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By G. E. Burpee

A COMPREHENSIVE study of insoluble residues in the productive Permian limestone in the Hobbs and Eunice fields, Lea County, N. M., has been conducted by Shell Petroleum Corp. engineers {luring the past two years. This study was prompted by the belief that the stratigraphy of the producing formation might be worked out in detail and that some relationship might be established between the permeable oil, gas, and water zones and correlatable lithologic horizons within the productive formation. As a result of the study, correlations have been established which have proved of great value to both an orderly development and corrective program.

Jan 1, 1935

By W. A. Backofen, D. L. Holt

Push-pull fatigue tests have been carried out at 4.2°K, 77oK, and room temperature on two poly crystalline materials of widely different stacking-fault energy (?): pure copper (? - 70 ergs per sq cm) and the Cu-8 wt pct A1 alloy (? - 2.8 ergs per sq cm). Constant stress-amplilude was imposed and measurement was made of the plastic-strain amplitude (ep) at saturation. Lives extended from 104 to 106 cycles. Designating lives at the various temperatures by NRT, N77, and N4.2. the ratios N77/NNT and N4.2/N77 ranged from 3.5 to 18 under the condition of common Ep . Metallo-graphic examination revealed different crack morphology in Cu-8 Al fatigued at room temperature, and at 77" and 4.2oK. At room temperature, cracks lay in or near grain and lain boundavies; at 77o and 4.2oK. cvacks were transcrystalline. Tests on single crystals of Cu-8 A1 showed that such a change in the cracking mode in polycrystallitle material accounted for a factor of- about 3.25 in N77/NRT . The longer life at lower tewperatztre (conslant cp) has heels attributed to two deuelopinents: a reduced production of the dislocation tangles and subgrain boundaries which serve as paths of rapid cracking, and suppression of oxygen chetni-sorption at the crack tip It was concluded that in both materials the luller accounted for an extension of the life at 4.2oK beyond that at room temperature by a factor of 15. XV ECENT experiments on the fatigue of Cu-A1 alloys in the so-called high-cycle range (greater than lo4 cycles) have emphasized the importance of stacking-fault energy (y) as a quantity affecting crack propagation rate and fatigue life.1,2 It was found in comparisons at essentially fixed plastic-strain amplitude that crack growth rate decreased by a factor of about 5 over the composition range from copper (? - 70 ergs per sq cm) to Cu-8 wt pct Al (? - 2.8 ergs per sq cm). The argument was made that, when stacking-fault energy is high, cross slip and climb are favored, so that dislocation tangles and/or subgrain boundaries form more readily under cyclic loading. Since the boundaries and tangles act as paths of rapid crack propagation ,3, 4 life is shortened as a result. However, when stacking-fault energy is reduced (as by alloying), cross slip and climb become more difficult, with the result that substructure formation is retarded and growth rate is also reduced. A purpose of the present work was to investigate the substructure effect in relation to temperature. As temperature is lowered, ? is varied only slightly (if at all), but decreased thermal activation can interfere with cross slip and climb. Thus substructure formation could be curtailed and life increased. Fatigue life in the high-cycle range is also known to be strongly influenced by environment. Working with copper, Wadsworth and Hutchings observed that life in a vacuum of 10-8 mm Hg exceeded life in air by a factor of 20.5 They isolated oxygen as the agent that furthered cracking. While the details are still unclear, a requirement in any mechanism of oxygen-accelerated cracking is that there be chemisorption at the crack tip. That could prevent welding on the compression half cycle,= interfere with reversal of slip,1, 6 or aid in breaking metal-metal bonds at the crack tip.5'7 In the work being reported here, temperature was lowered by immersion in liquid nitrogen and helium, which also served to reduce both the oxygen concentration and chemisorption rate. A possible effect upon life, i.e., a lengthening, had to be recognized. Several researchers have determined fatigue lives at low temperatures presenting their results in the form of stress amplitude (S) vs cycles in life (N) curves.8-11 Such curves reflect, primarily, the fact that metal is strengthened by lowering temperature; effects of substructure and changing environment tend to be masked. The difficulty can be overcome by comparisons based on identical plastic-strain amplitudes, and in the present work the dependence of life on both plastic strain and stress amplitude was established. EXPERIMENTAL Materials. The principal materials were polycrystal-line copper (? - 70 ergs per sq cm)" and the Cu-8 wt pct Al alloy (? - 2.8 ergs per sq cm),I3 the latter being near the limit of solubility of aluminum in copper and having, therefore, the lowest stacking-fault energy in the CU-Al system. Specimens were machined from 0.118-in.-diam cold-swaged rods of high-purity (99.999 pct) copper and the Cu-8 Al alloy, the latter produced initially in a graphite boat by induction vacuum melting a mixture of 99.999 pct Cu and 99.99 pct Al. The machined specimens were annealed to produce mean grain diameters of about 0.070 mm in copper and 0.190 mm in the alloy. Specimen dimensions are given in Fig. 1. Values of the tensile yield stress, ultimate strength, uniform strain (determined by the Considgre construction), and reduction of area, for both materials at 4.2oK, 77oK, and room temperature, are listed in Table I. The tensile apparatus in which these results were obtained has already been described.14 Apparatus. Specimens were fatigued in push-pull with a machine that is illustrated schematically in Fig. 2. The specimen is first soldered into the top grip (1) with Woods metal, and the grip is then screwed into the inner tube (2) which is connected to the drive rod of the Goodmans vibration genera-

