Search Documents

By E. C. Bain

THE more familiar compositions of iron-carbon-chromium1 and the iron-carbon-tungsten2 systems have been investigated with a degree of thoroughness which has permitted the construction of their three-dimensional equilibrium diagrams; and it is probable that these equilibrium diagrams are sufficiently accurate for the present metallographic needs. Strangely enough, in spite of their importance, the alloys of iron, carbon and manganese apparently have not been investigated in the same systematic manner, and so far as is known, no three-component equilibrium diagram for this system is available. Even iron-carbon-nickel alloys3 have been studied rather more thoroughly; for these the solidus and liquidus surfaces have already been determined, but the solid transformations in this, as in the manganese system, have not been reported systematically. The present paper deals with the constitution at equilibrium of a series of 36 iron-carbon-manganese alloys of commercial purity limited by 1.5 per cent carbon and 15 per cent manganese, a range of compositions including most of the manganese steels. The temperature range of melting has not been determined, nor has the high-temperature (delta iron) ferrite equilibrium been included in the study, it being considered that the more important characteristics of the manganese steels are their ordinary transformations in the solid state. The delta iron region is almost certain to be a small tetrahedron not very different in magnitude or contour from that in the iron-carbon-nickel diagram. It is probably true

Jan 1, 1932

By Arthur Notman

THE COMMITTEE on Production Control of the Institute has accomplished little or nothing tangible during the last year. For this the chairman must accept responsibility and whatever praise or blame goes with it. However, we have all had plenty of opportunity to observe the results obtained by various producing groups in their attempts to regulate production to meet demand dur¬ing the last few years. It would be putting it mildly to say that these have not been such as to inspire confidence in the methods pursued. The present plight of the wheat, cotton, coffee and sugar growers; the oil, copper, lead, zinc and tin producers, to name a few of the unfortunates, suggests a common cause perhaps beyond their control. There is a growing tendency to question as outmoded the theories of laissez faire economics, with its laws of competition, supply and demand, with price as the automatic regulator. The position is maintained that something new should be substituted because these laws no longer work. Many solutions are offered, ranging in the world at large from the planned economy of Russia, with the profit element removed, to the military controlled economy of Fascism, and in our own country from voluntary curtailment to martial law. But one hardly feels driven by any irresistible logic to put his finger on any one of these proposals, and to say this is the one in which I believe. On turning to one's neighbors, one is still more confused by the realization that this intellectual uncertainty is wide-spread. Isolation or cooperation, protection or free trade, the gold standard, bimetallism or managed currencies, de¬flation or inflation, all have their proponents in whose eyes one or the other of these slogans will afford the panacea for all our ills.

Jan 1, 1933

NEW MEMBERS The following list comprises the names of those persons who became members during the period Nov. 10 to Dec. 10, 1915: BARTH, ERNEST, Petroleum Geol Box 552, Tulsa, Okla. BEROLZHEIMER, D. D.,.Chemist; Librarian, Barrett Mfg. Co., 17 Battery Pl., New York, N. Y. BLIEK, PIERRE FRANCISCO, Mgr., Compania Minera de Oruro, Oruro, Bolivia, So. Amer. BLOCS, JAMES A., Met 1076 1st Ave., Salt Lake City, Utah. BULKLEY, RALPH G., Mine & Mill Supt.; The Montezuma Mines & Mills Co., Montezuma, Colo. BURRAGE, ALBERT CAMERON, JR., Met. Engr.; Director, 85 Ames Bldg., Boston, Mass. CABELL, CHARLES ARNOLD, Vice-Pres Carbon Coal Co., Carbon, W. Va. CHAPMAN, LEWIS CARL, Economic Geol Producer Oil Co., Houston, Tex. CHOFFEL, FLAVIEN AURELIEN, Mgr Ingersoll-Rand Co., Paris, France COY, HARLEY A., Mine Supt American Zinc Co., Mascot, Tenn. DITTMANN, C. 0. ADOLF, Cons. Engr., Beer, Sondheimer & Co., Inc., Santiago, Chile, So. Amer.

