w UNCLASSIFIED ORNL . Ti INWA ho ? STRO .. ** W . 630 ORNLP-631 CONF-792-1 NOV 1 3 1984 MASTER ------------ LEGAL NOTICE --------- Tu, regret i peninsu kont of Innenment Awnin port. Nerober le found lub. Dor the (DNIOWA, W miare sung in den II w we Coun100 A Mabes 111) ammauttom, names or iONIN. 10 r. po dohode the arrow IM). Muunii , vt ha'mund the walimuulanud na wwe uit, ut Wal When we of an, lakinalim. mun len, weld, oi mut.Klourd i Wo ropuit a mwy waring . As IN, 11 illike u reopext is the weat, or hur d u rooling fra de Nowe) lahat, milk, s oul, ni wacom "Kloud I do ropusti A. In the news.. 'perman m uy on ball of the fonu1." INI uy •a · NON a raita W of the Conniska. or vapowo rodinkor, ha iwat what Oluplas, o manure we all who coulon. of onmoyo wa cvoirului poporo. honammo, o pork b. , My worsellon puimui b o nounler' contract Whe Coun... or da empleyi .10 . cogirarlor. Properties of Bell Compacts Irradiated at Fast-Neutron Doses Greater than 2021 Neutrons/cm2 * G. W. Keilholtz J. E. Lee, Jr. R. E. Moore Reactor Chemistry Division, Oak Ridge llational Laboratory, Oak Ridge, Tennessee *Research sponsored by the U. S. Atomic Energy Commission under contract with tz Union Carbide Corporation. Paper to be presented at the American Ceramic Society Meeting, San Francisco, October 28-30, 1964. Table of Contents Introduction Experimental Design Low Temperature Irradiations (~ 120°c) High Temperature Irradiations (650 and 1100°c) Gross Damage Effects Volume Expansion Micrographic Examinations X-ray Diffraction Examinations Single Crystal Studies Discussion and Summary 9 . . . . Introduction The BeO-irradiation program at ORNL, now of several years duration, has been directed primarily toward the determination of the effects of high fast-neutron doses (> 1021 neutrons/cm2) at elevated temperatures (up to 1100°c) on pure Beo compacts without additives. One of the major objectives has been to evaluate the mechanisms of fast-neutron damage under conditions to which Beo moderator bodies may be subjected in nuclear power reactors. Much of the large amount of data on the neutron irradiation of beryllium oxide, accumulated by many different investigators, cannot be compared satisfactorily because the data were obtained from Beo compacts made from different starting materials and fabricated by different methods. Also important, there may be sizable discrepancies in the flux, dose and temperature values in different axperimental assemblies and reactor systems. For these reasons, a series of experiments was designed to permit comparisons of radiation damage to Beo compacts of different grain-sizes and densities as a function of the flux, dose and temperature under controlled conditions. This paper presents the results of these experiments. Experimental Design The irradiation experiments (41-8, 41-9, and 41-10) were designed to determine the effect of fast-neutron irradiation on sintered Beo compacts of different densities, grain-sizes and specimen sizes as a function of the fast-neutron dose, fast-neutron flux and the temperature. There were two sizes of sintered cylindrical specimens (1/2 in. length x 1/2-in. dia. and 1/4-in. length x 1/4 in. dia.) for each of four types of sintered Beo (two densities and two grain sizes). The characteristics of the eight groups of samples irradiated in the experimental assemblies are given in Table 1. All the samples were prepared from tiie same batch of Brush Beryllium Company VOX Grade BeO powder by cold-pressing and sintering at 1750°C in a hydrogen atmosphere. The material of fine grain-size was sintered for one hour, and the ole material of large grain-size was sintered for 60 hours. The low-density Beo samples were made by including epoxy resin in the pressed material and removing 1t by heating at 900°C in air before sintering. The specimens were encapsulated in stainless steel and irradiated in the Idaho Engineering Test Roactor at 110, 650 and 1100°c. Temperatures were achieved in each case by gamma heat generated within the capsules (1, 2). The arrangement of the capsules in the experiments is shown in Fig. 1. Each