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By H. Biloni, R. Morando

The surface structure and substructure of Al-Cu alloys solidified as conventional ingots and under particular conditions such as those used by Bower and Flemings are studied. The influence of lampblack coating on the mold walls is especially considered and the results compared with those obtained in copper and graphite molds where no coatings exist. When high heat extraction conditions exist the observations show that mechanism of copious nucleation is responsible for most of the chill zone. When the heat extraction through the mold walls is low, a coarse grain structure with dendritic morphology arises, with a size that depends on the degree of convection present, analogous to that analyzed by Bower and Flemings. In both cases the effect of the convection on the macroscopic and microscopic appearance is discussed. The ingot macrostructure consists of one or more of three zones: "chill zone", "columnar zone", and central "equiaxed zone". The mechanism of the columnar-equiaxed transition has been subject of considerable interest and at present at least three theories exist about the formation of the equiaxed region: 1) the constitutional supercooling theory1 maintains that the equiaxed crystals nucleate after the columnar zone has formed, as a result of the constitutional supercooling of the remaining liquid; 2) chalmers2 pointed out, however, that there were several objections to this proposal, and that consideration should be given to the possibility that all the crystals, equiaxed as well as columnar, originated during the initial chilling of the liquid layer in contact with the mold; 3) Jackson et aL3 and O'Hara and ~iller~ suggested that a remelting mechanism of the dendrite arms is responsible for the formation of the equiaxed region. After the work of Cole and Bolling and other authors6 it became evident that convection (natural, reduced, or forced) plays a very important role in the transition from columnar to equiaxed and on the size of the resultant equiaxed structure. Until recently the accepted explanation of the chill zone was that it occurs as a result of copious nucleation in the liquid layer in contact with the mold walls.798 The columnar region is a subsequent result of the growth of favorably oriented grains and, as a result of a selection mechanism studied by Walton and Chalmers,9 elongated grains with marked texture are formed. Recently, however, Bower and Flemings" using an ingenious laboratory experiment introduced the idea that the "copious nucleation" mechanism is not responsible for the formation of the chill zone and that the presence of convection, introducing some form of "crystal multiplication", plays a decisive role in the formation of the chill zone. Unfortunately, it is important to consider that for their conclusions Bower and Flemings extrapolated the results obtained in their special experiments to the case of conventional ingots, and that these authors only analyzed the macrostructures of the specimens. Let us consider the work by Biloni and chalmers" concerning predendritic solidification. These authors were able to show that a study of the segregation substructure of A1-Cu gives information about the nucleation and growth of crystals formed in contact with a cold surface. A spherical predendritic region characterizes the first part of every grain nucleated in contact with the surface as a result of the chill effect. The aim of this paper is to elucidate through the observation of the segregation substructure the conditions under which (in the Bower and Flemings type of experiments and in conventional ingots) either the nucleation or the multiplication mechanism gives rise to the structure in contact with the mold walls. I) EXPERIMENTAL TECHNIQUES The experiments were performed on two alloys: Al-1 wt pct Cu and A1-5 wt pct Cu. The purity of the aluminum was 99.99 pct and the copper 99.999 pct. The results obtained with both alloys were similar. In the Bower and Flemings type of experiments the apparatus employed to obtain rapid solidification against a surface was similar to that used by those authors. The liquid was drawn by partial vacuum into the thin section mold cavity. Plate casts were 5 cm wide and usually 7.5 cm high. The thicknesses of the cast were 0.1 and 0.3 cm. Two different materials were used for the mold, copper and nuclear-grade graphite. The internal mold surfaces were polished and left uncoated for some experiments. In other experiments, the copper or graphite surface was coated with a thin film of lampblack material. In some of these particular experiments one of the mold walls was left with an uncoated region (usually in the form of a cross). The conventional ingots were cast in graphite or copper molds. In different experiments the mold walls were sometimes uncoated or coated with lampblack material. The results obtained in conventional and Bower and Flemings copper molds were compared with those obtained with copper molds coated with a very thin film of graphite; the results obtained were essentially similar. The size of the conventional ingots was 5 cm diam and 7 cm high in all cases. The cast surfaces produced by the Bower and Flemings type of experiments and conventional methods were observed macroscopically and microscopically without any metallographic preparation. As Biloni and Chalmers showed," the observation of the chill surface can give considerable information about the structure and segregation substructure.

