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By R. W. Smith, K. H. Lee

Bond type simulated closed-circuit grindability tests and batch grindability tests were run on six pure minerals plus a limestone and a taconite ore. The simulated closed-circuit tests were made at five different meshes of grind. The minerals tested varied widely in hardness and breakage pattern. For all simulated closed-circuit tests both Bond and Holmes work indices were calculated and compared. The Bond grindability testlm6 has been widely and quite successfully used for predictions of such items as ball mill power requirements and as an aid in plant comminution equipment selection. The test is interesting in that although run as a series of batch tests it is over-all a simulated closed-circuit test with a circulating load of 250%. The simulated closed-circuit feature is probably the primary reason for the notable success of the test. Perhaps the major criticism that can be brought against the test is that it is time consuming, since it normally takes a trained technician about an eight-hour shift to perform it.4 For many purposes this is an acceptable time requirement. However, if a grindability test is to be used for mill control purposes it should be performed in as short a time interval as possible, preferably under an hour. Sometimes in industry strictly batch tumbling mill tests are run and an attempt is made to correlate such batch tests with plant mill operation. Then an attempt is made to adjust operating tumbling mills based on data from the tests. The tests, however, frequently do not correlate well with operating data. The purpose of the present work was to explore some of the similarities and differences between a simulated closed-circui.t grindability test and a batch type test. Six different minerals plus a limestone and a taconite ore were tested in the experimentation. These materials varied widely in hardness, breakage characteristics, etc. Standard dry Bond grindability tests were mn on all materials at 48, 65, 100, 150 and 200 meshes of grind. Feed material was prepared by stage cmshing to -6 mesh. Initial feed volume was 700 cc. Care was taken to maintain the standard constant weight (about 20125 gm) and number of balls (283) during all the tests. Rotational speed was 70 rpm. Table I lists the materials studied along with pertinent data regarding the materials and Bond grindabilities obtained. In addition, dry batch tests were performed on all materials. These tests were made in the same mill as was used for the Bond tests. An identical ball charge and an identical feed volume were used. After rotating the mill for a predetermined number of revolutions at the same rotational speed as for the Bond test, the material was removed and separated from the ball charge. A screen analysis was performed on this product. Knowing the original size distribution of the feed and the size distribution of the product, it was possible to calculate the grindability or grams of a particular mesh produced per revolution of the mill. After the screen analysis of the product, the various fractions were recombined and placed back in the mill for further grinding. After grinding for additional revolutions of the mill the procedure was repeated. Thus, it was possible to obtain grindabilities for each material at a number of meshes of grind and for various revolutions of the mill. Grind-abilities obtained from batch tests are shown in Table 11. COMPARISON OF BOND AND BATCH GRINDABILITIES Figs. 1A through 1D show relationships between batch and Bond grindabilities. Figs. lA, lB, 1C and 1D show respectively graphs indicating the relationships for batch tests run for 100, 300, 500 and 700 revolutions of the mill. For a particular material on each graph, points are shown for 200, 150, 100, 65, and 48 meshes of grind except for several missing coarse meshes of grind for galena which did not fall conveniently on the figures. For each material and graph the point nearest the origin is for 200 mesh, the next for 150 mesh, the next for 100 mesh, etc. Considering Fig. lA, it is interesting to note that all relationships shown are essentially straight lines. There are, however, considerable differences

Jan 1, 1969

By George F. Comstock

It has been known for many years that the alloy containing 90 per cent. copper and 10 per cent. aluminum can be hardened, like steel, by quenching from a suitable temperature, and that the hardened alloy can be softened again by annealing or drawing the temper. It does not seem to be generally appreciated, however, that the effect of the first slight reheating after quenching is actually increased hardness, the softening effect not taking place until a certain temperature of "drawing" has been exceeded. This paper gives the results of a few experiments on various specimens of cast 10 per cent. aluminum bronze, quenched for maximum hardness, and subsequcntly annealed at different temperatures. The hardness measurements were made with both a scleroscope and a standard Swedish Brinell machine; some peculiarities of the scleroscope test on this material are described. The author is not aware of many previous investigations of the hardness of this alloy when quenched and drawn, but two important papers on the subject should be mentioned. The earliest was by Portevin and Arnou,1 in which it was stated that tempering quenched 10 per cent. aluminum bronze at 400" C. increased the hardness as compared with the quenched untempered alloy and that reheating above that temperature ' was necessary to obtain any softening effect. A later paper was by Seidell and Horvitz,2 who mentioned Portevin and Arnou's work, but did not report any increase in hardness obtained