narrow bar represents a capsule containing so 1/4-in. specimens; each wide bar represents a capsule containing 15 1/2-in. specimens. All four types of Beo samples were included in each of the capsules. Each of the eight capsules of Experiment 41-10 was maintained during irradiation at approximately 110°C. In both Experiments 41-8 and 41-9 which were irradiated for different periods of time in order to achieve a separation of the flux and dose parameters, four capsules were maintained at 650°C and four were maintained at 1100°c. Low Temperature Irradiations_(~ 110°c) The four types of Beo compacts were irradiated at approximately 110°C over the fast-neutron dose range 0.5 to 2.23 x 1024 neutrons/cm² (> 1 Mev). The fast- flux ranged from 1.3 to 5.7 x 1074 neutrons/cm² sec (> 1 Mev). The gross damage to specimens irradiated in this experiment is summarized in Table 2. An examination of the damage data revealed no significant differences between types of Beo. Although major fracturing of Type II began at a lower neutron dose than other types, a larger number of specimens of Type II survived intact up to a dose of 2 x 1022 neutrons/cm². Consequently, this difference is not considered to be significant. Nearly all specimens disintegrated to powder at doses above 2 x 1024 neutrons/cm2. . .. Volume expansion calculated from dimensional increason of the irradiated samples was found to increase nearly linearly from about 1.25% at a fast-neutron dose of 0.5 x 1021 neutrons/cm2 to ubout 5.5% at 1.4 x 1021 neutrons/cm2. There WAB a levelling off at higher doses, reaching about 6% at 2 x 102 neutrons/cma. Figure 2 shows the volume expansion of samples which survived without fracturing or powdering plotted against fast-neutron dose. It is apparent that there are no significant differences in volume expansion among the four types of Beo irradiated in this experiment. Aloo shown in the plot is the volume expansion calculated from density measurements of single crystals irradiated in the same experimental assembly and the volume expansion calculated from the lattice parameters from X-ray diffraction examinations of powdered Beo compacts. Self-constraint in the relatively very large single crystals may account for the lower values found for their volume increases as calculated from density changes compared with values calculated from lattice expansion of powdered specimens. Obviously, grain boundary separation contributes most of the expansion of compacts irradlated to doses above ~0.8 x 1021 neutrons/cm? (> 1 Mev). Two mechanisms have been proposed to explain grain-boundary separation in BeO compacts exposed to fast-neutron irradiation: (1) anisotropic expansion of randomly oriented crystals, resulting in stresses at the grain boundaries which ultimately overcome the intergranular bonding forces and (2) breaking apart of grain boundaries by gas pressure of hellum, which diffuses to the grain boundaries after its production by neutron reactions within the grains. In low temperature irradiations (less than 250°C, for example) the evidence indicates that the hellum mechanism cannot be significant. First, diffusion of helium to the grain boundaries should be very slow at low temperatures. Second, grain boundary separation has been observed in photonicrographs of Beo irradiated at very low fast-neutron doses where very little helium has been produced (3, 4). On the other hand, X-ray diffraction patterns of powdered BeO specimens irradiated at 110°C in Experiment 41-10 show lattice parameter increases large enough to produce grain boundary separation; the anisotropic expansion ratio (ac/s)/169/a) averages about 20 in these patterns. The lattice parameters of specimens irradiated at 110°C are given in Table 3. These data were obtained from measurements of the 21•1 and 21•0 reflections using Ni-radiation, and represent the average c and a parameters including the agglomerations of defects between some of the planes (5). Values of lattice parameters reported for specimens i previous experiments (1) were calculated from reflections observed as diffuse nii imt, but which represent