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By Goro Shimaoka, Kichizo Niwa

IN the past, the crystalline states of graphite in cast iron have been studied by many investigators. Recently several authors 1-4 have published interesting information on the crystal texture of the individual graphite grain, especially spherulites in nodular cast iron. In regard to the crystal structure of graphite, Lipson and Stokes0 howed by powder X-ray analysis that most of the crystals contain about 14 pct rhombohedra1 structure (ß-form) which differs from the hexagonal structure (a-form) in the sequence of layer stacking. Hoerni6 onfirmed the existence of the ß-form in a single crystal with electron diffraction by Kossel-Moellenstedt's method. Furthermore, Hoerni and Weigle7 found extra reflections in electron diffraction patterns, which are given by a unit cell twice as large as the usual one in the basal plane. Recently, Lukeshs observed graphite twinning and satellite reflections in his X-ray work and considered them as evidence for the existence of an orthorhombic superstructure. Owen and Street" and Matuyama" studied the structures of graphite crystals in several types of cast iron, using the X-ray powder method, and they showed that the graphite crystal contains a certain amount of the ß-form, an amount which varies with the sources of the cast iron used. The present study was made in order to secure structural information on graphitization in cast iron. Electron diffraction studies on the structure of single graphite flakes segregated from molten carbon or silicon-rich iron at 1200" to 1500°C are reported. Experimental Honkeiko pig iron (4.05 pct C, 1.59 pct Si, and 0.65 pct Mn) was used as the solvent of carbon or silicon. The pig iron was melted in an open furnace and a small quantity of metallic silicon was added to the melt at 1300°C. The melt was heated to 150O°C, and then retort black carbon or metallic silicon was added little by little. The components added to the bath contained approximately 5.0 pct C and 2.0 pct Si in the carbon-rich material, and 3.8 pct C and 5.4 pct Si in the silicon-rich iron. These two types were held at 1500°C and then cooled without graphitizing by cutting the heat sup-

Jan 1, 1958

By Frank A. Wardlaw

My subject covers the effect that recent metallurgy has had on operations at the Utah-Delaware mine. This mine is the old Highland Boy mine of Bingham Canyon, Utah, one that has now been in operation for about 30 years. It was first operated by Messrs. Weir and Newhouse as a gold mine, under direction of the Highland Boy Gold Mining Co. The ore was oxidized gold ore and it was treated on the property in a cyanida-tion plant. During the process of development, sulfide ore was found assaying about 5 per cent. copper. It proved to be the discovery of what is yet the largest sulfide copper orebody in the State. The first shipment was made in December, 1896. A smelter was built in Salt Lake Valley to treat this ore and not long after the property was sold to the Utah Consolidated Mining Co. From 1900 to 1924, the mine was a large producer of direct-smelting ore which averaged for many years 4.5 per cent. copper, then later dropped to 2 per cent. copper. During the years 1912 to 1920, direet-smelting lead ore was also mined. In 1918 and 1919 ore developments at depth showed a decided increase in silica content and a porphyry sill so closely associated with the ore that it was impossible to mine the ore clean and it was found necessary to build a copper flotation concentrator at Tooele. The mill had a capacity of 1000 tons a day and made a recovery of 90 per cent., and would have been responsible for a continuance of profitable operations had it not been for a slump in the copper market and the necessary high cost of mining ore on the lower levels. Results of Selective Flotation In 1924 the mine was on the point of a shutadown which had all the earmarks of being permanent; it was being operated at a heavy loss and preparations were made to pull the pumps and salvage the machinery. The plant at Tooele was remodelled for selective flotation by the International Smelting Co. in order to treat custom ores, and incidentally to clean up a possible 10,000 tons of lead-zinc ore which it was thought possible to get in the Utah-Delaware before shutting the mine down. Results were so encouraging that an effort was made to develop more lead-

Jan 1, 1928

US 4,141,854-Method of resolving water-in-oil emulsions from the organic solvent extraction of uranium from an aqueous ore leach solution The emulsion is treated at optimum temperature with a water-soluble acrylamide copolymer which contains 5-50% by weight of a lower alkyl substituted tertiary aminoethyl methacrylate or quaternary ammonium salts thereof The emulsion is broken, enabling recovery and reuse of the organic portion of the emulsion A M Pavilcius and M A Latko, assigned to Nalco Chemical Co Feb. 27, 1979 3 pp (252-301 1W) Filed: 12-14-77 (860,542). US 4,142,952-In the recovery of copper from an ore leach solution, the solution is contacted with a water-immiscible organic solvent containing 5 to 20 g/L of o-hydroxyaryloxime and 2 to 20 times the weight of the o-hydroxyaryloxime of nonylphenol The loaded solvent phase is separated from the aqueous phase and stripped with sulfuric acid Copper is recovered rapidly and in high yield from aqueous solutions containing high copper concentrations R F Dalton, as¬signed to Imperial Chemical Industries Ltd Mar 6, 1979 6 pp (204-106) Filed 1-3-77 (756,067). Priority: United King¬dom, 1-30-76 (3788/76), 6-15-76 (24722/76), and 10-21-76 (43711/76). Same- British 1,549,615, dated Aug. 1, 1979 US 4,148,631-In the recovery of nickel and cobalt from a mixed sulfate ore leach solution, both metals are extracted by means of a cationic extractant, the loaded extractant treated with an aqueous chloride or thiocyanate solution to back extract the cobalt, and the cobalt then recovered by solvent extraction or ion exchange with an anionic extractant Recovery is effected in a relatively few extraction steps. F Babjak, V A Ettel, and K. R Dymock, assigned to Interna¬tional Nickel Co , Inc, Apr. 10, 1979 6 pp (75-101 BE) Filed¬7-27-78 (928,401). Priority- Canada, 12-28-77 (293,967) US 4,148,813-An improved extractant for use in the recov¬ery of nickel and cobalt from an ore leach solution comprises a water immiscible organic solvent system containing solubilized mercaptide ions, e g , dodecanethiol. Cobalt and nickel mercaptides solvated in the organic phase are easily stripped in the presence of carbon monoxide and an aqueous alkaline solution A. S. Rappas and J. P. Pemsler, assigned to Ken¬necott Copp

