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Jan 1, 1962

By W. D. Robertson, E. G. Grenier, V. F. Nole

The electrical, mechanical, and corrosion cracking properties of an age-hardenable Cu-Ni-Si alloy have been studied over a range of time, temperature, and deformation states for the purpose of determining the relationship between the properties and the structural state. The precifitate has been identi3ed as and the sites of preferred precipitation have been located by electron microscope studies of the structures developed by various combinations of heat treatment and plastic deformation. An extreme form of deformation banding has been observed in the aged alloy that results in high strain concentration in bands lying parallel to {111} planes. These bands are the structural paths along which transcrys-talline cracks propagate in the deformed alloy. The observations provide a basis for a general mechanism of transgranu-lar corrosion cracking of face-centered cubic alloys in terms of stacking fault probability. AMONG the age-hardening copper alloys the copper-nickel-silicon (Silnic Bronze) type is outstanding in exhibiting a high strength combined with a considerable capacity for cold working, a relatively high conductivity, and a low to negligible susceptibility to stress corrosion cracking. It is not a new alloy and it has been the subject of a number of investigations,1-5 which were made primarily to establish practical composition and heat treatment limits. The structural characteristics of the aging processes in this alloy have not previously been studied in detail. This particular investigation was undertaken to explore, in detail, and over a wide range of conditions, the properties obtainable by various combinations of working and heat treatment and to correlate structural changes with the observed mechanical, electrical and corrosion properties. MATERIAL AND PROCESSING Eight different commercial heats of the alloy were made and used in the investigation. The range of composition among the eight heats is shown in Table I. Billets, 8 by 24 in., were cast into water-cooled molds, extruded to 1.687-in. rod, and quenched in water after extrusion. Extruded material was rod rolled to 0.750 in., annealed at 1450° F for 2.5 hr, and quenched in water. Subsequent working operations were performed by tandem rolling to various sizes depending on the degree of reduction required. Final cold-working operations were performed by drawing to a uniform size of 0.187 in. diam and straightening by a roller straightening machine (Lewis). The combinations of heat treatment, working and aging that were investigated are summarized in Table 11; the various treatments were performed in the order given in each row of the table, and they will be subsequently identified by the symbols shown in the first column. SOLUTION TREATMENT All material investigated in the cold-worked condition, or cold worked prior to aging, was solution

Jan 1, 1962

By G. H. Matheson, J. M. W. Mackenzie

The coal concentrates studied contained clay slimes which would not flocculate on the addition of a polymer flocculent alone. The mechanism of the flocculation process is interpreted on the basis of the flocculation of lyophobic colloids. The filtration rate characteristics are shown to deviate slightly from certain basic filtration equations. Cake moisture was shown to decrease with cake drying time and vacuum, and increase with cake thickness. Filtration is a commonly accepted method of dewa-tering the fine coal concentrates produced in coal cleaning operations. Dewatering of these concentrates, using drum or disc vacuum filters, usually presents few technical difficulties and will result in the production of a filter cake containing some 20 to 25 pct moisture. In many coal cleaning operations it is common practice to add flocculants to the coal concentrates prior to filtration to increase the filtration rate. The mechanism whereby flocculation increases filtration rate has been summarized by Gaudin,4 while Geer, et a15 have compared the effectiveness of starch and synthetic flocculants as filter aids for a variety of coal concentrates. Coal concentrates, containing appreciable quantities of expanding lattice clays of the montmorillonite-illite group, sometimes prove impossible to filter without flocculation of the pulp prior to filtration. The fine coal concentrates produced at the Newcastle washery of The Broken Hill Proprietary Co. Ltd. fall into this group. Coals mined in this district contain appreciable quantities of expanding lattice clays which break down in the washery circuit waters and, by processes of mechanical inclusion, contaminate the coal concentrate thickener feed. Despite the classifying action of this thickener, the underflow which is pumped to the filters contains sufficient clay slimes to render filtration of the unflocculated pulp impossible. Filtration leaf and plant tests were carried out to develop effective and economic flocculant combinations and to determine the filtration characteristics of the flocculated coal concentrates. The determination, by leaf testing, of the filtration characteristics, and the analysis of these characteristics in the light of the equations of Brown2 resulted in the successful trial operation of the filters in the Newcastle washq. Although the filtration characteristics are not entirely in agreement with the theoretical treatment of Brown, the equations developed made it possible to predict, from leaf tests, the effect in the plant filters of pulp density, form vacuum, and form time on filtration rate and filtrate volume. EXPERIMENTAL PROCEDURES The sample used for leaf testing was the coal concentrate thickener underflow, which in plant operations would form the feed to the two 12-disk Dorr-Oliver filters. The feed to the coal concentrate thickener comprises the undersize produced by dewatering the Diester table concentrate on 5-mm dewatering screens and the overflow produced by cycloning of the froth flotation concentrate. At the time of testing these filters were inoperative because of the difficulties in filtration, arising from contamination of the