Jan 1, 1916

By A. H. Bell

DEEPEST hole in the earth, and deepest producing oil well in the world-such is well No. K.C.L. A-2, of the Continental. Oil Co., completed on April 12 in the San Joaquin valley about four miles west of Wasco, Calif. It penetrated the earth's crust to a depth of 15,004 ft.- almost three miles-a depth that exceeds by over 2200 ft. that of the previous record holder in western Texas. It is now producing oil from sands at a depth from 13,092 to 13,- 175 ft., which is about 1500 ft. deeper than the record formerly achieved in Louisiana. Continental's new well was bottomed in what is possibly Domengine-Avenal Eocene sand, and is producing from the Middle Miocene equivalent to the Rio Bravo sand.

Jan 1, 1938

By J. E. House, J. L. Drobnick, R. R. Swanson, D. W. Agers

Since the commercial acceptance of the liquid ion exchange process in the mineral processing industry, it has been predicted that eventually the hydrometallurgist would have a wide selection of commercially available chemical reagents to make separations efficiently and economically of virtually all metals in solution under a wide range of conditions. Several years ago, General Mills began a research and development program to determine if it were possible to develop a reagent to extract a specific metallic ion from solution at a cost that would allow large scale commercial application. A giant step toward reaching this objective was announced in late 1963, when development quantities of LIX®-63 reagent, a highly selective reagent for the extraction of copper, were first offered to industry. The properties of this reagent were de- scribed in a previous paper.1

Jan 12, 1965

By G. E. Frantti

UNDER the auspices of the Geophysical Committee of Michigan College of Mining and Technology, an investigation was made in Michigan's Upper Peninsula to obtain geophysical data" related to the regional subsurface geology in the area covered by Paleozoic sediments. The area surveyed includes that portion of the Upper Peninsula which lies between R18W to R26W and T41N and T49N, covering approximately 1300 square miles. On the index map, Fig. 1, it is represented by the cross-hatched zone west of Munising. Four of the five sites of detailed investigation are indicated by the letters A, B, C, and D. A detailed gravity and magnetic survey had previously been conducted by J. G. Wilsonz near Perkins, 8 miles north of Rapid River, on a local anomalous area. Results of his work, which showed a large positive magnetic anomaly associated with a gravity anomaly, aroused interest in the possible economic significance of the formations underlying the Paleozoic sediments in this part of the Upper Peninsula. Early in the 1900's the Michigan Geological Survey, as well as many private companies, had done a considerable amount of dip needle work near the southwest corner of the area discussed in this paper. Most of the information available to the writer was obtained from indicated magnetic anomalies on the geological map of the northern peninsula of Michigan. Results of the geophysical activities of mining companies in the vicinity of the Marquette range and Gwinn district were unavailable to the author. Physiography and Geography: The region under consideration has low to moderate relief. About half the area is comprised of swampy lowlands, and because of the swamps and forests much of the land is almost inaccessible. The major drainage system is dendritic, with streams flowing into Lake Michigan on the south and Lake Superior on the north. The general geology, shown in Fig. 2, indicates an overlay of Paleozoic sediments on pre-Cambrian formations along a line running approximately south from Marquette (not shown on the geological map). Actual contact between pre-Cambrian and Paleozoic sediments is not known because most of the area is covered with glacial till, and outcrops are very scarce. Exposures of the Paleozoic sediments show that these beds in the northern areas dip gently under Lake Superior and that in the southern areas they 'dip gently to the southeast. Outcroppings of the pre-Cambrian formations occur primarily to the west of the surveyed area except in the northwest corner where the Laurentian series outcrop as far east as the Gwinn district and also in T46N, R24W. Instrumentation: Gravity measurements were made with the Worden portable gravity meter. Since this was chiefly a reconnaissance regional survey, both the large and small dials were used. The instrument used had a constant of 0.0035 milligals per scale division, a working range of about 25 milligals.

