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By D. B. Jugle, J. B. Darby, O. J. Kleppa

A systematic study has been made of the kinetics of solution under steady state, dynamic conditions of titanium, vanadium, chromium, iron, cobalt, and nickel in liquid aluminum. It was found that the temperature dependence of the solution rate obeyed an Arrhenius-type rate equation, and that at a given temperature the rate of solution of the various solutes correlates quantitatively with the equilibrium solubility of the solute in liquid aluminum. These results are consistent with a mechanism where the rate-controlling step is the diffusion of solute atoms through a liquid boundary layer. THE present study was initially started in order to explore the feasibility of liquid-metal solution calorimetry for transition metals and alloys. Previous work1 in this field employing liquid tin as a solvent at temperatures in the 500' to 600' range had indicated that the rates of solution of most transition metals in tin are very low. Under such conditions effective solution calorimetry is difficult. The objective of the present investigation was two-fold: a) To obtain, as far as possible, quantitative data on the rates of solution of a series of transition elements in liquid aluminum. b) To explore whether liquid aluminum might be a suitable solvent for liquid-metal calorimetry. In the course of this work a comprehensive set of data was obtained on the steady state rates of solution of transition metals in a common liquid-metal solvent. The results are consistent with the boundary layer model, which assumes that the rate-controlling step consists of diffusion of solute atoms through a viscous liquid layer. EXPERIMENTAL PROCEDURE A vacuum-tight stainless steel vessel was surrounded by a resistance furnace, as shown in Fig. 1. In all experiments the temperature of the liquid solvent was controlled to 2.5' by means of a Micromax controller. A high-vacuum manifold connected to the vessel maintained a vacuum of 1 x 105 mm of Hg or better. The vacuum vessel was equipped with a charging section isolated from the working chamber by a vacuum-tight gate valve. This arrangement allowed the specimen holder to be removed or inserted into the apparatus without removal of the liquid metal bath. The specimen holder was suspended from a closed end stainless steel tube, which also served as the thermocouple protection tube. The portion of the tube that was below the solvent level was surrounded by an alumina protection tube to isolate it from the liquid metal bath. The stainless steel tube was connected through a rotary vacuum seal and a gear train to a fractional horsepower motor. For most experiments the tube was rotated at a constant

Jan 1, 1963

By Aldo L. Furno

Sufficient quantities of combustible vapors are released by some sulfurs to produce flammable atmospheres under prolonged storage. Hydrogen sulfide and carbon disulfide appear to be the principal flammable constituents in the vapor space above molten sulfur. If sufficient carbon disulfide is present, ignition of the vapor-air mixtures can occur spontaneously on contact with the heated surfaces found within storage tanks.

Jan 1, 1963

The changes in layout and design over 48 years, from the first crushing and shiploading plant installed at Whyalla in 1915, up to the present plant being built at Koolan Island, Yampi Sound may be summarized as follows.1. Smaller motors and lower power consumption have resulted froma. oil lubrication, where practicable, in place of grease,b. a high pressure "oil-lift" device to reduce starting torque in crushers with white metal bearings, andc. roller bearings in place of white metal.2. Short centre drives with pivot-based motors permit controlled loads on bearings and a reduction in size of crusher houses and motor rooms.3. Dust proofing and pressurising of crusher houses and motor rooms reduces working temperatures and improves cleanliness.4. Variable speed pan feeders give improved plant control, with the use of one man only, and remove the need for large surge bins between crushing stages.5. The use of diesel quarry trucks to dump ore through a "drive over"tip results in faster truck cycles.6. Elevated cylindrical silos with air operated chutes, replace long horizontal storage bins with multiple manually operated side discharge chutes for loading rail cars, and give faster and more accurate truck loading. The silos are charged by belt conveyors with automatic distributors.7. Increased shipping bin capacity (40,000 tons at Whyalla and 6O,OOO tons being built at Koolan Island) caters for the bigger vessels now in use and envisaged for the future. Automatic travelling distributors deliver ore to the bins in layers to ensure, maximum mixing and a more uniform grade for blast furnaces.INTRODUCTIONThe Broken Hill Proprietary Company Ltd has six major crushing plants in Australia at its principal sources of raw material. These are at Iron Knob bench G, Iron Knob scree ore plant, Iron Baron, and Cockatoo Island, all of which are ironstone operations. The other two plants are at Rapid Bay, a limestone quarry, and at Ardrossan, which is the Company's only source of dolomite.

