Radiation damage to lyophilized mineral solutions during electron probe analysis: quantitative study of chlorine loss as a function of beam current-density and sample mass-thickness

The quantitative effects of beam current-density and sample mass-thickness on the loss of chlorine which occurs from lyophilized solutes of micro-droplets of mineral salt solutions irradiated in an electron probe analyser were studied. Results are reported for chlorine loss from lyophilized deposits with mass-thickness varying between 5 and 50 mg mm^?2 for NaCl salts and 5 and 80 mg mm^?2 for KCl salts. Electron accelerating voltage was kept constant at 15 kV. The range of beam current-density (I/S, current/sample surface area) was from 0.1 to 1.5 A mm^?2. Samples were irradiated for 1200 s. The results show that under some conditions there is a period of stable chlorine signal before chlorine loss occurs. This is observed between 0.1 and 1 A mm^?2, for a period which can last several hundred seconds depending on beam current-density and sample mass-thickness. For each value of I/S, however, no stable chlorine signal can be observed for samples whose mass-thickness exceeds a value negatively correlated with I/S. The curves of decrease of characteristic chlorine X-ray signal (expressed as per cent of count rate in the initial counting interval) versus irradiation time can be fitted by the sum of two exponentials with half lives T₁ and T₂. In NaCl, T₁ and T₂ values are highly correlated with I/S but not with mass-thickness. In KCl, T₁ is correlated only with mass-thickness and T₂ only with I/S. Mixing plasma with mineral solutions prevents chlorine loss.     

Radiation damage in stained catalase at low temperature.

Radiation damage, which occurs in the beam of the electron microscope, has been studied in uranyl acetate stained crystals. Damage is observed in terms of the disappearance of higher orders of the electron diffraction pattern. In this study it has been found that the damage at very low specimen temperatures proceeds both more rapidly and to a greater final degree than is the case at room temperature.     

Radiation damage of purple membrane at low temperature.

The intensities of diffracted electron beams for the purple membrane of Halobacterium halobium are found to decay exponentially as a function of the accumulated electron exposure, both at room temperature and at -120 degrees C. This permits us to define the "critical dose" Ne(h,k) for the (h,k) diffracted beam, as being the electron exposure (electrons/A2) at which the diffracteed intensity has fallen to e-1 of its initial value. The critical of purple membrane is found to increase from the room temperature value by at least a factor of four when the specimen is maintained at a temperature of -120 degrees C on a liquid-nitrogen-cooled stage. A relationship derived between the critical dose, Ne, and the dose for optimum imaging, Nopt. Both Ne and Nopt depend, of course, upon the spatial frequency, or resolution. The derivation is valid only for the case in which all sources of noise other than quantum fluctuations are neglected. In this case, Nopt approximately equal to 2.5Ne. Finally, Nuclear Track Emulsion plates have been shown to be advantageous for recording high resolution electron diffraction patterns of small (1 micrometer 2) patches of crystalline biological materials.     

Low-temperature EDX microanalysis of halogenated copper phthalocyanine samples

X-ray microanalysis at temperatures near that of liquid nitrogen is used to determine the halogen content of small volumes of halogenated copper phthalocyanine pigments. Details of the low-temperature stage used and the benefits conferred by cooling the sample are given. The experimental procedure adopted involved recording a series of spectra from the same area and extrapolating the measured compositions to zero dose. Factors affecting the accuracy of the analyses are discussed.     

Ice crystal damage and radiation effects in relation to microscopy and analysis at low temperatures

There are several limitations to the low-temperature techniques which are currently being used for the preparation, examination and analysis of biological and organic samples by means of high-energy beam instrumentation. The low thermal conductivity of samples and the inadequacy of rapid cooling techniques means that, with the exception of thin-film suspensions and the surface of impact-cooled bulk specimens which may be vitrified, ice crystals of varying sizes will be present in nearly all samples which are quench cooled. Data are presented which indicate the depth to which adequate cryo-fixation may be achieved for both morphological and analytical studies. Although dynamic processes may be time resolved in the outer parts of quench-cooled samples, the decreased freezing rate below the surface makes resolution of these processes much less certain. The quality of information which may be obtained from quench-cooled samples is limited by radiation damage. Low-dose microscopy of vitrified thin-film suspensions of macromolecules continues to provide valid structural information at the molecular level. The increased doses needed for X-ray microanalysis present serious problems with the high spatial resolution analysis of thin frozen-hydrated sections although much less damage is observed in dried samples. A case is presented for using the outer fracture faces of frozen-hydrated bulk samples for low-resolution analysis of cells and tissues.     

