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By S. F. Bartram, G. A. Chase

COMPUTED X-ray diffraction powder patterns of YNi3, YNi5, and CbBe3 are available on request from either author.

Jan 1, 1968

By C. D. Gilpin, Franklin Moeller

The application of electric power for driving mine hoists handling heavy loads at high speeds has recently been extended by the installation of what is probably the largest electrically driven hoist in this country at the Granite Mountain shaft of the North Butte Mining Co., Butte, Mont. While the weight of rock which is hoisted by this machine is not the largest now being handled by electric mine hoists, the speed of hoisting is so, and the combination of the high speed with the heavy load has resulted in a machine of considerable interest to all those actively engaged in mining. Aside from mere considcration of size, this installation deserves attention because of the careful attention given, not only to the question of economy of operation, but to the details of construction and installation of the entire equipment. The conditions to be met in this installation were as follows: Weight of rock to be raised per trip, 7 gross tons........... 15,680 1b. Weight of skip.......................................... 8,000 1b. Weight of cage.......................................... 1,800 1b. Maximum depth of hoisting.............................. 4,000 ft. Diameter of rope.......................................... 15/8 Total weight suspended on one rope from drum............. 42,000 1b. Normal hoisting speed.................................... 2,700 ft. per minute. Maximum hoisting speed.................................. 3,000 ft. per minute. Desired capacity-200 tons per hour from 4,000 ft. depth. The ore is mined in several levels and hoisting is carried on from the 800-ft. level down to the 2,700-ft., which is at present the maximum depth from which the ore is raised regularly. Development is proceeding and a depth of 2,900 ft. has already been reached. The rock is handled underground in cars holding % ton, and about 10 cars are the usual load for a skip. All of the ore is dumped into underground bins, which are of diffcrent capacities varying up to 250 tons. From the bins the ore is fed into the skips without passing into measuring pockets. At the surface the

Jan 1, 1916

By J. O. Betterton, W. M. Spicer

The solubilities of antimony in the a and ß-forms of zirconium were determined between 750" and 1300°C. The a-phase forms by a peritectoid reaction, and the a/(a + ß) and ß/(a + ß) phase boundaries rise in temperature with in- ' creasing antimony. Impurities in the 99.95 pct zirconium were sufficient to influence the phase boundaries and the variation reported is approximate. The restricted solid solubility of the terminal zirconium phases, which is especially characteristic of this system, is thought to result from the low free energy of the Zr2Sb phase. ZIRCONIUM-antimony alloys are important in zirconium alloying studies since antimony is one of the highest valent elements which can be used to make zirconium alloys. The dilute alloys are of further interest as they have somewhat better corrosion resistance' than pure zirconium. The first investigation of the phase diagram was made by Russi and wilhelm2 who found a eutectic reaction, liquid (- 17.5 at. pct Sb) = ß zirconium (- 11 at. pct Sb) + Zr2Sb, at 1430°C'. The Zr2Sb phase was of complicated hexagonal structure, and by thermal analyses of the relatively impure alloys then available, Russi and Wilhelm found evidence for the peritectoid formation of the a-phase. EXPERIMENTAL In the present work, the phase diagram was re-investigated in the region 0 to 5 at. pct Sb and 750" to 1300°C using iodide-zirconium alloys. Details of the procedure have been described earlier. Essentially the alloys were prepared by arc casting and were then examined by the annealing and quenching method. The times of annealing varied from 1 hr at 1300°C to 30 days at 760°C. As in other zirconium phase-diagram studies1"5 the impurities in the zirconium were still sufficient to affect the results, and the experiments will therefore be described in 3 parts. The results from the first 2 parts of the work are shown in Fig. 1. Here the ß/(ß + Zr2Sb) and a/(a + ZrzSb) phase boundaries were determined with alloys made from 99.9 pct zirconium,* and cast under such conditions that the Vickers hardness of a alloys extrapolated to 95 to 110 VPN at 0 at. pct Sb. Such alloys were not suitable for investigations of the (a + ß) region, and the results shown in Fig. 1 near the (a+ ß) and (a +ß + Zr2Sb) regions were determined with purer alloys. These alloys had an extrapolated hardness range of 75 to 85 VPN and were made from 99.95 pct zirconium. A deviation from binary equilibrium occurs in Fig. 1 as indicated by the (a + ß) region of pure

