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By M. G. Benz

The superconducting performmce of diffusion-processed Nb3Sn is influenced by its micro structure. High isotropic transverse current density may be achieved in this material by a process which forms a precipitate of ZrO, within the Nb3Sn. FOR an ideal type-I1 superconductor, little or no transport current can be carried in the mixed state; i.e., little or no transport current can be carried above the lower critical field H,,, where the field penetrates abruptly in the form of current vortices or fluxoids, even though full transition to the normal state does not occur until the upper critical field H,,.' Fortunately, nonideal type-I1 superconductors can be readily obtained and these carry large transport currents up to the upper critical field H. Both theoretical and experimental investigations have attributed this current-carrying capability for nonideal type-I1 superconductors to pinning of the fluxoid lattice by heterogeneities in the microstructure of the superconducting material. These heterogeneities may take the form of dislocations or dislocation clusters,2"5 grain boundaries: structural imperfections introduced by phase transformations; radiation damage,8"10 or precipitates.11"15 Nb3Sn formed by diffusion processing is a type-I1 superconductor. Heterogeneities are needed for high superconducting critical currents above H,,. This paper will cover: a) what the microstructure of diffusion-processed NbSn looks like; b) what changes in the microstructure take place when the system is doped with precipitates, and c) how these changes in microstructure influence the superconducting critical currents. EXPERIMENTAL Preparation of Samples. Diffusion processing was used to form the Nb3Sn. The procedure used was as follows: a) coat the surface of a niobium tape with tin; b) heat-treat this tape at a temperature above 930°C to form a layer of Nb3Sn at the Sn-Nb interface. Such a layer of NbsSn is shown in Fig. 1 The thickness of the NbsSn layer formed was controlled by the time and temperature of the heat treatment. The same general procedure was used for preparation of both undoped samples and samples doped with a precipitate. An additional step was included in the preparation of the doped samples which consisted of internal oxidation of zirconium to form ZrOn. The details of the doping process will be reported in a later paper. Sample Testing. The Nb3Sn tape samples were soldered to a copper or brass shunt. Current and voltage leads were then attached to the sample in the usual four-probe resistance measurement configuration. The sample was cooled to 42°K. In some cases it was cooled in the presence of a high magnetic field and in other cases with the field turned off. The results were the same for both cases. The samples were oriented in a configuration with field transverse to current but could be rotated such that the angle between the field vector and the wide side of the tape sample could be changed. Measurements up to 100 kG were done in a superconducting solenoid and measurements above 100 kG in a water-cooled copper magnet at the MIT National Magnet Laboratory. Once the test field was reached, the current in the sample was increased until voltage was detected across the sample. The critical current was taken as the current at which voltage was first detected in excess of background noise. In most cases this was 1 to 2 x 10~6 v for a— in.-wide sample carrying several hundred amperes with a in. separation between voltage leads and with a 10 "-ohm shunt resistance. RESULTS AND DISCUSSION Microstructure. Examination of the microstructure of the undoped Nb3Sn shows rather large-diameter (1 to 2 columnar grains growing outward from the niobium surface toward the tin surface. As the layer is made thicker by longer diffusion times, these grains grow longer. Few new grains are started. Transmission electron microscopy shows little or no second-phase material within the bulk of the Nb3Sn layer. The microstructure of a diffusion-processed NbsSn layer changes quite drastically when the system is doped so as to form a precipitate within the NbsSn layer. Instead of large-diameter columnar grains of NbaSn forming, smaller-diameter (0.5 to 1 ) equiaxed grains of Nb3Sn decorated with the precipitate form. Fig. 2 shows a transmission electron micrograph of a Nb3Sn layer doped with zirconium oxide. This layer has been etched so that one may look between the grains

Jan 1, 1969

By Kendrick C. Hardcastle

The practice of transporting an ore or matrix from a pit area to the plant process area by means of a hydraulic pipeline has long been used by the mining industry. The industries which have classically used hydraulic transportation of ore to the plant include the phosphate mining industry, the heavy minerals mining industry, the clay mining industry, and the sand mining industry. As the advantages of this method become better known throughout the mining industry as a whole, and as techniques and expertise improve, its use will undoubtedly spread. Its use is presently being contemplated in iron mining diatomaceous earth mining, and several industries where massive removal of overburden is a predicate to economical mining. The widely recognized advantages of hydraulic transport at ion of ore from the pit area to the mines are: 1) Its relatively low initial capital costs. 2) Its speed of relocation at the mine site. 3) The washing and scrubbing action given to the ore by its hydraulic passage into the pit pump and the subsequent trip through booster pumps down the pipeline to the plant.

