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By Alden B. Greninger, Alexander R. Troiano

Metallurgists have long believed that martensite in steel forms as plates along the octahedral {111} planes of austenite. Much has been written about mechanisms whereby units of the austenite lattice are pictured as transforming to martensite by shearing movements initiated along the octahedral planes of austenite, supposedly resulting in plates of martensite lying parallel to these planes of shear. A critical inspection of two or three photomicrographs of quenched hypereutectoid steel led us to the conclusion that the orientation habit of martensite, at least in hypereutectoid austenite, could not possibly be octahedral. Inasmuch as recent studies,30,31 of the martensite-type reaction in nonferrous alloy systems have established the irrational orientation habit as characteristic of this type of lattice transformation, the need for a thorough restudy of the crystallography of martensite formation in steel was evident. The present paper reports the results of such a study, extended to include both cementite and some of the products of constant-temperature decomposition of austenite. Also reported are a few of the results obtained from a microscopic and X-ray study of the austempering process in very high-carbon steel. I. The Martensite Transformation Previous Work Microstructure and Crystal Structure of Martensite.—Among the best series of published photomicrographs of quenched steels are those of Whitely,1 Robertson,2 Hanemann and Schrader,3 and Lucas.4 The crystal structure of martensite is body-centered tetragonal, with axial ratio varying from 1 near 0.0 per cent carbon to 1.08 for 1.75 per cent

Jan 1, 1940

By H. J. Booss

THERE is a considerable lack of data on thermody-namic properties of hard-metal alloys. Only two papers 1,2 give mean values of specific heat in an unknown temperature range; more recently the author3 gave more detailed information on the mean specific heat in the temperature range from 20" to -190° C.. EXPERIMENTAL 1) Method—Experimental procedure followed a method suggested by Oelsen and coworkers.4 It requires samples of some 100 g of weight. The time of measurement is prolonged (30 min) but one run allows the measurement of a lot of positions on the heat-content curve. Results4 were found to be in good agreement with "best values" given by kelley,5 Kubaschewsky and Evans,6 etal.

Jan 1, 1960

By Carl Henrich

In the planning and erection of smelting-works, especially of such as contain the modern large water-jacketed blast-furnaces, we are often confronted with an insufficiency in the watersupply. It may be impossible to find in the immediate neighborhood of the selected site a sufficient supply to furnish the jackets with cold water. Or there may be enough water for this purpose, but it may be highly charged with scale-forming minerals held in solution. Or, the main water-supply, if pumped from the workings of a mine, may carry iron- or copper-salts, or even some free acid in solution, all of these substances being derivable from the oxidation of sulphuret-ores in the mine. Moreover, such mine-waters sometimes contaminate the waters of the creeks, so that these become unavailable, and we have to fall back on an inadequate supply of pure water furnished by some spring or springs, entirely too small in

Jan 1, 1896

By Homer Staley

THE casting alloy 88 copper, 10 tin, 2 zinc, commonly known in England as Admiralty metal and in this country as Government bronze, gun metal, or Naval Department composition G, has, at its best, many valuable properties. However, its physical properties are known to vary widely with slight changes in method of manufacture of the castings, such as slight variations in composition, variation in pouring temperature, kind of mold used, method of pouring and gating of molds, size and shape of castings, amount and kind of heat treatment., and so forth.1 The microstructure of castings made from this alloy is influenced by slight variations of composition, rate of cooling, and kind and length of heat treatment. This is best understood by reference to the equilibrium diagram. The part of the diagram in which we are interested and the effect of the thermal equilibrium relations on the physical properties of the alloy 88 copper, 10 tin, 2 zinc, have been discussed by Hoyt, Camp-bell, Primrose, and Rawdon.2 In Fig. 1 is given the equilibrium diagram of the copper-tin alloys. Briefly stated, the relations of composition and temperature changes are as follows. Compositions between A and a consist of but one constituent-the a bronze, which is a, solid solution of copper and tin, rich in copper. On cooling from the molten state these compositions gradually crystallize, at temperatures above 790°, into a mass of interwoven tree-like crystals or dendrites. The cores of the dendrites are rich in copper and the percentage of tin gradually increases as the surfaces are approached. As cooling progresses, after all the metal has crystallized, no further changes occur, in the crystals other than diffusion within the crys-

