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By Augustus Locke

San Francisco Meeting, October, 1911.) Two Opposed Interpretations of the Tonopah Structure.-The important geological publications concerning the Tonopah mining-district are those of Spurr 1 and of Burgess.2 In these publications are presented fundamental differences of interpretation, which are the more interesting because both authorities have had ample opportunity for observation, and because both are geologists of proved ability. I was vastly puzzled to know which had the better of it, and in order that I might reach a conclusion in my own mind, I recently spent some time in the district going over the physical evidence. Surprising as it may seem, this evidence looks agreeably conclusive. A review of it will, I believe, be of interest to those who are familiar with the previous publications. The general geological features of Tonopah are shown in Fig. 1, and the differences of interpretation referred to are outlined in the accompanying notes. Briefly, Burgess regards the various rocks as flows, lying in the order of their deposition. Spurr regards them in part as flows, and in part as flat-lying intrusives. The disagreement, then, concerns the rocks regarded on the one hand as intrusives, and, on the other hand, as flows. These rocks are chiefly the so-called calcitic andesite, the upper rhyolite, and the lower rhyolite. Economic Importance of the Question of Interpretation.-The economic importance of the question of interpretation is, of course, limited to its bearing on the probable distribution of 1 Geology of the Tonopah Mining District, Nevada, Professional Paper No. 42, U. S. Geological Survey (1905). Report on the Geology of the Property of the Montana-Tonopah Mining Co. (1910). An abstract of this report is given in the Mining and Scientific Press, vol. cii., No. 16,p. 560 (Apr. 22, 1911). 2 The Geology of the Producing Part of the Tonopah Mining District, Economic Geology, vol. iv., No. 8, pp. 681 to 712 (Dec., 1909).

Feb 1, 1912

By D. O. LIVINGTON

(Presented by invitation at a meeting of the Spokane Local Section of the institute, Feb. 17, 1912.) THE Pilares de Nacozari mine is located in Sonora, 75 miles south of Douglas, Ariz. The town of Douglas is on the International Boundary and is the place at which the ores from the Bisbee mines are smelted. The Moctezuma Copper Co. owns the mines at Nacozari, and the copper-concentrates shipped to the Copper Queen smelter, at Douglas, make a good smelting-mixture with the Bisbee ores. The Moctezuma Copper Co. and the Copper Queen smelter at Douglas, as well as the railroad from Douglas to Nacozari, are owned by the Phelps Dodge Co. The ore-deposit occurs in the form of a large ellipse with a major axis of approximately 2,000 ft. and a minor axis of about 600 ft., the major axis bearing about 90 W. of N. The whole of this ellipse is more or less mineralized; the surface being principally an iron gossan with some occasional copper-stains. Below the oxidized zone, which is not more than 50 ft. deep, the minerals are pyrite and chalcopyrite, with occasional seams of chalcocite, the latter being rare. There appears to be no well-marked zone of secondary enrichment, the oxidized gossan over the greater part of the deposit changing suddenly to what is apparently the original unaltered ore. The copper-values are concentrated around the perimeter of the ellipse, and it is principally around this perimeter that the mining is done. The ore mined averages a little more than 3 per cent. of copper, with a small amount of silver, less than an ounce per ton. Some ore of considerably higher grade than this has been shipped, however, but the above average is of the mill-run. The ore is wider near the two ends of the ellipse than along the sides, and is mined in some cases to a width exceeding 200 ft. The country-rock for the first vertical 500 ft is a volcanic acid breccia, probably rhyolitic; below

Sep 1, 1912

By AIME AIME

THE Seventh International Petroleum Exposition and Congress to be held in Tulsa, Okla., Oct. 4 to 11, inclusive, in true western spirit promises to be bigger and better than ever. The Exposition has become an established institution. It gives opportunity to petroleum engineers, technologists, and operators to see each year at one place what the tool makers and machinery manufacturers have to offer which is new or better. It has truly become a place "where men, methods and machinery meet." It is also a convenient focus for technical meetings of various kinds devoted to petroleum and natural gas problems. 'The Petroleum Division of the A. I. M. E. has for several years held its chief fall meeting at Tulsa just preceding the opening of the Es- position. This year our meeting will be on Oct. 2 and 3 and it will be held as usual at Hotel Mayo. The Mid- Continent Oil and Gas Association will, as usual, hold a meeting during the Exposition and this year the Petroleum Division of the A. S. M. E. will hold a three- day session, Oct. 6-8, in the auditorium on the Esposition grounds. In all, six technical sessions are planned by this Society, and aside from reports of committees some 20 technical papers are to be presented. Members of the Institute should attend its own meeting and stay over for as many days as possible for the other meeting at which they will hear and see much of helpful interest.