Jan 1, 1969

By N. J. Grant, B. C. Giessen, Paul Predecki

ALLOYS of gold, silver, and aluminum with elements of the groups BII, BIII, BIV, and BV were prepared by a rapid quenching technique (splat) and were examined by X-ray diffraction. Five new intermediate phases were found and will be described briefly herein. For the gold and silver systems, the concentration ranges having an electron/atom ratio e/a of 1.4 to 1.5 ("3/2 Hume-Rothery phases") were studied primarily. Master alloys were prepared from high-purity metals (99.9+ pct or better) by melting either in evacuated fused silica capsules or by nonconsum-able-electrode arc melting in an argon atmosphere. Small pieces, 20 to 50 mg, of each alloy were blast-atomized to form a splat, by a technique similar to that described by Duwez and Willens.1 The technique used for this study is described in detail in Ref. 2; it utilizes a resistance-heated graphite crucible with a small hole at the bottom, directed toward a metal substrate or quenching plate. The prepared alloy rests over the fine hole, through which it is expelled by an explosion shock wave in the form of fine droplets (1 to 50 µ) of molten metal onto a copper or silver substrate, which is maintained at about -190°C. The resulting very high cooling rates (see Ref. 2 for quantitative measurements) can prevent the process of nuclea-tion and growth in many instances, resulting in the formation of metastable phases. The splat particles were transferred to a GE-XRD5 diffractometer and maintained at -190°C, where they were examined with CuKa radiation. The samples were then allowed to warm to room temperature or were heated to higher temperatures until the equilibrium structures formed. Of fifteen alloy systems considered, nonequi-librium structures were encountered in six; these are described below and summarized in Table I. In the system Au-Sb a metastable £ phase (A3 type, hcp, a = 2.898 + 0.002A; c = 4.731 * 0.004A; c/a = 1.633) was found in the concentration range Au + 13 to 15 at. pct Sb. This phase is isomorphous with the stable phases in the systems Au-Cd, Au-In, and Au-Sn, all at an average e/a ratio of 1.4 to 1.5. The concentration range of one-phase metastable was deduced from the small amounts of supersaturated gold solid-solution phase present in the splat product. It was found that ? could also be retained by splatting onto a substrate held at room temperature: however, decomposed into the equilibrium phases Au + AuSb2 after heating to 200°C for 1/2 hr, or on holding the powdered splatted alloy at 20°C for several months. Calorimetric measurements will be made in an attempt to decide the question whether ? is metastable at all temperatures or whether it is a stable phase at low temperatures. There is evidence that another phase, possibly also close-packed but with a different stacking sequence, can be obtained by rapid quenching of alloys with a different antimony content. Klement, Willens, and Duwez3 reported the existence of an amorphous phase on quenching Au-Si alloys (25 at. pct Si) to - 196°C. They found that on heating to room temperature another phase of unknown crystal structure was formed. This was confirmed (see Table I); however, the new crystalline phase, designated as ?, could also be formed simply by rapid quenching to room temperature, and even was found to exist already in the as-cast Au + 20 at. pct Si alloy. It was found that ? decomposed into Au + Si on the specimen surface at room temperature. This behavior, and the question whether or not there is an equilibrium-temperature region for ?, have not yet been resolved. It is probable that ? (Au + 20 to 21 at. pct Si) is cubic of the -brass type (D81-3) with a = 9.60, + 0.01A and N = 52 atoms per cell [compare 6 (CU-Sn)4]. Except for two very weak lines, the powder pattern of about thirty lines could be indexed on this basis; however, a determination of the atom positions has not yet been attempted. For Au-Ge the C phase was observed at about 21 at. pct Ge as reported by Luo et at.5 Lattice parameters a = 2.876A, c = 4.73,A, c/a = 1.64 were found. In the Au-Pb system, formation of a ? phase was not observed, but in the lead-rich region at 75 at. pct Pb, broad peaks belonging to an amorphous phase were found. The maximum diffracted intensity occurred at 28 = 32.4 deg which is about 1 deg larger than the position of the (111) line of lead (Cuka). For Ag-Pb, an amorphous phase analogous to the one found in the Au-Pb system was observed; this metastable phase exists probably at about 75 at. pct Pb. Since no lead-rich alloys were tested, all alloys consisted of silver + amorphous phase at -190°C. In A1-Ge alloys, line-rich and complex powder patterns were obtained at about 30 at. pct Ge; they bear similarities to those of aluminum and germanium, but are of lower symmetry; the existence of more than one intermediate phase is possible. The authors are grateful to the Kennecott Copper Corp. for Fellowship support, and ARPA (Contract

