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By John Hays Hammond

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

Jan 1, 1902

By G. Willard Quick, John R. Freeman

Jan 1, 1930

By Paul T. Allsman, E. W. Newman

Trenching, sampling, and core drilling in Stillwater and Sweetgrass Counties, Mont., by the Bureau of Mines have delimited over 5,000,000 tons of chromite ore containing more than 20 per cent chromic oxide. The Benbow and Mouat-Sampson mines have been developed and are fully equipped for mining and milling 500 tons and 2000 tons a day, respectively. Introduction The Montana chromite deposits were the first to be explored under the Strategic Minerals Act of 1939. In June of that year, the Bureau of Mines started exploration by trenching, test pitting, sampling and diamond drilling, and completed the project in March 1943. The U. S. Geological Survey cooperated by mapping the geology and logging the cores. The project was to determine the extent and grade of the chromite ore and to indicate sufficient reserves to justify development and exploitation of the deposits for the national emergency. Exploration has indicated that the district contains the largest and most important reserve of chromite ore in the United States. The Benbow and Mouat-Sampson mines have been developed and a 500-ton concentrating mill has been constructed on the Benhow property and a 2000-ton mill on the Mouat-Sampson property. Concentrates were produced from the Benbow mill three months after the attack on Pearl Harbor, when the nation's major chromite supplies from foreign sources were cut off. History It has been known for 50 to 60 years that some chromite deposits existed in an east-west belt along the north escarpment of the Beartooth Mountains about 25 miles north of Yellowstone Park, but nothing was known of their size and extent until the war demand of 1917 and 1918 stimulated the search. In those years two properties in the Stillwater region were actively developed, but no shipments were made. The Benbow property was located in 1918 by a local group. The property comprised seven claims along the strike at the east end of the belt. An adit was driven several hundred feet on the Eclipse claim. The seven claims were sold to the Chromium Products Corporation of Livingston, Mont., and were subsequently patented. In 1929, an eastern group obtained an option, installed some equipment, and erected several log cabins. The "crash" in the market in 1929 caused the operators to drop their lease, and the property remained inactive until 1939, when the Bureau of Mines began its exploration. Fourteen claims were located on the Boulder River in 1918 and subsequently patented by the U. S. Chrome Corporation.

Jan 1, 1949

By Paul T. Allsman, E. W. Newman

Trenching, sampling, and core drilling in Stillwater and Sweetgrass Counties, Mont., by the Bureau of Mines have delimited over 5,000,000 tons of chromite ore containing more than 20 per cent chromic oxide. The Benbow and Mouat-Sampson mines have been developed and are fully equipped for mining and milling 500 tons and 2000 tons a day, respectively. Introduction The Montana chromite deposits were the first to be explored under the Strategic Minerals Act of 1939. In June of that year, the Bureau of Mines started exploration by trenching, test pitting, sampling and diamond drilling, and completed the project in March 1943. The U. S. Geological Survey cooperated by mapping the geology and logging the cores. The project was to determine the extent and grade of the chromite ore and to indicate sufficient reserves to justify development and exploitation of the deposits for the national emergency. Exploration has indicated that the district contains the largest and most important reserve of chromite ore in the United States. The Benbow and Mouat-Sampson mines have been developed and a 500-ton concentrating mill has been constructed on the Benhow property and a 2000-ton mill on the Mouat-Sampson property. Concentrates were produced from the Benbow mill three months after the attack on Pearl Harbor, when the nation's major chromite supplies from foreign sources were cut off. History It has been known for 50 to 60 years that some chromite deposits existed in an east-west belt along the north escarpment of the Beartooth Mountains about 25 miles north of Yellowstone Park, but nothing was known of their size and extent until the war demand of 1917 and 1918 stimulated the search. In those years two properties in the Stillwater region were actively developed, but no shipments were made. The Benbow property was located in 1918 by a local group. The property comprised seven claims along the strike at the east end of the belt. An adit was driven several hundred feet on the Eclipse claim. The seven claims were sold to the Chromium Products Corporation of Livingston, Mont., and were subsequently patented. In 1929, an eastern group obtained an option, installed some equipment, and erected several log cabins. The "crash" in the market in 1929 caused the operators to drop their lease, and the property remained inactive until 1939, when the Bureau of Mines began its exploration. Fourteen claims were located on the Boulder River in 1918 and subsequently patented by the U. S. Chrome Corporation.