Jan 1, 1963

By R. O. Scattergood, P. Beardmore, M. B. Bever

THE stored energy and microhardness of a Au-Ag alloy deformed by explosive loading were measured previously as functions of shock pressure' and compared with corresponding data for drawn wires.' The difference of the two processes has been explored further by investigating the annealing behavior of explosively loaded specimens and drawn wires. Sheet specimens, 0.042 in. thick, of a Au-Ag alloy containing 82.6 wt pct Au were explosively loaded in stacks of four.3 Wires prepared from the same melt of alloy were drawn through dies.' The annealing kinetics were determined by microhardness measurements on separate specimens for each annealing temperature and time. Several values of the stored energy were measured by tin-solution calorimetry Experimental details are given elsewhere. Wires were drawn until the microhardness or stored energy equalled the corresponding values of the explosively loaded specimens as nearly as possible. Wire drawn to a true strain 7 of 0.09 had approximately the same hardness and stored energy as specimens explosively loaded to a shock pressure of 70 kbar. The microhardness of specimens

Jan 1, 1963

By M. E. Tyrrell

Mixtures of zirconium diboride and iron, cobalt, and nickel were resistance sintered to high-density compacts using modified electric welding equipment. To evaluate the use of iron, cobalt, or nickel as binders for zirconium diboride, the sintered compacts were examined in polished section and tested for crushing strength, hardness, microhardness, oxidation rate, and resistance to mechanical shock. Each of the zirconium diboride-metal mixtures produced brittle cermets, but the hardness was generally satisfactory. The iron- and cobalt-bonded cermets exhibited rather poor oxidation resistance. Cobalt provided the least brittle bond, and nickel, the hardest and most resistant to oxidation. Iron tended to form chalky compacts with low resistance to mechanical shock.

Jan 1, 1963

This paper describes the results of a laboratory study on the upgrading of Algoma siderite by the amine flotation of silica and silicate gangue. The experiments indicate that a virtually complete removal of silica is possible in a rougher flotation con-ducted in tap water at natural pH, without prior desliming of the ore. Grinding considerably finer than the apparent liberation size is essential for maximum silica rejection. A cationic collector, Aeromine 3037, gave best results when used in combination with a modifier. Of the several modifiers tested, a Dutch potato dextrin, Dextrin 4356, was found to be the most effective. Both iron recovery and the grade of the final iron product are enhanced by floating the pyrite contained in the ore prior to the amine flotation of the silica, and by scalping the magnetics from the silica concentrate. F OR over twenty years, the Algoma Ore Properties Division of The Algoma Steel

Jan 1, 1963

By James Westfield

This publication covers the work of the Division of Coal Mine Inspection, Bureau of Mines, as performed under provisions of the Federal Coal Mine Safety Act. It presents background information and data since 1952 when the Act became effective and includes up-to-date statistics for the calendar year 1962. During that year, approximately 9,704 coal mines were active in the United States, and the Bureau made 12,810 regular inspections. BACKGROUND The Federal coal-mine inspection program was established to carry out the provisions in Public Law 49, 77th Congress, (H. R. 2082) approved May 7, 1941. This act has since been amended as Title I, Advisory Powers Relating to Health and Safety Conditions in Mines, under Public Law 552, 82d Congress, approved July 16, 1952, which also included Title II, Prevention of Major Disasters in Mines. Public Law 552 is known as the Federal Coal Mine Safety Act.

Jan 1, 1963

By J. Gordon Parr, M. J. Bibby

In addition to the (bcc) - (cph) transformation at 882°C a second distinct change of slope has been observed on a titanium cooling curve between 905" and 960°C.1,4 Duwez,1 commenting on work by McQuillan,2-4 attributed this arrest to contamination of the specimen with oxygen—a possibility that existed even at the reduced pressure of 10-5 mm Hg at which the experiments were conducted.