spacings between those planes which do not include defec: Selomerates. High-Temperature Irradiations (650 ':nd 1100°C) In each of the high temperatur". cxperiments (41-8 and 41-9), the four types of Beo were irradiated at both 650 anri 1100°c. The two experiments were similar was except that the irradiation time of Experiment 41-8 was about twice that of Experiment 41-9. The purpose of this procedure was to permit comparisons of the radiation damage to specimens of the same types irradiated to the same fast-neutron doses for different fast-neutron flux values. Gross Damage Effects The experimental conditions and the gross damage data (fracturing and powdering) for the four types of half-inch BeO specimens irradiated in Experiments 41-8 and 41-9 are sunmarized in the bar graph of Fig. 3. Each of the bars covers the range menito of fast-neutron exposure of the specimens of the type represented. The boundaries A of the dange regions shown in the bar graph are approximate. Some samples survived without visible gross damage, although in a greatly weakened condition, even in fast-neutron dose ranges where most samples of the same type were severely fractured e S or powdered. . CA Several conclusions may be drawn from the data summarized in Fig. 3: 1. The gross damage, which increases with increasing dose, is greater at 650 than at 1100°c for all four types of Beo. 2. Powdering of Beo compacts, which previously has been observed only in low temperature irradiations, can occur at temperatures as high as 1100°C after exposure to doses greater than 4 x 1021 neutrons/cm? (> 1 Mev). 3. In general, Type I Beo (low density-small grain size) withstood Irradiation better than the other types in both experiments, while Type IV Beo (high density-large grain size) was generally damaged to a greater extent than the other types, particularly in irradiations at 650°C. 4. Unexpectedly, there is no indication that damage is greater to samples was irradiated in high fast-neutron fluxes than to samples irradiated in low fluxes at equivalent fast-neutron doses. There is less damage to samples irradiated at 650°C in Experiment 41-9 than to samples irradiated at 110°C in Experiment 41-10 (See Table 2). This indicates that in-pile annealing occurs even at temperatures as low as 650°C. Therefore, the absence of a flux intensity effect on gross damage must be related to reactor operational variables such as thermal cycling or thermal stress. Volume Expansion The increase in volume of the half-inch Beo compacts which survived Irradiation without severe fracturing in Experiments 41-8 and 41-9 are plotted against fast-neutron dose in Figs. 4 and 5, respectively. The volume expansion of the quarter-inch specimens is not included because the dimensional data for these specimens were not consistently reliable. As can be seen in Fig. 4, the specimens irradiated at 650°C in the short term experiment (41-9) expanded less than specimens irradiated at 110°c in Experiment 41-10, but considerably more than the samples irradiated at 1100°C. No definite differences in volume expansion among the four types of Beo irradiated at 650°C are Y 5 evident, but in irradiations at 1100°c ít 18 clear that Type I Beo (low density- small grain size) expanded much less than Type IV (high density-large grain size). Types II and III were intermediate in expansion. There was no survival. in irradiatione at 650°C in the long term experiment (41-8). The volume expansion of the four types of samples irradiated at 1100°C, shown in Fig. 5, are in the same order as in Experiment 41-9, with Type I expanding the least, Type IV expanding the most, and Types II and III Intermediate. As in the case for Experiment 41-9, the volume expansion increases with increasing fast- neutron dose. If the volume expansions for irradiations at 1100°C in the two experiments are compared at equivalent dose values (See Table 4), 1t 18 apparent that there 16 greater expansion in Experiment 41-8 than in Experiment 41-9. Thle unexpected finding of greater expansion in lower fluxes for equivalent doses can possibly be explained as an effect