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By B. D. Cullity, A. Freda

It is well known that deformation by cold drawing or swaging produces a kind of preferred orientation called fiber texture in metal wires. Such textures have been extensively studied by means of X-ray diffraction, chiefly by techniques in which the diffracted X-rays are recorded photographically. This paper describes some results obtained with a new method, involving the use of a diffractometer. X-RAY METHOD Since the pole figure of a material having a fiber texture is symmetrical about the fiber axis, there is no need to present the entire pole figure. Instead, texture data can be summarized by means of a curve showing the variation of pole density along any meridian of the pole figure, if the north-south axis of the latter is made parallel to the fiber axis. The position of a pole on the meridian is specified by the angle 9 between the pole and the fiber axis (wire axis). The X-ray method1 used here to measure pole density as a function of 9 actually consists of two methods, referred to as A and B. In method a, X-rays are reflected from the wire surface. Pole densities can be measured by this method from O = 90 deg down to a limiting value which is dependent on the Bragg angle 8 and is typically of the order of 30 to 40 deg. Method B involves diffraction from the wire cross section and covers a range of 0 values from 0 up to an angle sufficient to overlap the measurements made by method A. By a combination of the two methods, a complete pole-density curve can be obtained. However, method A alone, which requires no specimen preparation other than etching, can often reveal enough of the pole-density curve to provide complete information about texture components. Both methods require that the measured diffracted intensities be corrected for changes in absorption and diffracting volume with changes in 9. A11 intensities I reported in this paper are corrected diffracted intensities; they are propor-

Jan 1, 1960

By H. P. Stuwe

It is investigated whether a model of sphere packing permits the computation of the lattice parameters and their variation with concentration in various a phases; it does, except in phases containing silicon. Several observations indicate that a particular role is played by the "E-atoms" in the lattice. THE phase is formed by many alloys of the transition elements.'-' Its structure has been described by Bergman and Shoemaker,5,8 Dickins, Douglas, and Taylor,7 and Kasper, Decker, and elanger.' There are five kinds of crystallographically equivalent positions for the 30 atoms in the unit cell which have been designated by these authors I, 11, 111, IV, and V or, in the same sequence, A, B, C,D, and E, as shown in Fig, 1. For the purposes of the present paper two elements of the lattice will be discussed separately: The lattice planes perpendicular to the c-axis which are made up by the atoms A, B, C, and D and which determine the a-parameter; and the close-packed "vertical rows" of E-atoms which determine the c-parameter. asper,9 and Frank and kasper10 described the a phase and other complex structures as sphere packings. In these papers particular attention is paid to the coordination polyhedra. Lattice positions with an equal number of nearest neighbors are considered equivalent regardless of their crystallo-graphic description. This seems to work very well for the explanation of ordering phenomena in the a phase as far as information on this is available." If the description of the phase as a sphere packing is valid it should be possible to draw two further conclusions: 1) It should be possible to calculate the lattice parameters from the atomic radii of the components, and 2) It should be possible to predict the variation of the lattice parameters with concentration within one phase field. Both points are discussed in this paper. PROCEDURE Measurements of lattice constants were done with a symmetrical back-reflection X-ray camera. With Cr-radiation, about a dozen a1 lines could be observed with most samples. From the (550/710)- and 720-lines the a-value was computed. With this value the c-parameter was calculated from the (333)- and (413)-lines. Finally, the position of all the other lines was computed from the lattice parameters thus obtained. In this way the validity of the indexing could be checked and, at the same time, this proce- dure gave an estimate of the accuracy of the lattice parameters. A correction was made for film shrinkage. The atomic radii used in the computations are the Goldschmidt radii for coordination number 12. Actually, some of the atoms have a coordination number of 14 or 15, but the error thereby introduced is small. * For the computation of lattice constants from the atomic radii an "average atomic radius" of all components was used, i.e., complete disorder was assumed. Although this seems to be true for some systems like OS-Cr,4 it is not true in others.11,13,14 The ordering model, however, which has been suggested by Kasper on the basis of extensive research lets both kinds of atoms contribute to both the ''vertical rows" and the lattice planes perpendicular to them, so that even with ordering of this kind the assumption of complete disorder cannot introduce a very serious error in calculating lattice parameters. RESULTS Bergman and shoemaker6 gave a table of the interatomic distances in the Fe-Cr phase. If we disre-