Jan 1, 1949

By Frank Milliken

IN September 1937, the Ohio Copper Co. inaugurated the treatment of its copper-bearing mill tailings at Lark, Utah. These tailings had been accumulated during the regular operation of the Ohio Copper mine and mill over the period 1007 to 1019. Gravity concentration had been employed except for a comparatively short period in 1919, when flotation was used. The ore milled during that period assayed about I per cent Cu. The chief copper mineral, chalcocite, was dissemi-nated in a shattered quartzite, mainly along fracture or cleavage planes. The quartzite gangue was extremely hard and grinding to liberation resulted in excessive sliming of the "sooty" chalcocite, with consequent high tailings losses. Recovery on the seven million tons treated was prob-ably less than 6o per cent of the total copper content. As early as 1918, attempts had been made to sample the dump. In 1928, a com-plete sampling program was undertaken. The sampling consisted of seventy-four 5-in. post auger holes drilled to the full depth of the dump at regular intervals of 250 ft. Each 10-ft. portion thereof com-prised a sample for analysis. Each sample was screened, rolled, divided into three parts, dried and assayed. The reject was retained for testing purposes. From the depth of the auger holes a contour map of the dump was plotted, Fig. 1, which gives percentages of tonnage and copper content.

Jan 1, 1940

By J. Kucera, J. Vreštál

DIFFERENT authors1 ' have been engaged in meas-uring the vapor pressure of pure cobalt. The results of their measurements satisfy the expected temperature dependence of vapor pressure and are in mutual agreement, with the exception of the results by De Dyk Man and ~esmejanov.~ The latter authors, by using the effusion method, have achieved considerably higher values than other workers. By using the isotope exchange method they obtained much lower values than other authors. The determination of thermodynamic functions of the binary Ni-Co system was carried out, as far as we know, only by De Dyk Man and Nesmejanov.4 This determination was based on extremely low values of vapor pressure over pure cobalt obtained by the isotope exchange method. Therefore we considered it useful to repeat these measurements. Furthermore, the reliable values of thermodynamic functions should complement the migration characteristics, the inner magnetic field data obtained by Miissbauer effect measurements, specific heat data, and the K effect and positron annihilation characteristics that have been achieved for the Ni-Co system in the Institute of Metallurgy of the Czechoslovak Academy of Sciences in Brno.5-9 The measurements in this paper were performed by the isotope exchange method. In this method, as has been shown by analysis,10-'3 the vaporization rate, w, can be calculated from the relation w = k/1oSw [1] i0Sw) [1] where L, is the activity per unit mass of the source, S is the area of evaporation, k is the tangent at the point t = 0 to the curve giving the radioactivity de-pendence of the target vs annealing time, t, and wis the probability for the tracer atom condensation on the target surface. The value for cc. can be obtained from the equation w = a + 2P(l-a) [2] where P is Clausing's coefficient and a is the condensation coefficient. In the present work the cylinder shaped containers for annealing the samples were used, characterized by the ratio 1:d = 1.06. Here 1 is the length and d the diameter of the container. For this ratio P = 0.514 and w =0.5, and w is independent of the condensation coefficient. The vaporization rate is related to the vapor pressure p by the relation where R is the gas constant, T is the absolute temperature, and M is the molecular weight of the component investigated. Measurements of the vapor pressure of the i component over the pure metal, p!, and the alloy, pi, at the given temperature and composition enable one to calculate the thermodynamic activity of this component from the equation ai=pi/pi [4] is and the activity coefficient ri=ai/xi [5] xi where xi is the molar fraction of the investigated alloy component. EXPERIMENTAL Evaporization rate measurements were carried out with pure cobalt and eight different Ni-Co alloys, which were kindly delivered by the Centre National de Recherches Me'tallurgiques Liege, Belgium. The composition of the alloys is given in Table I. The cobalt used in these alloys contained the following impurities: 0.016 wt pct Fe, 0.014 wt pct Cu, 0.01 wt pct Mn. Other elements were present in much lower concentrations. From the melts, samples in the form of small cylinders of 12 mm in diam were ma-chined. The thickness of the targets and sources was 2.5 and 1.2 mm, respectively. The lower thickness of the sources was chosen to make their over-all ac-tivity as low as possible. Sources were activated in

