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[Univ. of Atabama-University, Alabama-Mining and Metallurgical Society. William L. Mason, Faculty Sponsor; E. C. Wright, Dept. Head. Univ. of Alaska-College, Alaska-Mining Society of the Univ. of Alaska. Douglas W. Huber, Faculty Sponsor; E. H. Beistline, Mining & Metallurgy Dept. Head; Troy L. Pewe, Geology Dept. Head; James Crawford, Chapter Counselor. Univ. of Arizona-Tucson, Arizona-Miners Society. Wiltard C. Lacy, Faculty Sponsor; J. D. Forrester, Mining & Metallurgy Dept. Head; F. W. Galbraith, Geology Dept. Head. Univ. of Catifornia-Berkeley, California-Mineral Technology Association. H. E. Hawkes; Faculty Sponsor; Joseph A: Pask, Dept. Head.]

Jan 1, 1961

By Beverly W. Dunning

The effect of vacuum melting on the elimination of gases and nonmetallic inclusions for six low-alloy steels was investigated. The purpose of these studies was the analysis and comparison of differences in gas content and inclusions in air-melted and vacuum-melted steel. Data obtained from melts of 1-1/4 to 20 pounds indicate that vacuum melting decreases the number and size of nonmetallic inclusions and at the same time increases the degree of dispersion of the remaining inclusions. These improvements are undoubtedly related to the elimination of approximately 80 percent of the nitrogen and 90 percent of the oxygen as well as most of the undesirable metallic trace impurities.

Jan 1, 1961

By Howard W. Wainwright

The Bureau of Mines is engaged in a research program on the characterization of tars produced by low-temperature carbonization of coal and their economical upgrading to more valuable materials, Throughout the years, hydrogenation has played an important role in the treatment of these tars, mainly as a means of converting the whole crude tar or selected fractions to motor fuels; diesel oil, lubricating oil, or various solvents. In some instances, production of specialty chemicals has been the objective. The purpose of this report is to summarize, without critical review, the information of the past 25 years on the hydrogenation of low-temperature tars and related substances as presented in the literature or its English translation. Published articles and patents not abstracted in the main body of this report are included in a bibliography at the end. HYDROGENATION REACTIONS The hydrogenation of tar follows three general types of reactions; 1. The removal of oxygen, sulfur, and nitrogen in the tar to form water, hydrogen sulfide, and ammonia, respectively: [ ]

Jan 1, 1961

By Charles B. Kenaban

The possibility of using ultrasonic energy as a tool to improve the electrolytic deposition of copper and zinc from several electrolytes was investigated by the Federal Bureau of Mines. Sound with frequencies of 20, 26, 38, and 400 kilocycles per second and acoustical intensities of 0.25 to 1.5 watts per square centimeter was employed. Measurements of cell voltage, anode and cathode current efficiencies, and electrode potentials were made at various current densities. Effects of ultrasonics on the quality of the deposit and on anode corrosion also was noted. In the electrolytic recovery of copper from an acid copper sulfate solution at 50° C., adherent, well-consolidated deposits are normally obtained up to a current density of 30 amperes per square foot. As the current density is increased above this value, the deposits normally become progressively more spongy and less adherent. Ultrasonic irradiation resulted in adherent and well-consolidated deposits at current densities up to 300 amperes per square foot. Radiation also produced smaller grain size and preferred orientation of the copper crystals. In addition, radiation caused as much as 3-volt decreases in cell voltages at the higher current densities. These decreases were caused chiefly by depolarization of the anode, although small depolarization effects were also noted at the cathode. Radiation apparently did not greatly affect cathode-current efficiencies, but prevented excessive anode corrosion at the higher current densities and resulted in more uniform corrosion. Ultrasonic radiation at a frequency of 400 kilocycles per second was not as effective as radiation at the lower frequencies. Circulation of the electrolyte at rates up to 5 percent of the cell capacity per minute did not produce results comparable to those effected by ultrasonic radiation. Rapid rotation of the cathode up to 1,800 revolutions per minute gave results approaching those obtained with ultrasonics.

