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By J. B. Clark

The oil industry has long recognized the need for increasing well productivity. To meet this need, a process is being developed whereby the producing formation permeability is increased by hydraulically fracturing the formation. The "Hydrafrac" process, as it is now being used, consists of two steps: (1) injecting a viscous liquid containing a granular material, such as sand for a propping agent, under high hydraulic pressure to fracture the formation; (2) causing the viscous liquid to change from a high to a low viscosity so that it may be readily displaced from the formation. To date the process has been used in 32 jobs on 23 wells in 7 fields, resulting in a sustained increase in production in 11 wells. INTRODUCTION Need For Process Although explosives, acidizing, and other methods have long been used, there still exists a need for artificial means of improving the productive ability of oil and gas wells, particularly for wells which produce from formations which do not react readily with acids. This paper discusses the development of a hydraulic fracturing process, "Hydrafrac", which shows distinct promise of increasing production rates from wells producing from any type of formation. The method is also considered applicable to gas and water injection wells, wells used for solution mining of salts and, with some modification, to water wells and sulphur wells. Requirements of Process In considering such a possible process, it appeared that certain requirements must be met. Some of these are as follows: A. The hydraulic fluid selected must be sufficiently viscous that it can be injected into the well at pressure high enough to cause fracturing. B. The hydraulic fluid should carry in suspension a propping agent, such as sand, so that once a fracture is formed, it will be prevented from closing off and the fracture created will remain to serve as a flow channel for oil and gas. C. The fluid should be an oily one rather than a water-base fluid, because the latter would be harmful to many formations. D. After the fracture is made, it is essential that the fracturing fluid be thin enough to flow hack out of the well and not stay in place and plug the crack which it has formed. E. Sufficient pump capacity must be available to inject the fluid faster than it will leak away into the porous rock formation. F. In many instances, formation packers must be used to confine the fracture to the desired level, and to obtain the advantages of multiple fracturing. Development of Process As a necessary step in the development of this process, it was deemed advisable to determine if the Hydrafrac fluids were actually fracturing the formation or whether these special fluids were merely leaking away into the surrounding formation. To determine this, a shallow well, 15 feet deep, was drilled into a hard sandstone. Casing was set, the plug drilled, and the well deepened in the conventional manner. A fracturing fluid dyed a bright red was used to break down the formation. Sand mixed with distinctively colored solids was injected into the well with the fracturing fluid to prop open any fracture made in the formation. A simulated gel breaker solution dyed a bright blue was then pumped into the well to determine if the gel breaker would follow the first solution. The results are shown in Figure 1. It was noted that a fracture was formed about the well bore, that the propping agent was transported back into the break, and that the breaker solution did actually follow the fracturing gel out into the fracture. While it is realized that this shallow well test is probably not exactly equivalent to a deep test, the results were interpreted as being a definite indication of what happens down the hole during a Hydrafrac job. Of interest in this connection is an investigation reported by S. T. Yuster and J. C. Calhoun, Jr.' This study, re~orted after the Hydrafrac work was under way, presents some excellent field data supporting the theory of fracturing a formation with hydraulic pressure. METHOD Steps of Hydrafrcu: Process Figure 2 shows a simplified cross-sectional view of a well treated by one version of the process. The first step, formation breakdown, is done with a viscous fluid, usually consisting of an oil such as crude oil or gasoline, to which has been added a bodying agent. Due to availability and price, war-surplus Napalm has been used in the majority of experiments to date. Napalm is the soap which was used in the war to make "jellied gasoline". The next step consists of breaking down the viscosity of the gel by injecting a gel-breaker solution and then after several hours, putting the well back on production. Figure 3 shows diagram-matically, a typical field hookup. The oil or gasoline is unloaded into the 10 bbl. tank shown on the left rear of the truck. This base fluid is picked up by the mixing pump and pumped through the jet mixer, where the granular soap is added. Next it goes into a small mixing tub, from which the high-pressure pump takes suction. The solution is then pumped into the well. The breaker solution is then taken from an extra tank and is displaced into the well immediately following the gel. When required, additional trucks may

Jan 1, 1949

Two Canadian mining companies, Noranda Mines, Ltd., and Wright-Hargreaves Mines, Ltd., have agreed to buy $500,000 worth of shares each in Anglo-American Exploration Ltd., controllers of thousands of acres of possible oil-rich land in southern Saskatchewan and Manitoba. Samuel Clarence Nickle, Sr., reported as possible president of the newly formed exploration company, said that $20 million in assets have been accumulated by the firm, mainly in the Williston basin in parts of the Dakotas and Montana, aid extending into Southern Manitoba and most of Saskatchewan. The M. A. Hanna Co. reported a record profit for the seventh consecutive year with total 1951 profit reaching $14,081. The company handled a record 16.8 million tons of iron ore in 1951, compared with 14.9 million tons in 1950. The company is also preparing to open four iron ore mines in the Lake Superior district which are expected to produce more than 5 million tons annually by 1954. The company built two new iron ore concentrating plants at Mesabi range mines in 1951,a with a third plant going into, operations soon.