Jan 1, 1970

By R. C. Dalzell, A. E. Wells

In 1866, Thomas Graham1 called attention to the volume of gases, three times the volume of the sample, evolved from a meteoric iron heated in an evacuated porcelain tube. From that time to this the occurrence and significance of gases in metals have been the subject of investigation by many workers, among whom Sieverts,2 Iwasé3 and 0. W. Ellis4 stand preeminent. Sieverts and Iwasé concerned themselves with the solubility of a number of gases in metals in the liquid and solid states. They determined the absorption coefficients of these gases, and in all cases found a sharp change in solubility at the melting point of the metals. Ellis analyzed the gases evolved by solidifying copper and those occluded by the solidified metal. Lobley and Jepson5 endeavored to determine the effects of hydrogen, carbon monoxide and nitrogen on the porosity of copper that was allowed to solidify in the presence of each gas after 30 min. exposure to it in the

Jan 1, 1930

By J. R. Hunter

Current trends in mining practices within the United Kingdom, with particular reference to longwall retreating systems in thick and steeply pitched coal seams at depth, are explained. Various successful mining layouts are considered with their associated machinery and operation, together with the future trends in mining practices to obtain higher outputs. Environmental difficulties are tabled and discussed, including strata control, methane emmision, and dust prevention, together with some modified systems and techniques to overcome them. The problems associated with developing and maintaining a continuance of longwall panels are outlined. The constraints on technical designs and output achievement imposed by noncommercial factors are also considered.

Jan 1, 1978

Jan 8, 1950

By W. D. B. Motter

DURING the early development of blasting with liquid oxygen explosives the trend of experimentation was towards increasing the effectiveness of the explosive. Its characteristic of becoming inert after evaporation of the oxygen content made a strong appeal from the standpoint of safety, especially with missed holes. It later became apparent, however, with practical use of this explosive, that LOX lacked certain other safety characteristics. As its effectiveness was increased, it became more subject to detonation by impact. The object of this paper is to show the steps taken by one operating company to achieve greater safety in the large-scale handling of liquid oxygen explosives.

Jan 1, 1933

By B. G. Klugh

(New York Meeting, February, 1912). IN a paper before the Institute at Wilkes-Barre, Pa., June 1911,1 Mr. James Gayley discussed the application of this process to iron-bearing materials. The same author2 described the results of operations at the plant at Birdsboro, Pa. The purpose of the present paper is to present further discussion of some technical details involved in the operation of this plant, and of the theoretical and practical relations of this product to blast-furnace practice. Since Oct. 1, 1911, the Birdsboro plant has been in operation at the blast-furnace of the E. & G. Brooke Iron Co. The results have been highly satisfactory, although the material treated, being chiefly the flue-dust currently made by the furnace or taken from the accumulated stock-pile, was excessively high, and yet not uniform, in carbon, so that the desirable control or regularity of the amount of fuel in the mixture treated could not be maintained. Nothing could more forcibly demonstrate the flexibility of the process than the fact that, under these conditions, the sinter produced was, in all cases, of excellent quality. The Dwight & Lloyd process, as such, and its present highly-developed mechanical appliances were described by Mr. Gayley in the paper above mentioned. While the repetition of some particulars will be unavoidable in this paper, it will be confined to features bearing upon the metallurgical principles involved. According to the principle of the process, the finely-divided iron-bearing material to be sintered is intimately mixed with