Jan 1, 1959

By Ian J. Smalley

"Quickclay is an extreme case, it is by far the most mobile of all the common solid materials on the earth's surface. It has both a high water content and a mineral texture that allows it to flow with the utmost ease. A mass of quickclay that has lain undisturbed for thousands of years can be jarred into motion by any sudden shock." The quotation is from the paper by Kerr called, "Quickclay," which was published in Scientific American in 1963. This was probably the most widely read paper on quickclay ever published. It was reprinted by Fred Betz in his Benchmark collection on Environmental Geology (BM 25), A quickclay is an extremely sensitive soil. The sensitivity parameter is produced by dividing the undisturbed shear strength by the remoulded shear strength. If a value greater than 50 is obtained, then the soil can be classified as a quickclay. True quickclays are characterized by a very low remoulded strength of the order of 0.5 kPa. The classic quickclays are found in Scandinavia and Eastern Canada, but the 1964 Alaska earthquake revealed a considerable quick¬clay deposit underlying the town of Anchorage. This was discussed in a classic paper by Kerr and Drew in Engineering Geology in 1967. The Kerr views on quickclays were perhaps most clearly expressed in the paper with Liebling in Geol. Soc. Amer. Bull. in 1965. They suggested that the major critical conditions which contribute to quickclay movement are: substantial quantities of layer lattice silicates of colloidal size (about 40% or more by dry weight), sub¬stantial pore water (44%), a reduction in electrolyte concentration below 5 g/l of salt, and addition of a dispersant. There is still discussion and disagreement about the nature of quickclays and the mechanisms of quickclay slides; the "clay mineral"-based views favored by Kerr still find support, although an alternative "primary mineral" view suggests that it is the finely ground primary minerals

Jan 1, 1985

By David S. Butts

The high cost of energy has made many solution mining corporations turn from fuel consuming evaporators to solar energy and solar ponds. The generally held concept of a solar pond is an area enclosed by dikes into which brine is pumped, water evaporated by the sun, and the resulting salts scraped from the bottom of the pond. This paper will show that solar ponding is not simple. It is a science involving six main areas. These areas are (1) land conditions, (2) meteorology, (3) fresh water, (4) accessibility, (5) manpower and (6) mineral resources. Each area is discussed to identify important parameters that must be investigated before the viability of a solar pond complex can be established as a mineral recovery step.

Jan 1, 1985

By Julian E. Tobey

A MEMORABLE year has just passed in the field of coal utilization. Because of the war, oil conversions in industrial, commercial, and domestic installations have been made to the equivalent of 20,000,000 tons of coal. The war emergency has resulted in a great shifting of various types of coals to various markets. Huge tonnages of metallurgical-quality coals have been withdrawn from steam and domestic business and sent into the iron and steel industries. Marginal coals have replaced these coals in the steam and domestic field.

Jan 1, 1944

By Shiou-Chuan Sun

THERE are several postulations for the mechanism of slime-coating. Ince1 proposed the electrostatic hypothesis, del Giudice2 suggested the chemical theory; Bankoff3 reported that slime-coating is inhibited whenever the surfaces of the slime particles are ionized sufficiently for Brownian movement to occur, and is facilitated when they are not. These postulations were examined by experiments involving the Burton tube, the cataphoretic cell, and slime-coating. The techniques involved will be described elsewhere in this paper. The electrostatic hypothesis, supported by migration experiments in a Burton tube, was abandoned by del Giudice.2 Experiments of mineral migration in a Burton tube, after the idea of Ince with modification, indicated that this apparatus was inefficient for accurate observation. A cataphoretic cell was constructed. The experimental data, as shown in this paper, enable the correlation and advancing of this hypothesis. Del Giudice's chemical hypothesis considered that slime particles are attached to the galena surfaces by a cement formed as the result of a metathetical reaction between the sulphide and the slime particles. Applying this hypothesis, the calcite slime particles were cemented to the galena surface by the formation of a cementing lead carbonate. In a similar way, lead silicate was considered as the cement of quartz slime coating on galena. Experiments verifying this hypothesis were carried out according to the following procedure: Fresh mineral particles selected from the central part of the broken lumps and examined first under a microscope for ascertaining a clean surface were placed in a small beaker (1.5-in. dia. by 2.5 in. deep) half filled with one kind of slime pulp. The dilution of all slime pulp was 4: 1 and the particle size of slime was minus 400-mesh. After agitation for 5 min. the specimen was removed by a sharp-end tong and washed gently three times in three separate distilled water baths. It was dried before a small electrical fan and examined immediately under a microscope. A photograph was made of the observation. With reference to the published solubilities,4 several of these experiments, which contradict the chemical hypothesis, are listed as following: I. The coating of fluorite slime on the galena surface was light but the coating of galena slime on the fluorite surface was heavy. In a similar way, the coating of quartz slime on the galena was fairly light, but the coating of galena slime on the quartz particle was heavy. According to the chemical hypothesis, using the same constituents and regardless of which is the slime, the density of the coating should be expected to be the same. This, however, as shown above, is not true. Moreover, fluorite (CaF2), having a solubility of 16 mg.[4a] per liter of water, should not be