Jan 1, 1962

By T. V. Philip, R. E. Lenhart

When commercial silicon iron sheets of varying magnetic quality are isothermally annealed at high temperatures, extremely large grains develop in the material having good magnetic properties. These grains are of the (110) [001] orientation and are formed by secondary recrystallization. The primary driving force for this secondary recrystallization is grain boundary free energy. For the secondary grains, activation energies of 103 kcal per mole for nucleation, and of 75.5 kcal per mole for growth, were obtained. The activation energy for nucleation of the secondary grains is consistent with a model involving redistribution of a precipitate acting as the primary grain growth inhibitor. SINGLY oriented silicon iron sheet was first produced in 1935.1 The material as commercially produced today has a very highly developed preferred orientation or texture; up to 95 pct of the grains are crystallographically oriented with their (110) planes in the plane of the sheet and their [loo] directions parallel to the rolling direction. This texture, usually written as (110) [00l], is referred to as the "GOSS" or the "cube-on-edge" texture. Because the magnetic properties of this material are superior to those of the nonoriented sheets in the direction of rolling, the oriented silicon iron has acquired tremendous industrial importance especially in the manufacture of transformer cores and other electrical equipment. The commercially produced material is essentially an iron-silicon alloy containing about 3 1/4 pct Si with minor impurities totaling less than 0.15 pct. The silicon steel heat is melted in the open hearth or electric furnace. The ingots are hot rolled, with or without being slabbed, to strips of 0.100 to 0.080 in. thickness. They are then cold reduced to an intermediate thickness, recrystallized, cold reduced to final thickness, decarburized, and finally annealed at a high temperature. During this high-temperature anneal, extremely large grains with the cube-on-edge texture are produced in the sheet. Several papers have appeared in the literature2-10 relating to the production of the Goss-textured material. Most of these describe the textures produced on cold rolling and on subsequent annealing of single crystal or polycrystalline silicon iron. May and Turnbull11,12 have recently shown the necessity of a second-phase dispersed impurity in the material for the production of the Goss texture. However, none of these papers describes in detail the nucleation and growth kinetics of the (110) [001] grains during the final high-temperature anneal.* The present work, therefore, is an attempt to understand the nucleation and growth kinetics of the cube-on-edge grains in the silicon iron sheet during the final high-temperature anneal.

Jan 1, 1962

By G. B. Craig, J. Rezek

The critical resolved shear stress of zone-refined zinc single crystals deformed in tension is found to increase with increasing amount of striation substructure. The increase in strength with numbers of striations can be accounted for by a dislocation pile-up mechanism. A somewhat different means of plotting stress-strain data is introduced which allows a more unambiguous choice of yield stress to be made. FEW systematic studies of the role played by mac-romosaic or striation-type substructure in the de- formation of high-purity metal single crystals grown from the melt have been reported. McGrath and Craig' found that striations increased the critical resolved shear stress of zone-refined aluminum crystals, postulating a dislocation blockage by the striations as the strengthening mechanism. Lauri-ente and Pond2 found that, as the etch pit density increased in aluminum crystals grown from the melt, the critical resolved shear stress also increased. Fleischer and Chalmers3 also found changes in the critical resolved shear stress of aluminum crystals grown from the melt at varying rates, but could not be certain whether an increase of strength with rate was due to a higher concentration of impurity in the gage length or to an increase in the number of small-angled boundaries. An early work by Hibbard4 indicated that copper crystals containing lineage boundaries were stronger than those free from this type of imperfection.