Jan 1, 1963

By R. F. Abernethy

Recent investigations in the United States and in other countries have produced considerable information on the nature and occurrence of minor elements in coal. The possibility of recovering certain elements, particularly germanium and uranium, from coal ash and other coal products has received considerable attention. Some flue dusts are potential sources of germanium, and certain lignite deposits are potential sources of uranium, but industrial recovery of these elements has been limited to small quantities for technical and economic reasons. Considering the large amount of coal mined annually, a small percentage of a rare element may have industrial significance if an economical method of recovery can be developed. In 1944 information on the occurrence of rare elements in coal was reviewed in Bureau of Mines Technical Paper 669 (46).3 This report is a revision of that paper with the view of summarizing published information available for United States coals, and pertinent information concerning coals of other countries. Selected references from the original paper are retained. New references do not include all preliminary reports when more permanent literature describing complete projects is available. Consequently, the list of references should not be considered complete.

Jan 1, 1963

A revolutionary development in blasting materials has occurred in recent years. Ammonium nitrate, sensitized by the addition of a small percentage of No. (class) 2 diesel fuel or other suitable petroleum product, has been adopted as a low-cost, efficient blasting agent2 in a wide variety of mining, quarrying, and heavy construction operations. Moreover, the ready availability of the component supplies throughout the Nation, together with the ease of formulating them into effective blasting agents, has made it possible for the blaster himself to prepare the mixes at the site of use. Recently, most established explosives manufacturers have begun supplying premixed AN-FO (ammonium nitrate-fuel oil) or a comparable product to various mining operations. However, many individuals and small business establishments are marketing premixed products prepared in facilities that are often poorly constructed and poorly located. Although these blasting agents have partly or wholly displaced explosives such as dynamites in many applications, there are some blasting operations in which the fuel-sensitized ammonium nitrate agents do not appear to be well adapted. As long as the hazards they present are clearly understood and respected, ammonium nitrate-based blasting agents have important safety characteristics when prepared under competent factory control or field-mixed under equivalent close control. This publication attempts to summarize the knowledge of those hazards and to incorporate practical ways to cope with them.

Jan 1, 1963

By J. W. Downey, S. T. Zegler

A study has been made of the occurrence of Phases having the Cr30-type structure in ternary alloys having the general composition where B cept for iron and copper all the B components are known to form binary compounds having the type structure. The occurrence of the struc-ture type in the ternary alloys was investigated using optical and X-ray metallography. The results indicate that iron can replace virtually none of the cobalt in at 900°C, but substitutes for nickel in up to the approximate composition tually insoluble in V3Ni and 2) and exhibit complete solubility. At 100 nickel can be substituted for cobalt in VSCo up to the composition solubility; and 3) in the system , two solid solutions having the type structure occur. At the same temperature, 1000°C, V3Si exhibits limited solubility for V3Co but is completely mis-cible with V3Ga. Lattice parameters have been determined for all the binary and ternary phases. The solid solutions are discussed in terms of the atomic size and electronic factors which are thought to influence the occurrence of Cr30-type phases. The binary compounds V3Co and V3Ni were found to form peritectoidally from o phases and a vanadium, the former compound at a temperature between 1000" and 1050°C, the latter between 800°and 900°C. The substitutions of nickel and rhodium for cobalt in V3Co were determined not to raise the superconducting transition of VSCo to a temperature as high as 2°K. The occurrence and stability of binary intermediate phases having the Cr30- or A15-type structure (space group o;, Pm3n) have been discussed in several recent papers . Vanadium forms the struc -ture at or near V3B stoichiometry with all the mem -bers of the cobalt and nickel groups in the periodic table and also with Au, Ga, Si, Ge, Sn, P, As, and Sb. This paper describes a survey of the occurrence of the CrsO-type structure in ternary alloys having the general composition V3(B, B') where B and B' are Fe, Co, Ni, Cu, Rh, Ir, Si, and Ga. The purpose of the survey was to clarify the connection between the position of the B partner in the periodic table and its CrsO-type phase-forming tenden~y.~,~ The survey is part of a broader program concerned with the influence of B-partner substitutions on the superconducting transition temperatures of CrsO-type compounds. The transition temperatures, Tc, of some of the ternary Cr,O-type phases found in the survey are also discussed in this paper. EXPERIMENTAL PROCEDURE The alloys were prepared by arc-melting in an A-He atmosphere and were in the form of buttons, weighing approximately 3 g. The metals used in their preparation were received from commercial sources and were in all cases 99.9+ pct pure. The vanadium was spectrochemically pure except for 800 ppm of Si, 200 ppm of Fe, and 200 ppm of Al. For study of each pseudobinary system at least seven alloys were prepared having the general compositions case of alloys containing gallium, melting losses were small, usually less than 0.3 pct of the total weight of the metals charged for melting. Melting losses were somewhat greater for gallium alloys, ranging in general from 0.9 to 5.0 pct. Ternary V-Si-Ga alloys were chemically analyzed and the results are given in Table I. The analyses show most alloys to be within 2 at. pct of the intended composition. Throughout the balance of the paper the intended compositions are used in discussing the alloys. The cast buttons were annealed within evacuated quartz capsules for times ranging from 3 to 6 weeks at temperatures between 800" and 1000°C and water-quenched. The phases present in the annealed and quenched alloys were identified by optical and X-ray metallography. X-ray diffraction photograms were made with powders prepared from the bulk specimens, by the use of a 114.6-mm-diam powder camera with copper irradiation. The lattice parameter of CrsO-type phases and their standard errors