Radiation damage relative to transmission electron microscopy of biological specimens at low temperature: a review.

When biological specimens are irradiated by the electron beam in the electron microscope, the specimen structure is damaged as a result of molecular excitation, ionization, and subsequent chemical reactions. The radiation damage that occurs in the normal process of electron microscopy is known to present severe limitations for imaging high resolution detail in biological specimens. The question of radiation damage at low temperatures has therefore been investigated with the view in mind of reducing somewhat the rate at which damage occurs. The radiation damage protection found for small molecule (anhydrous) organic compounds is generally rather limited or even non-existent. However, large molecular, hydrated materials show as much as a 10-fold reduction at low temperature in the rate at which radiation damage occurs, relative to the damage rate at room temperature. In the case of hydrated specimens, therefore, low temperature electron microscopy offers an important advantage as part of the overall effort required in obtaining high resolution images of complex biological structures.     

Radiation damage in soft X-ray microscopy of live mammalian cells

When specimens are observed by soft X-ray microscopy, they always absorb many photons, causing radiation damage at the imaged site. The problems of radiation damage were studied in view of the principle of image formation; absorption contrast, scattering (holography), or phase contrast. In all cases, photons with a wavelength of 1–10 nm interact with the specimen mainly through the photoelectric effect followed by the transfer of energy to the imaging site either directly (absorption imaging) or indirectly (holography or phase contrast). This absorbed energy will cause structural changes to the imaging site. From a review of the literature the absorbed dose is estimated to be as high as 10⁷ Gy when the expected resolution of the specimen (1–10 thick) is 10 nm. This dose is far in excess of the amount required for cells to be able to survive when live mammalian cells are exposed. The levels of radiation effects were extrapolated to the estimated absorbed dose from the reported values for cell survival, chromosome aberrations, and DNA strand breaks with respect to observations on mammalian chromosomes. The extrapolated results show that some damage will occur in every 10 times 10-nm (expected resolution) size unit. Although these studies focused only on the effects on mammalian chromosomes, the present results are more or less common phenomena in the observation of biological specimens. Hence, the results suggest that dynamic observations will be difficult. On the other hand, a time-scale study of the effects of radiation on structural integrity suggests that single-shot imaging with short-pulsed (probably shorter than a few milliseconds) X-rays may be appropriate for the observation of intact live biological specimens in the hydrated condition, before they have deteriorated.     

Freeze-fracturing at low temperatures: I. A device for fracturing biological specimens at 77–10 K under high vacuum

Standard freeze-etching or freeze-cleaving is performed at 173 K in a vacuum of 133 μPa or at 77 K under liquid nitrogen with subsequent transfer of the specimen into a vacuum chamber. It has been suggested that the frequent poor resolution of morphological details, the poor complementarity of innermembrane protein particles and the semi-crystalline substructures in biomembranes are caused by structural distortion or plastic deformation due to sheer forces which occur even at 77 K during fracturing or cleaving. In addition, water contamination and radiant heat damage occurring during replication introduce artefacts to the structural record. These artefacts could be avoided or reduced by lowering the temperature at which fracturing or cleaving and shadowing is carried out, to about 10 K. Therefore, a device for cleaving biological specimens at 15–10 K under high vacuum was constructed. To allow the use of existing equipment, the device was built into a standard Balzers 301 vacuum unit, where the specimen transfer is done via an airlock system which allows hoar frost contamination free transport of the specimen holder onto the specimen table. To reduce or prevent the condensation of water and other residual gases in the vacuum onto the freshly cleaved specimen surface at 10 K, the specimen is surrounded by two cooled surfaces of 6 and 20 K. All condensable gases outside those shielding shrouds will condense on these surfaces before reaching the specimen. This makes it possible to work at a high vacuum of 3 μPa outside the cooled shrouds, which can be reached with standard turbomolecular pumps. The actual vacuum within the cooled shrouds is estimated to be approximately 13 nPa. Residual gas analysis before and during replication reveals equal conditions to ultra high vacuum systems. An analysis of the yeast cell paracrystalline plasmalemma structure shows that the topographic resolution of the crystalline arrays has been improved by working at 12 K. However, plastic deformation still occurs under these conditions. This observation points to the possibility that what is described as plastic deformation, for at least some membrane proteins, may be a loss of resilience at low temperatures.     

