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IN GATHERING material for this chapter on Yerington and the one to follow on Silver Bell, the A.S.& R. project near Tucson, Arizona, I was fascinated at the way the two stories paralleled each other. For example, here are a few instances: (1) The first copper mining in the Yerington district of Nevada was in the late 1860's; the first in the Silver Bell area in 1873. (2) Each district was served by a branch railroad about 25 miles long from a main line of the Southern Pacific (by quizzical coincidence); and, in each instance, the railroad was later abandoned and torn up. (3) Each district had a sizable blast-furnace smelter ten or fifteen miles from the principal mines, and in each instance the smelter was later dismantled for junk. (4) Up to 1954, the Yerington district was credited with a production of 100,000,000 lb of copper; the Silver Bell district with 80,000,000 lb. (5) In each district the entire production had come from deposits other than the low-grade ore bodies now being exploited. (6) In each instance, existence of the low-grade deposits of the Porphyry type was recognized in the period circa1910-1914 and a substantial amount of exploratory drilling had been done, on one deposit at Yerington and on two at Silver Bell. (7) In each instance, the properties containing the Porphyry ore were acquired by a strong company (Anaconda Copper Mining Company at Yerington and American Smelt-

Jan 1, 1957

Since 1571, when the Institute was founded, many of the most important papers in the English language, on the various phases of mining and metallurgy, have appeared as Institute publications. As members of the Institute regularly receive the publications in which they are interested, this discussion is primarily for nonmembers who wish to know of them. The Institute has several means of issuing papers which have been submitted and accepted. The monthly journal, Mining and Metallurgy, is the magazine of the Institute. In it appear notices and reports of official business as well as many papers and contributions which do not appear otherwise. The annual subscription price of the magazine to nonmembers is $3 per year; Canadian and foreign postage $1 extra; single copies 50 cents; back issues $1 each. Many papers are published separately each year. They are issued in one or the other of two numbered series; namely, Technical Publications and Contributions, and of the latter there are four forms: Preprints, Mimeographs, Reprints, and Unpublished Manuscripts. A Technical Publication or Contribution (in any form) is issued by the Institute when it is listed in Mining and Metallurgy. Technical Publications are sent automatically to members who have asked in advance for papers on a given subject. All members are entitled to a copy of every paper in either series, except when a Contribution is an Unpublished Manuscript. Con¬tributions in the form of Unpublished Manuscripts are filed in the Engineering Societies Library and copies of some of these papers may be found in a few selected libraries throughout the country.

Jan 1, 1933

By W. A. Knoll

THE sinking of a new shaft at the Newport mine, Ironwood, Mich., was started in May 1931 and completed on Aug. 3, 1932. During this period, 2665 ft. of shaft in granite was completed, at, an average advance of 6 ft. per 24 hr. In November of 1930, experimental work was con-ducted oil 65 ft. of shaft through 22 ft. of overburden where ledge was encountered, and this work convinced the operators that all drilling could be clone with vertical holes with the blasting relief to a 4 ½ -in. hole drilled vertically in the center of the cut. The reason for not adopting the conventional V-cut was to get away from damaging the shaft steel. The blasting in a V-cut naturally tends to throw the broken material upward, but with the cut as adopted the relief was in a horizontal direction to a large extent. The scheme of mucking employed made it necessary to keep the steel shaft sets within 511 ft. of the bottom at all times. This could not be clone without serious damage with a V-cut when blasting in granite. The cut as drilled also broke 10.53 ft. per round of drilling, which was considerably more than the experience with a V-cut in the sane material. The extended cut reduced proportionately the delays for charging, blowing smoke and handling drilling equipment in the shaft. Another advantage was the ease in drilling vertical over inclined holes, and the preservation of the proper spacing of the drill holes at the bottom of the cut.

Jan 1, 1938

By G. W. Crane

WHEN ore was discovered on the Tintic Standard property in the spring of 1916, new developments were immediately started both north and south of that property, on the supposition that in East Tintic the ore would be found to occur in northerly trending channels, similar to those so characteristic of the older camp. But 9 years of developments have failed to establish the existence of such a channel. This is due undoubtedly to important differences in the geology of the two camps, that were not recognized, and is indicative of the danger in the general tendency toward interpreting the geology of East Tintic too strictly in terms of that of the older camp. It should not be forgotten that while the two sections have had practically the same geological history, the net results of a long series of geologic processes have developed in them conditions that differ so widely and in so many particulars that the necessity of regarding them as essentially different districts seems apparent. In an effort to emphasize this fact, this paper is devoted chiefly to a comparison of the geological conditions as found in the two camps and is addressed more particularly to those familiar with the geology of the Tintic district. Following a short description of the several ore discoveries and of the Tintic Standard mine is a brief discussion of the evidence of ore channels in East Tintic. For my information regarding the Tintic Standard mine, I am indebted to the courtesy and generous assistance of Messrs. Wade and Snow of the Tintic Standard Mining Co.