Jan 1, 1957

By N. O. Taylor

THE failure, by swelling, of several cast aluminum-zinc, spiral, pump rods, used to circulate water in a constant-temperature bath, brought up the question as to whether the presence of tin in varying quantities would have any appreciable influence in controlling this action. Previous workers had found the same difficulty with aluminum-zinc alloys, due to their swelling in water or solutions of electrolyte^.^ It was known that pure aluminum was practically insoluble in concentrated sulfuric and nitric acids, presumably due to the formation of an oxidized film on the surface. Concentrated sulfuric acid had little or no effect on pure zinc and tin and concentrated hydrochloric acid would attack all three metals. These facts aroused curiosity as to the probable reaction of the ternary alloys of these metals, and tests were made to determine their resistivity to the action of common laboratory reagents. Samples, covering the entire range of the ternary series of aluminum, zinc and tin alloys, were made up from good grades of the commercial metals.2 The materials were melted, at as low temperatures as possible, in graphite crucibles in a gas-fired crucible furnace. Graphite crucibles were used in preference to clay, to prevent the absorption of silicon by the aluminum, as found by previous workers. The melted materials were stirred thoroughly with pine sticks in order to ensure complete mixing and the greatest possible freedom from oxidation, and were cast in sectional, iron molds giving bars % in. in diameter and 5 in. long.

Jan 1, 1927

PRESIDENT HORACE V. WINCHELL MINNEAPOLIS, MINN. PAST PRESIDENTS PHILIP N. MOORE ST. Louis, Mo. SIDNEY J. JENNINGS NEW YORK, N. Y. FIRST VICE-PRESIDENT A. R. LEDOUX NEW YORK, N. Y. TREASURER GEORGE D. BARRON NEW YORK, N. Y.

Jan 1, 1923

By Arthur F. Wendt

Introduction.—In the year 1885, the writer signed a contract to take charge of the reopening and developing of the celebrated old mines of " El Cerro Rico de Potosi." Two years earlier, an Eng- . lish firm of engineers had made a very glowing report on the property. In the summer of 1885, telegrams arrived from the parties in charge of operations at the mountain, claiming the finding of one of the old veins, with an average richness of over 200 ounces to the ton. In the fall of 1886, the author first personally visited Potosi, but found neither the English report nor the telegram borne out by the facts. After an expenditure of over half a million of dollars and more than three years of continuons hard work, the writer succeeded in unwatering and developing one of the principal old veins of the mountain. This vein, called "Cotamitos," now yields ores of about 75 ounces to the ton, and the old historic mountains of Potosi may be said to have again fairly entered the list of silver-producers. The experience of the author, during his residence in Bolivia, and data obtained from Sr. Don F. Avelino Aramayo, form the basis of this description. POTOSI. Etymology of the Name.—The Quichuá (pronounced Keechna) Indians, known to North American students as the " Incas," although the word "inca" merely signifies ''king," or "chief," of the Quichuás, called the mountain "Sumac-orcko," or the beautiful mountain." Eighty-three years before the discovery of the mountain by the Spaniards, the inca, or king, Huaina Ccapac, travelling from Cantumarca to Calque-Porco, saw the mountain of Potosf and, admiring its grandeur and beauty, said that within its bowels there was, no doubt, much silver. He ordered his vassal* to work the mines. They, having carried their mining implements to the mountain, ascended it and were on the point of commencing work, when they heard a voice of thunder, which said: " Do not take

Jan 1, 1891

By John L. Watson

A conceptual model (MAGSEP) is described to simulate the beneficiation characteristics of a drum magnetic separator in terms of the probability of an individual grain being recovered in the magnetic concentrate. This probability is determined as a function of particle magnetic composition and magnetic field strength and is modified by particle size and the separator operating conditions. The model predicts the size, magnetic grade and distributions of magnetic and gangue minerals in the concentrate and tailings produced by the drum separator. The configuration of the magnetic concentration circuit may be altered to permit single or double drum units in parallel or series operation. The characteristics of the feed material, in terms of a magnetic parameter, are essential in permitting the determination of individual grain recovery probabilities upon which the model is based. Thus the model requires input data relating to the distribution of composite grains in terms of magnetic grade and particle size. To illustrate the use of the conceptual model an example is given for the beneficiation of New Zealand iron sands.

