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By L. L. Wyman

THE exact nature of the changes that take place in the iron-nickel alloys, giving rise to the interesting and useful expansion alloys in the Invar range, has yet to be fully understood. Similarly, the ternary iron-nickel-cobalt alloys, which also possess such commercially useful expansion characteristics, 1,2 are concerned with transformations that appear to be identical with those found in the parent iron-nickel alloys. The investigations on iron-nickel alloys in the range 26 to 29 per cent Ni have been reported by several authors" wherein it is shown that there are factors other than temperature, such as stress and grain size, which play an important part in determining the temperature at which the low-temperature transformation takes place. It will be shown in this paper that the ternary iron-nickel-cobalt alloys having nickel contents comparable to the alloys mentioned above behave in a parallel manner. The alloys in the range of 26 to 31 per cent Ni and 16 to 21 per cent Co have a coefficient of expansion of about 4.0 X 10-1 per degree Centi-grade, and the alloys in this range of composition find considerable application in making glass-to-metal seals, because these expansion properties so well match commercial glasses. The behavior of these alloys is not a simple matter, for it has been observed in alloys of 28.5 per cent Ni and 18.5 Co that severe working can cause the appearance of a second phase having a needlelike structure similar to the martensite structure in carbon steels. Fig. 1 shows the change brought about in an alloy of this composition when a strip of this material was cut with tin shears. This second phase has been identified as the body-centered cubic alpha phase, and it is the purpose of this paper to describe the results of some of the preliminary investigations in the study of the changes involved in these alloys.

Jan 1, 1939

By Haydn H. Murray, Sam H. Patterson

The term "clay" is somewhat ambiguous un¬less specifically defined, because it is used in three ways: (1) as a diverse group of fine-¬grained minerals, (2) as a rock term, and (3) as a particle-size term. Actually, most persons using the term "clay" realize that it has several meanings, and in most instances they define it. As a rock term, clay is difficult to define be¬cause of the wide variety of materials that com¬pose it; therefore, the definition must be gen¬eral. Clay is a natural earthy, fine-grained ma¬terial composed largely of a group of crystalline minerals known as the clay minerals. These minerals are hydrous silicates composed mainly of silica, alumina, and water. Several of these minerals also contain appreciable quantities of iron, alkalies, and alkaline earths. Many defini¬tions state that a clay is plastic when wet. Most clay materials do have this property, but some clays are not plastic; for example, halloysite and flint clay. As a particle-size term, clay is used for the category that includes the smallest particles. The maximum-size particles in the clay-size grade are defined differently on various grade scales, Soil investigators and mineralogists gen¬erally use 2 micrometers as the maximum size, whereas the widely used scale by Wentworth (1922) defines clay as material finer than ap¬proximately 4 micrometers. Some authorities find it convenient to use the term "clay" for any fine-grained, natural, earthy, argillaceous material (Grim, 1968). When used this way, the term includes clay, shale, or ar¬gillite, and some argillaceous soils. Even though no standard definition of the term clay is accepted by geologists, agronomists, engineers, and others, the term is generally un¬derstood by those who use it. Clay is an abun¬dant natural raw material, and it has an amaz¬ing variety of uses and properties which will be discussed in this chapter. Clays rank among the leading industrial min¬erals in both tonnages produced and total value. Their importance is indicated in Table 1, which lists the 1970, 1971, and 1972 production and values according to the U.S. Bureau of Mines (Ampian, 1972). Adequate reliable statistical data on which to summarize world production of clay are un¬available; this paragraph outlines the world re¬quirements for clay only in a very general way. According to one estimate, the world bentonite production in 1972 was 3.5 million tons (Anon., 1973a), but in the authors' opinion it was prob¬ably at least 5 million tons. The total fuller's earth produced was at least 1.5 million tons and may have been as much as 2 million tons. The total world kaolin production in 1972 was more than 10 million tons. Approximately 7 million tons of this total was produced in only two regions-the Georgia-South Carolina kaolin belt in the United States and the Cornwall re¬gion, United Kingdom. The world's 1972 out¬put of ball clay, which is also produced pri¬marily in the United States and the United Kingdom, was approximately 1.5 million tons or perhaps a little more. The total world fire clay production in 1972 was probably about one and one-half to two times and the miscellaneous clay production three times the United States production. As industrial minerals, clays are a complex group that consists of several mineral commodi¬ties, each having somewhat different mineral¬ogy, geologic occurrence, technology, and uses. In this chapter these commodities are organized