Jan 1, 1969

By Earl T. Hayes

This paper briefly reviews the laws enacted in the United States governing the coal miner. It discusses amendments to the Coal Mine Safety Act and describes the provisions of the Metal and Non-Metallic Mine Safety Act.

Jan 1, 1969

By M. L. Rizzone

Since time immemorial, Mother Nature has been transporting slurries with both air and water serving as the carrier medium. Consider for example the formation of the continental shelves off our coast lines which are being formed by rivers emptying erroded land surface and depositing it into bays and gulfs. As the erosion processes take place, the fines are suspended in water which flows in streams and rivers and deposits where the velocity of the flow reduces sufficiently to allow the fines to settle out. The same process in some crude form is provided when one hoses his driveway or patio and moves dirt so as to provide a cleaning action. These examples illustrate rather crudely how the formation of slurries allows for the transport of solids. In recent years, this mechanism has become fairly well understood and slurry pipelining of many materials is now a vivid reality. The movement of liquids in pipelines necessarily occasions the use of pumps for the purpose. Those of us who have had some rub with the petroleum industry are familiar with the transport of solids through mud pumps and cementing and fracturing pumps where the movement of slurries is an everyday matter. In the drilling of an oil well the circulating fluid utilized to remove chips which are cut by a drill bit from holes drilled deep in the earth is called drilling mud. This substance contrary to what the name might imply is usually a fairly sophisticated material designed to develop certain characteristics which are desirable in the drilling process. The particles which have been cut by the drill bit are suspended in the moving column of fluid and brought to the surface and deposited. The separation of the cuttings from the drilling fluids is accomplished by the use of shaker screens and settling pits. However, it is impractical to remove the fines completely from the drilling fluid and as a result they are pumped through the mud pumps back into the circulatory stream.

Jan 1, 1969

By William E. Lamont

As a part of the Department of the Interior's rutile and titaniferous materials development program conducted under the Defense Production Act, the Bureau of Mines investigated the potential for producing national stockpile grade rutile from plant products of phosphate beneficiation plants operating in the central Florida pebble phosphate district. The potential for producing ilmenite, zircon, and monazite concentrates from the plant products was also investigated. Results of these studies indicated that 3,000 to 6,000 tons of rutile, 28,000 to 55,000 tons of ilmenite, 9,000 to 19,000 tons of zircon, and 400 to 800 tons of monazite passed through the plant circuits annually. All of these minerals are presently being sent to waste ponds. Beneficiation of a bulk heavy mineral concentrate separated from the amine flotation tailing (froth product) of numerous plants in the district showed that it was possible to produce a rutile concentrate containing over 94 percent Ti02. Additional studies showed that over 70 percent of the Ti02 in the rutile concentrate could be isolated in a product containing 98.0 percent Ti02. The studies also showed that it was possible to produce ilmenite concentrates containing 63 percent Ti02, zircon concen¬trates containing 65 percent Zr02, monazite concentrates containing over 85 percent monazite [(Ce,La,Y,Th) (P04)], and xenotime concentrates containing over 35 percent xenotime (YPO4).

Jan 1, 1969

The following figures (Nos. 1-4) and tables (Nos. 1 and 2) were inadvertently omitted from the chapter entitled "Optimum Open-Pit Mine Production Scheduling" by Thys B. Johnson, Section 4, pages 539-562. [ ]