Jan 9, 1919

By W. L. Zeigler

THE gravity concentrator of the Hecla Mining Co. was originally constructed in 1888 by the Milwaukee Mining Co., which was operating the Gem of the Mountains mine. It was purchased by the Hecla Mining Co. in 1900, and placed in operation 2 years later. At that time FIG. 1.-HECLA MINING CO. GEM CONCENTRATOR, GEM, IDAHO. the capacity was only about 200 tons a day, but many additions and changes in equipment have been made so that the present capacity is about 800 tons. One of the outstanding improvements made was the substitution of Callow flotation cells for vanners, which occurred in 1915. The recent building of a flotation plant for treating jig tailings, and the construction of a modern surface plant at the mine, following the

Jan 1, 1927

By Hannu Penttila, Harrison R. Cooper, Olli Mattila

Two approaches to automated operation in metallurgical processes involve the conventional analog control or, more recently, digital control. The expanding use of digital controls applied to process automation is a comparatively new development. Several current technical reports describe digital control systems in concentrator grinding control, 1, 2, flotation, 3 and smelter operations. 4,5 The principle factors influencing trends to digital control are:

Jan 10, 1976

By S. Yukawa, M. J. Sinnott

A high resolution autoradiographic study of the diffusion of a nickel isotope (NP3) into copper in the temperature range of 650° to 925°C, with particular emphasis on grain boundary diffusion, has been made. The extent of grain boundary diffusion is a function of the grain boundary angle and the diffusion temperature. The ratios of the grain boundary diffusion coefficient to the lattice diffusion coefficient ranges from 104 to 105. The activation energy for grain boundary diffusion decreases with increasing grain boundary angle. STUDIES and reviews&apos;-8 of metallic diffusion have indicated that grain boundary diffusion is a common phenomenon but quantitative studies of the many variables involved are not numerous. The present work was concerned with determining the influence of the crystallographic orientation of the grain boundaries and the temperature on the extent of boundary diffusion of nickel into copper. The study involved essentially three steps: 1—the production of grain boundaries of known crystallographic orientation, 2—the determination of the extent of diffusion into the boundaries, and 3—the analysis of the resulting data in terms of the usual diffusion concepts. The grain boundaries investigated approximated the simple tilt variety having l° of freedom. They were produced by controlling the solidification from a melt of Cuprovac (a high purity vacuum-melted copper obtained from Vacuum Metals Corp.) of a pair of seed crystals so that the bicrystals of copper produced had a common <100> axis. By rotating one seed crystal relative to the other, a simple tilt boundary was produced. The angle of rotation between the two crystals is the grain boundary angle 8, or what is sometimes termed the misfit angle. In all, some 16 boundaries ranging from 2" to 72" in 5" to 10" steps were investigated. The crystallographic orientations were measured with the use of both X-ray and optical goniometric techniques. The <100> axes in the crystals were found to be parallel within 2" to 3" with the exception of one crystal (8 = 12") in which the axes were 6" from being parallel. All bicrystals showed evidences of sub-grain structures. Laue analyses showed that these subgrains differed in orientation up to a maximum of 2". Because of these variations, and some curvature in the boundaries, the grain boundary angles listed are actually average values and deviate from the 1 o of freedom boundaries. The stripping film technique of high resolution autoradiography was used to detect the diffusion of the nickel isotope into the grain boundaries of the bicrystals of copper. Kodak experimental permeable stripping film with an emulsion layer 5 u thick