Jan 1, 1975

By F. D. Weeks

THE Salida smelting plant, owned by the Ohio & Colorado Smelting & Refining Co., is situated at an altitude of 7,000 ft., about 2 miles west of Salida, Colo., and 215 miles southwest of Denver. Salida is a division point on the. Denver & Rio Grande R. R. where the narrow-gauge line serving the Sari Juan region joins the through standard gauge. This narrow-gauge road also serves the coal and coke companies at Crested Butte and the lime quarries and mines at Monarch and Garfield, which are only 20 miles distant. These facts, together with the possibility of an appropriate site, doubtless influenced the builders to locate at this point. The smelting plant and yard occupy 80 acres of land on the northeast side of the Arkansas River. The slope of the ground is such as to permit of the ore being delivered by cars at a point 25 ft. above the feed floor; and in front of the furnaces there is a fall of 50 ft. for the slag clump. A recent purchase of river bottom has provided slag room for 20 years. As originally constructed, the plant consisted of four blast furnaces, 40 by 144 in. at tuyeres, two copper-matting furnaces, dust chamber, stack, power plant, blowers, sampling works, and one railroad trestle about 16 ft. from bed floor to rails. Later 12 hand roasters of excellent design were added and the practice of smelting leady matte in-a copper-matting furnace was abandoned. Since the plant passed under the present management the equipment has been increased so that the following is a brief description of the same at this date: Two lead blast. furnaces, 48 by 180 in. at tuyeres, 17 ft. 6 in. tuyères to feed floor; four lead blast furnaces, 40 by 144 in. at tuyères, 17 ft. 6 in. tuyères to feed floor; two copper-matting furnaces, not used; blast-furnace flue, 900 ft.; area 245 sq. ft.; blast-furnace stack, 150 ft.; above furnace floor, 190 ft. When smelting a 500-ton charge per day, the gases approximate 63,700 cu. ft. per minute and travel at a speed of 260 ft. per minute.

Jan 8, 1915

Jan 1, 1967

By J. G. Mravec

The SO-called gas-tube method as developed by Hare, Peterson and Soler for determining the type and content of gases in molten steel is particularly adapted for determining the hydrogen content in molten steel. The development of this method has been quite completely discussed in a paper published by these co-workers in 1937.' The purpose of this paper, therefore, is to familiarize with this method those who arc not well acquainted with it. The principle of the gas-tube method is as fol1ows: One end of an evacuated gas tube is sealed with a very thin copper disk. when this end of the tube is immersed in a test spoonful of molten steel, the copper disk melts almost immediately, allowing a portion of the steel to be drawn up into the evacuated space. Any dissolved gases, and those produced by reactions between the components of the steel during freezing, are liberated into the unfilled portion of the sampling tube. A blob of steel that forms on the immersed end of the tube after the sample is drawn up seals up the end, making it airtight again. The evolved gases are subsequently drawn out of the gas tube through a suitable valve and analyzed by means of an Orsat apparatus. The volume of the sampling tube is sufficiently large so that a pressure considerably below atmospheric is produced after the gas evolution. The low pressure is necessary to effect a nearly complete removal of gases from the steel. Construction oF Sampling Tube The sampling gas-tube apparatus is illustrated in Fig. I. Seamless S.A.E. tubing used for section A is first cut into 7-ft. lengths. Through cxperiencc it was found necessary to use two sizes of tubing for this part, "is-in. and 3/4-in., respectively. The smaller tubing is generally used on the hotter or lower carbon steels. If the inside wall of the tube A is coated with grease or oil, it should be burned out before being machined as follows: One end is machined on the inside diameter to a depth of 34 in., so as to form a seat for a 7/8-in copper disk, which is stamped out from 0.005 to 0.007-in. thick copper sheet. The other end is machined on the outside diameter to a diameter of 1 5/16 in., to take a small reservoir or trap member I?. About 4 in. below the same end, a 1/2-in. hole is drilled to receive the 1/2-in. copper tubing leading to the large reservoir C. The inside of tube A is then thoroughly cleaned with a round wire brush, such as is generally used to clean out shotgun barrels. It is very important that the surface be absolutely free of rust or any nonmetallic coating. Next, the thin copper disk is soldered in place with low-melting silver solder.