Jan 1, 1943

By J. A. Bailey, J. H. Tundermann

The dihedral angles of the solid-liquid interfaces were measured at various temperatures above the solidus and the interfacial energies calculated when small additions of copper, indium, lithium, magnesium, antimony, and silicon were made to an aluminum alloy containing 3 pct Sn. When the results were compared with those of the Al-Sn alloy some differences were found which could be interpreted in terms of the ability of the added element to enter into solution or form intermetallic compounds with the aluminum and tin. It was shown that in some cases considerable changes in the shape of intergvanular liquid films can be brought about by comparatively small compositional changes in the alloy. DURING the melting or solidification of an alloy a temperature range is usually found where the presence of a liquid phase may be detected at the grain boundaries of a solid. It is believed that the presence of this liquid phase is responsible for hot tearing in castings and welds and hot shortness in the working of some alloys at elevated temperatures. Rosenberg, Flemings, and Taylor1 in a study of the solidification of aluminum castings have indicated the importance of intergranular liquid films and shown that their shape and distribution at the end of solidification effect the hot tearing characteristics of the material. The shape of such intergranular liquid films are determined largely by the ratio between the solid-liquid interfacial energy (yLS) and the grain boundary energy (ySS). A measure of this ratio (yLS/ySS , relative interfacial energy) is the dihedral angle 8. The dihedral angle 0 is related to the relative interfacial energy by the following expression: Rogerson and Borland 2 have also suggested that the shape of the intergranular liquid is an important factor in determining the susceptibility of a material to hot shortness. They showed that on a comparative basis materials having the lowest dihedral angles at a given temperature gave the greatest severity of cracking. They stated that liquid in the form of globules should be less harmful than liquid in the form of extensive films as more intergranular cohesion should be possible. Rogerson and Borlland 2 also showed that the susceptibility of an A1-Sn alloy to hot cracking can be reduced by small additions of cad- mium. It was found that the cadmium gave an increase in the dihedral angle at all temperatures. Ikeuye and smith3 investigated changes in the dihedral angle and relative interfacial energy with temperature for a number of ternary alloys formed when small additions of bismuth, cadmium, copper, lead, and zinc were made to an A1-Sn alloy. They found that in most instances changes in the dihedral angle were caused by compositional changes in the liquid phase; as the composition of the liquid approached that of the solid the dihedral angle decreased. They noted that the addition of a third element which was soluble in both the liquid and solid phases at a given temperature may decrease the dihedral angle (e.g., the addition of copper or zinc) but otherwise the ternary alloys formed exhibited dihedral angles between those of the A1-Sn binary alloy and those of the binary alloy of aluminum with the added element. Dwarakadasa and Krishnan4 investigated the changes in dihedral angle and relative interfacial energy with temperature when small additions of magnesium, iron, silicon, manganese, sulfur, cobalt, and silver were made to a copper alloy containing 3 pct Bi. They found that in all cases the added elements gave an increase in the dihedral angle and relative interfacial energy when compared with the values obtained for the simple binary alloy at the same temperature. It was noted that an increase in temperature gave a decrease in dihedral angle and relative interfacial energy in each of the ternary alloys studied. Similar results have been obtained by Ramachandran and Krishnan5 for the addition of small quantities of lead. This paper describes the application of dihedral angle measurement to the determination of the shapes of liquid phases at various temperatures above the solidus when small additions of copper, indium, magnesium, lithium, antimony, and silicon are made to an aluminum alloy containing nominally 3 pct Sn. An attempt is made to correlate the measurements with the relative solubility of the added elements in tin and aluminum. The work was undertaken to provide more data concerning the effects of temperature and composition on the shape of liquid films above the solidus. EXPERIMENTAL PROCEDURE In the present work ternary aluminum alloys containing nominally 3 pct Sn and small additions of high-purity copper, indium, lithium, magnesium, antimony, and silicon were made. The alloys were melted in a graphite crucible under an inert atmosphere of argon and cast into ingots 6 in. long by 0.5 in. diam. The ingots were then cut into rods 1.5 in. long, given a 50 pct cold reduction, and machined into test pieces 0.5 in. long by 0.5 in, diam for heat treatment. The alloy samples were annealed at the various test temperatures between the liquidus and solidus for approxi-

