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By AIME AIME

THE first fall meeting of the new Coal Division started on time on Thursday morning, Sept. 11, at Pittsburgh, with Paul Sterling of the Anthracite Section presiding and over a hundred members and guests in the room. The attendance increased from session to session, the total registration being 248. Excellent arrangements had been made by the officers of the Division covering all features of the meeting, the only drawback being that more papers-were listed for presentation than could be discussed in the time available. Howard-N. Evensong, chairman of the Division, explained this situation as sore and sore papers case in by likening it to the case of the small boy who wanted a second niece of pie at the end of a large seal. When his mother remonstrated that if he ate any more he would certainly burst, the young man replied, "Well, you just hand over the pie and then get out of the way." With that Mr. Evensong turned the meeting over to Mr. Sterling, who handled it so well that with ample discussion it was still possible to adjourn at lunch time, all but the group of junior papers having been heard. This series of papers, the output of the .very lively Junior Section organized last spring by the younger men of the Division was regretfully put over until Friday morning, when that on "Heat Drying" by S.. M. Parsley was read.

Jan 1, 1930

By T. Egleston

THE works of the Ore Knob Copper Company are situated in the county of Ashe in the northwestern part of the State of North Carolina, about ten miles from the Virginia line, at an elevation of 4600 feet above the sea. The nearest railroad station is at Marion, Smythe County, Virginia, about forty-five miles distant. The roads from the railroad to the works have been constructed by the company for the transportation of their material, and are very hilly, and in certain seasons of the year in bad repair. Transportation is therefore always limited and never easy, although it is done by contract at a very low price. The main difficulty with the transportation is not so much its cost as the fact that it puts a limit to the production of the works. These unfavorable conditions make it necessary for the owners of the mine to smelt their ores and to send to market nothing except the metal, which alone will bear the cost of transportation. The mine was opened previous to 1860, but has only been worked systematically during the last five or six years. The vein is a fissure vein from ten to twenty feet in thickness in the gneiss of the

Jan 1, 1882

By T. Egleston

The works of the Ore Knob Copper Company are situated in the county of Ashe in the northwestern part of the State of North Carolina, about ten miles from the Virginia line, at an elevation of 4600 feet above the sea. The nearest railroad station is at Marion, Smythe County, Virginia, about forty-five miles distant. The roads from the railroad to the works have been constructed by the company for the transportation of their material, and are very hilly, and in certain seasons of the year in bad repair. Transportation is therefore always limited and never easy, although it is done by contract at a very low price. The main difficulty with the transportation is not so much its cost as the fact that it puts a limit to the production of the works. These unfavorable conditions make it necessary for the owners of the mine to smelt their ores and to send to market nothing except the metal, which alone will bear the cost of transportation. The mine was opened previous to 1860, but has only been worked systematically during the last five or six years. The vein is a fissure vein from ten to twenty feet in thickness in the gneiss of the

Jan 1, 1882

The General Committee met in the Treasury Building at Washington on Oct. 6 and 7. At the first meeting, Cornelius P. Kelley was appointed chairman, and Paul Armitage, secretary. Sub-committees were ap-pointed on Invested Capital, Mine Valuation, and Depletion and De-preciation. On Oct. 7, the reports of these committees were submitted to the General Committee and were referred to the Executive Committee. A motion was carried that the Executive Committee he constituted a permanent committee to continue the work of the Committee, with full power to acid to and increase its membership, that. as thus increased, it should constitute a permanent organization to act- and cooperate with the Treasury Department in matters of mining taxation under the Federal Income and Excess Profits Tax Laws. Thereafter the Executive Com-mittee met and formed a permanent committee as follows: Cornelius F. Kelley, chairman, 42 Broadway, New York City. J. L. Darnell, office of the Commissioner of Internal Revenue, Wash-ington, D. C. J. Parke Channing, 61 Broadway, New York City. Walter Douglas, 99 John St., New York City. R. V. Norris, 542 Second National Bank Bldg., Wilkes-Barre, Pa. J. E. Spurr, Engineering and Mining Journal, 10th Ave., and 36th St., New York City. W. G. Swart, 808 Selwood Bldg., Duluth, Minn. J. P. Finley, 45 Cedar St., New York City. W. A. Williams, Bartlesville, Okla. F. S. Peabody, Peabody Coal Co., McCormick Bldg., Chicago, Ill. Matthew C. Fleming, 71 Broadway, New York City. H. B. Fernald, 54 Wall St., New York City. William G. Mather, Cleveland, Ohio. Walter Fitch, Eureka, Utah. Arthur Thacher, 900 Security Bldg., St. Louis, Mo. John P. Gray, Coeur d'Alene, Idaho. Paul Armitage, secretary, 233 Broadway, New York City.