Jan 1, 1960

By H. B. Farnam

"THE IRON ORE Company of Canada has been using do-it-yourself type explosives for three years. During the last 12 months we have used over 10 million pounds of ammonium nitrate-fuel oil explosives and either purchased or formulated one million pounds of slurried explosives.W e have been moving approximately one million cubic yards of stripping and ore per month and we expect our production rate to in-crease. Eighty per cent of our strip-ping and ore is soft enough to be blasted successfully with ammonium nitrate-fuel oil mixtures. Twenty per cent of our material is extremely hard and requires an explosive having greater strength than an AN-fuel oil mixture.W e had been using canned am-monium nitrate base explosives and TNT pellets to give maximum bottom loading density to fracture hard rock. As AN -fuel oil became widely used, it was apparent that other types of explosives could be formulated to fit our blasting requirements. Dr. M. A. Cook of the University of Utah was consulted regarding new explosives and together we developed the blasting slurries.Figure 1 shows a general view of one of our hard rock pits. The foot wall is on the right-hand side and this material is called iron forma-Figure 1.-General view of hard rock pitstion by our Company but is called 'Taconite by the operators on the Mesabi Range. This material runs 35 to 45 per cent iron and many pieces are hard enough to scratch glass. The formation is tilted at an angle of 55 degrees as can be seen in Figure 3.The bedding planes of this rock are about 24 to 36 inches apart and if the material is not well broken or fragmented, large chunks or slabs must be handled by the shovels which reduces shovel capacity and efficiency and increases maintenance costs."

Jan 1, 1960

By Wallace W. Key

Chalk is a natural calcium carbonate occurring as the remains of soft, friable, minute marine organisms. Whiting can be either finely ground calcium carbonate prepared from chalk, marble, or limestone or the product obtained by chemical precipitation from a solution or suspension containing lime. Until relatively recently, whiting made from limestone was termed "whiting substitute," but it is now usually designated as limestone whiting. Precipitated calcium carbonate, sometimes called "precipitated whiting" or "precipitated chalk," is a finely divided calcium carbonate product obtained by chemical precipitation from a solution or suspension containing lime. Considerable quantities of precipitated calcium carbonates are produced from many chemical processes. Naturally occurring calcium carbonate in a variety of crystalline forms and in all degrees of chemical purity forms a substantial part of the earth's crust. Exactly where a chalk grades into a marl or calcareous shale through increase of clay or silt or into a hard limestone through consolidation and crystallization is difficult to determine because no rigid specifications have been promulgated for classifying them. Composition and Properties Once considered to be amorphous, chalk was later found to be cryptocrystalline. In the pure state it consists entirely of CaCO3, but many deposits are impure. When impurities are removed and the material is reduced to a finely divided state, it is known as chalk whiting. Much confusion attends the use of the term "chalk" as well as the classification of whiting materials. For instance, blackboard chalk is not necessarily chalk but is sometimes plaster of paris or a form of talc. Colored "chalks" may be true chalk colored and compressed with a binder but are probably such materials as hematite, clays, or carbonaceous matter. The term whiting was applied exclusively to the product derived from true chalk before World War I. Chalk imports were difficult to acquire during World War I, and whiting substitutes, a term applied to the products derived from natural rock deposits and precipitated calcium carbonate, were introduced. Substitute whitings were not acceptable at first, but it was found that blending true chalk with substitutes often created an improved product; eventually by selection of limestone and finer grinding, products not only acceptable, but for some uses superior to chalk whiting, were developed. Gradually the term "substitute" was dropped because chalk whiting had lost its importance, being largely supplanted in the United States by other whiting materials. Whiting is now made in ever-increasing quantities from limestone, marble, dolomite, marls, vein calcite, oyster-shell, as well as primary and byproduct precipitated calcium carbonates. Distribution of Chalk Europe-In England, France, Belgium, Denmark, and other European countries highpurity chalk occurs in extensive beds. The Cretaceous period, or the "age of chalk," in geologic history receives its name from the great deposits of chalk exposed on either side of the English Channel. It has been estimated that oceans in which chalk and allied deposits were formed covered more than 500,000 square

Jan 1, 1960

By W. A. Krivsky, R. Schumann

Relaxation calculations were made to find the temperature distribution in the refractory wall surrounding a tuyere pipe. One set of boundary conditions approxiwated those of a standard copper converter while a second set represented a hypothetical,thermally insulated tuyere pipe. The pvonounced cooling effect of the tuyere is related to the problem of tuyere accretions and tuyere bunching. PARTICULARLY severe service conditions are encountered in the tuyere zone of a basic copper converter during the matte blow. High-temperature gradients result from the juxtaposition of the hot charge and the tuyere pipe carrying cold air. Refractory temperatures near the tuyere mouth vary rapidly with time when the blast is turned on or off. One of the most serious problems is the formation of magnetite accretions around the tuyere mouth, which occurs very rapidly under some operating conditions. As a result, continual punching of the tuyeres is necessary to maintain a satisfactory rate of converting. Thus, if some means could be devised for keeping the tuyere pipes fully open without necessity for punching, a considerable saving should result from reduction in labor cost, maintenance of full capacity operation, and reduction in refractory costs. Recent quantitative studies of the FeO-Fe,O,-SiO, system1 have shown that the solubility of magnetite in iron-silicate slags decreases rapidly with de- creasing temperature in the range of copper converting temperatures. Data taken from the previous work are shown in Fig. 1. Thus the formation of "horns" and accretions around the tuyere mouth can result simply from the freezing out of magnetite on the cooler areas of refractory immediately adjacent to the tuyere pipes. One might expect to find a correlation between the severity of magnetite formation and the area of refractory surface which is cooled below the freezing point of the slag (corresponding to magnetite precipitation). Magnetite itself has a very high melting point (1597°C) so that the accretions are for all practical purposes infusible. The accretions might be dissolved by increasing the silica content of the slag and at the same time raising the temperature, but this approach is not feasible because it results in rapid corrosion of the basic refractory lining of the converter as a whole. In order to understand better the problems involved in tuyere design and operation, it seems essential to have at least a semiquantitative idea of the thermal conditions in the tuyere zone. Accordingly, this paper presents results of thermal calculations for an idealized copper converter tuyere. These calculations follow the so-called relaxation