Jan 1, 1930

By Moshe Sheinkin, Douglas E. Julin

Large tonnage operations face many problems in adequately planning ahead for future years production. In order to maintain desired levels of production, such problems as source of tonnage, man- power and equipment requirements, tailings disposal and water requirements must be anticipated. Of course, before any of these problems can be analyzed, daily tonnage requirements and its source must be determined. Looking ahead for one year or even two or three is usually not sufficient time to adequately prepare an area for production. Because of the sequence of mining and the multilevel nature of the 42,000 tpd Climax mine in Colorado long-range planning must be on a ten-year basis. By using a ten-year base, adequate time is allowed to gain access and prepare a new level for production. Usually eight years will be required for this phase of the initial mine preparation. Once production has been started on a level and access to the area is available, three years is usually sufficient to prepare a new block for production as long as it follows in the normal sequence of mining.

Jan 4, 1967

Adams, Benjamin C., Jr., Student, Univ. of Oklahoma Norman, Okla. '36 Adams, Ernest C., Student, Univ. of Illinois 908 W. Green St., Urbana, Ill. '35 Adams, George H., Student, Colorado School of Mines Golden, Colo. '36 Adams, Robert Keller Mitchell Hotel, No. 18, Golden, Colo. '35 Afshar, Hadji Khan A., Student Box 63, Univ. Sta., Moscow, Idaho. '36 Ahrenholz, Herman William, Jr., Student, Lehigh Univ Bethlehem, Pa. '35 Alger, Robert P., Student, Missouri School of Mines & Met.Rolla, Mo. '36 Allen, Paul W., Student, Mass. Inst. of Tech Cambridge, Mass. '35 Allen, R. M., Jr., Student, Virginia Polytechnic Inst., "G" Co.Blacksburg, Va. '35 Alley, John Arnold, Student, Montana School of Mines Butte, Mont. '36 Amberger, R. H., Student, Michigan College of Min. & Tech Houghton, Mich. '35 Ambrosiani, F. Peter, Student, Michigan College of Min. & Tech Houghton, Mich. '36 Andersen, Burton Lee, Student, School of Mines, Univ. of Washington Seattle, Wash. '36 Anderson, Carlos, Student, Univ. of Oklahoma Norman, Okla. '36 Anderson, J. Wendell, Student, Pennsylvania State College State College, Pa. '36 Anderson, Joseph S. Cornelia Hotel, Ajo, Ariz. '35 Anderson, R. C., Student, Univ. of Washington Seattle, Wash. '35 Anderson, Roy A., Student, Washington State College Pullman, Wash. '35 Anderson, Willard. Student. Univ. of Oklahoma Norman, Okla. '36

Jan 1, 1936

By W. F., Netzeband

SEVERAL criteria have been used more or less successfully in finding and developing orebodies in this district. Among them is the relation of the fracture to the orebodies. It has been known for some time that there was some relation, but it has been but recently. that careful study has been given to this subject. Like all the criteria used in this district, this relationship must be used with caution, for what-is true in one part of the district is not necessarily true in another.

Jan 1, 1928

By D. W. Hutchinson, W. W. Wen, A. A. Terchick, J. C. Anderson

It is estimated that approximately 3% of the raw coal processed today in coal preparation plants throughout the nation will ultimately report to slurry-tailing disposal (Anderson, 1975). The usual disposal method is to pump refuse slurry containing - 48 mesh (300 pm) refuse into dams or impoundments constructed of coarse refuse. The failure of an impoundment at Buffalo Creek, Saunders, WV (Anon., 1972) resulted in an evaluation of refuse disposal methods by various regulatory agencies as well as coal producers. The result of this evaluation was the promulgation of federal regulations dealing with the construction, operation, and final abandonment of coal refuse disposal area. As a consequence of these regulations, the use of the landfill/impoundment method of disposal became in some cases economically unfeasible or technically impossible. US Steel has studied a number of alternative methods of refuse disposal. During an investigation of mechanical dewatering with a pressure filter, portland cement was added to the slurry to solidify the filter cake. Because of the success of the cement addition, it was decided to study the stabilization of fine coal refuse slurry through use of cement-type additives. The goal of the investigation is to develop a process that will use cement-type additives to solidify the refuse slurry into a form that can be handled and stacked with the coarse refuse, thus eliminating the need for slurry impoundments.