Jan 12, 1919

By John McDonald

THIS report is a continuation of an earlier one with a similar title,1 to which the reader is referred for such details of procedure as do not appear here. A brief summary will be given of the objects and methods of the research at this time. It was pointed out in the previous paper that properties of magnesium alloys, as re-ported by different workers, often differ. This was thought to be due to differences in the preparation of the specimens tested. The ideal way to compare alloys would be to prepare each of them in so many ways that reasonable assurance would exist that the best properties of each alloy had been developed. The alloys would then be com-pared on the basis of these properties. The treatment actually given the alloys of these studies is necessarily a compromise with completeness. Nevertheless, enough treatments have been given so that a con-siderable degree of assurance exists that the properties obtained are representative of the alloy as such, and not merely of the manner in which it was worked and heat-treated.

Jan 1, 1940

By Mitchell, Edmund I.

VARIOUS suggestions as to proper fees for engineering services have been put forth by individual practitioners and by the American Institute of Consulting Engineers, the Connecticut Society of Civil Engineers, the Iowa Engineering Society and the Mahoning Valley (Ohio) Engineers, for the guidance of both the engineer and his client. The American Institute of Architects also has a schedule of minimum charges (revised 1908). So far as can be determined, however, the four national societies representing civil, mining, mechanical and electrical engineering have never given consideration to this question. An examination of technical periodicals published during the past decade shows that these schedules make provision for three methods of charging; i.e., (A) a percentage of the cost of the completed project; (B) a per diem rate; and (C) a fixed sum. Suggested minimum charges are as follows:

Jan 1, 1921

By John Hays Hammond

The Transvaal comprises about 120,000 square miles (nearly • the size of the United States Territory of New Mexico). Besides the famous Witwatersrand, which will here be de scribed in detail, there are two quartz-mining districts of some importance, viz., Lydenburg and De Kaap. The Lydenburg district first attracted attention in 1876, when the alluvial deposits of that section began to be exploited. At a later period vein-rnining was started, and at the present time several companies are operating in that district. The product in 1898 of five companies, running 137 stamps, was 154,560 tons of ore, yielding 108,884 crude ounces of gold (an average of 14.09 dwt. crude gold per ton) valued at £392,378. The De Eaap gold-fields were discovered in 1884. In 1898, seven companies, running 200 stamps, produced 89,760 crude ounces of gold, valued at £314,792. I. Mining Titles in the Transvaal. The mining laws of the Tranuvaal are most excellent in char acter, and while the claims cover every square foot of land for an area of nearly 40 miles long by from 2 to 3- miles wide, there have been practically no conflicts over extra-lateral rights. Notwithstanding the change in the political status of the Transvaal likely to follow the present war, it may be coufi dently assumed that the main features of the mining law of the South African Republic will be retained, and certain op pressive featureu of monopolies, etc., bearing with special weight on the mining industry, will be abolished. The dynamite mo nopoly was one that bore most heavily on the mining industry; and, according to the Reports of the State Mining Engineer, explosives, including fuse and detonators, amounted to nearly 10 per cent. of the total working costs of the mines. Further more, it was impossible to obtain the proper quality for the most economical working, and often 80-per-cent. or 40-per-cent. gelatine had to be used- in many instances where 60-per-cent.

