techniques are needed to evaluate the degradation. In this study, test materials with several different degradation levels were prepared by isothermal aging heat treatment at 630°C. The DC potential drop method and destructive methods such as tensile and fracture toughness were used in order to evaluate the degradation of 1Cr-1Mo-0.25V steels. In this result, we can see that tensile strength and fracture toughness can be calculated from resistivity and it is possible to evaluate material degradation using DC potential drop method, non-destructive method.     

Focused ion beam sample preparation of continuous fibre-reinforced ceramic composite specimens for transmission electron microscopy

The microanalysis of interfaces in fibre-reinforced composite materials is dependent on the successful preparation of specimens suitable for transmission electron microscope (TEM) inspection. Ideal samples should possess large amounts of structurally intact and uniform thin area in the fibre/matrix interface regions of the samples. Because fibre/matrix interfaces in this class of materials are often designed to fail under mechanical stress, conventionally prepared samples are prone to interfacial failure and differential thinning, both of which preclude detailed TEM microanalysis. These effects were seen in a conventionally dimpled and ion-beam-thinned specimen prepared from a continuous fibre reinforced ceramic composite composed of CaWO₄-coated Nextel 610^TM fibres in an alumina matrix. The dimpled specimen showed large amounts of interfacial failure, with only thick regions of the specimen left intact. To overcome these limitations, a focused ion beam (FIB) technique was applied to this same material. The superiority of the FIB-produced sample is evident in both the morphology and scanning transmission electron microscopy analyses of the sample.     

Oolong tea extract as a substitute for uranyl acetate in staining of ultrathin sections

In conventional transmission electron microscopy, uranyl acetate staining is used to enhance the cellular components. However, uranyl acetate is considered a radioactive material that is very toxic if ingested or inhaled and subject to restrictions in many countries. In an attempt to introduce a substitute for uranyl acetate, we evaluated oolong tea extract (OTE) for staining of ultrathin sections. Tissue sections from normal rat liver representing an ideal model organ were processed according to a routine electron microscopic fixation and embedding procedure. Serial ultrathin sections were cut and processed with either routine double electron staining or 0.2% OTE staining for 30–40 min at room temperature followed by lead citrate staining (OTE staining method). Transmission electron microscopy observations revealed that all sub‐cellular structures in hepatocytes were clearly visible with OTE staining and the quality of staining was highly compatible with those of routine double staining methods. It is suggested that OTE could be used as a non‐radioactive and hazard‐free substitute for uranyl acetate in transmission electron microscopy staining.     

镍基定向凝固高温合金蠕变寿命预测的改进方法

一种应用简单、物理依据清晰、稳健的蠕变和持久寿命性能方法是开展航空发动机热端部件强度评价的重要基础。针对航空发动机用典型的镍基高温合金,首先讨论了Wilshire方法对宽温度/应力条件下蠕变性能的预测精度,并证实该方法体系中的等效蠕变激活能比传统方法更接近晶格扩展激活能,所预测的应力分界点与合金不同温度/应力条件下的蠕变变形机制密切相关;其次,通过引入拉伸强度相关的晶向函数对Wilshire和传统的Larson-Miller法进行修正,结果显示修正方法顺利实现了不同晶向下蠕变持久性能的高精度预测;最后,基于Wilshire方法提出了一种基于归一化应力的热强综合参数,该热强综合参数可用于评估高温合金材料在归一化应力条件下的蠕变持久性能,同时基于该热强综合参数有利于发挥材料的高温性能潜能。     

多壁碳纳米管增强无石棉垫片性能研究

为了优化配方并提高无石棉垫片的性能,以加入多壁碳纳米管(MWCNTs)的无石棉垫片为研究对象,对MWCNTs和无石棉垫片的主要组成材料进行均匀配方设计,对制备的无石棉垫片材料进行拉伸强度、压缩率与回弹率、密度和老化系数的性能测试;采用多元线性回归分析建立垫片各项性能与材料配方之间的回归模型,并进行验证。结果表明:综合性能最优时的配方(按质量分数)如下:多壁碳纳米管2. 48%、QY棉18. 58%、矿物棉23. 22%、高岭土23. 22%、云母6. 19%、滑石粉13. 93%、纸浆12. 38%;得到的回归方程式可以用来预估垫片材料的各项性能;不同组分材料对垫片材料性能的影响不一样,其中MWCNTs的含量对垫片的各项性能影响最大,且MWCNTs的加入能改善复合垫片材料的老化性能;随着MWCNTs含量的增加,无石棉垫片的拉伸强度、回弹率、密度和老化系数都增大,但压缩率逐渐减少。因此,在保证垫片材料的压缩率满足要求的前提下,适当增加MWCNTs的含量能显著提高无石棉垫片的性能。     

Minimization of focused ion beam damage in nanostructured polymer thin films

Focused ion beam (FIB) instruments have proven to be an invaluable tool for transmission electron microscopy (TEM) sample preparation. FIBs enable relatively easy and site-specific cross-sectioning of different classes of materials. However, damage mechanisms due to ion bombardment and possible beam heating effects in materials limit the usefulness of FIBs. Materials with adequate heat conductivity do not suffer from beam heating during FIB preparation, and artifacts in materials such as metals and ceramics are primarily limited to defect generation and Ga implantation. However, in materials such as polymers or biological structures, where heat conductivity is low, beam heating can also be a problem. In order to examine FIB damage in polymers we have undertaken a systematic study by exposing sections of a PS-b-PMMA block copolymer to the ion beam at varying beam currents and sample temperatures. The sections were then examined by TEM and scanning electron microscopy (SEM) and analyzed using electron energy loss spectroscopy (EELS). Our empirical results show beam heating in polymers due to FIB preparation can be limited by maintaining a low beam current (≤100 pA) during milling.     

Magnetic estimation of stresses applied to a two-layer steel CT3-steel 08X18H10T composite material during elastoplastic deformation by uniaxial tension

The effect of uniaxial-tension stresses on the structure and physicomechanical properties of a two-layer Steel C_T3-Steel 08X18H10T composite material that underwent preliminary rolling and steels that contain this material was studied. Within the practically important elastic-deformation region, the coercive force, maximum magnetic permeability, and residual inductance of the materials under study were found to exhibit unambiguous behavior and can be used for estimating changes in the stressed-deformed state of articles that are made from the composite material under conditions of uniaxial tension. We demonstrated that it is possible to use the heights and positions of peaks in the field dependence of the magnetic permeability for determining the degree of elastoplastic deformation by uniaxial tension of both the composite material as a whole and the components that comprise the material for estimating the applied stresses.