Jan 1, 1965

By Juan Sodi, John F. Elliott

The standard free energy of ReS2 has been measured in the range of 1050° to 1250°K using H2/H2S mixtures and a slight variation of the method described by Hager and Elliott.1 The result is: The experimental method and apparatus were modified slightly for this study. Measurements on Cu2S were made to verify the application of the method to the work on ReS2. THE EXPERIMENTS AND RESULTS Briefly, the experimental method consisted of exposing a chip of copper or rhenium at a known temperature for 8 hr to a slowly flowing gas stream at the same temperature in which Ph2S and PH2 were known. The chip was withdrawn quickly from the hot furnace, and subsequently it was inspected for the presence of a sulfided surface. In the experiments described here, there was no ambiguity in any case as to the presence or the absence of the sulfide. At a given temperature, gas compositions for sulfidization were explored systematically until two compositions were found whose values of ?G°, Eqs. [I] and [2], were within approximately 100 cal of each other, one of which was sulfi-dizing and the other was not. These are termed the "straddle" compositions and it is assumed that the equilibrium composition lies between them. The chief modification to the apparatus, which is shown schematically in Fig. 1 of Ref. 1, was to support the metal specimen on a small alumina boat which could be moved along the reaction tube, 6 mm ID, by platinum wires. An appropriate seal at each end of the reaction tube permitted the sample to be moved from the cold end of the tube into the hot zone in 2 to 3 sec, and the sample could be withdrawn equally rapidly. Thus, it was possible essentially to quench the specimen from the reaction temperature with the reaction gas or helium flowing and without danger of breaking the reaction tube. The usual practice at the end of the experiment was to switch the gas system to the helium tank, flood the reaction chamber with helium, and pull the sample out of the hot zone. The purpose of the modification was to permit study of the sulfidization of copper without the complication of the back-reaction between the gas and the specimen as the latter cooled during slow withdrawal of it from the hot zone; this was a problem in the earlier work.&apos; A further improvement located the tip of the temperature-indieating thermocouple and the specimen precisely at the hottest part of the furnace. A carefully calibrated thermocouple, with its tip at the position of the specimen and with other conditions duplicating those of an actual experiment, showed that in the temperature range of 900° to 1122°C the temperature of the specimen differed from that of the tip of the indicating thermocouple by less than 0.5°C. The two positions were 0.5 cm apart. The reaction gas was prepared from ultrahigh-purity hydrogen (<l ppm O2, <0.5 ppm H2O) and CP grade hydrogen sulfide (99.5 pct H2S). High-purity helium (99.995 pct He) was used. All of these gases were purchased from the Matheson Co. All flow meters were recalibrated by the soap-bubble method with hydrogen, H2S, helium, and several gas compositions used during the study. These calibrations gave a linear relationship with a slope of 1.0 for the plot of log flow rate vs log pressure drop across the flow meter, in accordance with the Hagen-Poiseuille equation. The analysis of the gas was determined in the same manner as was reported previously. Good checks were obtained between the composition of the gas established by the flow-meter settings and by chemical analysis of the gas taken after the mixing bulb and ahead of the furnace. The pressures of H2S, H2, S2, and HS in the equilibrium gas at temperature were calculated from the following data :3 The pressures of the species S and S8 were negligible for the conditions of the experiments.3 There was no sign of vaporization of ReS2 either by weight loss or deposits in the reaction tube. Thus it is not possible to account for the apparent volatility of the compound reported by Juza and Biltz.2 The inlet gas composition and the calculated equilibrium ratio of PH2 S/PH2 for the "straddle" points of each experiment are shown in Table I. The specimens of metal for the experiment were small clippings of annealed copper (99.9+ pct) sheet 0.005 in. thick that was obtained from Baker and Adamson and of "high-purity" rhenium (99.9+ pct) sheet 0.005 in. thick that was purchased from Chase Brass and Copper Co. A specimen was removed from the apparatus; inspected for the presence of the sulfide, and then stored in a sealed vial. A fresh clipping was used in each measurement. The condition of the surface of each specimen after the experiment is noted in Table I.

