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By Eugene P. Pfleider

RECENT interest in germanium centers around its use as a semi-conductor of electricity in electronic devices. It is generally believed that germanium transistors, diodes, triodes, photocells, and rectifiers will largely replace the present-day vacuum tubes. The germanium electronic devices are much smaller, lighter, and more resistant to shock, and they require only a small fraction of current required for conventional devices. Hence only a small amount of heat is given off by the equipment. This development will require many times the quantity of germanium now being produced, which in 1948 was approximately 1000 lb' and was obtained almost entirely from zinc ores in Missouri, Kansas, and Oklahoma. No one knows with certainty what the demand will be for ger-manium by 1956. It may be 40,000 lb.1 Known concentrations in zinc ores are not sufficient to

Jan 1, 1954

By D. P. Koistinen, K. E. Beu

THE application of the integrated intensity X-ray diffraction method to the measurement of retained austenite concentrations in hardened steels has been fully described.'-' In developing this particular method, the assumption was made that the samples used would have flat surfaces which were free from voids and in which austenite was homogeneously distributed. The original calculation procedure' was modified to include the constant factor G which relates the intensity of a given diffraction line to the concentration of the component giving rise to that line. In order to include A (0) in the constant factor G, it was further assumed that the geometrical conditions relating the X-ray beam, camera cylinder, and sample surface were precisely met.V has been demonstrated that these geometrical conditions can be met experimentally without difficulty in many cases;' however, for those samples which have irregular surfaces or where it is impossible to locate the sample in the proper position with respect to the X-ray beam and film cylinder, it is desirable to evaluate experimentally what effect these nonideal conditions have on the reliability of the austenite determination. This note decribes the results of such experiments. SAE 1095 bar stock was used throughout and all samples were heat-treated as follows: 1600°F for 1 hr in a neutral atmosphere, brine quench, and 300°F temper for 30 min. To control heat-treatment conditions as closely as possible, all samples were plated with 0.002 in. copper to protect the immediate surface from the heat-treating atmosphere. After heat treating, the samples were deplated electroly-tically so that only the copper was removed. The heat-treated surfaces thus obtained were nearly as bright and polished as the original surfaces before copper plating although no mechanical work was done on the samples after heat treating.

Jan 1, 1954

By A. A. Burr, D. G. Ebeling

The effects of casting texture, grain orientation and grain size upon the performance of Alnico permanent magnets is described. Single-crystal specimens were produced by special sintering and grain coarsening techniques to study the effect of crystal orientation. In addition to texture and orientation effects, an analysis of the results indicates that the permanent magnet performance is impaired by a refinement of the grain size. AN excellent historical review of the development of Alnico permanent magnets has been prepared by Bozorth.1 The desirable permanent magnet characteristics of Fe-Ni-A1 alloys were discovered in 1932 by Mishima.2,3 The work of Ruder' showed that the alloys were age-hardenable, and Betteridge5 defined the best composition and heat treatment for the magnetically isotropic alloy known as "Alnico 3." Horsburgh and Tetley0 increased the energy product by the addition of cobalt and copper, "Alnico 2," and Oliver and Sheddon7 demonstrated that cooling in a magnetic field improved the residual induction of this alloy. Jonas8,9 then disclosed the great practical benefits of heat treating an alloy of higher cobalt content in a magnetic field and the resulting alloy, "Alnico 5," has become the standard of the industry. This paper describes the fundamental aspects of a procedure which can be used to further improve the properties of these anisotropic permanent magnet alloys. A study of the casting techniques used in the production of anisotropic Alnico permanent magnets indicated that the magnetic quality was affected by the as-cast macrostructure. Improved performance was observed in magnets containing a high percentage of columnar grains whose long axes were parallel to the magnetic axis of the casting. McCaig10 studied the effect of such columnar grain structures upon the magnetostriction characteristics of similar alloys, however no data was presented showing the effects on other magnetic properties. The following paragraphs describe two experiments which were conducted to determine the effect of various grain orientations upon the energy product. Special composite molds were prepared of highly conductive and highly refractive components to remove the heat of solidification from the casting in a controlled manner. Representative macrostructures produced by these techniques are shown in Fig. 1, along with the relative volumes of favorably oriented columnar grains. The alloy, Alnico 5, has the highest permanent magnet performance of any commercial magnet material. It has the nominal weight composition of 8 pct Al, 14 pct Ni, 24 pct Co, 3 pct Cu, and 51 pct Fe. A heat of this material was cast into molds producing the type A and B grain structures shown in Fig. 1 and pairs of the resulting magnets were placed in heat-treating boats so as to eliminate any biasing effects of boat position. After a standard heat treatment the type A magnets, with 16 pct of the volume composed of favorably aligned grains, had a maximum energy value of 3,940,000 gauss-oersteds, while the type B magnets with 73 pct aligned grains averaged 5,090,000. This large im-