Characterisation of lattice damage formation in tantalum irradiated at variable temperatures

The formation of radiation‐induced dislocation loops and voids in tantalum at 180(2), 345(3) and 590(5)°C was assessed by 3MeV proton irradiation experiments and subsequent damage characterisation using transmission electron microscopy. Voids formed at 345(3)°C and were arranged into a body centred cubic lattice at a damage level of 0.55 dpa. The low vacancy mobility at 180(2)°C impedes enough vacancy clustering and therefore the formation of voids visible by TEM. At 590(5)°C the Burgers vector of the interstitial‐type dislocation loops is a<100>, instead of the a/2 <111> Burgers vector characteristic of the loops at 180(2) and 345(3)°C. The lower mobility of a<100> loops hinders the formation of voids at 590(5)°C up to a damage level of 0.55 dpa.     

防锈铝合金5083锻件的焊接方法

介绍了防锈铝合金5083的力学性能,分析了其在低温阀门上尤其是在空气分离设备上应用的特点。论述了铝合金阀门的焊接工艺方法。     

二维回归分析法在电磁辐射测量误差中的应用

分析温度在电磁辐射测量中的影响。通过重复性温度实验和二维回归分析法,分析了温度变化与用磁场探头测量的磁感应强度的关系,得到了计算磁感应强度的二维回归方程。结果表明,通过二维回归方程所得的计算结果与标定值吻合较好,减少了温度变化给测量带来的误差,同时通过温度补偿能提高电磁辐射测量的精度,结果能准确地反映电磁辐射的真实大小。     

Electron beam radiation damage to organic inclusions in vitreous,cubic, and hexagonal ice

Frozen hydrated specimens of various latex spheres were used as well-defined systems for the study of electron beam radiation damage to organic inclusions in vitreous, cubic and hexagonal ice. We found that radiolysis of organic material is modified by the presence of ice and that radiolysis in vitreous ice is different from that in crystalline ice. The pattern of damage depends also on the nature of the irradiated polymer, e.g., damage to poly(vinylchloride) is quite different from damage to polyacrylates, although in both polymers the main radiolytic process is chain scission. Some polymers such as polyacrylates were found to be much more stable in vitreous ice than in crystalline ice. The experimental results indicate that free radicals formed at the ice–organic matter interface play an important role in the radiolysis process which affects both the ice and embedded organic particles. Ice may play also a physical role in the process by limiting the diffusion of free radicals away from the interface. Although net mass loss is not much affected by ice, massive structural changes including repolymerization take place in its presence.     

Dynamic measurements of damage generation in single crystal silicon due to sliding contact with a spherical diamond

Single or multiple linear unidirectional scratches were made on (111) n-type single crystal silicon surfaces, at room temperature, by a dead-loaded spherical diamond indenter translated in the [110] direction at a speed of 5 cm s⁻¹. The damage was measured with a simulated four-point probe technique consisting of a voltage detector designed and fabricated on the silicon wafer. The scratches were made between four electrical pads of the detector through which the electrical resistance of the damage region can be recorded in real time by a data acquisition system. The relative change in voltage, between 3 and 10%, was correlated to the time for the diamond to move past the probes and depended on dead load on the diamond, and the silicon properties. This measurement technique is used to develop a model for subsurface crack generation and propagation. If subsurface damage is modeled as a Hertzian crack then a measure of the voltage provides an estimate of the crack size. This relationship between the measured relative change in voltage and load on a pyramid diamond can be expressed as M(%) P^4/3.     

汶川地震中西安市塔式起重机的损毁分析

针对西安市区塔式起重机受损的基本状况、主要破坏形式及特点,分析了塔式起重机不同部位出现损坏的原因,为今后塔式起重机的研究、设计及计算中需要进行考虑地震载荷的影响以及提高塔式起重机的安全性提供了参考.     

Mass loss rate in collodion is greatly reduced at liquid helium temperature

The mass thickness of collodion films has been monitored at several temperatures, under conditions typical of electron microscopy, through the use of an electron energy loss spectrometer. Compared to room temperature, only a five-fold reduction in the rate of mass loss was observed through the use of a commercial liquid nitrogen cooled stage; in contrast, the rate of mass loss was reduced more than one hundred fold when these films were held at liquid helium temperature.     