Jan 1, 1961

By F. M. Morris

A large reserve of thick coal in southwest Virginia was developed by Clinch-field Coal Co. in 1957-1958 to produce a nominal rate of 1500 tph raw coal. Operation features coal cleaning in transit. Refuse removed averages 35 pct. Evolution of plant from initial conception to completion is discussed, selection of means applied is explained, and performance to date us design expectation is described. The long-range plan calls for ultimate handling capacity of 40,000 tpd raw coal with anticipated clean coal capacity of 26,000 tpd on a three-shift basis. From a materials handling viewpoint, the Moss No. 3 operation is principally of interest as an ensemble. Generally speaking, it uses time-tested equipment and ideas but some of these are employed on a scale that may be new in the industry. At present about 20,000 tpd of raw coal are being handled. This is expected to increase to 40,000 tpd as soon as business conditions justify it. The purpose of this paper is to discuss the evolution of the plant as to materials handling practices, to describe briefly the equipment and methods used, and to comment on performance in certain areas. The subject divides itself naturally into four phases: 1) operations at the mines, 2) transportation from mines to plant, 3) raw coal handling into the plant, and 4) transportation of refuse away from the plant. OPERATIONS AT THE MINES The coal reserves for Moss 3 are in southwest Virginia where Dickenson, Russell, and Buchanan Counties come together. This area contains about 15 square miles and over 100,000,000 tons of coal. Here the No. 4 (Tiller) and No. 5 (Jawbone) seams of the Norton Formation lie so closely together that for practical purposes, they constitute one seam of coal. This seam, which is called the Thick Tiller, varies from 10 to 18 ft in thickness and underlies Sandy Ridge, a mountain cresting between 2400 and 3300 ft above sea-level. At 18-ft seam height (which is considered to be the maximum practical mining height) the parting between seams will be about 3 1/2 ft thick and each bench of coal will be about 7 ft thick. Depending on the amount of impurities in the seams Drover. total reject in this height coal may approximate 50 pet by wt. It will average about 35 pet for the property as a whole. The first move in developing this resource was made in 1953 when contour maps of several square miles around Duty, Va., including all the known outcrop, were made by photogrammetry. At this time, it was felt the prospective operation would be served by the Clinchfield Railroad and a photogrammetric route survey was made by this railroad from Haysi to Duty. Study of the resulting maps indicated only one site—adversely owned—which might accommodate the size washing plant to be erected. Water resources of a dependable nature seemed nonexistent. In 1954 bulk washability tests were made on the Tiller Bench at the Moss No. 1 preparation plant. The tests indicated this portion of the seam, mined separately, would wash to 4 pet ash with good recovery. Also in 1954, development of Moss No. 2, south of Sandy Ridge, was begun. This mine is in the Tiller Seam where it is about 100 ft below the Jawbone Seam. The reasons for developing a mine in the normal Tiller Seam before tackling the Thick Tiller seemed compelling: Railroad service could be established quickly, communications were better (though not good!), more was known of the seam (it had been mined in the years 1911 to 19241, and there was no essential property to be acquired. After some legal skirmishing, the Norfolk & Western Railroad was granted the right to serve the new mine. Three decades earlier the old mine had been served by the Clinchfield Railroad. The event which triggered active development of Moss 3 was the Appalachian Power Co.'s decision in 1956 to build a 450,000-kva power plant on Clinch River at Carbo. This solved the problem of marketing the steam coal which inevitably must be a product of a mine in the Thick Tiller. Management promptly decided to build the preparation plant at Carbo where an excellent site was owned; where railroad service existed; where telephone service could be obtained; and where roads, bridges, and water supply were tolerable.

Jan 1, 1961

By Willard L. Hunter

The separation of tantalum and columbium by solvent extraction was under-taken as part of the Bureau of Mines research program to improve methods for extracting, separating, and reducing these elements to metal. The diethyl ketone aqueous HCl-HF system was one of several systems studied to determine the effect of metal and acid concentrations in aqueous solutions upon the transfer of tantalum and columbium into selected ketones. The tantalum-columbium oxide mixture used in this investigation was obtained by chemical extraction from Geomines slag. The investigation showed that tantalum 99.4 percent pure and columbium 97.2 percent pure can be produced by the selective transfer of tantalum into diethyl ketone from a solution of 2-N HF and 1-N HC1. The relatively low acid concentration necessary for tantalum transfer and the excellent selectivity of the system recommend its use for the separation of tantalum and columbium.