Jan 1, 1962

By R. J. Wasilewski

Electrical resistivity variation with temperature was measured on a series of alloys containting up to 33 at. pct of oxygen over the range 77° to1500°K. The resistivity behavior is highly anomalous and itzconsistent with simple metallic conduction. Both composition and temperature-depended resistivity singularities were observed. A few experiments carried out on Ti-N and Zr-O alloys indicate the presence of similar anomalies. These observations, together with the published data on effects of substi-tutional alloying on the resistiuity of titanium, suggest that the anomalies are inhevent in the electron structure of this group oj metals. The existence of two-band conduction, and a significant shift of bands relative to each other with temperature and/or the electron concentration are suggested. CONSIDERABLE advances have been made in recent years in the alloy theory of simple metals. Very little, however, is known about the bonding in transition metals and their alloys.&apos; Titanium, with its relatively few electrons, may be expected to show simpler alloying behavior than the more complex transition elements. Its alloys with the interstitial elements appear particularly attractive in an investigation of bonding characteristics because of a) the simple nature of the solute elements, b) the remarkable similarity between the equiatomic structures Tic, TiN, and TiO, and c) the extensive solid solubility ranges of oxygen and nitrogen in a titanium reported.2,3 The Ti-O system was chosen for the most extensive investigation because of the relative ease of preparation of suitable specimens. Since the main object of the work was to obtain data on the bonding and its changes on alloying, electron-sensitive properties were primarily investigated. The present work describes the investigation on the electrical resistivity-temperature-oxygen content relationships. A few experiments were also carried out at selected compositions in the Ti-N and Zr-O systems. EXPERIMENTAL Materials and Method. Polycrystalline specimens were prepared in the form of hairpin strips some 50 by 5 by 0.15 to 0.50 mm by direct metal-gas reaction. This was carried out by controlled oxidation followed by a homogenizing anneal at a higher temperature. All the test specimens were fully homogenized as judged from the uniform microstructure and microhardness. To avoid preferred orientation, each strip specimen was annealed in the ß range prior to the oxidation, this procedure assuring random orientation in the strip;4 hence any texture resulting from the oxidation reaction itself affected all the specimens to a similar extent. Titanium used was of high purity (66 DPN, 10 Kg load; major impurities 0,-43G ppm, N,-70 ppm, C-25 ppm, Fe-14G ppm). The solute content of the alloys was determined by weighing, after the reaction with a known amount of oxygen. The specimens in which the discrepancy between the volumetric and gravimetric measurements exceeded 2 pct (or 0.2 mg for the low oxygen alloys) were rejected. The mean between the two measurements was then taken as the oxygen content of the alloy. Check analyses showed no measurable nitrogen contamination. All oxygen contents are given in atomic percent. Zr-O alloys were prepared in identical manner from hafnium-free crystal bar metal, cold-rolled to strip 0.25 mm thick. Ti-N alloys required very long reaction times at the maximum temperature available (1250°C). In order, therefore, to detect possible oxygen contamination, duplicate specimens were reacted in every experimental run, and one of these was analyzed both for oxygen (vacuum fusion) and for nitrogen (Kjeldahl). Only the specimens in which the check analysis showed < 1000 ppm O were then used for resistivity investigation. Since only relatively high nitrogen alloys (7.1 at. pct; i.e., 2 wt pct N,) were investigated, this oxygen contamination was considered permissible. Dc resistance was measured by the four-probe method as previously described.= The temperature was determined with a calibrated thermocouple placed in the center of the specimen hairpin. The errors in the specimen resistance values thus obtained were estimated at 1 pct due almost exclusively to the finite thickness of the potential wires and the consequent uncertainty as regards the true resistance length of the specimen. For the calculation of the specific resistance, however, no dimensional measurements could be carried out on most of the