Jan 1, 1968

By A. Bauer, P. Calder, N. H. Carr, G. R. Harris

Smallwood mine is part of the Iron Ore Company of Canada's Carol Lake operation and is situated in Labrador, 240 miles north of Sept-Iles, Quebec. Last year, 15 million tons of crude ore were crushed to yield 6.3 million tons of concentrate and pellets. This year the figures will be 17 million of crude and 7 ¼ million tons of concentrate and pellets, which is the full plant capacity. Carol Lake ores consist primarily of specularite and magnetite mixed with quartz. Since both rotary and jet piercing drills are used, it is often desirable in planning to know in which regions of the orebody, or new orebodies, a particular drill will be most economic. This makes it necessary to establish a correlation between drillability and pierceability and some physical rock property. For the rotary drills a good correlation was found with penetration rate and grinding factor index. The jet piercers were found to have a reciprocal relationship in the sense that the best rotary ground was the worst jet ground and vice versa. It is also indicated how an economic comparison could be made using these penetration rate versus grinding factor index curves, the hole size distribution curves for single pass and chambered holes, and the mine distribution curve for grinding factor index.

Jan 9, 1965

By B. J. Kochanowsky

To improve blasting methods it is necessary to know how the explosive force acts and how rock resists this force. Because of the tremendous power developed within milliseconds and the great number of other factors directly affecting the technical and economic results, an analysis of the fundamentals of blasting theory is difficult. But since the rules used for layout design and for calculations of size of explosive charges are based on theoretical assumptions, complete knowledge of blasting theory has great practical importance in mining. Analysis of Blasting Theory: It is interesting to note the opinion of blasting experts with respect to contemporary blasting theories. F. Stussi,' Professor of the University of Zurich, stated: "We do not have enough experience yet to change our army engineering regulations in blasting and base it on new fundamentals. It is our duty to collect more practical data and to do more research in blasting to close this gap." K. H. Fraenkel,' editor of the Manual on Rock Blasting published in 1953 in Sweden and written by well-known Swedish, German, Swiss, and French blasting and explosive experts, said: "To the best of our knowledge no suitable formulas for civil blasting work are to be found in the American, French or German literature."

Sep 1, 1955

By Krahmann, Rudolf

THE following is an account of a survey undertaken to test the possibility of outlining a kimberlite pipe by magnetouietric methods. Kimberlite is a basic igneous rock closely related to melilite-basalt or alnoite, which occurs either in the form of volcanic plugs or as dikes intruded into rocks of various types and geological ages up to and includ¬ing the Lower Cretaceous. The famous diamond mines of South Africa are all in kimberlite pipes and these pipes are probably the original source as well of the vast alluvial deposits found in various parts of the country. The pipe chosen for this experiment is one that ' occurs on the farm Goedgevonden No. 20, about sixteen miles north of the village of Klerksdorp and ninety miles southwest of Johannesburg. Some prospecting has been done on this pipe and diamonds were produced from it but not in paying quantities. The magnetometric survey was made in June, 1932, by R. Krahmann and H. Wallisch and the results are shown on the accompanying plan. On the plan are shown also the boundaries of the pipe as exposed at the surface and details in regard to the surrounding foundations. These are taken from a geological survey made at a later date by W. Beetz, of Johannesburg.

Jan 1, 1935

By S. J. Leach

The possible solution of some of the problems raised in H. L. Hartman's article "Determining Ventilation Requirements for Continuous Miners," which appeared in the March 1962 issue of MINING ENGINEERING, is offered by recent investigative work done at the Safety in Mines Research Establishment, Ministry of Power, Sheffield, England. Highlights of this research are outlined here. Accumulations and layers of methane form in a mine roadway because it is difficult to mix methane with air beneath it by turbulent diffusion. Such mixing involves work contrary to buoyancy forces. In specifying requirements for good ventilation it is not, therefore, sufficient to state that the airflow must be turbulent in the absence of methane. Fundamental work at SMRE on the behavior of methane roof layers has led to the formulation of rules for controlling methane roof layers which specify the ventilation velocity needed to ensure adequate mixing in terms of the rate of flow of methane into the layer (V = cu ft per min) and the airway width (D = ft). A "layering number" for methane and air has been defined by [U37/V/D] where U is the mean ventilation velocity in ft/min in the upper half of the airway. In a horizontal airway there is no mixing by turbulent diffusion for values of the layering number less than about 2, resulting in extensive roof layers. But with a layering number of 5, the layer is "brought under control"-i.e., a further increase in the layering number will shorten the length of the layer only slightly, and a small decrease in the layering number will cause only a small increase in the length of the layer. In a sloping roadway with uphill ventilation, higher values of the layering number are needed to achieve this "controlled" condition; the values range from about 5 at small slopes to about 8 at a slope of 1: 10. In downhill ventilation it is possible for layers to "back" against the ventilation, i.e., to flow uphill. The critical condition for preventing backing can also be expressed in terms of the layering number. Backing will be prevented if layering numbers are about 3 for small slopes and about 4.5 for large slopes; these values for downhill ventilation also give good control of the layer.