Jan 1, 1960

By Arthur B. Cummins

Mineral fillers are employed in United States industries to the extent of more than seven million tons annually, valued in excess of a hundred million dollars. This substantial usage involves a wide variety of mineral materials. To this may be added products manufactured from minerals, such as carbon black, portland cement, lime or chemically precipitated calcium carbonates, which would add substantially to the total. The purposes for which fillers are used differ considerably. Minerals used as fillers are mostly silicates, silicas, and carbonates as referred to hereinafter. The term "mineral filler" has various meanings in mineral technology and in the arts. Fillers are comparatively inert and their action is mainly physical. Materials that are employed primarily for chemical reactivity, or for pigment or abrasive functions ordinarily would not be considered to be fillers when used for these purposes. Nearly all filler usages are based on advantages which are gained by desired modification of composition properties or by improvements in processing. A simple definition for a filler is an inert material that is included in a composition for some useful purpose. This definition may be amplified or made more specific for each of the filler usages, the major ones of which are: paints, paper, plastics, rubber, bituminous compositions, pesticides and fertilizers. There are in addition a whole host of minor usages. Powdered minerals when employed as components in paints, varnishes and lacquers are considered as extender pigments or low refractive index pigments. In paper, the term loading material as well as filler is used; in pesticides, the terms diluents and carriers connote different functions. For bituminous compositions, rubber and plastics, the usage of the simple word "filler" is more usual, but the designation loading material is sometimes used. Minerals Used as Fillers Most of the industrial minerals, and many rock powders are employed to some extent for different filler uses. These usages vary from year to year depending on availabilities, costs, technologic trends and advancements. For the major applications, however, and for the more particular requirements at any given period, there are general trends which favor a more or less restricted group of filler products for each of the major consumer fields. This selection of materials is determined by the characteristics of the individual filler products, their effectiveness in fulfilling the primary function or functions for which they may be employed, and the cost after incorporation in the finished product. The mineral-bearing materials of major importance as fillers are: limestones, clays of several types, talc, pyrophyllite, mica, barite, diatomite, crystalline silicas, asbestos, slate and other rock dusts. Others of secondary importance include: gypsum, vermiculite, phosphate rock, perlite, and pulverized wastes, such as slag and fly ash. A considerable number of other minerals are used to lesser extent. Among these minor mineral materials are: feldspar, pumicite, wollastonite,18 tripoli, nepheline syenite,6 coal, altered volcanic rock and others.2 Indeed, most mineral materials, when reduced to fine particle size may have some potential usage as fillers, depending on their properties, availability and price. On the other hand, the more exacting filler requirements

Jan 1, 1960

By Ward C. Smith

The industry of producing and processing boron compounds is called the borax industry because the chief product is borax, the decahydrate of disodium tetraborate. For the same reason, it is common to speak of borax mining. Reference to borate mining also is common, and while appropriate where it emphasizes the diversity of borate minerals that are mined in various countries, it is rather unsatisfactory where used in a general sense, because it seems to exclude the important production of borax from brine at Searles Lake, California, and of boric acid from steam vents in Tuscany, Italy. The terms "boron industry" and "boron mining" might seem more comprehensive, but are little used, and this is fortunate because they would be misleading-the element boron is manufactured only in small amounts for special uses, and it is not found free in nature. In most occurrences, boron is combined with oxygen and is in a borate or borosilicate material. The history of the modem borax industry starts with the introduction into Europe of borax from Tibet in the 13th century, about the time of Marco Polo, if not actually by him. The discovery that borax has unique value as a flux in metal soldering and ceramic glazing must have been made at some unknown time much earlier. As a rule, any mineral that has been used so long that its early history is lost must occur in deposits that are easily recognized and worked, and this is undoubtedly true of borax in Tibet. According to meager accounts,9 the borax occurs there in arid mountain basins as surficial crusts that coat the ground about thermal springs and seeps of mineralized water, and as coarser crystals in the bottom muds of shallow pools and lakes. Much the same essential features of surface exposures and minerals easy to recognize and recover characterize most of the deposits later found and worked elsewhere. The borax industry at the present time is faced with rising demands for its products, and consequently is increasing its productive capacity and appraising its borate resources.18 The areas that contain the known borate deposits are most likely to yield additional production, hence their distribution in the world is of interest, and is summarized later in this chapter. Mineralogy The mineral raw materials used by the borax industry include various borates mined in several countries, borax extracted from brines at Searles Lake in California, and boric acid extracted from the steam of vents in Tuscany in Italy. The hydrated borates[$] of chief commercial importance are listed in Table 1, which also shows their chemical composition. The properties of only the four most important borates are summarized here, but detailed descriptions of the borates and the minerals commonly found with them can be found in mineralogy textbooks.41 Ulexite generally forms clusters of silky fibers rather than large individual crystals. A