Jan 9, 1925

By Jean A. Andre

In 1969 "Société des Mines et Fonderies de Zinc de la Vieille-Montagne" produced 221,000 tons zinc ingots and 22,000 tons zinc dust, thus rating highest on the world's zinc producer list. The Company's plant at Balen, Belgium, with an output of 135,000 tons electrolytic zinc is the most important one of this group; it is an integrated metallurgical zinc and lead unit with recovery of most by-products. The present paper describes the zinc production facilities. The roasting section includes four fluid bed roasters (total concentrates charged: 740 tpd) and two sulfuric acid having a corresponding capacity. Calcine is leached in a fully automated plant by a two-step continuous process. Leaching residues, mixed with lead furnace slag, are treated in a shaft furnace. The recovered zinc fume is leached separately. In the near future, the leaching residues are to be treated by a wet process, developed in the Company's own laboratories. Purification of solutions is accomplished in two steps: antimony and zinc dust are added in the first one, only zinc dust in the second one for removal of cadmium. Electrolysis cells are partly of a conventional type. A new type of cell configuration was put onstream in October, 1969, planned output 60,000 tpy. Main features of the new cell rooms are the fully automatic pulling, stripping and replacing of the jumbo-size cathodes (immersed area 2.6 m2). Zinc cathodes are remelted in induction furnaces followed by in-line automatic casting and stacking machines.

Jan 1, 1970

By Edward H. Robie

THOUGH the final figures are not available as this is written, it seems certain that the Institute accounts will show $7000 to $8000 surplus for the year 1951. This is the first time this has happened since 1941. No money had to be taken from any of the Funds to bring about this happy condition. Furthermore, the amounts allowed for depreciation, bad debts, and inventory adjustment were more liberal than in the past. Income increased some $29,000 over 1950. Dues received from old members increased moderately, but dues from new members dropped off $2000 and from initiation fees quite severely-from $17,000 to $11,000. The number of new members did not come up to expectations and a change in procedure caused a delay in getting some of them on the rolls. A large number of the new members paid an installment of $5 on their initiation instead of the full $20. Junior Members, of course, pay no initiation fee. Brightest spot in the income picture was the increase in advertising income-from $103,000 in 1950 to $143,000 in 1951. All three of the journals shared in this, Mining being up $18,000; Metals, $9000; and Petroleum $13,000. Nonmember sales of the journals dropped off slightly, and sales of Transactions volumes more so from $35,000 in 1950 to $27,000 in 1951, with a further drop of $5000 accounted for by a change in accounting procedure. On the other hand, sales of other publications increased by $10,000.

Jan 1, 1952

By Frederic P. Dewey

The improvement in leaching introduced by the Russell process has stimulated the development of processes for refining lixiviation-sulphides. In the early days several processes for dealing with the sulphides were proposed, and some of them were tried more or less ; but the business finally settled down to sending the sulphides to the smelters, although this was known to be both troublesome and expensive. In 1891 Mr. C. A. Stetefeldt* introduced at the Marsac mill, Park City, Utah, an unpatented process, built up out of the general fund of information available. It consisted in matting the sulphides, grinding, roasting, grinding again, and dissolving the copper out in diluted sulphuric acid, then melting the silver and crystallizing the bluestone. It did not yield fine bullion, hence the bullion had to be refined as well as parted; besides, there was some loss. This process was thoroughly tried at the Marsac refinery and then a year's run was made, the net result of which was that it did not prove sufficiently better than the sending of the sulphides to the smelters to warrant its substitution for that practice. In 1893 the Dewey-Walter Refining Company undertook the refining of the Daly sulphides in the Marsac refinery by the sulphuric acid process, upon which two United States patents ? have been issued to the writer. Naturally, difficulties were encountered in starting a new process, and most of 1893 was taken up in getting it into smooth working order; but in 1894 a run was started, in which all the regular sulphides produced by the

Jan 1, 1897

By P. F. Gnirk

Consideration is given to creater formation with shallow, contained, chemical explosions in rock masses which exhibit different inherent physical and mechanical properties as determined by standard laboratory techniques. The primary purpose is to determine whether or not a simple but useful generalized correlation can be established between explosive crater formation and one or more common rock properties. Such a correlation could be beneficial in predicting with some degree of reliability the size of a crater which could be expected in a particular rock type for a given input of explosive energy. A series of crater formation experiments employing constant weight charges of Gelex 2 explosive was conducted in five submembers of the taconite formation at the eastern end of the Mesabi Range in northeastern Minnesota. Five mechanical and physical properties-unconfined tensile and compressive strengths, Young's modulus of elasticity, longitudinal wave velocity, and density-were determined by conventional laboratory techniques using core samples from the taconite submembers. Although insufficient data were obtained to warrant the use of mathematical methods in the determination of empirical relationships, the results provided a fairly strong indication that with an increase in magnitude of any one of the five rock properties definite decreases in the optimum crater volume and surface area occur. Furthermore, for a constant explosive energy input, the presence of bedding planes and joint systems in a rock mass influences the formation of craters in such a manner as to increase the volume of rock broken substantially above that expected from the same rock mass without joint systems and, in particular, without bedding planes.

Jan 1, 1968

By Donald R. Reichmuth

Most brittle solids are relatively weak in tension and this weakness can be very significant in determining their performance in structures and excavations. Consequently, accurate knowledge of the tensile strength of brittle materials has long been recognized as important. In the past, measurements of the tensile strength of materials such as concrete, ceramics, and particularly rock have been hindered by problems encountered in fabricating test specimens and in accurately loading them. These difficulties have resulted in a scarcity of published tensile strength data. This can be readily seen in tabulations such as Wuerker's "Annotated Tables of Strength and Elastic Properties of Rocks."1 There are now three distinct approaches being used to determine the tensile strength of brittle materials. These are shown schematically in Fig. 1. The first method consists of simply pulling the specimen apart by applying an axial load. Although this procedure is the easiest to understand, the technical problems encountered during testing are numerous. Specimens cannot be readily fabricated into dumbbell-shaped specimen* like those customarily used for testing inetals. Cylindrical specimens cannot be loaded in jaw-clamps because adverse stress conditions arise at the clamping points, which causes unreliable results. An innovation developed by Niles Grosvenor at the Colorado School of Mines, in which the load is applied through steel-end caps glued to the ends of the specimens, has considerable merit, hut the samples are costly to prepare.2 All tests using a direct pull are further handicapped by the possibility of small amounts of bending being present, the specimen's surface condition, and