Jan 1, 1961

By H. J. Heinen

This report summarizes preliminary research studies by the Bureau of Mines in electrowinning molybdenum directly from pure or impure molybdenum trioxide (MoO3) by fused-bath electrolysis in an open graphite cell without need of a protective inert atmosphere. A formulated electrolyte of the tertiary system containing 41.6 percent sodium pyrophosphate, 16.7 percent sodium tetraborat, 33.3 percent sodium chloride, and 8,4 percent molybdenum trioxide, by weight, electrolyzed at 1,000° C,, gave excellent results. Current density studies were made over a range from 20 to 260 amperes per square decimeter. Current efficiencies of 80 to 90 percent were obtained over the entire range. Yields up to 500 grams of molybdenum per kilowatt-hour were obtained. Higher current densities, however, reduced yields and produced a finer grained metal. The two most important facets in electrowinning molybdenum from MoO3, in an open cell, are temperature and electrode spacing to minimize or eliminate the formation of the suboxide MoO2, the major source of oxygen contamination. At temperatures of 1,000° C. and higher, together with the proper spacing of the electrodes, formation of oxides are practically eliminated. Molybdenum metal electrowon from pure MoO3 was 99.9 percent pure and contained 0,056 percent oxygen and 0,007 percent carbon. This metal, when arc-melted, had a Vickers hardness number of 175 and contained 50 parts per million oxygen and less than 10 parts per million carbon. Molybdenum metal electrowon directly from an impure MoO3 containing 90 percent MoO3 resulted in a metal of 99.8 percent purity.

Jan 1, 1961

By John C. Machisak

Injury data and experience, with related employment statistics, at coal mines in the United States for 1959 are presented in this publication under the following general sections: (A) General injury experience: Tables 1 to 6: Current data on number of injuries degree of injury, frequency and severity rates, average severity, and related employment and production data by work location. (B) Selected injury experience: Tables 7 to 38: Current data on principal agencies of injuries, distribution of injuries by part of body injured, days of disability, extent of hand and machine loading, experience by employment and production groups, and various other operating factors and physical conditions related to the occurrence of injuries at the Nation's coal mines.

Jan 1, 1961

Solvent extraction has recently been introduced into Australian hydrometallurgical practice for the production of a high grade uranium concentrate from El Sherana ore by a sulphuric acid leach and solvent extraction process. The solvent is a 5 per cent solution of tri(iso-octyl)amine in kerosene modified with 4 per cent of a long chain alcohol. The stripping reagent is a molar solution of sodium chloride.Preliminary testing for the development of the process showed that the leach liquor was quite amenable to the solvent extraction process and that the equilibrium and rate considerations of both the extraction and stripping steps were very favourable.The industrial plant contains four stages of extraction, three stages of chloride stripping and one stage of secondary carbonate stripping. An internal type of mixer-settler is used for the stagewise contact, the design being based on tests with model equipment.The performance and control of the industrial plant is satisfactory; 99·7 per cent of the uranium is recovered for a loss of 0·3 gallons of kerosene and 0· 4 pounds of amine per 1,000 gallons of liquor treated.INTRODUCTIONThe processing of El Sherana uranium ore from the South Alligator River valley commenced in April, 1959, and thereby introduced into Australian hydrometallurgical practice the unit operation of solvent extraction on an industrial scale. Although there are now some twelve mineral processing plants in the United States and Canada using solvent extraction, its application to the field of primary hydrometallurgy is quite new. Prior to 1956 none of these twelve plants was operating and hydrometallurgical application waslimited to the refining of comparatively high grade uranium compounds and fission products from nitrate and nitric acid solutions.