Jan 10, 1962

By N. J. Grant, C. F. Flo, F. B. Cuff

An investigation of the Ti-Cr system has shown the presence of a complete series of solid solutions in the ß phase, with a minimum in the solid us near 50 pct Cr. An intermetallic compound, TiCr2, forms during cooling from the ß solid solution. There is a eutectoid reaction at the low chromium side of the system. IN view of the recognition of the potentialities of titanium and its alloys as important structural materials there has arisen a need for a systematic investigation of various titanium binary diagrams. Of these, the Ti-Cr system was of particular interest because of the improved properties imparted to titanium by small chromium additions. A literature survey disclosed a partial constitution diagram that had been suggested by Vogel and Wenderott,¹ This diagram, shown in Fig. 1, is the result of work done on the Fe-Cr-Ti ternary system. Alloys containing less than 43 pct Cr were not investigated. In addition to this, a study of alloys in the Ti-Cr system was reported by McPherson and Fontana.² Adenstedt3 furnished a number of dilato-meter curves obtained from specimens containing 5, 10, and 15 pct Cr. Very recently, McQuillan4 submitted a proposed diagram covering the complete range of compositions between titanium and chromium. This diagram was in general agreement with the one described here. Experimental Procedure Sponge titanium (99.7 pct) and electrolytic chromium (Bureau of Mines analysis: 99.03 pct Cr, 0.40 pct Fe, 0.53 pct O2) were used for the initial determination of the system. Subsequent refinement of points, particularly for the low chromium side of the diagram, was accomplished by using iodide titanium and high purity chromium (National Research Corp. analysis: 0.050 pct C, 0.045 pct O2). The Ti-Cr alloys were prepared by melting 25 g charges in an enclosed, water-cooled copper crucible using a movable tungsten electrode. The atmosphere was helium, prepurified by first passing it through a drying agent and then through sponge titanium heated to 850°C. Particular care was taken to avoid any large scale segregation resulting from insufficient mixing of the components. Each charge was melted and kept molten for approximately 1 min, allowed to cool, inverted, remelted, and kept molten for an additional minute. In order to ascertain the amount of impurity pickup (oxygen and nitrogen) during the melting procedure, three iodide titanium specimens were melted in sequence and then checked for increased hardness. The specimens in the as-cast condition showed a relatively large hardness increase over the hardness of the as-received iodide titanium. The scattering on these readings was large. However, after the specimens had been homogenized at 840 °C for 2 hr and slowly cooled, the measured increase in hardness over the as-received titanium was small with a corresponding decrease in scatter. The reason for this hardness change is that in heat treating these specimens below the transformation temperature (885°C) there was a conversion from the as-cast structure to the more nearly equilibrium structure of the annealed specimen. The alloys were analyzed for chromium content and although the actual percentage was invariably low the deviation from the nominal composition never exceeded 0.6 pct Cr.

Jan 1, 1953

By Philip McKenna

WHEN a new material becomes available to industry, it is useful to describe its properties as a guide to its most effective application; and when the new material may be produced in compositions having a series of graded properties, tests to select the combination of properties best adapted for various uses are helpful. The class of materials to be con-sidered in this paper are hard tool materials produced by processes of powder metallurgy from hard carbide constituents and various matrices of iron, nickel or cobalt, or alloys of them with tungsten, or tungsten and carbon. The customary use of carbide hard alloys is for metal-cutting tools; although wire-drawing dies, lathe centers, follow rests, grinding rests, burnishers, rolls, extrusion dies, measuring gauges and micrometers, and a number of other tools are also made with these hard alloys as the essen-tial wear-resisting parts. The properties and tests to be considered are those affecting these uses. In the development of tool, materials since the industrial revolution we have had carbon tool steels, Mushet steel, high-speed steels, stellites, and now cemented carbide compositions. For an understanding of the latter category of materials their properties and uses relative to the older and more familiar tool materials will be considered.