Jan 1, 1968

By E. C. Harder

IN view of the gradually decreasing known reserves of high-grade manganese ore and the rapidly increasing consumption of iron-manganese alloys in the steel industry, it is well to turn our attention to the development of low-grade manganiferous ore deposits and to the utilization of these ores in steel manufacture. The dependence of this country on imported manganese ore and ferromanganese has been forcibly brought to the attention of steel makers during the last few years by the cessation of manganese-ore imports from Russia, the restriction of manganese-ore imports from India and of ferromanganese imports from Europe. Should the importation of manganese ore from Brazil cease, the steel industry of this country would face a serious situation. The present practice of steel making requires ferromanganese in large quantities and ferro-manganese of the grade used at present can be produced only from high-grade manganese ores such as the United States appears to possess only in insignificant amounts. There are in the United States, however, large reserves of manganiferous iron ore which could probably be used extensively in the steel industry if certain changes in the practice of steel manufacture were made. Thus high-grade manganese ore could be conserved. Among the most important deposits of manganiferous iron ore in this country are those of the Cuyuna iron-ore district of Minnesota. It is probable that in case of restriction of foreign supplies, the users of manganese in the United States would have to rely to a large extent on the Cuyuna district to make up the shortage.

Jan 9, 1917

By W. Kennedy

THROUGHOUT northeastern Texas we have an extensive series of iron-ore deposits, occupying portions of nineteen counties and having approximately an actual ore-covered area of 1000 square miles. The existence of these ores has long been known. Kennedy* says: "Iron-ore is distributed in profusion throughout Texas, being found almost everywhere except in the level region of the coast." Before this, C. Newell† had mentioned the existence of these ores thus: " Iron is found in abundance in the eastern, northern and middle portions of Texas;" and in 1849 Edward Smith‡ said: " We met with immense hills of iron which were said to be, and appeared to be, of excellent quality, in Cass and Titus counties.. . .. It is well known that Texas abounds with iron of first-rate quality." In 1859, Dr. Shumard? reports that detailed surveys had been made in several counties, and says: " Our labors have demonstrated the important fact that we have a vast iron-region in the eastern part of the state, embracing considerable areas in Cass, Harrison, Rusk, Panola, Smith, San Augustine and Shelby counties. The ore-deposits belong to the Tertiary era and consist chiefly of hematites and limonites, of which there are several varieties. We have also found in this district extensive beds of carbonate of iron." Dr. Shumard gives no very exaggerated description of Cass county§ as it then existed when he says : " Cass county alone is capable of supplying a number of furnaces with an abundance of excellent iron-ore for many years." Of Rusk county he says: "Our de-

Jan 1, 1895

By G. Van Esbroeck, M. Van Weyenbergh

The copper mines of the Katanga region in the Belgian Congo lie along the same mineralized belt as those of Northern Rhodesia. There are two distinct types of deposits in that belt, the dolomitic and the quartzitic. In the dolomitic type the metallic minerals are found in a dolomitic limestone country rock. Through oxidation and enrichment, large deposits of high-grade oxidized copper ores were formed, some of which are being worked by the Union Minière du Haut Katanga. Such deposits are all in Katanga. The quartzitic deposits are found in Katanga and Northern Rhodesia. Here the primary mineralization occurred in sandstones and quartzites, in horizons stratigraphically lower than the dolomites. These rocks are not favorable to secondary enrichment and the oxidized zone is poorer than the sulphide zone, which alone contains the ore. There are also in Katanga a few ore-bearing veins. One of them is being worked in the Prince Leopold mine at Kipushi. Prince Leopold Mine The Kipushi ore body fills a fault vein and invades the wall rocks more or less extensively by metasomatic replacement. The vein strikes north-northeast and south-southwest and dips to the west. The variable dip averages 60' to a depth of 300 ft., and more uniformly 80' below 400 ft. In the upper section the average width is 200 ft. and below the width is about 150 ft. The length of the ore body is 2300 feet. The eastern side of the vein—the footwall—is dolomitic and contains irregular masses of ore sometimes extending 100 ft. or more from the main

Jan 1, 1940

By M. Van Weyenbergh, G. Van Esbroeck

The copper mines of the Katanga region in the Belgian Congo lie along the same mineralized belt as those of Northern Rhodesia. There are two distinct types of deposits in that belt, the dolomitic and the quartzitic. In the dolomitic type the metallic minerals are found in a dolomitic limestone country rock. Through oxidation and enrichment, large deposits of high-grade oxidized copper ores were formed, some of which are being worked by the Union Minière du Haut Katanga. Such deposits are all in Katanga. The quartzitic deposits are found in Katanga and Northern Rhodesia. Here the primary mineralization occurred in sandstones and quartzites, in horizons stratigraphically lower than the dolomites. These rocks are not favorable to secondary enrichment and the oxidized zone is poorer than the sulphide zone, which alone contains the ore. There are also in Katanga a few ore-bearing veins. One of them is being worked in the Prince Leopold mine at Kipushi. Prince Leopold Mine The Kipushi ore body fills a fault vein and invades the wall rocks more or less extensively by metasomatic replacement. The vein strikes north-northeast and south-southwest and dips to the west. The variable dip averages 60' to a depth of 300 ft., and more uniformly 80' below 400 ft. In the upper section the average width is 200 ft. and below the width is about 150 ft. The length of the ore body is 2300 feet. The eastern side of the vein—the footwall—is dolomitic and contains irregular masses of ore sometimes extending 100 ft. or more from the main