Jan 1, 1967

By E. A. Jones

THE Southeast Missouri division of the St. Joseph Lead Co. normally hauls and hoists over 5 million tons of lead ore each year. This ore is mined in the stopes and headings of 20 mines, hauled to a main line system, see above, and transported up to 6.4 miles to ore-hoisting shafts. Average haulage distance is 2.16 miles. A few years ago a distinguished mining engineer visiting this area for the first time remarked, "You do not have a mining problem; yours is a haulage problem." Its relative importance may be gaged by the fact that mine haulage represents about 25 pct of the total cost of mining ore, the most costly single underground operation

Jan 4, 1953

By Shiou-Chuan Sun

There are several postulations for the mechanism of slime-coating. Incel proposed the electrostatic hypothesis, del Giudice2 suggested the chemical theory; Bankoff3 reported that slime-coating is inhibited whenever the surfaces of the slime particles are ionized sufficiently for Brownian movement to occur, and is facilitated when they are not. These postulations were examined by experiments involving the Burton tube, the cataphoretic cell, and slime-coating. The techniques involved will be described elsewhere in this paper. The electrostatic hypothesis, supported by migration experiments in a Burton tube, was abandoned by del Giudice.2 Experiments of mineral migration in a Burton tube. after the idea of Ince with modification, indicated that this apparatus was inefficient for accurate observation. A cataphoretic cell was constructed. The experimental data, as shown in this paper, enable the correlation and advancing of this hypothesis. Del Giudice's chemical hypothesis considered that slime particles are attached to the galena surfaces by a cement formed as the result of a metathetical reaction between the sulphide and the slime particles. Applying this hypothesis, the calcite slime particles were cemented to the galena surface by the formation of a cementing lead carbonate. In a similar way, lead silicate was considered as the cement of quartz slime coating on galena. Experiments verifying this hypothesis were carried out according to the following procedure: Fresh mineral particles selected from the central part of the broken lumps and examined first under a microscope for ascertaining a clean surface were placed in a small beaker (1.5-in. dia. by 2.5 in. deep) half filled with one kind of slime pulp. The dilution of all slime pulp was 4:I and the particle size of slime was minus 400-mesh. After agitation for 5 min. the specimen was removed by a sharp-end tong and washed gently three times in three separate distilled water baths. It was dried before a small electrical fan and examined immediately under a microscope. A photograph was made of the observation. With reference to the published solubilities,' several of these experiments, which contradict the chemical hypothesis, are listed as following: I. The coating of fluorite slime on the galena surface was light but the coating of galena slime on the fluorite surface was heavy. In a similar way, the coating of quartz slime on the galena was fairly light, but the coating of galena slime on the quartz particle was heavy. According to the chemical hypothesis, using the same constituents and regardless of which is the slime, the density of the coating should be expected to be the same. This, however, as shown above, is not true. Moreover, fluorite (CaF2), having a solubility of 16 mg.4a per liter of water, should not be

Jan 1, 1943

By Shiou-Chuan Sun

There are several postulations for the mechanism of slime-coating. Incel proposed the electrostatic hypothesis, del Giudice2 suggested the chemical theory; Bankoff3 reported that slime-coating is inhibited whenever the surfaces of the slime particles are ionized sufficiently for Brownian movement to occur, and is facilitated when they are not. These postulations were examined by experiments involving the Burton tube, the cataphoretic cell, and slime-coating. The techniques involved will be described elsewhere in this paper. The electrostatic hypothesis, supported by migration experiments in a Burton tube, was abandoned by del Giudice.2 Experiments of mineral migration in a Burton tube. after the idea of Ince with modification, indicated that this apparatus was inefficient for accurate observation. A cataphoretic cell was constructed. The experimental data, as shown in this paper, enable the correlation and advancing of this hypothesis. Del Giudice's chemical hypothesis considered that slime particles are attached to the galena surfaces by a cement formed as the result of a metathetical reaction between the sulphide and the slime particles. Applying this hypothesis, the calcite slime particles were cemented to the galena surface by the formation of a cementing lead carbonate. In a similar way, lead silicate was considered as the cement of quartz slime coating on galena. Experiments verifying this hypothesis were carried out according to the following procedure: Fresh mineral particles selected from the central part of the broken lumps and examined first under a microscope for ascertaining a clean surface were placed in a small beaker (1.5-in. dia. by 2.5 in. deep) half filled with one kind of slime pulp. The dilution of all slime pulp was 4:I and the particle size of slime was minus 400-mesh. After agitation for 5 min. the specimen was removed by a sharp-end tong and washed gently three times in three separate distilled water baths. It was dried before a small electrical fan and examined immediately under a microscope. A photograph was made of the observation. With reference to the published solubilities,' several of these experiments, which contradict the chemical hypothesis, are listed as following: I. The coating of fluorite slime on the galena surface was light but the coating of galena slime on the fluorite surface was heavy. In a similar way, the coating of quartz slime on the galena was fairly light, but the coating of galena slime on the quartz particle was heavy. According to the chemical hypothesis, using the same constituents and regardless of which is the slime, the density of the coating should be expected to be the same. This, however, as shown above, is not true. Moreover, fluorite (CaF2), having a solubility of 16 mg.4a per liter of water, should not be