Jan 1, 1954

Coal Division Industrial Minerals Division Minerals Beneficiation Division Mineral Economics Division Mineral Industry Education Division Mining, Geology and Geophysics Division MINING BRANCH AND DIVISIONS OFFICERS AND COMMITTEES Council Ralph E Kirk, '55, Chairman (Coal). C M Cooley, Secretary, M D Cooper, '56 (Coal), Harold Bannennan. '55 (Ind Min Div ). R C Stephenson, '56 (Ind Min Div ) , E P Pfleider, '55 (MGGD) . J D Forrester. '56 (MGGD) , Donald W Scott, '55 (MBD). S D Michaelson, '56 (MBD). J K Richardson (MED). J R Van Pelt, Jr (MIED) COAL DIVISION Established as a Division September 20, 1929 M D Cooper. Chairman H F Yancey, Chairman-elect David R Mitchell, Secretary-Treasurer Professor of Mining The Pennsylvania State University State College. Pennsylvania

Jan 1, 1954

By Jas. E. Thomson

"The Kirkland Lake-Larder Lake gold area is in northeastern Ontario and is a continuation of the ore-bearing belt that extends across northwestern Quebec through the Rouyn, Cadillac, Malartic, and Bourlamaque areas. It is the oldest mining camp along this famous mineral belt. Gold discoveries were first made at Larder Lake and Swastika in 1906, but it was not until 1913 that important developments at Kirkland Lake created a real interest in the country. Total gold production of the camp passed the million dollar a year mark in 1920 and increased in amount yearly until the advent of the second World War when there was a falling off due to labour shortage. The Kirkland-Larder camp ranks as the second largest gold producing area ' in Ontario. To the end of 1944, twenty-two mines in the area had produced bullion valued at $515,631,428 and ten mines had distributed dividends amounting to $205,981,116. The average grade of the ore milled in this period has been $15.17 a ton for the mines in the Kirkland Lake area and $6.49 a ton for the mines at Larder Lake.ROCK FORMATIONS OF THE AREAIn a general way the rocks of the country may be divided into the lithological groups indicated on the accompanying geological sketch map. This map has been compiled largely from recently issued geological sheets of the Geological Branch of the Ontario Department of Minest. Owing to the present difficulty of separating the formations of the Larder Lake country into the twofold age divisions of Keewatin and Timiskaming, the usual custom in the past, a lithological grouping of formations has been adopted. The age terms 'Keewatin and 'Timiskaming' are loosely used in this article to express the often used but not necessarily accurate distinction between the main groups of older strata."

