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By L. S. Darken, H. A. Wriedt

An investigation has been made of nitrogen absorption by the lattice defects in a low-carbon steel afte~ Plastic deformation. Specimens in which defects were distributed by various combinations of cold rolling and vacuum heat treatment were equilibrated with controlled ammonia + hydrogen mixtures at 300° to 450°C to study the relation between the solubility and the thermodynamic activity of nitrogen. The results are interpreted in terms of nitrogen being absorbed upon two different types of defect sites, called A sites and B sites. The concentrations of these sites are calculated for specimens with various histories of straining and annealing; and the thermodynamic relations descrihing the equilibrium distribution of nitrogen among the A, B, and ordinary interstitial sites in ferrite are evaluated as follows: THE generalization that the solute atoms in a solid solution interact with imperfections in the solvent lattice is now universally recognized and the subject of an extensive literature. All types of imperfections—point, line, or surface—exhibit these interactions, but the relative importance of each type depends upon its concentration, the strength of its interaction with the particular solute atom, and whether the interaction is attractive or repulsive. The strength and sign of the interaction vary with the vectorial displacement of the solute atom from the imperfection in the crystal. The concentration of lattice defects increases during plastic deformation and the effect of the imperfections upon the solute atoms is usually perceived only after cold work or irradiation. Two experimental methods have previously been used to observe the effects of interaction between nitrogen atoms and lattice imperfections in a iron. Internal friction, which was first used for this purpose by Dijkstra,1 has been applied more often than the electrical-resistivity method of Cottrell and Churchman.2 The method of the present investigation has not been used before.* Uniform specimens of steel with a metastable defect structure are produced by cold rolling and subsequent heat treatment below the recrystallization temperature. Variations in the defect structure are obtained by varying the amount of strain and the heat-treatment conditions. The specimens are then saturated with nitrogen at moderately elevated temperatures in ammonia + hydrogen mixtures having various thermodynamic activities of nitrogen below saturation with Fe4N. From the nitrogen contents of analyzed samples, the metastable equilibria of interactions between the defects and nitrogen can be established and the concentration of sites for nitrogen atoms in the lattice defects calculated. A steel was used in the present experiments instead of purified iron or iron alloys because the amount of nitrogen absorbed at defects is larger in the steel over a much wider range of experimental conditions and could therefore be measured more accurately. The effect of alloy composition is discussed in Part II of this paper; it is sufficient to say here that impurities and phase heterogeneity in ferritic alloys favor the generation and/or retention of larger defect concentrations during plastic deformation and annealing at 300° to 500°C. MATERIALS AND EXPERIMENTAL PROCEDURE The experimental specimens were prepared from stock of a low-carbon steel, which will be called "X steel" here, with the composition: C, 0.12 pct; Mn, 0.43 pct; P, 0.010 pct; S, 0.034 pct; Si, 0.007 pct; As, 0.086 pct; Cu, 0.022 pct; Ni, 0.009 pct; Cr, 0.003 pct. The stock was all from a single ingot made by the basic open-hearth process, which was hot-rolled to strip 0.080 in. thick.. This hot-rolled strip, given the code designation "XH", was the starting material for preparing a series of cold-rolled sheets. The latter are designated "XC27",

Jan 1, 1965

By B. Amero, W. Petruk, D. R. Owens, D. R. Morris

Samples taken at different heights in the lead blast furnace of Brunswick Mining and Smelting corporation were studied to determine the phases present in order to interpret the reactions In the furnace. The main phases in the blast furnace feed are Pb3Ca2S13011, Zn ferrite (ZnFe204), and hardystonite (Ca2ZnSi207); rninor ones include lead and a Pb silicate. The temperature in the furnace varies from about 300°C at 4.2 m above the tuyeres to 1150°C at 1.1 m. There is no evidence of reactions in samples from points cooler than 800°C. Some reaction occurs between 950° and llOO°C and the lead sinter is nearly decomposed at about 1150°C. The first evidence of reaction was the decomposition of Pb silicate to lead and S102. At higher temperatures the Pb Ca2Si3011 decomposed to form lead and hardystonite (Ca2ZnS120rf. The Zn required for hardystonite was derived from the Zn ferrite which apparently re-equilibrated to a new Zn ferrite with less Zn. The decomposed sinter consists essentially of lead, hardystonite, wustite and a Zn ferrite with a low Zn content.