Jan 1, 1952

By James Douglas

I had the good fortune to visit the Stockholm Exposition just before its close in October last, and to get a glimpse of the methods used in Sweden in making the wonderful steel and iron for which its furnaces are so famous. My time and opportunities for observation were limited, but some points which I noted may be worth bringing to the notice of the Institute. The Exposition itself was confined to the natural and artificial products of Scanclinavia, and therefore iron and steel held a very prominent place in it. There was a complete collection of the rocks and ores of the Peninsula made by the Geological Survey; and every iron-mine of note exhibited a glass model of its workings, as well as classified specimens, accompaniecl by thorough analyses of the ores. Another feature of interest was the display of models of the old mining-machinery, in the invention and introduction of which Sweden led the way, and of the old and new surveying-instruments and compasses devised for the exploration of the Swedish iron-ore bodies, all of which are more or less magnetic. The magnetometric collection and exhibit of methods of operation made by Prof. Nordestrijm were supremely instructive. The larger metallurgical works, such as those of the Kopparberg and Sandvik companies, exhibited their wares in separate pavilions, in which crude and manufactured objects were arranged most eflectively and tastefully; while the smaller companies erected in the Industrial Arts Building trophies, every one of which was an object of beauty. One was struck on all sides by the fine asthetic feeling exhibited in the ingenious installation of materials and objects not easily lending themselves to artistic treatment. Hammers, picks and drill-steel were grouped into mural designs which it was a delight to look at.

Jan 1, 1899

By Arthur C. Green

A group of 13 cities situated in Los Angeles and Orange counties in Southern California is engaged in constructing an aqueduct to carry water from the Colorado River at a point near Parker, Arizona, to a distribution point near Riverside, California. The aqueduct will have a total length of approximately 241 miles, and is designed to deliver 1605 cu. ft. of water per second, or a little more than one billion gallons per day. The aqueduct crosses a barren, desert waste and the project includes approximately 91 miles of 16-ft. tunnel. The large amount of tunnel driving that has been done in this country in the past few years has resulted in some remarkable developments in equipment and methods. The building of the Colorado River Aqueduct,, with its 91 miles of tunnels, has called on the best engineering knowledge in the country. New and better equipment has been designed for all phases of the work, and this equipment has been coordinated and adapted to the various conditions with a high degree of efficiency. The result has been that records for tunnel driving have been set under adverse natural conditions that exceed the estimates for progress under good conditions. All of the tunnels in the main aqueduct, except the Valverde and Bernasconi at the western end, have a finished diameter, inside the concrete lining, of 16 ft. Fig. 4 shows a section of the tunnel with the concrete lining in place. Fig. 5 illustrates the finished tunnel in three typical sections. The standard tunnel grade is 3.432 ft. per mile in the 16-ft. tunnels, but the Valverde and Bernasconi tunnels have a steeper grade and a finished diameter of 15 ft. 3 in. The rough bore of the large main aqueduct tunnels averages 12.95 solid cubic yards of material per foot of advance in timbered sections and 10.76 solid cubic yards per foot in unsupported sections. Tunnel Driving While the Conway mucker has been used on tunnel work for years, a larger and more powerful Conway was designed to meet the require-

Jan 1, 1937

By Henry Phelps Howland

During the last decade no topic has created more interest or received more thought among blast-furnace men than coke. One reason for this is, undoubtedly, the remarkable increase in the use of byproduct coke. Formerly our coke was made at a distance from the furnaces and by a distinct organization. There was little cooperation or development possible under these conditions. Today the situation is greatly changed. Much of our coke is made by the organization operating the furnaces and the coke oven is operated with the primary object of obtaining the best results in the blast furnace. The effect of changing the method of coke manufacture, even in some minor detail, is often felt almost immediately at the blast furnace. There naturally results one of the most valuable assets of the byproduct coke oven, i.e., the possibility of increased blast-furnace efficiency due to close observance and correct operation of the ovens. The results are evident, but often it is difficult correctly to account for them. In attacking the solution of a problem of as much importance as why one coke is better than another, there are facts which should be kept clearly in mind. The author hopes, in this paper, to bring out some points relative to the use of carbon in the blast furnace which will be of value in solving this question. GeÜner's Ideal Working Years ago GrÜner made a statement regarding the use of carbon in the blast furnace, which has been very generally accepted by metallurgical and blast-furnace men. I quote this theory as given by Prof. Richards on p. 248 of Metallurgical Calculations: "From the standpoint of the generation of the maximum quantity of heat in the furnace, GrÜner was right in formulating his dietum of the ideal working of a blast furnace, vie.: All the carbon burnt in the furnaee should be first oxidized at the tuyères to CO and all reduction of oxides above the tuyères should be caused by CO, which thus beeomes Co2."