Jan 1, 1980

By P. Greenfield, P. A. Beck

RECENT work by J. Darby, Jr. in this laboratory has shown that the reported vanadium-rich limit of the s phase in the Co-V system at 1200°C is in error. The appearance of a second phase in s actually is restricted to alloys containing over 68 atomic pct V. The error in the original value is due apparently to a reaction that takes place along the numerous cracks in the s specimens between the alloy and the impurities present in the He + 8 pct H atmosphere in the annealing furnace. Such a reaction and the consequent appearance of a second phase can be suppressed if the alloys are sealed under vacuum in Vycor tubing. The new value of 68 atomic pct V for the vana-dium-rich limit of the s phase in the Co-V system effects slightly the s compositions calculated from average values of N, and N,. for various s phases. The standard deviation between experimental mean compositions and those calculated from the assumption that s is characterized by a constant number of 3d + 4s electrons per atom (N,), is slightly reduced from 9.1 to 8.8 pct. The maximum divergence for the V-Mn s phase is reduced from 15.5 to 14 atomic pct. The standard deviation calculated from constant electron vacancy numbers given by N.. = 4.66 (Mo + Cr + V) + 3.2 (Mn) + 2.2(Fe) + 1.71(Co) + 1.6(Ni) is now greatly reduced, as the maximum divergence for this correlation previously occurred in the V-Co system. This maximum divergence is reduced from 7.6 to 2.3 pct, and the standard deviation for all s- phases is reduced from 4.1 to only 2.9 pct. The correlation for electron vacancy numbers given by N. 5.66 (V when with Ni or Co) + 4.88 (V when with Mn or Fe) + 4.66 (Cr + Mn) + 3.3 (Mn) + 2.66 (Fe) + 1.71 (Co) + 0.61 (Ni) is made slightly worse, and the standard deviation increases from 2.8 to 3.9 pct. These changes, however, do not affect the conclusions of the paper.' The deviation between calculated and experimental s compositions is much less for either one of the electron vacancy correlations than for the correlation with the number of 3d + 4s electrons.

Jan 1, 1955

Records of coal in Colorado begin only a few years before the Civil War. In 1859 Macomb reported beds of lignite on both sides of Galisteo Creek, and in the foothills of the Placer Mountains, a place where an outburst and overflow-of trap had changed the lignite into bright, hard anthracite.1 The Union Pacific Railroad sent Joseph T. Hodge to investigate the coal deposits in the Rocky Mountains, close to the projected line, in the fall of 1863. He was told of coal on South Boulder and Rock Creeks, and that somewhere on Lodge Pole Creek it was being worked for supplying fuel for stage stations; a bed was also reported seven miles north of the stage road between Laporte and Latham. It was only in the vicinity of Denver that coal mines were being worked to any extent; these openings were on Coal Creek about 22 miles north of the town, said to have been opened in. 1860. The coal was used by the smiths with ,difficulty and slacked badly on exposure., Some coke was made from one of the seams, the coke being preferred to the raw coal by smiths. Another district was opened along South Boulder Creek, about two and a half miles from the base of the Rocky Mountains, two mines being worked to supply the Denver market.2 Hayden reported a large bed of coal at Golden in 1861 and of having seen a similar one in 1862 about 65 miles east of Pikes Peak, and in 1866, he saw large beds on Rock Creek 16 to 19 miles from Golden. In 1867 he saw the Belmont or Marshall's mines opened in 1863 on South Boulder Creek, which he said was the finest exhibition of coal in the state. The next one was the Murphy mine, on Ralston Creek, five miles north of Golden. A mine was also being worked near Canon City at that time.3 The coal at Golden was being worked in 1864.4 In 1867 the coal mined at Golden was being used in a firebrick' works. At Canon City and other places on the waters of Arkansas River, coal was being mined for use in the valley towns, bringing $5.00 per ton at the mines.5

Jan 1, 1942

By J. J. Frawley, W. J. Childs

PREVIOUS studies have shown that if a supercooled liquid metal was perturbed by vibration the probability of nucleation is is During a recent investi- gation to determine quantitatively the amount of energy needed to cause nucleation in a given supercooled liquid specimen, it was found that at low-energy values in the megacycle range, below the threshold energy value for cavitation, the amount of dynamic supercooling was greater than the amount of static supercooling. That is, if a specimen had a given amount of thermal supercooling under static conditions, its thermal supercooling could be increased by the addition of low-energy sound waves. The material used in this investigation was high-purity bismuth. This material was chosen because of its low melting point and the high degree of supercooling which could be easily obtained. The sound gener- ator employed in this work was a commercially built Sperry ultrasonic testing unit. This unit was equipped with a barium titanate crystal as a piezoelectric transducer. These sound waves were transmitted to the supercooled melt by a Pyrex rod, as shown in Fig. 1. The transducer was coupled to this Pyrex rod wave carrier by motor oil. The Pyrex wave carrier was approximately 1.5 ft long to prevent damage to the transducer by heat. The diameter of the Pyrex wave carrier appears to be critical. In the initial tests a wave carrier of 0.5 in. in diam was employed. However, the sound waves had no effect on the amount of dynamic supercooling. When the diameter of the wave carrier was increased to approximately the inside diameter of the Pyrex crucible, the sound waves were more effective. Approximately 200 g of metal was melted under a stannous chloride flux in a 30-ml beaker by induction heating. The temperature was recorded by a Pyrex-encapsulated chromel-alumel thermocoule which was placed in the beaker after the bismuth melted. The Pyrex wave carrier was immersed slightly below the surface of the liquid bismuth and the specimen was reheated to about 500°C. It was observed that the amount of supercooling depends on the amount of superheating the specimen receives; therefore, for meaningful results the amount of superheating was the same for all heating cycles. The specimen was allowed to cool in air and the change in temperature was continuously monitored with a potentiometric strip-chart recorder.