Jan 1, 1982

By John J. Howard

WE are approaching the depletion of our principal source of iron ore-the Great Lakes deposits, which have provided 85% of the nation's requirements for the past fifty years. This situation presents a threat to our standard of living and our position as a world power. Fortunately, in the Great Lakes region there are still tremendous quantities of potential iron ore in the form of the low iron, high silica rock called taconite. The economical extraction of iron from taconite will insure our future steel supply if no new deposits available to the United States even in time of war are discovered. In the new process presented here, the iron is reduced directly by a simple method and then separated from the silica. The product is "feed," not to the blast furnace, but to the steel plant. This process requires very much less plant, less physical and chemical treatment, and less fuel and auxiliary materials than the conventional ore concentration-blast furnace method. In my opinion, this new, fundamentally different approach offers a better hope for the solution of the iron ore problem.

Jan 5, 1950

By G. W. Healy, W. D. Forgeng, N. R. Griffing

The liquidus surface of the C-Cr-Fe system to 1900°C has been mapped from carbon solubility and freezing point measurements, metallographic observations, and published data. In the graphite field, the surface drops precipitously to meet a slope descending from the Cr3C2-C join through the mixed carbide fields to a meandering eutectic valley; this flows from the Cr-C to the Fe-C edge. On the low-cavbon side of the valley, the surface rises to the chromium corner. 1 HE purpose of this inquiry was to gain a more complete knowledge of the C-Cr-Fe liquidus surface. This required an extensive study of carbon and chromium-rich alloys which, in the past, have received the least attention. Sanbongi el al.1 measured the solubility of carbon in liquid alloys containing up to 25 wt pct Cr at temperatures of 1460" and 1545°C and found that it increased with chromium content and temperature. Lucas and wentrup2 also made solubility experiments in graphite crucibles, but at higher chromium contents in the range of 38 to 80 pct and at temperatures of 1550" to 1700°C; however, their experiments were relatively few, and the effect of temperature was not consistent. The present investigation included compsitions ranging from 0 to 94 pct Cr and 1.4 to 11.7 pct C at temperatures up to 1800°C. Saturation experiments in graphite crucibles, thermal analyses during freezing, and metallographic and X-ray diffraction studies were employed to obtain desired information which, together with published data from other investigations about the binary edges and the ternary system at lower carbon levels, made possible the construction of a comprehensive C-Cr-Fe liquidus surface. C-CR-FE LIQUIDUS SURFACE The derived ternary liquidus surface is shown in Fig. 1 where the solid curves are liquidus isotherms. The dashed curves and the binary edges are the liquidus field boundaries of the primary crystals, the arrows along these boundaries indicating their direction with decreasing temperature. Each intersection of three internal boundaries is the composition of liquid involved in four-phase isothermal equilibrium with the three primary crystals whose liquidus fields touch there. It may be observed that a total of six four-phase equilibria occur at melt temperatures. The general topography of the liquidus surface consists of a eutectic valley sloping down from the Cr-C edge at 3.2 pct C to the Fe-C edge at 4.25 pct C. The liquidus surface rises in two directions from the valley, one hillside terminating at the Cr-Fe edge while the opposing hillside rises toward the carbon corner out beyond the top edge of Fig. 1. Both hillsides are interrupted by intersections of surfaces or joints representing the liquid colmpositions of various three-phase equilibria. Seven primary crystals occur, namely a(bcc), ?(fcc), graphite, (Fe, Cr)3C capable of dissolving as much as 15 pct Cr, and three different chromium carbides in which iron is partially soluble by substitution for chromium. The composition ranges of the primary l~hases at melt temperatures are shown

Jan 1, 1962

By V. GUDKOV

THE iron-ore deposits of Russia were estimated at 2,200,000,000 by the Russian Geological Survey, in 1910; but this estimate must be considered as being far too low. The estimate for Siberia, which had been explored very little for iron ore, was placed at about 27,000,000 tons. The exploration, in 1912-14, of the three iron deposits-Blagodat, Baakal and Kamensk-raised the estimate of the iron-ore reserves or the Urals from 282,000,000 tons to about 400,000,000 tons. Conservative estimates of the explored deposits made by the writer in 1915, gave the following figures: Southern Russia 900,000,000 tons, Ural Mountains 500,000,000 tons, Central Russia 900,000,- 000 tons, Siberia 100,000,000 tons, Caucasus 20,000,000 tons, or a total of 2,420,000,000 tons of iron ore, or 1,200,000,000 tons of pig iron.