Jan 1, 1962

By J. F. Butler

Boron nitride, BN, has been identified in boron low-carbon steels by means of light microscopy, electron microscopy and diffraction, and chemical analysis. This boron nitride is responsible for strain aging suppression in these steels through the removal of nitrogen from solution; however, small oxidizing potentials which result in deboronization In the austenitic temperature range also result in boron nitride decomposition and the subsequent occurrence of nitrogen strain aging. THE addition of boron to low-carbon steels is an effective means of eliminating the detrimental effects of strain aging;&apos;,&apos; however, the mechanism by which boron suppresses strain aging has not been established. In studying the effect of heat treatment on the strain aging of boron low-carbon steels, Butler3 found that no detectable nitrogen was present in the ferrite solid solution after various heat treatments even though the total nitrogen analyses of the steels were 0.003 pct N. Apparently the function of boron in suppressing strain aging is the removal of nitrogen from solution to form a relatively stable second phase. A clue to the identity of this phase was found by Speight4 who extracted from an aluminum-killed boron steel an acid insoluble residue which contained boron and nitrogen in proportions corresponding to the compound, BN. Shyne and Morgan5 found that the addition of nitrogen to a hardenable boron steel lowered its hardenability in a manner which suggest-d the presence of nucleating particles (presumably BN) even at high austenitizing temperatures. Although this indirect evidence for the presence of boron nitride in boron steels has been found, the compound was not identified metallographically as a separate phase in these steels. Because boron has an affinity for oxygen comparable to that of silicon,5 boron steels must be thoroughly killed with aluminum in order to prevent the reaction of boron with oxygen.7 The affinity of boron for oxygen also is demonstrated through the ease of deboronization of a boron steel in an oxidizing atmosphere. Digges, Irish, and Carwile8 found that a mixture of wet natural gas and air caused both deboronixation and decarburization of a boron steel at 1900°F. The boron content rose at the surface of the steel due to the formation of boron oxide. Shyne and Morgan9 encountered deboronization at much lower oxygen potentials; loss of boron occurred in steels treated at 1750o F under argon purified to 0.0014 pct 0, even though decarburization did not occur. Boron oxide, B2O3, is much more stable than the nitride, BN, as is indicated by the standard free energies of formation at 980oC: -235 kcal per mol of B2O3 (liquid) and -28 kcal per mol of BN (crystal). It is evident that the oxygen potential must be kept low in the presence of BN in order to prevent its decomposition and the subsequent formation of B2O3&apos; The purpose of the work described in this paper was to identify the nitride phase responsible for the removal of nitrogen from solution and to study its stability under oxidizing conditions. IDENTIFICATION OF BN In order to identify the phase containing boron and nitrogen, several alloys high in boron and nitrogen were made up in a small vacuum furnace. In alloys 3 and 4, Table I, electrolytic iron was used as a charge material. Boron additions were made in the form of 18 pct B ferro-boron after the iron was molten. In the case of alloy 3, the charge was solidified at this point; for alloy 4, nitrogen at 1 atm pressure was admitted over the melt before it was

Jan 1, 1962

By H. R. Ogden

The notch sensitivity of titanium alloys is affected by impurity content, microstructure, and heat treatment. Using notch tensile properties to evaluate notch sensitivity, three commercial titanium-base alloys were investigated over the temperature range of -320o to 390°F. The alloys studied were Ti-5Al-2.5Sn, Ti-6Al-4V, and Ti-2Fe-2Cr-2Mo. Six interstitial levels were studied for each alloy in four mi-crostmctural conditions. The ff- 0 alloys were studied in both the annealed and heat-treated condition. All tests were conducted using 1/4-in. diam round tensile samples. The notched samples had a 50 pct notch with a notch sharpness (a/r) of 53, corresponding to Kt 6.3. Notch sensitivity was increased by increased interstitial content, low temperature, and acicular-type microstructures. The heat-treated, high-interstitial content - 13 alloys were more notch sensitive than the same alloys in the annealed condition. In addition, minima in the notch tensile-temperature curves were observed at temperatures near 32°F. These minima became more pronounced with increasing interstitial content. 1 HE increaseduse of titanium alloys in high strength applications at subzero temperatures requires that a better under standing of the low-temperature behavior of the alloys be obtained. At low temperatures, metals generally exhibit increased strength with lowered ductility and tohness. Notch sensitivity and the factors which influence it become more important as the strength level is increased and the temperature is decreased. Some of the factor s which affect notch sensitivity in ti- tanium alloys are composition, interstitial content, microstructure, and heat-treatment condition. In this paper, the results of a study of these variables on the notch sensitivity of three titanium alloys at temperatures from —320o to 390o are reported. The notch geometry selected for this program was chosen to provide a severe test of notch sensitivity. The ability of the metal to flow without initiating fracture under these severe conditions is reflected in the notch-strength values. Since notch strength is, in part, determined by the constraint exerted by the combined tensile stresses, the behavior of notch specimens reflects the properties of the material under combined stresses. For example, a material with a high notch-unnotch strength ratio may be expected to withstand the biaxial stresses encountered in a pressure vessel better than a material with a low ratio of notch-unnotch strengths. This implies that maximum strength alone is not a sufficient criterion for applications of this type. It further may be concluded that the various conditions that promote poor notch behavior also will affect adversely the performance of materials under combined stresses. In the alloys studied, these included low temperatures, high interstitial levels, and hasformed microstructures. EXPERIMENTAL PROCEDURES Three alloys, Ti-5Al-2.5Sn, Ti-6Al-4V, and Ti-2Fe-2Cr-2Mo, were purchased from commercial producers as 2-in.-dam rod stock. Oxygen and nitrogen were added to these alloys by remelting to obtain a variety of interstitial contents as shown in Table I. In order to Compensate for the much more potent strengthening effect of nitrogen compared with oxygen, an oxygen equivalent content is used to describe the total oxygen plus nitrogen contents studied. It has been suggested previously1 thatnitro-gen is approximately twice as effective in strengthening as oxygen, and carbon, to the extent it is in so-