Jan 1, 1984

By Milton E. Wadsworth, R. Ted Wimber

Cobalt sulfate solutions containing ammonium acetate and chloroplatinic acid were reduced by hydrogen in a pyrex-glass lined autoclave in the temperature range of 170o to 232°C and hydrogen partial pressure range of 115 to 830 psia. The reduction rate was directly proportional to the hydrogen partial pressure and surface area of the pyrex glass and was independent of the quantity of chloroplatinic acid added initially. Experiments involving the variation of the relative concentration of ammonium acetate indicated that the reducible cobalt complex was probably the diacetate complex of cobalt, Co(AC)4H20, or a new mononcetate complex Co Ac, which was in solubility equilibrium with a pink precipitate of CO(AC)-4HzO. THE reaction in which a metal is dissolved by an acid to produce gaseous hydrogen and a salt solution was discovered early in the history of chemistry. In 1859 Beketoff found experimentally that this reaction could be reversed; i.e., a salt solution could be reduced by gaseous hydrogen to produce a metal and an acid. A review of work done on this phenomenon since that time may be found elsewhere., The hydrogen reduction of a cobalt salt solution is facilitated by complexing the cobalt ion. An ammonia complex of cobalt has been reduced commercially in the recovery of cobalt metal. A new reducible complex of cobalt was discovered5 when it was found that a co-baltous sulfate solution containing ammonium acetate could be reduced by hydrogen at temperatures in the region of 200°C. When a cobalt sulfate-ammonium acetate solution was heated to a temperature below its normal boiling point, a violet color became apparent, indicating complex formation. The nature of this complex was investigated5 by the addition of NH4Ac to a CoSO4 solution maintained at 85o. During the first additions of NH, Ac, the pH of the solution remained fairly constant at about 5.85. However, as the ratio of NH,Ac to CoSO, approached two, the pH rose and then leveled off at about 6.05. The absorption spectra of a Co(Ac), solution and a CoSO,, NH Ac solution were obtained at 85°C and were compared and found to be the same. These findings suggested that the diacetate complex of cobalt, Co(Ac),.4H20, was formed at 85°C. When a cobalt sulfate-ammonium acetate solution was heated to a temperature above about 165o, a finely divided pink precipitate appeared. The X-ray diffraction pattern of this precipitate indicated that it was Co(Ac), - 4H,O. In addition, it was discovered that when chloroplatinic acid, H,PtCl;, was added initially to the cobalt sulfate-ammonium acetate solution, a faster reduction was obtained. The roles of the solution complex, pink precipitate and chloroplatinic acid in the reduction process were then investigated. APPARATUS The experimental work was carried out in a two-liter stainless-steel autoclave. Adetailed description of the autoclave and the auxiliary equipment used in maintaining constant temperature and pressure may be found elsewhere.= Because the stainless steel was corroded, and also because it acted as a hydrogena-tion catalyst, an all-glass liner was fabricated such that the solution came only into contact with flame-polished pyrex glass. EXPERIMENTAL PROCEDURE The solutions used in the experimental work were prepared by dissolving reagent grade chemicals in distilled water. Although variation of the brand of ammonium acetate appeared to have no effect on the experimental results, CoSO, 7H O from the J. T. Baker Chemical Co. of Phillipsburg, N. J.,was found to give faster reductions than that prepared by Allied Chemical and Dye Corp., N. Y. The former was used throughout the course of the experimental work and was weighed up at the outset of each experiment. The ammonium acetate was dissolved to form a 6M stock solution, which was stored under refrigeration. A 10 pct solution of chloroplatinic acid (J. T. Baker Chemical Co.) was diluted to a 1.15 x 1Q2 M stock solution, which was standardized by precipitation of K,PtCl, as outlined by Scott. The appropriate volume of the chloroplatinic acid, H,PtCl,, solution was pipetted into the clean, dry glass liner. The cobalt sulfate-ammonium acetate solution, which had previously been saturated with