Jan 1, 1960

By H. Conrad Meyer

The wizardry of nucleonics has added new and greater dimensions to the almost inseparable "twins"-zirconium and hafnium. So close is their relationship that neither element is found free of the other in any presently known mineral. Although zirconium in the form of its oxide was discovered in 1789 by Klaproth, the metal in an impure, nonductile form was not isolated until 1824 by Berzelius. About 100 years later -1925-van Arkel and deBoer developed and patented a technique for the deposition in vacuo of crystalline, coherent, highly ductile metal of extreme purity on an electrically heated filament through the dissociation of gaseous zirconium tetraiodide. Within the past five years both zirconium and hafnium have been dramatized by the press and in popular science magazines. This has led to the false assumption that practically all of the world consumption of zirconium ores is used in the production of the metals. Recent statistics on the subject show that not over 15 pct of the zirconium ore consumed in 1958 went to ferrosilicon zirconium and zirconium metal. The rest was consumed in refractories, foundry sand and facings and ceramics. The importance of zirconium as a component in compact, relatively lightweight nuclear energy units, such as those now used in the submarine Nautilus,6 is well established. A rival of zirconium metal as a casing for atomic fuels is a newly developed ceramic body. It is claimed to be cheaper than zirconium-to withstand higher temperatures-and to be more resistant to corrosion. Whether such ceramic casings have the required low thermal neutron absorption cross section, high strength and easy formability of zirconium is yet to be demonstrated. Hafnium, because of its low order of abundance and its close chemical relationship to zirconium, was not definitely recognized as a new element until around 1923, despite prior claims. A study of the X-ray spectra of zirconium led to its identification. The circumstances leading to the discovery of hafnium were much less fortuitous than those surrounding zirconium. The more precise tools of arc and X-ray spectrometry lent themselves admirably to the search for elements to fill certain gaps in the periodic table. [ ] Pure, ductile hafnium-a metal similar in appearance to stainless steel-has a specific gravity of 13.3 (zirconium 6.52) and a melting point of 2,200°C. In other respects it closely resembles zirconium except in one important respect which gives it a preeminent position in nuclear energy development, namely, a high thermal-neutron absorption cross section. This explains the necessity of hafnium-free zirconium in atomic piles. The ability of hafnium to capture thermal neutrons makes it an excellent "moderator" of "governor" when used as control rods in nuclear reactors (Table 1).

Jan 1, 1960

By W. E. Horst

John Dasher (Central Research Laboratory, Crucible Steel Co. of America, Pittsburgh. Pa.)— Getting spodumene to float quickly and cleanly can be a problem. The author has presented an excellent account of a valid and useful approach to the scale-up of such problem floats. This indicated advantages for doubling retention time, i.e., buying another set of flotation cells. The author states that 21 pct of the spodumene floated in 2 min in the laboratory cell, that the grade of the rougher was about 75 pct spodumene, and that the final tailing contained 4 to 12 pct spodumene in different sizes with the present cells and 1 to 9 pct spodumene with twice as many cells. About 20 years ago, this writer obtained in the laboratory the flotation of over 90 pct of this spodumene in a King's Mountain sample in 1 min at a grade of 90 pct spodumene in the rougher and a final tailing that contained only 1 pct spodumene. The methods of Norman, Ralston," and Gieseke' were used, which teach that spodumene floats quickly and cleanly if its surfaces have been properly conditioned chemically and/or mechanically prior to flotation. Although feed preparation is not discussed, the results reported indicate that it is inadequate. This writer suggests that improvements in this area might be more effective than doubling the number of cells. W. E. Horst (author's reply)—Dasher's comments are appreciated by the author and require some clarification. He suggests that improved spodumene flotation performance may be obtained by feed preparation techniques rather than increased retention time in flotation. Certainly flotation performance is dependent on feed preparation and this is an important feature in the flotation process. It is true that certain types of spodumene ores, particularly weathered ores, require more complicated feed preparation processing than clean ores to achieve the desired flotation results. It was not implied that current feed preparation techniques are the same as experienced during the scale-up investigations. Although discussion of feed preparation was omitted from the article on scale-up relationships, the important feature was that pre-treatment processing was the same for each level of operation investigated— laboratory, pilot plant, and plant scale. Under these similar conditions large differences existed in recovery for comparable time intervals in each scale of operation. It is highly probable that feed preparation techniques could be modified and thereby increase the flotation rate for each scale or all scales of operation discussed. However, modifications would have to be justified on an economic basis.