Jan 1, 1917

By Richard P. Rothwell

Though coal has been mined in this country for more than a century, no systematic effort was ever successfully made to ascertain the total amount produced. The production of the Cumberland Basin, Md., and the shipments from the anthracite fields of Pennsylvania, have been placed upon record, thanks to the intelligence and foresight of Mr. C. Slack in the former case, and to the late Mr. B. Bannan in the latter. For some of the years between 1822 and 1842, the production of the Richmond Basin was reported by Mr. R. C. Taylor, but since that date till the author undertook this work it was impossible to obtain any statement of the production of this field. A few of the newer fields, such as that of Mt. Diablo, Cal., have been fully reported, and a few of the newer States have also had this service performed by some intelligent private individuals; but no statistics of coal production have ever been collected either by the State or General Government, if we except the returns for the years 1869—70 of the census report. During the year 1875, by great exertions, I succeeded in obtaining, and July 3d, 1875, gave in the Engineering and Mining Journal what, " though not an accurate statement of our coal production," was " by far the most full and reliable that had ever been published." Though that report showed the production of bituminous coal to be 23,630,094 gross tons, or about six million tons more than had ever before been reported, it was in reality two and a half million tons below the actual output. The more full returns I obtained for 1875 gave many figures for 1874

By Oliver Bowles

SUPERFLUOUS varieties and standards which are meriting the critical scrutiny of the manufactur-ing industry have a special significance in the non-metallic mining industries, where, many of the final or intermediate products are manufactured at the mine or quarry. Such processes of manufacture must be considered an integral part of mining in its broader sense. Improvements may be either elimination or standardization. - The chief requirement of elimi-nation is an agreement between consumers and pro-ducers based on facts deduced from: statistical data. Standardization is much, more complex. Standards .may be established only when a very; thorough knowledge has been gained of the physical and chemical properties of the products, and the requirements of consumers. The activities of the Bureau of Standards are. largely directed toward such determinations. Paving-brick manufacturers, together with highway engineers, representatives of certain engineering socie-ties, and Government bureaus, have agreed that of the 66 styles of paving brick on the market 11 only are, essential and 55 are superfluous. Steps have been taken to reduce the output of -all but the 11 standard types. It is customary for manufacturers of structural slate to prepare it in sizes specified by builders and architects. Thus the material cannot be manufactured in advance and the result is irregular activity of mills, delays in filling orders, etc. To improve this condition, the Structural Slate Co. has issued a series of pamphlets giving complete specifications of structural slate for various purposes. Architects find it so much easier .to, order slate from these sheets that standard sizes are specified in preparing plans for new structures. Slate switchboards are usually manufactured after. the order has been received. One manufacturer claims that 80 per cent. of all switchboards are of standard sizes, and he keeps such sizes in stock. The facility with which orders may be filled from stock, and the improved quality of seasoned switchboards, will undoubtedly influence electrical, companies toward a more uniform standardization in size. Simplicity, could be further attained by the elimination of minor irregularities in .style; for example, in the beveled. edges.

Jan 2, 1922

By Falih Ergunalp

REGULAR production of chrome in Turkey started in 1860 with the operation of the Bursa deposits (5, Fig. I). Others were discovered at Makri, near Fethiye (3, Fig. I). For 33 years Turkey remained the principal source of this mineral. While new discoveries were coming in elsewhere, Turkey's output declined until 1921, as a result of four successive wars, which ruined the economics of the country. In 1927 a revival came with the production of 18,000 tons. In that year the Société Minière de Fethiye was formed. This company now operates mines in the Vilayets of Aydin, Denizli, Burdur and Mentese, and it has reached a maximum production of between 80,000 and 90,000 tons annually. The Turkish output therefore increased from 29,000 tons in 1930 to 55,000 tons in 1931; and to 119,009 tons in 1934. The second phase in the increase in chrome production in Turkey came about in 1935, when the Government decided to reorganize and control the mineral industry of the country according to the principles of "government control" of the present regime. Up to that time the mineral resources of the country had been exploited by private concerns. In 1935, the M.T.A. (Maden Tetkik ve Arama) Institute (Institute of Mining Research and Geological Survey) was established by the Government to do the geological and geophysical survey work and discover new mineral resources for the country. Before the establishment of the M.T.A. Institute, the chief chrome-producing region was Fethiye (3 and 4, Fig. I). As a result of the extensive work of this bureau, many new chrome deposits have been discovered and are now in production. The operational field of the mineral industry was given to Eti Bank, another Government-sponsored and Government-controlled establishment. Eti Bank gradually took over the exploitation of existing mines by purchasing them from privately operated companies. Attention was first given to the Zonguldak collieries and to the different chrome deposits scattered over the country. The Guleman mines (14, Fig. 1) were developed and put in operation in 1936. Since then the bulk of Turkish chrome output has come from this mine, which yields the highest grade ore in the world (averaging 52 per cent Cr2O3). In 1939, the recently discovered chrome deposits to the north of Eskisehir went into production, yielding ore having a Cr2O3 content of 51 to 52 per cent. Today, more than ever, the efforts of both the M.T.A. Institute and the Eti Bank are concentrated on finding new deposits and placing them in operation. There are still many promising regions of the country that merit systematic surveying and prospecting for chrome ores. Thus it is probable that Turkey will continue to make noteworthy progress in chrome output. As the annual chrome production of