Jan 1, 1956

By F. H. Rhines, A. H. Grobe

The constitution of the indium-zinc alloy series has been investigated by Wilson and Peretti,1 who determined the liquidus and eutectic temperatures by the conven-tional method of cooling curves and the eutectic composition by analyzing eutectic exudations. Recent developments affecting the availability of indium and consequent increased interest in its applications make a more complete knowledge of the constitu- tion of its alloys desirable. As a part of a program far the reexamination of the constitution of indium alloys by precision methods, the indium-zinc phase diagram (Figs. I and 2) has been redetermined in its entirety. The eutectic temperature (I43. 5°C.) reported by Wilson and Peretti has been confirmed exactly, but their value of the zinc concentration at the eutectic, 4 per cent, was found to be high; the new value is 2.8 per cent of zinc. There is also a rather large difference between the forms of the liquidus curves of Wilson and Peretti and those found in the present studies. The solidus curves herein have been located for the first time and the limits of solid solubility have been tenta-

Jan 1, 1944

By A. H. Grobe, F. H. Rhines

The constitution of the indium-zinc alloy series has been investigated by Wilson and Peretti,1 who determined the liquidus and eutectic temperatures by the conven-tional method of cooling curves and the eutectic composition by analyzing eutectic exudations. Recent developments affecting the availability of indium and consequent increased interest in its applications make a more complete knowledge of the constitu- tion of its alloys desirable. As a part of a program far the reexamination of the constitution of indium alloys by precision methods, the indium-zinc phase diagram (Figs. I and 2) has been redetermined in its entirety. The eutectic temperature (I43. 5°C.) reported by Wilson and Peretti has been confirmed exactly, but their value of the zinc concentration at the eutectic, 4 per cent, was found to be high; the new value is 2.8 per cent of zinc. There is also a rather large difference between the forms of the liquidus curves of Wilson and Peretti and those found in the present studies. The solidus curves herein have been located for the first time and the limits of solid solubility have been tenta-

Jan 1, 1944

By A. Ross Rornmel

ABILITY to speak effectively is one of man&apos;s most longed for and coveted abilities. It is the ability to stand on one&apos;s feet, transfer knowledge and thoughts to others, to reach an objective professionally or otherwise by leading groups through a channel of planned thought. Each day group speaking plays an important part in making or marring success, and the engineering profession often provides this opportunity and requirement. An ability to speak effectively develops courage, poise, confidence, and prestige for the speaker. The technical man cannot be reluctant to face an audience. He is often called upon to do this in presence of employees, supervisors, and other groups. His ability to speak effectively is as much a requirement as the fundamentals of his profession. The three fundamentals of effective speaking are: (1) Enthusiasm and Confidence. These are joined because of their close relation. (2) Preparation. This includes knowledge of the subject. (3) Presentation. By this is meant the features of delivery.

Jan 1, 1946

By Igor Plaksin

Interaction of sulfide minerals and native metals with reagents in flotation is largely determined by particle-surface changes resulting from action of the medium and dissolved gases. A number of early studies were devoted to the selective action of various gases on minerals.1 Mc- Lachlan2 paid attention to oxygen as the most active gas affecting flotation properties of sulfide minerals.

