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By Arthur Hockman, Howard W. Jaffe, Howard F. Carl

THE problem of establishing practical techniques for evaluating natural corundum ores arose from the desire to improve the existing purchase specifications for crystal corundum procured by the Federal Government for stockpiling. Such purchase specifications had been developed for a large number of products, including minerals and ores considered to be critical and strategic because of the country's dependence on foreign sources of supply. It will be apparent to anyone considering the subject of purchase specifications that the determination of whether or not a submittal meets the specifications is a prime consideration. Consequently satisfactory specifications for minerals should not only incorporate physical, chemical, and mineralogical requirements that are practical but should also establish the means by which both buyer and seller can be assured that materials meet stated requirements. The Munition Board's Material Purchase Specification for corundum, dated February 1954, covered two grades of crystal corundum intended primarily for abrasive use. It established limits of size and of composition: Grade A, at least 95 pct +3 mesh and 92 pct alumina (Al2O3); Grade B, at least 95 pct +7 mesh and 90 pct alumina. It also specified that "of each lot of material, not less than 95 percent shall have a hardness equal to or exceeding nine (9) on Moh's Scale." These specifications were unsatisfactory for several reasons. They did not allow the purchase of lower grades of corundum being used by industry. Neither did they specify exactly what a corundum ore actually was, except that it should contain so much alumina and have a certain scratch hardness. Nothing was said about the abrasive qualities of the material that was to be purchased primarily for abrasive use. During the period 1946 to 1948 supplies of the two grades defined in the then current specifications continued to decrease. Early in 1949 industry recommended that the finer sizes of corundum known as "crystal corundum concentrates," ¼-in. to 16-mesh material, be added to the stockpile specifications and that lower grades of crystal corundum also be included. In the spring of 1949 the National Bureau of Standards and the Bureau of Mines were asked by the Munitions Board to cooperate in developing more practical specifications for grading natural corundum ores. The National Bureau of Standards indicated that it would investigate physical test methods for determining abrasive characteristics of corundum, and the Eastern Experiment Station of the Bureau of Mines at College Park, Md., stated that it would consider the mineralogical aspects of the problem. Members of these two agencies, in consultation with representatives of the Office of Materials Resources of the Munitions Board and of the Federal Supply Service of the General Services Administration, and with the cooperation of industrial suppliers and consumers of abrasive corundum, developed, in a fairly short time, more practical specifications for six grades of corundum ores. The new specifications, issued January 1951, were for corundum, natural crystals, as by this time high-purity synthetic corundum was available and widely used. Nevertheless, for certain specific applications the natural product was preferred over the synthetic material. It has been extensively used in forming snagging wheels. It breaks into more or less cubical particles, whereas artificial corundum fractures into splintery shapes. These produce irregular cuts in glass, while the more symmetrical shape produces a more uniform ground surface. For this reason natural corundum has been preferred for certain types of lens grinding. Pure corundum is clear, colorless alpha alumina (A12O3), but it is rarely found in nature in this form. The most important gem varieties include the blue and yellow sapphires and the ruby. Minute impurities of titanic oxide impart a blue color,

Jan 1, 1955

By John Fritz

THE John Fritz Medal was presented to Ambrose Swasey of Cleveland, Ohio, in the Auditorium of the Engineering Societies Building, in New York, on April 23. Charles F. Rand, Chairman of the Board of Award, presided and, after speaking very briefly of Mr. Swasey, whose friend he has been for a great many years, ,introduced Gen. William Crozier, formerly Chief of Ordnance, U. S. Army, who spoke most entertainingly of, Mr. Swasey's accomplishments in designing and manufacturing instruments of precision, particularly for the use of artillery in range finding: Dr. William Wallace Campbell, Director of the Lick Observatory, and President of the University of California, described Mr. Swasey's, contribution to astronomical advancement by his notable development of the largest telescopes in this country.

Jan 1, 1924

By AIME AIME

BLANDFORD. C. BURGESS, the new Chairman of the Industrial Minerals Division, took the advice of Horace Greeley in reverse-he turned his hack on San Francisco and the Golden Gate, and after a few side excursions toward Alaska and Arizona, hit the trail eastward, not for the lonesome pine, but for Spruce Pine, N. C. Born Aug. 10, 1893, in San Francisco. Burgess found his first job, shortly after finishing high school at 19, as axeman for a surveying party of engineers working for the Southern Pacific Co. in Oregon. Later he moved on up with them into Alaska. He liked the engineering profession, and decided to equip himself further so he entered the University of California in the fall of 1913. and for the next two years devoted himself to acquiring an education in civil engineering.

Jan 1, 1945

By Euclid P. Worden

In 1977, an article in World Mining1 reported a total of 2726 rotary blasthole drills in service. This figure included only those machines produced by three of the manufacturers building drills of this type. The total, therefore, is much higher. Rotary drilling in the mining industry is big business to the manufacturers and suppliers involved, and a significant cost item to mine operators. The time has come to take a hard look at rotary drilling technology with an eye to reducing costs by increasing drilling efficiency. The efficiency of any rotary drilling operation is best measured in terms of the rate of penetration achieved by the bit. In blast hole drilling, there are five factors which affect the rate of penetration. They are: (1) bit selection, (2) weight on the bit, (3) rotary speed, (4) hole cleaning, and (5) formation properties. Of these factors, all but one may be controlled by the operator. Looking at any one in detail may reveal possible improvements in the system. One of these factors -- proper hole cleaning - will be discussed in this paper. In order for a bit to perform at its maximum capability, each tooth or insert should strike fresh clean rock as it falls into its drilling position. If the tooth or insert lands on previously drilled cuttings, a major portion of the energy delivered to the bit is absorbed in redrilling this broken material. A major portion of the interest, therefore, should be directed to the proper cleaning of the bottom of the hole. In an in-depth study of the cleaning of large diameter holes, Allen2 reports that horizontal air velocities of 38.10 m/s are necessary to prevent the saltation of drilled cuttings on the bottom of the hole. The exact flow pattern on the bottom of the hole, however, is not generally known. The air leaves the bit through the jet nozzles and the mouths of the cones, but where it goes from there is uncertain. This problem should be investigated by the bit manufacturers because they can best utilize the results of such an investigation to provide a more effective product. Some work has been initiated in this area and competition will probably increase its intensity. Bailing velocity is the best criteria to measure the cleaning of the hole, including the bottom, and is the factor on which efforts toward improvement must be concentrated. The first consideration is "What should the bailing velocity really be?" In drilling deep holes for oil and gas, 15.24 m/s is the generally accepted figure. In blasthole drilling, the figures of 25.40 m/s for average rock to 35.56 m/s for iron ore were first mentioned by Capp3 in 1962. The recommendations are the same to this day. A number of questions could be asked in regard to the apparent disparity between these two sets of figures. Various investigators have derived formulas which support one or another of these criteria. A thesis on the subject was written by Alexander4 who derived a formula based on research which resulted in velocities in the lower end of the ranges quoted previously. He set out to compare this figure to laboratory tests and his tests indicated that the velocities given by the derived formula appeared to be high.1 Perhaps the best reason that the 25.40 to 35.56 m/s range has been used, is that these velocities seem to work. Below the accepted figures, low bit life and slow penetration rates occur. Above these figures, increasing amounts of abrasive wear on the drill pipe and stabilizers seem to appear. There is a fallacy to this entire approach, however. The entire velocity calculation is made using nominal bit and pipe sizes and compressor deliveries with no compensation made for losses in the system. Perhaps an examination of some of the things that are not presently considered could lead to some practical improvements in the operation.

