Swift heavy ion irradiation effects on structural,optical properties and ac conductivity of polypyrrole nanofibers

Polypyrrole (PPy) nanofibers have been synthesized by interfacial polymerization method and irradiated with 160?MeV Ni¹²⁺ ions under vacuum with fluences in the range of 10¹⁰–10¹²?ions/cm². High-resolution transmission electron microscopy results show that upon swift heavy ion (SHI) irradiation the PPy nanofibers become denser. The crystallinity of PPy nanofibers increases upon SHI irradiation, while their d-spacing decreases. Upon SHI irradiation, the polaron absorption band gets red-shifted indicating reduction in the optical band gap energy of the irradiated PPy nanofibers. The indirect optical band gap energy is decreased as compared to corresponding direct optical band gap energy. The number of carbon atoms per conjugation length (N) and carbon atoms per cluster (M) of the SHI-irradiated PPy nanofibers increase with increasing the irradiation fluence. Fourier transform infrared spectra reveal the enhancement in intensity of some characteristic vibration bands upon SHI irradiation. The thermal stability of the PPy nanofibers is enhanced on SHI irradiation. The charge carriers in both pristine and irradiated PPy nanofibers follow the correlated barrier hopping mechanism. Scaling of ac conductivity reveals that the conduction mechanism is independent of the SHI irradiation fluence.     

The interpretation of X-ray diffraction from the pyrocarbon in carbon/carbon composites with comparison of TEM observations

Three different carbon/carbon (C/C) composites based on needle-punched felt made of layered T700 carbon fiber cloth were fabricated by chemical vapor infiltration and were studied using transmission electron microscopy (TEM) and X-ray diffraction (XRD). The TEM observations show that one of the composites contains only low-textured pyrocarbon. The other two contain both low-textured and high-textured pyrocarbon, one with predominantly low-textured and the other with mainly high-textured pyrocarbon. High-resolution TEM images show that the high-textured pyrocarbon in the two composites has the same microstructure as local areas with the graphite structure. XRD measurements show that the interlayer spacing and crystallite size of pyrocarbon are not only affected by the poorly graphitized carbon fiber phase, but also by the amounts of the different types of pyrocarbon and the orientation of crystallites. Comparison of the TEM observations and the XRD measurements reveals that structural parameters, such as the interlayer spacing and crystallite size, of pyrocarbon in C/C composites as determined by XRD are not accurate. Therefore, XRD profiles of C/C composites should be interpreted with caution. TEM observations for detailed microstructure analysis of C/C composites are thus important.     

Characterization of superlattices of monodisperse Fe3O4 nanoparticles in a polystyrene matrix with TEM and XRD

Superlattices of monodisperse Fe₃O₄ nanoparticles in a polystyrene matrix are fabricated by directly blending the monodisperse Fe₃O₄ nanoparticles with the polystyrene at slightly above the melting point of polystyrene. We characterized the superlattices with TEM and XRD. We observed that the superlattices scatteredly formed in the polystyrene matrix and their sizes increased with increase in the concentration of the Fe₃O₄ nanoparticles in the polystyrene matrix.     

Study of defect evolution by TEM with in situ ion irradiation and coordinated modeling

The paper describes a novel transmission electron microscopy (TEM) experiment with in situ ion irradiation designed to improve and validate a computer model. TEM thin foils of molybdenum were irradiated in situ by 1?MeV Kr ions up to ～0.045 displacements per atom (dpa) at 80°C at three dose rates ?5?×?10^?6, 5?×?10^?5, and 5?×?10^?4?dpa/s – at the Argonne IVEM-Tandem Facility. The low-dose experiments produced visible defect structure in dislocation loops, allowing accurate, quantitative measurements of defect number density and size distribution. Weak beam dark-field plane-view images were used to obtain defect density and size distribution as functions of foil thickness, dose, and dose rate. Diffraction contrast electron tomography was performed to image defect clusters through the foil thickness and measure their depth distribution. A spatially dependent cluster dynamic model was developed explicitly to model the damage by 1?MeV Kr ion irradiation in an Mo thin foil with temporal and spatial dependence of defect distribution. The set of quantitative data of visible defects was used to improve and validate the computer model. It was shown that the thin foil thickness is an important variable in determining the defect distribution. This additional spatial dimension allowed direct comparison between the model and experiments of defect structures. The defect loss to the surfaces in an irradiated thin foil was modeled successfully. TEM with in situ ion irradiation of Mo thin foils was also explicitly designed to compare with neutron irradiation data of the identical material that will be used to validate the model developed for thin foils.     