Jan 1, 1969

By N. F. Dyson, T. R. Scott

The iilzfluence of catalytic agents on the oxidation of ZnS has been studied under pressure leaching conditions, using a chemically prepared sample of ZnS which was substantially unreactive on heating at 113°C with dilute sulfuric acid and 250 psi oxygen. Nurnerous prospective catalysts were added at the ratio of 0.024 mole per mole ZnS in the above reaction but pvonounced catalytic activity was confined to copper, bismuth, rutheniuwl, molybdenum, and iron in order of. decreasing effectiveness. In the absence of acid, where sulfate was the sole product of oxidation, catalysis was exhibited by copper and ruthenium only. Parameters affecting the oxidation rate were catalyst concentration, temperature, time, oxygen pressure, and a7riount of acid, the first two being most important. The main product of oxidation in the acid reaction was sulfur, with trinor amounts of sulfate. An electrochemical (galvanic) mechanism has been suggested for the sulfuv-forming reaction, whereby the relatively inert ZnS is "activated" by incorporation of catalyst ions in the lattice and the same catalysts subsequently accelerate the reduction of dissolved oxygen at cathodic sites on the ZnS surface. Insufficient data was obtained to Provide a detailed mechanism for sulfate fornzation, which is favored at low acidities and probably proceeds th'rough intermediate transient species not identified in the preseni work. THE oxidation of zinc sulfide at elevated temperatures and pressures takes place according to the following simplified reactions: ZnS + io2 + H2SO4 — ZnSO4 + SG + HsO [i] ZnS + 20,-ZSO [21 In dilute acid both reactions occur but Reaction [I] is usually predominant, whereas in the absence of acid only Reaction [2] can be observed. Both proceed very slowly with chemically pure zinc sulfide but can be greatly accelerated by the addition of suitable catalysts, as suggested by jorling' in 1954. Nevertheless, an initial success in the pressure leaching of zinc concentrates was achieved by Forward and veltman2 without any deliberate addition of catalytic agents and it was only later that the catalytic role of iron, present in concentrates both as (ZnFe)S and as impurities, was recognized and eventually patented.3 It is now apparent that another catalyst, uiz., copper, may have also played a part in the successful extraction of zinc, since copper sulfate is almost universally used as an activator in the flotation of sphalerite and can be adsorbed on the mineral surface in sufficient amount The importance of catalysis in oxidation-reduction reactions such as those cited above has been emphasized by various writers and Halpern4 sums up the situation when he writes that "there is good reason to believe that such ions (e.g., Cu) may exert an important catalytic influence on the various homogeneous and heterogeneous reactions which occur during leaching, particularly of sulfides, thus affecting not only the leaching rates but also the nature of the final products." Nevertheless relatively little work has appeared on this topic, one of the main reasons being that sufficiently pure samples of sulfide minerals are difficult to prepare or obtain. When it is realized that 1 part Cu in 2000 parts of ZnS is sufficient to exert a pronounced catalytic effect, the magnitude of the purity problem is evident. An incentive to undertake the present work was that an adequate supply of "pure" zinc sulfide became available. When preliminary tests established that the material, despite its large surface area, was substantially unreactive under pressure leaching conditions, the inference was made that it was sufficiently free from catalytic impurities to be suitable for studies in which known amounts of potential catalytic agents could be added. The first objective in the following work was to identify those ions or compounds which accelerate the reaction rate and, for practical reasons, to determine the effects of parameters such as amgunt of catalyst, temperature, time, acid concentration, and oxygen pressure. The second and ultimately the more important objective was to make use of the experimental results to further our knowledge of the reaction mechanisms occurring under pressure leaching conditions. The fact that catalysts can dramatically increase the reaction rate suggests that physical factors such as absorption of gaseous oxygen, transport of reactants and products, and so forth, are not of major importance under the experimental conditions employed and an opportunity is thereby provided to concentrate on the heterogeneous reaction on the surface of the sulfide particles. As will appear in the sequel, the first of these objectives has been achieved in a semiquantitative fashion but a great deal still remains to be clarified in the field of reaction mechanisms. EXPERIMENTAL a) Materials. The white zinc sulfide used was a chemically prepared "Laboratory Reagent" material (B.D.H.) and X-ray diffraction tests showed it to contain both sphalerite and wurtzite. The specific surface area, measured by argon absorption at 77"K, varied between 3.9 and 4.6 sq m per g. Analysis gave 65.0 pct Zn (67.1 pct theory) and 31.9 pct S (32.9 pct theory). Other metallic sulfides (CdS, FeS, and so forth) used in the experiments were also chemical preparations of "Laboratory Reagent" grade. Samples of mar ma-