Jan 1, 1960

By N. A. Richard, A. E. Austin, R. E. Maringer

AS part of a detailed study of the structure of metallic meteorites, the concentration and distribution of iron and nickel in the various phases of meteor -itic iron have been measured using an electron-probe microanalyzer. The specimen used was cut from a position about 3 in. below the surface of the Grant meteorite, a one-half-ton iron specimen (containing 9.35 pct Ni) found in New Mexico some years ago. A photomicrograph showing the general Widmanstztten structure, somewhat typical of iron meteorites, is shown in Fig. 1. The line across which the analyses were made is indicated by arrows. This area was chosen so as to evaluate the iron-nickel concentration in the three principal phases visible in Fig. 1. These phases, in the language of meteoritics, are kamacite, taenite, and plessite. Kamacite is the a-

Jan 1, 1960

By R. J. Borg, C. E. Birchenall

Vapor pressures of eight compositions of Mg-Cd have been determined by the Knudsen effusion technique. Measurements are made at several temperatures for each alloy and the results interpolated to a common temperature for the calculation of the activities. It is not possible to obtain values for the partial molar enthalpies because of the narrow temperature range spanned by the measurements. The results show less precision than those obtained for pure Cd which are also reborted. These alloys are extremely susceptible to corrosion which provides a possible explanation for the lack of precision. Nevertheless, the values of the activity are in good agreement with the results of electromotive force measurements previously reported for the Mg-Cd system. MAGNESIUM and cadmium are mutually soluble in all proportions in the solid state and form a single phase which has the hexagonal close-packed structure. X-ray investigations of this system1,2 have revealed a rapid variation in the relative dimensions of the unit cell occurring at approximately 50 at. pct. The rate of change of the c/a ratio with composition increases markedly for alloys containing more than 50 at. pct Cd. The purpose of this investigation was to determine the activity of Cd in the neighborhood of 50 at. pct and to discover whether or not the thermo-dynamic properties undergo a similar rapid change. The activities are calculated from vapor pressure data obtained by the Knudsen effusion method. Unfortunately the precision of the data from which the thermodynamic values are calculated is insufficient to establish unequivocally a departure from the normal trend. The results are reported primarily because they substantiate the only previously reported activity measurements3 and because they include values for pure Cd which in contrast to those of the alloys show excellent precision. The Cd-Mg system is known to contain several ordered phases. However, this investigation was made at temperatures considerably above the transition temperatures, and the alloys may be regarded as nearly random solid solutions. EXPERIMENTAL Apparatus—The effusion cells are machined from solid tantalum rod. The lids consist of threaded, flanged rings of tantalum onto which are welded shallow cups of 4 mil molybdenum foil. The orifice, which is located at its center, is made by grinding off a small dimple produced with a sharpened punch. Such an orifice has been mounted in plastic, sectioned, and the thickness of the orifice edge measured in a microscope. The maximum thickness is 0.00016 in., and the Clausing factor is consequently equated to unity. The area of the orifice is determined by tracing its projection on the screen of the metallograph at a known magnification and measuring the area of the tracing with a planimeter. Excellent temperature control is achieved with a 4 by 18-in. alundum core, gradient-wound, furnace

Jan 1, 1960

The Rosebery and Hercules mines, situated in the Rosebery-Williamsford district in western Tasmania, have a history of production dating back to 1896-7, although full scale production did not commence until 1936, following the development of a satisfactory process of selective flotation (Hall, Cottle, Rosenhain and McGhie, 1953). The mineral composition of the Rosebery zinc-lead ores was first described in detail by Stillwell (1934). The Hercules ore is generally similar, but as yet no descriptions of it have beenpublished.Since Dr. Stillwell's paper appeared, the management of the Rosebery and Hercules mines has from time to time submitted a number of interesting mineral specimens to C.S.I.R.O. Mineragraphie Investigations. Examination of these specimens brought to light eight minerals, some relatively uncommon, not previously recognized in these ores.They are cassiterite, molybdenite, stannite, electrum, meneghinite, boulangerite, pyrargyrite and pyrrhotite. Some of the specimens are also rich in tetrahedrite and gold. In addition each of the other ore minerals described by Stillwell, viz. pyrite, sphalerite, galena, bournonite, chaleopyrite and arsenopyrite, was detected in one or more of the specimens examined during the present study. The principal gangue minerals were found to be quartz, manganiferous carbonate, sericite and barite, agreeing closely with the observations of Stillwell.The present study was based on the examination of the following eight specimens.

Jan 1, 1960

By W. H. Ode

Because trade increased among various nations after World War II, the Coal Committee of the Economic Commission for Europe established a Classification Working Party in 1949 to develop an International system for classifying coal. Although national classification systems existed, they had been developed in accordance with characteristics of domestic coals without reference to coals of other countries. Terms for describing similar or identical coals differed in each nation. This caused confusion in evaluating coals shipped in international trade and also hampered exchange of technical information on problems of coal utilization. Experts4/ participating in the classification project early in their work agreed that two systems should be formulated, one for the higher rank coals or so-called "hard" coals in European terminology and the other one for the lower rank coals, the latter designated mainly as brown coals and lignites in the various countries. Rank refers to the degree of metamorphism (progressive alteration) in the natural coalification series from lignite and brown coal to anthracite. The system for classification of hard coals was published late in 1956 as a document of the United Nations.5/ Results of a study for applying this system to American coals were published in 1958.6/