Fabrication of high quality plan-view TEM specimens using the focused ion beam

We describe a technique using a focused ion beam instrument to fabricate high quality plan-view specimens for transmission electron microscopy studies. The technique is simple, site-specific and is capable of fabricating multiple large, >100 μm² electron transparent windows within epitaxially grown thin films. A film of La_0.67Sr_0.33MnO₃ is used to demonstrate the technique and its structural and functional properties are surveyed by high resolution imaging, electron spectroscopy, atomic force microscopy and Lorentz electron microscopy. The window is demonstrated to have good thickness uniformity and a low defect density that does not impair the film's Curie temperature. The technique will enable the study of in-plane structural and functional properties of a variety of epitaxial thin film systems.     

高能重离子辐照的低活化钢硬化效应

为了探讨聚变堆候选低活化钢的抗辐照性能,在兰州重离子加速器国家实验室HIRFL的材料辐照终端,利用63 MeV的~(14)N离子和336 MeV的~(56)Fe离子在-50?C下对一种国产低活化钢进行辐照实验.借助离子梯度减能装置,使入射离子能量在0.22—6.17 MeV/u之间变化,从而在样品表面至24μm深度范围内产生0.05—0.20 dpa的原子离位损伤坪区.利用纳米压痕仪测试样品辐照前后的显微硬度,通过连续刚度测量(constant stiffness measurement)得到低活化钢硬度的深度剖面信息.使用Nix-Gao模型很好地描述了纳米压痕硬度随深度递减的现象(压痕尺寸效应,indentation size effect),从而有效避免了低能离子辐照的软基体效应(softer substrate effect).正电子湮灭寿命谱显示低活化钢在辐照之后长寿命成分增加,说明样品中产生了大量缺陷形成空位团,从而导致了材料力学性能的变化,在离子辐照剂量增加至0.2 dpa时,平均寿命τ_m增加量逐渐变慢,材料中辐照产生的缺陷趋于饱和.     

采用EPR谱和TEM对YSZ单晶辐照损伤的研究

 利用电子顺磁共振(EPR)谱和透射电子显微镜(TEM)研究了YSZ单晶的辐照效应。200 keV的Xe和400 keV的Cs离子注入［111］取向的YSZ单晶中,注量均为5×10¹⁶ cm^-2。EPR结果表明辐照产生了共振吸收位置g‖=1.989 和 g⊥=1.869、对称轴为［111］的六配位Zr³⁺顺磁缺陷。Cs辐照产生了比Xe 离子辐照多约150倍的六配位Zr³⁺顺磁缺陷。两种样品的剖面电子显微分析表明没有发现非晶化转变,但是Cs离子辐照的样品在损伤集中区域产生了密度较高的缺陷。因此,EPR谱和电子显微观察均说明在相同离位损伤(约160 dpa)的情况下,Cs离子辐照比Xe 离子辐照产生了更多的缺陷。造成这一现象的原因是Cs离子是化学活性的而Xe 离子却是惰性的。     

Effect of dose on irradiation-induced loop density and Burgers vector in ion-irradiated ferritic/martensitic steel HT9