Jan 1, 1969

By L. F. Rooney

In June 1964 the Indiana Geological Survey discovered gypsum beds more than 10 ft thick in rocks of Devonian age in La Porte County, Ind. Although the extension of the Michigan Basin evaporites into northern Indiana has been recognized for some time, the gypsum beds have been regarded as either too thin or too deep for exploitation. Current Survey research, however, indicates that exploration by industry might find commercial deposits of gypsum less than 50 miles from Chicago. In four cores taken by the Survey within 1 sq mile in La Porte County, the maximum thickness of inter-bedded gypsum and anhydrite is 35.8 ft. Both gypsum and anhydrite beds contain irregular masses of limestone and dolomite that average a few inches in cross section and total about 20% of the rock by weight. The maximum thickness of gypsum in one minable unit verified by core is 12.5 ft, and its purity is 81.3%. Chloride content of the gypsum beds is less than 0.005%. Depth to the gypsum in La Porte County is 330 to 500 ft, about the same depth as the gypsum being mined in Martin County, Ind. In June 1964 the Indiana Geological Survey discovered gypsum deposits of probable commercial thickness near La Porte, Ind. (Fig. 1). This article presents preliminary data on the distribution, thickness, depth and chemical composition of the gypsum, the possible causes of gypsification, and economic considerations of immediate interest to industry. Because of the preliminary nature of the work, only a few geologic relationships concerning the genesis of the deposits will be mentioned. DEFINITIONS The following terms used throughout this article have been restricted to the following definitions: evaporites: anyydrite (CaSO4) or gypsum (CaSO4 . 2H2O). minable evaporites: any evaporite unit which may contain more than 80% evaporites, which is more than 10 ft thick, and which in places may be completely gypsified. PREVIOUS WORK The presence of gypsum and anhydrite in the Devonian rocks of northern Indiana has been recognized for at least 70 years1-4 and can be inferred from a number of reports on the geology of Michigan. For example, in a cross section from southwestern to central Michigan, Ells5 indicated the presence of

Jan 1, 1965

By completing a double-track railroad cut-off, involving a large volume of cut and fill, in addition to a half-mile bridge spanning an important French river, engineers in the zone of the Services of Supply have opened up a route by means of which hours of valuable time are being saved in transporting men and materials to combat areas. Its most valuable feature is that it provides a means for by-passing a certain city where several, French railroad lines converge and where, consequently, congestion of traffic has been responsible for delayed train movements. To avoid a double-track turnout, which would have involved a cross-over cutting one of the French tracks, the two track connections of the cut-off are taken off from opposite sides of the French right-of-way. This involved running one of the new lines of the cut-off out from the main line track on a fill to a point where it could be brought back and over the French track on a steel girder bridge. Beyond this bridge the two tracks of the cut-off converge and straighten out in the standard type of double-track construction. The new cut-off is about 5 3/4 mi. (9 km.) long and has required 160,000 cu. yd. of cut (122,329 cu. m.) and 414,000 cu. yd. (316,527 cu. m.) of fill. In the biggest continuous fill a-yardage of 180,000 has been placed; the road-bed in this section-being-about 40-ft. (12 m.) above the original ground surface. The bridge portion of the cut-off, 2190 ft. (667.5 in.) long, is made up of ninety-nine 14-ft. (4.3 m.) timber spans and sixteen 50-ft. (15.3 m.) steel girder spans. This is the longest bridge which engineers of the American Expeditionary Forces have built in France. The timber spans are supported by pile trestle bents, while the longer steel girders rest on clusters of 43 piles. Two pile drivers of the steam-hammer type worked from each -end of the bridge toward the center of the river, while a drop hammer worked westward from the shore end. In this structure nearly two thousand piles 50 ft. or so in length had to be driven.

Jan 12, 1918

The Library belonging to the Institute is now administered as part of that of the United Engineering Society, the members of the Library Committee representing the Institute on the Library Board of the United Engineering Society. The main collection now consists of 115,900 books, 3680 pamphlets, 5811 maps, and 4402 searches, making a total of 129,793, a net gain of 7701 within the year. There is in addition a lending collection of 1004 volumes and one of duplicates amounting to 11,310. The library grows steadily both by gift and purchase. The cataloging is now substantially current covering 124,100 items represented by 362,145 cards. There are many rare and notable books, especially those relating to early engineering. It is truly a great treasure house of knowledge. While no severe effort is made to record all visitors the books showed 23,470 to have used the Library in 1928. In addition 5102 telephone requests for information were answered, 202 searches and 196 translations made and 34,964 photo prints furnished. The service department is maintained by small fees which cover the cost. The total amount appropriated for operating expense for the year was $46,300, of which $8,240.02 was furnished by the Institute, $5,399.45 being derived as income from the Douglas Library Fund and the remainder from current receipts. Within the year a slight change was made in the method of meeting the expenses of the Library, a flat charge of $5,000 per year being made against each of the four Founder Societies and this being supplemented by a surcharge based upon membership. The effect of this has been for the present to decrease slightly the amount that the Institute would otherwise need to pay. Placing in one collection all the books of the four societies greatly increases the number of books accessible to the members of each and opening the Library to the public is an important factor in keeping the tax exemption privilege enjoyed for the building. The Director and Staff of the Library make every effort not only to accommodate those who come in person to consult the collection but members resident elsewhere who communicate by letter or wire. The facilities of the Library are truly available to all.

Jan 1, 1929

The State Mining Experiment Station, Missouri School of Mines and Metallurgy, Rolla, Mo Charles H. Fulton, Director of the School of Mines Martin H. Thornberry, Director of the Mining Experiment Station. From the State Mining Experiment Station are issued all the general and technical bulletins of the School of Mines The latest bulletin containing a complete list of publications will be sent upon application to the Director of the Station Residents of the state may obtain bulletins as issued without charge, or may ask to be placed on the mailing list. Nonresidents should write to the Director for further information concerning specific bulletins. From the long list of bulletins the following have been care¬fully selected as being most likely to interest the geologist and the mining engineer. Vol 8, No. 1 (1916), Bibliography of concentrating ores by flotation, by J Cunningham, vol 1, No 3 (1912), Some apparatus and methods for demonstrating rock drilling and the loading of drill holes in tunneling, by L E Young, vol 2, No 1 (1915), Comparative tests of piston drill bits, by C R Forbes and L M Cummings; vol 2, No 3 (1916), Cupellation losses in assaying, by H. T Mann and C. Y Clayton; vol 4, No 1 (1917), The hydrometallurgy and electrolytic precipitation of zinc, by F D. James; vol 4, No 2 (1917), The effect of additional agents in flotation, pt 1, by M. H. Thornberry and H T. Mann, vol 5, No 1 (1919), The carbonization of Missouri cannel coals, by H L. Dunlap, K. K. Kershner and V. X Smiley. Vol 5, No. 4 (1921), Coal mining methods in Missouri, by W W Weigel, vol 6, No 1 (1921), The problem of the St Peter sand¬stone, by C L Dake, 50 cents, vol 6, No. 2 (1922), Bibliography on the electrothermic metallurgy of zinc, by B M. O'Harra, vol 6, No. 4 (1923), Experiments on the distillation of zinc from complex zinc-lead-silver ores, by B M. O'Harra and E S. Wheeler, vol 7, No 3 (1924), Underground loading devices, by C. E. van Barneveld, 81; vol 7, No. 4 (1924), Briquetting of zinc ores, by B. M. O'Harra; vol. 8, No 2 (1925), A treatise of Missouri clays, by M. H. Thornberry.