Jan 1, 1969

By J. Leslie Goodier

The International Law of the Continental Shelf, so far ratified by 35 nations, extends the national boundary of any coastal nation to the edge of the continental shelf, this normally being at a continuous water depth of 200 m. The Law further extends this boundary to include the floor of the deep ocean to any depth that can be mined by advanced mining technology. In effect, proof of mining can constitute proof of ownership of the subaqueous land and the minerals on or below the sea floor. Irrespective of the fact that present technology is too limited to permit mineral exploitation in the high seas-and the law regarding the right to mine appears hazy-the U. S. Treasury Department&apos;s Bureau of Customs, has a ruling that would further deter mining operations on the high seas. This law contends that minerals mined on the continental shelf of the United States are actually mined within the continental United States and are free of tariff, but mined products or other articles obtained from the ocean or the sea floor beyond the continental shelf, if brought into this nation, must be considered as imported and are subject to such customs duties as are applicable under the tariff schedules of the United States.

Jan 7, 1968

By AIME AIME

ASIDE from the annual dinner-dance, the two outstanding social events of the Annual Meeting were the dinner- smoker on Monday night and the informal dance on Tuesday night, both of which were held at the Commodore Hotel. Approximately 400 attended the former event, compared with 570 a year ago, and about 250, people were attracted to the dance.

Jan 1, 1933

By Ernest J. Stocking

ENGINEERS are the key men in our war program today. Upon the technical knowledge and skill of the engineer and upon his administrative and executive abilities rests the entire success for the production of vital materials of the war. Naturally the work load of the engineering examining unit of the U. S. Civil Service Commission has increased greatly since our active participation in the war. At present, over 550 separate requests for certification of eligibles are received by the engineering unit per week. These represent more than a fourth of the total requests received for personnel by the Commission&apos;s central office at Washington and represent a recruitment work load of three to four times that carried by the whole Commission previous to January 1940. These requests represent a minimum of a thousand vacancies to be filled each week, while an average week will produce, at present, approximately 1400 vacancies and a weekly maximum may approach well over 2000 vacancies.

Jan 1, 1942

By William B. Plank

RECENT interest in the character of employment of young mining engineering graduates has been stimulated by my studies, during the past ten years, of student enrollment and employment of graduates of the mineral technology schools of the United States and Canada. Enrollment data in the following article are taken from these studies and information about the kind of work engaged in by mining engineers is assembled from my professional experience, sixteen years of which have been as professor of mining engineering.

Jan 1, 1938

By L. W. WALLACE

IN an engineering fashion we have made an assay of the engineering profession, using as a. sample the engineers listed in "Who&apos;s Who in America" (1928-1929). We are aware that some will say it is an unfair sample; that it came from the best mine. This is readily admitted, with this qualification: that all engineers and architects by virtue of their training and experience have been freed of most of the dross to which mankind is heir. They are -a selected group to begin with, having all the potentialities those in the sample possess. We are also aware that some will say a part of those included in the sample are not engineers. Our answer to that criticism is this: An engineer is no less an engineer because for the time being he is president of a bank, a university, an opera company, or a hotel company. Moreover, he is no less an engineer because he is a governor of a commonwealth, a United States senator, a member of the Cabinet, or the President of the United States.

Jan 1, 1929

By Wm. E. Milligan

DESPITE the zero weather of Monday, the morning meeting on nonferrous ore-reduction metallurgy got under way promptly under the efficient control of Arthur A. Center. The first and third portions of the paper on the Tri-State region were presented by B. M. O&apos;Harra, with R. H. Lowe substituting for co-author Illidge on the second part. Attention was drawn to the compact design attainable when "Sink and Float" was employed as a means of primary concentration. The teaching profession should welcome this concise correlation of data from such a renowned center of lead and zinc production. H. R. Hanley and C. R. Hay¬ward were much interested in the mechanics of charging, manufacture, and life of the retorts.