Jan 1, 1954

By B. Post, F. W. Glaser

Three borides of zirconium have been reported: ZrB,l ZrB2,2,3 and ZrB12, 4 The phase relationships, ranges of stability, and some physical properties of these compounds are described. THE zirconium borides differ considerably from one another, particularly with respect to their relative stabilities at high temperatures in the presence of carbon.4,5 ZrB2 is extremelv stable at all temperatures (to the melting point) in contact with carbon. Both ZrB and ZrB12 tend to decompose at elevated temperatures when carbon is present in excess of about 0.5 pct. ZrB forms ZrB2 and ZrC, and ZrB12 decomposes to form ZrB2 and a boron-carbide phase. In the ZrB12 preparation, boron present in excess of that needed to form ZrB2 reacts with carbon, if present, to form carbides, in preference to forming the higher boride. Similar instability of borides, other than diborides of the transition metals of the 4th and 5th groups of the periodic table, has been reported.5,6 special precautions had, therefore, to be taken to minimize carbon contamination in the preparation of ZrB and ZrB12. Reactions below 1400°C were carried out by heating powdered mixtures of zirconium hydride and boron in quartz tubes in a hydrogen atmosphere. For temperatures above 1400°C, reactions were carried out in graphite molds. Carbon contamination from the molds was minimized by employing extremely rapid heating rates to reduce carbon diffusion into the body of the specimen, and by subsequent "shaving" of sample surfaces that had been in contact with the graphite dies. A heating rate of about 2000°C per min was obtained by heating the dies (by direct conduction), using a current of 40,000 amp. Although this type of heating cycle apparently allowed little time for "homogenization," close approximations to equilibrium conditions were usually obtained as a result of the very strongly exothermic reactions between zirconium hydride and boron at elevated temperatures. Reproducibility of results in repeated runs under varying conditions was taken as a reasonable indication that equilibrium conditions had been effectively achieved. Quenching was accomplished by rapidly immersing the entire die, containing the reaction products, in water. Specimens could also be cooled at controlled rates by adjustment of the rate of flow of water through the water-cooled copper electrodes in contact with the graphite dies.

Jan 1, 1954

By J. O. Jones

[Willis Mountain in southeastern Buckingham County is one of several kyanite deposits its central Virginia. It is composed principally of kyanite resulting from metamorphism of siliceous sedimentary beds rich in alumina. The mountain, which trends north-south, is 2 miles long and is topped by a narrow ridge with sleep rugged sides rising to an altitude of 1,160 feet and projecting 500 fast shove the surrounding countryside. Bureau Mines engineers examiner Willis Mountain early in 1949, when bonded concentrations of coarsely crystalline kyanite were observed in the kyanite-quartzite on the northern end of the mountain and in loose boulders on the eastern slope. Commencing in late July 1949, the investigations continued on the Long Mountain segment for 11 months, ended in June 1950. A total of 600 samples from 32 diamond-drill holes, aggregating 3,876 feet of drilling, and from 255 feet of sampling in 3 trenches was assayed for kyanite and ferric oxide.]

Jan 1, 1954

By Bernard York, John J. Reed

Mine opening stability was investigated by loading model openings to failure. Eight-inch plaster blocks were cast with small uniform section openings passing through the centers. After curing, the models were jacketed and loaded hydrostatically in a closed vessel. Opening size, shape, and orientation were varied to determine how these factors influence opening stability. THE investigation described in this paper is a continuation of a project begun in 1946 by Bernard York and W. E. Bush. .The experimental method used in the investigation involves the hydrostatic loading of a model mine opening to failure. Most investigators agree that this loading closely approaches actual conditions in very deep mines. The conditions are further idealized by using an essentially isotropic model material. The experiments consist of casting 8-in. plaster cubes, or 8-in. diam cylinders 8-in. long, having a relatively small uniform section hole passing through their centers. After thorough drying, the models are jacketed in a flexible plastic bag and loaded hydrostatically with water in a closed vessel. At about 300 to 500 lb per sq in. pressure the central opening fails. The fracture pattern resulting from opening failure is studied in a plane normal to the longitudinal axis of the opening. The model block is sawed through its center after loading to expose this plane and to eliminate the possibility of end effect. By changing