May 1, 1912

By Betty M. Miller

INTRODUCTION In September 1974 the Resource Appraisal Group of the Branch of Oil and Gas Resources, U. S. Geological Survey, was asked to aid the Federal Energy Administration (FEA) in its legal responsibility to generate by June 1975 an independent appraisal of the undiscovered oil and gas resources of the United States, both onshore and offshore. As a result, the Resource Appraisal Group accelerated its ongoing efforts to develop sound appraisal methods and procedures that would permit the systematic collection and evaluation of basic data from petroleum provinces throughout the Nation. The results of this independent appraisal of the Nation's conventional oil and natural gas resources were published by the U. S. Geological Survey as Circular 725, June 1975 (1). The estimates in this report of undiscovered recoverable oil and gas resources for the United States were made: (1) by carefully re- viewing a large amount of geological and geophysical information gathered on more than 100 different provinces by over 70 geologists within the Survey; (2) by applying a variety of resource appraisal techniques to each potential petroleum province; and (3) by application of subjective probability procedures to group appraisals for each petroleum province. These methods provide a range of estimates which are summarized in terms of low, high and mean values for the various provinces and groups of provinces, or regions. The basic data and procedures used are documented and are being incorporated into a dynamic, data- intensive system that can be upgraded, updated and reevaluated periodically. These data are open to public inspection. In this study, the primary emphasis was placed on conventional crude oil and natural gas in the onshore provinces and the provinces on the continental shelf out to water depths of 200 metres; estimates

Jan 1, 1977

By William H. Morris

At the Glen Summit meeting, the question of controlling the silicon in pig-iron WAS raised; and as this has been deemed by most furnace-men for years past a matter of special difficulty, an account of our experience in the matter may be of interest. When running on mill-iron, some years ago, we aimed to keep

Jan 1, 1893

By G. Derge, R. E. Grace

Diffusivity of bismuth in liquid Pb-Bi alloys has been measured by the capillary reservoir method as a function of temperature and composition. Fair agreement between theory and experiment is found for the measured diffusion coefficients and activation energies of diffusivity and viscosity in dilute lead alloys. The measured diffusion coefficients in the high bismuth alloys describe mass transport in special concentration gradients. THE study of diffusion in liquid metals has been restricted largely to the amalgams over small ranges of temperature and composition. In contrast to this, diffusion and transport of ions and molecules in aqueous and organic solvents have been studied extensively for the past 50 years. The general difficulty of measuring diffusion coefficients in both gases and liquids at high temperatures has been that of eliminating convection currents. Measuring techniques based on freezing and sectioning after the diffusion period1 are not particularly satisfactory because of the volume changes and segregation which occur during freezing. The most promising technique which is currently being developed for liquid metals is the capillary reservoir method. This eliminates convection currents from the diffusion zone and requires measurements only of the length and initial and final compositions of the alloy within the capillary. Anderson and Saddington' have measured the diffusion coefficient of tungstate anions in aqueous Na,W04; Wane4' and Hoffman- ave studied structure and self-diffusion in water and self-diffusion in mercury, respectively, by similar techniques. Selection of the Pb-Bi system for initial study was made for several reasons: I—It afforded a low temperature system for development of techniques which would be suitable for high temperature measurements in liquid iron. This research on diffusion in liquid iron is now in progress as a part of a general program on the rates and mechanisms of slag-metal reactions. 2—Activity data on liquid Pb-Bi alloys of all compositions are available from the emf meas- urements of Strickler and Seltz.9 3—Some data are available on the diffusion of bismuth into solid lead. The measurements on solid alloys were made by von Hevesy and Seith7 for the concentration range of 0 to 2 pct Bi. An appropriate solution to Fick's law (unsteady state) for the capillary reservoir has been found by considering the mass flow which passes through a unit area of surface on a slab of infinite thickness as a function of time. This is the first application of this solution to diffusion measurements, although a similar solution is available for identical boundary conditions.' By analogy with heat conduction, the problem reduces to a perfectly insulated infinite slab at temperature C,, one surface of which is quenched to C, for all times, t. Heat is permitted to flow from quenched surface of the slab to an infinite supply of coolant at C.' (see Appendix). For the corresponding solution for diffusion in liquids, these terms become Where Cu is the initial concentration of component A" in entire capillary at t - 0, C, is the final con- In this case. component A is bismuth, and C, = 0. centration of component A in entire capillary at t = t, C, is the concentration of component A in bath for all t, 1 is the length of the capillary in centimeters, t is the time of diffusion period in seconds, and D is the diffusion coefficient in square centimeters per second. By comparison with solutions to Fick's law used in the solid state, this solution for liquids is similar to the Grube solution for solids, where the change in D with chemical composition is not taken into consideration. Difficulty is to be expected if large concentration gradients are employed and if the concentration gradients extend over an appreciable length of the capillary.