Jan 1, 1943

By Horace V. Winchell

The St. Helens mining-district, indicated in sketch-map, Fig. 1, is chiefly in Townships 9 and 10 North, Ranges 5 and 6 East of the Willamette meridian, in Skamania county, Wash. There is no railroad or even a wagon-road at present connecting it with any base of supplies; access is usually by wagon-road for about 50 miles from the town of Castle Rock to Spirit lake, and from that point by pony-trail from 6 to 10 miles farther. History. Nearly 20 years ago two German farmers, totally inexperienced in prospecting, penetrated this region upon a hunting-and fishing-trip. Their attention was drawn to numerous joints and crevices filled with black, glistening tourmaline, and con-

Jan 1, 1913

By George F. Beardsley

The silver-fields of Zeehan and Dundas are located on the "West Coast" of Tasmania, 30 miles from the port of Strahan on the Macquarie Harbor. This harbor is 17 miles long, from 4 to 5 miles wide, and completely landlocked. Its only drawback is a shallow bar with 9 feet of water on it. The hills on the western side of the harbor vary from 200 to 300 feet in height, and are all composed of quartzite or a quartz grit. From 15 to 20 miles back from the eastern shore of the harbor is a conglomerate-capped range of mountains, rising to the height of 4700 feet. The immediate eastern

Jan 1, 1893

By G. R. St. Pierre, A. Ghosh

In the Si-C-0 system at temperatures of interest in process metallurgy there are four stable condensed phases—silicon, carbon, silica, and silicon carbide (Sic). Silicon melts at 1683oK1 and shows negligible solubility for carbon and oxygen at 1700°K. However, silicon dissolves approximately 1.5 at. pct C at 2500oK.2 Carbon in the form of graphite remains pure and dissolves negligible amount of silicon.' Silica (crysto-balite) melts at 2001°K' and is essentially a stoichio-metric compound. Silicon carbide is a solid and shows negligible deviation from stoichiometry up to approximately 2800oK.2 Besides the condensed phases there is a gas phase

Jan 1, 1970

By J. Mark Gronseth

The instantaneous shut in pressure often times is not a well defined feature of pressure-time records from in situ stress determinations by hydraulic fracturing. As the applications of in situ stress data become more sophisticated, the grea5er the need for an unambiguous method with which to identify the instantaneous shut in pressure becomes. Controlled experiments suggest that the instantaneous shut in pressure should be equated with the pressure at the inflection point of the pressure-time record following shut in. A method for determining this value is presented. Often times the minimum instantaneous shut in pressure determined after several pressurization cycles is the best estimate of the stress acting perpendicular to the fracture plane.