Jan 1, 1933

By John Henry Harden

THIS shaft, located in the northern anthracite coal-field about 2300 feet southwest from the court-house at Wilkes-Barre, in the County of Luzerne, Pa., is the property of the Lehigh & Wilkes¬Barre Coal Company. The sinking and cribbing to the solid rock (see isometrical view on Plate IX) was conducted by Mr. W. W. Kenrick. Dimensions of the earthwork to the foundation of the cribbing, 51' 1/2" long, 17' 4" wide, 31' deep. Total amount of excavation in cubic yards, 998.5. Dimensions within the permanent cribbing, 45' 4" long, 11' 16" wide, 31' deep, divided into six parts by buttons 8" x 12", each division, 7' x 11’ 16". Permanent cribbing 12" x 12"; temporary cribbing 8" x 10"; backing, 3" thick ; clay puddle to ex¬clude surface water, 12" thick; conductors, 8" x 5"; lining, 1" thick from top to bottom of the shaft. In the latter part of the year 1871, Mr. H. Murray & Son contracted with the company for the continuation of the work at the rate of four hundred dollars per yard in depth, to a point 100 feet below the Hillman seam of coal ; for the succeeding 100 feet the price to be increased twenty-five dollars per yard, and so on until the bottom rock of the Baltimore seam of coal was found. The size of the shaft within the cribbing timbers is 45 feet 4 inches by 11 feet 6 inches, having six divisions of equal dimensions, 7 feet by 11 feet 6 inches, giving room for what is known as the" standard diamond" car, whose capacity when level full is 100 cubic feet, but when loaded by the miner 4 inches above the top contains 112 cubic feet.* Two divisions of this shaft are intended for hoisting coal from the Hillman seam, two from the Baltimore seam, one for ventilation, and one for pumps. The works were planned for two pairs of direct-acting, high-pres¬sure engines, twenty-four boilers, and for an estimated output of 2500 tons of coal per day from the two seams. * Size of the "standard diamond" car, 8' 10” x 4' 3" x 2’ 8” = 100.1.4; loaded 4 inches above the top, 8' 10” x 4’ 3” x 3’ “0"= 112.7.6.

Jan 1, 1877

By Robert M. Betts

The Cornucopia district is situated in northeastern Oregon 25 miles from the Snake River branch of the Oregon Short Line R.R. and 75 miles northeast of Baker City, in the Wallowa Mountains. The formation is principally granodiorite, which has intruded much older rocks locally known as greenstone, and which are probably altered schists. In the upper horizons of the veins, greenstone is found as inclusions in the granitic mass. Both of these formations have been cut by numerous basalt, aplite, and porphyry dikes. Veins of the district are the result of faulting and the consequent crushing of the wall rock. The ore has been deposited irregularly along these faults and formed a lenticular type of vein. The ore varies in width from a few inches to 20 ft.; the average stoping width is about 5 ft. As the basaltic dikes are subsequent to the ore deposition, they are at times a hindrance in development and mining operations; on the other hand, a dike which has followed a vein as a line of least resistance often serves as a good mall in place of the crushed, rather loose granite. The veins generally strike northeast-southwest and dip about 35" to the west. Orebodies are from 100 to 300 ft. in length and about the same in height. The lenses are irregular; inclusions of wall rock are common in the ore and are a factor in reducing the grade. The ores are quartz, carrying some free gold near the surface, but the metals for the most part are in iron sulfides, sometimes associated with chalcopyrite. The gold and silver are in a mechanical combination with the iron, which requires find grinding to liberate them. The ratio of silver to gold is 5 to 1, by weight. Development The Cornucopia Mines Co. owns, and operated until 1920, two mines and two mills of 100 tons capacity each. The sustained high costs and labor shortage, however, necessitated the abandoning of the Union mine, the oldest in the district. Two crosscut tunnels were then started, first, to cut the Last Chance vein at a much lower horizon and, second, to prospect two parallel veins. The ore from the Last Chance vein will go to the old Union mill and the ore from the new veins to the Last Chance mill.

Jan 1, 1925

By Harold R. Bradford

EXPANSION initiated during and after the war has placed industrial plants in new areas and increased reduction and manufacturing facilities in communities already established. With added expansion interest has grown in possible area contamination from waste products. Evolved flue waste contains many chemical contaminants that may or may not cause concern; however, atmospheric pollution has always been a problem to industrial communities. For some time effects attributed to small quantities of compounds of fluorine in various waste gases have been studied by industrial, medical, agricultural, and associated interests.1'2 Aside from an article by Churchill, Rowley, and Martin in 1948," little has been published on the subject of fluorine in coal except by foreign investigators. The first indication of fluorine compounds in coal was noted in England in 1934 by R. Lessing,4,5 who found that the presence of fluorine in Midland and West County coals was definitely established by etching of glass and by severe corrosion of porcelain fillings in a gas works scrubber. Etching of glass in a direct contact annealing kiln initiated research, and in 1944 four papers were published by H. E. Crossley,6-9 giving results of investigations of fluorine in coal of England by the Fuel Research Board, Department of Scientific and Industrial Research. These investigations studied methods of determining fluorine, the quantities present in various coal deposits, the geographical distribution of fluorine in British coals, occurrence of fluorine in minerals associated with coal, amounts of fluorine compared to other constituents of coal, the nature of fluorine compounds, and industrial significance of fluorine in coal. It was shown that British coals contain from 5 to 200 ppm of fluorine, which is probably present as fluorapatite [Ca10F2(PO4)6], often written as [3Ca3P2O8.CaF2]. The fluorapatite is intimately associated with shale in some coals and can often be separated from these coals along with the shales. H. E. Crossley8 also reported no correlation between the amounts of chlorine, sulfur, or ash and the amount of fluorine in different coals. He found, however, a relationship between the content of fluorine and phosporus in many British coals. Thus it should be possible to anticipate likely fluorine-rich coals from existing data giving phosphorus content. Behavior of the fluorine compounds of coal was compared with that of 12 fluoride-phosphate minerals in sink-float separations and solvent ex-