Jan 1, 1902

By G. F. LOUCHLIN

A FEATURE of the International Geological Congress to be held at Pretoria, South Africa, in the summer of 1929,. will be a symposium on the gold resources of the world. In this connection the U. S. Geological Survey and Bureau of Mines have been asked to prepare a report, showing production in the United States, describing the geology of its principal gold- producing districts, and estimating reserves (a) assuming a continuation of presen6economic conditions, and (b) assuming lower costs. This report will not be completed before April 1, but data thus far assembled are here presented with the hope of profiting by discussion and by information from those well informed on any of the important gold-producing districts. Gold production in the United States rose to a maximum exceeding $100,000,000 in 1915 and then rapidly declined to about $52,000,000 in 1920. Since then it has fluctuated, but on the whole slightly declined. Reviews of the eight leading states afford the following tentative conclusions :

Jan 1, 1929

By E. Gaujot

IN connection with the question of coal waste and economy in mining, we would call the attention of those interested to an apparatus invented by M. Dernencourt, Superintendent of the Anzin Division of the Anzin Coal Company, North of France. This apparatus is known in France and Belgium under the name of prop screw jack (vis botte), and has been used with good results in the above-named countries for some years past. M. Ponson gives, in his " Traité de l'exploitation des Mines," a description of it (page 533), but as the description given is old, the work not widely known in this country, and as some valuable improvements have been made since, I thought it might be useful to give a description of it, having seen it in operation in 1867, while in Europe to attend the great Exposition, and on a scientific tour to the mining districts of France, Germany, Belgium, and Italy. The prop screw jack is composed of the following pieces: I. The body or column B, Fig. 4 [Plate (1)], of oak or yellow pine, sawed square, the bark taken off, and any length, proportionate to the vein. The smallest are 10 inches diameter at the base, and 9 inches at the top, the height being from 12 to 15 inches less than the size of the vein. In the axis of this column, and at the top end, is a cylindrical opening or hole, C, 2 3/4 inches diameter, 10 inches deep, for the screw, S. II. Two wrought-iron rings, R R, to strengthen the two extremities of the column ; the rings must be put on hot. III. A cast-iron washer, E, with hole in centre a little larger than the screw, to be put on the top of the column, and on which the nut is to rest; the top side of this washer must be faced on the lathe, also the bottom of the nut, to prevent friction. IV. The screw, S, having a total length of 12 inches and a diameter of 21/2 inches (for very high veins this diameter may be in¬creased to 3 inches), and has on its top a wrought-iron plate, T,

Jan 1, 1873

By J. B. Umpleby

PRoduction engineering in 1927 may be characterized by a great. clarification of fundamental conceptions, and many improvements in technique. During the year the profession has received tnarked recogni-tion by the industry and to an extent never before attained has become an integral part of it. History Petroleum production engineering is a new profession. Prior to 1925, when this Institute undertook the work, no forum existed for the open discussion of its technical problems. There was no attempt at a handbook of the subject prior to "Petroleum Production Methods by J. R. Suman, in 1921, and no textbook prior to Petroleum Production Engineering" by L. C. Uren, in 1924. As late as 1926, only six schools and universities offered special courses in petroleum production engineering. Prior to about 1923, engineers engaged by oil companies were used almost exclusively for construction and location work. Two of the leading production engineers in the Mid-Continent field, although with their respective companies more than twelve years, were not definitely assigned to production work until 1924. Both men now head large departments giving almost their entire time to production problems. Because of the newness of the profession, the leading production engineers of today have had their fundamental training in mining, civil, mechanical and electrical courses. Not unlikely this diversified training is in considerable part responsible for the amazing growth of the profession. I believe, however, that recognition is due principally to economic pressure within the industry which has directed attention more and more sharply on costs and efficiency. After all, the justification for the growth and continued development, of the profession is to recover more oil from a given unit of sand at less cost per barrel. In this new profession, it seems to me that greatest progress will result from focusing thought and effort on this single objective, and if I might offer one suggestion to the com-