Jan 1, 1982

By Gilbert L. Eggert

The effects of reactor irradiation on age hardening in a Cu-2 wt pct Be alloy have been investigated in two neutron-energy ranges. During some of the irradiations, specimens were exposed to high-energy fission neutrons which passed through a boron-10 shield; during other bombardments, the boron-10 was omitted and specimens were irradiated in a reactor thermal column, or the fuel configuration was modified to increase the thermal-neutron flux at a location in the core. Differences in length, X-ray diffraction angle, and hardness indicated that low-energy neutron irradiation made a small contribution to changes in the measured properties. The influence of defects generated by knock-om with less than the Brinkman critical energy or by prompt (n,y) recoil is suggested as the cause of this effect. EXPERIMENTS designed to test the effects of reactor irradiation on the properties of age-hardening alloys have to the present time employed fluxes un-differentiated according to neutron energy. Billing-ton and Siegell in 1950 were the first to perform such an experiment and to compare the results with those obtained by thermal aging. These authors concluded that precipitation in a Cu-2 wt pct Be alloy was not enhanced by the radiation. However, 4 years later, Murray and Taylor,2 working with specimens of the same Cu-2 wt pct Be alloy, reported that an increase in density, hardness, and resistivity which followed reactor irradiation resembled changes associated with thermal aging at about 100°C. (It should be noted that these authors reported that higher aging temperatures caused a decrease in resistivity.) cupp3 reported hardness results similar to those of Murray and Taylor. Koppenaal4 showed that irradiation-enhanced precipitation and irradiation defect hardening were not simply additive but that they acted separately in an irradiated alloy. Kernohan et a1.,5 working with Ni-Be, offered evidence that beryllium was removed from solid solution by reactor irradiation and suggested that the mechanism was one of increased diffusion through the use of vacancies in the structure. piercy6 also found that more precipitate particles were formed by fission-neutron irradiation of a Cu-Co alloy which contained a small amount of particles before irradiation. He proposed that the additional particles were caused by an appreciable amount of diffusion during the final cooling of displacement spikes. The retrogression of extant precipitate particles found by Murray and Taylor2 and Boltax7 as well as piercy6 indicated that nuclei were dissolved within a high-energy spike region and, upon resolidification of the perturbed volume, new nuclei precipitate and grow by enhanced diffusion. Bleiberg et al.' and Konobeevski et al.' explained phase changes obtained by irradiating fissionable alloys in terms of retrogression and re-precipitation in regions of high-energy spikes. Parsons and Balluffi10 used electron microscopy to verify that crystallization did indeed occur in displacement spikes which were formed in amorphous germanium by fast-neutron irradiation. The concept that low-energy neutron irradiation might cause structure-sensitive property changes in semiconductors by atomic recoil associated with the (n, y) reaction was first proposed by Schweinler" and walker." This thesis was tested by Cleland and crawford" and found to be valid. Coltman et al.14 exposed a variety of pure metals to thermal-neutron irradiation at cryogenic temperatures and attributed the resulting resistivity changes to the action of defects created by (n, y) recoil. The present work was undertaken to extend the concepts of Schweinler," walker," and Coltman et al.I4 to the case of an age-hardening alloy and to determine whether or not the action of defects produced by thermal-neutron irradiation would en-hance age hardening. EXPERIMENTAL PROCEDURE Omeea West Reactor Irradiations.* Thermal-

Jan 1, 1965

By Charles Stein

The effects of several different prior treatments an the creep behavior of 99.9995 pct aluminum at 260°C and 1000 psi canstant stress are compared with annealed specimens. Quenching from 538oC, irradiation with 2 mev electrons, and tension-compression room temperature fatigue damage were used to change the substructure of the specimens prior to their creep testing. The quenched and the irradiated specimens showed a larger primary and transient stage contribution to the creep curve than those specimens which were only annealed prim to creep testing. The specimen receiving prior fatigue damage at room temperature showed no first stage or transient creep when tested under identical conditions as the above specimens and had an average creep rate seven orders of magnitude lower than that of either the annealed, the quenched or the irradiated creep specimens. In a previous electron transmission microscopy investigationl of the substructure developed during the creep of pure aluminum at 0.57 Tm, it was noted that a large concentration of vacancy loops and dislocation loops were present in and near the subboundaries while the interior of the subgrains contained few of these defects and had a low dislocation density, see Fig. 1. Yim and Grant2 and Hazlett3 have shown that the presence in nickel of a substructure developed by prior cold work effectively reduces the primary and transient contributions to the creep curve. Hultgren,4 McLean,5 Gervais, Norton, and Grant,6 Chang and Grant,7 and others have shown the same effect with the higher stacking fault energy material, aluminum. However, the specific defect responsible for the change in the creep behavior developed by the prior cold work was not established. Specifically, what effectively interfered with dislocation motion in these materials at elevated temperatures? Was it jogs on dislocations produced by their interaction with other dislocations or with vacancy or dipole loops, see Fig. 1, or did the subgrain walls determine the mean free path for glissile dislocations? This would be a realistic possibility only if subgrain boundaries are effective barriers to dislocation motion. The ability of a subgrain boundary to act effectively against glissile dislocations depends on the number and the arrangement of dislocations in the subboundary,8 which in turn is a function of the creep strain.' This paper compares the creep rate of specimens possessing a large vacancy concentration to that of annealed specimens and with specimens having a stable subboundary wall containing Lomer locks produced by prior fatigue damage. EXPERIMENTAL PROCEDURE Vacancy Loops. Aluminum creep specimens, 99.9995 pct pure, were machined from zone refined rod to a 2-in. gage length and a cross-sectional area of 0.025 in. These specimens were annealed at 538oC, 1000°F, for 10 min and quenched into ice water. They were then reheated to the creep test temperature of 260°C, 500°F, and held at this temperature for 18 min to al-low for vacancy condensation and loop formation. The specimens were subsequently creep tested at 1000 psi constant stress at 260°C. The temperature along the gage length was monitored by three Pt-Pt, 13 pct Rh thermocouples, two embedded in the upper and lower shoulders of the specimen and one attached to the mid-point of the gage length- The temperature gradient was held to ± l°C or less throughout the Creep test. Elongations were measured by two LVDT's 'connected in an averaging 'On-figuration, with quartz extension arms placed against the specimen at the extremes of the 2-in. gage length. i K 3J?--' * *H - >^> - ' ^L r 77 . *y J OJL, J Fig. 1—Transmission electron micrograph of pure aluminum strained 8.2 pct at 260°C and 1000 psi constant stress. Note the presence of numerous loops near the light dislocation tangle