Jan 1, 1980

By Arnold H. Kackman

At the Kaiser Cement and Gypsum plant near San Jose, Calif., one rod-ball mill has taken over the entire raw grinding function for the largest single cement operation in the West. Installed as part of a major overhaul performed on the plant by Kaiser Engineers, the new mill does the work of seven previous mills in feeding the plant's six kilns and keeping pace with its annual capacity of 8.5 million bbl of cement. Installation of the mill, which is the largest in the world, was started in December of 1966 and completed in April of 1967. The over-all modernization program surrounding the new mill has included the modification of existing crushing facilities; the building of new raw materials handling and blending facilities, new raw milling facilities, and new slurry handling facilities; and the installation of a digital-analog control system.

Jan 7, 1967

By R. R. Vandervoort

The creep behavior of Nb(Cb), Ta, Mo, and W was determined under conditions of constant atomic dif-fzisivity, constant stress to elastic modulus ratio, and nearly equivalent grain size, and the steady-state creep rates obtained from these tests were correlated with calculated stacking fault energies for the metals. These results, in conjunction with similar data for several fccMetals,13 suggest that stacking fault energy may influence the creep strength ofbcc metals. The interrelationship between steady-state creep rate, subgrain size, and stacking fault energy was examined. It was found that the subgrain size for a given creep stress, increased as stacking fault energy increased, but that this relationship did not cormpletely account for the effect of stacking fault energy on creep rate. The crystallography and energetics of stacking fault formation in bcc metals has been discussed by a num-ber of authors,1-5 and impurity stabilized stacking faults on (112) planes have been observed in Nb,6,7 w,8,9 Fe,] and V" by transmission electron microscopy. However, a crucial question is whether or not stack-ing faults influence the mechanical strength of bcc metals. Potentially, stacking faults could increase strength by reducing the mobility of the partial dis-locations bounding the fault, by acting as barriers to slip dislocations, and by retarding the climb of dislo-cations during high-temperature deformation. The objective of this study was to seek a correlation be-tween creep strength and stacking fault energy for several bcc metals; namely, Nb, Ta, Mo, and W. The creep behavior of most polycrystalline metals and alloys at high temperatures and moderate stresses can be described by the following relation:11,12 im=Af(s) where i, = minimum creep rate, A = constant, j(s) = a function involving metallurgical structure, a = applied stress, E = average elastic modulus at the test tempera-ture, w = constant (equal to 5 for most pure metals), D = diffusion coefficient. One factor in the structure function F(s) which sig- R. R. VANDERVOORT, Member AlME is Research Metallurgist, Process and Materials Development Division, Chemistry Department, Lawrence Radiation Laboratory, University of California, Livermore, Calif. Manuscript submitted February 28, 1969. IMD nificantly affects the creep resistance of fcc metals is stacking fault energy, and creep rate has been shown to vary directly with stacking fault energy to the 3.5 power." In the latter investigation, four fcc metals of widely different stacking fault energies (Ag, Cu, Ni, and Al) were creep tested at a constant stress to modulus ratio of 1.21 x 10-4, at a constant diffusivity of 2.7 x 10-12 sq cm per sec, and at nearly equivalent grain sizes of about 0.7 mm. The creep data were then correlated with stacking fault energies. In the present study, a similar procedure was followed. All materials used in this work were consolidated by powder metallurgy techniques. Impurity contents in the as-received materials are listed in Table I. Chemical analyses showed that no measurable contamination of the test specimens occurred during pretest annealing treatments or creep testing. Specimens with a gage section 0.75 by 0.125 by 0.050 in. were creep tested in tension in a vacuum of less than 10-9 torr. Deformation at temperature was measured by tracking fiducial marks on the gage section of the specimen with an optical comparator. Optical deformation measurements also permitted observation of the macroscopic characteristics of the deformation Table I. Typical Specimen Impurity Content, ppm Nb Ta Mo W C 45 10 155 6 O 185 30 4 10 N 30 6 3 2 H 5 I 1 <1 als 3 10 2 15 Ca <5 I3 5 Cr 5 <3 10 <5 Cu 10 50 2 15 Fc 10 10 150 35 Ni 2 150 20 <5 Si <I0 1 3 <10 Ta 100 Ti 10 8 1 Zi 15 50 1 3 Table II. Test Conditions for Constant Stress-Modulus Ratio of 6 X 10.&apos; and Constant Diffusivity of 2.7 X 10-12 sq cm per see, and Grain Size Values for the Given Pretest Annealing Treatments Literature references Pretest Annealing for E and D Treatment Stress, Temperature, ___"&apos;Values__ Grain Tempera-Metal psi "C E D Size, mm ture, .C Time hr Nb 745 1525 14 15 to 17 0.83 1650 I Ta 1220 1770 18 19.20 O.91 1800 I Mo 1975 1630 18 21 0.77 2200 I W 2140 2265 18 22 040 2400 5

Jan 1, 1970

By T. M. Morris

A SEARCH of the literature reveals that no measurements have been made of the forces acting between a small solid particle whose surface is hydrophobic, and an air bubble to which the solid adheres, both immersed in water. Analyses have been made of the forces acting to support a greased solid on the surface of water, and the forces acting to cause a solid, whose surface is hydrophobic, to adhere to an air bubble in water. The latter analysis T. M. MORRIS, Junior Member AIME, is in the Department of Metallurgical Engineering and Mineral Dressing, School of Mines and Metallurgy, Rolla, Mo. New York Meeting, February 1950. TP 2734 B. Discussion of this paper (2 copies) may be sent to Transactions AIME before Feb. 28, 1950. Manuscript received May 16, 1949. This paper is the result of work done for part of a doctor&apos;s thesis at the Missouri School of Mines and Metallurgy. is often incomplete, however, because the internal pressure of the bubble has been neglected. It will be demonstrated that the internal gas pressure is not a negligible factor when dealing with bubbles of the size encountered in flotation. A study of the forces acting between an air bubble attached to a large flat surface is informative. It must be borne in mind, however, that this is not the condition present in a flotation cell, where the particle is small compared to the size of the bubble. The bubble is allowed to spread to its maximum contact angle on a large flat surface in the first case, whereas in the second case, the spread of the bubble is limited to the surface of the small particle which is presented to the bubble. Kabanov and Frumkinl studied the forces acting to cause adhesion of bubbles of hydrogen to a large surface of mercury, which served as an electrode in a dilute sulphuric acid solution. The force acting to hold the bubble to the mercury surface was found to be the vertical component of the surface tension between hydrogen and the sulphuric acid solution. The forces tending to cause the bubble to separate from the mercury surface were found to be: (1) the force exerted due to the internal pressure of the bubble acting upon the area of contact between the bubble and the mercury surface, and (2) the buoyant force of the bubble minus the hydrostatic force acting at the base of the bubble. These investigators photographed bubbles that were just on the verge of separating from the mercury surface. From these photographs, they measured the contact angle between the mercury surface and the tangent to the hydrogen-solution interface at the point of contact between bubble and mercury surface. They calculated the volume of the bubble and the internal pressure of the bubble. The equivalence between the upward acting and downward acting forces was remarkable. Wark2 pursued an investigation similar to that of Kabanov and Frumkin, and at the same time. His deductions verified those of Kabanov and Frumkin. He also considered the conditions present in flotation and was aware of the effect of the internal pressure of the bubble. Further, he proposed several conditions under which a small solid particle would adhere to an air bubble in water. In 1922, Edser," an English physicist, made the following statement. "It must be remembered that no particle could float stably, but for the possibility of variation of the contact angle, for if this were a constant, a slight tilt would inevitably cause the particle to sink." Wark criticized this statement, maintaining that the contact angle does not vary. The experimental data to be presented indicates that Edser was correct. Experimental Procedure: Briefly, the experimental procedure was as follows. A bubble of air was generated in distilled water. A rod of known diameter, one end of which was water repellent, was attached to this bubble. The weight of the &apos;rod was measured. The internal pressure of the bubble was measured with a manometer. The hydrostatic head from the surface of the water to the bottom of the rod was measured. The angle between the horizontal projection of the end of the rod and the tangent to the bubble at the circle of contact be-