Jan 1, 1944

By C. M. Warner

In both the Flat River district of southeast Missouri and the Joplin district of southwest Missouri the lead concentrates are of very high grade, free of arsenic, antimony and bismuth, and contain no gold and very little silver. The general practice in both districts is to smelt the concentrates containing 70 to 85 per cent lead on Scotch hearths, to recover 70 to 85 per cent of the lead, and then smelt in a blast furnace the slag formed in the Scotch hearths to bring the total recovery of lead from lead concentrates to over 97.5 per cent. At the lead smelter of the St. Joseph Lead Co. at Herculaneum, Mo., no Scotch hearths are used. In the other smelters in the district the blast furnace plays a minor role to the Scotch hearth . The concentrates produced from the Flat River district are either table concentrates or flotation concentrates containing: Both types of concentrates are received at Herculaneum in box cars after being sampled. Great care is taken in weighing and sampling of cars of concentrates and in the determination of moisture and lead contents. The concentrates are unloaded into bins by an adaptation of scoop grain unloader. Four men unload and sweep a 40 to 45-ton box car of concentrates in 30 minutes. The same grade of concentrates is received each day and no metal-bearing fluxes are available. The problem is to get as high a recovery as possible as cheaply as possible from the high-grade lead concentrates produced by the company's concentrating mills. Sintering The bulk of the sulphur is removed from the concentrates and the fine concentrate particles are agglomerated by double roasting on typical Dwight and Lloyd sintering machines.

Jan 1, 1937

By C. S. Smith, W. M. Williams

THE quantitative study of grain shape in three dimensions has been a difficult one from the practical standpoint. Experiments on grain shape have usually been based on indirect observations of two-dimensional metallographic samples or on grains separated by intergranular corrosion or fracture. The latter method was used in particular by Deschl in 1919 in observing the shapes of ß-brass grains which had been separated with mercury. The similarity in detail of shape and packing that exists between bubbles in a soap froth and metal grains was noted by Desch who remarks that: "Surface tension has an. important share in determining the form of the crystal grains in a solidifying metal and such grains have a tendency to assume the shape of foam cells." More recently the relation between grain shape and grain growth has been studied by Harker and Parker.' The importance of surface tension forces in determining microstructure has been discussed by Smith," and an analysis of the topologi-cal rules that apply to such structures has been made by the same author.' Biologists have made valuable contributions to the general problem of shape and form in an assembly of space-filling cells subject to surface tension forces. Particular mention must be made of the extensive researches of Lewis5,8 on botanical and anatomical tissues, and Matzke and Nestler,7,8 who have made painstaking studies of bubble shapes in different kinds of foam. The present paper introduces a new method of studying individual grains in particular alloys—a method which may well find use in other metallurgical researches, and which seems also to be applicable in biological problems. Metal Grains in Three Dimensions The individual grains in a piece of metal or the bubbles in a soap froth must satisfy two conditions —they must be in juxtaposition so as to fill space and their interfaces must conform to the laws of surface tension. If a further restriction is imposed, namely, that only one type of polyhedron be used, then the sole possibility is an assembly of "minimal" tetrakaidecahedra," each polyhedron having eight doubly-curved hexagonal faces and six plane quadrilateral faces, the angles between adjacent faces being 120". Such cells could be stacked on a body-centered cubic lattice and would be quite stable. For many years it was believed that soap bubbles actually possessed the shape of this ideal body, and the hypothesis was the starting point for several investigations on the shapes of soap bubbles, biological cells, and metal grains. These investigations have shown, what might have been obvious in the beginning, that if the condition of symmetry is relaxed the tetrakaidecahedron is almost never found. If we retain only the rule that all contacts should be in local surface tension equilibrium and that the assembly should fill space, metal grains may then take a nearly infinite variety of shapes and no single one may be regarded as an archetype. These two conditions, which are fully discussed in one of the previously mentioned papers,' lead us to think of a typical grain in an annealed metal as having the following characteristics: 1—A grain may have any number of faces, but usually between nine and eighteen. The faces (each of which is, of course, shared by two grains in the assembly) may have any number of edges, but usually between four and six. Pentagons are by far the most frequent. 2—In the assembly of grains each edge is shared by three faces and by three grains. Each vertex is a point shared by four grains, six faces, and four