Jan 1, 1940

By R. E. Shinkosk

This paper outlines the development of a program for increasing the life of woolen bags used for filtering Dwight-Lloyd gases by treating the bags and gases with hydrated lime. Methods and apparatus are described for determining alkalinity of dusts, acidity and breaking strength of bag cloth. Procedure and results, based on several years of operation, are presented. DURING 1939, additional facilities were constructed in the Dwight-Lloyd Blast Furnace and Baghouse departments at the Selby, California, Plant of the American Smelting and Refining Co. In order to handle adequately the increased volume of gases from the resultant increase in production, it was necessary to increase gradually the amount of water used for cooling gases ahead of the sinter machine baghouse. As a result of this increased water cooling, the average bag life dropped from 27 months in 1939 to 14 months in 1941. (Table I). This drop in life meant an increased. bag cost, as well as lower recovery of dust and some curtailment of operation. During 1941, it was found new bags showed as high as 0.3 pct acidity* after two weeks of opera- tion and as much as 2.0 pct acidity after some months of operation. This high acidity was present in spite of the fact that free oxide or relative alkalinity of the unburned dust ran from 5 to 6 pct. In view of these circumstances, a twofold program was started in Nov. 1941.t Part one of this program consisted of vigorously dipping all new bags in a weak lime solution, containing 50 lb of hydrated lime per 50 gal of water. Part two consisted of feeding fine, dry, hydrated lime into the gas stream intake of the sinter baghouse fan. Apparatus for feeding this lime is shown in fig. 1. All baghouse chambers are shaken in rotation about once each hour. On alternate hours, the baghouse operator places 50 lb of hydrated lime (one sack) into the lime feeder, starts feeder and immediately starts the bag shaking machinery. The rate at which lime is fed is set to coincide with the approximate time necessary to shake all sinter bag-house chambers, or about 15 min. It is felt this method of lime addition is most effective for getting lime into the woolen bag fabric. The amount of lime so fed averages about 600 lb per day. The amount of lime fed per day is varied to keep a minimum relative alkalinity of 9 pct in the unburned sinter dust. A daily dust sample is taken for alkalinity by allowing dust to accumulate in a sample pipe over a 24-hr period. This sample pipe, placed in any chamber cellar, is 2 in. in diam, 4 ft long, is sealed on the inner end, and capped on the outer end. It has a 1/2 in. slot cut for 18 in. along the tip end. This slot faces upward and allows the pipe to fill gradually with dust as bags are shaken. Breaking strength of bags has, in most cases, been the deciding factor in bag replacement. Bags that normally test 100 psi breaking strength when new are replaced when they test under 35 lb. The method for determining breaking strength is shown in the description accompanying fig. 2. Since the start of the liming program in 1941, bag life has increased from 14 months to an average of over 23 months, with a consequent material decrease in bag cost per year. Acidity, as per cent sulphuric acid, may be determined by means of a Beckman pH meter as follows: From a piece of bag cloth. which has been thoroughly cleaned of dust, a 5 g sample is weighed on a balance. Cut the sample into fine pieces and place in a 400 cc beaker. Add 100 cc (measured) of distilled water and stir vigorously. Filter on suction funnel, holding cloth pulp in beaker with a stirring rod. Wash cloth sample and filter wash water four additional times, each time with 20 cc distilled water, the last time squeezing cloth pulp over funnel. Discard pulp and rinse funnel and filter paper. Pour wash solution jnto measuring graduate and make up to exactly 300 cc with distilled water. Place into clean 600 cc beaker and measure the pH on meter. The per cent acid in bag cloth is read from the following table:—