Jan 1, 1951

By F. J. Haller

IN 1943, we found, in the new Mather operation, a very unusual and disappointing condition in the footwall rock where all of our main haulageways were to be located. With the exception of a few hundred feet out of the thousands then planned and since driven, all of the openings require support. In general, the ground is not particularly heavy, at least by our standards, but it must be supported and the back carefully covered. Also, our operations require rather wide plat openings (16 to 18 ft) and rather flat curves at the turn-outs, all of which adds to the problem. When this completely unforeseen condition was discovered, ordinary timbering was the only answer, because of the impossibility of obtaining adequate steel supplies in time due to war shortages. Then by the time steel supplies were obtained and a practice developed, we found ourselves with between four and five miles of main haulage drifts and plat openings of a permanent nature, all of which were supported by hardwood timber, some of which had already rotted to an unsafe degree. Also, our drifting program was adding some two miles per year to the above figure. F. J. HALLER, Member AIME, is Superintendent, Mather Mine, Cleveland-Cliffs Iron Co., Ishpeming, Mich. AIME Columbus Meeting, September 1949. TP 2840 A. Discussion (2 copies) may be sent to Transactions AIME before May 31, 1950. Manuscript received Aug. 22, 1949. Revision received Jan. 17, 1950. To give all of the details of our experiments, studies, and experiences would fill a large book, but we were satisfied that our organization had done an excellent job, starting from scratch. You can appreciate our surprise when we discovered that we had added very little to an existing record. Attention was called to a footnote in a copy of "Carnegie Pocket Companion" year 1923. The note read: "Full information as to uses of H-Beams is given in pamphlet entitled &apos;Steel Mine Timbers.&apos; " A search of our Engineering Library brought to light a pamphlet printed in 1911 showing extensive use of steel for this purpose. Except for welding in place of riveting, we have added very little to the designs in that book. We have, however, developed an experience which proves, at least to our own satisfaction, that steel mine supports pay off under the proper conditions. We are now convinced, in spite of the relatively high initial cost of materials, that steel sets, because of comparatively low installation cost, are actually cheaper than either treated or untreated wood sets, if they are properly designed and adapted. Several Sections in Use: Convenience guided our first experiments in steel sets, since for a number of years, we had used the 4-in. WF, 10 lb per ft section in 10-ft lengths as safety forepoles along with wood forepoles. This section replaced the 40-lb rail which had formerly been used for the purpose. Having the 4-in. WF sections on hand, it was natural that our first experiments in steel sets involved their use. Later, the rolling of the 10-lb section was discontinued in favor of the much stronger 13-lb section, which is now standard for both legs and caps in areas of no particular weight, but which, none the less, require permanent support. Our experiments involved the use of the 10- and 13-lb sections as legs and 6- and 8-in. I beams, 16 and 23 lb per ft, respectively, as caps. Experience soon indicated that, if the ground were heavy enough, and the opening wide enough to require a cap stronger than 13-lb, the 8-in, 23-lb should be used, eliminating the 6-in. I beam. We now know that the 8-in. WF section of the same weight, which we propose to use in the future, is considerably stronger for the amount of money involved. Comparative Strengths: Tables I to IV giving strengths of several species of timbers as compared with the structural sections that we now use have been prepared in accordance with accepted practice. Experience indicates that failure due to compression perpendicular to the grain of the wood does not destroy the effectiveness of a wood set frequently enough to be a practical factor. Therefore, no table of these values is included.

Jan 1, 1951

By B. H. Caudle, R. L. Slobod, E. R. Brownscombe

An earlier publication has discussed three methods lor obtaining relative permeability data on small core sample-: and the apparatus and technique for the capillary pressure displacement method. This paper describes the apparatus and technique for the solution gas and the dynamic displacement methods and presents a routine procedure for obtaining oil-gas and water-oil relative permeability data. Theoretical and experimental considerations are presented to show that the end effect commonly associated with the dynamic flow mechanism is extremely small where constant rates are employed in the flowing phase. An effect of flow rate on relative permeabilities obtained by the dynamic system is found only when gas is one of the flowing phases and this effect is ascribed to a form of channeling in the capillary system. The apparatus and procedure* used to obtain relative permeability data with three phases flowing are described and some preliminary results of the use of this method are shown. INTRODUCTION In a previous publication from this laboratory there appeared a brief discussion of the concepts behind three basic methods for obtaining relative permeability data.&apos; These three methods were called the capillary pressure displacement method. the solution gas displacement method, and the dy. namic displacement method — the names being suggestive of the type of process used for obtaining the desired saturation prior to making the permeability measurements. In the same publication, the apparatus and technique for the capillary pressure displacement method were described and some typical results obtained by this method were presented. This paper will present: 1. The routine procedure used to obtain complete relative permeabilitv data (In small core samples with two phasec flowing; 2. The experimental techniques for the solution gas and dynamic displacement methods for obtaining relative permeability data; 3. The results of some studies on the mechanism of fluid flow through consolidated porous media; and, 4. The preliminary results on the determination of relative permeability for a system in which three phases are flowing. TECHNIQUE AND APPARATUS FOR THE DETERMINATION OF RELATIVE PERMEABILITY WITH TWO PHASES FLOWING In order to obtain relative permeability data on a small core sample which will describe the various phases of reservoir depletion. it is necessary that the methods used duplicate, as closely as possible, the various mechanisms involved in rescbrvoir depletion. It is important that. in any type of relative permedbility determination. the core be originally at virgin reservoir conditions with respect to the fluids within the pore *paces. (for example. oil used to displace water from core until connate water saturation estahlished). and that the subsequent saturation changes in the core be analagous to tile reservoir depletion mechanism for which the data are to he used. PROCEDURE OF DETERMINING RELATIVE PERMEABILITY DATA WITH TWO PHASES FLOWING A standardized procedure has been set up for obtaining relative permeability data and other information on small core samples. This procedure essentially consists of 11 steps as shown below: 1. Determination of tile capillary pressure curve.&apos;! This information is used to help select samples for relative permeability determinations and to charactrrize. in general. the pore size distribution of the sample. 2. Determination of the specific permeabilities to air, oil. and water. These values are those on which the relative pern~eahility calculations are based. 3. Reduction of the core to connate water by an oil drive using the high speed centrifuge. 1. Determination of the critical gas saturation value and the associated relative permeability to oil by the solution gas drive method. 5. Determination of the relative permeabilities to oil and gab in the region where both phases are flowing by the capillary presqure method. 6. Reduction of the sample to residual oil in the centrifuge by an air drive. and the determination of the relative permeability to gas at this point.