Jan 1, 1958

By A. H. Geisler, J. H. Keeler

Preferred orientations in rolled and annealed titanium sheets were determined by the Geiger counter spectrometer X-ray diffraction technique. Five annealing textures dependent upon the temperature range of annealing were found, and in order of increasing annealing temperature pendent upon the temperature range are: 1—a deformation like texture, 2—a rotated inorder a-recrystallization temperature texture, 3-a retained u-recrysraIlization texture, on annealing at lower temperatures of the ß-region, 4—a transformation texture based on recrystallized a and predicted by the Burgers' relationship, and 5—a ,ß-cube texture. These results are examined in terms of current theories of recrystallization textures. UMEROUS investigators have described the tex- ture obtained by cold rolling the hexagonal metals, titanium, zirconium, and beryllium, which have c/a ratios less than that of ideal packing, 1.633. The basal planes are rotated out of the rolling plane, about the rolling direction, so that the basal poles are tilted toward the transverse direction as shown schematically in Fig. la. In all instances but one,' it was also reported that the [1010] direction was parallel to the rolling direction (see Fig. lb). Hot rolling has been reported as causing a similar tilt of the basal poles in the transverse direction (see Fig. la) and causing the [1010] direction also to be parallel to the rolling direction as shown schematically in Fig. lb. Annealing after deformation does not appreciably change the tilt of the basal poles in the transverse direction." Beryllium2-7 continues to have the [1010] direction in the rolling direction after annealing, and similar observations for titanium and zirconium' . have been reported for annealing at fairly low temperatures, again as in Fig. lb. At higher annealing temperatures, however, the recrystallized grains of titanium" and zirconium have an orientation such that the [1120] direction is approximately in the rolling direction, although the basal poles are still inclined in the transverse direction. Figs. la and lc show the resulting orientations schematically. This change in orientation has been described as a nominally ±30° rotation of the hexagonal crystallites about the basal poles of the cold rolled texture and is apparent from the results which are summarized in Table I for investigations with the X-ray diffraction technique employing film. The angles y, , and ß are indicated in Fig. 2 which represents the stereographic projection of (1070) poles for the mean orientation of a pole figure. Texture determinations for titanium using the Geiger counter spectrometer have provided similar results except that in some instances additional components of the texture were proposed, as shown by the summary of data in the upper half of Table 11. On the other hand, the spectrometer technique, when applied to zirconium,* has revealed a splitting Recently completed studies of the textures of annealed zirconium", show zirconium to possess textures very similar to those reported here for titanium. Therefore, much of this discussion will include zirconium by virtue of its close similarity to titanium in pref erred orientations. of the intense areas of the pole figure for samples annealed at 600°C. This splitting could be described by a 7" rotation of the tilt axis about the normal to the rolling plane. Such a splitting for the annealed texture relative to the cold rolled texture was not observed in other determinations for either zirconium or titanium using the less sensitive film X-ray methoe and makes the relationship between the two types of texture more complex than the simple rotation about the (0001) pole based on film work. The more precise investigations on zirconium permit the descriptions in the lower part of Table 11, which show that the texture depends quantitatively on the temperature of annealing. When zirconium is annealed at temperatures up to 400°C, the texture is similar to the cold rolled texture, while annealing in the range 500" to 900°C produces a texture which is only approximately described as [11%] in the rolling direction. More precisely described results for zirconium show that the two types of splitting ( 1—about an axis in the rolling plane through an angle given in the second column in Table II and 2—about the normal to the rolling plane through an angle given in the third column of Table 11) depend on annealing temperature. The [1120 is the rolling direction only when the annealing temperature is in the vicinity of 900°C

Jan 1, 1957

By R. C. Ku, A. J. McEvily, T. L. Johnston

The microplastic response of a series ofas-quenched Fe-Ni-C martensites has been measured at 77°K. At strains less than JO'3 the flow stress is governed primarily by the transformation-induced dislocation structure of the martensite. Only at strains in excess of 10-3 is the influence of carbon manifested in the flow stress. At these macroscopic strains, typically 10-2, the solid-solution hardening is proportional to (wt pct C)1/3, and, in an alloy containing 0.39 wt pct C, amounts to 50 pct of the flow stress. THE technological significance of high-strength ferrous martensite has stimulated many investigations of its structure and properties. Although our knowledge of the characteristics of martensite has increased immensely, especially with the advent of high-resolution techniques, an understanding of the basic strengthening mechanism still remains elusive. The purpose of the present paper is to consider certain aspects of micro-plastic behavior of Fe-Ni-C martensite which we feel can help to resolve this important problem. Such alloys are particularly suitable for experimental investigation because their compositions can be adjusted to reduce the M, to a temperature low enough essentially to eliminate the diffusion of carbon in the freshly formed martensite.1 The mechanical properties in this condition are of interest inasmuch as they reflect a state that is free of the important but complicating influence of precipitation processes. In this virgin martensite the carbon is distributed as it was inherited from the parent austenite; i.e., it is present interstitially, and gives rise to tetragonality through strain-induced ordering.' In order to determine the source of strength of such alloys, Winchell and Cohen1 investigated the low-temperature macroscopic stress-strain behavior of a series of virgin martensites of increasing carbon content but of common M, temperature (-35°C). They found that the flow stress increased rapidly with carbon content up to 0.4 wt pct; beyond this point the flow stress increased at a much slower rate. It was concluded that martensite is inherently strong. To account quantitatively for the strength of virgin or as- quenched martensite in terms of the role of carbon, Winchell and cohen3 suggested that the carbon atoms, trapped in their original positions by the diffusionless martensite transformation, interfere with dislocation motion according to a model akin to that of Mott and Nabarro. 4 In this treatment, individual carbon atoms are considered to constitute centers of elastic strain and thereby generate an average stress resisting the motion of dislocations throughout the lattice. The additional stress necessary to move dislocations, over and above that necessary for motion in a carbon-free martensite, is given by where L is an effective length of dislocation capable of motion. L was assumed to be limited to the spacing between the twins that are an essential structural element of Fe-Ni-C martensites. They assumtd the spacing to be invariant and of the order of 100A. However, recent work5 has shown that L is variable and can be in excess of 1000Å, so that the assignment of an appropriate value of L is not straightforward. In contrast to the above conclusion that there is an intrinsically high resistance to plastic flow, it has been suggested by Polakowski6 that freshly quenched martensite is in fact "soft" in the sense that dislocations are initially free to move upon application of stress. The high indentation hardness and macroscopic yield stress of ferrous martensites are then a consequence of rapid strain hardening that depends upon carbon in solution. Consistent with this point of view are the results of Beau lieu and Dubé who measured the rate of recovery of internal friction as a function of aging (tempering) temperature in a freshly quenched steel containing 0.90 wt pct C, 0.37 wt pct Mn, 0.1 wt pct Cr, and 0.07 wt pct Ni. The kinetics were clearly consistent with the idea that many dislocations are unpinned in the as-quenched state and that during aging they become progressively pinned by carbon at a rate controlled by carbon diffusion in the body-centered martensite lattice. In order to provide a basis upon which to distinguish between the "hard" and "soft" interpretations indicated above, we have made studies of the initial stages of plastic deformation in Fe-Ni-C martensites similar to those'used by Winchell and Cohen. It will be shown that the results support the contention that dislocation segments in as-quenched material are indeed

