* -->' ..'. . . --. ... I OFT ORNL P 3336 . . ... EEEFEEEE - 11:25 | 1.4 ILLE MICROCOPY RESOLUTION TEST CHART NATIONAL BUREAU OF STANDARDS - 1963 " .. . :1 ,'. T ., . -.. :* * ;; - ,,.; - 9 .-'*" ' ' .-! ! ! ;. ... . .. . ..."," s " . .. . ... 1 - . - - - - Orm - * - - . - - - - - - - - . - - - -- . + . . - - . . -- - - - Y - :. i -- - - ' - - 1 - ... - - - .- ".. - - - .3330 CESE BRICHES HC 3.40, ww e65 CON 4-670533-6 J - r - .. -- - - - -- > - - . - + - --- + - - + + - - . - + aw- . - -- . C-+ . - • - • • - • • • -- * EAU . • . . • ' .- • . • - - • . . 1 APPLICATION OF ELECTRON METALLOGRAPHY TO.. PRECIPITATION STUDIES OF HASTELLOY N* mer Yuyun S - - 1 . - : :... Kinesteranderende olie ewige Vilniathirimedit. ********* - TURN EN .VN - 2 . - .- ' RECEIVED BY DTIE OCT 2 1967 - R. E. Gehlbach and J. T. Houston Metals and Ceramics Division Oak Ridge National Laboratory Oak Ridge, Tennessee - - :- - *. 1 - T ::.... - U . - - . - -- - - .-- A - . 1 - ABSTRACT . . - yeni S 1 -"- - - - - - . - - - . .. . 7 . - Various techniques available in electron metallography must be used to complement each other in order to gain a clear understanding of precipita. tion reactions. Besides transmission microscopy of thinned bulk samples, we have found that techniques for extraction of all precipitates in contact with a surface are important to reveal precipitates not observed in trans- mission or by usual replication techniques. Extraction replicas permit detection of sheets of very thin grain boundary precipitates as well as those seen by the usual techniques. Electron diffraction patterns may be easily obtained, without interference from the matrix, to get precipitate crystal. lography. The use of a microprobe attachment on the electron microscope permits qualitative identification of precipitates and, in many cases, a quantitative analysis. . . - . 1 . INTRODUCTION : . 1 . - - - 71 Hastelloy N, a nickel-base molybdenum-chromium-iron alloy which was developed at Oak Ridge National Laboratory (ORNL) specifically for its ex- cellent creep strength and resistance to corrosion by molten fluoride fuel salts, exhibits the pronounced loss in high-temperature ductility typical of nickel-base alloys. As shown in Fig. , irradiation further reduces the high-temperature ductility, its effect being essentially superimposed on that of unirradiated material. Since Hastelloy N is the structural material for the Molten Salt Reactor Experiment reactor vessel which has an operating temperature of 650°C, well into the range of the ductility decrease, it is imperative that the material be more fully understood and improved for future use in molten-salt systems. Preliminary examination of several unirradiated . - - ---, 42 • , • W .: V - AW - *Research sponsored by the U. 8. Atomic Energy Commission under contract with the Union Carbide Corporation. : LEGAL NOTICE . - - - . " ..2 - - - * ---- :-... - This report was prepared as an account of Government sponsored work. Neither the United States, nor the Commission, nor any person acting on behalf of the Commission: 1 A. Makes an; 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, molbod, or proceso disclosed in this report may not infringe privately owned rights; or B. Assumes any liabilities with respect to the use of, or for damages resulting from the use of nay information, opparatus, method, or process disclosed in this report. As used in the above, "person acting on behalf of the Commission" Includes any en ployee or contractor of the Commission, or employee of such contractor, to the extent such employee or contractor of the Commission, or employee of such contractor pr disseminates, or provides access to, any Information pursuant to his employment a with the Commission, or his employment with such contractor, -- BASTRIBUTION OF THIS DOCUMENT IS ONLINUTED Merry SA !* * - * NT$777 - - . ' . -- -- . - - 2 - specimens by transmission electron microscopy indicated grain-boundary pre- cipitation occurring in the same temperature range as the drop in ductility, Thus, an investigation was initiated to determine the pattern of. precipita- tion in this system and its relation to mechanical properties, and to iden. tify harmful as well as beneficial precipitates. TRANSMISSION ELECTRON MICROSCOPY . - - - * -.. Initial precipitation studies employed transmission electron microscopy. Matrix precipitation often was not detected although large blocky M&C car- bides were present both in the matrix and in grain boundaries. Figure 2, a low magnification optical micrograph, shows the distribution of the blocky carbide precipitate and the heterogeneous nature of this system. This alloy was quite unattractive for transmission work, Difficulty arose in routine preparation of transmission saraples having uniformn thin regions extending nuore than 50 H from the edge of a hole, creating problems associated with biased sampling and erroneous interpretation of results. The extensive grain-boundary precipitate from an aging treatment or from hign-temperature testing was not always homogeneous. Transmission techniques were also limited in that the true nature of grain-boundary precipitates could not be studied, since we were seeing only a thin cross section of the grain bound- ary. Also thin precipitate films were usually undetectable in