Jan 1, 1951

By P. C. J. Gallagher

A number of recmt determinations for the ratio of extrinsic to intrinsic stacking fault energy in fcc solid solutions are examined. Some of these arise from incomplete analyses which can yield only approxi?nate values for the ratio. Reliable results, on the other hand, obtained using extrinsic-intrinsic fault pairs, show that the extrinsic and intrinsic fault energies are essentially equal in several materials. There is some reason to believe that this finding is of general applicability to fcc elements and alloys. A wide range of values has been obtained for the relative magnitudes of the extrinsic and intrinsic stacking fault energies (yext and yint, respectively) in recently published studies in a variety of materials. In contrast, Hirth and Lothe' using a central force model have shown that out to tenth nearest-neighbor interactions the perturbation in energy caused by both types of fault is the same. Although the model used is not completely valid in metals, there is nevertheless some indication that marked variations of yext/nnt should not be observed from one material to another. In early work in Cu-A1, Cu-Ge, Ni-Co, and stainless steel all the deformation faults observed in the electron microscope were found to be intrinsic in nature, which led to an attitude that the extrinsic fault energy must be considerably greater than the intrinsic. Extrinsic faulting arising from deformation has, however, more recently been directly observed in Au-4.8 at. pct n;~ Ag-6 at. pct Sn and Ag-8 at. pct sn; Ag-7.5 at. pct In and Ag-11.8 at. pct 1n;"' pure silwer and Ag-0.5 at. pct ~n;' and Cu-22 at. pct Zn, Cu-30 at. pct Zn, and Cu-7.5 at. pct ~1.l' Multilayer loops containing extrinsic faulting have also been observed in quenched aluminum." While peak asymmetries in X-ray faulting probability studies were generally attributed to the presence of twins,Lelel2 has recently reinterpreted earlier X-ray data in Ag-Sb alloysU in terms of the presence of extrinsic faulting. The determinations of yeXt/yint made from the above studies are shown in Table I, with a brief description of the techniques employed. A number of the methods utilized are deficient in one or more respects, and the reliability of the values listed will be discussed. ~ele'~ recognizes that his approximate determinations of yext/yint assumes equal numbers of extrin-sically and intrinsically faulted dislocations. It is well-known, however, that such an assumption is not at all justified since extrinsic faulting has but rarely been observed in samples studied in the electron microscope. The only conclusion that should be drawn from the X-ray results at present is that the total intrinsic scattering cross section (i.e., the product of the width of the intrinsically faulted dislocations with their density) is approximately ten times greater than for extrinsic faulting in these particular samples. An important point is that the relative magnitudes of the energies cannot be inferred from results of this type, unless the intrinsic and extrinsic faults form with equal ease. One must recognize that, although a formation barrier may restrict the amount of extrinsic faulting which occurs, this in no way implies that the extrinsic and intrinsic energies should be different. It is unlikely that a worthwhile estimate of the relative densities of extrinsically and intrinsically faulted dislocations can be made at the high deformations present in X-ray samples. ~oretto,'~ from a statistical argument applied to the nonobservation of extrinsically faulted tetrahedra out of a large sample, concluded that yeXt/yint could not be less than -4.5. However, the present author feels that a high-energy formation barrier as just supposed also explains this finding satisfactorily and that no conclusion can possibly be drawn concerning the actual extrinsic stacking fault energy. The same argument also serves to explain the fact that extrinsic faulting has been relatively little observed in the electron microscope. Extrinsic-intrinsic node pairs and isolated extrinsic nodes were first reported by Loretto~ and subsequently by Ives and Ruff,' Gallaher,' and Gallagher and Wash-burn.' Ives and Ruff' found a wide spread in the ratio of extrinsically to intrinsically faulted area in the node pairs they observed, and drew the very tentative conclusion that yeXt/yint 2 2. They recognized that a straightforward comparison of the size of the faulted areas could provide no more than a qualitative result without a theoretical analysis of the dislocation geometry associated with extrinsic faulting. A theoretical

Jan 1, 1969

By Sidney Fischler

Large striation-free single crystals of bismuth have been grown from the melt by rapid freezing. Zone-refined bismuth, together with doping impurities if desired, is placed in a shallow flat-bottomed graphite boat and melted in air with a propane hand torch. The torch is then withdrawn in a manner which causes the melt to freeze direction-ally. Crystallization, which resuires only a few minutes, usually results in the formation of a single crystal even when a seed crystal is not used. Crys -tals of any desired orientation may be grown by using oriented seeds. Undoped crystals grown by this method have residual resistivity ratios greater than 200. THE growth of large single crystals of bismuth by either the Czochralski or horizontal zoning technique is not entirely satisfactory. Specifically, difficulties are encountered in producing single crystals of the required dimensions in all desired orientations, and striations caused by low-angle polysynthetic twins are frequently present in the crystals. In addition, both methods are time-consuming and require special apparatus of some complexity. A simpler method has now been developed for growing large striation-free bismuth single crystals of desired orientation in a short time. Fig. 1 shows a typical setup consisting of a rectangular graphite boat which contains zone-refined bismuth, a 1/8-in.-thick flat quartz plate which covers the entire inner bottom of the boat, and three additional quartz plates about 1/4 in. thick which are used to separate the bismuth from the graphite everywhere except at a small area at the left of the boat. The graphite boat is 1 in. high, and its sides and bottom are about 1/8 in. thick. The quartz plates should be smooth and clean. The graphite boat is heated from the right with a propane torch, as shown in Fig. 1, until the bismuth is completely melted. The melt has the shape of a triangle with a narrow neck at the apex farthest from the torch. The melt is frozen direc-tionally by gradually moving the torch toward the right, away from the boat. The bismuth in contact with the graphite, at the left end of the neck, freezes first. The freezing interface then moves down the neck into the main bulk of material, where it develops a convex shape ideal for the continuation of single-crystal growth. The interface continues to move through the melt until the entire bulk is solid. The entire procedure may be completed, in air, in a matter of minutes. The technique described almost always yields a single crystal whose basal plane is nearly perpendi,cular to the bottom of the graphite boat. In earlier experiments, in which the bottom of the melt was in direct contact with the graphite boat, single crystals were grown with basal planes parallel, perpendicular, or at some intermediate angle to the bottom of the boat. At times the orientation of the bulk of the material differed from the orientation of the material in the narrow neck. In these cases, a nucleation site initiated the growth of a differently oriented crystal, and the thermal conditions favored the new orientation over the initial one. The thermal conditions depend on a number of factors, including the heating technique, the placement, shape, and thickness of the quartz plates, the thickness of the walls and bottom of the graphite boat, and the quantity of bulk bismuth employed. All of these factors, plus the initial orientation and the presence and effectiveness of nucleation sites, will determine the orientation of the final large single-crystal slab. When a crystal of specific orientation is desired, an oriented section of a rapid-freeze crystal is shaped by spark cutting and grinding for use as a seed. To grow a doped crystal, the desired impurity is placed in the graphite boat together with the bismuth chunks and seed. Crystals doped with mercury, cadmium, lead, and selenium have been grown. The rate of freezing is so great that the distribution coefficient of any impurity approximates unity. On a gross scale, therefore, impurities should be more homogeneously distributed in rapid-freeze crystals than in Czochralski or zoned crystals. Because of the possibility of constitutional supercooling, however, it is quite possible that impurities are not homogeneously distributed on a microscopic scale in the rapid-freeze crystals. Generally the single crystal slabs which have been prepared are initially 5 to 7 mm thick. Thicker crystals may be obtained by using one of these slabs as a seed. The slab is placed in a graphite boat resting on a large aluminum block, either air- or