Jan 1, 1960

By B. S. Crocker

Pebble grinding was used at Lake Shore Mines in 1949. A full description of experimental evidence and test plant results was published in 1952 1 and further operating details in 1954 2.' In more recent years the term autogenous grinding has been coined and is now frequently seen in the technical literature. Autogenous crushing and/or grinding covers any grinding mill in which the larger pieces of ore are made to grind the fine pieces; the crushing and grinding may be either dry or wet. This discussion deals only with wet autogenous grinding, and only in the fine grinding part of the circuit, i.e., from 6 mesh to 92 pct —325 mesh. The term pebble milling could apply to fine autogenous grinding in which the pebbles are made from the ore itself, or it could also refer to grinding with pebbles, such as flint pebbles, from a source outside the mine. The first mill to use screened ore to grind the ore (1949) was Lake Shore Mines, Kirkland Lake, Ont. Pebbles were screened from the jaw crusher discharge and used in 5x16-ft tube mills which had been converted to 6 ft 8 in. by 16-ft grate discharge pebble mills. The same general practice was adopted the following year by the Wright-Har-greaves Mine in Kirkland Lake. Shortly after that the Neptune Mines in Nicaragua started correspondence with the writer concerning the possibility of using screened ore for grinding in their plant. They first ran some plant-scale tests which confirmed the Lake Shore findings, with the ultimate result that their plant was successfully converted in 1956 to an autogenous grinding plant. In 1957-1958 the writer was successful in converting the grinding plant of Renabie Mines in northern Ontario to autogenous grinding. In all these plants the existing grinding equipment was converted, usually by expanding the diameter of the shell to make the change from steel grinding to ore pebble grinding mills. In all the above plants primary grinding was done in either small rod mills or ball mills. These mills first reduced the pebble mill feed to about 6 mesh. The final grinding in the pebble mills varied from 75 pct —200 mesh to 92 pct —325 mesh. At Lake Shore three stages of pebble milling were used, with a different size pebble in each stage. In other parts of the world interest was being shown in this form of grinding, and in March 1952 the writer had some correspondence with the mill staff at Outokumpu in Finland, with regard to the pebble system used at Lake Shore. At Stockholm in 1957 the account of the crushing and grinding system at Outokumpu was presented in a paper by H. Tanner and T. Heikkinen.V his is the only ore grinding plant that does not use grate discharges on its pebble mills; trunnion discharges equipped with heavy reverse spirals retain the pebble load. The first new mill designed to use screened ore as a grinding medium was the Bicroft mill at Bancroft, Ont., which began operation in the fall of 1956. In 1957 this plant was followed by similar installations at Faraday Mines, also in the Bancroft area, and the North Rankin Nickel Mines in the North West Territories. In 1958 the Dyno Mill at Bancroft was converted, using the same type of grinding. Since all these plants, designed by Kilborn Engineering (1954) Ltd., were originally planned as pebble grinding mills, they were able to take full advantage of the latest design and technique. They are neat in appearance and very efficient and easy to operate. Effect of Ore Hardness: It is often commented that this type of autogenous grinding applies only to hard siliceous ores. Experience has shown that this is not so. In the past ten years the author has had an opportunity to test more than a dozen ores, several of which were quite soft. One of these was shale. The softer ores actually make better looking pebbles than the hard ores. These soft ores produced no particles in the intermediate size range which could not be ground by the largest pebbles in the mill charge. Slabby ores, such as shales, make a suitable pebble for the —6 mesh grinding. It is not generally recognized that for fine grinding a spherical medium is not essential or more efficient. Another frequent objection to pebble grinding is the belief held by some operators that there is too much variation in the hardness of their particular ore to make it acceptable as a source of pebble media. Experience has also shown that this is not a serious problem at all. The variation in pebble load due to changes in the ore hardness is nothing like as great as most people would expect, and the method used for feeding the ore and controlling the the load in the mills is more than sufficient to take care of daily variations in ore hardness. This point