transmission. - To - Several of these problems are illust ed in Fig. 3, a transmission micrograph of Hastelloy N irradiated at 650°C for 5000 hr and tested at 650°C. We see a great deal of precipitate both at grain and incoherent twin boundaries but none at coherent twin boundaries. However, most co- herent twin boundaries in the particular material were found to have large amounts of precipitates. Strain fields often exist around particles to obscure observation, such as the dark area in the center caused by & Large carbide in the grain boundary. - - - , 1 -- Despite the limitacions of transmission electron microscopy, it does provide information that is unobtainable by other techniques, such as the presence of fine precipitates and factors concerning the dislo ture, Thin foils were prepared from bulk materials, as previously described using an electrolyte consisting of 30% HINO, 5% H3POs, and 65% methyl alcohol, with phosphoric acid added to obtain uniform rates of thinning of both car- bides and matrix. - e r - . - ... .-. - - . EXTRACTION REPLICAS - . . . -. ... me .... In order to overcome the limitations of the transmission technique and to study the precipitates more fully over large regions of the sample, electrolytic extraction techniques were utilized. Specimens were mounted and mechanically polished, the final polishing step using half-micron diamond abrasive. Provision was made for an electrical contact, usually through the back of the mount. After polishing, the samples were lightly C.K.H. DuBose and J. 0. Stiegler, Semiautomatic Preparation of Speci. mens for Transmission Electron Microscopy," ORNL-4066, February 1967. ............ .. ......... . ---. - - - etched, either chemically or electrolytically, to reveal all precipitates and to remove any smeared matrix material. Carbon replicas were obtained using a solution of 10% HCl in ethyl alcohol with a current density of 0.1 amg/in. or less. Etching times varied, depending on the amount of connected grain-boundary precipitates. In some cases the samples were etched for 24-36 hr to dissolve sufficient matrix and to release the grain- boundary precipitates. ------ ----- ---- - --- ----- Extraction techniques permit observation of precipitates in the same distribution as that existing in the bulk sample, with the exception that grain-boundary precipitates are no longer supported by the matrix and col- lapse against the substrate. However, this permits direct observation of the grain-boundary precipitates on essentially the surface of the original grain boundary. This is demonstrated in Fig. 4 by an el ectron micrograph. of an extraction from Hastelloy N which was aged at 87 showing grain- boundary precipitation where the precipitate has t'allen against the replica. If the polished somple surface or replica were parallel to the plane of the micrograph, the distribution of dendritic-like precipitates in the bulk sample would project towards the viewer at an angle corresponding to that of the grain boundary. If we were then to remove a thin slice, parallel to the page, from the projecting precipitate, the results would be the morphology seen optically or in transmission, as in Figs. 5 and 6, respectively. Fig- ure 7 shows another example of cellular grain-boundary carbide formation and also the appearance of the replica when the precipitate is not fully retained. When Hastelloy N 13 annealed at hicb temperatures, optical micrographs show a lamellar precipitate in the grain undaries. Extractions from this material show a variety of morphologies, several of which are seen in Fig. 8. Variations in contrast are due to differences in thickness of the precipi- tates. Here we see thin dendritic-like sheets, probably on the order of 100A in thickness, as well as the lamellar type which is 20 to 50 u thick. The thin sheets are usually undetectable by transmission techniques. Hastelloy N which has been modified by decreasing the molybdenum con- centration and adding small amounts of titanium shows an improvement in properties. The microstructure appears to be quite clean, both by optical and transmission examination. Extraction replicas, however, reveal a con- siderable amount of grain-boundary precipitation. Figure ga shows an inter- action between a small precipitate particle and a thin film of precipitate extracted fron a grain boundary. Ti(C,N), identified by electron diffraction, is the major precipitate found in this titanium-rodified system and, like MC in the standard Hastelloy N, may assume various morphologies. Ti(C,N) is present in Fig. 9. In Figs. 9c and 9a, Ti(C,N) exists with another phase, as yet unidentified. The thin film and thread-like precipitates in Figs. 9c and 9d are Ti(C,N) with the unidentified phase taking the form of the thicker spines and polyhedral particles, Fig. 9d. ." . " High-Temperature Materials Program Progress Report No. 61, QE-NMPO, GEMP-61, Sept. 30, 1966, p. 128. - .4 . ELECTRON DIFFRACTION The identification of crystal structure and the determination of lattice parameters of precipitates are greatly simplified using extraction replicas since matrix interference is eliminated. Diffraction patterns are very easily obtained from thin grain-boundary precipitates and the large blocky carbides often have thin edges due to metallographic mlishing, thus alloy- ing sufficient transmission to obtain satisfactory patterns. We generally evaporate a thin layer of gold or copper onto the replica 'before insertion into the microscope. This provides a standard for deter- mining the lattice parameters, and eliminates the camera constant error associated with 3light changes in lens currents. If microprobe analysis is to be carried out simultaneously, the standard must be chosen so as to not interfere with the analyzed elements. Diffraction patterns obtained from these precipitates are often quite complex and measurement of spots quite tedious, but we have a method which permits relatively good accuracy and rapid solution for routine identifications, .. . ... . .. .... - - ". . . .. -.