Samples of F/M steel HT9 were irradiated to 20?dpa at 420°C, 440°C and 470°C in a transmission electron microscope with 1?MeV Kr ions so that the microstructure evolution could be followed in situ and characterised as a function of dose. Dynamic observations of irradiation-induced defect formation and evolution were made at the different temperatures. Irradiation-induced loops were characterised in terms of their Burgers vector, size and density as a function of dose and similar observations and trends were found at the three temperatures: (i) both a/2 <111> and a <100> loops are observed; (ii) in the early stage of irradiation, the density of irradiation-induced loops increases with dose (0–4?dpa) and then decreases at higher doses (above 4?dpa), (iii) the dislocation line density shows an inverse trend to the loop density with increasing dose: in the early stages of irradiation, the pre-existing dislocation lines are lost by climb to the surfaces while at higher doses (above 4?dpa), the build-up of new dislocation networks is observed along with the loss of the radiation-induced dislocation loops to dislocation networks; (iv) at higher doses, the decrease of number of loops affects more the a/2 <111> loop population; the possible loss mechanisms of the a/2 <111> loops are discussed. Also, the ratio of a <100> to a/2 <111> loops is found to be similar to cases of bulk irradiation of the same alloy using 5?MeV Fe²⁺ ions to similar doses of 20?dpa at similar temperatures.     

On the formation of temperature-induced defects at the surface of TEM specimens prepared from TiAl using high-energy Gallium and low-energy Argon ions

ABSTRACT

Specimens for transmission electron microscopic (TEM) investigations were prepared from γ titanium aluminide alloys with Gallium and Argon ions using a focused ion beam (FIB) and a precision ion polishing system (PIPS). Preparation to electron transparency by Gallium ions alone leads to the formation of crystalline platelets of the α titanium phase at the specimen surfaces, revealed through conventional and high resolution (HR) TEM analysis. The platelets are assumed to precipitate from priorly formed amorphous layers. The required crystallisation temperature of about 480°C is generated through the ion bombardment implying that the γ titanium aluminides can be heated substantively during sputtering. The primary reason for this is the restricted transfer of heat away from the beam impact point when the specimen thickness comes close to the beam diameter. The formation of the platelets can be avoided by terminating the Gallium ion treatment prior to that, while providing for a sufficient thermal bonding of the specimen to the grid as well and polishing off the remaining material by Argon ions, which are much less focused and less energetic, so that the local heat peaks are reduced.     

Structure of PtFe/Fe double-period multilayers investigated by X-ray diffraction, reflectivity, diffuse scattering and TEM

Double-period [(Pt 1.7 nm/Fe 0.9 nm)₅Fe(t_Fe2)]₈ and [(Pt 1.8 nm/Fe 0.6 nm)₅Fe(t_Fe2)]₈ multilayers with different thickness t_Fe2 (between 0.23 and 4.32 nm) of the additional Fe layers, prepared by combinatorial sputter deposition, show differences in the mosaic spread and the vertical interfacial roughness when deposited on native or thermally oxidised Si wafers. Simulations of the wide-angle X-ray scattering intensities revealed the presence of interdiffusion in the (Pt/Fe)₅ bilayers and systematic variations of the grain sizes, perpendicular to the film surface, as well as the rms variations of the two superlattice periods with the total film thickness. A comparison of ω-rocking scans shows an increase of the correlated vertical roughness of the (Pt/Fe)₅ multilayers with the total multilayer thickness.     

Effect of swift heavy ion irradiation on photoluminescence properties of ZnO/PMMA nanocomposite films

We report a study on the SHI induced modifications on structural and optical properties of ZnO/PMMA nanocomposite films. The ZnO nanoparticles were synthesized by the chemical route using 2-mercaptoethanol as a capping agent. The structure of ZnO nanoparticles was confirmed by XRD, SEM and TEM. These ZnO nanoparticles were dispersed in the PMMA matrix to form ZnO/PMMA nanocomposite films by the solution cast method. These ZnO/PMMA nanocomposite films were then irradiated by swift heavy ion irradiation (Ni⁸⁺ ion beam, 100 MeV) at a fluence of 1×10¹¹ ions/cm². The nanocomposite films were then characterized by XRD, UV-vis absorption spectroscopy and photoluminescence spectroscopy. As revealed from the absorption spectra, absorption edge is not changed by the irradiation but the optical absorption is increased. Enhanced green luminescence at about 527 nm and a less intense blue emission peak around 460 nm were observed after irradiation with respect to the pristine ZnO/PMMA nanocomposite film.     