resulting from reactor operational variables such as thermal · cycling. For instance, the long term experimental assembly (41-8) experienced three times the number of thermal cycles during irradiation as did the short term assembly (41-9). Thermal cycling of anisotropically strained grain boundaries in a Beo compact may result, therefore, in fracturing of some of the boundaries with each cycle. A greater number of thermal cycles during an irradiation could result, consequently, in greater expansion caused by grain boundary separation. Out-of-pile control tests were conducted in which specimens of all four types of beryllium oxide were subjected to the same thermal treatment that the same four types received during irradiation of Experiment 41-9 at 650 and 1100°c. During the irradiation of Experiment 41-9 there were 45 thermal cycles of the reactor. Dimensional measurements of the diameter and length of these specimens after the conclusion of the tests showed that there were no significant changes. Photomicro- RY -9- graphs of the samples in the as-polished condition at 100x revealed no grain- boundary separation or transgranular fracture. Thermal cycling of unirradiated beryllium oxide compacts, therefore, does not cause grain-boundary separation. The results may mean that thermal cycling can cause grain boundary separation in samples irradiated at 'high temperatures only if there is some radiation-induced anisotropic strain on the boundaries. Micrographic Examinations Photomicrographs of as-polished specimens clearly demonstrate that grain- boundary separation 18 the primary mode of fast-neutron damage in Beo compacts irradiated at low temperatures or to high doses at high temperatures. Transgranular fracture also occurs to some extent, especially in specimens of large grain size (~ 70 u). Grain boundary separation in irradiated specimens is illustrated in Figs. 6 and 7. Figure 6 shows photomicrographs comparing unirradiated Beo of high density - 10- (2.9 g/cm”) and small grain-size (23 u) with Beo of the same type which was irradiated at 1100°c to a fast-neutron dose of 3.92 x 1024 neutrons/cm2. Extensive grain boundary separation can be seen. There is no significant reduction in apparent grain size from that of the unirradiated Beo, indicating that transgranular fracture is not severe. Figure 7 shows high density Bell of large grain size (70 m) Irradiated to a dose of 3.4 x 1021 neutrons/cm? (> 1 Mev) at 1100°c. Separation between grains appears to be wider than in the small-grained Beo, and there 18 evidence of a considerable amount of transgranular fracture. There 16 an apparent grain-size reduction of about 25% as a result of the transgranular fracture. X-Ray Diffraction Examinations Results of X-ray diffraction examinations (5) of selected BeO samples irradiated at, 650 and 1100°C in Experiments 41-8 and 41-9 are presented in Table 5. The - - vaiues for the c parameter were calculated from measurements of the 21•1 and 21.0 - - - - reflections from Ni-radiation from Beo compacts ground to a fine powder. Almost all the volume expansion calculated from the lattice parameters results. from the increase in the c parameter; the a parameter increase is negligible in irradiations at 650 and 1100°c. The anisotropic volume increase calculated from the lattice parameters of samples irradiated at 650°C 1s considerably less than that of samples irradiated at 110°C (See Table 3), but it 18 large enough (1.4 to 2.2%) to cause grain boundary 'separation observed in photomicrographs of these samples. The increased rate of in-pile annealing at 1100°C substantially reduces the g parameter increases from the values found for samples irradiated at 650°c. There 18 a question whether the small anisotropic volume expansion (0.02-0.34%) calculated from lattice parameters of samples irradiated at 1100°C can cause the grain boundary separation observed in photomicrographs. Most samples 11sted in Table 5 are of diametrically opposite type (Type I, low density-small grain size and Type IV, high density-large grain size) to provide - . ܠܐܐܫ a test of whether density