Jan 1, 1945

By W. S. Steele

Vermiculite is a nonmetallic mineral of the mica family, probably related to biotite mica. Its occurrence has been noted at numerous places in the United States and in some foreign countries, but it can be said that vermiculite is of only moderately wide distribution. A laboratory and field survey of over 60 deposits in the United States by F. 1;. Schundler & Co., of Joliet, Ill., indicates that the purest deposit represented in this survey is on the property of the Zonolite Company at Libby, Montana The Zonolite Company is commercially active and the vermiculite it produces is sold as Zonolite. Hereafter, in this report, the word "Zonolite " will be used to designate the vermiculite produced by the Zonolite Company. Values given herein to Zonolite are peculiar to the vermiculite produced from the Zonolite Company's deposits. References to " vermicullite," are to he interpreted as covering the broad field covered by the Schundler survey. Composition and Characteristics of Vermiculite Vermiculite is an aluminum-nmgnesium silicate. The following typical analysis is published by the United States Bureau of Standards: silica, 41 per cent; iron oxide, 7; aluminum oxide, 18; magnesium oxide, 21; calcium oxide, 1; alkalis (sodium and potassium), 1; moisture, 11. Vermiculite breaks down into platelike formation in crushing and grinding operations. Its cleavage is basal. Crude, screened, dry Zonolit,e weighs between 80 and 90 Ib. per cubic foot; its specific gravity is 2.8 and its specific heat is approximately 2. The fusion point of Zonolit'e is 2462" F. Crude vermiculite contains between 7 and 9 per cent of chemically combined moisture. The instantaneous introduction of crude Zonolite into an expansion furnace at a temperature of between 1800" and 2000" F. transforms the combined moisture into steam, which in an effort to liberate itself forces all explosive expansion of the platelike crude material

Jan 1, 1934

By R. D. Lord

The search for the best practical means of storing sulfide bearing tailings, where there is no residual excess of carbonate material is discussed in this paper• Usually the sulfide content decomposes, with the aid of bacterial action, and the resulting sulfuric acid escapes, along with any heavy-metal solutes, through embankments that are usually porous to some degree• The problem is typified in the tailings of the uranium operations of Elliot Lake, Ont., where mining started some 20 years ago• The approach to tailings disposal paralleled the practice for other hydrometallurgical plants treating gold and base-metal ores• Impoundment areas were designed to retain solids, and a clear and neutral overflow was considered satisfactory practice• Now experience has shown that these areas, some of which have been idle for over a dozen years, release acids in seepage and overflows to an unacceptable degree• To protect natural water courses, neutralizing plants are operated wherever required• Lime slurry is fed continuously into the tailings outflows in a quantity sufficient to raise the pH to 8•5 and precipitate heavy metals that may be in solution• The objection to this procedure is that the plants will require servicing indefinitely, unless a better remedy is found• The problem differs only slightly from that common to base-metal concentrators in that here the ore has been leached with sulfuric acid for the recovery of uranium• Any native content of calcareous material has been digested, and only that added for final neutralization is available to maintain a pH unfavorable to bacterial activity• Chemical oxidation slowly lowers the pH and when this reaches a level of 4•5 or less, bacteria become active and greatly accelerate the formation of acid. The bacterial process is probably at least ten times as fast as the chemical oxidation• Location and Processing The operations referred to, uranium and one copper mine, are located at approximately 46°N and 82°W longitude• This is typical Canadian Shield country, a land of lakes, deeply glaciated and rocky, with sparse soil which supports mixed forest cover• Drainage is to Lake Huron, 25 miles to the south• Average temperature is 45°F, ranging from -40° to +95°F• Annual precipitation is 38 in•, about half of which is snow• The ore is Precambrian, quartz-pebble conglomerate, with mineralization in the matrix• From 5 to 10% pyrite is present• All known means of pre-concentration have been tested, but a bulk sulfuric acid leach has proved the most efficient. Tailings have from the outset been neutralized before release• Current practice is to add ground limestone to bring the pH to 4•5, and then lime to raise the value to 10•5• Environmental regulations have recently been increased and the foregoing meets the new standards• Separate measures are taken to precipitate radium• Remedial Measures Since the outstanding environmental problem is the oxidation of pyrite by bacterial action, the solution is to contain the products, or arrest the process• Given the ambient temperature, favorable half of the time, four items are essential to the activity• 1) Pyrite• 2) Moisture pH < 4•5. 3) Oxygen• 4) Bacteria• Removing any one of these out of the range of tolerance will bring the reactions under control• A variety of proposals considered, and a number tested for the arrest of the process, are: (a) render embankments impermeable, (b) provide an impermeable cover, (c) cover with an oxygen absorbing layer, (d) provide a vegetative cover, (e) flood the site, (f) remove pyrite from current tailings, (g) add excess limestone to current tailings, (h) poison the bacteria• Bank Seal-On existing impoundment areas, where the embankments are several thousand yards in length, it is believed that any program of injecting sealants can have small chance of success• However, a moisture barrier is an indicated specification for future construction, and this can be highly expensive• Surface Seal-Depending on the configuration of the deposit, the downward travel of water should be prevented, and oxygen excluded• Burying a plastic membrane just below the surface has been considered, as has the application of a liquid sealant that would penetrate the surface. The objection to these remedies is the excessive cost of dealing with large areas and the expectation of only temporary benefit as a result• Frost penetration is over 4 ft, and frost action breaks up asphalt paving and all but heavy concrete in a few years• Organic Layer-An oxygen-absorbing layer, such as bark fines from paper mills has been proposed as a surface treatment• Cultivated into the tailings such material might be expected to arrest subsurface oxidation for some years• Estimates are 100 tons per acre of bark fines, or 35 tons per acre of sawdust, and these enormous quantities do not so far give assurance of providing a long-term remedy• Vegatative Cover-Several obvious benefits would result from a good growth of grass or other vegetation on abandoned tailings• While restoring the natural green of the tract the growth would prevent wind-blown dust and reduce erosion• Subsurface oxidation should be reduced, as well as the upward movement of ground moisture as occurs in dry weather. To this end, considerable research and field testing has been carried out to arrive at a formula - a prescription which will provide a self-sustaining growth on the tailings surface, or at least one that would survive with reasonable maintenance attention. Many test plots have been run with different combinations of surface treatment and seed mixtures. Generally, by addition and close cultivation of limestone, lime, and fertilizers, technical success has been demonstrated• Plants with a high tolerance for acid soil seem the more hardy, and a pH above 3 is indicated so that nutrients can be absorbed• Recommendations are for 12 to 15 tons of