Jan 1, 1951

By D. B Kibler

The Florida hard-rock field extends from Suwanee and Columbia Counties in northwest Florida to south of Croom, Florida, in Hernando County. This area is approximately 100 miles long and varies from 2 to 30 miles in width. Florida hard-rock phosphate was discovered at Hale Springs, about one mile northwest of the town of Dunnellon, Marion County, in the year 1888, by Alber-tus Voight, who lived within a few hundred yards of the spring. Soon after this discovery there was a great influx of land speculators and wildcat operators into the vicinity of Dunnellon. A few years later phosphate was found in Alachua, Levy, Citrus and Hernando Counties, and a great number of small crude plants were built from Newberry, Alachua County, all the way to Croom, Hernando County. Phosphate was found in many places as "outcrops." Looking for outcrops was the first method used by the early prospectors in searching for deposits. Several years passed before any systematic method of prospecting was used. Early Mining The early method of mining hard-rock phosphate was with picks and shovels, wheelbarrows, mules and wagons. The pick-and-shovel method was used altogether until about 1900, when some of the larger operators began to use railroad-type steam shovels of from ½ to I-yd. capacity Picks and shovels, with negro labor loading the phosphate ore (called "matrix") into wooden side-dump skip-cars, was continued until about 1907. From the discovery of hard-rock phosphate until approximately 1905, overburden was removed with mules and scrapers. At some places, the overburden was loaded into side-dump skip-cars by negro laborers and the cars were then pulled up an incline with a steam hoisting engine. The maximum depth of overburden that could be economically removed by hand labor, mules and scrapers was approximately 15 feet. About 1905 one of the companies erected a producer-gas power- I house near Dunnellon and generated its own electricity and about the same time the larger companies began using hydraulic methods for the removal of overburden. From the year 1888 through the year 1939 approximately 75 companies were operating at one time or another in the hard-rock territory, on approximately 500 locations. The hard-rock deposits are more irregular and have higher mining costs than the pebble-rock deposits, therefore 1 they have not been competitive in the domestic market, but because of the higher grade of the hard rock it is in demand for I the export trade. Discovery of phosphate outside of the United States has made it increasingly difficult in recent years for the hard-rock companies to survive, so today i only three companies are operating. These

Jan 1, 1942

By M. E. True, B. L. Stone

To cope with the problems encountered when drilling at greater depths and to reduce the amount of physical effort required on the part of drilling crews in making round trips, a new type of semiautomatic power-operated drilling machinery has been developed which permits round trips to be made without the drill pipe being touched by hand. This equipment consists of hy-draulically operated tongs which perform the stabbing, spinning, and tong-ing operations, and two power-operated racking units mounted in the derrick for carrying the pipe to and from the center of the hole and positioning it on the mat and in the rack. With this equipment all of the operations of the various units are controlled remotely by manipulation of hydraulic valve levers and electric switches. INTRODUCTION As horsepower rises to meet the demand for deeper drilling, it is necessary to increase the weight of surface drilling equipment. Also, the duration of repetitive operations in making round trips to change bits is greatly increased with depth. Harder formations encountered at greater depths reduce bit life rapidly, resulting in more frequent round trips and in some instances more time is consumed in changing bits than in drilling. Since the introduction of the first rotary employed to drill for oil in 18951, there has been relatively little change in the general procedure for making up, breaking out, stabbing, and racking drill pipe in making round trips to change bits. The conventional method of making round trips with the drill pipe requires that drilling crews lend strenuous physical assistance to manually operated tools. Although many new devices have been developed to improve efficiency, increase speed of making round trips, improve safety, and reduce the amount of physical effort required in handling drill pipe, it is considered a vital necessity to substitute automatic or semiautomatic power-operated machinery for many of our more or less manual operations if extremely deep drilling is to be carried out successfully on a production basis in the same manner as our shallower drilling of today. Field tests have been made of remotely controlled power-operated tongs, spinner, stabber, and racking equipment. The tongs, which include a built-in pipe spinner, are mounted on a column, are capable of gripping and supporting the weight of a 90-foot stand of drill pipe, and are provided with means for moving the pipe vertically as well as to and from the center of the hole. The racking equipment consists of two units, one at the level of the conventional monkey board and the other at the first girth on the ladder side of the derrick. Most of the physical effort of making round trips with drill pipe has been eliminated in that all of the operations of tonging, spinning, stabbing, and racking of pipe on the floor are controlled by an operator in a seated position by manipulation of hydraulic and electric valve levers and buttons. The driller is relieved of operating the cathead, leaving only the hoisting and slips to be controlled. Complete round trips are made without the drill pipe being touched by the drilling crews. Although the speed of pulling or running a single stand with the power-operated equipment is approximately the same as that with conventional equipment, it is possible to maintain this rate for long periods, whereas fatigue slows crews working conventionally during round trips, especially under adverse weather. After completing round trips with this equipment, drilling crews are not exhausted, consequently, are able to perform effectively their duties while drilling, which is essential for maximum over-all efficiency. Safety is substantially improved as the derrickman performs his duties from a platform enclosed by rails and the tong lines and spinning chain are eliminated from the derrick floor. The hazards encountered in racking drill pipe on the floor and in stabbing are also eliminated. Figure 1 shows a drawing of a derrick equipped with the power-operated drill&apos;pipe handling equipment.

Jan 1, 1949

By I. W. Walling, F. B. Plummer

Bastin and others have demonstrated the presence of sulphate-reducing bacteria in oil wells producing salt water. Analyses show that at 125°F. bacteria alone reduce sulphates in East Texas salt water by only 3 per cent in 30 days, forming principally hydrogen sulphide and sodium or calcium hydroxide. The hydrogen sulphide reacts with soluble iron compounds to produce iron sulphide in the absence of oxygen, and ferric hydroxide where oxygen and air are present. Where iron or other metals and iron sulphide are already in the water containing bacteria, I00 per cent reduction of the sulphates is complete in 30 days or less; where magnesium is present, reduction is complete in 15 days. The effects of changes in temperature, of different bactericides, and of concentration of bactericides on sulphate reduction are described in detail and illustrated by tables and curves. The significance of sulphate reduction on corrosive properties of oil-field water is briefly discussed. Chemistry of East Texas Oil-field Water The chemical composition of the water in the East Texas field salt-water disposal pits is shown in Table I. This salt water corrodes pipes, pumps, and steel tanks excessively, principally because of its content of oxygen, hydrogen, sulphide, and carbonic acid. The carbonates in the water when exposed to air tend to give up carbon dioxide and to precipitate calcium carbonate in large quantities. This forms coatings in tanks, settling pits, and ditches, and soon, unless removed by acid treatment, will effectively clog an injection well and reduce the flow of water back into the ground. The iron compounds in the water, most of which are dissolved from tanks and pipes, are in the ferrous form, and when exposed to the air are oxidized from soluble ferrous carbonate to insoluble ferric hydroxide, resulting in the precipitation of a gelatinous precipitate that will clog oil-field sands effectively: 2Fe(HCO3)2 + O + H2O -> 2Fe(OH)3 + 4CO2 The sulphates in strong sulphate-bearing water may be attacked by swarms of sulphate-reducing bacteria and more hydrogen sulphide may be produced. The hydrogen sulphide reacts with soluble minerals in the water to form black sludges. A knowledge of the chemistry of each reaction in oil-field water is important to the oil-field engineer, since means must be devised to prevent the formation of harmful precipitates that clog injection wells and to prevent corrosion of tanks by harmful products of biochemical processes. Methods of Treating Water before Injection into Ground* The open system of handling the waste salt water in the East Texas field consists of aerating and chemically treating the water to precipitate the unstable iron,