Jan 1, 1928

By Robert T. Ault

The nature of fracture in unnotched tensile and notched tensile sheet and round specimens and V -notched and precracked Charpy-type sheet specimens of both wrought stress -relieved and re-crystallized molybdenum was investigated over the temperature range of -78° to 300°C. The sharp rise in fracture stress, for unnotched tensile samples, as the temperature is increased above the brittleness transition temperature (Tb), is found to be a result of an increase in flow stress due to plastic constraint and an increased strain rate which results from the onset of necking at Tb . Quasi-brittle fracture in notched tensile samples is found to occur when the tensile stress at the elastic-plastic interface, beneath the root of the notch, reaches a maximum critical value, which is independent of test temperature over the range from —78° to 25°C, but dependent on microstructure. In the temperature range between 150° and 300°C, unnotched tensile and notched tensile samples alike are found to fracture by a ductile fibrous tearing process which is discontinuous in nature, as a result of the competition between the processes of tearing, through continued plastic flow, and local work hardening. Results from the V-notched and fatigue-cracked Charpy-type impact tests demonstrate that crack initiation is the governing factor in the low-temperature (-78° to 25°C) fracture process for molybdenum. In recent years, there has been considerable interest, and a commensurate number of investigations, concerning the duc tile-to-brittle transition in refractory metals. There has not developed, however, a satisfactory explanation for the uniaxial tensile fracture-stress transition which accompanies the well-known ductility transition. This matter therefore warranted investigation. In a similar manner, the increased importance of notched tensile strength values in evaluating materials and in design criteria requires a better understanding of the factors which control the fracture behavior of notched tensile samples. In a previous investigation1 of the nature of initial yielding and fracture in notched sheet molybdenum at room temperature, it was suggested that plastic constraint was the controlling factor in governing the fracture behavior of notched samples. The final portion of this investigation was concerned with the fracture toughness of molybdenum. Of particular interest was the comparison of effective surface energies for fracture in V-notched samples with fatigue-cracked, Charpy-type samples in order to ascertain the relative importance of the initiation and propagation phases of the fracture process. MATERIALS AND TEST PROCEDURE Sheet tensile, notched tensile, and V-notched Charpy specimens were prepared from 50-mil, stress-relieved molybdenum sheet.* Half of these specimens were vacuum-annealed for 1 hr at 1200°C and 7.5 x l0-5 Torr and furnace-cooled to produce a relatively uniform grain size of 0.30 mm diameter. Round notched and unnotched tensile specimens were prepared from warm-rolled and swaged 5/8-in.-diam bar.* These specimens were vacuum-annealed for 1 hr at 1350°C and 5 x lom5 Torr and furnace-cooled to produce a grain diameter of 0.11 mm. Material analyses in ppm were: C N O H Sheet 290 10 4 1 Bar 50 30 30 2 The unnotched tensile sheet specimens had a 1/4-in. gage width and a 1-in. gage length. The unnotched tensile round specimens had a 9/32-in. gage diameter and a 1-1/4-in. gage length. The sheet and round notch tensile specimens are shown in Fig. 1. All of the notched tensile specimens tested were tandem-notched in order to study the location and mode of fracture initiation. The tandem-notched specimens were carefully machined so that the largest variation in notch depth on a single specimen was 0.001 in. Thus, when fracture occurs, the extent of plastic deformation that exists in the un-fractured notch section is that which exists just prior to fracture. All of the tandem-notched sheet specimens were electrolytic ally polished and chemically etched prior to testing. The V-notched Charpy-type specimens machined from the 50-mil sheet material had the standard dimensions of 2.125 in. long, 0.394 in. deep, and a 0.010-in. root radius. The unnotched tensile and notched tensile tests were conducted over the temperature range of -78° to 300°C, in a 10,000-lb Instron Universal Testing Machine, at a constant crosshead speed of 0.020 in. per min. The V-notched Charpy-type

Jan 1, 1964

By F. F. McINTOSH

STEEL is a general name applied to the alloys of iron and carbon. These alloys always contain , other elements such as manganese, silicon, sulfur, and phosphorus. Manganese and silicon are usually considered to be alloying elements. Sulfur and phosphorus are regarded as impurities. Tradition has damned them both and, in addition to classifying them as impurities, has established the general impression that many of the ills of steels are the result of the presence of one or both of these elements. Metallurgists are inclined to question the soundness of this tradition. The fact that one blast-furnace plant is devoted entirely to the production of ferro-phosphorus which is used to rephosphorize basic open-hearth steel, and that sulfur is added to many heats of steel, indicates that these so- called impurities might also be classed as alloying elements, and that the tradition which damns them may not be altogether fair and well founded. A critical search through the technical literature on the effect of phosphorus on steel will disclose many references to its harmful effect. Most of these are general in character, but there has been a strong tendency to accept this traditional belief in the harmful effect of the element.