Jan 1, 1977

By Frederick Laist

This paper is a review of Montana reverberatory smelting practice covering a period of approximately fifty years, during which time the small furnaces that had been in use elsewhere for a century or more, without much change in size or method of operation, were revolutionized and were developed into the huge, continuously operating furnaces of today. A study of Montana practice is particularly instructive, since reverberatory furnace smelting for the production of copper matte received more attention there than in other smelting centers and many of the improvements that finally resulted in establishing the preeminence of this type of furnace over the blast furnace originated in Butte and Anaconda. The material in this paper was gathered from original sources, wherever possible, and all of the illustrations were made from original drawings, some of which have been simplified and worked over so as to be better adapted for reproduction. The aim has been to trace the modifications in design and operation which took place during the period in question—the reasons for the changes and the results achieved through them. For developments during the first twenty years, the technical literature of the period was freely drawn upon, but I am particularly indebted to W. M. Kelly, general foreman at the Anaconda Works, whose recollections and personal experience extend back to the early days. I wish to acknowledge the use made of publications of E. P. Mathewson, William Wraith and L. V. Bender, as well as information obtained here and there from friends and associates. The resume of Great Falls practice was compiled from correspondence, notes and drawings found in the files of the old Boston & Montana Co. and the tabulations showing the performance of furnaces at Butte and Anaconda are adapted from plant records and correspondence in the files of the Anaconda Copper Mining Company. The paper deals with some interesting comparisons that were made between furnaces operated under various conditions in connection with the Carson Case, and results obtained when using natural gas as fuel. This part of the paper may be considered original to the extent that these results have not previously been published.

Jan 1, 1934

THOSE MARKED THUS * ARE MEMBERS, MARKED THUS ?ARE ASSOCIATES. THESE SIGNS DOUBLED INDICATE LIFE MEMBERS AND ASSOCIATES RESPECTIVELY. THE FIGURES AT THE END OF THE ADDRESS INDICATE THE YEAR OF ELECTION. HEAVY-FACED TYPE SIGNIFIES HONORARY MEMBERSHIP. *AARONS, J. BOYD, Vivian Gold Mining Co., Ltd., Harris, West. Australia. &apos;05 *ABADIE, EMILE R., Cons. and Min. Engr., 214 Union Savings Bank Bldg., Oakland, Cal. &apos;76 ?ABBÉ, MAX F., Prest., Abbé Engineering Co, 220 Broadway, New York, N.Y. &apos;07 ? ABBÉ, PAULO., Secy.,Abbé Engineering Co., 220 Broadway, New York, N.Y. &apos;07 *ABBOTT, AI ARTHUR Morococlia, Peru, So. America. &apos;95 *ABBOTT, CLARENCE Chief EDgr., Iron Mines, Dic Tennessee Caol, Iron & R. R. Co., Bessemer, Ala. &apos;04 *ABBOTT, JAMES W., Min. Engr: Ploche, Lincoln Co., Nev. &apos;94 *ABE, MASAYOSHI, Prof. of Mining, Imperial University Kyoto, Japan. &apos;05

Jan 1, 1910

By Donald F. Saunders

Means and relative standard deviations were calculated for eU, eTh, K, and their ratios for aerial gamma-ray spectral data in 29 quadrangles at 1:250,000 scale. Known or suspected uraniferous provinces were characterized by: 1) Higher eU, eTh, and K means (due to generally higher radioelement concentrations); 2) Higher relative standard deviations for eU, eU/eTh, and eU/K (reflecting the presence of local uranium enrichments); and

Jan 12, 1979

Jan 1, 1938

PRODUCTION of nonmetallic mineral raw materials used by the fertilizer, ceramic, chemical, and construction industries and many others, was greater during 1953 than in any previous year. Production of fertilizer minerals was the highest in history despite somewhat decreased consumption in the second half of the year. Marketable phosphate rock production increased 10 pct to an estimated total of 13.1 million LT, valued at $78.5 million, and potash production was estimated at 1.8 million tons of K2O equivalent, valued at over $60 million. Crude gypsum output exceeded the 1952 total and approached the record of 8.66 million tons mined in 1951, with indications that 1953 will show a new all-time high. Gains and losses among gypsum products were irregular, with major gains in plate- glass and terra-cotta plasters, sanded building plasters and miscellaneous building plasters, and principal declines in base-coat plasters, prepared finishes and tile. Lath and wallboard outputs were each about 20 pct higher than in 1952.