Jan 1, 1970

By C. G. Dunn, F. W. Daniels, M. J. Bolton

IN recent investigations1. a data on relative grain boundary energies in silicon iron have been obtained. The present investigation is a continuation of this work along similar lines for the purpose of obtaining additional information on boundary energies. One aim has been to extend the data for a (110) series, which was formerly studied,' to small differences in orientation, since a recent theory3,4 based on a dislocation model of grain boundaries predicts a E. ? (A-ln ? )* form of energy curve for small differences in orientation. Another aim has been to provide data for a (100) series—all grains having (100) planes parallel with the surface of sheet speci-mens—and to compare the results with the predicted form of energy curve. Finally, information on the nature of approach to equilibrium conditions was to be obtained through observations on the movements of grain boundaries. Recently published papers2,3,5 have treated the mathematical problem of expressing equilibrium conditions for grain boundaries for the general case when boundary energy depends upon boundary orientation. The equilibrium equations, which relate equilibrium angles and grain boundary -free energies, contain additional terms that express the variation of energy with boundary rotation. It has been necessary in the present investigation, however, to neglect these additional terms since no data for their evaluation were available. Dropping the additional terms leads to the following approximate equations which were used: E12/sin ?3 = E18/sin?2 =E28/sin?1 or those of the form: E28 + E13 cos ?3 + E12 cos ?2 = 0 Experimental Procedure Except for sample F1, all specimens were made from two lots of silicon iron called C and L respectively. The compositions of these are listed in table I. In the preparation of 12 three-grain specimens for the present investigation, a controlled grain growth technique, which has been described previously,' was used. After preparation, the specimens were notched at the boundaries to shorten them as a means of providing more rapid approach to equilibrium in the anneals. Initial grain boundary angles were determined from micrographs taken at X500. Seven anneals, totaling about two days at 1300°C and two to four days at 1400°C, were run in an atmosphere of pure dry argon as described in a previous paper.' Boundary changes generally could be followed without metallographic surface preparation, because thermal etching occurred during the anneals. These observations indicated angle changes of as much as 35" in some instances, with the major changes occurring during the first anneal. Annealing was discontinued when the angles reached stationary values. Fig. 1 gives a schematic diagram for purposes of defining crystallographic and boundary directions for three grains with common plane parallel with the sheet. Differences in orientations (expressed by A) are the angles between [00l] directions. They can be calculated with the aid of the ?'s. The grain boundary angles can be calculated from the w'S. Results Results are given in table 11. Types of crystal-lographic planes refer to those parallel with the sheet. Orientations are given in terms of [00l] direc-tions as shown in fig. 1. Except for grain 3 of specimen H6, which was unintentionally tilted 7" out of a (100) plane, all grains generally were within 1" or 2" of the plane specified. The directions of boundaries were measured generally to within 1" on both upper and lower surfaces, and the average direc- tions were determined for use in calculating the grain boundary angles. Variations in grain boundary directions refer to deviations from average directions. Boundaries near the junction point for all specimens generally were very close to perpendicu-