Jan 1, 1926

By Sir Albert E. Kitson

The manganese ore deposits of the Gold Coast, British West Africa, occur in very ancient rocks, of both sedimentary and metamorphic types. In certain respects they have a strong resemblance to those of India and Brazil, as contrasted with those of Tertiary age in Georgia, but in this paper no careful comparison with them can be made. Viewed from the present condition of the manganiferous rocks, the oldest deposits are in the sediments. Later than these are the progressively metamorphosed representatives of these sediments. Youngest are the products of decay and degradation with the concentration of manganese oxide in the rocks of both groups. The oldest occurrences are in argillaceous and siliceous phyllites and slates, which show only a moderate degree of metamorphism. They belong to a series which also includes mudstones, sandstones, grits, conglomerates and subordinate limestones, with tuffs and lava-flows, largely of basic types. This has been named the Birrim System. Its age is unknown, for no definite fossils have been discovered in it. Since these non-fossiliferous strata at many plaees are of a character which in many parts of the world are suitable for the preservation of fossils, and which contain them, it is assumed that the Gold Coast deposits are pre-Cambrian. These rocks of the Birrim System have normally a northeast-southwest strike, and are folded, but not to any very great degree except in certain belts. From the Eastern Province of the Gold Coast they may be traversed diagonally across their strike for upwards of 600 miles, to the extreme northwestern corner of the Northern Territories. Thence they probably extend much farther into French territory.

Jan 1, 1927

By Sadtler, C. B.

IT is generally assumed that in most metals and alloys a given tensile stress produces a given deformation irrespective of the length of time during which the stress is applied. This assumption is justified in most of the important engineering applications of metallic materials; however, in the case of some metals and alloys used or tested at temperatures over or slightly under that at which recrystallization can occur the assumption is not warranted.1 This paper deals with the variations of deformation produced by a constant tensile stress acting for varied lengths of time in the special case of thin aluminum alloy sheet of the duralumin type, which had been subjected to different thermal and mechanical treatments. The material investigated was in the form of a sheet approximately 0.002 in. thick, which had been cold-rolled from a thickness of 0.020 in. It has been found that at a sufficiently high constant tension such material deforms continuously with the elapse of time and that the rate at which this deformation occurs is greatly influenced by the previous thermal and mechanical treatments.

Jan 1, 1927

By Leslie F. Tedsen, John E. Dorn, Alan E. Flanigan

It is necessary occasionally to use aluminum-alloy sheet where moderately elevated temperatures are encountered. Considerable attention has been directed toward determining the influence of "artificial aging" on the room-temperature properties of the precipitation-hardenable alloys, as testified by numerous company reports and by references I to 4. Investigations on the properties at elevated temperatures are few, however, and have not always covered the range of times and temperatures of greatest interest. The present investigation was instituted to overcome this deficiency. The work was done for the Office of Production Research and Development of the War Production Board, under the supervision of the War Metallurgy Committee, as a part of the "restricted" Project NRC-548. It has been released for publication by the Office of Production Research and Development. AS is well known, the high-strength aluminum alloys achieve their remarkable properties as a result of precipitation-hardening. In production they are subjected to a solution heat-treatment followed by quenching, to retain the supersaturated solid solution. The solution treatment is followed by "aging" (precipitation-hard- ening) either at room temperature or at a suitable elevated temperature. A considerable increase in tensile and compressive yield stresses results from precipitation at room temperature ("natural aging"). Through the elevated-temperature process ("artificial aging") it is possible to obtain values of yield stress considerably higher than those attainable by natural aging. The increase in yield stress is accompanied by a smaller gain in ultimate tensile stress and by a decrease in elongation. During the first stages of artificial aging the yield stress increases steadily until it reaches a maximum value. In this condition the material is said to be "fully aged." Further exposure results in "averaging," attended by a steady decrease in yield stress. In the production of the artificially aged materials, temperatures and times are selected to achieve full aging. The following important characteristics are associated with the process: 1. The higher the temperature, the more rapidly is the fully aged condition attained. :7