Jan 1, 1925

By A. N. Mitinsky

Discussion of the paper of A. N. MITINSKY, presented at the San Francisco meeting, September, 1915, and printed in Bulletin No. 104, August, 1915, pp. 1697 to 1705. LAWFORD H. FRY, Burnham, Pa. (communication to the Secretary*). -The author assumes that the proportional limit and the elastic limit are coincident or very nearly so, and then further assumes that the stress corresponding to these two points is the least stress which if repeated will cause failure. The point is extremely interesting and it is to be regretted that the author did not quote experimental data to show the relation between the limit of repeated stress and the other properties of the material. The author's suggestion that a steel of poor quality may have a normal value for the yield point and tensile strength (see Fig. 2) and an abnormally low elastic limit, and that this will correspond to a low resistance to repeated stress, may account for a number of failures of axles in which the tensile tests show normal physical properties. If so and if a determination of the proportional limit would have eliminated the material before it was put into service, this determination will merit most earnest attention. It appears, however, that considerable further research is necessary before any definite conclusion as to the quality of a steel can be drawn from its proportional limit. Mr. Mitinsky's paper is extremely interesting and if it stimulates thought and work along the lines indicated, it may prove of considerable practical benefit. H. V. WILLE, Philadelphia, Pa.-The paper discusses the difference between the proportional limit, or elastic limit, and the yield point, and refers to the fact that much harm results from confusion of the terms yield point and elastic limit. Similar confusion has arisen in this country; the American-Society for Testing Materials does not even consider the elastic limit and proportional limit to be identical and recently adopted the following definitions:

Jan 12, 1915

By W. C. Lilliendahl, H. W. Highriter

THE method developed and used in this laboratory for the production of metallic uranium of such purity that it is ductile and can be cold-worked to fine wire or thin sheet by rolling has already been described1. It consists, briefly, in the electrolysis of potassium uranous fluoride (KUF6) in a molten bath composed of equal parts of sodium and calcium chlorides. The bath is contained in a graphite crucible, electrically heated to about 775° C., the crucible serving as the anode for electrolysis. The uranium deposits in finely divided form mixed with salts upon a molybdenum cathode suspended axially in the crucible. Upon completion of the electrolysis the cathode is removed and cooled, the deposit broken and leached to remove salts. The metal powder is washed with water and dilute acetic acid and dried in vacuo to reduce oxidation. Suitable amounts are then pressed into pellets and heated in vacuo by high-frequency induction, using a thoria crucible. The uranium melts and flows away from the pellet, leaving a shell, which is largely oxide. In general, this method produced a satisfactory metal, although at times the uranium was not ductile. The investigations recorded here were made to find the cause of this embrittlement. It was known that the metal generally contained carbon, derived from disintegration of the graphite crucible in which electrolysis is conducted, in amounts dependent upon the thoroughness of washing the metal powder. Accordingly, analyses of several samples, both ductile and brittle, were made by combustion and absorption of CO2 in Ascarite, using air instead of oxygen to reduce the temperature and rate of oxidation. Several of these metals were made with special precautions to reduce carbon content. The results show no relationship between ductility and carbon content in the range investigated (Table 1).

Jan 1, 1935

By Douglas A. Sloan

Who would believe that young elementary school children could understand something as complex as the mining industry? The Challenge The challenge of accomplishing this is tremendous. An examination of Canadian school children indicated that they knew very little about the world of work in general, and hardly anything about the mineral resource industry in particular. It calls to mind the story about two youngsters who decided to play house. The little girl played her role well as she went about the house doing things she had watched her mother do every day. When it was the little boy's turn, he grabbed his lunch, waved goodbye to his "wife," jumped on his bicycle and pedalled furiously down to the end of the driveway-where he stopped. The youngster explained that he saw his dad go out of the driveway each morning, but he didn't know where he went, or what he did on the job. When you stop to consider the number of families today with two working parents, you can begin to appreciate the importance of the opportunities for role identity provided by this project. The Approach The challenge of teaching the school children of Canada about the world of work and, specifically, the mining industry is the challenge which the Canadian Institute of Mining and Metallurgy met with the Curriculum Development Research project. It started when a small, dedicated group of Vancouver members met Dr. Doreen Binnington. After this meeting, Dr. Binnington, an expert in curriculum development at the University of British Columbia, set herself to develop a curriculum program for the elementary shcools which accomplishes two main goals: It uses the "Identity Approach," developed by Dr. Binnington, an expert in curriculum development at the enable students to understand and appreciate the contribution of people, in this case, working with mineral resources. It has pupils enthusiastically exploring the importance of rocks, minerals, and the mining industry in their lives [(Fig. 1)]. Evolution of the Curriculum Development Research Project When the curriculum development research project was presented to the Vancouver Branch of the Canadian Institute of