Jan 1, 1984

By Dan E. Lewis, William E. Saegart

Similarities of certain geologic and mineralogic parameters are recognized among the various Philippine porphyry copper deposits. Lowell and Guilbert3 described a model of the typical porphyry copper deposit as the result of comparing numerous Western Hemisphere occurrences. Many of the characteristics of the Philippine porphyry copper deposits differ from the model developed by Lowell and Guilbert. A model of the typical porphyry copper deposit is presented and the characteristics of the Philippine model are compared with those of the Western Hemisphere model. Estimated Philippine copper production in 1975 was 242 446 mt. The total in 1948 was 2091 mt. This represents a 116-fold increase in copper production during the 28-yr period. The Philippines now rank seventh in total world production of copper.

Jan 1, 1978

By J. C. Wright

A practical program of education for workers of the mining industries is being formulated by the Federal Board for Vocational Education in cooperation with the states in which this industry is a dominant one. The Federal Government last year passed a law, known as the Federal Vocational Education Act, that provides for the promotion of vocational education and for cooperation with the states in the promotion of such education in agriculture and trades and industries and in the preparation of teachers of vocational subjects. More than 1,000,000 men in the continental United States are employed in mines and quarries. The following table, from the 1910 Census Report, shows the relative importance of mining and manufacturing pursuits: Manfactures Mines and quaRRies Employees.......... 7,405,313 1,109,410 Capital............. $18,428,269,706 53,380,525,841 Value of product..... $20,672,051,870 $1,238,410,322 Of the more than 1,000,000 men employed in mining, almost three-fourths are engaged in the production of bituminous and anthracite coal; one-fifth, in the production of copper, iron, lead, zinc, and other metals; and the remainder in getting out structural and miscellaneous materials from quarries. The meeting of the needs of the coal-mining industry, therefore, is the problem of greatest importance in the point of numbers to be served. Moreover, the dangers in coal mining are greater than in metal mining. Practically all states have set up educational and technical standards for the position of foreman, boss, superintendent, etc., and every applicant for these positions must have a certificate of competency. The qualifications, too, are becoming increasingly difficult in the field of technical information. In some states, every miner must have a certificate, which is issued by the mine examining board only after an oral examination. Did these state laws not call for definite and comprehensive plans for the vocational education of men in the mining regions, the conditions

Jan 1, 1919

By H. A. Kuhn

The Pittsburgh coal field in Western Pennsylvania is conceded to be the most important in the world.

Jan 1, 1915

By S. Usui, I. Matsuoka, H. Sasaki, J. Shimoiizaka

Depression of galena by sulfite or chromate ion in xanthate flotation was investigated by means of adsorption measurements, electron diffraction and flotation tests. Flotation of galena was depressed by sulfite ion only when galena had been oxidized; no depression took place with unoxidized clean galena. A similar behavior was found when chromate ion was used as a depressant, with the exception that the chromate ion depressed unoxidized clean galena around neutral pH. Depression was attained with galena on which xanthate still remained in appreciable amounts, indicating that the depression is not due to a decrease in xanthate adsorption. The galena surface produced sparingly soluble films under conditions in which depression of galena took place. These films were identified by electron diffraction as lead sulfite and lead chromate on oxidized galena and as chromic oxide on unoxidized clean galena. These observations in conjunction with contact angle measurements, indicate that the depressing action of sulfite or chromate ion arises primarily from film deposition resulting from the reaction between depressants and the galena surface. The thickness of the film was analyzed by means of electrochemical polarization.

Jan 1, 1976

By A. L. Holley

THE members of the society are doubtless aware that the production of American Bessemer steel works is constantly increasing ; that the same converters and machinery are doing more work every year. This enlarged output is due to various causes, chiefly the following: 1st. Better organization-better knowledge on the part of both managers and men, of the plant and the process ; of the way to economize the more exhausting labor, and of the arrangement of the details of labor and operations so that they shall not conflict; also, more pluck-a greater willingness to take risks, or, more properly, such an intimate knowledge of the nature and capacities of the refractory tory linings in various stages of disrepair, and the probable be- . havior of the fluid metal at various stages of its treatment, that the precise nature of the risk may be better known, so that the works may be crowded to their full capacity. In the early practice, after getting four or five consecutive heats in a day, the men preferred to "let well enough alone," and to devote the remaining time to preparation for another turn. Now, thirty, and sometimes forty heats are regularly made during the twenty-four hours, day after day, without the frequent occurrence and without the fear of breakdowns or "messes," as the spilling of steel charges was graphically named in Sheffield. 2d. Although no new refractory materials have been developed, improved means of preparing such as we have, and of imbedding