Jan 3, 1959

By O. C. Ralston, F. Fraas

VIRTUALLY all commercial use of electrostatic separation has employed separators depending on differences of conductance of the broken, solid mixtures treated by them. The two main types of conductance separators have been: (1) Those in which the separating field is as near a static field between two charged electrodes as it is possible to maintain in the face of the usual leakage that takes place between electrodes with some 5 to 50 kv tension between them and spacing of 1/2 to 3 in.; (2) those in which a convective discharge of corona or spray type, but not a spark discharge, takes place between the carrier electrode and a charged electrode facing it, which is of very restricted area, such as a row of needle points or a small diameter wire parallel to the face of the carrier electrode. The present paper deals with this latter type. The principle is usable in separators where the carrier electrode, usually grounded, has the shape of a roller, a conveyor belt, a vibrating table, a sloping chute, or a nearly vertical plate. The innovation studied by us has been the use of the convective field for charging material on the carrier electrode and succeeded by a field between the carrier electrode and an electrode made of a true dielectric which cannot take on a charge by conduction but is charged by being in the radius of the corona discharge. The acquired charge is of the same sign as that of the corona but is not dischargable by contact with a good conductor. However, high-tension charge tends to leak off because of the ionization of the ambient air. The field between this electrode and the carrier electrode is as near static as it is possible to obtain. There are some differences in behavior of this electrode and that of the gas tube electrode used by Sutton, as will be discussed below. Both electrodes cause increased adhesion of nonconductive particles to the carrier roll. The particles are pinned there because they are convectively charged on their outer surfaces facing the corona electrode. The electrodes also cause increased rate of release of conductive particles tending to be pinned by corona charging but conveying the charge to the grounded carrier roll almost as rapidly as it is received by the particles. The sign of the potential on the corona-emitting electrode makes little difference in the separation. An electrode usually emits negative corona somewhat more easily than it emits positive corona, as electrons are then the fundamental particles emitted. With a positive electrode the flow of electrons involved in positive corona discharge is onto the electrode from the ambient gas. Theory In the separator illustrated in fig. 1, the nonioniz-ing electrode is a rotating, nonconductive dielectric cylinder designated as B. The ions emitted by the corona electrode, or wire F, charge both the particles on the carrier electrode, or roll A, and the surface of the dielectric electrode B. Whereas the space between roll A and wire F contains ions, the space between electrode B and roll A is a pure static field free of ions. The dielectric electrode has been described by Bullock.1 However, the corona electrode, which Bullock uses for the purpose of charging only the dielectric electrode, is adapted here to also charge the particles on the carrier roll. In operation the ionic field from the corona electrode is balanced with the static field from the dielectric electrode. The ionic field charges the particle so that it adheres to the roll. The static field intensifies the discharge of the corona charge by interfacial conduction and permits the release of the particle. The ionic and static fields therefore have opposing effects.2 The values of both fields are adjusted so that the poor conductor will adhere and the good conductor will be released.

Jan 1, 1951

By O. C. Ralston, F. Fraas

VIRTUALLY all commercial use of electrostatic separation has employed separators depending on differences of conductance of the broken, solid mixtures treated by them. The two main types of conductance separators have been: (1) Those in which the separating field is as near a static field between two charged electrodes as it is possible to maintain in the face of the usual leakage that takes place between electrodes with some 5 to 50 kv tension between them and spacing of 1/2 to 3 in.; (2) those in which a convective discharge of corona or spray type, but not a spark discharge, takes place between the carrier electrode and a charged electrode facing it, which is of very restricted area, such as a row of needle points or a small diameter wire parallel to the face of the carrier electrode. The present paper deals with this latter type. The principle is usable in separators where the carrier electrode, usually grounded, has the shape of a roller, a conveyor belt, a vibrating table, a sloping chute, or a nearly vertical plate. The innovation studied by us has been the use of the convective field for charging material on the carrier electrode and succeeded by a field between the carrier electrode and an electrode made of a true dielectric which cannot take on a charge by conduction but is charged by being in the radius of the corona discharge. The acquired charge is of the same sign as that of the corona but is not dischargable by contact with a good conductor. However, high-tension charge tends to leak off because of the ionization of the ambient air. The field between this electrode and the carrier electrode is as near static as it is possible to obtain. There are some differences in behavior of this electrode and that of the gas tube electrode used by Sutton, as will be discussed below. Both electrodes cause increased adhesion of nonconductive particles to the carrier roll. The particles are pinned there because they are convectively charged on their outer surfaces facing the corona electrode. The electrodes also cause increased rate of release of conductive particles tending to be pinned by corona charging but conveying the charge to the grounded carrier roll almost as rapidly as it is received by the particles. The sign of the potential on the corona-emitting electrode makes little difference in the separation. An electrode usually emits negative corona somewhat more easily than it emits positive corona, as electrons are then the fundamental particles emitted. With a positive electrode the flow of electrons involved in positive corona discharge is onto the electrode from the ambient gas. Theory In the separator illustrated in fig. 1, the nonioniz-ing electrode is a rotating, nonconductive dielectric cylinder designated as B. The ions emitted by the corona electrode, or wire F, charge both the particles on the carrier electrode, or roll A, and the surface of the dielectric electrode B. Whereas the space between roll A and wire F contains ions, the space between electrode B and roll A is a pure static field free of ions. The dielectric electrode has been described by Bullock.1 However, the corona electrode, which Bullock uses for the purpose of charging only the dielectric electrode, is adapted here to also charge the particles on the carrier roll. In operation the ionic field from the corona electrode is balanced with the static field from the dielectric electrode. The ionic field charges the particle so that it adheres to the roll. The static field intensifies the discharge of the corona charge by interfacial conduction and permits the release of the particle. The ionic and static fields therefore have opposing effects.2 The values of both fields are adjusted so that the poor conductor will adhere and the good conductor will be released.