Jan 1, 1960

By A. G. Guy

Zinc vapor from a reservoir of liquid zinc maintained at lower temperatures was diffused into sets of copper-zinc alloys at 759° and 870° C and into sets of silver-zinc alloys at 650° and 700° C. Each set of ,four copper-zinc alloys consisted of pure copper and 90/10, 80/20, and 70/30 brass. Similarly the set of silver-base alloys consisted of specimens containing 0, 7, 15, and 20 pct Zn. Natural markers at the initial surfaces of the specimens ware "trapped" under a thin electroplate and their depth of burying was measured after diffusion. The ratio of diffusivities of the two components determined from these data and the chemical diffusion coefficient calculated by the Matano method agreed with previously reported results. The line of markers was irregular and was often discontinuous when a grain boundary was crossed. TECHNIQUES involving the vapor phase have been widely employed in studying diffusion phenomena in metals. Many investigators have evaporated the more volatile component from an alloy, but it is generally believed that the porosity created under these conditions interferes with adequate interpretation of the experimental results. The extensive work of Gertsriken6 has been criticized on this score. Accary1 found that the diffusion coefficient for de-zincification of brass is larger by a factor of five than that for zincification, although he attributed the difference to a higher vacancy concentration under conditions of dezincification. Balluffi and siegle2 thoroughly investigated the technique of adding a more volatile component to a less volatile base metal as a means for studying diffusion. They verified that no porosity forms in a brass under these conditions and that the diffusivities of the two components can be determined from observations of the motion of markers originally placed on the surface of the specimen. The mathematical analysis that they developed for treating the experimental data was modified in a later note, but essentially it involved using the graphical Boltzmann-Matano method that is customarily applied to solid-solid diffusion couples. The experimental method used in the present research was similar to that employed by Balluffi and Siegle except for two modifications. Balluffi and Siegle used alloy chips as the source of metal vapor. This procedure has the disadvantage that the concentration of solute at the surface of the specimen changes during the diffusion experiment as the alloy content of the chips is gradually decreased. This disadvantage was overcome by employing liquid zinc as the source of zinc vapor in a manner similar to that described by Herasymenko.9 There was then no limitation on the amount of solute usefully available, and several relatively large specimens could be diffused in a given experiment. The second modification was the use of natural markers on the surface of the specimen rather than larger, artificial markers, such as the alumina powder employed by Balluffi and Siegle. It was expected that the fine, natural markers would permit more precise measurement of the buried interface as in the case of ordinary sandwich specimens.10 EXPERIMENTAL The experiments were designed so that zinc from the vapor phase would maintain a constant zinc content at the surface of pure copper (or silver) and

Jan 1, 1960

By J. M. Ohm, C. M. Bunker

Two special tools for recovering gamma-ray probes and logging cable from drillholes have been designed by Ohm and Bunker and constructed by Ohm. Though intended specifically for U. S. Geological Survey equipment, they may be used with other equipment of the same general type. Fishing Tool for Probes: A fishing tool of the overshot type (Fig. 1) was designed to retrieve logging probes (sondes) that become disconnected from the logging cable and are trapped in the drillhole. When the tool slides over the top of the gamma-ray probe, studs on the bottom engage the shoulder near the top of the probe (Fig. 2), which is then pulled to surface. The barrel can be constructed from brass or steel tubing. Wall thickness is not a critical dimension, but the tool should be heavy enough to sink through mud or water in the drillhole. The internal length of the tool must be enough to prevent interference with the upper end of the probe head as the tool slides over it. The design of the probe head used by the USGS required a minimum free space of 2 1/2 in. inside the fishing tool, which was made 7 1/2 in. long to increase the weight. The lower end, which engages the shoulder of the upper end of the probe, contains three studs placed at 120" around the circumference of the tool and held in the engaging position by the tension of a spring wire. The studs can be made of any metal, such as steel, having high tensile strength. As the tool slides over the probe the studs are pushed outward from the center against the spring tension, allowing the tool to slide into position below the shoulder of the probe head. The spring tension forces the studs inward into the engaged position after they pass the shoulder. When the tool is raised the studs stop against the shoulder, preventing the tool from sliding up over the top of the probe. Once it engages the shoulder of the probe it cannot be freed until both probe and fishing equipment are recovered from the drillhole.

Jan 1, 1960

By J. H., R. W. Guard, Westbrook

In 1953 Kornilov and Mints' presented data on thermal expansion and electrical conductivity of the compound Ni3A1 which indicated the possibility of a transformation in Ni3A1 at about 600°C. The present paper gives results of some observations

Jan 1, 1960

By S. H. Moll, R. E. Ogilvie

The investigation of solid-state diffusion phenomena may lead to much information concerning binary alloys. In particular, a study of the concentration gradients present in multiphase diffusion couples can lead to the determination of the solubility limits of the single-phase fields in the phase diagram. The specific concentration gradient which results from the heat treatment of a diffusion couple depends not only upon the time and temperature of diffusion, but also upon the number of phases existing in equilibrium at the diffusion temperature. Such concentration gradients possess sharp discontinuities whose terminal points correspond to the solubilities existing at the limits of the two-phase field in the phase diagram at the diffusion temperature. In general, there will be a discontinuity in the concentration curve for each two-phase field which exists in the phase diagram between the concentration limits of the couple. A number of investigators have analyzed the gradients present in multiphase diffusion couples. 1-8 The iron-titanium phase diagram exhibits a y loop in the temperature range from 900" to 1400°C, and the limit of the a + y field lies at some composition which is less than 1 wt pct Ti for any temperature. It was felt that a diffusion study could yield values not only for the diffusion coefficients involved, but also for the chemical solubilities in the phase diagram. The concentration gradients were analyzed by an X-ray absorption technique developed by Ogilvie.6 The absorption of a monochromatic X-ray beam is measured in steps parallel to the diffusion direction and the resulting intensity gradients are transformed into concentration gradients by applying the laws of X-ray absorption in a binary system. This technique has been applied by ogilvie6 to the systems Ni-Au, Cu-Au, Fe-Cr, and Ni-Cr; by Gelles7 to the systems Be-Fe, and Be-Ni and by Hilliarde to the system Al-Zn. Linear X-Ray Absorption Analysis—The use of X-ray absorption analysis as a tool for determining concentration gradients arises from the fact that the beam is absorbed according to the quantity and species of elements present in the sample and not according to their state of aggregation. This method is more advantageous than the chemical analysis of machined layers since it is less time consuming and less expensive and can analyze a very small area. IF a homogeneous binary alloy (A + B) is analyzed with two different monochromatic X-ray beams I0(2) and lo(2) the following relation between the transmitted intensities, the intrinsic absorption coefficients of A and B for the two different radiations and the weight fraction of each element may be derived.' In (I/Io) (a+b) xa(u/p)a(2) + xb(u/p)8(2) Eq. [1] is independent of specimen thickness and density, but requires that either element A or B possess an absorption edge between the wavelength limits of the two monochromatic beams. I, is evaluated for each radiation by measuring the transmitted intensity through a varying number of foils of a suitable absorber. A plot of the natural logarithm of the transmitted intensity as a function of the number of foils, when extrapolated to zero foils, yields the value of I,. If a plot of the ratio in Eq. [ I] is calculated as a function of xA, then a master curve results. From