Jan 2, 1954

By M. J. Marcinkowski, K. S. Raghavan, A. S. Sastri

A detailed transmission electron microscopy investigation was carried out in connection with a manganese Hadfield Steel. At small plastic strains, numerous individual intrinsic stacking faults are observed. With increased plastic deformation, the stacking faults thicken into twin lamellae which in turn subdivide the original austenite matrix into smaller domains. The twin boundaries act as strong barriers to subsequent dislocation motion and is in a sense equivalent to grain refinement. It is this "grain refinement" which is believed to be the cause of the very high work hardening rates in the Hadfield Steels. In many cases, especially where an hcp phase is the stable one at low temperatures, the stacking fault energy in fcc metals and alloys decreases with decreasing temperature.&apos; Since stacking faults of the intrinsic type are precursors of both twins as well as the hexagonal close packed structure, both of these entities should become more frequent as the temperature of a fcc crystal is lowered. In the case of the twin, there is no chemical driving force for its formation and it is generally necessary to provide the required driving force by an applied stress, i.e., strain energy. In the case of the hcp structure the transformation from the fcc modification can occur spontaneously (marten-sitically) since a decrease in chemical energy does in fact occur; however, an applied stress will provide an even greater driving force toward complete transformation. Since the transformation products mentioned above occur in an inhomogeneous manner throughout the crystal and since these can act as potential barriers to further plastic deformation2 marked strengthening effects can be anticipated. Also because metal and alloy strenghening is in general proportional to the shear modulus, these effects should be greatest in steels of the austenitic type (y), i.e., the fcc types. Perhaps the two most important steels in this category are the austenitic stainless steels and the Hadfield manganese steels. Both may be quenched from elevated temperatures so as to retain the austenitic states characteristic of those temperatures. The effect of subsequent deformation at lower tem- peratures has a profound effect on the stress-strain curves of these alloys. In particular Fig. 1 shows the compressive stress-strain curves obtained with an 18-8 stainless steel which was quenched from 1850°C after annealing for 1 hr so as to produce all y. As the temperature is lowered, the work hardening rate increases markedly. Although some hcp or c mar-tensite can be generated by plastic deformation as the temperature is lowered,~ it is believed to be a transition phase4 and most of the martensite produced is of the bcc or a variety.3 It is this stress induced martensite which gives rise to the very low initial work hardening at 77°K as can be seen in the stress-strain curve in Fig. 1. Similar low initial work hardening rates have been observed in the stress induced Ni-Ti martensites.5 Fig. 2 shows that an even more rapid rate of work hardening occurs in the Hadfield steels treated in the same way as that described for the 18-8 stainless steels a; the temperature is lowered. It is this ability to work harden to such high stress levels that makes the Hadfield steels particularly suitable for armor plate and heavy construction equipment. However, unlike the case of Fig. 1, no initial low rate of work hardening is observed in any of the curves in Fig. 2. Thus the stress induced formation of any low energy martensite phase in any significant quantity must be ruled out. This observation is in accord with the X-ray findings of Otte.~ On the other hand, small quantities of the E phase have been observed by other investigators using transmission electron microscopy (TEM) above Even more significant was the fact that large numbers of deformation twins were observed in the deformed Hadfield steels,678 which were postulated to be one of the reasons for the high work hardening ability of this class of steels.8 It is the purpose in what follows to discuss a series of experimental observations pertaining to the stress induced transformation in a Hadfield steel and to formulate a dislocation mechanism which adequately accounts for the observed results. EXPERIMENTAL PROCEDURE The stainless steel used to obtain the curves shown in Fig. 1 was of the AISI Type 303 containing approximately 18.0 pct Cr and 8 pct Ni. On the other hand, the Hadfield manganese steel used to obtain the curves shown in Fig. 2 contained between 1.00 to 1.25 pct and 11.5 to 13.5 pct Mn. In all cases the samples were in the form of compression cylinders 0.220 in. in diam and 0.370 in. long. Prior to testing the samples were annealed for a hr at 1050°C and rapidly quenched into a brine solution. This treatment was sufficient to preserve the y phase for subsequent testing at lower temperatures. All samples were compressed in an Instron testing machine using a cross head speed of 0.02 in.