Jan 1, 1961

By C. Feng

HE sensitivity of twinning in molybdenum alloys containing 20 or more at. pct Re was reported by Dickenson and Richardson&apos; and Sims et a1.&apos; The latter3 also studied the effect of twinning on plastic deformation of these alloys. Recently, in this laboratory, the twinning planes in a series of Mo-Re alloys were successfully identified by tracing their boundaries on two known surfaces of the crystals, with the aid of stereographic projection. The nominal alloy composition and the results of the determination are listed in Table I. Metallic powders of molybdenum and rhenium with 99.9 pct purity were mixed, pressed and arc-melted into buttons under purified argon in a water-cooled copper hearth; the buttons were annealed at 2400 °C in vacuum (10-&apos;mm Hg) for 1 hr, remelted under argon and finally reannealed in vacuum at 2400°C for another hour. This treatment yielded a homogeneous alloy. Large-grain specimens devoid of subgrains were obtained with grain diameter varying from 1/8 to 1/2 in. A typical specimen weighed about 15 g. Orientations were determined by taking X-ray back reflection photographs for each grain on a polished surface of the specimens. Two surfaces were cut and polished; the angle between the two surfaces was measured with an accuracy of *2o. The twins were produced by compression in a hydraulic press at room temperature. Usually, several sets of twins could be obtained within each grain. Except in cases where no twins were formed, (Crystals 7, 8, and 9) the twinning planes were identified consistently as the (112) family over a wide range of alloying compositions and surface orientations of the crystals, as indicated in the stereo-graphic triangle in Fig. 1. The twins, however, were not broad enough to accommodate a conventional X-ray beam and no identification could be made of the twinning direction. Nevertheless, the direction must be one that lies in a plane of symmetry perpendicular to the twinning plane. There are only two such possible planes in a bcc lattice, namely the (110) and the (100) planes. Of these, only the (110) planes are perpendicular to (112), and the <111> direction is the intersection of the two perpendicular planes. It can thus be concluded that <1l1> is the twinning direction. The twinning elements of molybdenum have been reported as the (112) planes and the <111> directions,4 which are also the operative elements in other body-centered-cubic metals, such as W, a-Fe, and ß -brass.5 Thus, the present finding of the twinning elements in Mo- Re alloys supports the concept that twinning formation is mainly governed by the lattice structure. It is of interest to note that for specimens containing 12 at. Pct Re or less, no twins were found after being plastically deformed to as much as 30 pct reduction in height by compression, while for the 35 at. pct Re alloy, twins were formed with less than 1 pct deformation. This, of course, does not exclude the possibilities that for Re-Mo alloys containing 12 pct Re or less, twins could be formed under different conditions, such as at liquid air temperature or under impact loading. The present results, however, suggest that under the same conditions twinning is increasingly sensitive with increasing rhenium content. Consequently, the plastic strain at which twinning starts was found inversely proportional to the amount of rhenium in solid solution with molybdenum. This plastic strain necessary to cause twinning may be used as a criterion in the study of twinning characteristics.