Jan 1, 1921

THE third annual Joint Western Mining Convention, held at Los Angeles, Sept. 10 to 13 inclusive, was a notable success both as to attendance and interest. Registration the first day amounted to 201, and the total crept up to 347 before the close. The American Institute of Mining Engineers was well represented, approximately 80% of those registered and most of the speakers being members. This illustrates largely the amount of interlocking membership and the reason for holding at one time and place meetings of the several related organizations. The plan has proved so successful that it is probable that Spokane will extend an invitation for next year that seems likely to be accepted. It is proposed that the convention be timed so as to permit visitors from the East to stop there Oct. 3 to 5, en route to the American Institute of Mining Engineers meeting at San Francisco, Oct. 7 to 9. Simultaneously, it is expected that the Petroleum Division will hold its fall session at Los Angeles, the two streams of travel meeting in San Francisco, just before departure of the party of engineers traveling to Japan to attend the World's Engineering Congress. The Los Angeles meeting opened Monday morning with a general session under the auspices of the Western Division of the American Mining Congress with Philip Wiseman in the chair. After a series of short responses to the welcome extended, Charles W. Merrill discussed the needs of the western mining industry. A complimentary luncheon to members and delegates followed.

Jan 1, 1928

By Louis D. Huntoon

After the completion, in 1905, of the Hammond Mining and Metallurgical Laboratory of the Sheffield Scientific School, Yale University, it became necessary to secure and assay a large assortment of ore-samples, and to arrange the results in such a manner as to admit of use with the least amount of work on the part of the instructor. At first, pulp-samples, together with their respective assays, were secured from the mines, smelters, and public aesayers, but this practice did not prove satisfactory. It was not only difficult to secure a suffciently large supply of material, but it was also impossible to secure the proper assortment required for instructing students. It involved considerable work for the donors to select the samples and furnish a record of the assays, and also for the instructors to examine each pulp and determine its character. Some of the samples did not contain a sufficient quantity of pulp for the student to check his work in case his first assay did not correspond to the record. In order to increase the number of samples and to vary the character of the material, pulp-samples were later mixed with barren rock and with sulphides, but this method also was unsatisfactory and has been discontinued. At present, small lots of ore are secured by gift or purchase from engineers, public assayers, and the managers of mines, mills, and smelters. These lots weigh from 10 to 100 lb. each, and are rarely finer than 0.25 in. in size. The larger samples permit of a careful study by the instructor in order to determine the best method of assaying to be followed. In universities in which assaying is taught the record of the samples should fulfill the following requirements:

Jan 1, 1910

By William J. Coulter

WITHIN the past thirty years the United States has been involved in two tragic, vicious, and costly world wars. To make the world safe for democracy was the reason given for our participation, but the confusion and misunderstanding that prevails all over the world today suggests that war is not the proper approach to the attainment of that utopia. These conflicts were conceived and prosecuted by nations far advanced in civilization and culture. Their best manhood was sacrificed, a staggering tax burden was saddled on their peoples, huge financial losses were incurred, destruction of property was appalling, and cultural and peaceful scientific advancement received a setback that may require centuries to retrieve. Therefore, some basis is established for the conclusion that progress in the past fifty years has been most outstanding in the development of instruments used for death and destruction, and that progress in this direction between the two World Wars would indicate that the next war will go far toward total destruction of world civilization.