Bubble-loop complexes induced by helium irradiation and effect of pre-irradiation and post-irradiation of hydrogen in reduced-activation ferritic/martensitic steel

In the present work, the synergistic effect of high concentration hydrogen and helium on the dislocation loops and bubbles as well as their correlations in reduced-activation ferritic/martensitic (RAFM) steels is investigated. Such an effect was transmuted from 14?MeV neutron irradiation and has been one of the most challenging issues for RAFM steels for future fusion reactors. After low dose (0.18?dpa) high concentration (5000 appm) single-ion helium irradiation at 723?K, very large dislocation loops were observed, and the majority of bubbles were inside dislocation loops, forming bubble-loop complexes. These bubble-loop complexes defects were also present in hydrogen/helium and helium/hydrogen sequential-ion irradiated steels. Pre-irradiated hydrogen ion effectively inhibited the later growth of loops induced by helium post-irradiation, and the higher the ratio of hydrogen to helium fluence, the greater the effect of inhibition. At high fluence of hydrogen pre-irradiation, the structure of bubble-loop complexes disappeared. On the other hand, hydrogen post-irradiation promoted the growth of loops induced by helium pre-irradiation, and the higher the ratio of hydrogen to helium fluence, the greater the effect of promotion. The mechanisms for hydrogen/helium synergistic effects are discussed.     

Effect of gamma irradiation on synthesis and characterization of bio-nanocomposite SF/Ag nanoparticles

This study describes the synthesis of silver nanoparticles (AgNPs) using aqueous silk fibroin (SF) solution obtained from Bombyx mori silk under gamma radiation environment. The obtained AgNPs were characterized using UV–visible (UV–Vis) spectroscopy, X-ray diffraction (XRD) measurements, dynamic light scattering experiment (DLS) and transmission electron microscope (TEM) images. The UV–Vis absorption spectra of the samples confirmed the formation of AgNPs by showing surface plasmon resonance (SPR) band in the range of (= 428–435?nm. The XRD study revealed metal silver with the face-centered cubic (FCC) crystal structure. DLS measurements showed the dose-dependent average size of the AgNPs. TEM images showed formed AgNPs are nearly spherical in shape with smooth edges. From this study, it was found that the increasing radiation dose increases the rate of reduction and decreases the particle size. The size of the AgNPs can be tuned by controlling the radiation dose.     

分离X射线衍射线多重宽化效应的新方法和计算程序

在近似函数的基础上，提出并建立分离微晶与微应力、微晶与堆垛层错、微应力与堆垛层错二重宽化效应的最小二乘法和微晶-微应力-堆垛层错三重宽化效应的最小二乘法，同时编制了相关的计算机求解系列程序.这些方法适用于密堆六方(cph)、面心立方(fcc)和体心立方(bcc)结构.还给出和讨论了几个应用实例. 关键词： 最小二乘法 微结构 X射线衍射 计算程序     

Comparative studies of p6m siliceous mesostructures by powder X-ray diffraction and nitrogen adsorption

Two-dimensional mesostructures with p6m symmetry such as MCM-41 and SBA-15 are the subject of intensive studies by using nitrogen and argon adsorption, transmission electron microscopy, and powder X-ray diffraction/scattering techniques. The latter may involve the X-ray diffraction (XRD) or small angle X-ray scattering (SAXS) measurements. The XRD/SAXS patterns for the aforementioned ordered mesostructures often exhibit four or more reflections, the most intensive one, 1 0 0 peak, and three less intensive peaks, 1 1 0, 2 0 0, 2 1 0. So far, analysis of these patterns was usually limited for the evaluation of the unit cell parameter and the identification of the observed peaks. In this work we present an attempt to analyze the XRD/SAXS patterns by including not only the position of observed peaks but also their intensity. It is shown that the intensity of these peaks, especially 1 1 0 peak, depends on the ratio of the pore diameter to the unit cell parameter. In particular, this dependence was studied for the intensity ratio of 1 1 0 and 2 0 0 peaks assuming 2 0 0 peak as a reference reflection because of its nearness to 1 1 0 peak (which minimizes the influence of other factors than the structural ones on the 1 1 0/2 0 0 intensity ratio analysis) and similar intensity to that of 1 1 0 peak. The values of the 1 1 0/2 0 0 intensity ratio were determined for many MCM-41 and SBA-15 samples and analyzed in relation to the pore width/unit cell ratio, where the pore width was estimated on the basis of nitrogen adsorption data or by the XRD/SAXS structure modeling. Comparative analysis of this intensity ratio for numerous MCM-41 and SBA-15 samples allows for a quick estimation of the pore width and provides some information about hexagonality of mesopores in these materials.     