Jan 1, 1951

By S. Shapiro, G. Krauss

RECENT investigations1 3 of the products of marten-sitic transformation in Fe-Ni and Fe-Ni-C alloys have made use of light microscopy to describe mar-tensitic fine structure. The application of conventional metallographic techniques to this problem was possible because of the similarity of distributions of parallel striations developed by etching polished surfaces to distributions of transformation twins which are positively identified in thin films by transmission electron microscopy. The surface striations frequently are not well-defined, and could also be due to, for example, rows of etch pits which are not resolved by the light microscope. This note describes the etching effects revealed by examination of surface replicas of mar-tensite in the electron microscope. The application of a replica technique both extends the observations of fine structure made with the light microscope and allows the results of conventional metallography to be used with more confidence. Samples of an Fe-33 wt pct Ni alloy were used for this study because of the detailed knowledge of the fine structure of martensite which has been developed'-4 for alloys of about this composition. Samples transformed to martensite at -120°C, and transformed samples heated to 340°C to effect a small amount of reversal of martensite to austenite, were examined. Surfaces were first prepared for replication by elec-tropolishing in a chromium oxide-acetic acid electrolyte at a current density of 0.1 amp per sq cm and a temperature of 15°C or a perchloric acid-acetic acid electrolyte at a current density of approximately 2 amps per sq cm and a temperature of 15°C. The polished surfaces were then etched for 4 to 7 sec by immersion in a solution of equal parts HC1, HNO,, and H20. Application of the etchant for this period of time produced discrete attack of certain features without loss of resolution due to overlapping of areas most susceptible to etching. The etched surfaces were replicated by 1) preshadowing with Pt-Pd alloy at an angle of 20 to 30 deg, 2) depositing a thin carbon film, and 3) stripping the film and shadowing material by immersion in a 5 pct nital solution. Two types of etching effects were observed by examination of the surface replicas in the electron microscope: l) continuous striations centered at the bottom of long grooves or the tops of pyramidal elevations on the sample surface, and 2) high densities of fine etch pits. Examples of both types of features are shown in Figs. 1 to 4. The striations are in each case continuous and have the same characteristic configurations as do transformation twins in martensite. Fig. 1 shows that the density of grooves decreases toward the edge of a martensite plate and Fig. 2 shows a region where the striations are of varying length. Similar examples of transformation twin arrangements determined by transmission electron microscopy of thinned foils of martensite have been shown in the literature,'~ and, based on these similarities, the striations and their associated grooves or mounds are considered to be evidence for the presence of transformation twins. The transf~rmation twins in martensite are on the order of l00 A thick, much too fine for resolution by the light microscope. It appears that orientation-dependent etching of the matrix martensite about the twins results in grooves or surface elevations which

Jan 1, 1967

By J. Lindbo, B. Vigeholm

IN transmission electron microscopy, specimen thicknesses quoted are frequently based upon either traditionally familiar values or a few evaluations representing the whole material. Taking aluminum in 100 kv TEM as an example, average and maximum values are widely accepted as being 2000 to 2500 and 6000 to 7OOOÅ, respectively. It is the purpose of this note to revise these figures and to point out the importance of evaluating individual specimens carefully. All evaluations have been based upon slip trace widths and lattice orientations as determined from diffraction patterns. In many cases where two or more slip systems have been operating the geometrical method described by Crocker and Bevis1 has been applied as a check. The foils were usually oriented to within 2 deg from the exact Bragg angle. Kikuchi patterns were used as indications of correct orientations but not applied in the evaluations. The tilt of the foil surface relative to the beam normal may with certain geometrical relations between the tilt axis and the operating slip plane lead to substantial errors.2'3 Where these geometries were inevitable the samples were omitted in the investigations. Various measures were taken in order to overcome ambiguities, e.g., comparison with neighboring grains, tilts, evaluations based upon two or three slip systems,' and comparison with extinction contour evaluations where s = 0 conditions were obtained. Errors caused by misinterpretation of the slip traces on a micrograph are easily avoided by considering the bright-dark sequence on opposite surfaces and by taking into account the tapering of the foil usually leading to a distinguishable divergence of the pair of traces. In the investigations described here the interpretation was further facilitated as the slip trace formation was observed on the microscope screen and sketches taken down. In a few observations slipping was so violent that the distinction of pairs was considered dubious and consequently given up. To assess average values, thickness evaluations carried out in two independent investigations were analyzed: I) 99.998 pct A1 extruded, cold-drawn, and recrys-tallized to grain sizes between 35 and 500 um were deformed in tension at room temperature. In order to determine the dislocation densities as a function of strain,4 specimens prepared by spark machining and electropolishing in a PTFE holder were analyzed in the electron microscope at 100 kv. Thicknesses were evaluated for 569 selected areas. Histogram I in Fig. 1 shows the results, the average thickness being 4900Å. II) Electropolished specimens prepared from 99.9999 pct A1 with magnesium contents from 0.005 to 0.5 pct rolled to foil and annealed were subjected to fission fragment irradiationa2 For volumetric dose and defect concentration determinations thickness evaluations were performed on 123 areas. Histogram II in Fig. 1 shows the thicknesses of these areas averaging 4250Å. Whereas in investigation I no selection related to thickness has been made, some thin as well as thick areas have been omitted from I1 for experimental reasons. This and the application of two different microscopes although of the same type may account for the difference in average thickness. Assuming a mean error of 10 pct for a single evaluation, the error of the average should be negligible. In order to investigate the maximum transmissible foil thickness in aluminum, specimens were prepared from single crystals with (111) and (110) orientations parallel to the beam, and from polycrystalline material. Maximum values of thickness that could be measured were given by the stopping of the dislocations. The visibility often extended far beyond the end of the slip trace, but with no means of knowing the

Jan 1, 1970