Jan 1, 1970

By A. B. Kinzel

IT is with sincere appreciation and a deep sense of responsibility that I accept the honor of delivering the Howe Memorial Lecture. In our time metallurgical research has delved into phenomena ever more complex in character, so that much of this work must be done by organized teams. We, of the Union Carbide and Carbon Research Laboratories and the Electro Metallurgical Co., are truly a team and the lecture which is to follow is due largely to a few of the outstanding members of that team here cited and well known to you in their own right: John Lamont, whose work deserves special recognition, Walter Crafts, William Forgeng, William Binder, Robert Fowler, and David Swan. Thus it is a fitting pleasure to accept this honor for the research institution which I represent. Henry Marion Howe was truly inspirational and his breadth of view was such that he could use either the method of rigid proof or implied mechanism to further the broad understanding. But perhaps his outstanding characteristic was his sound judgment and his ability to weigh observations. The following is replete with observations and judgment as to their implication. We would like to feel that it is the type of dissertation which Howe, himself, would have enjoyed. Chromium carbides in stainless steel have, in a sense, been a key to the progress of the stainless steel industry. Brearley&apos;s first stainless steel, containing approximately 0.30 pct C, was successful because it differed from previous Fe-Cr alloys in that the carbides were present in such amount and form as to provide the stainless and cutting properties. Again, the 12 pct Cr die steels with a carbon content of 1.5 pct or more achieved their properties by virtue of the form and distribution of the chromium carbides. In the straight chromium steels with from 12 to 25 pct Cr, chromium carbide amount and distribution are once more the determinants with respect to physical properties and corrosion resistance. In each of the cases just cited the role of the carbide is in essence similar to that of iron carbide in carbon steel and this story is so well known that we need not dwell on it. In the austenitic stainless steels, the chromium carbide plays only a minor positive role with respect to mechanical properties, and for corrosion resistance the objective is to achieve maximum homogeneity. Thus the tendency has been to ever lower the carbon and correlatively the chromium carbide content of the austenitic steels. Today stainless steels with carbon less than 0.03 pct are beginning to find their true place, and this is being aided in major degree by our Company&apos;s introduction of a new type of ferrochromium having negligible carbon. The role of carbon in these austenitic steels has long been recognized, and a truly enormous amount of research has been devoted to the subject. Much has been learned about corrosion resistance, but the attack on the problem from the point of view of carbide precipitation and the nature thereof has left much to be understood. Because of its fundamental importance to the future of stainless steels, further study of the mechanism of carbide formation in austenitic steels is of interest. In the 18-8 Cr-Ni steels, which are typical of the austenitic class of steel, carbon is soluble in the aus-tenite to the extent of approximately 0.15 pct at 1832°F (1000°C). The solubility becomes less with decreasing temperature, so that at 1652°F (900°C) the solubility limit is approximately 0.06 pct, at 1472°F (800°C) it is about 0.03 pct, and at 932°F (500°C) it is approximately 0.01 pct. Obviously this is the ideal situation for the classical precipitation phenomenon. It is true that, in a sense, 18-8 austenite resulting from annealing is in a metastable state, and the phenomenon of ferritic precipitation from this austenite should be considered. However, in a so-called fully austenitic 18-8 steel this is secondary with respect to the carbides and can be neglected. A wide variety of chromium carbides is known. Only one chromium carbide, Cr,,C,,, frequently referred to as Cr,C, has been found in unmodified low carbon 18-8 steel. This, fortunately, simplifies the study of the precipitation phenomena. For this study an A.I.S.I. type 304 stainless steel of commercial quality was selected. Analysis showed C 0.07 pct, Mn 0.49 pct, Si 0.33 pct, Ni 9.34 pct, Cr 18.91 pct, and N 0.033 pct. As expected with this composition the steel was homogeneous after annealing except for a few pools of ferrite, which were disregarded in that their location was not coincident with subsequent carbide precipitation areas. On corrosion testing the steel was normal and typical of good commercial quality. Specimens 1/2xlx4 in. were annealed and subjected to precipitation heat treatment for 100 hr at 100" temperature intervals from 1000° to 1500°F and for ten selected intervals ranging from 5 min to 64 hr at 1300°F. These blocks were then cut into small pieces for metallographic studies. The first problem