Jan 1, 1943

By Charles H. Fulton

FOR some time it has been thought that there should be > closer relationship between the members&apos; of the Institute engaged in education in the mining schools, the mining, metallurgical, ceramic, and geological departments of universities, and the members of the Institute actually engaged in the production of mineral products and the operation and direction of works. The American Society of Chemical Engineers and the American Ceramic Society have for some years past devoted especial attention to the educational matters of their respective fields. The Engineering Foundation, representing the great engineering societies of the country, is deeply interested in technical education and maintains a Committee on Educational Research.

Jan 1, 1932

Jan 1, 1907

Albert Arents, Alameda, Cal.: From Mr. Furman&apos;s description of his crucible-assays I infer that he regards iron nails as a necessary or advisable adjunct. Against such a notion I must beg leave to protest. Nails should not be used in

Jan 1, 1896

Extremes in temperature and weather, along with the highly corrosive nature of acid leach solutions used at open-pit copper mines, necessitates the use of pipeline systems that are both corrosion resistant and impervious to the environment.

Jan 6, 1976

By AIME AIME

INSTITUTE members attending the Annual Meeting in New York who want to see one of the mining engineers&apos; newest aids, photoelastic stress analysis, are due for an interesting afternoon on Thursday, Feb. 15, when open house: will be held at the Columbia University mining laboratory. Information as to the direction and distribution off stresses in mine structures, which has been developed by Professor Bucky, associate professor at the Columbia School of Mines, and David Sinclair, research assistant, is useful in the design of pillars and in the placing of openings relative to working places such as gangways and haulage levels.: This work has been sponsored during the last ten years by the Engineering Foundation.. It is fully reported in T. P. No. 1140.

Jan 1, 1940

THERE have been two important accomplishments of the Truman administration; the Hoover Commission report on inefficiency and waste in government and the report of the Paley Commission on the natural resources of the United States. Both reports are in the interest of the American people and should transcend the boundaries of political parties. Both reports are starting points for the formulation of policies which must be continuously revised to meet changing conditions. Regardless of the outcome of the election the principles embodied in these two great documents must be kept alive. The Paley report is right in our own bailiwick of mineral raw materials and it behooves us to study it carefully as our responsibility to posterity. To those in the mining industry who have limited their field of observation to moving rock or to metal prices it may come as a surprise that our production of such staples as copper, lead, and zinc has fallen behind increased requirements to the point that substantial tonnages must be imported. Iron ore is next on the list and everybody knows that such metals as tin, tungsten, chromium, manganese, nickel, and cobalt are imported almost exclusively. The crisis in raw materials pointed up by the Paley report has been reported annually by Elmer Pehrson and others to small gatherings at the Mineral Economics Division sessions at the Annual Meeting for as long as we can remember. In September 1949, the United Nations Economic and Social Council held an international resource conference at Lake Success which disclosed these same grave conclusions: - Consumption of raw materials is multiplying at an alarming rate, faster than discoveries or replacements are being made. - Production has been wasteful and utilization lavishly beyond enginee¬ing and practical requirements. - Industrialized nations are depleted and many raw materials consumed by industry are not found in the industrialized countries. - Nations formerly exporters of raw materials are increasingly building their own consuming industries. - Political forces in the world are limiting access to raw materials. The Paley Commission selecting the quarter century, 1950 to 1975, to project raw material requirements for the United States, pointed out obstacles to meeting these requirements, and made recommendations for procurement. It is not important that we disagree that cobalt consumption will reach 344 pct of present, or fluorspar 187 pct when iron and ferroalloys are only expected to increase 75 pct. What is important it that the fabulous appetite of the United States for mineral raw materials has consumed more since World War I than was consumed by the entire world in all recorded history prior to 1914. And, unless the people of the United States are satisfied to remain at their present standard of living (which is unthinkable) this consumption is correctly plotted by the Paley Commission as continuing to expand. If the U. S. is to continue on a course of progress, it must procure raw materials wherever it can at the lowest possible cost. Natural resources are clearly an area in which the broadest cooperation between industry and government must exist to achieve efficient exploitation, economic consumption, and expansion of sources of supply. The message of the Paley report requires action comparable to that of the North Atlantic Pact. Its implication is as significant as military preparedness. It is a world problem. It is a mining engineering problem. Don&apos;t let it die!