Jan 1, 1967

By V. B. Kurfman

Grain refinement of Mg-Al melts by carbonaceous additions has been attributed to nucleation by aluminum carbide. The effects of process and alloy variables are interpreted and predicted in terms of the dispersion and chemistry of this phase. The grain coarsening action of Be, Zr, Ti, R.E., chlorination, temperature extremes, and prolonged holding times is described. Measures necessary to insure an adequate dispersion of the catalyst are discussed. CARBON inoculation treatments have become fairly well known and used for grain refinement of magnesium alloys containing Al. Although there is general agreement that a nucleation process occurs, the process is not understood and the inoculants are used in a rather empirical fashion. The treatment is applied to the class of alloys containing 3 to 10 pct Al, i.e., AZ31A to AM100A. Typical methods involve melting, alloying, and adjusting the temperature to 1400° to 1450°F. Then 0.01 to 0.5 pct C as CaC2, C6C16, or lampblack is added by any convenient means, and the melt poured within 10 to 30 min. Investigators generally have been impressed by an assumed similarity of this refinement process to superheat grain refinement, which depends on heating approximately the same alloys to a temperature in the range of 1550" to 1650°F, then pouring promptly after the melt is cooled to the pouring temperature. Various predictions have been made that carbon refinement would replace superheating in commercial practice due to reduced process costs, but this replacement has not fully taken place because of production difficulties and conflicting observations. Davis, Eastwood, and DeHaven1 agree with Nelson2 and wood3 in suggesting that an excess of inoculant may be harmful. Wood however says that overtreat-ment is not a problem in production use of hexa-chlorobenzene inoculation, and Hultgren and Mitchell4 claim no evidence of harm from excess additions. Various grain coarsening reactions are known to occur, including the possibility of overtreatment mentioned above. Trace amounts of Be,2 Zr, and Ti may prevent refinement by either a carbon treatment or a superheat. Occasionally treatment with cl25 may cause coarsening, although the Battelle refinement process' uses a CC14-C12 blend. Grain coarsening also tends to occur on holding at temperatures below 1350°to 1400°F, especially after a superheat treatment, and for this reason Nelson2 stresses the desirability of a refinement method useful at lower temperatures for open pot melting practice. Since a carbon treatment can be made to work at temperatures below 1400°F, it seems desirable to investigate the mechanism of the refinement and the mechanisms of the coarsening reactions in order to establish control conditions for use in commercial production. The identity of the nucleating phase must first be established and then the factors affecting its chemistry and physical dispersion must be determined. THE IDENTITY OF THE NUCLEATING PHASE Davis, Eastwood, and DeHaven suggested that the nucleating phase in this system is Al4c3,1 but Mahoney, Tarr, and LeGrand8 disagree, largely because they found no evidence of the compound in alloys after carbon treatment and because there is no indication that aluminum carbide should be unstable over the temperature range used in the superheat treatment. This latter objection is based on the assumption that both the carbon treatment and the superheat treatment introduce the same nuclei. Electron diffraction studies have been made to identify the nucleating phase. Samples of grain refined A292 have been selectively etched SO that clean surfaces are obtained and so that secondary phases are in relief. Electron diffraction patterns from these surfaces have established that the carbon treatment of A292 introduces into the metal a large number of small, plate-like particles with a structure very similar to Al4C3. In most cases, the plate-like nature of the particles prevented positive identification but in the cases where the identification could be made the particles proved to be AIN A14C3. However, enough variation in lattice constants was observed so that all compositions from pure A14C3 to the 50:50 solid solution A1N.Al4C3 were probably present.14 In A14C3 and especially AlN.Al4C3 the A1 atoms occur in layers within which they have the same hexagonal symmetry and spacing as the Mg atoms in a single basal plane of a magnesium crystal. The solid solution spacing lies between the 3.16 of AIN and the 3.3? for Al4C3, in satisfactory agree-

Jan 1, 1962

By P. K. Koh, H. A. Lewis, H. F. Graff

New data on the distribution of silicon between slag and carbon-saturated iron at 1600Oand 1700OC are presented which, in combination with previously published data, permit the determination of silica activities over a broad range of compositions in the CaO-Al2O3-SiO2 system. The distribution of silicon between graphite-saturated Fe-Si-C alloys and blast furnace-type slags in equilibrium with CO has been described in previous publications.1"3 In this past work the silica-silicon relation was established at temperatures of 1425" to 1'700°C for slags containing up to 20 pct A12O3. This paper presents the results of additional studies at 1600" and 1700° C which extend the silicon distribution data at these temperatures for CaO-A12O3-SiO, slags over a range from zero pct Al2O3 to saturation with Al2O3, or CaO.2Al2O3. The upper limit of SiO2 is set by the occurrence of Sic as a stable phase when the metal contains 23.0 or 23.7 pct Si at 1600" or 1700°C, respectively. The activity of silica over the expanded range is determined directly from the distribution data.3 Recently4-7 other investigators have studied the activities of SiO, and CaO, principally in the binary system, using different methods and obtaining somewhat different results. EXPERIMENTAL STUDY The experimental apparatus and procedure have been fully described in previous publications.1, 3 Six new series of experimental heats have been made, four at 1600° and two at 1700°C. Master slags of several fixed CaO/Al203 ratios were pre-melted in graphite crucibles, and these were used with additions of silica to prepare the initial slag for each experiment. Slag and metal were stirred at 100 rpm and CO was passed through the furnace at 150 cc per min. The initial sample was taken 1 hr after addition of slag at 1600°C or 1/2 hr after addition at 1700°C. The run was normally continued for 8 hr at 1600°C or 7 hr at 1700°C, and the final sample was taken at the end of this period. Changes in Si and SiO2 content indicate the direction of approach to equilibrium, and in a series of runs where the approach is from both sides this permits approximate location of the equilibrium line. Fig. 1 shows the results of such a series of 15 runs at 1600°C for slags of CaO/Al,O3 = 1.50 by weight. Figs. 2 and 3 record other series at 1600°C and Fig. 5 a series at 1700°C with fixed CaO/Al0 ratios. The results of the experiments at 162003°C have been reported in part in a preliminary note.3 In the experiments recorded in Figs. 4 and 6, the slags were saturated with A12O3 (or with CaO.2A12O3 within its field of stability) by suspending a pure alumina tube in the melt during the course of the run. The final slag analyses were used to establish the liquidus boundaries8 in the stability fields of CaO.2Al2O3 and of Al20,. ACTIVITY OF SILICA The free-energy change in the reaction has been calculated by Fulton and chipman2 from recent and trustworthy data including heats of formation, entropies, and heat capacities. The more recent determination by Olette of the high-temperature enthalpy of liquid silicon is in satisfactory agreement with the values used and therefore requires no revision of the result which is expressed in the equation: SiO2 (crist) + 2C (graph) = Si + 2CO(g.) [1] &F° = + 161,500 - 87.4T The standard state for silica is taken as pure cristobalite and that of Si as the pure liquid metal. Since the melts were made under 1 atm of CO and were graphite-saturated, the equilibrium constant for Eq. [I] reduces to K1 = asi /asio2. The value of this constant is 1.77 at 1600°C and 16.2 at 1700°C. Through K1, the activity of silica in the slag is directly related to the activity of silicon in the equilibrium metal.