Jan 1, 1961

By Y. L. Yao

A scale based on existing data for the mutual solid solubilities of metals in binary systems has been compiled. This scale is useful for estimating the relative magnitude of two solubilities, provided that these two metals do not form a continuous series of solid solutions. In his classic work on the theory of metallic solid solutions, Hume-Rothery proposed that, other things being equal, a metal of lower valency should be regarded as more likely to dissolve one of higher valency than vice versa. He called this the "relative valency effect". Later he found that the application of this general principle was limited to the three univalent metals: copper, silver, and gold. In dealing with alloys of these metals with metals of higher valency, Hume-Rothery stated, it is usually found that the solid solution of the univalent metal is of the greater extent.&apos; The question of whether there is a systematic trend in comparing the relative magnitude of mutual solubilities, if valency is not considered a criterion, naturally arises. The present paper proposes a "mutual solid solubility" scale on an empirical basis. The order of its arrangement is determined by the relative magnitude of mutual solid solubilities. Some applications of and inferences from this scale are given. ORIGIN AND SCOPE OF THE SCALE An extensive survey of over 400 binary phase diagrams shows that, with certain exceptions and within certain limitations, metals can be arranged in the following order: Na Zn Cd Ga Bi Ge Sb As Hg Sn Si Mg Li Ba In Tl Pb Al Ca Be Mn Cr Re W Mo Cu V Ta Fe Ru Cb Co Ti Hf Ni Os Zr Ir Pt Au U Rh Ce Pd Ag Th so that a metal higher on the scale tends to have a higher solubility in a metal lower on the scale than vice versa. some experimental solubility data are given in Table I. These data, unless otherwise specified, are taken from Hansen and Anderko.6 Throughout this paper, the term "solubility of A in B" is taken to mean the maximum solid solubility of A in B in atomic percent, while the maximum solid solubility of B in A in atomic percent is called "reciprocal solubility". The exceptions found in the above-mentioned survey are: Al-Ag system, 20.34 at. pct Al in Ag, 23.8 Ag in Al; Mg-Pb system, 5.9 Mg in Pb, 7.75 Pb in Mg; As-Sn system, vanishingly small amount of As in Sn, a large As primary solid solution; Cd-Hg system, Cd in Hg <Hg in Cd; Mg-T1 system, 5(?) Mg in ßT1, 15.4 T1 in Mg; W-Ti system, -21 W in ßTi, -25 Ti in W; Zr-Ag system, probably small amount of Zr in Ag, 20 Ag in ßZr.7 Considering the large number of examples, the exceptions are few. It is remarkable that metals may be so arranged without considering other factors such as size, crystal structure, electronic structure, and so forth. A limitation to the use of the scale is the fact that it cannot be tested for two metals forming a continuous series of solid solutions. It is interesting to point out that when the continuous solid solutions have a miscibility gap the critical composition is

Jan 1, 1961

By S. J. Rothman, A. L. Harkness, L. T. Lloyd

Self-diffusion in Y uranium has been measured using U235 as the tracer isotope. The diffusion coefficient fits an Arrhenius-type equation D = 2.33 x 10 -3 exp (- 28,5000/RT) cm2/sec The values of Do and Q are unusually low and are not consistent with the values expected from theories based on a simple vacancy mechanism of diffusion. CYLINDRICAL samples, 1 cm in diam and 1/2 to 1 cm long, were prepared from high-purity uranium containing 0.0343 pct u235, Table I. The samples were water quenched from 690°C (the a-ß transformation is at 668°C) to remove preferred orientation, and annealed at 450 "C to minimize residual stresses. One end of each cylinder was polished on a 1-µ diamond lap and electropolished in a phosphoric acid solution. After a final cleaning by cathodic sputtering, a 1- to 3-µ thick layer of the tracer isotope, uranium containing 93 pct u235, was sputtered onto the sample.&apos; To prevent contamination during the diffusion anneal, the diffusion couples were placed in a tantalum cup and covered with another piece of uranium, and the whole assembly was sealed off in an evacuated quartz tube. Annealing temperatures were constant within +2.0°C. The samples were heated and cooled slowly between room temperature and the ß-? transformation (774°C) in order to minimize distortion of the sample surface that might arise from aniso-tropic thermal expansion and density changes during phase transformations. After machining off 1/16 in. from the radius to

Jan 1, 1961

By Marvin L. Whisman

This report describes the preparation of tritium-labeled organic compounds to be used by the Federal Bureau of Mines in studying the role of certain gasoline constituents in gum-forming mechanisms. The gasoline constituents that have been investigated boil within a range of approximately 90 to 230° C. and can be classified as paraffins. naphthenes, olefins, diolefins, monocyclic aromatics, polycyclic aromatics, and organic sulfur, nitrogen,: and oxygen compounds. The technique of Wilzbach has been applied to more than 50 samples. Purification techniques have been developed that accomplish rapid and effective purification as well as removal of labile tritium in a one-step operation. Data are presented to show the rate of exchange between tritium and hydrogen that can be expected for a variety of compounds common to a full-boiling-range gasoline. These values should be useful to other investigators using tracer programs involving tritium labeled compounds.