or grain size affects lattice parameter expansion. The data are scattered somewhat, but there is no indication, within the limits of. precision of the data, that density and grain-size have a bearing on lattice parameter increase. A comparison of lattice parameter changes of samples irradiated in the short term experiment (41-9) with those of the long term experiment (41-8) at comparable fast neutron doses provides a suggestion of a flux intensity effect on crystal damage. That is, the lattice parameter expansion tends to be greater for samples irradiated in high fluxes than in low fluxes when samples irradiated to equivalent doses are compared. Single Crystal Studies (5) Single crystals of beryllium oxide were irradiated in Experiments 41-8, 41-9 und 41-10 together with Beo compacts. The single crystals irraidated at 650°C in Experiment 41-9 exhibited a dark banding parallel to the basal-planes which was not seen in crystals irradiated at 110°C in Experiment 41-10. The crystals irradiated Seo at 650°C were found to be quite fragile, fracturing easily along the basal planes. Optical and X-ray diffraction data showed that the material in the dark banding is isotropic and amorphous, which strongly suggests that it consists of very large regions of Beo defect agglomerates. These regions are so large that they would not contribute to the values obtained for the c parameter through X-ray diffraction examinations. Single crystals irradiated at 1100°C show some striations, but very little as compared with crystals irradiated at 650°c. Apparently, at 1100°C in-pile annealing of point defects is so rapid that very little long-range agglomeration can occur. 12. 12. 1 In Figure 8 No. 2 shows the dark banding in a crystal Irradiated at 650°C to a fast-neutron dose of 1.1 x 1022 neutrons/cm?, No. 4 18 a crystal irradiated at 650°c to a dose of 4.1 x 1022 neutrons/cm2 in which the dark banding appears to fill the crystal almost completely; No. 3 18 a crystal irradiated at 54°c to 3.6 x 1021 neutrons/cm?; and No. 1 18 an unirradlated crystal. Discussion and Summary Irradiation of sintered beryllium oxide compacts in high fast-neutron fluxes produces crystal damage through production of point defects, as indicated by lattice parameter expansion, and leads ultimately to grain boundary separation and fracturing and powdering of the material. In Irradiations at ~ 100°c, a temperature at which in-pile annealing of point defects is insignificant, the anisotropic crystal volume expansion increases from about 1.25% to about 3.6% over the fast- neutron dose range 0.7 to 2.2 x 1024 neutrons/cm2, which produces grain boundary separation in the compacts. The grain-boundary separation produces an additional volume expansion of irradiated compacts. The total volume expansion of compacts Irradiated over this dose range increases from 2.5 to 6%. Many specimens irradiated to doses greater than 104 neutrons/cm² fractured, and most samples disintegrated to powder above 2 x 1021 neutrons/cm. In-pile annealing of point defects occurs to some extent in Irradiations at 650°C, as evidenced by a reduction in the lattice parameter expansion compared with Irradiations at 110°c. Microscopic examinations of relatively very large single crystals irradiated at 650°C showed striations parallel to the basal planes which consist of defect agglomerates much too large in size to be included in the parameter expansion obtained from X-ray diffraction examinations. These defect agglomerates produce an anisotropic crystal expansion in addition to that calculated from lattice parameters. There 18 less total volume increase and gross damage at . . 