Jan 1, 1953

Bailey, Lewis Newton, Master Engineer, Senior Grade, 4th Regiment, U. S. Engineers, Headquarters Company, died of pneumonia at Camp Merritt, N. J., on April 30, 1918. Baird, Louis, Lieut., Royal Field Artillery, British Army, died on the battlefield in 1915. Ballamy, John H., Capt., 103c1 Engineers, killed in action near Fismes, Aug. 9, 1918. Bowles, Martin F., 2d Lieut., Co. B, 355th Infantry, killed in action, Sept. 3, 1918. Burt, Andrew, died in active service, 1916. Cobeldick, William Morley, Royal Engineers, died from gas poisoning on Oct. 7, 1915. Dougall, Ralph,. 4th University Co., Princess Patricia Regiment, killed in action early in the war. Evans, Alfred Winter, Lieut.-Col., New Zealand Rifle Brigade, D. S. 0., D. C. M., killed in action on Oct. 12, 1917. Gordy, Sheppard B., died in service, Oct. 9, 1918. Gorman, Thomas C., Lieut., Canadian Engineers, killed in France, Mar. 18, 1918. Hague, William, 1st Lieut., Engineer Officers' Reserve Corps, died in active service, Jan. 1, 1918.

Jan 1, 1919

By William Kent

Mr. ASHBURNER's paper on the Classification and Composition of Pennsylvania Anthracites, read at this meeting, well shows the need of new and accurate determinations of the heating value of these coals. A similar need exists for the determination of the value of bituminous coals, since the variation in quality of the latter is greater than the variation in anthracites. The recent extensive use of liquid and gaseous fuels, " patent" fuels, tan-bark, and other refuse fuels, also makes a necessity fix some correct method of determining the relative values of each of these fuels. Mr. Ashburner has recommended that tests of coals should be undertaken by the Second Geological Survey of Pennsylvania, and Professor Dewey, as stated in Mr. Ashbnrner's paper, has suggested a plan for tests of American coals, by the Smithsonian Institution, for which an appropriation by Congress will be asked. It is to be hoped that if any extensive series of tests of coals is carried on under either Government or State auspices, the erroneous methods of test which were followed by Professor Johnson in 1842, and by Quartermaster-General Meigs in 1882, will not be adopted.* The first requisite in determining the heating-power of a fuel is proper apparatus, such as has not been used in any of the tests of American coals yet reported. In the hope that more accurate means may be used in future tests, the writer desires to call attention to an apparatus which he has designed for the purpose. Not having had opportunity for making a trial of it, nor even of having it criticised by others, he does not offer it as the best possible apparatus; but if it contains any points of value, and leads to the design of still more suitable devices by others, the object of the presentation of this paper will be accomplished. The tests by Professor Johnson and General Meigs were made by evaporating water into steam in ordinary steam-boilers. A steamboiler of ordinary construction is not a good apparatus for determining the heating power of a fuel, for the following reasons:

Jan 1, 1886

By T. E. Leontis

The specific effect of various rare-earth metals on the room- and elevated-temperature properties of magnesium has been evaluated. Alloys containing didymium exhibit the highest tensile and compressive strengths at room and elevated temperatures. All the rare-earth metals increase the creep resistance of extruded magnesium at temperatures in the range of 400° to 600°F, but the degree of enhancement depends on the temperature and on the concentration of the added metal. THE effects of rare-earth metals on the properties of sand-cast magnesium were discussed in some detail in earlier paper by the author.' The present paper deals with the effect of the same alloying elements on the properties of extruded magnesium. This investigation also had as its aim the development of a wrought alloy having a better combination of room-temperature strength and ductility and elevated-temperature strength and creep resistance than is found in magnesium-Mischmetal-manganese alloys, which have been reported earlier.2-5 The only known attempt to study wrought magnesium alloys containing pure cerium instead of Mischmetal was made by Mellor and Ridley.6 They found that in the form of rolled bars there is a definite, optimum cerium content for creep resistance at 200 °C and that the creep resistance of these alloys at 200 °C is significantly Improved by heat treatment at 550" to 580"C. In the present investigation the compositional variation in mechanical properties of the following alloy systems is presented: I—magnesium-Misch-metal. 2—magnesium-cerium-free Mischmetal. 3— magnesium-didymium. 4—magnesium-cerium. 5— magnesium-lanthanum. Alloys containing predominately praseodymium are not included in this series because of the lack of this material. Experimental Procedures The alloying ingredients used in preparing the alloys described herein are the same as those reported in the earlier paper.' Cerium-free Mischmetal is the rare-earth mixture remaining when the cerium is removed from Mischmetal, which contains all the rare-earth metals as they occur naturally in mon-azite sand, the ore from which Mischmetal is produced. Removal of both cerium and lanthanum from Mischmetal leaves what is commonly called "didym-ium," consisting predominantly of neodymium and praseodymium. Although the composition of the particular batch of each metal used may differ somewhat from the analysis presented previously, these differences are not great enough to warrant repeat- ing the specific composition of each material. The electrolytic magnesium used as the starting material in these alloys has the same typical analysis as that given in the earlier paper.' The alloys were prepared in small laboratory melts applying all the necessary precautions for alloying rare-earth metals with magnesium described by Marande.' Most melts were large enough to cast one 3 in. diam billet 10 in. long. In a few cases, particularly the didymium-containing alloys, the lack of sufficient amounts of the rare-earth metal limited the size of the billet to 6 to 8 in. All billets were scalped to a diameter of 2 15/16 in. and faced to a length of 9 ¼ in. as limited by the size of the extrusion container. The alloys were extruded into ½ in. diam rod on a 500-ton direct-extrusion press using a 3 in. container. The details of the extrusion step are: billet preheat, 925°F (2 hr); container temperature, 900°F; die temperature, 900°F; extrusion speed, 10 ft per min; reduction ratio, 36:1; and percent reduction, 97.3. The lower melting point of alloys containing didymium' necessitated reduction of the extrusion speed to 5 ft per min in order to prevent hot shorting during extrusion. Adequate lengths were cropped from both ends of each extruded rod to assure that all the material used for tests was extruded under uniform conditions. Tensile and compressive properties at room temperature are reported in the several conditions of heat treatment. The ASTM designations are used to distinguish these conditions as follows: T5—Direct age at 400°F (16 hr) T4—Heat treat at 950°F (4 hr) for alloys containing didymium T4—Heat treat at 1050°F (4 hr) for all other alloys T6—T4 + age at 400 °F (16 hr) The lower heat-treating temperature for alloys containing didymium is necessitated by the lower melting point of these alloys. All heat treatments were conducted in electrically heated, circulating-air furnaces. A protective atmosphere containing 0.5 to 1.0 pct sulphur dioxide was used for the high temperature heat treatments. Tension and creep specimens 6 Yz in. long and compression specimens 1½ in. long were cut from the extruded rod. A reduced section of ? in. diam was machined on the tension specimens, whereas on the creep specimens a reduced section of 0.450 in. diam

Jan 1, 1952

By W. A. Alexander, L. M. Pidgeon

Metallic magnesium and similar meta!s near the top of the electromotive series have been commercially produced by the electrolysis of a suitable molten salt. Despite the success of electrolysis, sufficient inherent objections exist to justify the search for a direct reduction method. Such a method would widen the choice of raw materials, relax the rigid electrolytic requirements of raw-material purity, and, by obviating direct current, over simplicity of plant equipment. This paper describes the pilot-plant development of one such method, which has subsequently formed the basis of operation of six commercial plants-—one in Canada and five in the United States. Unlike aluminum, magnesium is volatile at relatively low temperatures. This physical property, which produces its greater inflammability, also offers possibilities of direct reduction that are not available with aluminum. In the basic reaction MgO + X = XO + Mg if X is nonvolatile, the reaction may be forced to the right at high temperatures by the evolution of magnesium vapor, despite the large negative value of the heat of reaction which is almost bound to follow the use of any available commercial reducing agent. The cheapest X, of course, is carbon, but this notable advantage is modified by the production of a volatile oxide CO, so that both Mg and CO are evolved simultaneously. Elaborate devices are required to shock-cool the equilibrium mixture in order to prevent back reaction. At best, a pyrophoric powder is produced, requiring redistillation to provide marketable metal. The practical development of this process, is due to F. Hansgirg, and his methods have recently been given a trial on a grand scale in the plant at Permanente, California, and smaller plants were previously built in Austria, England and Japan. A second class of reducing agents is available, those which produce nonvolatile oxides. When XO and X are relatively nonvolatile, magnesium is the only volatile member of the system. It may be evolved in a simple distillation step and condensed without the formation of powder. Two basic requirements must bc fulfilled in order that such a reaction may proceed: I. The reducing agent when heated to a reasonable temperature in presence of MgO must cause the production of an appreciable equilibrium vapor pressure of magnesium. This magnesium must be removed continuously. z. A supply of heat must be maintained. In order to fulfill the first requirement, operations must be conducted in vacuo or in a stream of Hz. Owing to its greater efficacy and relative safety, vacuum has been employed in the work to be described. The choice of a suitable reducing agent formed the subject of an extensive series