Jan 1, 1946

By Tibor Stefansky, John E. Dorn

MOTT and Nabarro1-5 were first to illustrate the importance of the flexibility of dislocations in accounting for the strengthening that metals undergo due to the presence of internal-strain centers. Such strain-centers might arise from a number of causes such as radiation damage, the presence of semicoherent and coherent precipitates and clusters, as well as individually dispersed interstitial and misfit substitutional solute atoms. Each strain-center induces positive and negative shear stress fields on the slip planes of the surrounding alloy matrix. In order to effect plastic deformation, therefore, the alloy must be subjected to sufficiently high applied shear stresses to push dislocations past all such internal stress fields. If dislocations were inflexible and moved as rigid lines, they would be equally pushed and pulled by internal stress fields. At this extreme the strengthening would be vanishingly small. Dislocations, however, are not rigid; they are flexible and extensible. They wiggle between positive and negative strain-centers, thus increasing their line energy at the expense of their interaction energy with strain-centers. cottrel16 and Friedel7,8 have independently presented lucid reviews of the significance of the Mott-Nabarro dislocation-flexibility concept to the strain-center strengthening of alloys. Their analyses however were only semi-quantitative. There is evidence in the recent literature of renewed interest in a more rigorous analysis of flexibility. Thus, Gleiter9 and Gerald" have shown that the calculated strain-energy interaction between a dislocation and the stress fields of coherent precipitates can be seriously in error if the flexibility of the dislocation is not taken into account. This report will be concerned with a more detailed analysis of the problem based on the following approximations: 1) Although many types of strain-centers exist, the following analysis will be limited to the case of solute-atom strain-centers in fcc substitutional alloys. 2) To facilitate the analysis by avoiding statistical considerations, the strain-Centers are assumed to be in regular arrays on the slip plane. Although the quantitative results are somewhat dependent on the type of array that is assumed, the qualitative trends are similar for various arrays that were studied. 3) An adjustment of the results from those for square arrays to those for the more realistic case of a random distribution of strain-centers is accomplished by adopting the interesting statistical theory first introduced by Kochs,11,12 elaborated on by Dorn, Guyot, and stefansky,13 and analyzed by Foreman and Makin14 in their computerized experiments. 4) For simplicity the dislocation lines are taken to wiggle about their edge orientation and no correction is applied to their line energy for deviations from edge configurations or for the elastic interaction between segments of the now curved dislocation. It will be shown that for extremely low concentrations of atomic strain-centers the strengthening increases with the square root of their concentration. For slightly higher concentrations the strengthening rate becomes less rapid. At a critical concentration a maximum strength is obtained and a decrease in the strengthening takes place as the concentration of solute atoms is further increased. These trends are a direct consequence of dislocation flexibility. They arise from changes in the amplitude of the waviness of the dislocation line at the yield stress with solute atom concentration. Despite the simplifying assumptions that were made, the results agree qualitatively with appropriate experimental data. I) STRESS FIELDS ON SLIP PLANES Internal stresses are introduced in a lattice whenever a host atom of radius ro is replaced by another that has a different atomic radius. According to the classical theory of linear elasticity,15 the stress field about a solute atom at the origin of a spherical coordinate system is given by arr=-4G€(?_0)3 ffflfl ="W =2G€{t) f°rr^ro(l+e) UJ where G is the shear modulus of elasticity and Y, = ro(l + E) is the radius in situ, of the substituted atom. As shown by ~shelb~,&apos;~ this approximation assumes that the bulk modulus of elasticity of the substituted atom is identical with that of the host species. ~abarro&apos;~ suggested that the strain E can be deduced

Jan 1, 1970

By Jeff Steinhoff

INTRODUCTION The Henderson mine utilizes a highly mechanized, continuous, panel-caving, mining system to extract ore from a deep, massive, molybdenite deposit. The mine is located 80.5 km (50 miles) west of Denver, Colorado. The mine surface facilities are located 3,170 m (10,400 feet) above sea level in a steep valley on the eastern side of the Continental Divide. Milling facilities are 24 km (15 miles) west on the western side of the divide at an elevation of 2,804 m (9,200 feet) above sea level. The ore- body is located approximately 3,000 feet south of the valley under Red Mountain. Access to the ore for men and materials is through a 915 m (3,000-foot) deep, 8.5 m (28-foot) diameter, vertical, concrete-lined, service shaft. Access from the mill is through a 15.5 km (9.6-mile) rail haulage tunnel. The mine is ventilated through an additional intake shaft and two exhaust shafts. Mine production at this time is 27,255 mtpd (30,000 stpd). The mine ventilation system supplies 1,038 cubic meters per second (2.2 million cfm) through approximately 60 miles of drifting or 2.7 tons of air per ton of ore mined. There are 130 fans in the mine in fixed locations and in vent lines with 6,900 connected horsepower in the mine. MINING METHOD AND LAYOUT The orebody is divided vertically into two major zones. The upper zone is the 8100-level production area. The bottom zone is the 7700- level production area which is in the early development stage. The rail haulage level at 7500 feet is common to both production zones. Each mine production zone consists of five associated sublevels. The cave undercut level is 16.8 m (55 feet) above the production level. Two boundary cutoff levels are located 44.2 m (145 feet) and 62.5 m (205 feet) respectively above the production level. The fresh-air level is positioned 15.2 m (50 feet) below the production level, and the exhaust vent level is 19.8 m (65 feet) below the production level. Horizontally, each production zone is divided into three panels each, 224 m (800 feet) wide. These panels are caved from south to north. As the caving in one panel nears completion, caving in the adjacent panel is initiated. Development for the caving panels is continuous so that the sublevels above the production level and the production level itself have a combination of development drifting and production-related activities. UNDERGROUND VENTILATION NETWORK The ventilation system is zoned in the same manner as the orebody itself. One major split of 600 cubic meters per second (1,270,000 cfm) ventilates the 8100-level production zone; one split of 100 cubic meters per second (210,000 cfm) ventilates the development of the 7700- level production zone; and one split of 165 cubic meters per second (350,000 cfm) ventilates the 7500 rail haulage level. The haulage tunnel requires an additional 188 cubic meters per second (400,000 cfm) of air. Development-drift ventilation is accomplished by hanging 1.0 m (3.5-foot) diameter steel ducting in the drifts with 40-horsepower, 0.96 m (38-inch) diameter fans supplying 9.4 cubic meters per second (20.000 cfm). The normal maximum length for these systems is 300 m (1,000 feet). The 8100-level production-area ventilation system is especially suited to a high level of mucking activity confined in a small area. Approximately 93 per cent of the mine&apos;s total production is transferred from the drawpoints to ore passes in 10 production drifts. The active area in each drift is 300 m (1,000 feet). Twelve 5-cubic-yard LHD units with Cat turbo- charged 170-horsepower engines are assigned to the area. Under these conditions, more than one LHD is assigned to a particular production drift. Adequate ventilation is maintained by making an air change every 97 m (320 feet) along the production drifts. Fresh air is brought into the production drifts from the fresh-air level through 1.37 m (4.5-foot) diameter raises. Air travels south along the production drift to the ore pass where it is exhausted down the ore pass to the exhaust level. The ore pass is followed by another intake which is followed by an ore-pass exhaust. At the south end of the production area, a series of exhaust fans maintain a southerly air- flow through the production level.