Jan 1, 1946

By Raymond C. Johnson

GASIFICATION is important to the anthracite industry, as it is to the entire solid-fuel industry and to the nation. However, to the anthracite industry it may have particular significance in that it would increase the market value of many millions of tons of a by-product fuel, which the industry now has in storage and is currently producing, in addition to increasing the potential market for all its products. The by-product fuel is of usable quality but the ash content is higher than it can be in other products and therefore it must be converted or used at the point of production. Gasification is one method by which the product may be given increased value. The inherent characteristics of anthracite make it well suited for producing a fuel or synthesis gas. It is the most concentrated form of natural commercial carbon, noncaking and noncoking; it does not produce smoke, tar, or soot and has a low sulphur content; and the volatile matter, which ranges between 2 and 8 pct, is 80 to 85 pct hydrogen with small amounts of methane, carbon dioxide, carbon monoxide, and nitrogen. The ash fuses at high temperatures, which allows it to be burned at high rates without slagging. However, with the addition of small amounts of dolomite, the ash will form a slag, or glass, which is very fluid. Anthracite has long been used in the manufacture of city gas and it is extensively used in various parts of the country to make water gas to be converted to hydrogen. Buckwheat and rice anthracite are used in Galusha producers to make producer gas. Excellent synthesis gas has been made in a Galusha producer with rice and barley anthracite with oxygen in tests at the Consolidated Mining and Smelting Co., Trail, British Columbia. In these tests, anthracite was shown to have advantages over competitive fuels, in that the gas had a higher hydrogen content and could be cleaned with less difficulty. The anthracite seams are steeply pitching and in mining the parting strata and some of the roof and bottom materials are taken with the coal. In preparation, these materials are separated by gravity from the commercial product and stored in refuse banks. This refuse contains a mixture of rock, slate, or shale, and high-ash anthracite with bone coal, which is low-ash coal that is interspersed with thin bands of shale. The bone coal contains between 25 and 50 pct ash with an average ash content of approximately 30 pct, with a

Jan 1, 1953

By Paul Hunt

UP to June, 1923, the Park-Utah mine had shipped about 94,000 tons of a direet-smelting ore of a gross value of $4,200,000, or about $45. a ton. These values were in gold and silver only, although the ore carried small amounts of lead, copper and zinc. Freight, treatment and deductions had averaged $15.40 a ton. At the expiration of the Pittman Silver Act there was in sight about 30,000 tons of a similar ore with a gross value of about $15 a ton in gold and silver, and a large body of partly developed lead-zinc ore of a gross value of about $20 a ton, 40 per cent. of which was represented by the lead-zinc content and the balance by the silver and gold. Mine costs had been high during the life of the Pittman Act, but as a large part of the profits had gone into equipment of the mine and the orebodies were large and had good walls, we knew that mine costs could be greatly reduced. We were therefore faced by the necessity of getting lower freight and smelter rates or of concentrating the ore. We did obtain better freight rates on lower grade ore, and a favorable smelting rate on the small tonnage of siliccous silver-gold ore, but this smelter rate could not be applied to the lead-zinc ore with any profit to ourselves. The Judge mill of the Park City Mining & Smelting Co., with which we were affiliated, was running to capacity; if we built our own mill it ineant a 5-mile freight haul to a satisfactory millsite and a year's delay. Fortunately, the International Sillelting Co. had just inherited a mill at Tooele which, with some changes, was about double the catpscity required for its own ores. Flotation tests were run on Park-Utah ore and a contract entered into with a low base treatment charge per ton, the tariff being largely fixed by the metallurgical deductions. This contract has been admirably calculated so that the miner can follow a lean orenbody to its limit. Such a procedure has no doubt made it difficult for the smelting company at times, but it has resulted in finding ore extensions that otherwise might have been missed, so In the long run it has profited too. A flat rate per ton would have been like mining up to the claim endlines in a great many of the stopes. In order to offer such a contract it can be inferred that the smelting company must have been able to make high reeoveries and high-grade products on a very lean ore.

Jan 1, 1928

By John W. Padan, John E. Crawford

Beginning with a small but positive participation in undersea mining, the Bureau of Mines continues its active investigations into this potentially tremendous field. The Bureau began its active role in undersea mining in September 1963, with a small task force of three dedicated scientists and a secretary, establishing headquarters at the old Tiburon Naval Net Depot about seven miles up the coast from San Francisco. The past months have been both busy and productive. With 22 Federal agencies involved in oceanography, it logically was the intent of Congress that the Bureau of Mines undertake research concerned only with the technology of marine mineral production and utilization. The Bureau has maintained this purpose in its activities at Tiburon, for while institutes, universities, the Navy and other Government agencies have developed exceptional programs in the fundamental science of the oceans, commonly called oceanographic research, little has been done toward advancing man's ability to exploit the ocean floors other than by drilling for oil and gas and sulfur.