Jan 1, 1956

Jan 1, 1920

By Albert Ladd Colby

PAGE I. Introduction,...........577 11. PRocess of Manufacture. 1. American Specifications. 2. Foreign Specifications, . ......... 580 III. Chemical Properties. I. Chemical Composition: (a) American Specifications ; (b) Foreign Specifications. 2. Chemical Analysis: (a) American Specifications ; (b) Foreign Specifications ; (c) Number of Analyses Required ; (d) Sample for Analysis ; (e) Check-Analyses Impracticable ; (f) Rejection Solely on Variation in Com-' position,............581 IV. Physical Properties. 1. Drop-Test and Drop-Testing Hachine: (a) American Specifications ; (b) Foreign Specifications ; (c) Limits in Deflection. 2. Tensile Test: (a) American Specifications; (b) Foreign Specifications ; (c) Test-Pieces are not Representative ; (d) Specified Tensile Strength is Affected by the Section ; (e) BpeciBed Tensile Strength is Often Inconsistent with Specified Chemistry ; (f) Specified Tensile Strength is Often Inconsistent with Specified Elongation ; (g) Amount of Tensile Testing Required is Excessive ; (11) Conclusions. 3. Dead-Weight Test: (a) American Specifications; (b) Foreign Specifications; (c) Number of Tests Specified. 4. Bending-Test: ((1) American Specifications ; (b) Foreign Specifications,..........589 V. Section. 1. American Specifications. 2. Foreign Specifications: (a) Templets ; (b) Sample Piece of Rail; (c) Allowable Variation from Templet,...........601 VI. Weight. 1. American Specifications. 2. Foreign Specifications,. . 603 VII. Length. 1. American Specifications. 2. Foreign Specifications, . . 604 VIII. Drilling. 1. American Specifications. 2. Foreign Specifications, . 604 IX. Finish. 1. American Specifications. 2. Foreign Specifications, . . 50.5 X. Branding. 1. American Specifications. 2. Foreign Specifications : (a) Data to be Rolled in Raised Letters on Web of Rail ; (b) Marking of the Blow-Number on Each Rail; (c) Additional Marking and Painting of Rails,........605 XI. Inspection. 1. American Specifications. 2. Foreign Specifications: (a) Prior Notice of Rolling; (b) Free Access to the Works ; (c) Cost of Inspection, Analyses and Tests to be Borne by the Manufacturer ; (d) Rails after Inspection by Manufacturer to be Sorted into Lots Prior to Inspection by the Engineer ; (e) Disposition of Rejected

Jan 1, 1907

By J. C. Febles

HISTORY. THE use of iron for the precipitation of copper was known at least as early as the fifteenth century. Both Paracelsus and Basil Valentine refer to it in their writings, as early as 1500 A. D. It was used in Peru, for this purpose prior to 1637, and at Rio Tinto, Spain, as early as the sixteenth century. The statement has been made repeatedly that in the early history of the mining industry at Butte, the practicability of this method of recovering copper from solution was overlooked, and that enormous quantities of copper-bearing water were allowed to go to waste, the copper in which might easily have been recovered at small cost; and that this oversight on the part of the mine operators was due to ignorance of this method of recovering copper. As a matter of fact, very little copper-bearing mineral was encountered in the mines of Butte until a depth of 400 or 500 ft. bad been reached, and in many cases much greater depths were necessary to reach the copper-bearing zone. The water encountered in the upper levels (although in most cases quite highly mineralized) contained little or no copper, and it was only after considerable areas of copper-bearing ore had been uncovered and developed that copper sulphate began to. appear in the mine water in any considerable quantity. In fact, the first water that was observed to contain copper carried it in such small amounts as to be of little or no importance. It was only after years of underground work had opened extensive areas of stopes, drifts, and other underground workings, these being subsequently filled with waste, nearly all of which contained small copper values, which became oxidized by exposure to the air and were acted upon by the slowly percolating mineral water, that the recovery of copper from mine water became commercially important.