Jan 1, 1962

By James R. Finlay

SOMETIMES the American Institute of Mining and Metallurgical Engineers appears to be a strictly technical society, and if so my paper should deal with the technical operations of finding and producing gold. But I have not been engaged in practical gold mining since 1910. What I have been doing mainly for the last 25 years is to try to figure out what the income of a mine-gold, or any other-would be worth to an investor. So I have been in contact with gold mining, in one way or another, for some 42 years. I say that with a purpose. In that time the industry has been through one of its cycles. The value of gold mines is very dif¬ferent at different points in one of these cycles. For this reason the cycle of gold mining is a highly practical study. The cycle of gold is a more or less rhythmical change in its value or purchasing power measured in the grand average of other commodities, which is the same thing as its price. Taking the price of gold in 1897 as a stand¬ard, a dollar at that time declined to 55c. in 1913, to 26.8c. in 1920, and since then it has risen to 47.4c. in 1930 and to about 64c. in 1932. It is worth about 21/ times as much now as it was in 1920, but less than two¬thirds as much as in 1897. When this change is applied to the value of a gold mine still greater differences are evident. The cost of producing gold is of course measured in labor and other commodities, and as that cost goes down the margin of profit measured in the gold itself increases. Thus a mine which might make only 10 per cent profit in 1920 on its gross output may easily make 25 per cent now. The stockholder gets 2 ½ times more gold that is worth 2 1/2 times as much in purchasing power, therefore the real value of his holding has risen by the one factor multiplied by the other, giving him 61/4 times as much goods or services as he had in 1920.

Jan 1, 1933

By A. Faber du Faur

At the request of some of the members to whom I have shown a collection of specimens of sulphur from southern Utah, I herewith present some notes relating to the mines and the method of extracting the sulphur from the ore. In preparing these notes I have borrowed from a paper by Prof. G. vom Rath, published in the Neue Jahrbuch fur Mineralogie, vol. i., 1884, dated Salt Lake City, December, 1883. The Cove Creek sulphur-bed, now worked by the Dickert & Myers Sulphur Co., is in Beaver county, near the line of Millard county. It was first discovered by Mr. Ferdinand Dickert in 1869 ; other beds in the same neighborhood mere found by him from 1872 to 1875, making altogether 22 mining claims. The want of railroad communication prevented the early development of these claims; but in 1883 Mr. F. Dickert put up a plant for extracting sulphur from the ore, which proved a perfect success; and in 1885 the property was transferred to a stock company organized under the laws of Utah. The railroad station nearest to the Cove Creek mines is Black Rock, on the Utah Central Railroad, 204 miles south from Salt Lake City, and about 26 miles west of the mines. The road from Black Rock to the mines passes through desert and lava-bed, to the road leading from Kanosh to Beaver, which latter road it joins near Cove Creek fort, a square stone enclosure, erected by the Mormons for protection against the Indians. Cove Creek fort is situated near the eastern limit of a plain bounded on the west at a distance of about 12 miles by the Mineral range, and on the east by the Sulphur mountains, forming part of the Tushar mountains. To the northwest the plain runs into the Sandy desert. About 3 miles from the fort rises a solitary hill about 1000 feet above the

Jan 1, 1888

By P. Bandopadhyay, T. C. Rao

Geologically the Indian coals belong to Gondwana formations. Being of drift origin, these coals contain high percentage of mineral matter distributed in finely disseminated form. Indian coal-preparation plants process prime coking and medium coking coals for use in steel plants. Limited resources of good quality coking coals (Table 1) could not keep pace with the rapid developments of the iron and steel industry in India. This resulted in the introduction of coal-preparation technology and the establishment of washeries in India in the last 30 years or so. The first four washeries were set up during the early fifties at West-Bokaro, Jamadoba, Lodna and Kargali. Next came the first non-coking coal washery at Nowrozabad set up by the Associated Cement Company. In 1961, following the recommendation of Central Coal Washeries Committee (1953-54), Hindustan Steel Ltd. had set up five central washeries at appropriate locations, viz Durgapur, Dugda (2 washeries), Patherdih and Bhojudih, so that the raw coal feed having similar washability characteristics can conveniently come from a number of collieries to a particular washery. Subsequently, to meet the increasing demand of metallurgical coal by steel plants, two more central washeries (at Durgapur and Chasnala) and three pit-head washeries (at Kathara, Swang and Gidi) were installed by 1970. The prime objective of washing Indian coking coal is essentially to reduce the ash content. All the washeries in India, taken together have an installed capacity of about 26 million tons of raw coal input per annum. Details of these washeries in respect of their annual capacity, main washing systems adopted and the nature and size of the products are given in Table 2. It can be observed from this table that (1) bulk of the coal is processed in units like jigs HM baths and HM cyclones; (2) only two of the washeries have cleaning circuits for treatment of fines.