Jan 1, 1952

By S. G., Lasky

IT seems to be in the nature of concepts that they have many meanings, and that the meaning best reflecting the primary interests of a person tends to be accepted by him as the normal meaning of the concept. The concept of ore reserves is no exception, for there is no unanimity of meaning among the several groups of us who are interested in ore reserves, nor even among the individuals of a single group. The groups most interested in ore reserves would seem to include at least the mining industry, perhaps State taxing agencies, and the Federal Government in all its diversified activities, and I would include also the citizenry at large or at least that part of it that consciously thinks about problems-of national welfare. To each of these, and to different individuals within them, the term reserves represents something different, and the farther away the individual or group gets from physical contact with the ore, the more abstract does his or its concept become. It is something different to the policy maker from what it is to the fact-finder or to the miner.

Jan 1, 1945

By BERNARD PLANNER

PRODUCTION COSTS, profits, and quality are the primary factors in the peacetime production of iron and steel. In a war emergency, as high production rates and as complete utilization of readily available raw materials as possible, consistent with securing passable quality, become the most important factors. In this connection a discussion of some of the recent developments in the German iron and steel industry, where the problem of scarcity has naturally always been more acute than in the U.S.A., maybe of interest. To get more pig iron out of the existing blast furnaces it was necessary to obtain the maximum efficiency from the iron-bearing raw materials. This was achieved by eliminating all "excess baggage," chiefly by beneficiating the ore. The preparatory work for this was done by various methods which are effective when the ore either is too poor or contains too many impurities or too much gangue. Some of the beneficiation methods are well known, some are combinations of wet-mechanical, magnetic, roasting, sintering, and other treatments.

Jan 1, 1942

By C. H. White

Discussion of a Paper by Mr. C. H. White, read at the Atlantic City Meeting, February, 1904. (Annual Meeting, February, 1005.) ARTHUR JARMAN, Sydney, New South Wales, Australia (communication to the Secretary*) : All designs for modern metal¬lurgical and chemical laboratories should provide each student&apos;s desk with a hood or cupboard for the removal of fumes, but I doubt the advisability of placing air-baths and similar apparatus close to the hot plate. It seems to me that unless the draft be exceptionally strong the fumes from ordinary wet assay work will corrode the iron-work of the fittings, in which case the baths would have to be removed to a general desk in order to lighten the work of the laboratory attendant. Since the laboratory described by Mr. White has been in use for two years, I should like to ask if any inconvenience has resulted from this corrosion. If not, it is certainly an important improvement to have the air-baths and similar apparatus placed -on the student&apos;s desk. The hoods described by Mr. White are supplied with a good draft by means of a fan, which gives them a great advantage over those at the metallurgical laboratory at the University, Sydney, in that no doors to the hood are needed. Each hood in the laboratory at Sydney is connected by a glazed earthenware drain-pipe with a vertical flue, 20 ft. high, having a lighted gas jet at the bottom to assist the draft. Although the draft is good, fumes of sulphuric acid cannot be drawn o$ unless the doors of the hood are lowered more than half-way. In my opinion, a fan should be used for the purpose of creating the draft, and glazed drain-tile should invariably be used for the flues because no other material possesses the same advantages. I know of a recent instance in which a laboratory containing

Mar 1, 1905

By AIME AIME

IN an address before the New York Section. A.I.M.E., Oct. 20, Alex L. ter Braake, speaking on the tin industry of the Netherlands East Indies, interjected a few remarks, at the chairman&apos;s request. on the mineral stock-piling project now before Congress in a bill sponsored by Senator Scrugham. The full text of Mr. ter Braake&apos;s paper was published in the Nov. 6 issue of the American Metal Market. Following mention of the buffer stock scheme as applied in the tin industry, Mr. ter Braake continued:

Jan 1, 1943

By C. E. MacQuigg

BY and large the education of the engineer has been conservative and the reasons for this are obvious. Quite properly it has been a tradition of engineering education that facts and not fancies must be adhered to. Without a doubt, those men who formed the mold of our engineering philosophy as much as it is possible for such molds to be established-rightly held the highest standards of intellectual honesty. Fortunately, it was unthinkable to them to temporize with untried theories and naturally the men whom they trained as engineering educators carry this philosophy in turn to their students, thus handing down the tradition of stability.

Jan 1, 1943