Jan 1, 1981

By Eugene A. Stephenson

The writer apologizes for presenting this very elementary analysis of one aspect of proration, but a search of the literature failed to disclose any concrete illustrations of the effect of various proration formulas upon the allowable oil produced by tracts of different sizes. Many engineers have doubtless made somewhat similar calculations and are fully acquainted with the results. The various allocation formulas that are in use are based on one or more of the following factors: (1) wide-open well potential, (2) potential through an orifice, (3) uniform well allowable, (4) acreage, (5) sand thickness, (6) bottom-hole pressure, (7) productivity index, and (8) volumetric displacement. Of these, the unrestricted potential formula, or open-flow test, and the uniform well allowable are commonly regarded by engineers as those least likely to give each producer his proportionate share of the oil or gas, as represented either by acreage or by sand thickness, or both, except when the wells are located on tracts of large size. Unless the mechanical equipment that may be used during the potential test and the method of taking the test are both specified, the net result of the potential formula is to practically force the operators to use special equipment and adopt special procedures prior to and during the potential test, so as to secure the largest possible allowables. Much ingenuity and skill have been devoted to this,problem, but the general effect is to permit excessive allowables for very small tracts, and stimulate unnecessary drilling. It is interesting to compare some of the high yields from the Wilcox horizon at Oklahoma City with each other, as an illustration of the effect of an allocation factor based solely on potential (Table 5). One of the glaring instances is a well on a ½-acre lease, which had produced, as of September 1936, at the rate of almost 3,000,000 bbl. per acre. This is at least twice as many barrels as could have been present under the property if the reservoir had consisted of a tank of oil 200 ft, deep and 56 acre in area. Numerous combinations of acreage, potential, bottom-hole pressure, sand thickness, etc., have been proposed and are in use in various fields.

Jan 1, 1937

By Wallace Ralston

The East Texas area includes the northeast 38 counties of the state of Texas. It covers all, and extends beyond, the borders of what is commonly described as the East Texas Basin. It is one of the most important oil and gas-producing areas of the Mid-Continent Province. It includes four important oil fields—Van, East Texas, Cayuga and Long Lake— and the recent extension of Rodessa field into Cass County, Texas, may prove to be of major size. Four commercial gas fields are in this area— Bethany, Waskom, Cayuga and Long Lake. Up to January, 1936, all of the oil has been produced from the Upper Cretaceous formations, and most of that from the basal member, the Woodbine sand. Gas is produced from both the Upper and Lower Cretaceous formations. Development in Fields East Texas Field.—This field continued to dominate the drilling and production situation throughout the United States. There were 4036 wells completed in this field during 1935; that is, 365 more wells than were completed during 1934. Drilling activity was due to close spacing of wells and the addition of 10,000 acres to the field. The field is now drilled to a density of one well to 6½ acres, which is certainly more wells than necessary for economic production of the field. The close spacing of wells is due mostly to the type of proration, which is per well allowable based on a potential test, and does not take acreage into consideration, and also to the numerous small acreage tracts such as town lots and excess strips. The field now has 19,519 producing wells. The allowable production for the field during 1935 was 161,118,659 bbl.; estimated production, including illegal or "hot oil," was 174,200,150. The illegal production of oil gradually decreased throughout the year, until an estimated low was reached of 20,500 bbl. daily during the months of November and December. The price of oil remained at $1.00 per barrel throughout the year. As stated, about 10,000 acres were added to the field during the year, making a total of 128,000 productive acres. There is a possibility that

Jan 1, 1936

By Robert Adams

Secondary or scrap materials appear at all stages in the industrial process and in a bewildering variety of forms, grades, and values. It is useful to begin analyzing them by dividing the broad concept of "Secondary Supply" into three parts First, the concept must encompass the stock, or pool, of secondary materials. In the process of satisfying his wants, man produces desired products from the materials and natural resources found around him. As long as the rate of production is greater than the rate of obsolescence of a given product, the total stock or pool of materials embodied in that product will increase in size This stock concept relating to secondary materials is directly analogous to the "resource" concept used for primary raw materials in the preceding chapter, and includes all materials embodied in existing products (Obviously, this excludes those materials which are destroyed in the consumption process, viz , fuel oil burned to provide heat.) Consumption of a primary material in a productive process tends to reduce the resource base of that primary material In direct contrast, however, the production or use of products increases the resource base of the secondary material. Thus, we find that a country which has no resource of a primary material can, by importing products that contain the material, build up a large enough stock to provide a basis for secondary recovery. The estimated growth of the pool of copper in use in the United States through 1967 is shown in Table 5.B.1.a The estimate of 39 3 million tons at the end of 1967 includes only technologically recoverable copper and is, therefore, somewhat less than the stock concept described previously, which does not distinguish between recoverable and unrecoverable material. Nevertheless, Table 5 B.1 does give an idea of how a nation's secondary resource of a material can grow over the years. A second aspect of the concept of secondary supply is the generation of secondary materials. This includes materials generated as scrap in production as well as the movement of a material out of the stock of existing products via wear, damage, or obsolescence The quantity of materials generated is usually either nearly or completely independent of the technologic capabilities and economic forces which prevail in the secondary recovery market.b The justifications for and the qualifications to this statement are considered later. The final aspect of the concept of secondary supply consists in the secondary recovery process It is at this point that the technologic and economic forces of the secondary recovery market become the controlling fac-