Jan 1, 1951

By A. S. Yue

Small-angle tilt boundaries have been observed in a lamellar eutectic structure. These boundaries are morphologically similar to a theoretical till boundary originally proposed by Burgers. The production of a small-angle tilt boundary in the lamellar eutectic structure is attributed to the formation of an indentation on a planar solid-liquid interface during growth. Constitutional supercooling due to the accumulation of impurity atoms ahead of the interface is primarily responsible for the generation of an indentation. The distance between two faults of like sign, designated as lamellar fault distance, is calculated by the Burgers equation for small-angle boundaries. It was found that the lamellar fault distance decreases exponentially and the tilt angle increases exponentially with freezing rate. SMALL-ANGLE tilt boundaries have been observed in many crystals in the as-grown states by etching techniques. However, a detailed substantial proof for revealing the presence of dislocations in the form of etch-pits was recently accomplished by Vogel. These boundaries are described as an array of dislocations of like sign. The angle of tilt associated with a boundary is treated theoretically by Burgers3 and is given by 0 = b/D for small tilt-angle where b is the Burgers vector of the dislocations and D is their average spacing. During the course of experimentation on the solidi fication of the lamellar Mg-32 wt pct Al eutectic a microstructure which was strikingly similar to a dislocation tilt boundary was observed. An example of the type of microstructure is given in Fig. 1, which shows a combination of transverse and top sections of the lamellar eutectic structure. The lamellae of the top section on one side of the apparent tilt angle are not parallel with those on the other side. Consequently, some lamellae must be terminated somewhere. Fig. 1 shows that the termination of lamellae is analogous to a dislocation tilt boundary in a crystal lattice originally proposed by Burgers. This work represents a closer look at such structures. The factors governing the production of the small-angle tilt boundary are discussed in terms of the freezing condition and impurity distribution in the melt. The effect of freezing rate on the distance between two faults, designated as lamellar fault distance, and the tilt angle is also described. In addition, the lamellar fault distance is determined by means of the Burgers equation for small-angle tilt boundary. EXPERIMENTAL PROCEDURE The slightly impure Mg-32 wt pct Al eutectic rods, 5/8 in. in diam and 12 in. long, were made from 99.99 wt pct Al and 99.98 wt pct Mg and were cast in a high-purity graphite mold. Some of these rods were purified by zone-refining the eutectic using direct-radiation helical-coil furnaces5 A molten zone about 2 in. long was passed through the cast rods at a speed of 5.3 x 104 cm per sec for ten passes of the molten zone. Before the freezing experiment was begun, 2-1/2 in. of the material from the head and tail ends of the zone-refined eutectic were removed from the rod to eliminate any impurity. The freezing experiments were carried out under controlled conditions,8 using a protective atmosphere of purified argon. At the end of each run, observation of the tilt boundary was made throughout the entire length of the rod with a light microscope on the top, longitudinal, and transverse sections (three mutually perpendicular sections) of the lamellar eutectic solid. The experimental data used for the determination of interlamellar spacing and tilt angle were taken from the middle portion of