Jan 1, 1954

By A. H. Lang

"The name Barkc:rville district is applied loosely to the gold-bearing area around the historic town of Barkerville; the first mining camp in western Canada. The region is partly in the Cariboo mining division and partly in the Quesnel mining division. It contains two producing lode gold mines; the Cariboo Gold Quartz and the Island Mountain; and numerous other deposits. The regional structural pattern is outlined in this paper; the structural details of the producing mines are described in the papers that follow.The discovery of rich placer deposits in this district in 1860 was followed by the Cariboo gold rush. Placer mining in the area flourished until 1875 and then declined as the shallow diggings were exhausted, but important operations are still active. The total placer production amounts to about $50,000,000. An extraordinary number of quartz veins outcrop in the district, but many have only a small gold content. The miners soon recognized that the placer gold must have been derived from the erosion of these veins, and some directed their attention to the possibility of quartz mining. The erection of a 4stamp mill in 1876 was the first attempt at ore reduction in British Columbia, exclusive of arrastras. Efforts to mine the Cariboo lodes on a large scale were not successful, however, until 1933, when, due to the pertinacity of F. M. Wells and to the increased price of gold, the Cariboo Gold Quartz mine commenced production, followed by the Island Mountain mine in 1934. This success led to development work at many properties in the district, but the only ones that have reached production to date are the Columbia Tungstens, where scheelite has been mined intermittently since 1937, and the Cariboo Hudson, from which gold was produced in 1938 and 1939."

Jan 1, 1954

By H. L. Riley

Cleaning and handling of fine coal are generally conceded to be more difficult problems than preparation of the coarser sizes. Increased mechanization in the coal-mining industry has, in general, resulted in an increased percentage of the fine sizes in the total coal mined. If the coal fines are cleaned by wet methods, the minus-1/16-inch square-mesh particles cause most of the sludge and slurry problems encountered in preparing wet coal. Equipment that separates coal from refuse on the basis of specific gravity is not efficient on sizes that, because of their fineness, do not follow the same laws of hindered settling as the larger particles. Probably the best solution of fine-coal cleaning problems is to use other methods, such as flotation, that utilize other physical characteristics than those determining hindered-settling ratios. Regarding the type of flotation known as the Elmore vacuum-flotation process there has been a scarcity of data and information available in this country. An investigation has therefore been made to obtain additional date and information on this process under laboratory conditions. During this investigation an effort has been made to evaluate the relative efficiencies of vacuum and mechanical laboratory froth flotation cells. The investigation included float-and-sink, screen-sizing, and flotation tests on 2 different samples of 14-mesh to 0 raw coal and an a sample of slurry from the settling-tank overflow of a typical washer. One raw-coal sample was obtained from the American bed and represented a type of coal that is relatively easy to clean. The other raw-coal sample was from the Mary lee bed and represented a type considered difficult to clean.

Jan 1, 1954

By George F. Sowers

THE geophysical methods of exploration employed so extensively in mining and petroleum investigations are now being used in civil engineering. Requirements differ from those of mineral ex- ploration and therefore modified techniques have been developed. The civil engineer is primarily interested in the uppermost soil and rock strata. In highway engineering the materials affecting design and construction may be found within 15 or 20 ft of ground surface, and data on soils and rocks is seldom needed for more than a depth of 100 ft even for the heaviest structures.

Jan 1, 1954

By H. C. Gunnings, C. O. Swanson

"The Sullivan mine; at Kimberley in southeastern British Columbia; is the largest silver-lead-zinc mine in the Empire and one of the largest in the world.The original discovery was made in 1892 by four prospectors. Until 1899, when the branch line of the Canadian Pacific railway from Cranbrook to Kimberley was completed, little work was done on the property. In 1900, systematic development was started, and during the next 3 years 5,000 tons of ore was shipped to the smelters at Nelson and Trail. By 1903, some 300,000 tons of ore was developed, and a smelter was started at Marysville, about 5 miles from the mine. However, this smelter closed down in 1907 because of metallurgical difficulties after treating 75,000 tons, and the property came under the control of the American Smelting and Refining Company. An option on the property was taken in 1909 by the Consolidated Mining and Smelting Company of Canada, who exercised their option in the following year. During the next 5 years by selective mining and sorting 188,000 tons of high-grade ore was produced and shipped to Trail. This tonnage came from the upper levels, about 4,600 to 4,800 feet in elevation. At the same time, deep drilling down to the 3,900-foot level showed the presence of an immense body of complex ore. In 1915, the main adit-the 3,900-foot level-was started, and by 1919 this had been driven a distance of 2 miles to develop the ore above this level. Meanwhile, progress was being made in overcoming the milling problems. An interesting account of this work was written by the staff ( 4). In 1923, the first unit of the present concentrator was erected, with a capacity of 2,500 tons a day, and thereafter the rate of production increased rapidly. In 1934 it was around 8,000 tons a day, and to date a total of about 30,000,000 tons of ore has been sent to the mill. In recent years, a considerable part of the production has come from levels between the 3,900-and 3,350-foot, which were opened by an internal incline shaft started in, 1930. In 1942, tin was added to the products separated at the concentrator."