Jan 7, 1913

By M. W. Ditto

THe conversion of the beehive coke plants, in this country, to byproduct plants has been slow, because the coal supplies were near the centers of the steel industry. With the growth of this industry, especially with its development around Chicago, it became necessary to transport large tonnages of coal from the eastern districts and then convert it into coke. The losses due to transportation costs were partly offset by the value of the byproducts recovered. To save the transportation costs, it was desirable that the coal deposits of Indiana and Illinois be utilized. This coal had always been classified as non-coking; it was also considered unsuitable for the metallurgical field because of the high ash and sulfur contents. The conditions, however, were promising enough to start experimental and development work, which crystallized in the design of the Roberts coke oven. The fundamental features of most coke ovens, with respect to the application of heating gas and the recovery of byproducts, are the same and, in the last few years, the tendency has been toward the better application of heating to the walls, higher thermal efficiency, and, by the control of heating conditions, the increase of byproduct yields. Structural features also have been improved and the use of high-grade refractory material has allowed the use of higher temperatures with the resulting higher rated capacity per oven per day. Great improvements have been made in both recuperators and regenerators, particularly with reference to the individualizing of each oven with respect to its adjacent oven, so that each can be operated as a unit if desired. The highest development of the flue type of oven has been applying individual regenerators for the recovery of waste heat. After some research work, it was found that the high-volatile Illinois coals could be utilized for coke by obtaining the better application and control of the heating conditions in the oven. Most of this high-volatile coal that had been used gave a good coke structure under certain conditions. The fact that coke was occasionally made from this coal, demonstrated the possibiity of making coke from it at all times pro-

Jan 1, 1923

By M. W. Ditto

THe conversion of the beehive coke plants, in this country, to byproduct plants has been slow, because the coal supplies were near the centers of the steel industry. With the growth of this industry, especially with its development around Chicago, it became necessary to transport large tonnages of coal from the eastern districts and then convert it into coke. The losses due to transportation costs were partly offset by the value of the byproducts recovered. To save the transportation costs, it was desirable that the coal deposits of Indiana and Illinois be utilized. This coal had always been classified as non-coking; it was also considered unsuitable for the metallurgical field because of the high ash and sulfur contents. The conditions, however, were promising enough to start experimental and development work, which crystallized in the design of the Roberts coke oven. The fundamental features of most coke ovens, with respect to the application of heating gas and the recovery of byproducts, are the same and, in the last few years, the tendency has been toward the better application of heating to the walls, higher thermal efficiency, and, by the control of heating conditions, the increase of byproduct yields. Structural features also have been improved and the use of high-grade refractory material has allowed the use of higher temperatures with the resulting higher rated capacity per oven per day. Great improvements have been made in both recuperators and regenerators, particularly with reference to the individualizing of each oven with respect to its adjacent oven, so that each can be operated as a unit if desired. The highest development of the flue type of oven has been applying individual regenerators for the recovery of waste heat. After some research work, it was found that the high-volatile Illinois coals could be utilized for coke by obtaining the better application and control of the heating conditions in the oven. Most of this high-volatile coal that had been used gave a good coke structure under certain conditions. The fact that coke was occasionally made from this coal, demonstrated the possibiity of making coke from it at all times pro-