Jan 1, 1938

By J. Skrove, C. R. Boardman

In situ permeability of the rock outside the Hardhat chimney was determined by pressurization of long holes with air. Experimental data indicated a remarkable difference between fracture permeability of the rock near the chimney and that at a considerable distance. Although permeable fault zones were known to exist in the granite stock, the measurements of background permeability were quite low, on the order of tenths to several millidarcies. The observed difference is about two or three orders of magnitude above this background in the region 125 to 215 ft radially from the shot point, or 80 to 165 ft radially from the vertical axis of the chimney. The presence of a collapsed drift immediately beyond this region precluded measurements which could have defined the maximum extent of the zone of high permeabilily. INTRODUCTION Previous exploration has revealed that contained nu-clear explosions create cavities which generally collapse, resulting in rubble-filled chimneys and annular fractured zones. These geometries have been shown to result in complex flow regimes which should increase the production rate from hydrocarbon reservoirs.' Empirical scaling equations have been developed for estimatina chimney radii and heights for a variet; of rock media.' The exten; of the annular fractured zone has been documented and associated permeability changes have been observed qualitatively for several explosions. This study was begun to establish the nature and magnitude of the permeability of the latter region. It is anticipated that results will be useful in estimating permeability changes and consequent production stimulation which might ensue from a contained explosion in a hydrocarbon reservoir. The post-shot environment of the Hardhat event (a 5-kt contained nuclear explosion in granitic rock) was c'hosen for the experimental measurements. The Hardhat device was detonated at a depth of 939 ft, and subsequent exploration revealed a chimney of broken rock with a radius of 65 to 70 ft and a height above shot point of 281 ft.' BeFore the explosion, the Hardhat medium was highly jointed and fractured (Fig. I). Jt was expected that differential rock motion along these and other weaknesses induced during cavity growth and collapse would significantly alter the permeability of the rock mass. EXPERIMENTAL METHOD Initially, three 2-in. diameter holes (Nos. 10, 12 and 19) were drilled about 25 ft outward through the walls of the 500-ft level drift (elevation 4,253 ft, Fig. 2). One was drilled near the chimney and two holes, one vertical and the other horizontal, were drilled near the shaft. Order-of-magnitude differences in permeability obtained by pressurization measurements indicated further: investigation was warranted. A series of 3-in. diameter holes was then drilled with water as a coolant into the walls and roof of the drift (Fig. 2). An 11-in. long packer was set from 1 to 8 Et inside each hole and air was injected at measured Row rates. Hole pressures were monitored at the collar. Permeability was low enough in the holes near the access shaft that pressure could be maintained long enough to obtain good pressure decay rates. In the vicinity of the chimney, however, permeability was so high that this was not possible and air was injected under steady-state conditions. About one year later, these same holes were retested to

Jan 1, 1967

By V. V. Clark

WHEN a district is more or less primitive, and a trained mining engineer attempts single- handed to prospect it according to old standards, he generally fails. He has not the ability to live out in the open alone for months at a time and carry on with enthusiasm and determination like the old-time prospector. But the same engineer, placed in an organized group where modern prospecting methods are employed, is immediately put on his mettle and his chances of winning are greatly increased. Marsman Investments, Ltd., with headquarters in Manila, has at the present time, Sept. 4, 1937, six prospecting parties in the Netherland East Indies. Three of these groups are combing their assignments for lode mines, studying structures, developing and reaching out into veins and zones with diamond drills. The other three are searching for placer mines with pans, pits, and Empire drills. I am in charge of one group seeking commercial gold placers on the Island of

Jan 1, 1937

By M. J. Sheriff, D. H. Smith, W. Macdonald

The paper outlines the basic procedure used in electrical system planning and design. Consideration is given to the use of applicable codes and standards, development and use of a system One Line Diagram, power availability, load requirements and power factor. Also discussed are the factors influencing the selection of power supply and distribution arrangement, voltage levels, system grounding, distribution and utilization equipment such as switchgear, transformers, motor control, cable systems, motors. Short circuit calculation methods and system protection are discussed.

Jan 1, 1978

A. SILVERMAN,* Pittsburgh, Pa.-Prof. Richards has described a very interesting process. In addition to the method described, electroplating and a number of other processes have been used. In one, the two metals were heated and united under hydraulic pressure; in a second, the steel was coated with an alloy, brass for example, and the molten copper cast around this. The process that I would like to bring to the attention of the metallurgists present consists simply of pouring molten copper, brass, or cupronickel around a clean red-hot steel billet. 'It is covered by the Roth patents. The 8-in. cylindrical billet containing about 70 per cent. steel (core) and 30 per cent. copper is hot drawn or rolled until several inches in diameter and afterward cold drawn or rolled to rod, wire of any desired diameter, or sheet. The wire is used for electrical conduits where conductivity and high tensile strength are required, also for the manufacture of cables and screen cloth. The sheet is employed for the manufacture of spouting, molding, shells, etc. The last application is particularly interesting. In testing rifle cartridges, which usually contain lead-filled copper noses, pine boards 1 in. thick, covered with ¼ -in. rawhide, are placed 1 ft. apart. The value of the cartridge depends on the number of boards penetrated by .the bullet. In government tests made with copper-coated steel noses (15 per cent. copper on either side of the steel) the penetrating power was found to be approximately double that of pure copper noses. The advantage of copper-coated steel over cupronickel lies in the fact that the- former does not require any special heat treatment during the punching. Rifle cartridges were prepared from copper-coated steel in a number of government arsenals. The value of the combination was attested by the awarding of a contract for the construction of a $3,300,000 plant. Unfortunately, the contract was signed on the day preceding the signing of. the armistice and was cancelled several days later. Tests were conducted for about 1 yr. before the contract was awarded to determine the value of this combination of metals. Since the war a number of cartridge and shell manufacturers have signified their intention of using copper-coated steel.