Jan 1, 1964

By R. M. Waterstrat

The phases occurring in the V-Mn system were studied by means of X-yay diffraction and metallo-paphic techniques, using are-melted alloy specimens annealed in the temperature range 800° to 1150°C and quenched. The bcc solid solution extends at 1250°C all the way from vanadium to 6-manganese. Below 1050°C the a-phase is formed, and the terminal a-manganese phase is stabilized up to about 900°C by vanadium in solid solution. IN the only previous general survey of the V-Mn system Cornelius, Bungardt and Schiedtl reported the existence of three intermediate phases corresponding to the approximate compositions VMn,, VMn, and V5Mn. The phase VMn8 has recently been identified as a o phase2 but the alloy VMn was found to have a bcc structure2 corresponding apparently to the vanadium solid solution rather than to the large cubic unit cell reported by Cornelius et al. 1 Subsequent work by Rostoker and Yamamoto3 has shown that the vanadium-base bcc solid solution extends to at least 15 pct Mn at 900°C. An alloy corresponding to the composition VMn, was examined by Elliott,4 who reported that the as-cast sample as well as samples annealed at 1200o and 1300°C had bcc structures, but that annealing at 1000°, 800") and 600°C produced two phases. One of these phases was apparently the bcc solid solution and the other resembled the o phase structure. Hellawell and Hume-Rothery5 established the phase relationships in manganese-rich alloys above 1000°C, and showed that the o phase in this system is replaced by the 6 Mn (bcc) solid solution at temperatures above 1050°C. These results suggest that a continuous bcc solid solution may exist above 1050°C between vanadium and 6 Mn. The present investigation was undertaken in order to develop more complete information in regard to this system. EXPERIMENTAL METHODS The alloys used in the present work were prepared by arc-melting electrolytic manganese having a minimum purity of 99.9 pct and vanadium lumps with a purity of 99.7 pct. The major impurities present in these metals were carbon, nitrogen, and oxygen and this would account for the small percentage of nonmetallic inclusions observed metal-lographically. The arc-melting was at first performed under a helium atmosphere and it was necessary to keep the melting times as short as possible in order to minimize the loss of manganese by vaporization. It was later found that the evaporation of manganese was considerably reduced when the melting was done under argon atmosphere. The final composition of each alloy was calculated by assuming that the total weight loss during melting was due to evaporation of manganese. Compositions which were calculated in this manner agreed reasonably well with the results of chemical analysis, as shown in Table I. Spectrographic analysis revealed the presence of contamination by tungsten, but in no case was the percentage of tungsten greater then 0.4 at. pct. The specimens were in each case broken in half and the fractured section was examined visually and microscopically for evidence of inhomogeneity. Each specimen was homogenized at temperatures near l100°C, as shown in Table I. After this treatment most specimens consisted of large columnar grains of the bcc vanadium solid solution. The etchant used in most of the metallographic work consisted of 20 pct nitric acid, 20 pct hydro-flouric acid, and 60 pct glycerine. It was found that this etchant would clearly delineate the phases present in these alloys although it does not produce any striking contrast between the phases. For certain manganese-rich alloys, a 1 pct aqueous solution of nitric acid was used. This etchant gave a brown color to the a-manganese phase, whereas the o phase was virtually unattacked and appeared very light as shown in Fig. 1. The etchants used by Cornelius et a1.l were found to produce spurious effects in some of these alloys. In particular, the vanadium-rich alloys etched in hot sulfuric acid often appeared to consist of two phases when both X-ray diffraction and etching with the glycerine-acid mixture indicated the presence of single phase bcc solid solution. A few percent of what appears to be an oxide or nitride phase was found at the grain boundaries and in the interior of the grains, especially in the vanadium-rich alloys. All alloys were annealed in sealed silica tubes containing 1 atm of pure argon and these tubes were then quenched in cold water. Although some manganese loss occurred during annealing, the loss seemed to be confined to the surface of the speci-