Jan 1, 1946

By Leslie F. Tedsen, Alan E. Flanigan, John E. Dorn

It is necessary occasionally to use aluminum-alloy sheet where moderately elevated temperatures are encountered. Considerable attention has been directed toward determining the influence of "artificial aging" on the room-temperature properties of the precipitation-hardenable alloys, as testified by numerous company reports and by references I to 4. Investigations on the properties at elevated temperatures are few, however, and have not always covered the range of times and temperatures of greatest interest. The present investigation was instituted to overcome this deficiency. The work was done for the Office of Production Research and Development of the War Production Board, under the supervision of the War Metallurgy Committee, as a part of the "restricted" Project NRC-548. It has been released for publication by the Office of Production Research and Development. AS is well known, the high-strength aluminum alloys achieve their remarkable properties as a result of precipitation-hardening. In production they are subjected to a solution heat-treatment followed by quenching, to retain the supersaturated solid solution. The solution treatment is followed by "aging" (precipitation-hard- ening) either at room temperature or at a suitable elevated temperature. A considerable increase in tensile and compressive yield stresses results from precipitation at room temperature ("natural aging"). Through the elevated-temperature process ("artificial aging") it is possible to obtain values of yield stress considerably higher than those attainable by natural aging. The increase in yield stress is accompanied by a smaller gain in ultimate tensile stress and by a decrease in elongation. During the first stages of artificial aging the yield stress increases steadily until it reaches a maximum value. In this condition the material is said to be "fully aged." Further exposure results in "averaging," attended by a steady decrease in yield stress. In the production of the artificially aged materials, temperatures and times are selected to achieve full aging. The following important characteristics are associated with the process: 1. The higher the temperature, the more rapidly is the fully aged condition attained. :7

Jan 1, 1946

By KING HAMILTON GRAYSON

IRON and steel were the only basic industries in the Soviet Republic in 1928 that lagged behind the pre-war production on a comparative basis. This was due to the almost complete obliteration of all industrial units manufacturing iron and steel products during the Revolution, which resulted in the production of 1921 being only 4 per cent of that of 1913. By the end of 1927 the production of pig iron had reached a point equal to 70.5, per cent of 1913; steel was 84 per cent ; and rolled iron was 78 per cent. According to the. planned program of the Supreme Economic Council, the pre-war level of the iron and steel industry was to have been reached and exceeded during 1929-30. The production of the entire period from 1917 to 1928 in comparison with 1913, is shown in the following table

Jan 1, 1929

By E. A. Nesbitt

THE important permanent-magnet alloys 15 years ago contained carbon and depended upon it for their permanent- magnet properties. In recent years great, advances have been made in a number of new alloys substantially free of carbon. These include Remalloy,l an alloy of iron, cobalt, and molybdenum, the various iron- nickel-aluminum alloys of the Mishima2 type, and the more recent Alnico V3 in which the best properties are developed by heat-treating in a magnetic field. The Mishima and the Alnico types of alloys are very brittle and after casting must be ground to size. This article describes a permanent-magnet material4 that can be machined as cast, and when handled with some care can be .rolled to thin sheet and drawn to fine wire. Optimum magnetic properties are developed by a simple heat- treatment, and at this time the ductility A of the alloy disappears. If the cast alloy is heat-treated without cold-working the magnetic energy product is about 1.0 X 106. This material is called Vicalloy I (pronounced vicalloy, V for vanadium, I for iron, and C for cobalt). When the alloy is first hot-worked and then considerably reduced in area by cold-swaging, drawing or grooved rolling, it is found that after heat-treatment the magnetic energy product measured in the direction of previous extension can be increased to 2.0 to 3.5 X l06. These higher values have been obtained only after reductions in area of 75 to 95 per cent, and since the material hardens considerably during working, the reduction ordinarily can be accomplished only in fine wires, although larger sizes can be reduced by the use of powerful machinery. When the material has been cold- worked in such a manner as to improve its energy product substantially, it is called Vicalloy II. Commercial use of Vicalloy has been made in the recording of speech. Tape 0.002 by 0.050 in. has been found superior in quality to all others tried, and is now used in the Western Electric Mirrorphone In a variety of forms Vicalloy I or II is useful in many laboratory instruments, and in experiments in which the sizes and shapes required cannot be obtained with the other more brittle permanent-magnet materials. In 1936, during a study of other age- hardening magnetic systems, it occurred to the author that some of the iron-cobalt-vanadium alloys might be suitable for permanent magnets. The proportions of iron, cobalt, and vanadium were varied and a range of alloys of particular interest was found, as shown by the indicated area in Fig. I. The limits of this range of com- position are 30 to 52 per cent iron, 36 to 62 per cent cobalt, and 4 to 16 per cent vanadium. The compositions indicated by points outside this area were also tested. PREPARATION AND PROPERTIES OF VICALLY I The alloys were usually cast in graphite molds into bars ¾ in. in diameter and