Jan 1, 1954

By A. M. Gaudin, W. D. Charles

IN flotation lime is used to depress pyrite. For this purpose it is preferred to caustic soda. The low cost of lime and the widespread availability largely account for this preference. However, there is some evidence' that pyrite is more readily depressed by calcium than by sodium ions at the same pH. To measure the difference in adsorption of calcium and sodium, which is thought to lie at the basis of the differences in depressing action, radionuclides of calcium and sodium have been used. The experimental work has included an evaluation of the effect of dissolved oxygen, of the concentration of calcium or sodium, of the concentration of hydrogen ion, and of the anions present. Preliminary work in the investigation entailed preparation of the pyrite, development of a technique for counting pyrite coated with Ca and Na, the radionuclides used, and development of an apparatus to study the adsorption of calcium and sodium on pyrite. The main experimental work included calcium adsorption and sodium adsorption studies detailed below. The following are the most salient observations made during these experiments. Oxygen in solution increases the adsorptive power of pyrite for calcium

Jan 1, 1954

By N. A. Gokcen

EQUILIBRIA in the reactions between gases and liquid metals have been the subject of many interesting investigations. The experimental realization of true equilibrium, however, is questionable in certain cases due to the lack of conclusive studies in reaction rates. It -will be shown here that a systematic interpretation of rate studies with the analysis of prevailing experimental conditions leads to valuable practical information. The reactions of particular interest are: H2(g) +S(inFe) - H2S(g) [1] H2(g) +O (inFe) =H2O(g) [21 2H2(g) + SiO2(s) = 2H2O(g) + - (inFe) [3] The usual and perhaps the most convenient method of investigation may be illustrated with reaction 1. A stream of gas mixture consisting of H2 + H2S is passed over or bubbled through the liquid metal at constant temperature. The ratio of H2S/H2 in the entrant mixture is fixed in each experimental run, and, therefore, the composition of melt varies until the establishment of equilibrium. The purpose of this paper is to derive a formula expressing the minimum time required for the establishment of equilibrium and to compare the calculated values from such a formula with the available data. Equations Reaction 1 is used for the purpose of illustrating the derivation. Let E represent the equilibrium and X the nonequilibrium sulphur in weight percent at any time t in minutes. For the sake of simplicity, it is first assumed that E > X although the results are of general applicability without restriction. It has been shown by Morris and Williams' that within a difference of 1 pct S or less, i.e., E-X5 1.00, the value of K'1 = Ph2s/Ph2.S% is very nearly constant. The maximum ratio of available Ph2s/Ph2 = H,S/H,, from which sulphur can be absorbed by metal, is equal to H2S/H2 in equilibrium with E (which equals H2S/H2 in the entrant gas), minus H,S/H, in equilibrium with X. Thus: Available H2S/H2 = EK'1 - XK'1 [4] Eq. 4 expresses that sulphur can be absorbed by metal from the H2S/H2 in the entrant gas until the gas leaving the metal assumes a value of H2S/H2 which is in equilibrium with the dissolved sulphur X at that time. H,S constitutes up to approximately 1 pct of the gas mixture. Its disassociation into H2 and SL is about 1 pct at 1600°C, hence, the H2S/H2 impinging on the surface of metal is very close to that in the entrant gas. The rate of flow of hydrogen entering the reaction chamber is kept constant experi-