Jan 1, 1980

By HUGH E. McKinstry

OPENING the sessions of the Mining Geology Committee, the program on postwar mineral controls drew a larger attendance than any other session of the entire meeting. In view of its general interest, the papers of this session, or a substantial portion of them, are printed elsewhere in this issue. Whether control of mineral resources can help to promote peace, how controls could be applied and to whom, are questions so far-reaching that naturally no pat answer was agreed upon. In fact the discussion took on something of the flavor of a debate between those who favor strict control and those who felt that attempting to ration nations in peacetime would defeat its own ends. Discussion from the floor emphasized the difficulties in administering any international control and the $64 question, that no one cared to answer, asked by a courageous young lady who was induced to mount the rostrum for the purpose, was whether the United Nations should exchange mineral controllers to police each other.

Jan 1, 1944

By Smith, George Otis

ENGINEERING is in essence quantitative, and the engineer must deal with exact figures when he plans and, constructs. Engineering truths are not best expressed by adjectives, yet my wish, today, is not to attempt a quantitative measure of the dominant position of the mineral industry of the United States in the existing scheme of material things, but rather to seek a clualitative appraisal of what mining and metallurgical engineers are doing to promote and make secure our , national progress. Statistics help when we wish to gage material prosperity, but they fail when we desire to determine what share the engineers have in adding to the happiness and welfare of our people

Jan 1, 1928

By W. M. Small

From the one producing well in Austria, 7000 bbl. of heavy oil was produced and sold in 1933. This well, owned by the Raky-Danubia, was completed late in 1932 in the formation called Flysch (Upper Cretaceous or lower Eocene) near Zistersdorf north of Vienna. Two wildcats drilling in the vicinity have not yet reached the producing beds. Near Vienna, the European Gas and Electric Co. drilled five shallow wells for gas, three of which were failures. One gas well was completed for 8 million cu. ft. capacity at 260 meters depth and with a pressure of 570 lb. Another is being tested following blowouts. One gas well and one dry hole were completed in the pool in 1932. In Upper Austria, the same company abandoned one wildcat at 679 m. and is drilling at 280 m. on a second. No gas was sold during the year, but a line is being completed to supply fuel to boilers of the Vienna Electric Works. Hungary No deep drilling was done in 1933. Oil and gas concession was granted by Parliament to the European Gas and Electric Co. on Trans-danubia. Active geological and geophysical investigation is in progress. Czechoslovakia In the Gbely and Hodonin shallow fields, some 26 wells were drilled of which three were reported as failures. The total production of the fields was 111,736 bbl. of oil and 40 million cu. ft. of gas used as fuel in the field. At Vacenovice, where there were already two small gas wells, a third producer was completed at 420 m. This pool markets a small amount of gas, which is compressed and used to light railway carriages. Wildcat wells were reported drilling at about 300 m. depth at both Jasina and Telnice. One 700-ni. wildcat near the Hodonin field was abandoned. Another failure was reported completed and abandoned at 820 m. near Holic.