15 .. . * . - . .! . Stiri -13- 650°c than at 110°c. Although gross damage data for irradiations at 110°C showed no significant differences among the four grain size-density combinations, in Irradiations at 650°C, Beo compacts of low density and small grain-size withstood irradiation better than other types, and Beo of high density and large grain-size was damaged to a greater extent than the other type 3. No indications of a flux intensity effect on gross damage can be found in comparisons of results of the long term experiment with those of the short-term experiment. Very small crystal volume increases were found in samples irradiated at 1100°C where in-pile annealing must be quite effective. The anisotropic volume expansion at 1100°c calculated from lattice parameter ranges from 0.02 to 0.34%. Density measurements of single crystals irradiated at 1100°C, however, give values for volume expansion as high as 0.9%. The additional expansion is probably a result of defect agglomeration. There is a question as to whether crystal volume expansion even as great as 0.9% can produce the amount of grain boundary separation and i volume increase observed in the compacts irradiated at 1100°C. For example, crystal volume expansion greater than 1% must occur before grain boundary separation begins in irradiations at ~ 100°c. . The gross damage and total volume expansion of Beo compacts irradiated at 1100°C 16 less than that at 650°C. The beryllium oxide compacts of low density and fine grain-size are damaged less and expand less than the other types, and the compacts of high density and large grain-size are damaged to the greatest extent and expand the most. If the gross damage to samples irradiated at 1100°C in the long-term experiment and the short-term experiment are compared at equivalent fast-neutron dose values, no indication of a flux intensity effect can be seen. If anything, . there is greater damage in low fluxes than in high fluxes. The data for volume expansion clearly show, however, that there 18 greater expansion in low fluxes. PS4 .14. This unexpected result is difficult to explain as a radiation effect, particularly in view of the fact that the lattice parameter data suggests that there is a flux intensity effect on crystal damage. The explanation may be that reactor operational variables such as thermal cycling cause grain-boundary separation in samples Irradiated at high temperatures. There may be more grain-boundary separation in long-term experiments with a greater number of reactor thermal cycles than in short-term experiments. This explanation could also account for the unexpectedly large amount of grain-boundary separation in samples Irradiated at 1100°c relative to the small amount of crystal expansion observed. High-temperature thermal cycling may produce grain boundary fracture under conditions of slight anisotropic strain. . N sų r. WH References 1. G. W. Kellholtz, J. E. Lee, Jr., and R. E. Moore, "The Effect of Fast- Neutron Irradiation on Beryllium Oxide Compacts at High Temperatures", J. Nuclear Materials 11 (13) 253-64 (1964). Q. W. Kellholtz, J. E. Lee, Jr., R. E. Moore, and R. L. Hamner, 'Bebavior of Beo Under Neutron Irradiation", Oak Ridge National Laboratory Report ORNL-TM-742 (December 11, 1963). J. Elston, "Radiation Damage in Solids", Proc. Symp. Radiation Damage in Solids and Reactor Materials, Venice, May 7-11, 1962, Vol. II (Vienna, TAEA, 1962). High Temperature Material: Program Progress Report, No. 12, Part A, Nuclear Materials and Propulsion Operation, Flight Propulsion Laboratory Department, General Electric, Cincinnati (USA) Report GEMP-21A (June 15, 1962). L. Yakel, Metals and Ceramics Division, Oak Ridge National laboratory, personal communication. 4. 5. 14. Table 1. Characteristics of Beryllium Oxide Specimens Irradiated in Experiments 41-8, 41-9, and 41-10 Beo Type Batch Mumber Specimen Size (in.) Average Bulk Density Average Grain Size I. (Low density, small and All (Low density, small grain-size) 0.25 0.5 .25 2.7 2.7 2.7 A18 II. (Low density, large grain-size) Al3 Alg 0.25 0.5 2.7 2.7 Sin (High density, small grain-size) 0.25 0.5 2.9 2.9 ANO IV. IV. (enten en eety, large (High density, large grain-size) and n 2.9 o tes 0.25 de A17 0.5 Table 2. Gross Damage to Half-Inch BeO Specimens Irradiated in Experiment 41-10 (~ 11000) Beo Type Fast-Neutron Fast-Neutron Fast-Neutron Fast-Neutron Dose Range for Minor Dose for Major Dose for Major (neutrons/cm2) Fracturing . Fracturing Fracturing with (neutrons/cm) (neutrons/cm2) Powdering (neutrons/cm2) x 2021 * 1021 * 2022 x 1021 I. 0.61-2.23 1.1 1.6 2.0 (Low density, small grain size) II. 0.56.2.23 (Low density, large grain- size) le remotys - 0.56 0.56 2.0 III. 0.67-2.2 1.3 2.0 (High density, small grain- Bize) IV. 0.5-2.22 1.5 2.1 (High density, large grain- size) -15- Table 3. Kesults of X-Ray Diffraction Examination of Beo Irradiated at 110°C in Experiment 41-10* Beo Type Fast-Neutron Dose Fast- Neutron Flux Fast-Neutron Flux 13/. Ac/S AV/v.