scholarly journals Faculty Opinions recommendation of Radiation damage and dose limits in serial synchrotron crystallography at cryo- and room temperatures.

Author(s):  
Chu-Young Kim
Keyword(s):  
2020 ◽  
Vol 117 (8) ◽  
pp. 4142-4151 ◽  
Author(s):  
Eugenio de la Mora ◽  
Nicolas Coquelle ◽  
Charles S. Bury ◽  
Martin Rosenthal ◽  
James M. Holton ◽  
...  

Radiation damage limits the accuracy of macromolecular structures in X-ray crystallography. Cryogenic (cryo-) cooling reduces the global radiation damage rate and, therefore, became the method of choice over the past decades. The recent advent of serial crystallography, which spreads the absorbed energy over many crystals, thereby reducing damage, has rendered room temperature (RT) data collection more practical and also extendable to microcrystals, both enabling and requiring the study of specific and global radiation damage at RT. Here, we performed sequential serial raster-scanning crystallography using a microfocused synchrotron beam that allowed for the collection of two series of 40 and 90 full datasets at 2- and 1.9-Å resolution at a dose rate of 40.3 MGy/s on hen egg white lysozyme (HEWL) crystals at RT and cryotemperature, respectively. The diffraction intensity halved its initial value at average doses (D1/2) of 0.57 and 15.3 MGy at RT and 100 K, respectively. Specific radiation damage at RT was observed at disulfide bonds but not at acidic residues, increasing and then apparently reversing, a peculiar behavior that can be modeled by accounting for differential diffraction intensity decay due to the nonuniform illumination by the X-ray beam. Specific damage to disulfide bonds is evident early on at RT and proceeds at a fivefold higher rate than global damage. The decay modeling suggests it is advisable not to exceed a dose of 0.38 MGy per dataset in static and time-resolved synchrotron crystallography experiments at RT. This rough yardstick might change for proteins other than HEWL and at resolutions other than 2 Å.


Author(s):  
M. Isaacson ◽  
M.L. Collins ◽  
M. Listvan

Over the past five years it has become evident that radiation damage provides the fundamental limit to the study of blomolecular structure by electron microscopy. In some special cases structural determinations at very low doses can be achieved through superposition techniques to study periodic (Unwin & Henderson, 1975) and nonperiodic (Saxton & Frank, 1977) specimens. In addition, protection methods such as glucose embedding (Unwin & Henderson, 1975) and maintenance of specimen hydration at low temperatures (Taylor & Glaeser, 1976) have also shown promise. Despite these successes, the basic nature of radiation damage in the electron microscope is far from clear. In general we cannot predict exactly how different structures will behave during electron Irradiation at high dose rates. Moreover, with the rapid rise of analytical electron microscopy over the last few years, nvicroscopists are becoming concerned with questions of compositional as well as structural integrity. It is important to measure changes in elemental composition arising from atom migration in or loss from the specimen as a result of electron bombardment.


Author(s):  
T. E. Mitchell ◽  
M. R. Pascucci ◽  
R. A. Youngman

1. Introduction. Studies of radiation damage in ceramics are of interest not only from a fundamental point of view but also because it is important to understand the behavior of ceramics in various practical radiation enyironments- fission and fusion reactors, nuclear waste storage media, ion-implantation devices, outer space, etc. A great deal of work has been done on the spectroscopy of point defects and small defect clusters in ceramics, but relatively little has been performed on defect agglomeration using transmission electron microscopy (TEM) in the same kind of detail that has been so successful in metals. This article will assess our present understanding of radiation damage in ceramics with illustrations using results obtained from the authors' work.


Author(s):  
L. Reimer

Most information about a specimen is obtained by elastic scattering of electrons, but one cannot avoid inelastic scattering and therefore radiation damage by ionisation as a primary process of damage. This damage is a dose effect, being proportional to the product of lectron current density j and the irradiation time t in Coul.cm−2 as long as there is a negligible heating of the specimen.Therefore one has to determine the dose needed to produce secondary damage processes, which can be measured quantitatively by a chemical or physical effect in the thin specimen. The survival of micro-organisms or the decrease of photoconductivity and cathodoluminescence are such effects needing very small doses (see table).