Jan 1, 1969

By H. L. Retcofsky

Carbon-13 nuclear magnetic resonance (18CNMR) spectra of nine 2-substituted pyridines, seven 3 -substituted pyridines, and nine 4-substituted pyridines have been obtained and analyzed. Substituents included both electron-releasing groups and electron-with hawing groups. Substituent effects on the magnetic shieldings of the ring carbons, except for those in the 2-positions of 2-substituted pyridines, were found to be quite similar to the effects reported for the monosubstituted benzenes, Thus, at least to a first approximation, the two classes of compounds have similar shielding mechanisms. Shieldings of the carbon atoms in the 5-positions of 2-substituted pyridines and those in the 6-positions of 3-substituted pyridines were found to reflect electron release or withdrawal by substituent groups, The pyridinium cation and the compounds 2,2'-dipyridyl and benzonitrile were also investigated.

Jan 1, 1969

Applications of helium in aerostatics, cryogenics, space, and undersea work are described in papers from the Helium Applications Symposium. Specific subjects include investigations of X-ray sources by means of balloon-borne instruments, meteorological soundings by balloons, powered lighter-than-air flight, tethered balloons, refrigeration techniques, large superconductive magnets, electronic devices, superconducting transmission lines, high-precision thermal conductivity analysis, He3-He4 dilution refrigerators, uses of helium in the atomic energy program, helium-cooled nuclear reactors, power- plant applications for high-temperature gas-cooled reactors, helium welding of stainless steel tubing and pipe, development of helium-shielded arc welding, helium as a diluent in spacecraft atmospheres, helium utilization in the Saturn-Apollo program, and helium utilization in diving environments. Papers from the Helium Centennial Symposium at the national meeting of the American Chemical Society cover the history of the discovery of helium, the history of its development by the Bureau of Mines from a laboratory curiosity to an important item of commerce, the source of helium in natural gases, the world of liquid helium, and liquid helium-3.

Jan 1, 1969

By Paul W. Johnson

A computer program for calculating capital and operating costs from material and energy requirements and equipment costs for use in preparing cost estimates for metallurgical process evaluations has been written by the Bureau of Mines' College Park process evaluation group. The program permits rapid recalculation of processing costs when changes of data or equipment are desired, and produces tables of capital and operating costs suitable for publication. Equipment cost summary tables for each process section end supplemental information for input-data checking is included in the computer printout. The program is written in Fortran IV except for several subroutines which are written in machine assembly language for the IBM 7094.3 With a few modifications, the program can be used on other computers.

Jan 1, 1969

By Haskiel R. Shell

While the original purpose of the Bureau of Mines work on fluorine micas was to synthesize large single crystals or film suitable to replace natural muscovite or phlogopite, the objective was broadened to include development of the many possible fluorine micas as a class of new, unique materials. Several methods were developed for the synthesis of the fluorine micas at atmospheric pressure: Solid state reaction, melting in crucibles, internal resistance electric melting, and arc resistance electric melting. The latter two methods are now med commercially. A variety of fluoromicas were synthesized by isomorphic substitution including disilicic, trisilicic, and tetrasilicic. Fluorophlogopite, KMg3AlSi3O10F2, is the fluoromica most widely used. While most of the fluoromicas are completely stable to water, many water-swelling fluoromicas and fluoromontmorrilonoids were synthesized. Single crystals or film of the fluorine micas were grown to 2 inches or more by a number of methods, but none has as yet proved economical. In the report, detailed data and descriptions are given on compositions, syntheses, products, and uses, and on the properties including physical, dielectric, chemical, X-ray, optical, and structural.

Jan 1, 1969

By Frank B. Fulkerson

Barge traffic on the Nation's inland waterways over the past 15 years has been increasing at a rate much faster than intercity freight traffic by all modes, largely due to the growing consumption of mineral commodities, development of more powerful towboats and large and more specialized barges, improvements to loading and unloading facilities, and competition among bargelines for contract shipment of bulk commodities. The Bureau of Mines, in a study to determine barge traffic projections for inland waterways in the South-Central States to the year 1980, gathered data on origin-destination patterns by commodity, quantity moved, equipment used, and rates charged; the trend of each of these factors over time; and the extent of competition between water trans-port and other means of transportation. The Mississippi River and the Gulf Intracoastal Waterway, which together carryover half the Nation's barge traffic, are major carriers of coal, crude petroleum, steel, marine shells, sulfur, salt, cement, and alumina. Greater quantities of these products will be transported by barge; however, oil pipe-lines and unit trains for coal are expected to limit increased barge traffic of these two commodities. Increasing quantities of fertilizer materials will be transported upstream. Although congestion at certain locks is a current problem, the Mississippi River below St. Louis and other open-river stretches have the capacity to handle the increasing number of barges for the foreseeable future.