Jan 1, 1963

By W. W. Weller

Low-temperature heat capacities of scandium sesquioxide (Sc203) and a mixture of cerium sesquioxide (Ce203) and cerium dioxide (CeO2) were measured over the temperature range from 50° to 298° K. The entropy of scandium sesquioxide at 298.15° K was evaluated directly as S°298.15 = 18.4 ± 0.1 cal/deg mole. That of cerium sesquioxide was extracted by combining the heat-capacity data for the mixture with those for pure cerium dioxide; the result was S298.15 36.0 ± 1.0 cal/deg mole.

Jan 1, 1963

By Elgin D. Bell

Within the next, year or two, Western Canada should overtake Mexico and France. to become the worlds second largest producer of elemental sulphur, surpassed only by the United States, By 1965, it should produce about 25% of the world's total elemental production and, about 10% of sulphur produced in all forms. In 1952 Alberta had but one small sulphur recovery plant. By 1962, it had fifteen plants with a total designed capacity of almost 6,000 long tons of sulphur per day and actual production of almost one million long tons per year. This decade of dynamic growth was the result of Alberta's rapidly developing natural gas industry. More particularly it was the result of approval in 1960 to export natural gas in large volumes into the United States. Prior approval to export gas from Alberta to eastern Canada and relatively modest volumes to the U. S. had resulted in the construction of several plants but none were of the scale required to serve the U. S. market.

Jan 1, 1963

By Arcy, D&apos Banister

Drilling practices at the Silver Summit mine in Shoshone County, Idaho, and the steps taken to increase drilling efficiency are described for the 1952 to 1958 operating period. Mining and development methods are outlined, and drilling equipment and practice are discussed, Cost and performance data include drilling time, bit duty, steel failure, drill repair, and compressed-air consumption. Steps taken to increase drilling efficiency and decrease costs are described, including modifications of bit design, new procedures for drill-rod fabrication and new processes for completing certain drill-machine repairs.