Jan 1, 1976

By Roscoe C. Clark

In a previous technical note' by Walter Rose, evidence is offered in support of the contention that "the possibility of describing oil recovery features in terms of capillary pressure phenomena has not been established entirely." It is not the purpose of this note to present further discussion of this possibility but rather to point out that the argument presented there does not appear to be generally valid. In the cited note' reference is made to the experiments of Welge2 wherein it was shown that when water was displaced by oil from a core the pressure in the water phase was less than in the oil phase but that when this oil was then produced by water drive the pressure in the water phase was greater than in the oil phase. Rose has concluded from these observations that conditions of static equilibrium did not obtain since the fluid saturations were such that phase discontinuities seemed unlikely. The argument from which this conclusion was drawn is based on the contention that "the pressure is always greatest in the non-wetting phase at each static interstitial interface of contact with the wetting phase." This premise appears to have been reached from a consideration of capillary phenomena in cylindrical tubes, although it may a1so hold for other types of pore geometry, hut as will be shown below it does not hold for all pore shapes and hence is not generally applicable. Since the pore structure of porous media such as reservoir rocks i- in general so complex as to defy exact description. it is undoubtedly of great value to establish a model in terms of pore shapes of known geometry, provided of course that the limitations of the model are recognized. That the limitations of the capillary. or cylindrical, tube model have not always been fully recognized will be evident from the following discussion of a pore of different shape hut one which may a. logically he considered a.; the capillary tube. The pore space to be considered is that shown in Fig. 1, which may be thought of as the "hole in a doughnut."* Consider the interface, A-B-A', between two immiscible fluids, P, and P2, which interface meets the solid alone a line, A-C.A'-C'. The interface A-B-A' is the surface of a spherical segmen† while the line of mutual contact be-

Jan 1, 1950

By Arthur F. Taggart

In 1900, Elmore found that if an acidulated pulp was stirred up with an oil which was relatively insoluble in and lighter than water, and the mixture was allowed to stratify, much of the sulfide would be found hanging to the lower surface of the floating body of oil and could be skimmed off or overflowed with it. The action of the flotation agent here is twofold, first to select the sulfide from the gangue—what today is called collection—and second, to buoy the collected sulfide away from the gangue. The action in collecting is illustrated by Fig. 1: which contrasts the behavior of drops of oil brought, under water, to the surfaces of gangue and sulfide particles, respectively. The oil displaces water from the surface of the sulfide; the water displaces oil from the gangue surface. If, instead of considering the solid particles the fixed parts of the system of oil, water and solids. we consider the oil and water fixed and the solids presented to the surface of contact, the condition will be as shown in Fig. 2; the sulfide tends to be drawn into the interface and the gangue to be excluded. The sulfide particles are held in the oil-water surface by the tension of this surface. The buoyant effect is supplied by the oil droplets in bringing the sulfides to the water surface, but not in holding them there. Gas as Buoyant Medium of Flotation In 1906 Sulman. Picard and Ballot discovered a practical and substantially fool-proof method of doing what Everson, in 1886, and Fro-nlcnt. DeBavay Bessel and Elmore had been doing in the intervening years, viz.: using gas in place of oil as the buoyant medium for flotation, but retaining oil as the agent. To all of these inventors "oil," with no qualification as to its kind and no true understanding of its function, was the important thing. Hut they placed on the oil an additional burden viz.: froth-making, and it soon became apparent that not all oils were suitable for the dual purpose. As a matter of fact, it is probable that each of these inventors knew only one suitable oil at the time he wrote his patent, but used the generic term in the patent with the usual idea

Jan 1, 1928

By L. W. Page

PREVIOUS to the introduction of the motor vehicle the broken stone or macadam road met the conditions of rural horse-drawn traffic better than any other type of road, but under fast motor traffic it has been proved to be quite unsatisfactory, and necessitates high maintenance charges. Such a road depends for its success upon the fact that the rock dust fills the voids between the stones and acts as a cement or binder. Under ideal conditions it should be constructed of rock so suited to the volume and character of horse traffic that only enough fine dust is worn from the stones of which the road is composed to take the place of that carried off by wind and rain; and when these conditions are met, the fine dust resulting from the wear. of traffic forms with the stone a smooth, impervious shell, shedding the surface water and protecting the foundation. With increase in the number and speed of motor vehicles, however, it was soon found that the cost of maintenance also increased, until at the present day highway engineers consider the old method of constructing and maintaining broken-stone roads increasingly inadequate, and are introducing every known type of binding material other than rock dust to cement the stone together. Among the most prominent types of products in use are those produced from our various petroleums. That the value of modern methods of road preservation was appre¬ciated in this country much earlier than we have been accustomed to believe is demonstrated by the recent revival of an old patent which was granted to one John Martineau, of Elbridge, N. Y., in 1834. Petroleum had, of course, not been discovered at that time, but he claims as his invention and improvement "The application of tar, turpentine, or any of that class of tenacious, cohesive substances, reduced before use to a fluid state, and that state used as a cement, to apply to, and combine with sand, gravel, pebbles, and pulverized stone, such as is used for a Mc-Adam road, or cobble stone, the interstices of coarser material being in all cases filled, as well as may be, with sand and gravel and cemented with tar or turpentine, to form the wearing face or surface of streets,