** (> 1 Mev) (> 1 Mev) (neutrons/cm2) (neutrons coma sec) x 2021 * 2014 1.8 4.3 0.7 1.67 2.22 2.23 0.0010 0.0100 0.0012 0.0256 0.0013 0.0298 0.0013 0.0326 0.0120 0.0280 0.0324 0.0352 5.7 5.7 *Lattice parameters were calculated from measurements of the 21•1 and 21.0 reflections from Ni-radiation from Beo compacts which were 'ground to a fine powder. ** The fractional volume increase, AV/V., was calculated from the equation AV/v. = 2(/,) + (Ac/s). 16. Table 4. Volume Expansiou of Half-Inch Beo Specimens Irradiated in Experiments 41-8 and 41-9 at 1100°c* Beo Type Experiment Percent Volume Increase at Fast-Neutron Dobe 2.0 x 1021 4.0 x 1021 7.2 x 1022 neutrons/cm neutrons/cm2 neutrons/cm 2.0 2.2 41-8 · 41-9 0.7 1.4 III 41-8 2.8 3.1 III 41-9 1.3 2.6 IV 41-8 4.0 4.3 41-9 2.6 * The values of volume increase at the three neutron doses were interpolated from linear data plots. Type II was omitted because there were too little data available, but the expansion appears to lie between Types I and IV. 0 AS JULI -17- Table 5 Results of X-Ray Diffraction Examination of Beo Irradiated at 650 and 1100°C* Temp. a/a. Ac/c. AV/Vo** Experiment Bell Type Fast-Neutron Fast-Neutron Dose (>1 Mev) Flux (>1 Mev) neutrons/cm2 neutrons/cm2 * 2022 x 2014 41-9 IV 1.' 1.65 1.9 650 3.6 650 요요요요요 ​0 0.0150 0.0158 0.0001 0.0140 0.0226 0.0212 0.0004 0.0209 2.25 5.0 5.1 3.65 5.7 0.0150 0.0158 0.0142. 0.0226 0.0212 0.0217 3.7 5.1 7.95 65 650 650 1.8 4.0 IV 41-9 41-9 41-9 .41-9 41-8 41-8 4.0 2.25 2.45 5.5 5.5 1.2 2.3 II · 1100 0 1100 1100 0.0019 1100 0.0034 1100 0.0001 0.0016 1100 0.0001 0 1100 0.0028 1100 0.00010 0.0019 0.0034 0.0018 0.0002 0.0028 0.0002 IV 142-8 3.9 41-8 4.2 Lattice parameters were calculated from measurements of the 21.1 and 21.0 reflections from Ni-ravitation from Beo compacts irradiated in Experiments 41-8 and 41-9 which were ground to a fine powder. ** The fractional volume increase, AV/vo, was calculated from the equation * = 24 + 4 . -18- Figure Captions 1. ORNL-41 Beo Irradiations, ORNL- LR-DWG-71668R. 2. Volume Increase of 1/2-in. Beo Compacts and Single Crystals vs Fast-Neutron Dose in Experiment 41-10, ORNL-DWG-64-8398. 3. 'Gross Damage to Beo Specimens in Experiments 41-8 and 41-9 as a function of the Fast-Neutron Dose and Temperature, ORNL-DWG-64-1886. 4. Volume Increase of 1/2-in. Beo Specimens vs Integrated Fast-Neutron Flux in Experiment 41-9, ORNL-DWG-63-1936. 5. Volume Increase of 1/2-in. Beo Specimens vs Integrated Fast-Neutron Flux in Experiment 41-8, ORNI-DWG-64-4404. 6. Experiment 41-9, Cold Pressed and Sintered BeO, ORNL-PHOTO-62909. 7. Experiment 42-9, Cold Pressed and Sintered Beo, ORNL-PHOTO-62910. 8. Irradiated Beo Single Crystals, ORNL-PHOTO-63235. - - - - - - - - - - . A 1. ve F . F UNCLASSIFIED ORNL-LR-DWG 71668R EXPERIMENT NUMBER 8 -20 YUX * . . ATNA 2. 1 .14) . cuanto mala ............, (0.1) o'i'MO'YNONYWA .*ymGro 970 (0,1) r , - REACTORÇ T 925 1100 gw OISYER Onni.nu. **4444447 AAI. USIJILTOOI.... 1100 H100 LAU 0 . 2.074106 7.66 x 108 4.4x107 7.33 X 106 IRRADIATION TIME (sec) 3.9 x 106 1 2 3 4 5 x 10'4/> 1 Mov) DAMAGE FACTOR (0) SOUND SPECIMEN (1) FIRST CRACKS 2) GENERAL FRACTURES (3) POWDER PRESENT CAPSULE NO. TEMPERATURE (°C) - DAMAGE FACTOR II- ORNL-44 BeO Irradiations Fig. 1 UNCLASSIFIED ORAL-DWG 64-8398 SOLID SYMBOLS - VOLUME INCREASE FROM DIMENSIONAL MEASUREMENTS OPEN SYMBOLS - VOLUME INCREASE CALCULATED FROM LATTICE PARAMETERS LOW DENSITY (~2.7 g/cm3) FINE GRAIN-SIZE (~178) LOW DENSITY (~2.7 g/cm3) LARGE GRAIN-SIZE (~ 34 r1 A III HIGH DENSITY (~2.9 g/cm3) FINE GRAIN-SIZE (~2 V IV HIGH DENSITY (~2.9 g/cm3, LARGE GRAIN-SIZE (~ 7441 SINGLE CRYSTALS II T ~ 110 °C . . . 5 FROM DIMENSIONAL MEASUREMENTS OF BeO COMPACTS - : MEASUREMENI .