Jan 4, 1919

By Stanly A. Easton, H. M. Childs

Methods evolved at Kellogg have had primarily in view the safety of workmen and complete recovery of the ore; it is believed that these results have been secured at a minimum cost. The ore in the Bunker Hill mine is of good grade, relatively speaking; much of it is quite rich and no mining method would be successful which did not recover all of the ore. It would be possible to work certain of the orebodies by shrinkage methods, or some form of top-slicing, at probably lower costs than by the methods now applied, but the shapes of the orebodies are so irregular that satisfactory extraction of the ore in all its ramifications would be extremely difficult. In past years, much high-grade ore has been lost in blasting, due to the unskilful use of powder in a galena ore, which, by reason of its brittle-ness and great weight, tends to scatter widely. Any method by which large masses of ore and waste are broken together will result in an imperfect recovery of the ore, and whenever large masses are broken, ore and waste will unavoidably fall down together; ore and waste thus become entangled and, although a pile of broken material may seem to have been well picked over, quantities of ore will inevitably be lost. This fact has been shown by persons reworking the filling in stopes that were mined by methods defective in the foregoing particulars. Safety of the men is secured by avoiding large openings, and by working mainly under timber, and at small faces at close range and easily inspected. In former years the principal source of serious accidents was "falls of ground;" it is now over seven years since a serious accident has occurred from this cause. The most prolific source of accidents during recent years has been "timber and tools," workmen being struck by timbers passed into the stope from the level above; this danger has been greatly reduced by compressed-air warning whistles and the fencing in of dangerous areas. The lead-silver ore of the Bunker Hill and Sullivan and affiliated mines is found in bodies of almost every shape, although vertical or nearly

Jan 1, 1925

HenRy Clay FRick, a pioneer in modern coke and steel industry and, in more recent years, one of the outstanding financiers of America, died on Dec. 2, 1919, at his home on Fifth Avenue, New York. Although he had been ill since election day, when he had an attack of indigestion which developed into ptomaine poisoning, his death was a surprise to all. He is survived by his widow, Adelaide Howard Childs Frick; a son, Childs Frick, one unmarried daughter, Helen C. Frick, and four grandchildren. A quiet funeral service was conducted at the Frick home on Wednesday afternoon by the Rev. Dr. Leighton Parks, pastor of St. Bartholomew's Episcopal Church. This was attended by members and very intimate friends of the family, Trustees of the Metropolitan Museum of Art, Officers of the Links Club, and Directors of the United States Steel Corpn. Henry Clay Frick was born Dec. 19, 1849, in West Overland, Westmoreland Co., Pa. His father, John W. Frick, was a farmer of Swiss ancestG, and his mother, Elizabeth Overholt Frick, a member of an old Mennonite family. Until he was sixteen, he spent his time at school, on his father's farm, and in his grandfather's distillery, where he kept books. He attended Otterbein University, in Ohio, for a year. Frick, learning that coke was an essential of the already rapidly developing steel business, early invested every cent he could get in coking-coal lands. With the help of an associate of his grandfather, he formed the corporation of Frick & Co., coke dealers, and acquired fifty-one ovens in the Connellsville region and 300 acres of soft-coal lands. During the panic of '73, with the help of Judge Thomas Mellon, a Pittsburgh 'banker, he bought out his partners and while coke was selling at 90 cents a ton enlarged his purchases of suitable lands. Later, the price of coke increased until it was selling at $5 a ton. Before he was 30 years old, Frick was rated a millionaire. Association with CaRnegie In 1878, he sold an interest in the business Do E. M. Ferguson of New York, and later a share to Mr. Ferguson's brother. Four years later the business was reorganized into the H. C. Frick Coke Co. with vast coal lands, great banks of ovens, and a capitalization of $2,000,000. Then began his association with Andrew Carnegie. He exchanged a part of his coke interest for shares in Carnegie Brothers of Pittsburgh,

Jan 1, 1920

By J. E. Lawver, B. J. Clingan, R. E. Snow

Response surface methodology is a well-known and powerful technique for determining optimum conditions in flotation systems. One disadvantage is the onerous task of the numerical calculations and curve plotting. This paper describes a system in which the investigator simply selects the range of several flotation variables after which the design of the experiment, data analysis, generation of response surface equations, and response surface plots are automatically carried out using a digital computer and a computer-driven curve plotter. Several typical response surfaces of important variables in phosphate flotation are presented as examples.