Jan 2, 1914

By W. L. Fink, H. C. Stumpf, L. A. Willey

VERY few studies of the aluminum-sodium system have been reported. Heycock and Neville1 were unable to detect any solubility of sodium in liquid aluminum. Mathewson2 prepared an equilibrium diagram consisting of two horizontal lines at the melting points of the two metals. He was unable to detect solubility at either end of the system. Scheuer3 first developed a method for the chemical determination of sodium in aluminum and then studied the solubility of sodium in liquid aluminum. His method involved heating aluminum with excess sodium under hydrogen until the two liquids were at equilibrium, chilling the melt, and analyzing the aluminum-rich layer. He reported the solubility to be 0.l0 pct sodium at 700°C, 0.115 pct at 750°C, and 0.128 pct at 800°C. This paper on the aluminum-sodium system is the twenty-first in a series from the Aluminum Research Laboratories describing equilibrium relations in aluminum alloy systems. MATERIALS The alloys for this investigation were prepared from electrolytically refined aluminum (99.99 pct) and sodium of reagent quality conforming to specifications of the American Chemical Society.4 Chemical analysis of the aluminum showed the following impurities: 0.002 pct Si, 0.002 pct Fe, 0.002 pct Cu, <0.001 pct Mn, 0.002 pct Mg and 0.001 pct Na. The sodium content of all alloys was determined by either chemical or spectrographic standard procedures5 No. IIA and No. SII respectively. DETERMINATION OF LIQUIDUS The boundary of the miscibility gap was determined by a modification of the method of Scheuer3 and of that used by Henry and Cordiano.6 As finally developed the method was as follows: A fused alumina crucible 25 mm id with 75 mm depth and 1.5 mm wall thickness was placed on the bottom of a container made from a 4-in. length of 1 ½ -in. iron pipe and pipe caps. The space around the sides of the crucible was filled with 40 mesh crystalline alundum. A charge of 60 g of aluminum and 10 to 15 g of sodium was placed in the crucible, the sodium first being trimmed and rinsed with iso-pentane to remove kerosene. The container was tightly capped, filled with argon (99.6 pct pure), and heated to the desired temperature (between 670 and 800°C). A positive pressure of argon (about 8 mm of mercury) was maintained through a small pipe to the upper cap. After soaking for from 2 to 5 hr, the container was quenched by directing a stream of water onto the base, so that solidification of the aluminum-rich layer was rapid and essentially unidirectional. Analyses were made on drillings taken from the bottom of the ingots after machining off the surface layers. Pre-

Jan 1, 1948

By H. K. Work, G. H. Enzian

In the manufacture of steel for commercial purposes, the deoxidation practice used, i.e., the method and degree of deoxidation, is an important factor affecting the structure and mechanical properties of the finished steel. Deoxidation practice exerts a pronounced influence not only on the soundness of the ingots but also on the reaction of the steel to a number of mechanical and thermal treatments. The first mentioned effect of deoxidation is more or less obvious and was first demonstrated, though perhaps not fully appreciated, by Robert Mushet when, in 1856, he added speigeleisen to low-carbon bessemer blown metal. In 1861. Bessemer patented the addition of one pound per ton of silicon to his blown metal to "cause the metal to lie quietly in the mold." The second effect of deoxidation-—that is, the effect on the properties and behavior of the steel—is, one might say, more subtle, and certainly not as well understood as the first, although in many cases it is the more important consideration. This paper is limited to a discussion of only the second effect of deoxidation and: in particular, to the effect on the strain-sensitivity of low-carbon steels. General Discussion Originally it was thought that the function of a deoxidizer was to combine with the oxygen present in the steel as iron oxide and prevent its subsequent evolution as a gas. -More recently it has been realized that a deoxidizer does more than this. Frequent reference has been made to the effect of deoxidizers on the nitrogen in the steel, and some attention has also been paid to hydrogen. As a consequence of the above situation any study of deoxidation must be concerned with the gas content of the steel and the effect of the deoxidizer on the gases involved. The term "gas content" as used here refers to gases extracted from steel during melting in vacuum rather than to elements present in steel in the gaseous state. The extracted gases, at least in the case of oxygen and nitrogen, are generally accepted to be products of decomposition of oxides, nitrides, or other more complex compounds. The manner in which deoxidation affects the gas content of steel and the significance of gases in steel have been and still are subjects of considerable speculation. No attempt will be made here to give a complete discussion of the literature on this subject but a few references will be cited for purposes of illustration. N. Hamilton1 found a correlation between the oxygen content of alloy steel and the behavior of the steel during tube piercing. Davenport, Bain, and others associated oxygen with aging properties of steel while Köster5 and a number of others6-lo made similar claims for nitrogen. Daniloff, Mehl, and Hertyll stated that "deoxidation decreases the susceptibility of steels to aging directly