…... • CALCULATED FROM AVERAGE LATTICE PARAMETER EXPANSIONS IN POWDERED COMPACTS (21.1 AND/OR 24.0 REFLECTIONS, Cu-RADIATION) - VOLUME INCREASE (%) CALCULATED FROM DENSITY MEASUREMENTS OF SINGLE CRYSTALS 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 (x1021) FAST-NEUTRON DOSE (neutrons /cm2 , > 4 Mev) Volume Increase of 12-in. Beo Compacts and Single Crystals vs Fast-Neutron Dose in Experiment 44-10. Fig. 2 Fig. 3 UNCLASSIFIED Beo TYPE ORNL-DWG 64-1886 LOW DENSITY ( 2.7g/cm3) HIGH DENSITY (~2.9 g/cm3) SMALL GRAIN-SIZE (174 SMALL GRAIN-SIZE (254) LOW DENSITY (~2.7 g/cm) HIGH DENSITY (~2.9 g/cm3) "LARGE GRAIN -SIZE (~344) LARGE GRAIN-SIZE (744) O NO OBSERVABLE DAMAGE MAJOR FRACTURING Ø MINOR FRACTURES MAJOR FRACTURING WITH POWDERING BER FAST-NEUTRON DOSE (neutrons/cm -1 Mevl že : 1 III IV I II III IV I II III IV I II III IV 41-9-TIME, 41-8-TIME, 41-9-TIME, 41-8-TIME 7.33x 40 sec 1.4 x 10 sec 7.33x10 sec 1.4x10 sec 1100°C 650°C BeO TYPE AND TEMPERATURE Gross Damage to BeO Specimens in Experiments 41-8 and 41-9 as a Function of the Fast:Neutron Dose and Temperature. UNCLASSIFIED ORNL-DWG 63-1936 • 1900 °C, LOW DENSITY (~2.7 g/cm) o 650 °C FINE GRAIN-SIZE (~47 • 1100 °C LOW DENSITY (~2.7 g/cm) 0 650 °C “ LARGE GRAIN-SIZE (~34 H) • 1900 HIGH DENSITY (~2.9 g/cm) A 650 °C" FINE GRAIN-SIZE (~25) 1400 °C ... HIGH DENSITY (~2.9 g/cm) o 650 °C "Y LARGE GRAIN-SIZE (~74 ) I, II AND III-650 °C VOLUME INCREASE (%) IV-1400 °C. To III-1400 °C 11-1100 °C 0.4 0.8 9.2 9.6 2.0 2.4 2.8 3.2 3.6 4.0 (x1024) INTEGRATED FAST-NEUTRON FLUX (neutrons/cm2 > 4 Mev) Volume Increase of 12-in. BeO Specimens vs Integrated Fast-Neutron Flux in Experiment 41-9. Fig. 4 UNCLASSIFIED ORNL-DWG 64-4404 LOW DENSITY (~2.7 g/cm) FINE GRAIN-SIZE (~174) LOW DENSITY (~ 2.7 g/cm3) LARGE GRAIN-SIZE (~ 34 mi) HIGH DENSITY (~2.9 g/cm3) FINE GRAIN-SIZE (~25) HIGH DENSITY (~2.9 g/cm3) LARGE GRAIN-SIZE (~ 74 m) T~ 1100°C VOLUME INCREASE (%) 0.8 1.6 2.4 3.2 4.0 4.8 5.6 6.4 7.2 INTEGRATED FAST - NEUTRON FLUX (neutrons/cm2, >1 Mev) Volume increase of 12-in. BeO Specimens vs Integrated Fast - Neutron Flux in Experiment 41-8. Fig. 5 6 . ** .. . * . - - - - - - * .* .2 : UNCLASSIFIED PHOTO 62909 21. O R-15768 IRRADIATED SPECIMEN A10-63 AS POLISHED, 100X 3.92 x 1021 nut > 4. Mev 1100 °C O1 .18 .. Y-45349 CONTROL AS POLISHED, 100X DENSITY: 2.9 g/cm3 GRAIN SIZE: 234 Fig. 6 . : .: . . . - . = 2 A n eh .. . - . . . ... . . . --- - 2 + , , .' . - . . * * .- . - * N S -, - .-*1-*+ - = -_- . - - * . - UNCLASSIFIED PHOTO 62910 - - .. -..- . .. - -.. -.. r . . --- .. .-. .. -. --.- : . - :- 1001 . Y-45352 R-15762 AS POLISHED, 100X AS POLISHED, 100% DENSITY: 2.9 g/cm3 3.4 x 1024 nut GRAIN SIZE: 704 > 4 Mev 1100 °C CONTROL IRRADIATED SPECIMEN A15-34 Experiment 41-9, Cold Pressed and Sintered Beo. ........... . . Fig. 7 WS - " - . W : o''. ............................... .. .. ..... ........... is.. . Irradiated Beo Single Crystals. S Fig. 8 - - - . * * .55 . mentor . . 12 . ' Y N 010 . DATE FILMED / 15 165 .. M -LEGAL NOTICE This report was prepared as an account of Government sponsored work. Noither the United Statos, nor the Commission, nor any person acting on behalf of the Commission: A. Makes any warranty or representation, expressed or implied, with respect to the accu- racy, completeness, or usefulness of the information contained in this report, or that the use of any information, apparatus, method, or process disclosed in this report may not infringe privately owned righto; or B. Assumos any liabilities with respect to the use of, or for damages resulting from the use of any information, apparatus, method, or process disclosed in this report. As used in the above, "por son acting on behalf of the Commission" includes any em- ployee or contractor of the Commission, or employee of such contractor, to the extent that such employee or contractor of the Commission, or employee of such contractor prepares, disseminates, or provides access to, any Information pursuant to his employment or contract with the Commission, or his employment with such contractor. END MNIA TYUN ''** I '" 1 " . TO 7 ,