Jan 1, 1981

R. Schuhmann, Jr. (Purdue University)— Fulton and Chipman&apos;s results on rate of silica reduction from slags are analogous in many was to the results of Parlee, Seagle, and Schuhmann10 on rate of alumina reduction from alumina crucibles. Both investigations have given comparably low rates of reduction and slow approaches to equilibrium. Accordingly, we may hypothesize that the rate-determining step is the same in both kinds of experiments; that is, oxygen diffusion across the stagnant boundary layer on the liquid-metal side of the interface between the liquid metal and the oxide phase (slag or solid oxide). I suggest that silica reduction involves the following consecutive steps: I) At the slag-metal interface: SiO2(slag) Si+ 20 II) Transport of oxygen from slag-metal to gas-metal interface: a) diffusion across liquid-metal boundary layer at slag-metal interface. b) convection within the body of liquid metal. c) diffusion across boundary layer at metal-gas interface. 111) At the metal-gas interface: C +O- CO (gas) Iv) At the graphite-metal interface: C (graphite) -C At steelmaking temperatures it is reasonable to assume that equilibrium is attained in all three chemical reactions (I, 111, and IV) right at the respective interfaces. Convection within the stirred liquid metal (step IIb) is also rapid. Transport of Si and C should be orders of magnitude easier than transport of 0, because of the relatively high concentrations of Si and C. Accordingly, we might expect the overall reaction rate to be determined by boundary-layer diffusion of oxygen, either IIa or IIc. Fulton and Chipman&apos;s demonstration that bubbling CO through the system had no major effect on reaction rate indicates that IIc is not the slowest step. Therefore, it becomes logical to estimate the maximum rate for step IIa and to compare this theoretical estimate with Fulton and Chipman&apos;s experimental data. If oxygen diffusion across the liquid metal boundary layer at the slag metal interface (step IIa) is rate-determining, In this equation, dn sio, /dt is the rate of silica reduction in moles per sec,A is the area of slag-metal interface in sq cm, Do is the diffusivity of oxygen in sq cm per sec, 6, is the boundary layer thickness in cm, c,* is the oxygen concentration right at the slag-metal interface in moles per cubic cm, and co is the oxygen concentration in the body of the liquid metal, also in moles per cubic cm. Equilibrium data" on the silicon deoxidation reaction in liquid iron and steel at 1600°C indicate that the oxygen contents of the liquid metal in Fulton and Chipman&apos;s experiments at 1600°C probably fell in the range of 0.5 x10-3 x10-3wt pct. That is, the maximum conceivable value of co*-co for the system under consideration was on the order of 10"5 mole oxygen per cubic cm. On the basis of previously published data,1O,11 it is estimated that Do/0 will fall somewhere in the range from 10-3 to 10-1 cm per sec. The surface area A in Fulton and Chipman&apos;s experiments was approximately 20 sq cm, and the weight of metal involved was about 500 grams. Combination of all these figures with the above rate equation leads to an estimate that the rate of silica reduction should fall within the range from 0.002 to 0.2 wt pct Si per hr. This estimate is consistent with the experimental data. For example, Fulton and Chipman&apos;s Fig. 2 shows a change of about 0.3 pct Si in 10 hr, corresponding to an average rate of 0.03 pct per hr. According to the proposed hypothesis, increasing the temperature will increase the reaction rate ill two ways: 1) by increasing oxygen diffusivity and 2) by increasing the oxygen concentration (oxygen solubility) in the liquid metal. The combination of these two effects accounts for the high value of the observed activation energy. Summarizing, I propose that the rate of silica reduction, like that of the carbon-oxygen reaction, is diffusion controlled and that low oxygen concentration in the liquid metal is the major factor accounting for the very low observed rates of silica reduction. John Chipman (author&apos;s reply)—The authors thank Professor Schuhmann for his interesting contribution. His proposed explanation may well prove to be the correct one. There is clearly a need for much further experimental work on this problem, and further research is in progress.

Jan 1, 1961

By K. H. Coats

This paper presents the development and solution of a mathematical model for aquifer water movement about bottom-water-drive reservoirs. Pressure gradients in the vertical direction due to router flow are taken into account. A vertical permeability equal to a fraction of the horizontal permeability is also included in the model. The solution is given in the form of a dimensionless pressure-drop quantity tabulated as a function of dimensionless time. This quantity can be used in given equations to compute reservoir pressure from a known water-influx rate, to predict water-influx rate (or cumulative amount) from a reservoir-pressure schedule or to predict gas reservoir pressure and pore-volume performance from a given gas-in-place schedule. The model is applied in example problems to gas-storage reservoirs, and the difference between reservoir performances predicted by the thick sand model of this paper and the horizontal, radial-flow model is shown to be appreciable. INTRODUCTION The calculation of aquifer water movement into or out of oil and gas reservoirs situated on aquifers is important in pressure maintenance studies, material-balance and well-flooding calculations. In gas storage operations, a knowledge of the water movemenr is especially important in predicting pressure and pore-volume behavior. Throughout this paper the term "pore volume" denotes volume occupied by the reservoir fluid, while the term "flow model" refers to the idealized or mathematical representation of water flow in the reservoir-aquifer system. The prediction of water movement requires selection of a flow model for the reservoir-aquifer system. A physically reasonable flow model treated in detail to date is the radial-flow model considered by van Everdingen and Hurst.1 In many cases the reservoir is situated on top of the aquifer with a continuous horizontal interface between reservoir fluid and aquifer water and with a significant depth of aquifer underlying the reservoir. In these cases, bottom-water drive will occur, and a three-dimensional model accounting for the pressure gradient and water flow in the vertical direction should be employed. This paper treats such a model in detail — from the description of the model through formulation of the governing partial differential equation to solution of the equation and preparation of tables giving dimensionless pressure drop as a function of dimensionless time. The model rigorously accounts for the practical case of a vertical permeability equal to some fraction of the horizontal permeability. The pressure-drop values can be used in given equations to predict reservoir pressure from a known water-influx rate or to predict water-influx rate (or cumulative amount) when the reservoir pressure is known. The inclusion of gravity in this analysis is actually trivial since gravity has virtually no efFect on the flow of a homogeneous, slightly compressible fluid in a fixed-boundary system subject to the boundary conditions imposed in this study. Thus, if the acceleration of gravity is set equal to zero in the following equations, the final result is unchanged. The pressure distribution is altered by inclusion of gravity in the analysis, but only by the time-constant hydrostatic head. The equations developed are applied in an example case study to predict the pressure and pore-volume behavior of a gas storage reservoir. The prediction of reservoir performance based on the bottom-water-drive model is shown to differ significantly from that based on van Everdingen and Hurst&apos;s horizontal-flow model. DESCRIPTION OF FLOW MODEL The edge-water-drive flow model treated by van Everdingen and Hurst1 is shown in Fig. la. The aquifer thickness b is small in relation to reservoir radius rb. water invades or recedes from the field at the latter&apos;s edges, and only horizontal radial flow is considered as shown in Fig. 1b. The bottom-water-drive reservoir-aquifer system treated herein is sketched in Fig. 2a and 2b. Here the aquifer

