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By H. J. Levinstein, H. J. Guggenheim, C. D. Capio

An optical incestigation of the phase transformations in RbFeF, has been conducted. Details of the ferromagwetic phase transition and the metamagnetic state are disczrssed. The three-dimensional magnetic domain structure existing in bulk crystals of RbFeF3 is described, as well as the effect of the magnitude and direction of the applied magnetic field on the domain struclure. The strong magnetoelastic interaction in RbFeF, is demonstrated. The results of the direct observation of the role of dislocation subboundaries and slip bands as nucleation sites and as pinning sites for magnetic domain walls are reported. THE perovskite compound RbFeF, has recently been shown to exhibit three magnetic states.''' Above 102°K it is paramagnetic, between 102" and 87°K it is antiferromagnetic. and below 87°K it is ferromagnetic (i.e., exhibiting remanence) with a modification of the magnetization occurring at 40°K. The changes in magnetic structure at 102o, 87°. and 40°K are accompanied by shear transformations to successively lower crystal symmetry classes.3 At 102°K a second-order phase transformation to a tetragonal crystal structure occurs. The c/o ratio increases with decreasing temperature to a value of 1.0034 at 87°K where the crystal undergoes another shear transformation to an ortho-rhombic crystal structure. The magnetic modification at 40 K is also accompanied by a shear transformation to a lower crystal symmetry. RbFeF3 is unique in that in the ferromagnetic state it is transparent in the bulk to visible light, has a low saturation magnetization, a large magnetic rotation. and has good optical properties.' All these features make it an ideal material for the investigation of magnetic domain structures in bulk crystals. In addition a dislocation etch has been developed which reveals the point of emergence of dislocations with the (100) surfaces of RbFeF3,5 making it possible to determine the dislocation arrays in the material. As a result domain wall dislocation interactions can be observed in the bulk crystal. In this paper we report on 1) the crystallography of the phase transformations in RbFeF3. 2) the domain configurations as a function of magnetic field and crystal orientation. 3) the interaction of dislocations and magnetic domain walls in RbFeF,. EXPERIMENTAL PROCEDURE Since the temperature range of interest is below room temperature the dewar shown in Fig. 1 was employed. It was designed to fit on the stage of a Leitz panphot metallograph, and permitted examination of the sample at a magnification up to 150 times. The dewar consists of a double-walled glass cylinder bent into an L shape. The space between the walls is evacuated. The viewing wirldows were made of four optically flat quartz discs aligned parallel to each other and sealed to the sides of the concentric cylinders. The specimens were mounted in a holder attached to a flexible plastic shaft. Various holder designs were employed depending upon the type of observations to be made. For studies of the phase transformation between the antiferromagnetic and ferromagnetic state the holder shown in Fig. 2(d) was employed. This holder permitted accurate temperature control at 82" to 88°K by balancing the heat input from the carbon resistance heater against the heat loss to a heat sink immersed in liquid N2. Magnetic field studies were conducted by employing the holders shown in Figs. 2(a) and (b). The holder shown in Fig. 2(n) has a solenoid imbedded in it. such that the magnetic field direction is in the same direction as the incident light. The magnetic field provided by the holder in Fig. 2(b) is perpendicular to the incident light direction. The holder in Fig. 2(r) was employed when observations of the specimen were desired while an elastic bending stress was applied to the sample. The stress was applied to the sample by pulling a wire from outside of the dewar. The wire was attached to a lever pivoted on the holder. which caused the knife edge of the lever to push against the sample. The crystal growth and the sample preparation were described previously.' PHASE TRANSFORMATIONS The first phase transformation in this system is from the cubic perovskite structure to n tetragonal