Jan 1, 1874

By J. H. Hollomon, L. D. Jaffe, M. R. Norton

In the practical heat-treatment of steel the decomposition of austenite usually occurs during cooling rather than at constant temperature. Nevertheless, the course of this decomposition has generally been studied only isothermally. Isothermal studies are not only simpler experimentally, but have the great theoretical advantage that one of the variables, temperature, is constant. It is the purpose of this paper to outline the principles that govern the relations between isothermal and anisothermalt‡ decomposition of austenite, to present and systematize the available experimental information, and to indicate the gaps in the existing knowledge. Some of the experimental information is the result of new work.§ Most of it is derived from scattered data in the literature. Many of these data were obtained incidentally in the course of research on other subjects and their significance has not been pointed out and perhaps not understood. It is hoped that this paper will aid future planning of more extensive research on anisothermal decomposition. Method In order to study the relations between isothermal and anisothermal decomposition, it appears fruitful to view anisothermal decomposition as taking place at a series of constant temperatures1 (except for the martensite reaction, which does not occur isothermally to an appreciable extent). When the time the steel is at each temperature is finite, the over-all amount of the reaction is considered to be the sum of the amounts occurring at each of the successive temperatures. During continuous cooling or heating, the time the steel is at each temperature and the difference between successive temperatures can be considered to approach zero. The over-all amount of transformation will then be given by integration over the range of temperatures involved. This point of view is advantageous in that it considers anisothermal transformation to be a series of isothermal transformations. The problem thus becomes one of determining the effect of partial decomposition at any given temperature upon subsequent decomposition at another temperature. Single Anisothermal Reaction Consider a phase brought to a temperature at which it is unstable, held there until it has partially transformed, and then brought to another temperature at

Jan 1, 1947

By L. D. Jaffe, M. R. Norton, J. H. Hollomon

In the practical heat-treatment of steel the decomposition of austenite usually occurs during cooling rather than at constant temperature. Nevertheless, the course of this decomposition has generally been studied only isothermally. Isothermal studies are not only simpler experimentally, but have the great theoretical advantage that one of the variables, temperature, is constant. It is the purpose of this paper to outline the principles that govern the relations between isothermal and anisothermalt‡ decomposition of austenite, to present and systematize the available experimental information, and to indicate the gaps in the existing knowledge. Some of the experimental information is the result of new work.§ Most of it is derived from scattered data in the literature. Many of these data were obtained incidentally in the course of research on other subjects and their significance has not been pointed out and perhaps not understood. It is hoped that this paper will aid future planning of more extensive research on anisothermal decomposition. Method In order to study the relations between isothermal and anisothermal decomposition, it appears fruitful to view anisothermal decomposition as taking place at a series of constant temperatures1 (except for the martensite reaction, which does not occur isothermally to an appreciable extent). When the time the steel is at each temperature is finite, the over-all amount of the reaction is considered to be the sum of the amounts occurring at each of the successive temperatures. During continuous cooling or heating, the time the steel is at each temperature and the difference between successive temperatures can be considered to approach zero. The over-all amount of transformation will then be given by integration over the range of temperatures involved. This point of view is advantageous in that it considers anisothermal transformation to be a series of isothermal transformations. The problem thus becomes one of determining the effect of partial decomposition at any given temperature upon subsequent decomposition at another temperature. Single Anisothermal Reaction Consider a phase brought to a temperature at which it is unstable, held there until it has partially transformed, and then brought to another temperature at

Jan 1, 1947

By Arthur Clark, Terrill

THE Tri-State field is now believed to be the largest zinc district in the world. It has a potential production sufficient to supply the entire zinc demands of the country. It is estimated that a train 70 miles long would be required to haul the district's 1919 output of 60 per cent. zinc concentrates. For many years,, including 1917, Missouri surpassed Oklahoma in zinc production. In 1918, however, Oklahoma led by a wide margin and, in 1919, Missouri produced less than one-sixth of the total for the three states, when Kansas replaced Missouri in second place in the production. The district is now producing one-third of the zinc of the world and twice as much as ever before at the present price.