- . A circle, corresponding to the (111) ring of the standard when a photo- graphic plate of the diffraction pattern 18 projected through an enlarger to & convenient size, 1.8 inked on white cardboard. (We have found a gold (111) ring of 20- to 25-cm diam convenient.) Additional boards may be made for precipitates encountered frequently, such as MC or Tic, with rings for various (hk) positions calibrated to the standard (111) ring. Thus, a rapid diffraction pattern evaluation may be made and spots not belonging to the phase in question can be readily noted. Measuring of spots on patterns from unidentified precipitates is carried out on white paper after standard. izing plate magnification to the standard ring in the pattern. Since no wet processing is used, distortion associated with photographic paper shrinkage is eliminated. i 1 . i : -,. . - . . ELECTRON MICROPROBE ... Another promising aspect of extraction replicas appears to be with . microprobe analysis of individual particles. We have added a Hitachi HXA-Lii electron probe microanalyzer accessory to one of our electron microscopes, which permits at least a semi quantitative determination of composition. A beam size of ~ 24 is employed (second condenser crossover); but, since matrix effects are eliminated by using extraction replicas, only x-rays from the precipitate particles are analyzed. Areas for analysis may be selected with great accuracy and small particles may be analyzed, electron diffraction patterns obtained and high resolution electron micrographs madu without re- moving the area from the beam. The thin grain-boundary precipitate films may also be analyzed very easily. . Complete qualitative analysis of a particle may be made in ~ hr. The limit of detectability is on the order of 10-** gran grams of pure material, or in the case of nickel, a sphere of ~ 600 A 199dius. . 5 . Qualitative analysis of the blocky carbides in Hastelloy N with respect to the matrix shows a large lacrease in molybdenum and a decrease in nickel, which is in agreement with conventional microprobe studies carried out pre- viously. Although we have not performed any quantitative analysis at this time, this technique appears to be very valuable, particularly when used in conjunctioa with conventionsá microprobe work. SUMMARY The various techniques available for electron microscopy have limitations and must be combined for effective investigations of the structural state, Transmission techniques permit observation of dislocation structure and fine matrix precipitate, but many types of grain-boundary and large matrix pre- cipitates are difficult or impossible to study by this method. Extraction techniques permit the study of thin grain-boundary precipi- tates wridetectable in transmission. Other advantages include retention of Mulk" morphology, study of grain-boundary precipitate and precipitate on fracture surfaces, ease in obtaining electron-diffraction patterns, and applicability to microprobe work. Recently developed microprobe attachments for the electron microscope permit chemical analysis of particles without interference from the wiatrix, & problem encountered with the bulk microprobe. Electron micrographs, . selected area electron-diffraction patterns, and chemical analysis of either replica are now possible without removal of the specimen from the microscope. FIGURE CAPTIONS ORNL-DWG 67-24152 Fig. 2. Effect of Irradiation on the Tensile Ductility of Hastelloy N After Irradiation at 650°C for 4800 hr in the Molter Salt Reactor Experiment to a Fluence of 1.3 x 10". Y-75712 Fig. 2. Low Magnification Optical Micrograpk of Hastelloy N Showing Heterogeneous Distribution of Precipitates After Annealing 1 hr at 1177°C. Etched in lactic regia. YE-9342 Fig. 3. Transmission Electron Micrograph of Hastelloy N 5081 After Tensile Fracture at 650°c. Fig. 4. Extraction Replica from Hastelloy N, Aged 4 hr at 370°c. All precipitates are M&C. Y-77654 Y-75743 Fig. 5. High Magnification Optical Micrograph frora Hastelloy N, Aged : at 870°C. (See Fig. 4) Fig. 6. Transmission Micrograph of Grain Boundary Carbides After Aging at 870°c. (See Fig. 4) YE-9283 YE-9337 Fig. 7. Cellular Grain Boundary Carbides in Hastelloy N. YE-9343 Fig. 8. Extraction Replica Showing Various Morphologies at Precipitates in Hastelloy N Annealed at 1370°C. YE-9309 YE-9338 YE-9341 Fig. 9. Precipitates Extracted from Crain Boundaries of Titanium-Modified Hastelloy N. (a). Interaction between small unidentified particle and Ti(C,N) film. (b). Common Ti(C,N) morphology. 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