By F. W. Jessen, R. W. Durie

The development in the laboratory of mall salt cavities illustrated that the rate at which salt dissolved was affected by the rate at which fresh water was injected into the cavity. Experiments carried out with small salt cores indicated, however, that the rate of salt removal with forced convection was not significantly different from that with natural convection, provided the flow was in the laminar range. The rate of salt removal was apparently controlled by the water salinity, which was indirectly determined by the rate at which fresh water was injected. With turbulent flow at the salt surface, the rate of salt removal could be increased several-fold with the same salinity in the cavity. A quantitative evaluation of the rate of salt removal under natural convection was attempted by using techniques developed for the analogous heat convection system. The values of the rate of salt removal obtained experimentally were considerably greater than the calculated values due to surface irregularities. To determine the effect of these irregularities, the rate of salt removal was found for a smooth surface by experimentally determining the rate of salt removal as an irregular surface developed and then extrapolating this trend back to initial time. Excellent agreement between the experimental and calculated values then were obtained. INTRODUCTION Underground cavities leached from massive salt formations have been used extensively for many years for storing LPG products. The development techniques for storing methane gases in the liquid state at a low temperature leads to speculation that underground salt cavities of controlled geometry may be quite important in this field. In any case, the increasing number of salt cavities used for storage indicates an impending need for a better knowledge of the washing process to efficiently develop maximum storage volumes within specified regions. It is the purpose of this paper to discuss some aspects of -the mechanism of the dissolution of salt in the formation of cavities of controlled geometry. Although no attempt is made to resolve the problems that may be associated with the storage of methane in the liquid state in salt formations, the fact that salt cavities can be formed at reasonable cost would appear to justify investigation in this direction. Further, underground cavities have the advantage of allowing storage at higher pressures (and hence higher temperatures) than surface installations. Although the thermal conductivity of salt is somewhat higher than frozen earths, 0.017 cal/(sec) (cm)(c) for salt at 32F vs 0.005 cal/(sec) (cm) () for ice at this temperature, this disadvantage is offset by the higher storage temperature in underground cavities. For example, at atmospheric pressure, the temperature of liquid methane would be —258F. In a storage cavity at 2,000 ft, the pressure would be approximately 1,000 psia, which would allow a storage temperature of -9OF. The formation temperature would be roughly 110F at this depth, hence the total temperature differential would be 200F. Under surface storage conditions the corresponding temperature difference would be some 333 F (75 F + 258 F). The results of this difference can be compared more readily by substituting the appropriate values of thermal conductivity, temperature difference, heat capacity and density into the solution of the diffusion equation for the unsteady linear conduction of heat. For the underground salt storage, the heat flux is 15cal/(sec) (sq cm), where t is the time in seconds from the initiation of the cooling. For the surface system, and using the thermal properties of ice at the average temperature, the corresponding figure is 21cal/(sec) (sq cm). Hence, the heat losses through ice under surface conditions would be some 30 per cent higher than the underground salt storage. This ratio would vary, considerablv. Of course, for other conditions, but it indicates that an advantage over surface facilities may be obtained by storage in underground salt cavities.

Jan 1, 1965

By R. G. Treuting

Germanium single crystals strained in tension at 600°C slip on the {Ill} plane and, macroscopically at least, in the <110> direction. Deformation is in homogeneous: various localized rotations are observed, as is a banding consistent with secondary slip banding. The structure after deformation is polygonized with a domain size of about 2x1O-3 cm. In relaxation tests, an incubation period prior to flow is observed, of duration inversely related to temperature and applied stress. Under continuous loading, there is a sharp first yield point. A critical resolved shear stress therefore must be cited with respect both to temperature and to rate of loading. At 600°C, when loading proceeds at 2900 psi per min, it is 1310 psi. The yield point phenomenon is suggestive of Cottrell&apos;s solute atom atmosphere theory and five points of qualitative agreement with this theory are found. PLASTICITY of germanium at elevated temperatures has been reported by Gallagher,&apos; who ascribed it to slip on {Ill) planes and described some associated effects. Preliminary experiments with single crystals of silicon and germanium loaded as simple beams confirmed {ill) as the slip plane of both materials.V his was demonstrated by the standard technique employing traces on two surfaces of known angle on a deformed crystal of known orientation.3 These experiments did not fix the slip direction, since more than one glide system operated. Uniaxial tensile straining is preferred for this purpose in order to restrict slip to one predominant system and to provide an unequivocal determination of the orientation change with respect to the stress axis. Experimental Method Specimens were diamond-sawed from germanium crystals containing about 5x10-5 wt pct Sb prepared by the zone-leveling process described by Pfann and Olsen;4 these specimens measured about 81/2 in. long, 0.20 in. wide, and were of various thicknesses from 0.035 to 0.060 in. Prior to testing, a specimen was coated over 1 in. or more of length at each end with Apiezon wax, chemically polished (in a solution of 15 ml HF, 25 ml HNO,, 15 ml CH3COOH, and 3 to 4 drops Br2), and dewaxed in warm xylene. A brief re-etching after scribing through a complete wax coating with vernier dividers provided gage marks at 0.200 in. intervals on the polished surface. A specimen with grips soft soldered to the ends was passed through the furnace tube and the grips pinned to the tensile machine in series with a stress gage. The Schopper testing machine is best described by reference to the illustration on p. 107 of Schmid and Boas5 and is operated with the pendulum arm locked, fixing the upper head. Load is applied through the screw-driven lower head, manually or by reduced speed motor. The furnace is 21/2 in. long surrounding a 4x7/16 in. ID quartz tube and was positioned about the specimen to permit free motion. The inert or reducing atmosphere required was sufficiently provided by a flow of helium introduced at the center of the furnace tube, with the tube ends loosely plugged with asbestos paper. Surface corrosion was slight. The stress gage employs a Be-Cu strip with SR-4 units incorporated in a simple bridge network with provision for balancing and calibrating. The bridge output on loading is fed through a Leeds and North-rup dc amplifier to a Speedomax 10 mv recorder, and calibration is obtained by dead loading. Experiments of two types have been conducted. Most have been in relaxation at constant elongation. One stress-strain curve has been taken with the machine continuously driven. Following extension of a specimen, Laue X-ray photographs were taken to obtain the orientation change between deformed and undeformed regions, recorded on a single film by translating the specimen in a plane normal to the beam between exposures. Sequences of such multiple exposures were made on some specimens to include the entire orientation range on one film. Slip Direction To obtain a maximum orientation change with a single slip system, crystals of very closely <110> axial orientation were used. The classic determination of slip direction rests on establishing that direc-