Jan 1, 1945

By E. S. Greiner

STUDY of the plasticity of germanium or other semiconductor crystals affords unusual opportunities to extend our knowledge of deformation mechanisms. Crystals are available having extraordinary perfection and very high purity. They deform by slip on the systems {111} <110>,1-3 as do crystals of the simple face-centered-cubic structure. Dislocations generated in them during slip are easily revealed in the form of etch pits on either (111) or (100) surfaces.4,5 This fact alone makes possible more detailed studies of mechanisms than is usually the case with metals but, even further, the effect of deformation on their electrical conductivity is very large compared with metals. This comes about not only because the mobility of the charge carriers is reduced, as in deformed metals, but also because the number of these carriers is greatly altered. This latter effect seems closely related to the formation of both line and point imperfections during deformation and thus provides a needed tool for the study of the kinds and distributions of these imperfections. Other investigators have deformed germanium at elevated temperatures by bending,1, 6-8 compres-sion,6, 0,10 tension,2,3,6,11,12 torsion,23 and indentation." Wang and Alexander" have also reported successful indentation at room temperature. Dislocation etch pits consequent to deformation have been observed and studied.7,8,10,18,14,20 The experiments to be de- scribed here include principally the compression and the subsequent annealing of germanium with concomitant studies of etch pits, microstructures, and electrical properties. Both single crystals and heavily twinned specimens were used. Some indentation studies are included. Experimental Methods Plastic compression was effected in the apparatus shown schematically in Fig. 1. It consists of two tantalum platens contained in a helium atmosphere and so arranged that pressure can be applied by a hydraulic press. The specimen between the platens is heated by the surrounding furnace. The specimen is usually a small crystal cube about 0.30 in. on an edge. A control specimen is always inserted so, that it is subject to the same thermal cycle as the one being deformed. This serves to detect any impurity contamination that might accompany the thermal treatment. For high temperature work, where such impurity contamination often occurs, the specimens were first plated with gold whenever subsequent electrical properties were to be determined. This method" is effective in preventing significant contamination of germanium up to temperatures at least as high as 750°C, as evidenced by the constancy of the electrical conductivities of control specimens subjected to the same heat treatments. The total range of temperature used for deformation was from 375°C, the lowest at which significant flow was observed, up to 900°C. Microscopic examination was made after mechanical and chemical polishing and etching. Dislocation pits were revealed with CP-4 etchant by the tech-

Jan 1, 1958

By Allan T. Gwathmey, J. Bruce Wagner, Kenneth R. Lawless

Between 250°and 550°C in oxygen pressures of 10 to 760 mm Hg, the relative oxide thicknesses formed per unit time on the (100), (111), (110), and (320), decreased in this order. The predominant oxide orientation was (001)Fe3O4 and [110] Fe304 A small amount of a-Fe2O3 which exhibited a fiber pattern was observed in all oxides except those formed at 250°c in low oxygen pressures. IN order to understand the properties and behavior of thin films, particularly their role in oxidation reactions, there is needed more experimental information on their structure, composition, and kinetics of formation on clean surfaces of known geometry. The present study was undertaken to obtain such information for thin oxide films formed on single crystals of a body centered cubic metal, iron. Crystals in the form of spheres were used in order to expose all possible crystal planes to the reactant gases simultaneously. Using this procedure the relative rates of oxidation of all planes could be estimated, and those exhibiting, maximum or minimum oxidation rates could be selected for a more intensive study of composition and expitaxy. Since the three types of information were obtained from the same experiment using a single crystal substrate, any differences between rate, composition, and expitaxy on the several planes may be attributed to the influence of the substrate structure. EXPERIMENTAL The starting material for this study was Armco iron rods, 6 in. long and 3/8 or 1/2 in. in diam. The analysis was reported to be 99.8 pct Fe, with major impurities listed as carbon 0.018 pct, manganese 0.027 pct, phosphorous 0.005 pct, sulfur 0.029 pct, silicon 0.005 pct, and copper 0.11 pct. These rods were cleaned with ether and heated in an atmosphere of moist hydrogen at 950°C for three days. The purpose of this treatment was to decarburize the iron and to provide a consistent, uniform grain size for the growth of single crystals. Crystals in the form of rods, up to 1/2 in. in diam and 2 in. long, were prepared by a method similar to that reported by Leidheiser and Buck.2 Spherical crystals, 3/8 and 1/2 in. in diam and having a handle about 1/4 in. in diam by 112 in. long, were machined from the single-crystal rods. After machining, each crystal was etched in aqueous nitric acid to remove the cold-worked metal at the surface. Before each experiment, the crystal was polished mechanically with metallographic papers through number 4/0, and electropolished in a perchloric acid-acetic anhydride mixture by the method of Jacquet and Rocquet.3 The crystal was washed in running distilled water for at least 5 min. The excess water was blotted with a soft paper tissue, and the crystal was placed in an all-glass reaction vessel (See Fig. 1). The crystal was heated at 550°C in hydrogen for at least 8 hr prior to the oxidation in order to reduce any surface oxides and to help relieve any stresses in the metal. For the structure and composition studies, flat faces were cut parallel to (loo), (111), and (110) planes on the iron crystal spheres. The orientation of these faces was checked by a back-reflection X-ray diffraction technique. The faces were within 2 deg of the desired orientation. The flat faces were treated as described above except that prior to electropolishing they were given an additional polish on metallographic felt saturated with twenty-minute levigated alumina. After the crystal was heated in hydrogen for at least 8 hr, the temperature was adjusted to the desired value, and the hydrogen was evacuated. Commercial oxygen which had been purified by successively passing through tubes containing magnesium perchlorate, Ascarite and magnesium perchlorate was admitted to the desired pressure as measured by a mercury manometer. A resistance-wound furnace surrounded the oxidation chamber, and a temperature controller maintained the temperature within ±3°C. The furnace was provided with a small window for observing the crystal. The changes in thickness of the oxide films were followed by observing the interference colors. The oxidation was allowed to proceed until the desired oxide thickness was attained on a given crystal plane. The experiment was terminated by evacuating the oxidation