Author(s):  
T. A. Welton

Various authors have emphasized the spatial information resident in an electron micrograph taken with adequately coherent radiation. In view of the completion of at least one such instrument, this opportunity is taken to summarize the state of the art of processing such micrographs. We use the usual symbols for the aberration coefficients, and supplement these with £ and 6 for the transverse coherence length and the fractional energy spread respectively. He also assume a weak, biologically interesting sample, with principal interest lying in the molecular skeleton remaining after obvious hydrogen loss and other radiation damage has occurred.


Author(s):  
Robert C. Rau ◽  
John Moteff

Transmission electron microscopy has been used to study the thermal annealing of radiation induced defect clusters in polycrystalline tungsten. Specimens were taken from cylindrical tensile bars which had been irradiated to a fast (E > 1 MeV) neutron fluence of 4.2 × 1019 n/cm2 at 70°C, annealed for one hour at various temperatures in argon, and tensile tested at 240°C in helium. Foils from both the unstressed button heads and the reduced areas near the fracture were examined.Figure 1 shows typical microstructures in button head foils. In the unannealed condition, Fig. 1(a), a dispersion of fine dot clusters was present. Annealing at 435°C, Fig. 1(b), produced an apparent slight decrease in cluster concentration, but annealing at 740°C, Fig. 1(C), resulted in a noticeable densification of the clusters. Finally, annealing at 900°C and 1040°C, Figs. 1(d) and (e), caused a definite decrease in cluster concentration and led to the formation of resolvable dislocation loops.


Author(s):  
J. J. Laidler ◽  
B. Mastel

One of the major materials problems encountered in the development of fast breeder reactors for commercial power generation is the phenomenon of swelling in core structural components and fuel cladding. This volume expansion, which is due to the retention of lattice vacancies by agglomeration into large polyhedral clusters (voids), may amount to ten percent or greater at goal fluences in some austenitic stainless steels. From a design standpoint, this is an undesirable situation, and it is necessary to obtain experimental confirmation that such excessive volume expansion will not occur in materials selected for core applications in the Fast Flux Test Facility, the prototypic LMFBR now under construction at the Hanford Engineering Development Laboratory (HEDL). The HEDL JEM-1000 1 MeV electron microscope is being used to provide an insight into trends of radiation damage accumulation in stainless steels, since it is possible to produce atom displacements at an accelerated rate with 1 MeV electrons, while the specimen is under continuous observation.


Author(s):  
K. Izui ◽  
T. Nishida ◽  
S. Furuno ◽  
H. Otsu ◽  
S. Kuwabara

Recently we have observed the structure images of silicon in the (110), (111) and (100) projection respectively, and then examined the optimum defocus and thickness ranges for the formation of such images on the basis of calculations of image contrasts using the n-slice theory. The present paper reports the effects of a chromatic aberration and a slight misorientation on the images, and also presents some applications of structure images of Si, Ge and MoS2 to the radiation damage studies.(1) Effect of a chromatic aberration and slight misorientation: There is an inevitable fluctuation in the amount of defocus due to a chromatic aberration originating from the fluctuations both in the energies of electrons and in the magnetic lens current. The actual image is a results of superposition of those fluctuated images during the exposure time. Assuming the Gaussian distribution for defocus, Δf around the optimum defocus value Δf0, the intensity distribution, I(x,y) in the image formed by this fluctuation is given by


Author(s):  
N. Bonnet ◽  
M. Troyon ◽  
P. Gallion

Two main problems in high resolution electron microscopy are first, the existence of gaps in the transfer function, and then the difficulty to find complex amplitude of the diffracted wawe from registered intensity. The solution of this second problem is in most cases only intended by the realization of several micrographs in different conditions (defocusing distance, illuminating angle, complementary objective apertures…) which can lead to severe problems of contamination or radiation damage for certain specimens.Fraunhofer holography can in principle solve both problems stated above (1,2). The microscope objective is strongly defocused (far-field region) so that the two diffracted beams do not interfere. The ideal transfer function after reconstruction is then unity and the twin image do not overlap on the reconstructed one.We show some applications of the method and results of preliminary tests.Possible application to the study of cavitiesSmall voids (or gas-filled bubbles) created by irradiation in crystalline materials can be observed near the Scherzer focus, but it is then difficult to extract other informations than the approximated size.


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