Jan 1, 1960

By R. G. Aspden

Crystals with an (001) [loo] initial orientation of an iron-base alloy containing 3 pct Si were cold rolled with and without the use of constraints. A major difference in the rolling and annealing textures was observed between crystals rolled with and without constraints. These data show that the contribution of constraints at grain boundaries in a poly crystalline sheet should be considered in applying textural data on single crystals to grains in an aggregate. SILICON-iron alloys with a cube texture have been recently developed and their magnetic characteristics reported.1-4 Of interest in the development of this texture were the textural changes of single crystals accompanying rolling and annealing and the influence of constraints at grain boundaries in an aggregate on the behavior of individual grains. The present study was primarily concerned with the effect of constraints during rolling on the textures of 3 pct Si-Fe crystals initially (001)[100]. Barrett and Levenson5 were among the first to observe an influence of constraints at grain boundaries on the textural changes of individual grains during deformation. They tested Taylor's6 theory of plastic deformation of face-centered-cubic metals in which deformation textures were predicted. About one-third of the grains in poly crystalline aluminum did not rotate as predicted. Grains of the same initial orientation were observed to rotate in different directions under the influence of applied stress and anisotropic flow of neighboring grains. Recently, the various inhomogeneities of flow of crystals in an aggregate have been studied7'8 and reviewed.9-11 Barrett and Levenson" rolled (001) [loo] iron single crystals inserted in close-fitting holes in copper to limit lateral flow and to simulate rolling of grains in an aggregate. Deformation bands were formed after a 90 pct reduction in thickness, and the cold-rolling texture contained two components described by rotating the (001)[100] about 35 deg in both directions around the normal of the rolling plane. No annealing textures were reported. Chen and Maddin13 rolled molybdenum single crystals initially (001) [loo]. The crystals were mounted between two hardened silicon-iron plates and 96 pct reduced in thickness by rolling at a low rate of reduction, about 0.0001 in. per pass. The deformation texture had the mean orientation of (001) [loo], and the azimuthal spread included orientations described by rotating (001) [loo] about 35 deg in both directions about the pole of the rolling plane. The presence of deformation bands were not reported by Chen and Maddin or detected in subsequent work of Ujiiye and Maddin.14 The ideal orientation of the annealing texture was (001) [loo]. Recently, Walter and Hibbard 15 reported on the textures of 3 pct Si-Fe alloy crystals initially near (001) [loo]. Each crystal was in an aggregate cut from a columnar ingot. After 66 pct reduction by rolling, the texture consisted of two symmetrical components which had the orientations described by rotating (001) [loo] about 30 deg in both directions about the pole of the rolling plane. Annealing texture was near (001) [loo]. In the above work, the textures of body-centered-cubic crystals were studied after rolling under the influence of constraints. The deformation textures varied from (001) [loo] to near the (001) [110] type and appeared sensitive to the manner in which the crystals were rolled. No textural data were available on the effect of rolling (001) [loo] crystals with and without constraints. The purpose of the present work was to evaluate the influence of constraints during rolling on the textures of 3 pct Si-Fe crystals initially (001) [loo]. Rolling and annealing textures were studied for a) crystals rolled with no constraints at different rates of reduction, and b) crystals rolled with constraints imposed by neighboring grains and by plates between which a crystal was "sandwiched". PROCEDURES AND EXPERIMENTAL TECHNIQUES Data are presented on four crystals which are representative of several crystals studied. The orientation of each crystal prior to rolling was (001) [loo] as determined by the Laue X-ray back-reflection method," i.e., each crystal had an (001) within 3 deg of the rolling plane and [100] within 3 deg of the rolling direction. These crystals were obtained from two iron-base alloys containing 3 pct Si by weight which were prepared by vacuum melting electrolytic iron and a commercial grade of silicon. Crystals 1, 2, and S-1 were cut from a large single crystal grown from the melt of one alloy by the Bridgman technique17 in an apparatus described by