Jan 1, 1961

By Robert H. Merrill

Measurement of the deformation of a borehole in rock subjected to a change in applied stress can be used to calculate the magnitude and direction of the applied stress, provided a satisfactory deformation-applied stress relationship exists , In this investigation by the Bureau of Mines the deformation of a bore- hole in a rock model subjected to a known applied stress was compared with the theoretical deformation of a hole in an elastic, isotropic plate and was found to be in good agreement. Hence, this relationship can be used to calculate the applied stress on a borehole from borehole deformation measurements.

Jan 1, 1961

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By H. F. Yancey

Traditionally the Pacific Northwest has relied on hydroelectric power, which has been both abundant and cheap. However, comparatively few hydroelectric sites capable of providing low-cost power remain, therefore the need for supplemental thermal generation, perhaps within the next decade, is generally recognized. Based on the present cost and availability of competing fuels, coal seems to be the logical choice for projected thermal power plants. Power companies and public utilities have become interested in establishing reserves of coal for future use. One deposit explored in 1958-59 lies in southern Thurston and northern Lewis Counties, Wash., near Centralia. Drilling, totaling 22,700 feet, proved the existence of 70 million tons of strippable coal--an ample reserve for the projected power plant. The coal, like most others and particularly those of Washington and Oregon, when mined in full seam section by mechanical methods, would require cleaning to make it suitable for use. The amount and nature of the impurities in this coal dictated a thorough investigation of its cleaning characteristics to establish economic factors and to insure proper preparation-plant design. Therefore, arrangements were made through a cooperative agreement to conduct such work at the Seattle Coal Research Laboratory of the Bureau of Mines. This report describes that investigation. The results are of interest primarily in connection with the utilization of this particular deposit, but some of the information developed is applicable to other deposits of low-rank coals in the West, because the impurities in these coals differ greatly in behavior from those generally associated with the higher rank coals of the Appalachian field.

Jan 1, 1961

By R. T. Johansen

The wettability of petroleum reservoir materials by water and crude oil has been recognized as an important factor in determining waterflood behavior. The problem of simulating and studying reservoir conditions and characteristics, to produce laboratory results congruous with field experience, has been examined by many methods. (1, 2, 3, 4).4/ The most generally accepted approach to this problem is determining wettability of the porous medium by imbibition methods; or, after solvent extraction, predetermining the wettability of the samples by coating the surface of the medium to render it preferentially oil-or water-wet (3, 5). The emphasis of wettability studies has been placed on the characteristics of the reservoir materials with little consideration being given to the fluids themselves. Therefore, the wetting tendencies of crude oils have been investigated by a recently developed method (6). Imbibition and the more general phenomena of capillary pressure are the most direct ways to measure wettability. The simplest type of capillary pressure observations involves the use of an interfacial-tension capillarimeter, which does not produce as separate values either interfacial tension or contact angle. Actually, these quantities do not have independent significance in reservoir engineering, and the property of wettability they are intended to evaluate is given, immediately by capillarimetric measurements.

Jan 1, 1961

By W. Beckering

In characterizing tars obtained by the low-temperature carbonization of North Dakota lignite, infrared spectra have been an invaluable aid in both qualitative and quantitative examination. Quite, early in the tar-research program of the Federal Bureau of Mines it became evident that the small number of published spectra available for hydroxy-aromatics would be inadequate for comparative purposes when dealing with the wide range of compounds present in coal tar; therefore, compiling a catalog of spectra was begun as a continuing part of the tar program. Because these spectra should be valuable to other investigators in this and related fields, they are being presented in these reports. This supplement to the original publications presents the spectra (figs, I to 32), representing 32 compounds, largely phenolic materials. The major problem of this project has been the availability of materials for examination. Most of the compounds included in this supplement were synthesized at the Bureau of Mines Lignite Research Laboratory. Some were obtained from commercial sources, whereas the compound 2&apos;-hydroxy-l-phenylnaphthalene was synthesized at the Bureau of Mines laboratory in Bruceton, Pa. The spectrum of 2-ethyl-4-methylphenol, figure 32, is a correction of the spectrum presented as figure 26 in the original reports