Jan 1, 1970

By P. J. Spencer, J. N. Pratt

The vapor pressure of manganese over liquid Mn-Sn alloys has been determined by a high-temperature torsion-effusion technique. Alloys containing from 8 to 100 at. pct Mn were investigated in the temperature range jrom 1280" to 1580" and the measured pressure values were used to calculate the partial and integral thermodynamic properties of the liquid alloys. The activities show small negative departures from ideality while the integral heats and excess entropies of mixing are asymmetric inform, changing from positive to negative with increasing manganese content. The possible contribution of various factors to the observed thermodynamic properties is discussed. COMPARATIVELY few thermodynamic data are available for manganese alloy systems.' Therefore, as part of a continuing program of studies of the thermodynamic properties of transition metal alloys, measurements have been made on various binary alloys involving this element. In recent publications,2~3 investigations of liquid Mn-Cu alloys and of the Mn-Au system in both solid and liquid states have been reported. For the first-mentioned system the work suggested that magnetic interactions may be responsible for the observed form of the thermodynamic properties, while in the second the influence of the electrochemical factor appears to be dominant. The present paper describes a similar study of liquid Mn-Sn alloys. Again the thermodynamic properties have been obtained from vapor pressure measurements made by use of a high-temperature torsion-effusion technique.4 A detailed description of the apparatus and of the experimental procedures used in alloy preparation and pressure measurement may be found elsewhere.2'4 EXPERIMENTAL RESULTS Sixteen alloys, ranging in composition from 8 to 100 at. pct Mn, were prepared from spectroscopically standardized manganese of 99.99 pct purity and tin of 99.999 pct purity, both supplied by Johnson-Matthey and Co., Ltd. One-gram samples of the alloys were obtained by carefully weighing appropriate amounts of the pure components into an effusion cell; this was then suspended in the apparatus and the metals melted together in situ by heating under vacuum to approximately 1550°K. After allowing sufficient time for a homogeneous liquid alloy to be formed, vapor pressure measurements were commenced. These were determined as rapidly as possible at a series of steady temperatures within the range of interest. The duration of experimental runs on individual samples was kept sufficiently short to ensure insignificant varia- tion of alloy composition during investigation. After completing pressure measurements, the alloys were rapidly cooled and their compositions checked by weighing or chemical analysis. All experiments were conducted using effusion cells machined entirely from boron nitride. Measurements were made using a variety of cells with orifice areas ranging from 0.0032 to 0.0075 sq cm and lengths of the order of 0.04 cm; the usual effusion correction factors for orifice geometry and molecular distribution were calculated using Freeman and Searcy's equation5 and had values between 0.6 and 0.75 for the orifices employed here. The vapor pressures of manganese over the alloys were measured at approximately 20°K intervals in the temperature range 1280" to 1580°K. In view of the close approximation of the measured pressures to Clausius-Clapeyron behavior in the experimental temperature range, the data for each alloy have been expressed by equations of the form: logp(atm) =-A/T + B A least-squares computer treatment was applied to the vapor pressure values in order to obtain the coefficients A and B with their associated error. The resulting equations are listed in Table I, together with the equation for pure solid manganese obtained from a previous study.4 To minimize the effect of possible apparatus calibration errors, the activities and partial free energies of manganese in the alloys were calculated by initial reference to the latter equation, obtained from identical torsion-effusion measurements. The immediately resulting thermodynamic quantities, based on a solid manganese reference state, were then converted to refer to the more appropriate supercooled pure liquid manganese standard; tabulated values of the free energies of solid and liquid manganese from Hultgren et al.' were used for this purpose. Partial entropies of solution of manganese were calculated from the temperature coefficients of the free energies and partial heats from the Gibbs-Helmholtz relationship.