Jan 1, 1980

By R. W. Heckel, R. E. Trabocco

The recovery process in 400 Monel filings was followed, principally, by using the Warren-Averbach technique of X-ray peak profile analysis. The deformation fault probability, a, was 0.006 in samples of unannealed filings. a , the twin fault Probability , was approximately 0.002 in samples of unannealed filings. Both a and 0 were found to "anneal out" at 600°F. The effective particle size and mzs strain increased and decreased in the (111) direction, respectively, with increasing annealing temperature. The actual particle size was found to be almost equivalent to the effective particle size. Tile small values of deformation and twin fault probabilities accounted for the similarity in values of the effective and actual particle sizes. Stored strain energy and dislocation density calculations based on rms strain decreased with increasing annealing temperature. The dislocation density decreased from 10" per sq cm in the unannealed filings to 10' per sq cm in the partially re-crystallized filings. The square root of the dislocation density based on strain to that based on particle size indicated a random dislocation distribution in the unannealed filings. The dislocation arrangement changed to one with dislocations in cell walls with increasing annealing temperature. THE recovery processes which occur in metals are generally thought to be a redistribution and/or annihilation of defects.' Investigators' have shown that recovery processes can be characterized by X-ray line-broadening analyses. Michell and Haig4 measured the stored energy of nickel powder by calori-metry and found the value to be greater by a factor of 2.5 than that from X-ray data obtained by the Warren-Averbach technique.= Minor increases in particle size occurred up to 752°F (recovery), while above 752°F the particle size increased greatly due to recrystalliza-tion. X-ray microstrain values decreased between room temperature and 392"F, remained constant from 392" to 752"F, and decreased from 752°F to a negligible value at 1112°F. Faulkner developed an equation for calculating stored strain energy based on X-ray line-broadening data which gave a closer correlation of measured and calculated stored strain energy based on the data of Michell and Haig. The stored strain energy released during recovery is predominately dependent on the decrease in dislocation density which was p-enerated from cold work.7 Stored energy has been measured8 in alkali halides during recovery and recrystallization and 80 pct of the stored energy was found to be released during recovery. Dislocation distributions have been studiedg in a number of fcc metals by thin-film electron microscopy. Howie and Swann" found the stacking fault energy of copper and nickel to be 40 and 150 ergs per sq cm, respectively. ~rown" has pointed out that these stacking fault energy values should be corrected to 92 and 345 ergs per sq cm, respectively. The dislocation distribution of a metal is directly dependent on the stacking fault energy of the system. Metals of high stacking fault energy such as aluminum cross-slip readily and do not form planar arrays of dislocations. Metals of lower stacking fault energy such as stainless steels" do not cross-slip readily. Cold-worked nickel has been found to form a cellular dislocation structure after annealing.13 The relatively high stacking fault energy of nickel and copperlo to a lesser extent favor cellular structures of dislocations rather than planar arrays after deformation. The present study of recovery was carried out on a Ni-Cu alloy (Monel 400) to compare with prior studies for pure nickel and pure copper. X-ray line-broadening techniques were used to measure the effect of recovery temperature on rms strain and particle size and the results were compared with previous studies on copper'4-'7 and nickel., Calculations were also made on stacking fault probabilities, dislocation density, dislocation distribution, and stored strain energy as affected by temperature. EXPERIMENTAL PROCEDURE The nominal analysis of the Monel 400 used in this investigation was: 66.0 pct Ni, 31.5 pct Cu, 0.12 pct C, 0.90 pct Mn, 1.35 pct Fe, 0.005 pct S, 0.15 pct Si. The annealed material was cold-reduced in two batches, one 50 pct and the other 80 pct. It was originally planned to conduct line-broadening studies of these bulk samples; however, rolling textures that developed produced low-intensity peaks which were not suitable for line-broadening analysis. Filings were prepared at room temperature from both the 50 and 80 pct cold-reduced specimens, series A and series B, respectively, and were not screened prior to heat treatment or X-ray studies. Heating to the annealing temperature, 200" to 120O°F, was accomplished in a matter of minutes in a hydrogen atmosphere. Following heat treatment, some of the filings were mounted and polished for microhardness measurements with a Bergsman microhardness tester, using a 10-g load. A G.E. XRD-5 diffractometer using nickel-filtered Cum radiation was used to obtain all diffraction patterns. Only (111)- (222) line-broadenin data were used in the present study since the {400f peaks were too weak to use. The Fourier analysis of the (111) and (222) peak