Jan 1, 1920

By R. M. Jorda

The mechanism of parafin deposition and prevention has been studied in the laboratory using an apparatus which provides a quantitative means of studying parafin deposition on metal and plastic surfaces. The amount, hardness, adhesion, per cent wax and mean molecular weight of parafin deposits appear to be governed by surface roughness alone, all other conditions being constant. Tests of various plastic coatings indicate that most smooth, nonparafinic plastics are capable of reducing parafin deposits in oil wells, but flexible, highly polar, nonparafinic plastics are more suitable for providing long term resistance to parafin deposition in oil wells if the flow stream contains abrasive materials. INTRODUCTION The problem of paraffin deposition is one of long standing in the oil industry.' Crude oils often contain paraffins which precipitate and adhere to the liner, tubing, sucker rods and surface equipment as the temperature of the producing stream decreases in the normal course of flowing, gas lifting or pumping. Heavy paraffin deposits are undesirable because they reduce the effective size of the flow conduits and restrict the production rate from the well. Where severe paraffin deposition occurs, removal of the deposits by mechanical, thermal or other means is required, resulting in costly down time and increased operating costs. The troublesome paraffins are normal hydrocarbons ranging from approximately C15H38 to C38H78 mixed with small amounts of branched paraffins, monocyclic paraffins, polycyclic paraffins and aromatics.' The amount of paraffins found in crude oils varies from less than 1 to more than 30 per cent. Many publications are available which deal with this problem, and perhaps the most significant findings in recent literature are contained in a publication by Hunt3 ho developed the "cold spot tester", a really useful means of investigating paraffin deposition. Hunt's observations led to many generalized conclusions concerning the effect of surface roughness on paraffin deposits. He ascertained that there was an observable qualitative correlation between the severity of paraffin deposition and the roughness of the surfaces which he tested (cold rolled steel, stainless steel and several plastics). Because of the number of meaningful observations made by Hunt, his cold spot tester was modified somewhat and extensive tests were per- formed to study the quantitative relationship between surface roughness and the physical and chemical nature of paraffin deposits. LABORATORY TEST PROCEDURES The cold spot test apparatus consists of a flat circular plate mounted on a curved tube and positioned in a vessel containing a wax-oil solution (Fig. 1). The apparatus is arranged so that the temperature of the central portion of the circular plate can be varied by means of a circulating liquid stream; the test equipment includes provisions for maintaining a constant wax-oil solution temperature and stirring speed. In the paraffin deposition studies, the modified cold spot tester was used as follows. The cold spot probe consisted of a flat circular plat 2 in. in diameter and 1/8-in. thick positioned in the wax-oil solution kept at constant temperature. As in Hunt's earlier experiments," a cold liquid was circulated through a tube connected to the circular plate so that the liquid impinged on one side of the plate cooling the plate from the center outward, causing paraffin to deposit on the side of the plate exposed to the wax-oil solution.

Jan 1, 1967

By J. R. Cain

In every process for making steel there are one or more stages where the metal is exposed to gas of one kind or another. Thus, in the open-hearth furnace, the carbon dioxide and water vapor in the products of combustion are oxidizing toward the ferrous and manganous oxides in the slag, tending to convert these to higher oxides; the higher oxides then , oxidize the steel, so that indirectly the products of combustion are oxidizing toward the steel. In the Bessemer process, there is direct contact of air and steel; also, the water vapor in the air blown into the converter is continually decomposed by the molten steel, yielding hydrogen and ferrous oxide, both of which are in part taken up by the metal. In the electric-furnace processes, there is always more or less air in contact with the slag covering the metal, and this air and the gaseous reaction products from it are dissolved in the slag to some extent and thus transmitted in part to the steel. In the crucible processes, there is always entrapped air in the charges and the crucibles are more or less permeable to the gaseous products of combustion from the furnace. In all the processes of manufacture, the molten metal is exposed to air while tapping into ladles and ingot molds and has an opportunity to saturate itself with air or with gaseous or solid products generated by chemical reactions between air and steel. Sievertsl has shown that molten metals requirc but a few seconds to saturate themselves with a surrounding gas. No one familiar with the operations at a steel plant needs to be reminded of the important role that gases play at all stages. The familiar "boil" of open-hearth furnaces, due to evolution of carbon monoxide when iron ore is added to the molten steel; the spectacular operation of the Bessemer converter brought about entirely by a gaseous reagent; the almost magic effect of small quantities of silicon, manganese, or aluminum added to the molten metal in ladle or furnace in quickly preventing bubbling and evolution of gases; the unwelcome phenomena of blowholes in ingots that have not been properly manufactured—these