Jan 1, 1956

By R. I. Jaffee, F. C. Holden, H. R. Ogden

ECENT papers dealing with the properties of unalloyed iodide titanium have been directed primarily at the determination of base-line properties for alloy investigations. Early work was limited to a few tests because of the limited availability of iodide titanium at the time. In the results of papers by Campbell et al.,1 Gonser and Litton,2 Jaffee and Campbell,3 inlay and Snyder,4 and Jaffee, Ogden, and Maykuth, data on mechanical properties are presented for unalloyed iodide titanium in the annealed and cold-worked conditions. Data are presented in this paper which show the effects of heat treatment on the structure and mechanical properties of commercially produced iodide titanium. Correlation is made between microstruc-tural variables and the mechanical properties. Experimental Procedures Melting Stock: The melting stock used was as-deposited iodide titanium, produced by New Jersey Zinc Co. The furnished analysis showed the following range of impurities: N, 0.004 to 0.008 pct; Mn, 0.005 to 0.013; Fe, 0.0035 to 0.025; Al, 0.013 to 0.015; Mo, 0.0015; Pb, 0.0045 to 0.0065; Cu, 0.0015 to 0.002; Sn, 0.001 to 0.01; Mg, 0.0015 to 0.002; and Ni, 0.003. Hydrogen content as determined by vacuum-fusion analysis was 0.0091 wt pct (0.44 atomic pct) after arc melting and fabrication. Nitrogen analysis on the arc-melted and fabricated titanium showed a content of less than 0.002 pct N. The average hardness of the furnished stock was Rf 70, or approximately 85 VHN. Melting Procedure: The as-deposited rods were rolled, sheared, and degreased in preparation for arc melting. The charge was arc-melted with a tungsten electrode in a water-cooled copper crucible under a positive pressure of high purity (99.96 pct) argon. The final ingot was approximately 2 in. in diameter and showed no increase in hardness over that of the initial stock. Fabrication: Heating for fabrication was done in air. It was begun by forging the ingot into a 3/4 in. diam rod, at an initial temperature of 1600°F. Scale was removed by sandblasting. The rod was then swaged to 1/4 in. diam at room temperature through a series of 20 dies, with approximately 10 pct reduction in area between each die. An anneal of 1 hr at 850 °C in air was given after the 1/2 in. die, such that the final cold reduction was 75 pct. Sections cut from this rod were used for test and microstructure specimens. Heat Treatment: Heat treatments were carried out in resistance tube furnaces with stainless-steel linings, under an atmosphere of gettered argon. As further protection against contamination, the specimens were packed in titanium turnings in a titanium sleeve. Control experiments have shown negligible hardness increases with this method, indicating that contamination from oxygen and nitrogen is slight. Three cooling rates were employed in this work; these have been designated as water quenching, argon cooling (to simulate air cooling under a controlled atmosphere), and furnace cooling. The cooling rate for an argon cool is 100°C per min for the first minute, with an average cooling rate of 35°C per min over a 15-min period. A furnace cool requires about 10 hr, with an average cooling rate of 3.6oC per min during the first hour, and an average cooling rate of 1.2°C per min over the 10-hr period. Microimpact Test: The specimen adopted was based on the cylindrical Izod Type Y specimen (ASTM, E23-41T). All dimensions were reduced to half scale, including the notch radius. Specifications are shown in Fig. 1. The specimen is held vertically in an adapter and broken as a cantilever beam. Impact tests were run on a constant-velocity (11.34 ft per sec) Tinius Olsen impact testing machine with a total available energy of 100 in.-lb. Tests were made to determine the correlation between this microimpact and the standard V-notch Charpy impact test. Curves showing impact energy as a function of temperature for both impact tests are plotted in Fig. 2. Transition temperatures, when they occur, are about the same for both impact tests. All three titanium-rich materials have the same conversion factor, 10. Tensile Testing: Tensile tests were conducted on Baldwin-Southwark testing machines using the 600, 2400, or 3000 1b range. Specifications for the test specimen were taken from the 1948 edition of the ASM Metals Handbook, and are shown in Fig. 1. Strain measurements were made using an SR-4 resistance gage (Type A-7) cemented to the reduced section in conjunction with a lever-type extenso-meter. Readings on the SR-4 strain indicator were

Jan 1, 1954

By R. H. Hopkins, R. W. Kraft

X-ray and metallographic analysis reveal that the preferred cryslallograPhic relationships in direc-tionally solid~fied Pb-Sn eutectic specimens can be stated: interface growth direction, Experiments in which tin single-crystal seeds were used to nucleate the eutectic demonstrate that the normal lamellar structure observed at steady state can be forced to break down initially to a semide-generate structure when the crystallograPhic direction of the tin seed does not lie within the preferred eutectic interface plane. A normal structure eventually develops by preferred grain growth. X-ray topo-graphs and rocking curves substantiate that the perfection of eutectic samples increases as growth proceeds until steady-state conditions prevail. RECENT years have seen substantial progress made in the understanding of eutectic solidification through both intensive theoretical1&apos;&apos; and experimental investigations (see Ref. 7 for a review and extensive bibliography of both aspects). Several important observations concerning the nucleation and growth aspects of binary eutectic solidification have been brought to light. Briefly some of these include the nonrecipro-cal nucleation of one phase upon another,&apos;j9 the tendency for a specific low-index direction of one or both phases of the eutectic to be aligned in the growth direction during unidirectional solidification,&apos;0711 and the production of lamellar microstructures having a preferred interface plane between "11-13 phases. Questions quite naturally arise as to the mechanism by which preferred grain growth evolves during eutectic solidification and what relationships (if any) connect the initial nucleation of one phase upon another with the preferred growth directions and interface planes observed after a few centimeters of growth in many systems. This study was initiated in an attempt to answer these questions. An experiment was devised in which both the nucleation and growth steps in the crystallization of a binary eutectic, Pb-Sn, could be correlated with subsequently developed eutectic morphology and crystallography. This was accomplished by nucleating the eutectic upon a tin single crystal seed and then causing the eutectic to grow from the seed by directional freezing. The morphology of the structures produced in this manner was then monitored metallographically and the orientation relationships and substructural perfection determined by X-ray analysis. The information thus ob- tained was correlated to the growth history of the samples. EXPERIMENTAL DETAILS The eutectic of composition 38.1 wt pct Pb and 61.9 wt pct sn14 was prepared by accurately weighing lead and tin of 99.999+ (from ASARCO and Lytess Metals and Chemicals, respectively), melting in a clean Pyrex beaker under an argon blanket, and casting into the proper crucible for resolidification as described below. Tin seeds were grown by the method of ~halmers," saw-cut, oriented by the Laue method, and soldered to the pull rod of the Czochralski puller. All seeds were given a final electropolishing (to assure the removal of any deformed material from the cutting operation) and acetone degreasing immediately prior to the nucleation experiment in which they were to be used. Eutectic samples were unidirectionally solidified in a horizontal graphite boat1&apos; or by pulling from the melt16 with tin (or graphite) seeds. A flowing argon atmosphere was employed in all experiments and growth rates and temperature gradients, constant for a given run, varied from 2 to 4 cm per hr and 8" to 15°C per cm over the course of all the experi-

Jan 1, 1969