Jan 1, 1953

By M. H. Pilkuhn, H. Rupprecht

p layers on n-type substrates of GaAs were prepared by difhsion of zinc into these substrates. Experimental details about the diffusion technique will be presented. It will be shown that inhomogeneity in the substrate doping level and crystal shucture defects cause nonplanarity in the junction plane. These nonplanarities give rise to high threshold current densities. From incremental sheet-conductivity measurements the zinc profile is derived. Data about surface concentration and gradient of the zinc concentration at the junction are presented. Finally, some results of laser diodes, which were made of wafers with extremely planar diffusion fronts, are discussed. ThE investigations reported here are part of a program concerned with the materials aspect in the fabrication of GaAs laser diodes. This includes studies of the influence of crystal defects introduced both during the growth of the crystal and as a consequence of subsequent diffusion. Compared with the progress made in the investigation of structure defects, for instance by X-ray microscopy in materials like silicon, no similar results are known so far for the case of GaAs. The further progress in laser diodes will depend very much upon our knowledge of these structure defects and subsequently upon our ability to avoid them. Laser diodes of GaAs had been made mostly by diffusing an acceptor impurity, normally zinc, into an n-type substrate. This procedure was found more convenient than the inverse one for various technical reasons. We will follow this line and restrict ourselves to zinc diffusion only in this paper. DIFFUSION TECHNIQUES AND EXPERIMENTAL DETAIL In order to set a refgrence for our experiments, we used a standard procedure for the diffusion runs. The diffusions were carried out in a sealed quartz tube for 2-1/2 hr at 850°C. One milligram zinc arsenide (ZnAsz) per cu cm of the tube volume served as zinc source. Under these conditions the junction depth was between 25 and 30 p. It is assumed, according to the investigations of the zinc arsenide system by V. Lyons and V. ilvestri,&apos; that ZnAs2 dissociates completely at 850°C into ZnsAsz and Asg. Since there is a condensed phase of ZnsAs2 in the tube at 850°C, the partial pressure of zinc is controlled by the pressure of the arsenic formed by the dissociation of ZnAs2. Due to the fact that the zinc partial pressure resulting from the dissociation of ZnsAsz is only a weak function of the partial pressure of arsenic, the amount of the initial ZnAs2 is not very critical. Experimentally, we found that the junction depth, as well as the surface concentration, was practically the same, if the ingots of ZnAs2 varied between 0.2 and 5.0 mg per cu cm. The wafers were oriented with the main faces in (100). Surface damage due to cutting and lapping was removed by a chemical-etch treatment in a rotating beaker (etch solution: HzSOr, H202, and HzO in a ratio 3:l:l). The GaAs substrate material was n type and doped with tellurium, selenium, silicon, or germanium. It was grown by means of horizontal or Czochralski techniques. After the diffusion process, junction depth and planarity were checked either by grooving with a

Jan 1, 1964

By F. Keller, A. H. Geisler

Some of the important changes that take place in the structure of aluminum alloys are largely submicroscopic in character. This is especially true of the changes that accompany age-hardening and recrystallization. Although improved metallographic practices have been helpful in indicating some of these changes indirectly, results are limited by the resolving power of optical microscope lenses. The electron microscope, however, provides a new and important means for investigating the fine structure of metals in a range not possible heretofore. It is anticipated that this microscope will yield new and useful information to metallurgists when suitable techniques are developed to utilize its very high resolving power. Several unique methods have been devised to permit the examination of the structure of opaque samples by the electron microscope. These are all based on the principle of producing a very thin film that represents the prepared surface of the opaque metal sample, which can be examined in the transmission microscope; however, the available methods fall into three categories, depending on the manner in which the film is obtained. With the oxide-film method developed by Mahl3-17 a very thin surface layer of the metallographic sample is converted into oxide by a thermal, chemical or anodic treatment. After removal from the metal sample by one of the special techniques described by Evans,19 this oxide film is examined in the electron microscope, and is found to portray the structure of the original metal surface. Films formed on aluminum,8,17 nickel,7 iron 3,8,9 and a nickel-beryllium alloy" by heating; films formed on iron 8.9 by chemical action; and films formed on aluminum3-16 by anodic oxidation, have been examined. The other two are more recent methods developed principally in this country; they consist in making the thin film in the form of a mold or replica of the surface contour of an etched sample. With the negative replica method the thin film is made directly on the sample; with the positive replica method it is made on a negative reproduction of the sample. With both methods, variations in the contour of the metal sample, caused mainly by etching, produce variations in the thickness of the surface replica. Because of the direct dependence of the amount of scattering of the illuminating electrons upon the thickness of the film penetrated, only the variations in thickness of the replica are responsible for tones in the electron image. Negative replicas are made by forming a thin film of some suitable material directly on the polished and etched metal sample, and derive their name from the fact that after removal from the sample they have the high and low points in the sample reversed, as shown in Fig. I. Nega-