Jan 1, 1960

By W. C. Hagel, H. J. Beattie

Variations in the secondary phase reactions of six nickel-and cobalt-base alloys were determined as a function of solu-tioning from 1700" to 2200°F and aging at 1200" to 1800° F for times up to 1000 hr. Room-temperature impact energies and hardnesses were also measured. Precipitation hardening of these alloys results mainly from the grain-interior formation of ? '; M23C6 appears principally as grazn-boundary cells which can be eliminated by intermediate high-temperature aging treatments. Cellular precipitation of ?' occurs up to 1500°F in cobalt-nickel alloys devoid of chromium, where precipitation by this mode can be attributed to a large degree of lattice disvegistery. THE usefulness of nickel- and cobalt-base alloys is dependent on balancing the strength and ductility provided by the solid-solution matrix, dislocation-type subboundaries, grain-boundary phases and genera1 precipitation within individual grains. Since equilibrium relationships for complex austenitic alloys are not easily fixed, a satisfactory balance

Jan 1, 1960

By A. R. Troiano, E. A. Steigerwald, F. W. Schaller

The kinetics of crack propagation in a hydrogenated high-strength steel at subzero temperatures indicated that cracking progressed in a discontinuous fashion. The delayed failure process thus involves a series of crack initiations rather than the continuous growth of a single crack. The incubation time required for the initiation of delayed failure was controlled by the diffusion of hydrogen. The activation energy for the process was 9120 cal per g-alom. As the test temperature was lowered the incubation time constituted a greater percentage of the total tinze to fracture, and al -50°F the incubation and fracture times were essentially coincident resulting in instantaneous, catastroplzic fracture. A unique feature of hydrogen embrittlement is the delayed failure process in which the material fails under the action of a sustained load even though it is capable of supporting a higher load for a finite period of time.')' Delayed failure of steel and titanium is characterized by an incubation time, preceding the initiation of a crack in a highly localized region, and the subsequent growth of the crack to ultimate failure.3-5 The kinetics of crack growth in hydro-genated high-strength steels have been studied through the use of resistance measurements and have an important bearing on the mechanism of delayed failure. Delayed failure is believed to be merely a facet of hydrogen embrittlement in which sufficient time is allowed during a test for hydrogen diffusion. The current theories employed to explain hydrogen em-brittlement can be grouped into two types. one6-8 explains the embrittlement on the basis of the pressure exerted by molecular hdrogen in lattice voids or defects while the other9-10 attributes the embrittlement to the influence of hydrogen in the lattice. The mechanism used to explain the nature of the crack kinetics in delayed failure is based on the stress-induced diffusion of hydrogen to the area of maximum triaxiality.3 When the hydrogen concentration in this region reaches a critical value, a crack is nucleated. This initial crack propagates instantaneously until stopped by the higher fracture stress of the adjacent material of lower hydrogen content. The continuation of cracking must then await the further diffusion of hydrogen to the new region of triaxiality near the base of the crack where another initiation will occur. From this mechanism it follows that crack propagation is nothing more or less than a series of initiations with limited fracture. The purpose of this investigation was to examine the kinetics of crack growth in an effort to determine whether or not the process was discontinuous. Studies of crack propagation were conducted at low temperatures to retard the diffusion of hydrogen which is presumed to be the rate controlling process in delayed failure. MATERIALS AND PROCEDURE Specimen Preparation—A commercial heat of air-craft quality SAE-AISI 4340 steel, designated as Heat G, was furnished by the Republic Steel Co. in the form of %-in. hot-rolled bars. The material had the following chemical analysis: Composition of 4340 Steel—G Heat C Mn Si Ni Cr Mo 0,395pct 0.82pct 0.29pct 1.76pct 0.85pct 0.25pct Notched tensile specimens with less than a 0.001 in. radius, Fig. 1, were used throughout the investigation. The specimens were heat treated to a 230,000 psi strength level according to the following sequence: a) Normalize bar stock at 1650°F for 1 hr, b) Stress relieve at 1200°F for 4 hr and furnace cool,

Jan 1, 1960