Jan 1, 1954

By S. A. J. Hopper

"The Golden Manitou mine is in the northeast quarter of Bourlamaque township, Abitibi county, Quebec. During the summer of 1937 a body of gold-silver-zinc ore was outlined in a series of diamond drill holes located to the west of an old copper-zinc showing in the property of Quebec Manitou Mines, Limited. In 1938, a shaft was sunk and the orebody further explored from levels at depths of 210 and 360 feet.In 1941 the western half of the Quebec Manitou property was acquired by a new company, Golden Manitou Mines, Limited, and the installation of a mining and milling plant was at once undertaken. Milling started in August 1942. The following is a summary of production to December 31, 1946:The orebodies are sulphide replacements in a sericite schist shear zone. They vary in width from 8 feet to 65 feet and range in length up to 850 feet . Much of the ore is of the 'massive sulphides' type . The sulphide minerals in the ore are pyrite and sphalerite with minor quantities of .galena, tennantite, chalcopyrite, and arsenopyrite. Native silver (as wire and leaf silver) has been found in vugs and as coatings along fractures. In one section of the mine a few specks of gold were observed. Spectrographic analysis of ore samples has indicated the presence of zinc silicate."

Jan 1, 1954

D. C. JACKLING, the father of the porphyry coppers, has been honored for his pioneering in that field. There is another facet to Mr. Jackling's activities, one which now may prove an even greater monument than the big coppers-the story of his venture in taconite beneficiation. The essence of his porphyry development was mass handling of material. Not alone mining on a large scale, which was done on the Mesabi Range at the turn of the century, but the integration on a previously unknown scope of mining, milling, concentration, and in many cases, of final reduction to metal at the site. This was mass production applied to mining, treatment of a very low grade source material, previously considered submarginal.

Jan 1, 1954

By E. S. Machlin

An extension of the thermodynamic theory has been made for the case of irreversible growth processes occurring by the motion of an interface. The theory is applicable to such diverse phenomena as diffusion, growth in recrystallization, continuous grain growth, growth of carbides, etc., growth of eutectoid products, growth in solidification, recovery, "slipless" flow, etc. THE publication of a recent book1 has served to focus attention on a very powerful means of treating certain irreversible processes. This method which has been formally described as the thermodynamic theory of irreversible processes is applicable to processes which involve an approach to equilibrium and for which the deviations from equilibrium are small. The irreversible processes can be classified into three groups: chemical reactions, transport processes (diffusion, heat and electrical flows), and relaxation phenomena involving a degradation of internal energy to more stable states. The limits of applicability of the theory can be precisely defined1,2 for each type of irreversible process. For example, in a chemical reaction at constant temperature and pressure, the Gibbs free energy released per mol in the process should be less than the thermal energy, RT. Another type of irreversible process, which sometimes involves a combination of the first two of the above-mentioned groups, is treated in this paper. This process is one characterized by the motion of an interface separating two regions having different values of free energy and may be briefly described as a growth process. Prigogine2 and Herring3 have treated special cases of this type of process. Previous conscious applications of the theory in metallurgy have been limited to the field of diffusion, one of the transport processes. Darken,4 Bardeen,5 Prigogine2 and others have made significant contributions in this respect. Some other applications of the theory are described in this paper. The Theory The thermodynamic theory of irreversible processes is based on the work of Onsager,6 DeDonder,7 Prigogine2 and others. A resume of the theory has been given by Prigogine2 and DeGroot.1 A brief description of the theory follows, although for a complete understanding the reader is urged to read the references. It is first assumed that the change in entropy, even for a system removed from equilibrium, is given by dS = [dU + pdV - Si µi, dn, - Sk Pk dxk]T-1 Using this expression, the irreversible entropy production in the system is calculated by subtracting the contribution to the change in entropy of the system by transfer of heat, work, or matter from the surroundings. Thus, for example, the irreversible entropy production of a system at constant temperature and pressure is given by dtS = — — dG (DeDonder7) Now it has been shown by Prigogine,2 DeDonder,7 and DeGroot1 that the rate of irreversible entropy production diS/dt, when calculated in the manner suggested, can be written as a sum of products of conjugate forces XK and fluxes Jk, i.e., d,s/ = Sk Jk Xk [I-1] dt The assumption is next made that a linear relation exists between a given flux and the forces, obtained from Eq. I-1, i.e., Ji = Sk Lik Xk (i = 1, 2, . . . n) [I-2] Generally, there is a degree of freedom in choice of the fluxes and forces. However, for all the choices consistent with Eq. I-1 the Onsager8 relations, based on the principle of microscopic reversibility, namely, Lik = Lki, are valid. The coefficients Lik, depending upon the choice of the conjugate fluxes and forces, may be more or less dependent upon the parameters defining the state of the system. In general, the proper choice of fluxes and forces utilizing Eq. I-1, makes the coefficients Lik independent of time. Also, because many of the three classes of irreversible phenomena have already been treated,1,2 a proper choice can be made by analogy. In any case, the validity of Eq. 1-2, from whatever choice made using Eq. I-1, must be tested by experimentation. The theory, thus, comprises the following steps: 1—The irreversible entropy production is calculated to yield Eq. I-1. 2—The terms in Eq. I-1 are grouped