Jan 1, 1934

Jan 1, 1906

By C. M. Weld

(Cleveland Meeting, October, 1912.) IN the course of my professional work in China during the fall of 1907, I had an opportunity to visit the iron-ore mines at Ta-yeh in Hu-pei province (long. 114° 50' E., lat. 30° 20' N.). It occurs to me that a rescript and discussion of my notes taken at that time should be of interest, particularly as supplementing the exceedingly interesting recent paper-of Thomas T: Read on The Mineral Production and Resources of China.1 Ta-yeh is situated near the right bank of the Yangtze river. The mines are at an average distance of about 16 miles from the river-port Shi-hui-yao, which in turn is some 70 miles S-E. of Hankow. The ores are shipped to the works of the Han-Yeh-P'ing Iron & Coal Co. at Hanyang, as also very largely to the Japanese government iron- and steel-works at Wakamatsu, Japan. Smaller quantities have been exported to the Pacific coast of the United States. These ore-deposits have been briefly noticed in a number of publications, but, so far as I know, Mr. Read's description, in his chapter on the iron-ores of the Chinese Empire,2 contains the first attempt to define their geological character. In his more recent paper Mr. Read follows very closely the text of his earlier description. To quote briefly from the recent paper, he says : " The iron-ores at Ta-yeh . . . . lie along the contact between a marble and an intrusive body of a dark-gray syenitic rock." He refers to a figure which exhibits in plan, but not in section, the relative positions of the syenite, ore-bodies, and limestone. The contact is seen to trend approximately E-W., with the syenite on the north and the limestone on the south. " The syenite lies to the north of the marble, and a few miles farther north the marble again' appears, iron-ore again being present along the contact." No litho- 1 Bulletin Bulletin No. 63, March, 1912, pp. 293 to 343. 2 The Iron Ore Resources of the World', vol. ii., p. 913 (Stockholm 1910).

Oct 1, 1912

By Robert C. Linares

Cubic zinc sulfide has been grown from molten salt solutions substantially below the hexagonal-cubic phase transition of 1020°C. Crystals free of birefringence have been grown from molten lead chloride at temperatures from 500° to 800°C. Factors affecting the optical transmission and the birefringence are discussed. CUBIC zinc sulfide is of interest for electrooptic devices and as an optical coating material. However, it cannot readily be produced as large crystals which are free of birefringence. The birefringence arises from the fact that the cubic ZnS is usually grown as the high-temperature hexagonal phase and is transformed to the lower cubic phase by annealing.' This results in stacking faults, stress, and birefringence. A requirement for the growth of cubic ZnS is that it be grown below the phase transition of 1020°C.2 Crystals of cubic ZnS have been grown below 1020°C by the hydrothermal,3 flux,4 and vapor transport5 techniques. However, these all appear to have limitations in size or quality of material produced. It was felt that a new flux method might have a good chance of overcoming some of the previous problems. Mita6 reported the growth of hexagonal ZnS from molten NaCl and wilke7 reported the growth of iron sulfides from molten lead chloride solution, indicating that molten chlorides make good solvents for sulfides. An investigation of a number of possible molten chlorides as solvents showed that molten PbCl2 has an appreciable solubility for zinc sulfide and that crystals can be grown at temperatures from 500° to 800°C. EXPERIMENTAL Crystal growth was performed in open or sealed Vycor or fused silica tubes, in an argon atmosphere or vacuum. There were no deleterious effects due to using vacuum; however, a sealed essentially isothermal system must be used to prevent vapor transport mechanisms from dominating. This will be discussed later in detail. Noble metal containers were not usable as they were severely attacked by these melts. The materials used were: reagent-grade PbC12, reagent-grade ZnS, optical-coating-grade ZnS, and Irtran 2 (ZnS). Crystal growth was accomplished by both slow cooling techniques and gradient growth techniques. In the slow cooling techniques, 15 g of ZnS and 100 g of PbCl2 were used. The components were placed in the silica tube, heated at 800°C for 2 hr, and then slowly cooled (l° to 10° C per hr) to 500°C. The furnace was constructed so that the tube could be inverted, thus allowing the liquid to drain off the crystals at the end of the run. The gradient runs were made by placing the above mixtures in a silica tube at 550° to 600°c, Fig. 1. A temperature gradient was maintained such that the floating mass of undissolved sulfide was 10° to 50°C warmer than the bottom of the tube. Growth occurred on spontaneously nucleated sites at the cooler bottom. RESULTS When using high cooling rates (5° to 10°C per hr), crystals form in thin sheets perpendicular to the {111} face. Crystals 5 by 5 by 1.2 mm, Fig. 2, have been ob-

Jan 1, 1969