Jan 1, 1969

By E. L. Anderson, J. R. Long, R. S. Dean, F. S. Wartman

Titanium has been estimated to comprise about 0.65 per cent of the earth's crust and ranks fourth in abundance among the metallic elements suitable for engineering uses. In spite of this, applications of titanium for structural purposes have not as yet been developed. Its commercial exploitation has been largely confined to the chemical industries and the production of paints and pigments; no doubt because of the difficulties that lie in the way of preparing the pure ductile metal. Published reports, however, indicate that ductile titanium can be prepared and possesses some unique properties. This, together with the occurrence in this country of several important titaniferous deposits, has led the Bureau of Mines to investigate processes for the production of metallic titanium, methods required for its fabrication, and the properties that may be produced in this interesting metal. Methods of Preparing Metallic Titanium Many early investigators claimed to have isolated metallic titanium; but in the light of present knowledge, it seems that they really had produced various mixtures of carbides and nitrides that have a metallic appearance but are brittle, hard, and unworkable. The first metallic titanium pure enough to be malleable when cold was produced by Hunter1 in the early part of the twentieth century. Kroll,~ van Arkel,~ and Fast,4 subsequently confirmed the facts that pure titanium is a. ductile metal and that small amounts of impurities were responsible for previous reports of brittleness. When heated, titanium reacts chemically with various gases, such as hydrogen, oxygen and nitrogen; if the volume of gas thus absorbed is too great, the metal becomes brittle and unworkable. The principal difficulty in making ductile titanium is prevention of such contamination, and the success of a given process may be judged by the completeness with which it solves this difficulty in a practical manner. Of the gases mentioned, hydrogen is the least objectionable, since its absorption by the metal is completely reversible and, although dimensional changes occur and absorption of hydrogen embrittles the metal, the gas may be removed readily by heating in a high vacuum for a short time. On the other hand, the absorption of oxygen or nitrogen results in the formation of permanent solid solutions of the oxide and nitride, which cannot be decomposed by the strongest reducing agentsz with sufticient completeness to restore the inherent ductility of the metal. Because of

Jan 1, 1946

By J. R. Long, E. L. Anderson, R. S. Dean, F. S. Wartman

TITANIUM has been estimated to comprise about 0.65 per cent of the earth's crust and ranks fourth in abundance among the metallic elements suitable for engineering uses. In spite of this, applications of titanium for structural purposes have not as yet been developed. Its commercial exploitation has been largely confined to the chemical industries and the production of paints and pigments; no doubt because of the difficulties that lie in the way of preparing the pure ductile metal. Published reports, however, indicate that ductile titanium can be prepared and possesses some unique properties. This, together with the occurrence in this country of several important titaniferous deposits, has led the Bureau of Mines to investigate processes for the production of metallic titanium, 'methods required for its fabrication, and the properties that may be produced in this interesting metal. METHODS OF PREPARING METALLIC TITANIUM Many early investigators claimed to have isolated metallic titanium; but in the light of present knowledge, it seems that they really had produced various mixtures of carbides and nitrides that have a metallic appearance but are brittle, hard, and unworkable. The first metallic titanium pure enough to be malleable when cold was produced by Hunter1 in the early part of the twentieth century. Kroll,2 van Arkel,3 and Fast,4 subsequently confirmed the facts that pure titanium is a ductile metal and that small amounts of impurities were responsible for previous reports of brittleness. When heated, titanium reacts chemically with various gases, such as hydrogen, oxygen and nitrogen; if the volume of gas thus absorbed is too great, the metal becomes brittle and unworkable. The principal difficulty in making ductile titanium is prevention of such contamination, and the success of a given process may be judged by the completeness with which it solves this difficulty in a practical manner. Of the gases mentioned, hydrogen is the least objectionable, since its absorption by the metal is completely reversible and, although dimensional changes occur and absorption of hydrogen embrittles the metal, the gas may be removed readily by heating in a high vacuum for a short time. On the other hand, the absorption of oxygen or nitrogen results in the formation of permanent 'solid solutions of the oxide and nitride, which cannot be decomposed by the strongest reducing agents2 with sufficient completeness to restore the inherent ductility of the metal. Because of