Jan 1, 1962

By K. J. Gill, P. Chiotti, J. T. Mason

Thermal, metallographic, and vapor pressure data were obtained to establish the pkase boundaries and the standard free energy, enthalpy, and entropy of formation for the compounds in the Y-Zn system. Three coinpounds with stoichiometric formulas of YZn, YZn2, and Y2Zn17 melt congruently at 1105", 1080°, and 890°C, respectively. Four compounds with stoiclziometric formulas of YZn3, YZn4, YZn5, and YZn,, undergo perztectic reactions at 905", 895", 870º, and 685ºC, respectively. Three eutec-tics exisl in this system with the .following eutectic temperatures and zinc contents in wtpct: 875ºC, 23.2 Zn; 1015ºC, 51 Zn; 865ºC, 82 Zn. The YZn, pkase undergoes an allotropic transformation. In the two phase YZn2 -YZn alloys the trans.formation gives a weak thermal arrest at 750°C, whereas in the two phase YZn2-YZn3 alloys no thermal arrest is observed and the transformation occurs over a temperature range below 750°C. At 500°C the free mzergies of formation per lnole vavy from —18,090 for YZn to —53,430 fov YZr11 and corresponding enthalpies vary from -24,050 to -92,080. The free energies and enthalpies per g atom as a function of composition show a maximum for the YZn2 phase; the 500°C values are -9580 and -13,180, vespectively. 1 HE only information found in the literature on Y-Zn alloys was the observation reported by Carlson, Schmidt. and speddingl that Y-20 wt pct Zn forms a low melting alloy. The alloy was produced by the bomb-reduction of YF3 and ZnF2 with calcium in an investigation of methods for producing yttrium metal. The solubility of yttrium in zinc has been determined by P. F. woerner2 and reported by Chiotti, Woerner, and Parry.3 In the temperature range 495" to 685°C the solubility may be represented by the relation In these equations N represents atom fraction of yttrium and T is the temperature in degrees Kelvin. The purpose of the present investigation was to establish the phase diagram for the Y-Zn system and to determine the standard free energy, enthalpy, and entropy of formation for the compounds formed. MATERIALS AND EXPERIMENTAL PROCEDURES The metals used in the preparation of alloys were Bunker Hill slab zinc, 99.99 pct pure, and Ames Laboratory yttrium sponge. Arc-melted yttrium buttons contained the following impurities in parts per million: C-129, N-12, 0-307, Fe-209, Ni-126, Mg-13, Ca < 10, F-105, and Ti < 50. Some of the alloys containing 70 wt pct or more of Zn were prepared from yttrium containing 5000 ppm Ti as a major impurity. Tantalum containers were found to be suitable for all alloys studied and were used throughout the investigation. The pure metals, total weight about 30 g, were sealed in 1 in. diam tantalum crucibles by welding on preformed tantalum covers. A 1/8 in. diam tantalum tube was welded in the base of each crucible for use as a thermocouple well. Welding was done with a heli-arc in a glove box which was initially evacuated and filled with argon. The sealed crucibles were enclosed in stainless steel jackets and heated in an oscillating furnace at temperatures up to 1150°C. Homogeneous liquid alloys were obtained within a half hr at these temperatures except for alloys containing less than 20 pct zinc. The latter alloys were held at 1000º to 1100°C for 2 to 3 days in order to obtain equilibrium. After the initial equilibrations the tantalum crucibles containing the alloys were removed from the steel containers and used directly for differential thermal analyses. Further annealing heat treatments for alloys in which peritectic reactions were involved were carried out in the thermal analyses furnace. After thermal analyses the tantalum crucibles were opened and the alloys sectioned and polished for metallographic examination. In the following discussion alloys referred to as "quenched" were obtained by quenching the sealed stainless steel jacket containing the tantalum crucible and alloy in water. The differential thermal analyses apparatus used was a modified version of the one described in an earlier paper., The graphite crucible was replaced by an inconel crucible, the nickel standard and sampie container were separated by a 1/8 in. MgO plate, no getter was used, and provisions were made to

Jan 1, 1963

By D. J. Mack, R. E. Reiswig

Six examples of the peritectoid transformation were selected from the literature and studied by the method of isothermal transformation. The kinetics and mechanisms of five of the examples are presented as TTT diagrams and photomicrographs. The exist-enc- of a peritectoid in the sixth case is doubtful. ALTHOUGH the peritectoid transformation per se has been known for many years, no precise published data exist concerning the kinetics or mechanisms involved in transformations of this type, except for the brief treatment by Rhines, et al. 1,10 Bearing in mind the fact that investigations of recent years are uncovering more and more peritectoids and suspected peritectoids, a thorough study of the well-established peritectoids appeared to be in order. It was for this reason that a study of the kinetics and morphological mechanisms of six binary peritectoids was undertaken. The six peritectoids selected from the literature for study were those reported at 7.02 wt pct Al-Ag, 26.0 wt pct Sb-Cu, 30.5 wt pct Sb-Cu, 32.3 wt pct Sn-Cu, 8.35 wt pct Si-Cu, and 21.2 wt pct Al-Cu. These selections were based on availability and purity of components, ease of preparation and heat-treatment, and estimated reliability of the available equilibrium diagrams in the regions of interest. EXPERIMENTAL PROCEDURE The alloys used in this investigation were induction melted in electrode-grade graphite and chill-cast in cast-iron split molds. In all cases, the alloys were so brittle that they could easily be broken into samples weighing 1 or 2 g. Chemical analyses showed that the alloys used were close to the respective peritectoid compositions reported in the literature and that the impurity levels were low in all cases. Metallographic examination showed uniform distributions of phases in all samples, indicating uniformity of composition in the samples studied. Isothermal transformation studies were carried out in fused-salt media, using the familiar inter-rupted-quench method. Uniformity of temperature in the salt baths was maintained by continuous stirring with a stainless-steel agitator. On the basis of actual observations of the temperature fluctuations, the estimated temperature control was + 10C for the Ag-Al and Cu-Sb alloys and ±30C for the Cu-Sn, Cu-Si, and Cu-Al alloys. The accuracy of all temperature measurements was estimated to be ±1°C. It was found necessary to mount metallographic specimens of the Ag-Al alloy in cold-curing methyl methacrylate, since the temperatures encountered in mounting in bakelite or lucite caused an appreciable degree of transformation to the ß phase. For the other alloys, wood-flour-filled bakelite mounts were used to avoid extraneous X-ray diffraction lines during the later examination of the metallographic specimens on a Norelco Geiger-counter d if f r ac tomete r. In the X-ray diffraction procedure, agreement between the published diffraction patterns and those obtained in this study was good. This was particularly important for phase identification, since the literature contained little in the way of micrograph description in some cases. Etching of the silver-aluminum alloy for metallographic examination was done by swabbing with either of the following reagents: 1) 10 g CrO3, 1 g (NH4), SO2, 0.5 g NH4NO3, 100 ml H2O, or 2) 10 ml NH4OH, 1 ml 20 pct KOH, 4 ml 3 pct H2O2, 5 ml H2O. The other alloys were etched with the usual bichromate etchant: 2 g K2Cr2O7, 1.5 g NaC1, 8 ml conc. H2SO4, 100 ml H20 (swabbed vigorously). EXPERIMENTAL RESULTS A) The Ag-Al peritectoid at 7.02 wt pct Al— The phase equilibrium involved in this peritectoid is shown in Fig. I.2 The phase boundaries in the vicinity of the peritectoid were most comprehensively established by Hume-Rothery, et al,3 who placed the equilibrium temperature at 448 °C and the equilibrium compositions of the a ß&apos; and y phases at 6.11, 7.02, and 7.24 wt pct Al, respective The alloy used in this study analyzed4 6.95 wt pct A making it slightly hypoperitectoid according to the accepted equilibrium diagram. The rate of the transformation a+ y — ß&apos; varies rapidly with degree of undercooling below the equilibrium temperature, passing through a maximum in the vicinity of 350°C. Thus the TTT dia-