Jan 1, 1920

By Robert R. Abbott

The practice of carbonizing steel for the purpose of case-hardening has assumed great commercial importance within the past 10 years. Formerly, case-hardened steel was held in more or less contempt, since it was considered a cheap substitute for tool-steel. This is no longer the case. The development of the motor-car industry, and coincidentally that of modern alloy-steels, has resulted in overcoming many difficulties formerly experienced in case-hardening. This result has been accomplished by increased knowledge regarding the analysis of the steel which would respond most readily to case-hardening, and by more careful methods of treatment of the carbonized steel. The ordinary method of carbonizing consists in packing the steel with the carbonizing-material in cast-iron boxes and placing them in a furnace at a temperature of from 1,500° to 1,900° F. for a time sufficient to give the required depth of " case." The steel is then either quenched directly from the box, or is allowed to cool without unpacking, and finally given a single hardening-heat, or, for special work, two or three heats. During the year 1911, more than 100,000 tons of carbonizing-material was sold in the United States, at an average price of probably $55 per ton. More than 85 per cent. of this material consisted of granulated bone. Within the past four years, many manufactured compounds have been placed on the market, consisting largely of some form of carbon or carbonaceous material, with or without the addition of chemicals. Steel will absorb carbon placed in contact with it at the temperature of the atmosphere. The reaction is exceedingly slow, but increases rapidly with increasing temperature. Below

Jan 1, 1913

By Samuel Lasky

FAULTING at Kennecott, with its attendant fracturing, is unusual, complex, and important. As study. and knowledge of the various fault systems have progressed, appreciation of that importance has helped in the selection of proper horizons for exploration and in the avoidance of useless crosscutting and drifting. During the study of this faulting and fracturing, a suggestion concerning the formation of the ore-bearing fissures occurred to me. Further study in the available portions of the approximately 45 miles of workings in the Kennecott mines for the purpose of checking up the the suggestion led to the hypothesis which this paper will attempt to present. Briefly, the hypothesis may be stated as follows: The formation of transverse faults that stop against a main, system is connected with changes in the strike or dip of the main fault, and such cross faults or fractures lie in the moving block of the main fault system and indicate a change in strike or dip of the main fault. It has been found that each kind of change tends to produce definite effects and that careful study of the evidence can often suggest the exact type of change.

Jan 1, 1928

By John Gross

The study of the energy used in crushing operations has advanced from a period of perplexing confusion to one of greater clarity. Only within the last few years has any true conception of the work in crushing been possible, owing to the chaotic state of theoretical knowledge. For some 20 years a controversy existed between those advocating the Rittinger law and those advocating the Kick law. The Kick law now appears to be definitely out of the picture, and crushing efficiency may be based confidently on the Rittinger theory. There also seems to be a generally crystallized conception as to the meaning and nature of sub-sieve material. There is needed a simple, direct method for determining surface on a crushed ore product, and also a simple and accepted method for size determination on minus 400-mesh material. The Crushing Law The Rittinger(l)‡ theory of crushing was advanced in 1867 and the Kick(3) theory in 1885. While the Rittinger theory might have been accepted without much question and actually had been accepted by many investigators, a serious doubt as to its validity was raised by Stadler(10) who upon purely theoretical grounds proclaimed the Kick "law" as the true law of crushing. According to Rittinger the energy required in successive steps in reduction increases geometrically, while according to Kick the energy increases arithmetically. These "laws" therefore are at variance, and the establishment of the true law was recognized as of first importance. Many simple experiments have been made to demonstrate the application of the Rittinger theory to crushing, and it would seem that its simplicity should favor its acceptance. Experimental evidence, however, was not convincing, as no reliable data could be obtained on the finer material from a crushing or grinding operation. Gates,(13) Bell,(19)

Jan 1, 1935

Jan 1, 1909

By Paul Tyler

THE ferroalloying elements are connecting links between the steel industry and the nonferrous metal industries. Although ferroalloys are distinctly nonferrous themselves, they serve the steel industry either in the manufacturing process or in modifying the product-in some cases so that it may compete in the markets with nonferrous metals. Of the 92 elements generally accepted by chemists as constituting the primary building blocks of matter, all but the very rarest have been investigated with a view to employing them in steel manufacture. The surprising thing is that so few have been found commercially acceptable. Despite the relatively small number of elements involved, the employ-ment of alloys in steelmaking is one of the most complicated and probably one of the least well understood of modern industrial enterprises. A great deal has been written regarding the action of individual elements and a profuse and somewhat acrimonious literature covers pretty much the whole field of ferroalloy ore supplies. In the middle ground between the miner and the steelmaker developments are less carefully watched by most observers, and except for an occasional description of the technique of some conversion process or the tariff hearings in Congress, very little is said about them. The purpose of the present paper is to describe in relatively nontechnical terms this highly complex industry and to study its relations to our national progress.