Jan 1, 1944

By V. R. Garfias

EVEN before the arrival of Cortes in 1519, the history of Mexico was closely linked to that of its mineral production; the mining activities of the Aztecs being thus described by Clavigero, one of the early historians: In the mountains of Anahuac there abound in veins all kinds of metals, and infinite variety of other fossiliferous products. The Aztecs obtained gold from the countries of the Cohuijques, of the Mixtecas, of the Zapotecas and from various other places. They gathered that precious metal usually in grain, from the sands of the rivers, keeping a certain portion for the crown. They obtained silver from the mines of Taxco, of Tzumpango and others; however, this metal was not as esteemed by them as by other neighboring nations. They had two kinds of copper; one hard, which they used instead of iron to make sickles, lances and all kinds of rural and military instruments and another, soft, with which they made kettles, goblets and other receptacles. This metal abounds mainly in the province of Zacatula and in that of Cohuijques, which at present is in the kingdom of Michoacan. They obtained tin from the mines of Taxco and lead from those of Izmiquilpan, located in the country of the Otomiea. From the tin they made money, and the lead, we know they sold in the market places, but we ignore the uses to which they applied it. They also had mines of iron in Tlaxcala, in Taxco and in other places; but they either had not discovered them, or did not know how to make use of the metal they contained. In Chilapa there were mines of mercury, and in other places there were mines of sulphur, alum, vitriol, cinnabar, cohre and of a white earth which they esteemed highly. As regards mercury and vitriol, we do not know of what use they were to them; the other metals they used in paintings and dyes. There were then great abundance of amber and asphalt-bitu- men of Judea--on the coast of the seas and many cities of that territory paid tribute of one and the other to the kingdom of Mexico. They mounted the amber in gold, and it was only used as ornament and display by them. With the asphalt they made certain perfumes. The following extracts dealing with pre-Colonial gold are taken from the famous "Cartas de Relación" to Charles V, in which Cortea described the progress of the Conquest: . . . here there came two chiefs who owned lands in the valley; one four leagues down the valley and the other two leagues up the valley and they gave me some gold necklaces of little value and seven or eight girls. . . . . . . that day I left the City of Churultecal and traveled four leagues to some villages of the City of Cuasucingo where the natives received me very well and gave me women and pieces of gold. . . .

Jan 1, 1937

By Earl Bardwell

THE structural relations existing between cuprous oxide and copper -were first systematically studied by Heyn1', who suggested that a study of the microstructure of refined copper might be substituted for the analytical methods in vogue for determining the oxygen content of copper coming from the refining furnace. Hofman, Green and Yerxa,2 in their paper A Laboratory Study of the Stages in the Refining of Copper, working along the lines suggested by Heyn, showed that a study of the microstructure could be made to yield a correct estimate of the oxygen content of the specimen of refined copper under examination. In order to determine the oxygen content of the specimen of refined copper under. examination a photomicrograph was first made. From the relative areas of copper and eutectic, the percentage of cuprous oxide and the corresponding percentage of oxygen were then readily calculated. It was found that the values for oxygen thus obtained corresponded closely with the analytical results. With the idea of utilizing this method of determining the oxygen content of each charge dipped from the refining furnaces at the Boston & Montana Reduction Plant, the physical testing laboratory was equipped with suitable apparatus for carrying out the work. It may be of interest to describe certain of the methods which have been worked out in this connection and give such data as have been obtained bearing on the effect of the oxygen content of refined copper upon its conductivity. Apparatus.-For the benefit of those who may be unfamiliar with metallographical apparatus and methods and may be interested to know what equipment is required, a few words with regard to the apparatus is in place at this point.

Jan 7, 1913

By Charles Stein

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

Jan 1, 1970

By A. P. Young, F. C. Holden

IN many of the early investigations of the aging of titanium alloys, it was observed that the retained beta phase could be aged to a high hardness without an apparent change in microstructure; moreover, in some alloys it was found that even a very rapid quench produced beta having an anomalously high hardness. What appeared to be hard beta phase was designated as "beta prime," to distinguish it from the softer normal retained beta phase. Frost and co-workers'.' demonstrated that the increased hardness is caused by the formation of a metastable phase, omega, which can be identified from its X-ray diffraction pattern. This reaction also has been studied by Brotzen, et a1.,3 and the structure of the omega phase has been published by Silcock, et al.," and by Austin and Doig.3 The X-ray diffraction analysis by Austin and Doig indicated that omega is low in alloy content, approaching the composition of the stable alpha. The aging process proceeds by the path Thus, overaging results in the formation of alpha and the ultimate disappearance of omega. This is accompanied by a decrease in hardness and a recovery of ductility. The present work represents a study of the aging process in a high-purity Ti-6.4 Mn alloy, in which optical and electron microscopy, X-ray diffraction, and hardness data were correlated. The specimens, 1/8-in. sections cut from 1/4-in.-diam rod, were heated in argon to a temperature just into the beta field (810°C), held for 1 hr, and water-quenched. The aging samples were heated in air for 1 hr at 300 to 500°C. The specimens were ground and mechanically polished, finishing with alternate etching and polishing on a slow-speed wheel to remove disturbed metal from the surface. The surface finally was swab-etched, rinsed with tap water, and air-dried. The etchant used was an aqueous solution containing 1 1/2 pct HF and 3 1/2 pct HNO3. This procedure is identical with that used for preparing metallographic specimens, except that the optimum degree of final etching required for electron microscopy may vary from that used for light microscopy. Metal replicas, backed with silica, were prepared from plastic strip-pings for examination with the electron microscope. Complete details of the procedures used for preparing these replicas are available elsewhere." Fig. 1 shows a comparison between the structures revealed by the electron microscope and those obtained by conventional light microscopy. Hardness and X-ray diffraction data are listed in Table I. No evidence of a second phase is apparent in the optical micrographs for the as-quenched sample, or for the specimens aged at 300 or 400°C; fine alpha particles can be seen in the specimen aged at 500°C. In the electron micrographs, visible equiaxed pocks appear in the as-quenched specimen, and, with increasing density, in the samples aged at 300 and 400°C. After aging at 500°C, the structure becomes markedly coarser and develops an oriented appearance of a second phase, coincident with the appearance of visible alpha particles in the light micrographs. These observations are confirmed by X-ray diffraction and hardness data. In these specimens, aged for 1 hr, the intensity of the omega pattern increases to a maximum at the 400°C aging temperature, corresponding to maximum hardness and the maximum density of pocks in the electron micrographs. At this point the beta phase shows a definite enrichment in Mn. At 500°C, little or no omega re-