Jan 1, 1946

By T. E. Evans, C. T. Baroch

ZrB2 was produced in batches of 4 to 6 Ib by interaction of ZrO2, B4C, B203, and carbon at around 2000°C in a simple graphite resistance furnace. Techniques of production are discussed and the final design of a suitable furnace is described in detail. Several other borides were made by the same technique and the process appears to have possibilities for commercial production. N seeking out new hard and refractory com- pounds, many researchers have turned to the investigation of the borides and excellent papers have been published on the properties of these compounds. Few papers, however, have appeared on the techniques and problems concerned with the production of these high temperature substances. This report describes progress made in developing a method for preparing zirconium diboride, ZrB2, on a pilot plant scale. The literature of the borides and other refractory hard metals recently has been reviewed, annotated, and classified so completely' that it is needless to attempt such an outline here. It is enough to say that three borides of zirconium have been reported: ZrB, ZrB2, and ZrB12.2 ZrB2 is the most stable of these and is especially stable in the presence of carbon up to and including its melting point of around 3000°C. Like most borides, it can be prepared in several ways. It can be prepared by synthesis of the elements, but these are expensive and difficult to produce in a high state of purity. Obviously, production directly from the oxides would have decided economic advantages. In electrolytic production such as that of calcium boride,:' the product is recovered as a sludge mixed with electrolyte; and separation of product from adhering electrolyte and regeneration of the electrolyte is an involved and difficult process. The work on borides was started on a small scale in 1948. Late in 1949, Naval Ordnance expressed a specific interest in ZrB2 and the project then centered on this compound. After the usual experimental work necessary in a new field, ZrB2 of good quality was produced by heating mixtures of B4C, ZrO2, B2O3, and carbon to a temperature of about 2000 °C in a resistance-type electric furnace. Over 100 lb was made for experimental use tests, and the method of production probably could be expanded into a commercial operation. A similar process has been described by Kieffer and coworkers.' The main chemical problems were the development of proper charges to insure complete reduction of the elements, determination of the proper temperature range at which these reductions took place, and adoption of techniques necessary to pre- vent inclusion of such impurities as carbon and nitrides. The mechanical problems consisted of developing a simple practical furnace that would attain the high temperatures required and permit use of a controlled atmosphere when necessary and determining of suitable refractories. Both problems were solved by designing a crucible resistance furnace. Crucible Resistance Electric Furnace Attempts were first made to produce ZrB2 in an electric arc furnace, but such a furnace would not provide the degree of carbon control required for producing clean graphite-free borides, so it was decided to try working in a crucible. Obviously, the furnace would have to be constructed of graphite, as the temperatures required are too high for other refractories or heating elements. Crucibles were made by hollowing out segments of graphite electrodes, which were fitted with a cover and clamped between two electrodes so that the current passing through the thin wall of the crucible would generate heat, using the principle of the Helberger crucible furnace."? Preliminary tests with this type of furnace were encouraging and led to the furnace design shown in Fig. 1. The essential components were a thin-walled graphite crucible resting on a graphite block, which formed the lower electrode assembly, and a top electrode assembly swung from a pipe column making contact with the top of the crucible. The space around the crucible was filled with graphite prepared from waste electrodes crushed to about ¼ in. This packing had excellent insulating properties, both electrically and thermally, and could be removed easily and quickly from around the crucible by means of an industrial vacuum cleaner. The largest resistor crucibles were machined from 8 in. electrode stock and were 26 in. long, with a side wall Yi in. thick and a 1 in. bottom. Temperatures were determined optically by sighting down a 1 in. hole drilled longitudinally through the top electrode and the crucible cover. Sealing this hole at the top was a water-cooled brass sight-glass assembly, shown in Fig. 2. An opening was provided for a light flow of helium to keep the sight opening clear of smoke, and a glass prism above the sight glass changed the line of sight to the horizontal for easier reading. More recently, the prism and optical pyrometer were replaced by a photoelectric recording pyrometer. At first the charges were placed directly in the resistor crucible but this meant that everything had to be withdrawn from the furnace every time the charge was emptied. Later, smaller crucibles were made up that could be placed inside the resistor