Jan 1, 1933

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

THAT the march of civilization has synchronized with progress in the art of utilizing minerals is a proposition that needs no proof. It is a truism. Historians conveniently divide the time that the earth has been inhabited into the Stone Age, the Bronze (more accurately the Copper) Age, and the Iron Age. As archeologists are not entirely in accord as to dates, and as a few centuries make no difference whatever to this particular story, it may be approximated that the Age of Copper began about 8000 years B.C. and that it gave place to the Age of Iron about 1000 years B.C. The logic of this succession-stone, copper, iron-lies in the fact that copper first displaced stone, then iron displaced copper as the standard material out of which the utensils, implements, and weapons, the utilitarian articles of antiquity, were made. After the advent of iron, the mining and smelting of copper continued. Copper and bronze found use particularly in objects of artistic and ornamental nature; but the superior qualities of iron for many purposes were recognized. Useful manufactures of those days consisted principally of knives, hammers, chisels, spear-heads, arrow-heads, and battle-axes. First these were made of stone, then of copper and bronze, then of iron-particularly as there was plenty of iron ore, and the metallurgy was comparatively easy of accomplishment. Of course, the periods of transition dragged slowly. Definite as were the three Ages dominated by the mineral substance from which they get their names, ten or fifteen centuries probably elapsed from the time the first iron was smelted in a small charcoal furnace until it became the accepted material from which to shape a battle-axe. Contrast this with the pace of modern progress. In a brief span, half a dozen more or less deserving candidates for the distinction of having their name

Jan 1, 1933

By A. Berghezan, E. Bull Simonsen

A simple and general method is described for melting and zone refining refractory metals by induction heating on a specially shaped water-cooled copper crucible. The crucible is the essential part of the apparatus and is placed horizontally. It consists of either a copper plate, or a flattened tube, or of several parallel small diameter tubes all water cooled. The charge lies on the crucible, or whenever possible, is suspended above it. This assembly goes into a transparent quartz tube and the whole is passed through the coil of a radio frequency generator. Vaarious atmospheres can be used. No contamination is detected from the copper crucible. purification is obtained both by selective evaporation of impurities and by zone refining. METHODS of melting and refining relatively large ingots of all reactive and refractory metals as well as some semiconductor materials have been developed in this laboratory during the past several years using induction heating and cold crucibles. These methods are simple and permit the use of a variety of starting materials in preparing ingots of suitable shapes. Among these methods, two are of particular interest. One deals only with the problem of melting without contamination. In this method the induction coil has a specially designed shape and acts simultaneously as heating element and crucible. The second goes one step further, being designed for both melting and further purification of the refractory metals. The aim of this paper is to describe the second method which is of more general interest and of greater applicability to metallurgical problems. A) THE PRINCIPLE OF THE MELTING AND PURIFICATION METHOD As originally proposed by one of us1 the method consists of heating a charge of any refractory metal or semiconductor material to the melting point on a water-cooled copper crucible by passing both the charge and the crucible through the induction coil of a radiofrequency generator. Although both are subjected to the same induction field, one achieves the melting of a refractory metal on a copper crucible even when the refractory metal has a melting point of more than 2000°C above that of the crucible. This seemingly "odd" method works effectively for the following reasons. Because of its high electrical and thermal conductivity as compared with the material being melted, copper can be used as the crucible and kept at a low temperature while the material is heated by induction to its melting point. With water Silver and other highly conducting materials can also be used. If a nonconducting material is contemplated, e.g. SiO or a high polymer, a very thin wall should provide efficient cooling. cooling through ducts in the crucible its temperature can be kept between 40" to 70°C; thus its electrical resistivity is kept low, while the resistivity of the charge increases rapidly as its temperature is increased. B) APPARATUS The crucible is the essential part of the apparatus. It has been designed in various shapes depending on the atmosphere used, whether vacuum or an inert gas or hydrogen. In all crucible designs an effort was made to reduce its volume to "nothing but the cooling water" in order to avoid shielding the ingot from the induction field. In practice it is either a

Jan 1, 1962