Jan 1, 1962

By W. V. Kotlensky, H. E. Martens

In an earlier communication, Ref. 1, the authors presented the tensile properties and the changes in crystal structure and microstructure for pyrolytic graphite tested at 2750°C. It was suggested that changes in the structure may have an effect on the tensile properties of this material. Accordingly, tensile tests were run on a series of specimens, from one block of pyrolytic graphite, some of which were hot-worked by being strained at 2750°C, others of which were tested in the as-deposited condition. According to the manufacturer, General Electric Co., the polycrystalline material was deposited at 2100°C on a substrate of synthetic graphite by decomposition of a dilute natural gas mixture. The as-deposited material had a density of approximately 2.19 g per cc, and as shown in Fig. 1 had a structure of medium size growth cones which were regenera-tively nucleated. All specimens had a gage section 0.75 in. long by 0.06 in. wide by 0.1 in. thick with the thickness direction perpendicular to the basal planes. The testing method and equipment used have been previously described, Ref. 2 and 3. For both the hot-working and the testing the load was applied parallel to the basal planes; a cross-head speed of 1.5 x l04 in, per sec was used. All heating was done in an atmosphere of bottled helium.

Jan 1, 1962

This investigation was supported by a grant from the American Iron and Steel Institute and a fellowship given by the Armco Steel Corp. We are indebted to J. F. Butler of the Jones & Laughlin Steel Corp. for a portion of the alloys used in this investigation and to R. L. LeRoy of the Armco Steel Corp. for chemical analyses.

Jan 1, 1962

Jan 1, 1962

Jan 1, 1962

By Albert J. Phillips

The effect of impurities on the flowsheet in the smelting and refining circuits for copper, lead and zinc is reviewed and the interflow of by-poduct metals from copper, lead and zinc plants is pointed out. The principal points of separation of all impurities in the circuits are indicated and the additional steps added to these circuits in order to effect impurity separation me shown. In this day and age, when difficult metallurgy is mentioned, one thinks of the extraction of more refractory or possibly the alkaline earth or rare-earth metals. It is true that the extraction of metals having a high affinity for oxygen and deleterious solubility for that element in the liquid metal, affords some of the most difficult extractive metallurgy problems. When this is coupled with an affinity for hydrogen, nitrogen, and carbon a devious approach is required that sometimes rivals the complexity of the metallurgy with which this paper deals. However, in all such cases the aim is for a simple

Jan 1, 1962

By Werner Joseph, Richard R. Knobler

When the first batch of refined copper ingots was cast at Mantos Blancos in January 1961, eight years of exploration, development and metallurgical pioneering by Mauricio Hochschild & Co. had come to a successful conclusion. This Chilean copper deposit, located in the Atacama Desert 30 miles from Antofagasta, is now producing approximately 20,000 tons of copper per year. The Mantos Blancos deposit has been known since 1912 and various attempts had been made to work the high-grade zones before the present operation was started. The major drawback of the ore to any previous development was its chloride content which varies between 0.4% and 1.5% C1. Although the chloride ruled out the conventional leaching-electrolysis scheme, it did lend itself to the process of precipitating the copper as cuprous chloride.