Jan 1, 1956

By W. C. Knopf, I. M. LeBaron

In the Carlsbad area potash is dry-mined and wet-concentrated. Wet concentration involves recircu-lation of saturated brines, with resultant difficulties of brine disposal and inherent losses in recovery through solution of the KCl. A dry beneficiation process for potash minerals would offer many advantages over present methods. International Minerals & Chemical Corp. has been working on development of a dry process for some time. This article is a progress report. Potash ores available in this country are largely mixtures of halite and sylvite contaminated with slimes and often with many sulfate and magnesium minerals. Electrostatic concentration of KCl when the contaminating minerals are in low percentage has been accomplished. Continuous production of better than 60 pct K2O concentrate from high potassium sulfate ores has not been demonstrated at the present time. Laboratory Procedure: Laboratory work on electrostatic beneficiation of potash minerals has been carried out using both pure crystals and mined ore. Electrostatic separation of the two main components of potash ore, sylvite (KCl) and halite (NaCl), is accomplished by first heat-treating the ore to allow for electric charging of the particles. Preferential exchange of' electrical charges between different mineral particles through surface contact is the principal mechanism involved. After proper conditioning of the particle surfaces, the oppositely charged minerals are dropped vertically into a horizontal electric field having a field gradient from about 5000 to 15,000 v per in. The particles are free-falling in the field. A suitable power supply is used to produce the proper total voltage for the electric field. Total required voltage is, of course, a function of electrode spacing. A typical electrode arrangement with power supply is shown in Fig. 1. In general, the total voltage on any system is 75,000 to 90,000 v. Power consumption is negligible, as leakage at insulators and corona discharge are the main losses in the system. Optimum preheat temperatures for pure material components generally are not the same as for mined minerals. Fig. 2 shows clearly that maximum recovery on a 50 pct pure KCl, 50 pct pure NaCl mixture occurs at a preheat temperature of about 600°F. In this test the preheat mixture was allowed to cool to about 225°F before dropping through the electric field. The optimum temperature for sep- aration is practically never the optimum temperature of preheat. Optimum separation for mined Carlsbad potash ores occurs when a preheat temperature closer to 900°F is used, as shown by Fig. 3, which plots percent sylvite (KCl) in the concentrate and tails as a function of preheat temperatures. Here again the ore was allowed to cool to about 225°F before separation. It should be noted that efficiency of separation increases continuously with increasing preheat temperatures until incipient fusion of the ore takes place at about 950°F. The increase in optimum preheat temperature for Carlsbad ores over the pure minerals can be traced to the effect of the clay slimes intimately associated with the mined potash. If the slimes associated with the ore are removed by washing with alcohol or other non-aqueous material, the necessity of preheating to the high temperature is removed. This temperature range has been proved critical within these limits during continuous pilot plant operation. Concentrate and tailings grade and optimum recovery also are functions of the temperature of the potash mineral particles during separation in the electric field. Fig. 4 presents data indicating that feed to the rougher pass should range between 150°F and 275°F for best results. It has been found by subsequent pilot plant work that these temperatures can be maintained in actual operation.

Jan 1, 1959