Jan 1, 1946

By J. R. Long, E. L. Anderson, R. S. Dean, F. S. Wartman

Titanium has been estimated to comprise about 0.65 per cent of the earth's crust and ranks fourth in abundance among the metallic elements suitable for engineering uses. In spite of this, applications of titanium for structural purposes have not as yet been developed. Its commercial exploitation has been largely confined to the chemical industries and the production of paints and pigments; no doubt because of the difficulties that lie in the way of preparing the pure ductile metal. Published reports, however, indicate that ductile titanium can be prepared and possesses some unique properties. This, together with the occurrence in this country of several important titaniferous deposits, has led the Bureau of Mines to investigate processes for the production of metallic titanium, methods required for its fabrication, and the properties that may be produced in this interesting metal. Methods of Preparing Metallic Titanium Many early investigators claimed to have isolated metallic titanium; but in the light of present knowledge, it seems that they really had produced various mixtures of carbides and nitrides that have a metallic appearance but are brittle, hard, and unworkable. The first metallic titanium pure enough to be malleable when cold was produced by Hunter1 in the early part of the twentieth century. Kroll,~ van Arkel,~ and Fast,4 subsequently confirmed the facts that pure titanium is a. ductile metal and that small amounts of impurities were responsible for previous reports of brittleness. When heated, titanium reacts chemically with various gases, such as hydrogen, oxygen and nitrogen; if the volume of gas thus absorbed is too great, the metal becomes brittle and unworkable. The principal difficulty in making ductile titanium is prevention of such contamination, and the success of a given process may be judged by the completeness with which it solves this difficulty in a practical manner. Of the gases mentioned, hydrogen is the least objectionable, since its absorption by the metal is completely reversible and, although dimensional changes occur and absorption of hydrogen embrittles the metal, the gas may be removed readily by heating in a high vacuum for a short time. On the other hand, the absorption of oxygen or nitrogen results in the formation of permanent solid solutions of the oxide and nitride, which cannot be decomposed by the strongest reducing agentsz with sufticient completeness to restore the inherent ductility of the metal. Because of

Jan 1, 1946

By E. J. Fasiska, H. Wagenblast

The dilalion of a ivon by interslilial carbon was measured by two independent techniques —dilatometric mesurements at 719 c and X-ray measurments of the urlil cell parameters a1 room temperature after quenching. The relative expansion per increase in cavbon content by both methods is (2.9 + 0.3) x 10-3 pev at. pcl C nrzd is temperature- independent within experimental error. This corresponds to (6.3 5 0.6) cu cm per g-atom for the partial gram-atomic volume of carbon in a iron-only slightly smaller than the atomic volume for iron in the same temperature vange. THE only previous quantitative study of the dilational effect of carbon dissolved in a iron was performed in 1934 by Burns1 which, at the time, generated some discussion of possible sources of experimental error.2 For a system of such widespread importance, we felt that a new investigation was merited. Both X-ray diffraction and dilation measurements were used to determine the expansion of the a iron lattice by dissolved carbon, avoiding as much as possible any previous experimental problems and deficiencies. The dilation method at solution temperature offers not only measurements which are free of residual strain but also, in conjunction with the room-temperature X-ray measurements, a method to detect any large temperature dependence of the partial gram-atomic volume of carbon. To insure that quenching strains did not affect the room-temperature X-ray measurements, wire specimens of constant carbon content but different diameter were examined for such an effect. SPECIMEN PREPARATION The material used for both experimental techniques was "Ferrovac E" iron received in the form of 19-mm-diam rod and stated as having the following impurity contents: C, Cr, Cu, Mn, P, and V, each in the range of 10 to 50 ppm; Co, O, Mo, S, and Si, 60 to 100 ppm; W, 200 ppm; Ni, 230 ppm; N, 4 ppm. The stock material was cold-swaged to 0.71 mm diam for the Debye-Scherrer X-ray camera specimens and portions were cold-rolled from 6.3 mm diam to 0.79- and 0.25-mm sheet for X-ray diffractometer and dilation measurements. The wires were annealed in wet hydrogen for 6 hr at 840°C and 15 hr at 720°C, and then quenched into 0°C water. A chemical analysis for carbon after this treatment gave 0.0046 + 0.0014 at. pct C. Three portions of these wires were subsequently held at 719°C in three different hydrogen + methane mixtures and then quenched, resulting in carbon concentrations of 0.0283, 0.0598, and 0.1067 at. pct C by chemical analysis. After carburizing, the wires were swaged to 0.48 mm and electroplated with silver to prevent carbon loss during subsequent heat treatment. The final heat treatment consisted of holding the wires at 72 1°C for 5 min in a He-2 pct H mixture followed by quenching into 0°C brine. The wires were held at room temperature for a few minutes to remove the silver plating using a phosphoric acid-hydrogen peroxide solution, and then stored in liquid nitrogen until the measurements were made. EXPERIMENTAL TECHNIQUE A) Dilation Measurement. The dilatometer consisted of a gas-atmosphere vertical tube furnace modified so that length changes of a ribbon-shaped specimen could be measured externally. This was done by installing a gas-tight mercury seal at the top of the furnace as shown schematically in Fig. 1. The specimen (21.0 cm long, 1.27 cm wide, and 0.25 mm thick) was suspended in the center of the furnace by 3-mm-diam quartz rods with the upper one passing through the cap of the mercury seal. Above the cap, the upper quartz rod was coupled to a lever exerting a load of about 25 g (-12 lb per sq in.) on the specimen and having a 10 times mechanical magnification. The vertical position of a marker at the other end of the beam was read with a traveling microscope with a precision of 0.01 mm. The temperature gradient of the furnace was meas-

Jan 1, 1968