Jan 3, 1965

By B. T. Brady

Rock mechanics, like all engineering disciplines, must have a theoretical foundation. The subject of this chapter is the formulation of analytical methods that may aid in the rational design and determination of the stability of engineering structures in competent brittle rock materials. By an engineering structure in rock, we mean any (1) excavated sub- surface opening, (2) open surface structure, or (3) system of openings in rock that is virtually self-supporting-that is, not requiring artificial systems to carry structural stresses.

Jan 1, 1970

By F. P. Bullen

Empirical relationships between fracture stress, orientation angle, and diameter of crystal have been determined at 77°K. Orientation ranges of markedly different behavior were found—a law of constant normal stress&apos; of value a (diameter)-1/2 for the fracture of ductile crystals, and a condition of shear stress (or strain) for more brittle crystals. The observations are not consistent with current theories. An interpretation is advanced which is also applicable to observations on the effect of prestrain at room temperature on the subsequent fracture stress at 77°K and to the effect of cyclic stressing on the cleavage strength.&apos;&apos; The law of constunt normal stress&apos; and the brittle ductile transition are also explained. The interpretation is more consistent with the initiation of cracks by intersecting dislocations than with theories based on stress -concentration by dislocation arrays. ZINC single crystals are particularly suited to the study of cleavage because fracture occurs on the basal plane over a wide range of crystal orientations. Analysis of the conditions of stress and strain at fracture in crystals of different orientations should indicate which parameters control the cleavage process. Unfortunately, controversy has arisen over the correct empirical relationship between tensile fracture stress and orientation. Schmid&apos;s observations1,2 favored a &apos;law of constant normal stress&apos;, as observed in other materials.2 For zinc, however, the observed values are far below the theoretical strength and cannot represent the true limit of cohesion between neighboring atomic planes. Hence, the interpretation of such a &apos;law&apos; is not straightforward. Deruyttere and Greenough3,4 found a complex variation between tensile fracture stress and orientation; this variation did not agree with a &apos;law of constant normal stress&apos;. Two theories have been advanced to account for their observations: a) the propagation of cracks from low-angle boundaries,5 and b) the release of energy from piled-up dislocations during crack-propagation.4 The present work resolves the apparent discrepancy between the observations and shows that neither of the above theories are applicable to the tensile fracture of zinc single crystals. A phenomenological explanation, along the lines suggested by Gilman,&apos; is advanced and successfully applied to previously unexplained effects. EXPERIMENTAL DETAILS &apos;Crown Special&apos; redistilled zinc was used, except for one comparison series op tests using &apos;Tadanac&apos; electrolytic zinc. Crystals of 1 mm diam, subsequently called &apos;1 mm crystals&apos;, were grown from the melt in vacuo in precision-bore Pyrex tubes internally coated with graphite. Several specimens 1 in. long were cut from each crystal and chemically polished. Jigs were used to minimize handling strains, and crystals were mounted in the Polanyi machine the day prior to testing to allow recovery from any such strains. One-mm crystals were chemically polished for long periods to obtain 0.1 mm (approx) crystals. One-mm crystals were cemented into miniature gimbals by &apos;Araldite&apos; casting resin. The Appendix gives the reasons for using gimbals and the results obtained by other methods. More complete details of all techniques are given elsewhere.7 The symbols and terminology used are as follows: X = orientation angle (angle between tensile axis and line of greatest slope in the basal plane). T = tensile stress (on true cross-section) S,N = shear and normal stress (components of T with respect to the basal plane) ? = shear strain D = crystal diameter. The subscript &apos;f&apos; will be used to denote values at fracture. PART I-ANNEALED CRYSTALS EXPERIMENTAL OBSERVATIONS One-mm crystals were used to establish the variation of fracture stress at 77°K with orientation at fracture (Xf), Fig. 1. For 18 deg = Xf = 55 deg, a &apos;law of constant normal stress&apos; was observed. For Xf > 55 deg, the fracture condition approximated to a constant shear stress. At Xf< 18 deg, twinning occurred before fracture so that the results were not typical of homogeneous single crystals,4,8— such specimens will not be considered herein. The dependences of fracture stress upon Xf were of similar type for 6 mm,* 1 mm, and 0.1 mm crystals,