Jan 1, 1962

By Barbara A. Thompson

A previously reported high-resolution method for the location of boron-rich areas in metallurgical and biological specimens was been adapted for general use on a routine basis. The rnetlzod utilizes neutron activation and autoradiograpizy. Alpha-particles emitted by boron nuclei upon neutron capture are recorded on a photographic emulsion. The resulting a-particle tracks show the location of boron-rich areas. Experimental techniques, interferences, and limitations of the method are discussed in detail. The method is most useful where there is marked segregation of boron. In this type of sample, the segregation can be observed when the nominal boron concentration is as low as 0.0006 pct. THE positive identification and location of boron-rich areas in metals is frequently of great interest in metallurgical work. Unequivocal identification is often difficult to make by conventional metallo-graphic methods. Recently, a method has been described which accomplishes this objective by neutron activation and autoradiography.l-3 The method can be described briefly as follows. Upon neutron capture, a -particles are emitted by boron nuclei according to the following reaction: ,Blo + n - ,a4 + 3Li7 + 2.4 mev The energy is dissipated as kinetic energy of the products. By irradiating a boron-containing sample in contact with a photographic emulsion and subsequently developing this emulsion, a-particle tracks are obtained whose location corresponds to the location of boron-rich areas in the sample. Two factors combine to make the reaction extremely specific for boron. The first is the unusually high (755 barns) cross section of boron for thermal neutron capture. The second is the higher neutron energy required to produce (n, a ) reactions in essentially all other nuclei except lithium. These two factors make the method specific for boron by six to seven orders of magnitude when a predominantly thermal neutron source such as the Brookhaven reactor is used. The reported limit of detection of this method is of the order of 0.01 pct B., The present work was originally undertaken to determine whether this limit could be lowered by use of a thinner emulsion. However, initial experiments showed that in order to use the method at all, it was necessary to reestablish the optimum experimental conditions in terms of the available irradiation facilities. It is the purpose of this paper to describe these experimental conditions in detail, to discuss the factors influencing sensitivity, and to evaluate several techniques for increasing sensitivity. EXPERIMENTAL A) Preliminary Experiments—The first measure-ments were made using samples of crystal oriented silicon steel containing various concentrations of boron. In the later experiments, samples of various high-temperature alloys such as M-252, hcoloy 901, Nichrome V, and so forth, were used. Faraggi, et al.,2 reported that the lower limit of sensitivity in this type of sample was about 0.01 pct B using nuclear emulsions of 50- u thickness. but that it should be possible to extend this limit by the use of thinner emulsions. Accordingly, we first used Kodak Auto-radiographic Stripping Film (Permeable Base) which has an emulsion thickness of only 5 µ. This was mounted on the metallographic specimens according to the technique described by Boyd.4 The emulsion remained in contact with the metal surface throughout exposure and development. Since the emulsion is transparent after development, the autoradiograph and metal surface can be viewed simultaneously and any correlation between film blackening and structure of the metal can be made directly with no problems of realignment. Because the silicon steel is readily attacked by moisture alone, it was necessary to apply a protective coating to the metal surfaces before mounting the emulsion. The coating was made extremely thin in order to absorb as few a-particles as possible. Boyd4 and Gomberg5 have discussed various plastics used for this purpose; however, none was sufficiently impermeable to prevent chemical attack of the steel during the developing process. This attack resulted in the production of gross chemical artifacts in the emulsion. It was, therefore, necessary to use the method of Wolfsberg and John6 as follows. A very thin (approximately 1 µ) coating of Plexiglas II was applied by dipping the sample in a 2 pct solution of Plexiglas II in dichloroethylene. Then, because the emulsion will not adhere to Plexiglas 11, a thin coating of Parlodion was applied in a similar manner using 2 pct Parlodion in iso-amyl acetate. No protective coating was necessary with the high-tem-

Jan 1, 1961

By J. Grosso, D. J. Nagel

In many metallurgical studies, it is necessary to reveal the composition and structural properties of materials. Usually this is done by etching, but some substances do not etch well or easily. Anodizing is known to provide an alternate treatment in many cases. In general, this technique is simple, often more sensitive to composition differences than etching, has excellent resolution, and provides variable contrast in those elements and alloys which anodize. Here we report the use of anodizing in diffusion studies in the TiCb system. Fig. 1 shows a cross section of the diffusion zone in a TiCb couple. The anodizing has clearly revealed both composition and crystallographic features. The maximum bulk penetration of the titanium into the columbium is marked by a sharp line because of the steep concentration gradient. The titanium grain size and orientation differences are also evident. Variation in the grain size reflects the gradually decreasing columbium concentration.