Jan 1, 1954

Jan 1, 1954

By G. R. Strimbeck

This is a report on experimental work on development of a gasification process operating at near atmospheric pressures and using finely pulverized coal entrained in oxygen and steam. The gasifier was designed by The Babcock and Wilcox Co. in cooperation with engineers of the Bureau of Mines Morgantown station. The test work discussed in this report covers the first 34 tests made in the pilot plant in which a strongly coking Sewickley-bed coal, ground to either 70 or 90 percent through a 200-mesh screen, was used.

Jan 1, 1954

By H. D. Kessler, M. Hansen, R. J. Van Thyne

The phase diagram of the titanium-rich portion of the system Ti-Cr-Fe to 70 pct Ti was established by means of isothermal sections at 900°, 800°, 750°, 700°, 650°, 600°, and 550°C, using arc-cast alloys. An isotherm at 800°C was determined for the section bounded by Ti, TiFe2, and TiCr2. Micrographic analysis was employed as the principal method of investigation, supplemented by X-ray diffraction and incipient melting studies. A ternary eutectoid, ß ? a+ TiCr2 + TiFe, occurs at approximately 8 wt pct Cr, 13 wt pct Fe, and about 540°C. AMONG the first titanium-base alloys in commercial production were the Ti-Cr-Fe alloys. For this reason, the Materials Laboratory, Wright Air Development Center, sponsored an investigation of the system. No information on the constitution of the titanium-rich corner was available. Vogel and Wenderott studied titanium-poor ternary alloys.' As part of this program, the binary systems Ti-Cr and Ti-Fe have been determined previously by the authors.' Other investigators have also studied the binary systems Ti-Cr,3-7' Ti-Fe.³,8-10 Both of the binary systems are characterized by the eutectoid decomposition of the ß phase. Most of the effort of the present work has been concentrated on the titanium-rich corner with compositions of less than 30 pct total chromium and iron content. The determination of isothermal sections was the experimental approach used to obtain the ternary phase diagram. Vertical sections were used to check the consistency of the isothermal sections. While this investigation was in progress, a study of the Ti-Mo-Cr system at Armour Research Foundation disclosed the existence of a high temperature modification of TiCr2 above 1300 °C.11 This allotrope has a hexagonal structure of the MgZn2 type, iso-morphous with TiFe2, whereas the low temperature modification of TiCr2 is cubic," of the MgCu2 type. The existence of allotropy in TiCr2 of course means a more complicated set of phase relationships in this general region than if the phase were monomorphic, as was first assumed. Additional studies were made late in the investigation in order to clarify the part that the hexagonal TiCr2 phase plays in the ternary phase relationships. These will be discussed in a separate section. Because they are of greatest practical significance, the phase relationships in the titanium-rich corner will be presented first, omitting the equilibria involving the hexagonal modification of TiCr2 in an effort to simplify the presentation somewhat. Experimental Procedure Materials: The titanium used in the preparation of the alloys was iodide crystal bar (99.9 pct pure) produced by the New Jersey Zinc Co. High purity chromium and iron were obtained from the National Research Corp. Table I gives the analyses of these materials. Melting Practice: Over 100 alloy ingots weighing 10 to 20 g were melted in a nonconsumable electrode arc-melting furnace. As the techniques are identical to those reported previously,12,13 they will not be detailed here. The ingots were melted in the cavity of a copper melting block insert under a slight positive pressure of helium. No measurable hardness

Jan 1, 1954