Jan 1, 1963

By Sidney G. Parker, Jack E. Pinnell

Cubic ZnSe crystals have been grown with HCl, HBr, and I, as chemical transport reagents. The growth of large, well faceted crystals is in the order HCl < HBr < I, with some produced by I, transport being 1 cm on an edge. ZnSe:I crystals showed no strain in cross polarized light and were homogeneous as determined by electron microprobe. These ZnSe:I crystals had a mobility at 25°C of about 300 sq cm per v-sec and contained 103 dislocations per sq cm; further, these crystals were pure cubic and showed both photolumi-nescence and photo conductance. Doping was attempted during crystal growth. ZnS and Zn (S,Se) crystals were also grown by I, transport. ZnSe crystals have been grown by most of the common techniques.1"6 Of these, chemical vapor transport as developed by Kaldis2 showed promise of producing high perfection, cubic ZnSe. With chemical transport, crystals can be grown far below the transition temperature for conversion of cubic to hexagonal structure. A small temperature gradient between source and growth region tends to allow near equilibrium growth, which should lead to good crystalline perfection. Because it is necessary to form volatile compounds, halogens or their compounds are extensively used as transport agents. HCl, HBr, and I, were compared as transport agents for growth of ZnSe crystals. Doping during crystal growth was attempted. ZnS and ZnSxSe1-x crystals were also grown by chemical transport. Electrical and optical properties of the crystals were examined. EXPERIMENTAL Fig. 1 is a sketch of the growth apparatus, which was a modification of Kaldis&apos;. A quartz rod which butted against the seed crystal served as a heat sink to promote growth only on the seed. Initially, crystal growth was attempted with ZnSe prepared by wet chemical methods. Because such a material contained oxides and selenates, HC1 reacted with these oxygen compounds to form H2O and no ZnSe transport occurred. Further, this ZnSe contained about 10 ppm Cu plus other impurities. High purity ZnSe, containing small amounts or no oxygen compounds, was prepared by reaction of H2Se with zinc vapors at 600° to 800°C in an atmosphere of palladium diffused H2.7 The ZnSe thus produced was usually copper free and contained only 1 ppm by weight of magnesium as determined by emission spectrographic analysis. G.E.&apos;s electronic grade ZnS, which had about 10 ppm metallic impurities, was used without further treatment. ZnS-ZnSe charges were prepared by mixing the two compounds together, then sintering 24 hr at 1100°C in an H2S ambient. The gases, HBr and HC1, were commercial grade, of 99.9 pct purity, while the I2 was 99.999 pct pure. The single crystal seeds with (111) faces for growth were mechanically held in place by sealing the outer quartz tube to the growth tube. After the charge was introduced, the system was outgassed at l0-5 torr while heated to 500°C. The desired quantities of transport reagents were then sealed off in the system, which had been cooled to 25°C. The growth tubes were inserted into a furnace with the desired temperature and thermal gradient. The system was allowed to cool for 1 to 12 hr from growth temperatures of about 850" to 25°C. The tubes remained stationary during crystal growth. HCl CHEMICAL TRANSPORT GROWTH Preliminary runs with HC1 had a temperature gradient of 100° to 200°C and no seed or heat sink. Only small crystals were obtained in these experiments as