Jan 1, 1964

By R. W. Diamond

Low-grade ores can be designated by two main classifications: (1) simple low-grade ores, and (2) complex low-grade ores. As a rule the first type has a relatively small metal content, although low- grade iron ores contain a rather high percentage of metal. As the simple type is the one that is ordinarily in mind when the term "low-grade ore" is used, the paper will be devoted mainly to ores in this general category. Cheap treatment is the prime requirement in utilizing low-grade ores of the simple type, although in some cases the value of nonmetallic by-products, such as limestone for fer- tilizer and silica for flux, allows a little more lati- tude than in the usual situation. When the costs are divided under the three headings-mining, milling, and smelting-it is apparent that the last group will not constitute an important factor as a rule because the high concentrating ratio makes the smelting cost per ton of ore fairly low.

Jan 1, 1949

By Edward Steidle

It has been said that "the command of nature has been put into the hands of man before he knows how to command himself," and what we see about us gives particular emphasis to this observation. If this condition be granted, the vaunted boast of school and college, of the institution that had the training of this generation, and of its fathers, and of its grandfathers, the boast that education is a "preparation for life," stands exposed as a hollow claim, or as a ghastly, cynical conception of life, or else education has fallen far short of its intentions. It has been evident for some time that education was not meeting the fullest expectations of society. In recent years there has been a deal of speculation indulged in by both laity and faculty in regard to American education and American civilization, and some few and sporadic changes have been effected. Today, however, there is no longer time for mere hypothetical considerations; we are faced with certain definite facts and confronted with obvious conditions that will not wait for fine-spun theories. If educators do not put their house in order, someone else will do it for them. The trends in mineral industries education must be in harmony with this general realignment that is today visible on the educational horizon, and only as these trends are in conformity with this movement can they be called sound. Two questions, then, confront mineral industries educators: (1) What are the trends in mineral industries education, and (2) how do these trends correlate with the major educational movements of the day? Scope or Mineral Industries Education Before launching into these particulars, it might be well to define the scope of mineral industries education and to consider its present position. Mineral industries education embraces three main types of work: 1. Earth Sciences and Geography.—Geology, mineralogy, geography— courses basic to all mineral industries and to the humanities. 2. Mineral Engineering.—Mining, petroleum and natural gas—dealing with mineral producing industries. Application of earth sciences and all types of engineering to exploitation of natural mineral resources.

Jan 1, 1934

By Clinton H. Crane

DR. TILNEY, the great expert on the study of the development of the brain of human beings and animals, tells us that the greatest difference between the human brain and the brain of animals is that man alone has shown evidence of being able to predict the future. Just why he throws overboard the busy bee who lays up honey for the winter, the squirrel who gathers nuts, and the humble ant, I do not know. At any rate, it is nice to be assured by an authority that we have this power of prophecy. My own experience with attempting to prophesy the future has convinced me that our only possibility of being good prophets is to be good students of history.

Jan 1, 1940

By H. B. Muller

Single stage autogenous grinding of run-of-mine ore was selected by Broken Hill South Ltd., parent Company of Cobar Mines Pty. Ltd. for the concentrator to treat 60,000 tons per four weekly period of copper and complex copper-lead-zinc sulphide ores from the C.S.A. Mine at Cobar, Australia. Ore is mined by mechanised horizontal cut-and-fill stoping and is prepared for grinding by crushing under- ground in a 60 in. x 48 in. jaw-crusher set at 5 in. closed side setting. The ore is reduced to 80% minus 76 microns in two parallel sections each of one 22 ft. dim. x 7 ft. long autogenous grinding mill, powered by a 1,250 H.P. motor, operating in closed circuit with a single stage 20 in. dim. cyclone. Broken Hill South&apos;s original concept of the concentrator required the maximum use of reliable instrumentation, centralised control, and the minimum of manning. To achieve this objective the control room, housing the process recorders, alarms, closed circuit television monitors and all the control equipment, overlooks the grinding and flotation sections, and the whole plant is serviced by a public address system. The grinding units and associated equipment are located in the open and are serviced with the aid of a mobile crane and a mobile hydraulically-operated liner lifting device.