Jan 1, 1962

To Americans, Alaska occupies a unique position, both geographically and historically. The only integral portion of the United States lying in the sub-Arctic and Arctic regions of the Earth, the early remoteness and climatic conditions effectively combined to impede the economic development of this area. Although Alaska has been a part of our Nation since 1867, its mining industry is still at that stage of development which characterized the West 100 years ago when miners concentrated on high-grade lodes and rich placer deposits. Since World War II, however, there has been a noticeable increase of interest in the raw materials of the North. This concern has been most noticeable in Canada, Scandinavia and Russia, but it has been, and is being shown in Alaska. To the American mining industry, the potential importance of this State can be summed up by the question, "Can Alaskan mining compete successfully with those of other states and countries?" The answer revolves about the vital factors of geography, economics, and the political turmoil of the World. These aspects are among those discussed on the following pages in a series of articles by Alaskans and non-Alaskans alike. We invite you to read "Alaska: Regional Report."

Jan 12, 1961

By C. W. Merrill

Minerals research by the U.S. Bureau of Mines embraces the mining and metallurgical problems of some 80 metals and nonmetals excluding the mineral fuels. It requires the energies and talents of about 1400 persons, almost half of whom are professionally trained in the physical sciences or engineering. Of approximately $13 million appropriated to the Bureau for minerals programs in Fiscal Year 1962, 76% has been allotted to technologic research and 24% to resources examination and appraisal. In addition, almost $2 million will be made available to the Bureau for minerals research from other Government sources and from private organizations that wish to utilize Bureau experience and capabilities in cooperative studies.

Jan 11, 1961

By E. L. Fisk

First discovered and claimed in 1929, the Cordero cinnabar deposit lies 11 road miles southwest of McDermitt, Nev., near the Nevada-Oregon boundary. The name "Cordero" means "little lamb" in the Basque language and is symbolic of the fact that the first ore specimen was found during the lambing season. The Bradley Mining Co. held the property for several years during the early thirties, but it was not until 1939 that Cordero Mining Co., a subsidiary of Sun Oil Co., entered the picture. The company, then known as Horse Heaven Mines, Inc. conducted preliminary work in 1940 which proved enough near-surface ore to warrant the construction of a mill during the following year. By 1943, Cordero was being rapidly depleted when deeper churn drilling intersected the large underground orebody that is still being mined today.

Jan 11, 1961

By F. Windolph

There are no hard and fast rules for building tailing dams, and each case has to be analyzed individually because of special conditions encountered at each location. Certain criteria are used for building dams at Climax, Colo., where they must be placed in rather steep mountain valleys on foundations that are practically impermeable. The tailing is relatively coarse, and a coarse fraction stays near the berm where it is deposited, while most of the fines flow with the water to the pool. Thirty years experience has led to certain design for toe dams, decanter lines and towers and tailing dams. A new tailing disposal area, started at Climax in 1958, will ultimately have a height of 495 ft and impound about 300 million tons. The following applies to the construction of this new tailing area.

Jan 11, 1961

By H. M. Callaway

There are key words common to Government and the minerals industry, the use of which immediately spark interest, argument and confusion. Among these is productivity, a term ranking for widespread misunderstanding with mineral self-sufficiency and mineral conservation. Each interpretation of these words tends to emphasize a single aspect and either minimize or ignore the complex dynamic system of things that influence the Nations mineral productiveness. This paper1, abstracted from a monograph on lead now being prepared for publication by the Bureau of Mines, not only sheds light on the trend of productivity in the lead-zinc mining industry but it presents the basis for forming a common general notion of what the term productivity implies.

Jan 11, 1961

By A. C. Backeberg

There is no South African code for the design of reinforced concrete headframes, and all those erected have been designed on a uniform basis which, up to the present, has tended to be conservative. With certain exceptions designs have generally conformed with British Standard Code of Practice C.P. 114. In the design of reinforced concrete headframes the following loads are taken into account:

Jan 11, 1961