Jan 1, 1969

By W. G. Park

Long-range projection of demand for domestic crude oil indicates a continued upward movement and accentuates the need for increasing the recovery from known crude-oil resources to supplement expected future discoveries. Consequently, the industry and Government have given special attention to the viscous or heavy-oil deposits because they offer the distinct possibility of large order increases in ultimate recovery. This report presents data pertaining to 150 heavy-oil reservoirs in Arkansas including oil characteristics of samples from 38 of these reservoirs. To January 1, 1967, about 600 million bbl of heavy oil has been recovered from the 150 reservoirs in 63 oilfields; however, about 4.5 billion bbl, or 88 pct, of oil remained in the ground. Of prime importance is that much of this heavy-oil resource is in reservoirs having characteristics considered favorable for thermal-recovery operations. Data for the thermal projects initiated [thus Ear are presented in individual field discussions. Also discussed is the t crude oil supply-demand situation in the State.

Jan 1, 1969

By Forrest T. Moyer

The safety record of the coal-mining industry, both anthracite and bituminous, in 1966 was improved over that of 1965 in all general measures of injury experience. The improvement was more pronounced in the anthracite industry. The total of 10,679 disabling work injuries comprised 233 fatal and 10,466 nonfatal injuries, 26 and 692 fewer, respectively, than in 1965. The number of fatalities in 1966 was the lowest annual total since complete records were started in 1910. Similarly, the number of nonfatal injuries in 1966 was lower than in any year since 1930 when such data were first collected.

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By G. A. Peebles

"This paper describes the various types of radiometric instruments and the techniques of their operation for grade control, sampling, assaying and probing drill holes at Eldorado Nuclear's uranium mine in northern Saskatchewan. Modifications that have been made to these instruments are discussed, and suggestions are made for the development of more refined and specialized radiometric equipment."

Jan 1, 1969

By L. K. Smith, C. R. May, K. R. Schrag, H. Buchwald

"New contracts for 65 million long tons of coking coal valued at over $900 million, over the next 15 years, herald the rebirth of Alberta's coal industry. The industry is optimistic that export orders may reach 20 million tons per annum by the mid-1970's. Coal will be extracted from underground and surface mines and it is expected that the total labour force will double from the present 1,200 men within the next two years. Ali the health hazards associated with coal mining are likely to be encountered and it will be incombent on the Provincial Department of Health to specify the standards which relate to health and environment where no such standards have previously existed. This paper examines some of the problems which are being encountered in setting up an environmental health program and reviews the practicability of environmental monitoring methods, with special reference to respirable dust."

Jan 1, 1969

By W. H. Patterson

The history and experience of early companies in the Islands is illustrated by the typical transactions of Trans-Western from 1959 to date. Trans-Western had entered into farmout agreements with companies strong enough to carry out at least the required minimum exploratory work and then such development as might be warranted. The farmee companies were required to make deposits to guarantee work performance during the first period of validity, i.e. the first 3 years of the 12-year life of the permits, and at the rate of 5 cents per acre. At that time, a good deal of geology was available, as a result of extensive exploration that had been carried on by the Geological Survey of Canada and other geological enterprises, with field parties travelling over and camping on all of those Islands. Trans-Western's farmees then selected, from Trans-Western's priority on 13.5 million acres, what they believed were the lands most prospective of producing large oil and gas discoveries, and, having the right to trim off acreage which they considered less prospective, thereby reducing the acreage of Trans-Western and its farmees to in excess of 5.5 million acres. The farmees then commenced a 3-year program carrying out geological exploration to the required minimum of 5 cents per acre, and with some permanent and many mobile camps.

Jan 1, 1969