纳米Cu固体材料的X射线衍射与正电子湮没研究

 采用自悬浮-冷压法,在不同压力下制得纳米Cu固体材料并对其在不同温度和保温时间下进行退火,利用X射线衍射(XRD)和正电子湮没寿命谱(PAS)分析对材料的结构和微观缺陷进行了表征。XRD分析表明,压制而得的样品晶粒度为20 nm,低于300 ℃退火3 h后并未发现晶粒显著长大;PAS分析表明,压制后的样品缺陷主要为单空位和空位团,大空隙很少,随着退火温度的升高和退火时间的延长,单空位通过扩散结合成空位团,大空隙也在温度较高时分解为空位团,导致空位团的含量增加,而单空位和大空隙的含量降低。     

X-ray diffraction and photoelectron spectroscopy study of swift heavy ion irradiated Mn/p-Si structure

The electronic structure and interfacial chemistry of thin manganese films on p-Si (1 0 0) have been studied by photoelectron spectroscopy measurements using synchrotron radiation of 134 eV and from X-ray diffraction data. The Mn/p-Si structures have been irradiated from swift heavy ions (∼100 MeV) of Fe⁷⁺ with a fluence of 1 × 10¹⁴ ions/cm². Evolution of valence band spectrum with a sharp Fermi edge has been obtained. The observed Mn 3d peak has been related to the bonding of Mn 3d-Si 3sp states. Mn 3p (46.4 eV), Mn 3s (81.4 eV) and Si 2p (99.5 eV) core levels have also been observed which show a binding energy shift towards lower side as compared to their corresponding elemental values. From the photoelectron spectroscopic and X-ray diffraction results, Mn₅Si₃ metallic phase of manganese silicide has been found. The silicide phase has been found to grow on the irradiation.     

Synthesis and characterization of CoxZn1−xFe2O4 magnetic nanoparticles via a PEG-assisted route

We present an investigation of properties of Co_xZn_1−xFe₂O₄ (x=0.0-1.0) nanoparticles synthesized by a polyethylene glycol (PEG)-assisted hydrothermal route. X-ray powder diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and vibrating scanning magnetometry (VSM) were used to characterize the structural, morphological and magnetic properties. The particle size obtained from TEM and XRD are consistent with each other. It was observed that the lattice constant for each composition decreases with increasing Co substitution and follows Vegard's law. Magnetization measurements show that while the materials with high Zn substitution are superparamagnetic at room temperature, they are ferromagnetic at temperatures lower than the blocking temperature. The materials with less Zn substitution are ferromagnetic below room temperature. Magnetizations and the coercivities of the samples decrease with the Zn substitution. The resultant overall magnetic behavior of the superparamagnetic samples are found to be considerably different than that of conventional superparamagnetic systems due to the antiferromagnetic interactions both in intra- and inter-cluster spins, and size (effective moment) distribution of the particles.     

A high temperature powder neutron diffraction structural study of the apatite-type oxide ion conductor, La9.67Si6O26.5

High-resolution neutron powder diffraction studies of the oxide ion conductor La_9.67Si₆O_26.5 are reported for temperatures ranging between 25 and 900 °C. The best fit to the data was obtained for space group P6₃ and there was no evidence for any change in symmetry over the temperature range studied. Interstitial oxide ions are identified lying in sites similar to those predicted by previous computer modelling studies, and in agreement with structural studies on related materials. Furthermore, occupancy of these sites is enhanced by Frenkel-type disorder from neighbouring positions. The results thus add further weight to the interpretation that, in these apatite-type systems, the silicate substructure is important for the accommodation of interstitial oxide ions and their migration.