The research center for ultra-high voltage electron microscopy at Osaka University

High-voltage electron microscopy has shown itself advantageous for the study of natural science, including biology, but especially for materials science. The most important advantage for materials science is for in situ experiments about the detailed processes of the phenomena that occur in bulk materials. The present paper is mainly concerned with several types of in situ experiments that have been carried out in the Research Center for Ultra-High Voltage Electron Microscopy, Osaka University. The following subjects have been studied: (a) fundamental problems, such as the conditions necessary for in situ experiments, functional features of specimen treatment devices, and the effects of electron irradiation; (b) the dislocation behavior of crystals under various conditions; (c) high-temperature behavior of refractory materials, mainly ceramic composites; (d) new applications of electron irradiation effects, such as amorphization of crystalline materials and electron-irradiation-induced foreign-atom implantation; (e) environment-matter interaction, mainly chemical amorphization of alloys; and (f) future trends of the in situ experiment, such as combinations with Auger valency electron spectroscopy and high-resolution electron microscopy.     

A physical approach to the radiation damage mechanisms induced by X-rays in X-ray microscopy and related techniques

A physical approach is used to analyse the various mechanisms induced by the absorption of X-ray photons of energies in the 0.2–20 keV range. At the atomic scale, besides the (Auger and photo) electron transport in the bulk or the ejection into the surrounding media, special attention is devoted to the specific consequences of the initial Auger decay mechanism. At the macroscopic scale, the decisive role of the poor electronic conductivity of the radiation-sensitive materials is outlined and it is shown that the damaging effects occur in irradiated insulators because the lack of conduction electrons prevents the initial charge of the excited atoms being quickly restored. Correlating irradiation conditions and physical properties of the specimen, various expressions are proposed for the first time to quantify these effects. Some are neither dose- nor dose-rate-dependent and the influence of the surrounding medium is also considered. The fundamental mechanisms investigated here hold for a wide variety of specimens or components investigated in X-ray microscopy. Their consequences can be easily transposed to other techniques using transmitted X-rays.     

Modelling transverse cracking damage in thin, filament-wound tubes subjected to lateral indentation followed by internal pressure

Transverse cracking is a typical mode of damage in laminated composites. A continuum damage model has been established for the constitutive relationship which describes initiation and evolution of such damage. The constitutive model has been incorporated into an FE structural analysis using a commercial code, ABAQUS, via one of its user-defined subroutines, UGENS. The developed user subroutine can be applied to simulate transverse cracking damage processes in general laminated composites. As an example, the response of a thin ±55 filament-wound tube subjected to loading and unloading by lateral indentation has been analysed. The predicted load displacement curves and damage growth and stress and strain distributions in each lamina are presented. One of the emphases in this paper is on sequential loading. Subsequent to complete unloading, the tube is subjected to a different loading condition, internal pressure, and simulation of the deformation and damage process is continued. The results have been discussed and compared with experimental data wherever available.     

Application of combined EBSD and 3D‐SEM technique on crystallographic facet analysis of steel at low temperature

Electron backscatter diffraction has been increasingly used to identify the crystallographic planes and orientation of cleavage facets with respect to the rolling direction in fracture surfaces. The crystallographic indices of cleavage planes can be determined either directly from the fracture surface or indirectly from metallographic sections perpendicular to the plane of the fracture surface. A combination of electron backscatter diffraction and 3D scanning electron microscopy imaging technique has been modified to determine crystallographic facet orientations. The main purpose of this work has been to identify the macroscopic crystallographic orientations of cleavage facets in the fracture surfaces of weld heat affected zones in a well‐known steel fractured at low temperatures. The material used for the work was an American Petroleum Institute (API) X80 grade steel developed for applications at low temperatures, and typical heat affected zone microstructures were obtained by carrying out weld thermal simulation. The fracture toughness was measured at different temperatures (0°C, ?30°C, ?60°C and ?90°C) by using Crack Tip Opening Displacement testing. Fracture surfaces and changes in microstructure were analyzed by scanning electron microscopy and light microscopy. Crystallographic orientations were identified by electron backscatter diffraction, indirectly from a polished section perpendicular to the major fracture surface of the samples. Computer assisted 3D imaging was used to measure the angles between the cleavage facets and the adjacent polished surface, and then these angles were combined with electron backscatter diffraction measurements to determine the macroscopic crystallographic planes of the facets. The crystallographic indices of the macroscopic cleavage facet planes were identified to be {100}, {110}, {211} and {310} at all temperatures.