Jan 1, 1923

By J. P. Nielsen, H. Margolin, E. Ence

The Ti-Ni phase diagram has been investigated up to 68 pct Ni with iodide titanium base alloys by metallographic, X-ray, and melting point methods, and from 68 to 90 pct Ni by examination of as-cast structures of sponge titanium base alloys. NVESTIGATION of the nickel-rich portion of the I Ti-Ni phase diagram was first reported by Vogel and Wallbaum in 1938.' This work was subsequently extended to lower nickel contents by Wallbaum' who indicated the possibility of a eutectic reaction for nickel contents below 38 pct. Long et al.3 studied the titanium-rich portion of the phase diagram and found eutectic and eutectoid reactions below 38 pct Ni. However, the temperature of the eutectic indicated by Long et al. was considerably lower than that suggested by Wallbaum. Long and his coworkers synthesized their alloys by powder metallurgical techniques and encountered oxygen and/or nitrogen contamination. Thus the diagram which was obtained did not represent binary alloying conditions. However from these results the features of the binary diagram were predicted. At Battelle Memorial Institute4 the Ti-Ni diagram was investigated up to approximately 11.5 pct Ni with sponge titanium alloys. The range of temperatures used was not sufficient to define the eutectoid temperature or composition. The data of Wallbaum2 and Long et al.8 were of particular interest for the present study, and although the work was originally concerned with the region below 40 pct Ni, the investigation was extended to higher nickel contents in an attempt to resolve the differences between these workers. Experimental Procedure Preliminary work on the Ti-Ni system was carried out with duPont Process A sponge titanium alloys to reduce the amount of subsequent work to be done with iodide titanium base alloys. The sponge titanium used contained 99.71 to 99.77 pct Ti, 0.1 pct Fe and 0.005 to 0.009 pct Ni. The iodide titanium obtained from the New Jersey Zinc Co. contained 99.9 to 99.95 pct Ti. Nickel used with sponge titanium was 98.9 pct pure. The high-purity nickel alloyed with iodide titanium was cobalt-free with approximately 0.05 pct C and was obtained through the courtesy of the International Nickel Co. The 15 g sponge titanium charges for melting were prepared by compacting in a die or by placing the weighed portions of nickel and titanium directly into the furnace. Iodide titanium charges were made by drilling holes in the as-received rod and inserting the nickel or by wrapping the nickel in sheet. Sponge titanium alloys containing from 0.2 to 90 pct Ni and iodide titanium alloys containing 0.2 to 68 pct Ni were prepared by these methods. In addition to these alloys several 1/2 1b sponge titanium alloys were supplied by the Allegheny Ludlum Co. The charges were melted in an arc furnace under an argon atmosphere. The procedures used were similar to those reported in the literature5,' and the furnace has been described.' Except for iodide titanium alloys with 40 to 68 pct Ni (see section on copper contamination), each alloy was melted for 1 min, then either turned over or broken before re-melting for an additional minute. Currents of 200 to 400 amp were used depending on the melting point of the alloy. Prior to heat treatment, alloys containing less than 14.5 pct Ni were hot-forged at 750°C. With the exception of alloys in the homogeneity range of the compound TiNi, alloys of higher nickel contents could not be hot-forged. Heat treatment of iodide titanium base alloys was carried out in argon-filled quartz capsules which were broken under water at the conclusion of heat treatment to quench the specimens. Temperatures were controlled to ±5oC and annealing times up to 48 hr were used. For melting point determination, specimens were placed in carbon crucibles which were in turn en-capsuled in argon-filled quartz capsules. The start of melting was determined by rounding of corners and by metallographic examination. Complete melting was considered to have occurred at that temperature at which the specimen assumed the shape of the crucible. Specimens were prepared for metallographic examination by mechanical polishing or by an electrolytic procedure." For alloys containing up to 80 pct Ni Remington A etch7 50 pct glycerine, 25 pct HNO,, 25 8 HF) was used. For higher nickel alloys aqua regia and Carapella's etch (5 g FeCl,, 2 ml HNO,, and 99 ml methyl alcohol) were employed. Specimens to be exposed for powder patterns were prepared by filing, by breaking specimens in a

Jan 1, 1954