Jan 1, 1959

By John Mathews

DURING the prosecution of the aircraft-production program in 1917 and 1918, the writer visited many plants engaged in the manufacture of motors, planes and parts, in carrying out his duties as chairman of the Committee on Aircraft-engine Forgings. On several occasions, when the question of expansion was discussed, it was noted that there was confusion in the use of the terms: the true coefficient of expansion, a physical constant, and distortion in hardening. One engineer, referring to a steel shown in the accompanying table; stated that he could not consider it for crankshafts because of its excessive coefficient of expansion, while another steel, also listed in the table, as said to be especially good because it had no coefficient of expansion, since it came out of the oil bath perfectly straight. Many years ago one of our employees designed anew oil furnace; when asked what became of the products of combustion, he replied: "There ain't any, we burn them all up." While the coefficient of expansion is not without its effect in volume changes in hardened steel, it is not a determining factor in the matter of distortion and going out of shape. Irregular heating, uneven furnace bottoms, and carelessness in withdrawing the part from the furnace, as well as the manner in which the part enters the quenching bath are of greater moment. Generally speaking, also, steels of relatively low hardening temperature will distort less than those requiring higher hardening heats. The coefficient of expansion must be considered in engineering design most frequently when different metals or alloys are used in the same construction. For example, the difference of expansion between a steel crankshaft and an aluminum crank-case might be of real importance and a steel with no coefficient of expansion would be much less desirable than one with the normal coefficient. About 15 years ago, the writer made many determinations of the coefficient of expansion at low temperature ranges, usually between 20° and 100° C. Among the materials tested were: Pure forged electrolytic iron, 11.73 parts per million for 1° C.; cast aluminum (99.93 per cent. Al.),

Jan 2, 1920

By B. Alexander, G. Derge W. Peifer

This is part of a research project in the Metals Research Laboratory of Carnegie Institute of Technology, sponsored by the Carnegie-Illinois Steel Corporation. In organizing our program it became apparent that the problem of analyzing molten steel for hydrogen must be divided into two parts: (I) the correct analysis of a given sample, and (2) the correct sampling of the bath. Emphasis has been placed upon these divisions in the order named because methods of sampling cannot be evaluated until a satisfactory method of analysis is available. Vacuum fusion was selected from the list of possible analytical methods because it seemed to us to offer the best possibilities for giving rapid, accurate results on solid steel samples. A number of objections have been raised against this method as usually practiced. We have sought to meet some of these by proper design of the apparatus. Experiments will be described which show that others are not valid. In the conventional apparatus the sample is held under high vacuum for a period of several hours before it is actually analyzed and one might expect considerable hydrogen to escape during this period. We have provided a means of introducing the sample to the vacuum just before analysis. Another difficulty has been that the entire apparatus has been designed primarily for the purpose of analyzing for oxygen, which constitutes upward of go per cent of the total gases evolved from the sample The volume and pressure measurements have therefore been insensitive to the relatively small amounts of hydrogen present. This difficulty obviously can be taken into account in any apparatus designed especially for the amounts of hydrogen expected. Analysis in Vacuum-fusion Apparatus A number of experiments were carried out to determine the importance of several factors that have been stated as possible sources of error or uncertainty in vacuum-fusion analysis for hydrogen; namely, that hot graphite will absorb some of the gases, that metal vapor will cause discrepancies, and that low results may be obtained as a result of the water vapor (produced by the oxidation of the hydrogen) dissolving in the butyl phthalate of the manometer, or that the blanks obtained from the apparatus are so great as to make the method inaccurate. The experiments also checked on the accuracy and feasibility of using differential freezing as a method of gas analysis in a vacuum-fusion apparatus.

Jan 1, 1945