Jan 1, 1963

By D. L. Albright, G. A. Colligan

An investigation has been conducted to determine the nature of the crystallographic substructure of nickel and a 1.0 wt pct Ag-Ni alloy which had been undercooled 105°C prior to solidification. A rotating back-reflection X-ray technique and modified Weissmann diffractometer were used to orient single-crystal sections from these poly-crystalline ingots and to determine the substruc-tural features of these single crystals, The sub-grain size in the pure nickel ingot is 0.5 mm diam while the silver-doped nickel subgrain size is only 0.1 mm diam. The misorientation between adjacent subgrains is approximately 1 deg of arc in both ingots, and the spread of orientation of sub-grains about the mean orientation of the crystal is 5 deg of arc in both ingots. The addition of silver results in a stable impurity substructure which is preserved during isothermal solidification and subsequent cooling to room temperature. In the absence of silver the initial impurity substructure is destroyed by dislocation interactions which produce a secondary substructure which grows to a size five times larger than the initial substructure. THE process of undercooling a metal entails cooling of the molten sample below the equilibrium freezing point without the occurrence of solidification, i.e., by exercising proper constraint over the experimental variables contributing to nucleation in the melt. The current work of walker1 and Colligan Metal reports undercooling large continuous samples of nickel by imposing appropriate restrictions upon the parameters of solidification. The silver-nickel equilibrium diagram3 reveals the presence of a monotectic reaction at 1435°C. At this temperature the maximum solid solubility of silver in nickel is approximately 3 wt pct, but this solubility decreases with decreasing temperature and the solute is rejected as a silver-rich liquid phase at temperatures below 1435°C. Thus, the 1.0 wt pct solute should be held in solution during undercooling and solidification and subsequently precipitate as a silver-rich liquid phase at grain and subgrain boundaries following solidification during cooling below 1435. This assumes no solute segregation sufficient to cause the monotectic reaction. One would expect this second phase to inhibit grain and subgrain growth by retarding dislocation motion after solidification is complete. The effectiveness of silver addition in growth retardation of high-angle grain boundaries has been demonstrated by Colligan and suprenantS4 The principal [l00] dendrite growth directions in a 2 wt pct Ag-Ni alloy undercooled 53 all radiated from the nucleation site. A similar pure nickel ingot undercooled 59°C exhibited a random orientation of [l00] dendrite directions with respect to the nucleation site. Since undoped nickel ingots do not retain any evidence of the casting or solidification texture and silver-doped ingots do retain this texture, it is reasonable to assume that considerable grain growth has taken place in the pure nickel. These particular experiments were performed in order to reveal the differences, if any, in the features of the crystallographic substructure of undoped undercooled nickel and silver-doped undercooled nickel. 1) EXPERIMENTAL PROCEDURE Data are reported on selected specimens from two massive (approximately 260 g) undercooled ingots of nickel. One ingot consisted of electrolytic nickel and the other of this same material with 1.0 wt pct addition of high-purity silver. Powder patterns were taken of both the as-received and as-solidified materials; in all cases the reflections recorded were attributable to the individual elements nickel and/or silver. Fig. 1 is a. schematic diagram of the apparatus employed for the undercooling experiments. The equipment consists in part of a fused silica crucible for containing the charge. A fused silica tube encloses the system, which is covered by a brass cap to permit partial sealing of the inert atmosphere. This cap contains a hole through which a Pt-Pt 13 pct Rh thermocouple is inserted for temperature measurement. The charge is inductively heated under a purified argon atmosphere.

Jan 1, 1963

By J. Burlin Johnson

This report describes an investigation of the relationship between crater dimensions formed in laboratory blasting experiments and the mechanical properties of the material cratered. Scaled field data have been included when available. The results show that tensile strength and possibly other mechanical properties may be useful in predicting maximum crater dimensions.

Jan 1, 1963

By P. E. Churchward

Rhenium sources and recovery methods were investigated by the Bureau of Mines to delineate potential resources of the metal. The only significant rhenium resource appears to be about 28,000 lb of rhenium contained in the domestic annual output of approximately 20,000 tons of byproduct molybdenite concentrates from porphyry copper operations. An estimated 70 to 80 pct of this rhenium is potentially recoverable by processing the rhenium-bearing fumes and dusts obtained during conventional roasting of molybdenite concentrate. At 70 pct recovery this would amount to 19,600 lb of rhenium. A more conservative estimate by the Committee on Refractory Metals of the National Research Council (1513 is that 12,000 lb of rhenium metal could be produced annually from current production of molybdenite from porphyry copper operations in the United States. A procedure was developed in the laboratory for recovering rhenium in the form of electrolytic flake by electrowinning the metal from a solvent extraction strip solution. The procedure included (1) water leaching of molybdenite roaster flue dust, (2) selective extraction of rhenium from the leach liquor by contacting it with a kerosine solution of a quaternary amine, (3) stripping of rhenium from the loaded organic solution by a perchloric acid solution, and (4) electrodeposition of rhenium from the loaded strip liquor. Raw material for the studies was flue dust containing 0.48 pct Re, 35 pct Mo, and 23 pct S in sulfide and sulfate form, and small amounts of numerous metallic impurities. Water leaching dissolved 85 pct of the Re and yielded a solution that was 13 in sulfuric acid and contained, 1 g/l Re and 16 g/l Mo. The solvent extraction strip solution that was electrolyzed for rhenium deposition was 1 molar in perchloric acid and 1 molar in ammonium sulfate and contained 13 g/l Re and 0.01 g/l Mo.