Jan 1, 1967

By Francis F. Lucas

A microscope objective of given numerical aperture, when used with light of given wave length, has some fixed limit of resolution. This may be expressed as potential resolving ability—the ability to resolve is inherent in the lens but whether this limit is achieved in practice is quite another matter. Nearly 50 years ago Abbe evolved theoretical considerations which indicated that the ability of a lens to resolve detail is directly proportional to twice the numerical aperture of the objective and inversely proportional to the wave length of the light used. It is true, unquestionably, that as the numerical aperture of the objective is increased the potential resolving ability of the lens is increased and likewise when the wave length of the light used is decreased, the degree of resolution is increased. Whether Abbe&apos;s formula expresses the exact relationship is not a matter of great concern. It suffices to know that to improve resolution, other things being equal, two avenues of approach are available. Either the numerical aperture of the objective may be increased or the wave length of the light decreased. With the apochromatic system it is possible to employ successfully wave lengths from 400 to 500 uu and still secure reasonably short exposures. The present limit for numerical aperture is 1.40 N. A. although objectives of 1.60 N. A. are now an experimental possibility for metallurgical work. Thus certain well defined limits are set for those who work within the range of the visible spectrum. In order to take advantage of the increase in resolving power which accompanies a decrease in the wave length of light employed, Dr. A. Kohler and Dr. M. Von Rohr of the Zeiss Scientific Staff developed the "monochromats." These are quartz objectives corrected for the single wave length 275 uu which lies in the ultra-violet region of the spectrum. They also developed a series of quartz oculars and a complete photo-micrographic equipment with which to use the quartz optics. Quartz must be used for the optical parts because glass absorbs ultra-violet light almost completely. Thus there was made available about 20 years

Jan 1, 1926

SLAG composition, slag constitution, reactions in slag, and reactions between slag and metal-in other words, the physical chemistry of slags-are matters of great importance to the open-hearth operator, whether or not he makes use of any detailed knowledge of them. Although this is a relatively young branch of the science of steel- making, much progress has been made; however, much remains to be learned, and many of the statements that can be made at present are probably--or even certainly-subject to future change. Nevertheless, the physical chemistry of slags is sufficiently developed to provide a reasonably secure basis for real understanding of steelmaking reactions. FUNDAMENTALS OF SLAG CONTROL By way of introduction, some time is spent in this chapter on effecting an easy transition from some of the more "practical" manifestations of slag to discussions couched in the more formal language of physical chemistry. This necessitates a certain amount of repetition, but it is felt that the purpose of the chapter is best served in this way. Reactions in the metal phase have products that find their way into the slag and are important components thereof; they are discussed in detail in the preceding chapter. Some substances distribute themselves Between slag and metal in definite fashion, and others are found only in the slag. Their reactions are a large reason for this chapter. Limitations of Slag Control. The open-hearth process is essentially oxidizing and cannot be otherwise operated. (Oxygen gradients in the furnace, the mechanism of oxygen inflow, and similar subjects are discussed in Chapter XIX.) As shown in the calculations of material and heat balances for the charge (see Chapter XV), from 25 to 50 lb. of oxygen will flow from air or combustion gases into the charge or molten bath during the heat for each ton of liquid steel

Jan 1, 1944

Some 15 years ago, Dr. Adolf Schmidt, director of the Magnetic Observatory in Potsdam, Germany, developed an instrument, which was a modification of Lloyds balance, for the measurement of the vertical component of the earth&apos;s magnetism in the field. There was a keen demand for this because (1) it was desirable to have a field instrument that would measure the component of the earth&apos;s magnetism which stands in the closest and simplest relation to the configuration of the subterranean magnetic formations-the vertical component; (2) it was desirable to have an instrument that was not only more sensitive but also more reliable than the existing vertical magnetometers (the dip needle, for instance). The application of the magnetometer in oil geology demanded such an instrument, because the magnetic disturbances produced by most types of magnetic formations associated with the occurrence of oil (salt domes, faults, anticlines with crystalline core, etc.) are too small to be detected with the ordinary dip needle. The writer can prove, by some investigations recently made for the U. S. Bureau of Mines, that these instruments may be used also to very great advantage in mining, because they are capable of measuring anomalies which are as great as twice the normal strength of the earth&apos;s magnetic field. Even for such anomalies, the field balance is more advantageous than the dip needle. First, the instrument rests on a firm support and can be adjusted in the proper azimuth, which insures measurement of the vertical intensity only, without a part of the horizontal intensity, which is very important for the interpretation. The readings give the vertical intensity in linear terms and not as a function of an angle; and the field balance is insensitive to temperature when used with scale values that are adequate for the determination of large anomalies. In another phase of mining, the gold placer work, the field balance has also shown excellent results for which the dip needle is not adequate. What has been said about the dip needle holds also, though to a lesser extent, for two other types of vertical variometers recently used, the Tiberg balance and the Thomson-Thalen magnetometer.

Jan 1, 1929