Jan 1, 1970

By J. F. K. Brown

ANTHRACITE?S satisfactory showing in 1942 was accomplished in the face of adverse conditions, such as the loss of man power to the active services and to other industries, and the difficulty and delay in obtaining the necessary materials and equipment required in mining operations. Although the in- creased output was stimulated by the war, and thus does not impress one as contributing to continuing improvement in the industry, nevertheless the year witnessed several efforts ant1 consideration of others that have the appearance of permanent progress.

Jan 1, 1943

By H. T. Sumsion, A. U. Seybolt

The results of an investigation of vanadium-rich V-O solid solutions are presented, indicating the structure and lattice parameters of two solutions, a and ß, and their approximate temperature-composition existence. The a solution is the terminal body-centered cubic one, and contains up to 3.2 atomic pct 0. The ß solution has an ordered body-centered tetragonal structure, is formed at 1270°C, and exists from about 15 to 22 atomic pct 0. From the evidence available, the various phase boundaries have no appreciable temperature dependence. Evidence has been found for a polymorphic transformation in pure vanadium at 1550°C. IN an earlier investigation&apos; dealing with the preparation of pure vanadium by calcium reduction of the oxide, it was found that small amounts of oxygen drastically reduced the ductility of the metal. Because this effect was so marked, it was decided to make a study of the solubility of oxygen in solid vanadium. This report deals principally with this solubility and the nature of the phase relationships in the vanadium-rich region, particularly at temperatures below 1300 °C. However, during the investigation enough data on the V-0 system were obtained to make it appear worthwhile to present a tentative phase diagram up to the composition VO. The only significant prior work found on this system are the contributions of Klemm and Grimm,&apos; and Mathewson et al.3 Klemm and Grimm prepared a wide range of V-O compositions by powder techniques including the compositions VO.l, VO.2, VO.3 and VO4 (9.1, 16.8, 23, and 28.6 atomic pct 0, respectively). The first three compositions were found to consist of a body-centered tetragonal solid solution, while the last also showed lines of VO (NaCl structure). They found that the parameter c, increased and the parameter a, decreased with increasing concentration of oxygen. For their composition VO.27, or about 16.8 atomic pct O, they cite the values a, = 2.948A, c, = 3.53A, and c/a = 1.2. Klemm and Grimm made no attempt to determine the solid solubility limit nor to construct a phase diagram. They did, however, give some data on the homogeneity range of VO, and they proposed a structure for the body-centered tetragonal solid solution; these points will be taken up later. Materials and Preparation of Samples The vanadium used in this investigation was prepared in the laboratory by the method previously mentioned.&apos; A typical analysis is as follows: Fe, 0.007 pct; Si, 0.02; Ca, 0.06; C, 0.224; O2, 0.044; N,, 0.0017; H2, 0.003; and V, 99.34 ±0.3 (assay). The vanadium assay is probably low by about the error given. The impurities total about 0.36 which, if subtracted from 100, gives a purity of about 99.6. At the time material was being prepared for this work no suitable technique was available for melting vanadium without appreciable contamination. The procedure adopted therefore was to cut the calcium-reduced regulii into slices which were then rolled to strip about 0.025 in. thick for oxygen diffusion. Pieces of rolled vanadium of approximately 0.025xY4xl in. and weighing about 0.3 g were suspended in a vertical fused-silica tube which was part of an ordinary gas absorption apparatus. The silica tube was heated by an electric resistance-tube furnace which could be raised around the silica tube or lowered away from it as desired. This apparatus had no novel features which require detailed description. Other than the silica tube and furnace, it consisted of a glass system evacuated by a liquid nitrogen trapped mercury diffusion pump, a mercury-operated gas burette, a McLeod and a Pirani gage, and a mercury manometer. It was also equipped with suitably located stopcocks for isolating various parts of the system; the vacuum ordinarily attained was between 10" and 10-6 mm of mercury. Oxygen generated by decomposing MnO2 was passed through anhydrous magnesium perchlo-rate before introducing it into the gas burette and thence to the absorption chamber.

Jan 1, 1954