Jan 1, 1944

By F. W. Maclennan

ORE production from the property of the Miami Copper Co. began early in 1911. Until 1925 this ore came from the so-called high-grade orebodies, which contained a little over 2 per cent. copper. This ore was mined by the following methods. 1. Top slicing after mining the peaks by square setting, which produced 4,524,347 tons, including ore from square setting. 2. Shrinkage stoping with sublevel caving of the pillars, which produced 2,230,577 tons. 3. Undercut caving with hand tramming, which, produced 15,427,672 tons. Estimating December tonnage, the total ore mined to the end of 1929 will amount to slightly more than 43,000,000 tons. The first method was described by E. G. Deane1 and the second by D. B. Scott,1 and the third, together with a general, description of the mine, by J. H. Hensley, Jr.1 The geology of the district has been worked out by. Dr. F. L. Ransome.2

Jan 1, 1930

By M. L. Samuels

In a recent paper the authors1 discussed the reactions to tempering of hypereutectoid steels quenched from 1000&apos; C., as revealed by studies on changes in hardness, electrical resistivity, coercive force and metallo-graphic charaeteristics. The data, which related specifically to tempering temperatures of 550°, 650" and 710" C., for varying periods up to 125 hr., permitted the following important conclusions: 1. The rate of softening of the steels at the temperatures examined differed markedly although the steels were of "similar" general chemical composition. 2. The temperature of maximum softening spread over a range from about 650" C, to the eutectoid inversion. 3. The divergence in behavior was ascribed, at least in part, to a profound difference in tendency to graphitization on annealing at sub-eutectoid temperatures. 4. The mode of spheroidization of the cementite, as revealed by metallographic studies, also varied considerably in the different steels. The purpose of the present investigation is to pursue further the study of the difference in behavior of the steels on tempering over a wider range of temperature. To this end the following features have received particular attention: 1. Comparison of temperatures of maximum softening of the various steels when the quenched samples were tempered for 5 hi. and for 75 hr. followed by furnace cooling and by quenching in water. 2. Deterrnirlation of the effect of quenching temperature, prior to tempering, on the rate of softening. Quenching temperatures of 1000" and 850" C. were used in the investigations. 3. Examination of the microstructures obtained with the various heat-treatments employed.

Jan 1, 1938

By M. L. Samuels

In a recent paper the authors1 discussed the reactions to tempering of hypereutectoid steels quenched from 1000&apos; C., as revealed by studies on changes in hardness, electrical resistivity, coercive force and metallo-graphic charaeteristics. The data, which related specifically to tempering temperatures of 550°, 650" and 710" C., for varying periods up to 125 hr., permitted the following important conclusions: 1. The rate of softening of the steels at the temperatures examined differed markedly although the steels were of "similar" general chemical composition. 2. The temperature of maximum softening spread over a range from about 650" C, to the eutectoid inversion. 3. The divergence in behavior was ascribed, at least in part, to a profound difference in tendency to graphitization on annealing at sub-eutectoid temperatures. 4. The mode of spheroidization of the cementite, as revealed by metallographic studies, also varied considerably in the different steels. The purpose of the present investigation is to pursue further the study of the difference in behavior of the steels on tempering over a wider range of temperature. To this end the following features have received particular attention: 1. Comparison of temperatures of maximum softening of the various steels when the quenched samples were tempered for 5 hi. and for 75 hr. followed by furnace cooling and by quenching in water. 2. Deterrnirlation of the effect of quenching temperature, prior to tempering, on the rate of softening. Quenching temperatures of 1000" and 850" C. were used in the investigations. 3. Examination of the microstructures obtained with the various heat-treatments employed.

Jan 1, 1938

By P. Stark, B. S. Lement

ACCORDING to Hanemann1 the hardness of retained austenite in a 1.7 pct C steel is increased by subsequent tempering. He reported that the hardness of this constituent increases only slightly on tempering to 300°F, rises more rapidly above this temperature, and attains the same value as the tempered martensite present in steel at approximately 480°F. The variation of hardness of both retained austenite and martensite with tempering temperature as obtained by Hanemann1 is shown in Fig. 1. Hanemann attributes the increase in hardness of the retained austenite essentially to continued formation of fine needles of martensite on tempering. Although he did not explain the actual mechanism involved, work hardening of retained austenite by the plastic deformation associated with such martensite formation appeared to be a possibility. Recently Lement, Averbach, and Cohen2 reported the existence of subgrains, about l000Å in diameter, in retained austenite and suggested that they may be delineated by a subboundary carbide. This raised the possibility that carbide precipitation might be responsible for the hardening reported by Hanemann. In view of these conflicting possibilities, an investigation" was carried out on a high purity, Fe-C alloy containing 1.7 pct C in order to clarify the nature of the phenomenon involved in the reported hardening of retained austenite. This investigation involved correlation of changes in microhardness and microstructure of the austenite as a result of tempering. Microhardness tests were made with a Tukon tester using a 25 gram load and a Vickers diamond. It was found that two groups of austenite hardness values were obtained after tempering at a series of temperatures up to 450°F, which was the highest temperature at which retained austenite regions could be identified microscopically. One group represents a high hardness level which in-

Jan 1, 1955