Jan 1, 1960

By Charles L. Mantell, George Ferment

This investigation determined the jeasibility of current-potential curves as an analytical tool for monitoving manganese electroicinning solutions for metallic impurities. Nine metallic impurities were studied: trickel, cobalt, silver, copper, zinc, molybdenum, catlmiun magnesium, and sodium. The individual effect of each metallic irzplrl,iLy on the standard point-izatiorr was determined for a range of 'concentration. Not all of Ihe impurities affected the polarization curve; correlation between transition current and cotrcetztration of impurity. Molybdenum had an uncorrelated effect on the polarization curie. The effects of binary mixtures of impurities were studied to see if the transition current of the mixture could be predicted. Interactions occurred between impurities which prei'etzted the pvecliction the transition current of tile rrlisLitr.e by additive laws. The polarization curve was shown to be sensitive to metallic impurities which affect the current efficiency of a manganese cell. THE application of current-potential curves in manganese electrowinning is not new but played an important part in the conversion of an inoperative large-scale pilot plant into a continuous comnercial operation.1"" The effects of trace metallic impurities in manganese electrowinning solutions on cathode current-potential curves,5-19 specifically nine impurities (nickel, cobalt, silver, copper, zinc, molybdenum, cadmium, magnesium, and sodium) were studied for a range of concentrations. Cadmium, magnesium, and sodium had no effect. Nickel, cobalt, silver, copper, and zinc yielded a correlation between transition current and concentration of impurity: molybdenum had an uncorrelated effect. Binary mixtures of impurities were studied to de-termine if the transition current could be predicted from the values for the individual constituents. Interactions between impurities prevented the prediction of the transition current of the mixtures by an additive law. The polarization curve was shown to be sensitive to metallic impurities which affected the rurrent efficiency of a manganese cell. The electrowinning of manganese relies upon maintaining a high-purity electrolyte. Purification schemes were developed to remove all of the heavy metals, the magnesium and calcium. Concentration limits have been established for single impurities. With high-purity electrolytes, favorable cell efficiencies are consistently obtained; but with impure solutions there is a reduction in efficiency. With the rapid rise to commercial prominence of electrochemical processes, there has been a lag in developing rapid methods for determining whether an electrolyte is sufficiently pure for efficient electrolysis. The most sensitive test for impurities is the behavior of the electrochemical cell. Impure electrolytes will cause a serious reduction in cell efficiency, and in many cases metal deposition will be prevented or reversed. The effects of impurities are not usually evident until after long periods of electrolysis, resulting in a disruption of the process. A method which could predict the behavior of an electrolyte in terms of cell efficiency prior to reaching the commercial cell is needed. Van Arsdale and Maier," Allmand and Campbell,a1'22 and others attempted to develop an electrochemical process for manganese,"3"29 but all met with some degree of difficulty. Jacobs et a studied the effects of metallic impurities in manganese electrowinning. Plant methods were based on a 2-hr plating in a small electrolytic cell. The final method was based on a 24-hr plating run, performed in a relatively large test cell. Here, current efficiencies were calculated with and without impurities in the electrolyte, and the critical concentration was established as the maximum amount of impurity that the electrolyte could tolerate before there was a serious loss in efficiency. The amount of impurity that could be tolerated decreased as the plating time increased, indicating deposition of the impurity. This test duplicated the conditions of commercial practire, and was sensitive to impurities. Small amounts of impurities significantly affect the hydrogen overvoltage at a metal surface, increasing or decreasing it depending upon the nature of the impurity. ockris established the limit for the onset of poisoning at 10-l moles per liter. The effects of impurities were studied by potential-time curves at a constant current density. The technique did not lend itself to rapid analysis in that several hours were needed to establish stable potential-time curves. Serfass and coworkers3' developed calorimetric and spectrophotometric techniques for analyzing for trace impurities. Our method4'" is based on current-cathode potential curves produced by continuously changing the cell voltage at a programmed rate. Starting with a clean stainless-steel cathode, the cell voltage was initially adjusted to yield zero current: the program was then started and the current was plotted as a function of the cathode potential. Fig. 1 is a typical current-potential curve. In initial region A the hydrogen-evolution reaction predominates and the polarization curve

Jan 1, 1967

By C. J. Guntner, R. P. Reed

A commercial 18Cr-8Ni iron alloy (AISI 304L) was examined in tension at 300°, 76°, 20°, and 4°K. Continuous stress-strain recordings were made, X-ray analyses at periodic stress (strain) intervals were obtained, and the magnetic measurements were taken. From this data the percentage of martensitic products [bcc(a) and hcp (E)] was computed as a function of stress (strain). It was found thatup to 15 pct E phase forms at low temperntures. The amount of E formed increases to a maximum at about 5 pct strain, then decreases. This decrease indicates the additional transformation of E to a'. The total amount of E and a' was suppressed at constant stress (strain) at 4°K as compared to 76°K. It is proposed that the suppression of E and a' is associated with the decreased mobility of extended dislocations at very low temperatures. The yield strength decreased as the temperature was depressed below room temperature and then increased rapidly near 4°K. SOME ferrous alloys which are austenitic (fcc ?) at room temperature appear to be unique in that two martensitic products (hcp e and bcc a') may form on cooling to lower temperatures or on application of mechanical stress. The most common room-temperature austenitic ferrous alloys are 18Cr, 8Ni stainless steels. Most aspects of the spontaneous transformations have been previously described for these steels.' Several previous papers have described special aspects of the stress-induced transformations at low temperatures for the stainless steels, such as the existence of the hcp phase (c) after straining at 76oK,2-7 the morphology after straining using electron microscopy,7 and the decrease in E at higher strains at 76oK.4 However, for a complete representation, one must know the stress-strain characteristics and the dependence of both martensitic products on applied stress and temperature. It is the intention of this paper to provide that documentation. To accomplish this, continuous stress vs strain recordings were made at four temperatures: 300°, 76", 20°, and 4°K for annealed AISI 304L (a commercial 18Cr-8Ni alloy). At periodic stress intervals at each temperature the integrated X-ray line intensity of a selected peak for each phase (y, E, and a') was measured. In addition, photomicrographs of the strained surfaces were taken and magnetic measurements were made. The magnetic readings can be directly converted into percent a'.',e With these measurements the percentage of each phase may be plotted as a function of stress (or strain) and test temperature. It was found that up to 15 pct E phase forms upon stressing the AISI 304L alloy at low temperatures. The E percentage increases abruptly after the alloy yields, but then decreases gradually at higher stresses. The rapid increase in e at 76°K is associated with an "easy-glide" portion of the stress-strain curve. The total amount of a' + .G is suppressed below 76°K at a constant stress or strain. The yield strength decreases down to 76°K but increases rapidly below 20°K. EXPERIMENTAL PROCEDURE Tensile test specimens were cut parallel to the rolling direction from 0.1-in.-thick sheet. Continuous stress vs strain recordings were obtained at each test temperature (300°, 76o, 20°, and 4°K) using equipment and methods described elsewhere.' The specimens which were used in the X-ray analysis were stressed to successive increments of strain at each temperature, analyzed at room temperature, then restressed at the test temperature. This procedure was repeated until approximately ten X-ray analyses had been performed with approximately 1.0 pct strain increments. The specimens had a reduced section 1 in. long, 1.2 in. wide, and 0.1 in. thick. They were electro polished prior to testing and after each strain increment. Table I lists the chemical composition, grain size, and hardness for the alloy which was used. This is the same alloy for which extensive mechanical-property tests3 and morphological studies of the spontaneous transformations' have previously been made. For the low-temperature tests (76o and 4°K) below the Ms temperature the specimens were initially cooled to the test temperature, held for 1/2 hr, then warmed and X-rayed at room temperature. The results are listed in Table 11. From earlier work8 it was known that additional transformation on the second cycle would be considerably less (-0.1 pct

Jan 1, 1964