Jan 1, 1960

By C. M. Loeb, A. M. Gaudin, J. H. Brown

THE object of most size reduction operations in the mineral industry is to liberate the grains of valuable minerals in the ore from those of the gangue. This is usually accomplished by crushing and grinding the entire mass of ore until there is only a small probability that any single particle contains more than one mineral. During this size reduction only limited control exists over size or composition of the particles exposed to the breaking action, and there is no control over the paths followed by cracks generated during the operation. This lack of control usually results in overgrinding and in production of large quantities of very fine material. The first detriment, overgrinding, is costly in itself, but when combined with the second factor it is doubly so. Not only is the fracture of a free particle unnecessary—the fracture of these particles may also make subsequent separation operations difficult, inefficient, and wasteful. It has been pointed out&apos; that if the object of size reduction is to liberate the valuable mineral component of the ore then, ideally, fracture should follow intergranular paths to the exclusion of trans-granular ones. This would result in liberation of the valuable minerals with as little size reduction as possible. This ideal comminution operation is referred to as intergranular comminution, and it was the object of the investigation to determine the extent to which it could be developed by heat treatments. There are many indications in the literature that heating rocks prior to crushing may be favorable. Reports by Holman,2 Yates3 and Myers&apos; are pertinent. These investigators showed that heating certain rocks prior to crushing them did, in fact, improve their crushing characteristics in that fewer fines were produced, although the fact that intergranular comminution was being effected apparently was overlooked. In addition, Sosman noted that if there is appreciable anisotropism in the thermal coefficients of expansion of even a pure mineral, then considerable permanent separation of the grains of the rock can be expected as a result of heating the rock to a high temperature.&apos; By the same token, if there are ap- preciable differences in the thermal expansion coefficients of the various minerals of a multi-component rock, similar results should be obtained by heating this rock. This has been tested, partially, by Brenner," who obtained patents covering the heat treatment of some pegmatitic rocks in order to facilitate comminution of these materials. It has also been demonstrated that this may occur in taconite." Also, the possibility of causing decomposition of one mineral in a rock as a means of promoting intergranular fracture has been considered. Seigle2 and Schiffman et al. have obtained patents on such processes as applied to calcareous iron ores. These reports all indicate that heat treatments prior to crushing may contribute materially to intergranular comminution, but they also indicate that no organized attempt has been made to determine the controlling factors of the method or to determine its applicability in general. The present article is a report on the initial phase of such an investigation. The authors have reviewed the claims of prior investigators and have attempted, also, to establish the factors that might determine the applicability of heat treatments in the mineral industry. In this work 2000-g samples of various rocks were heated in a small laboratory furnace and crushing and sizing operations were carried out in standard laboratory equipment. All samples of each rock were as nearly identical as possible in particle size, grain size, and composition and contained only lumps coarse enough to contain many grains each. Tests on Granite A number of tests were made on a coarse grained Finnish granite obtained in the form of coarse chips from a local monument yard. This rock exhibited little variation from piece to piece in either composition or grain size. The minerals contained were quartz, orthoclase, small amounts of hornblende, and minute quantities of mica. Grain size ranged from about 1 mm to about 3 mm. Temperature of the Heat Treatment: In some cases the granite was heated to a particular temperature and crushed, hot, immediately upon withdrawal from the furnace—in others the rock was allowed to cool before crushing, but without quenching to room temperature after heating. In most tests on granite the heating period was about 2 hr with the furnace at the highest temperature for about 1 hr. Cases in which these periods were varied greatly will be presented separately.

Jan 1, 1959