Jan 1, 1963

By J. Weertman

It is shown that conditions suitable for the conversion of straight dislocations into helices are common in crystals hardened either through long-range dislocation interaction or by jog formation on dislocation lines. For dislocations other than screw dislocations or dislocations nearly screw in orientation, helices can be formed with the aid of core difhsion at temperatures low relative to the melting point of the material. It is assumed that, once formed, helices will degenerate into dislocation tangles. THE dislocation tangle is one major dislocation arrangement observed by the transmission electron microscope which had not been predicted previously from dislocation theory. Since first being observed, the tangle itself has become important in applied dislocation theory. The Cambridge school (P. Hirsch) bases part of its theory of work hardening upon this phenomenon.' In spite of the fact that the tangle obviously is a structure of prime importance to a cold-worked crystal, until recently relatively little attention has been paid to the question of exactly why or how tangles arise. It was generally assumed at first that cross slip and perhaps jog formation will lead to tangles. However Wilsdorf and schmitz2 concluded that cross slip cannot markedly contribute to the tangles. The Wilsdorfs and Maddin3'* have proposed that tangles arise by means of prismatic dislocation loops and superjogs which are produced by a precipitation of point defects. Dislocations with superjogs or which have joined with prismatic loops are themselves dislocation sources and they can produce new dislocations, a process they call "mushrooming", which then tangle with each other. There is no question that the Wilsdorfs et al. mechanism as well as the cross slip one can pro- duce tangles. However these may not be the only paths leading to tangle formation. In this paper we wish to consider another way tangles can form. Our work will be based on the theory of dislocation screw We wish to show that whenever a crystal is cold-worked there always is present a "driving force" leading to helix formation and thus to tangle formation. We do not expect to observe well-developed, regular helices in cold-worked metals. Rather we would expect that after a helix is formed random interactions with nearby dislocations will cause a well-developed helical dislocation to go over into an irregular form. A dislocation tangle is, of course, a grouping of dislocations with irregular forms. Therefore we feel that, in accounting for the formation of dislocation tangles, it is sufficient to show that many dislocations in a cold-worked crystal will take on helical form. The crucial step is helix formation. In order to have a straight dislocation assume a helical form, diffusion of vacancies, or interstitials, must occur. Our discussion of tangle formation therefore will be limited to crystals which have been deformed at temperatures ranging from about one fifth to half their absolute melting point. In this tem per a ture range appreciable core diffusion is possible. (There is no problem in explaining tangle formation at temperatures greater than half the melting point. At such temperatures dislocation climb through a bulk diffusion of point defects gives an extra degree of freedom to dislocation motion. This extra freedom of motion makes tangle formation easy.) At temperatures much below one fifth the absolute melting temperature diffusion processes are sufficiently slow that helix formation does not occur. Of course helix or tangle formation could occur in material deformed at very low tempera-tures which was subsequently warmed in order to make the thin specimen necessary for electron-microscope examination. Since within the temperature range of approximately one fifth to half the melting temperature the diffusion of point defects in the core of the dislocation is rapid, we can reasonably assume that within

Jan 1, 1963

By Gilman Y. Murray

The problems connected with the development of economically acceptable water supplies in arid regions are discussed. The techniques for capture and retention of runoff from infrequent desert storms are described and the major factors involved are emphasized. The exploration and planning for a typical water development in southwest United States is described, including an analysis of capital and operating costs for the proposed system.

Jan 1, 1963

By H. L. Riley

This report describes the methods and equipment used by the Watauga Stone Co. to drill and blast limestone in a two-level quarry, and to crush, screen, blend, and load this stone. Power requirements per ton of stone produced are reported. The personnel requirements for individual phases of the operation are tabulated in man-hours per ton of stone produced.

Jan 1, 1963