Jan 1, 1970

By A. Gemperle

Electron diffraction and transmission electron microscopy on foils at room temperature were used to investigate the ordering of Fe-Si alloys containing 10 to 23 at. pct Si. A certain degree of DO3 order was found in all alloys. With the exception of the lowest silicon concentration for which the antiphase domains could not be clearly resolved, the alloys have a domain structure of two-domain type with boundaries having 1/4a01<111> displacement vectors for less than 12.3 at. pct Si and with boundaries having 1/2 a0<100> displacement vectors for more than 12.3 at. pct Si. The alloys with 12.3 at. pct Si have a domain structure consisting of fine domains with 1/2a&apos;o<100> boundaries within much larger domains with 1/4a&apos;o<111> boundaries. The development of these structures can be explained by transition of the alloy from the disordered state into the B2-type order and then into the D03-type order by the mechanism proposed previously for the FeSAl alloys. The existence of the B2 structure in the lower part of the investigated concentration range reported in some articles can be explained by fine domains with 1/2a&apos;o<100> boundaries formed by several disordered planes within large domains with 1/4a&apos;o<111> boundaries. The ordered structure predicted by the theory —with practically no domain boundaries —is found in the alloys having 12.3 at. pct Si where it develops in the B2 structure region. ORDERING in Fe-Si alloys was first studied by phragmenl who found that beginning with 13 at. pct Si the DO3 (Fe3Si) superlattice reflections appear in the diffraction patterns. The equilibrium diagrams constructed later by corson2 and Haughton3 from various measurements proposed the existence of a homogeneous solid solution (a phase) in the range from 0 to 25 at. pct Si. Jette and Greiner4 and Farquhar et al.5 measured the relation between lattice parameter and composition and they considered the break in the curve at 9 to 10 at. pct Si to be caused by the ordered solution a"(Fe3Si). Glaser and Ivanick6 Determined critical ordering temperatures of the alloys containing from 10.9 to 27.9 at. pct Si from the measurement of the electric resistivity of quenched samples. In all cases the critical temperature was lower than the melting point and it was highest for 25 at. pct Si. Lihl and Ebel7 measured the lattice parameter curves at various temperatures up to 1000°C. The region between two breaks on these curves, corresponding to 10 to 12.5 at. pct Si at room temperature, was considered by them to be two-phase (a + a"). They concluded by extrapolation of the measured values that a" in the alloy having 25 at. pct Si is stable up to the melting point. Davies8 studied superlattice reflections in the X-ray diffraction patterns of an alloy containing 8.7 at. pct Si. He found the B2 structure and short-range order in the slowly cooled samples and the DO3 A. GEMPERLE is Research Scientist, Institute of PhysicS, Czechoslovak Academy of Sciences, Prague, Czechoslovakia. __Manuscript submitted January 2, 1968. IMD structure in the quenched and annealed samples. This investigation first reports the presence of the B2 structure, phase a&apos;: in Fe-Si alloys. Meinhardt and krisement9,10 also found its existence in Fe-Si alloys by neutron diffraction. No order was detected by them in the alloy containing 8 at. pct Si. The onset of B2 order was observed at a composition of 9.2 at. pct Si. They found almost perfect B2-type order with partial DO3-type order at room temperature in the 10 to 12.5 at. pct Si range and almost perfect DO3-type order in the 12.5 to 25 at. pct Si range. They established the critical temperatures Tc of both the structures through measurement at higher temperatures. The critical temperature for the B2 structure was found to be always higher than the critical temperature for the DO3 structure of the same alloy. They extrapolated the curves of the critical temperatures and concluded that the alloys with more than 17 at. pct Si have the B2 structure up to the melting point and the alloys with more than 23 at. pct Si have the DO3 structure up to the melting point. The results of Meinhardt and krisement9,10 were confirmed by Dokken&apos;s measurement" of the temperature dependence of the electrical resistivity in the 10.8 to 15 at. pct Si range. On the other hand chessin12 detected by X-ray diffraction a considerably lower degree of order in the 12.7 at. pct Si alloy. ANTIPHASE DOMAIN STRUCTURE IN ALLOYS WITH B2- AND DO$-TYPE ORDER The ordered structures B2 and DO3 can be described in terms of a subdivision of the bcc lattice into four fcc sublattices with a parameter double that of the bcc lattice. Following Marcinkowski13 we will label them I. 11, 111, IV. The B2 structure in the AB alloy is formed by placing A atoms on sublattices I and II and B atoms on sublattices III and IV. In a non-stoichiometric perfectly ordered alloy having concentration (A) > (B), A atoms occupy sublattices I and 11. and A and B atoms distributed at random occupy sublattices III and IV. The DO3 structure in an A3B alloy is formed by placing A atoms on sublattices I, 11, and 111, and B atoms on sublattice IV. In a nonstoichiometric, perfectly ordered alloy having concentration (A)/3 > (B), A atoms occupy sublattices I, 11, and 111, and A and B atoms distributed at random occupy sublattice IV. As further shown in Ref. 13, two types of domains are possible in the B2 superlattice and the antiphase domain structure has associated with it boundaries with displacement vectors 1/4 a&apos;o<ll1> only. Four types of domains are possible in the DO3 superlattice and the antiphase domain structure has associated with it boundaries with displacement vectors 1/4a&apos;o<111> and 1/2a&apos;o<l00>. Bethe14 suggested on the basis of theoretical considerations that in a structure with two sublattices at low temperatures only one domain should be present in the whole crystal at equilibrium. Similarly Bragg15 concluded that at low temperatures the domain struc-

Jan 1, 1969