Jan 1, 1961

By Alla D. Mah

Relatively pure aluminum nitride (AIN) recently has been prepared in sufficiently large amounts to permit a variety of experimental studies.4/ Several mechanical and chemical properties have been investigated, which show that this substance has good potentialities as a container for liquid aluminum, gallium, and boric oxide. The present work by the Bureau of Mines was undertaken to obtain thermo-dynamic data pertinent to the calculations regarding thermal stability and reactivity of aluminum nitride. The following measurements were made: (1) determination of the heat of formation from the elements at 298.15° K.; (2) determinations of the heat capacity over the temperature range 51° to 298.15° K. and the evaluation of the entropy at 298.15° K. therefrom; and (3) determinations of the heat content over the temperature range 298.15° to 1,800° K. These data are combined to obtain free energies of formation from the elements between 298.15° and 2,000° K.

Jan 1, 1961

By R. J. Charles, G. Agar

Experiments on single particles show that the amount of material created during impact that is finer than any chosen size is proportional to the energy of the impact. As the underlying principle of comminution, it might be stated that each unit of energy input to a given comminution system tends to add to the system an identical assembly of new particles and subtract an equivalent volume of larger particles. Thus, two of the consequences of the fact that each unit of energy tends to add identical assemblies of new particles to the system are: 1) on continued application of energy the total charge in any batch comminution system tends to assume the characteristics of this assembly, and 2) the process of comminution may be described by a relationship such as E = Ak-a. Recently Schuhmannl presented a theory of comminution which puts rational perspective on the extensive controversy surrounding most of the existent theories of comminution. With hindsight the origin of controversy can be ascribed to a relatively simple circumstance. In general, a progressive shift of a size distribution curve towards finer sizes is observed as energy is added to a comminution system. It is also observed that, with continued grinding, the size distribution curves usually change and appear to approach some constant shape. Inves-tigators generally felt that an appropriate method of relating and generalizing such data would be to consider the hypothetical case where particles in the system were uniformly subjected to comminution such that each of these particles, receiving its proportion of input energy, was transformed into a number of smaller particles of uniform size. Since the changes in shape of the size distribution curves during size reduction were clearly associated with the coarse particles in the system, it was also assumed that these changes accounted for little of the input energy and one could deal solely with the equilibrium shape towards which the size distribution curves tended. Although the unrealistic nature of the foregoing points of view was realized some justification was felt for such treatments since, in most cases, the resulting mathematical formulae could, by the adjustment of at most two parameters, satisfactorily describe experimental observation. Difficulties arose, however, in that the formulae required a specific influence of the feed size on the comminution process. In actual fact, the application of a feed size term in fitting experimental data was often found to be unnecessary or contrary to the above formulae. Secondarily, much discussion arose concerning the appropriate energy number that would relate the size change of one particle to the amount of comminution energy it received. As has been previously shown3 all the above theories that treat comminution as a continuous process of size reduction may be related to a proposition of the following form: dE = -Cfn [1] where dE is the increment of energy, dx is the size change, x is the particle size, and C and n are constants. It is now clear, as pointed out by Schuhmann, that Eq. 1 is inapplicable to comminution processes, since comminution cannot be considered other than as a discontinuous mixing process in which the overall size distribution of the product results from mixing, in various proportions, finished material with unfinished, and sometimes untouched, material. A striking illustration of this mixing phenomena may be obtained by comparing the size distributions of grinds in a typical batch ball mill with size distributions calculated on the basis of mixing various proportions of feed material with a ground material which obeys a power law size distribution relationship. Figs. la and lb illustrate such a comparison and the similarity of these figures indicates that mixing plays an important role in determining the overall shape of the product size distributions. Figs. la and lb illustrate, additionally, the underlying basis of the comminution theory presented by Schuhmann.&apos; In the preliminary grinding of relatively close sized feed particles in a batch ball mill, one may visualize that, when a successful encounter of a ball with a feed particle occurs, then the particle undergoes severe size reduction and the size range in which the resultant particles reside is far removed from the size of the feed particles. After a number of feed particles are reduced by independent but similar impacts and one examines the size dis-

Jan 1, 1961