Jan 1, 1969

By P. Beardmore, B. W. Howlett, B. D. Lichter, M. B. Bever

The heats of formation at 273°K of the compounds Mg2Ge, Mg2sn, and Mg2b, the heats of fusion and melting points of Mg2Sn and Mg2Pb, and the heats of solution of magnesium, germanium, and lead in liquid tin have been measured. The excess free energies of the liquid alloys and the free energies of formation of magnesium-Group IVB compounds at their melting points and their standard free energies of formation at 298°K have been calculated. The stability and bonding of the compounds are discussed with reference to these properties. Some thermodynatnic aspects of the liquid phases in the systems Mg-Sn and Mg-Pb are also considered. THE compounds of magnesium with the Group TVB elements, silicon, germanium, tin, and lead, have often been considered to constitute a nearly ideal homologous series. In particular, their thermodynamic stability has been assumed to decrease with increasing atomic number of the Group IVB element.' The binary-phase diagrams of the magnesium-Group IVB elements given by Hansen and Anderko2 have the same form. Each system has a single con-gruently melting compound of limited homogeneity range. The structures of these compounds, which have the formula Mg2X, are anti-isomorphous with the calcium fluoride structure. A recent investigation has found evidence of a second compound in the system Mg-Pb.3 The solid compounds Mg2Si, Mg2Ge, and Mg,Sn are semiconductors, while the conductivity of Mg2Pb approaches that of a metallic conductor. This difference suggests that other properties may also show a discontinuity. The investigation reported here is concerned with the thermodynamic properties of magnesium-IVB compounds and particularly their variations with the period of the Group IVB element. The heats of formation at 273°K of the compounds MgzGe, Mg2Sn, and Mg2Pb and the heats of fusion and melting points of Mg2Sn and Mg2Pb have been measured. The results, combined with published data, are interpreted in relation to the stability and the bonding characteristics of the compounds. Some thermodynamic aspects of the liquid phases in the systems Mg-Sn and Mg-Pb are also considered. In the course of the investigation the heats of solution of magnesium, germanium, and lead in liquid tin have been determined. 1) EXPERIMENTAL PROCEDURES 1.1) Samples. Samples of the compounds Mg2Ge, Mg2Sn, and Mg2Pb, supplied by Professor P. Aigrain, Compagnie Générale de Télégraphie Sans Fils, were used in measuring heats of formation, heats of fusion, and melting points. Samples of Mg2Sn and Mg2Pb, supplied by Dr. V. B. Kurfman, Dow Metal Products Co., samples of Mg2Sn, prepared at the Air Force Cambridge Research Laboratories, and samples of MgzPb, prepared in this laboratory, were used for additional measurements of the heats of fusion and the melting points. The samples were stored in evacuated Pyrex capsules or under nonreacting liquids. 1.2) Heats of Formation. The heats of formation at 273°Kof the compounds Mg2Ge, Mg2Sn, and Mg,Pb were measured by tin-solution calorimetry. In this method, samples of the compound and of a mixture of the constituent elements are added alternately from 0°C to a tin-rich bath. The difference between the heat effects, corrected for the change in composition of the bath, is the heat of formation of the compound. Details of the method have been given elsewhere. 4 The bath was maintained at 350°C for the dissolution of the compounds MgzSn and Mg2Pb. Since at this temperature the dissolution of Mg2Ge was too slow, a bath temperature of 400" or 450°C was used with this compound. At least three calorimetric runs, each of approximately six additions, were made with each compound. 1.3) Heats of Solution. The determination of the heats of solution of magnesium, germanium, and lead in tin was included in this investigation because they were not well-established at the time this work was started. To obtain the heat of solution, the difference

Jan 1, 1967

By G. Ferrara

The reserves of lead and zinc ores in the metalliferous district of Iglesias in south-western Sardinia are today estimated at about 30 million tons, grading from 4 to 10% Pb + Zn. Of these reserves, about 40% are in the mines owned by AMMI Sarda S.p.A. The working of these resources goes back to ancient times. Not infrequently, traces of old Roman workings and remains of ancient implements are come upon in the higher parts of some of the ore bodies. Exploitation of these mines on larger scale, however, dates from the middle of the 18th century. Initially, the more accessible zones of the ore bodies and the richer ores were worked - the galena and the rich oxidized ores (calamine* with 25-35% Zn), which were often found in large masses, the enormous empty cavities of which still remain. The poorer grade deposits have been gradually rendered workable by the development of technology - the perfecting of the

Jan 1, 1970

Executive R. C. ALLEN, Chairman ERLE V. DAVELER, Vice-chairman WILDER JUDSON R. M. ROOSEVELT G. B. WATERHOUSE Finance H. G. MOULTON, Chairman HENRY KRUMB PAUL D. MERICA H. T. HAMILTON, Consultant Admissions W. B. HEROY, Chairman GEORGE D. BARRON, Vice-chairman H. T. HAMILTON PHILIP KRAFT W. A. SINSHEIMER

Jan 1, 1937

PRESIDENT Michael Lawrence Haider New York City PAST PRESIDENT Willis McGerald Peirce New York City VICE-PRESIDENTS 0. B. J. Fraser, New York City J. B. Morrow, Pittsburgh, Pa. J. L Gillson, Wilmington, Del. ' L F. Reinartz, Middletown, 0. Philip Kraft, New York City R. W. Thomas, Tucson, Ariz

Jan 1, 1952

PAST PRESIDENT WILLIS MCGERALD PEIRCE New York City PRESIDENT-ELECT AND TREASURER ANDREW FLETCHER New York City VICE-PRESIDENTS O B J FRASER, New York City J B MORROW,' Pittsburgh, Pa. J L GILLSON, Wilmington, Del L F REINARTZ, Middletown, O PHILIP KRAFT, New York City W THOMAS,' Tucson, Ariz.

Jan 1, 1952

By K. S. TWITCHEEL

THE different lines leading out from the vocation of a mining engineer are,' perhaps, the most' varied of all the professions. The expedition sent by Charles R. Crane of New York 'as a gift to the Imam Yahia, king of the Yemen, Arabia, was probably unique. Mr. Crane made a visit, in January,1927, to the Imam Yahia at Sanaa, capital of the Yemen. He was received with the utmost cordiality and respect, as his friend- . ship for the ,Arab world is famous; He was 'greatly impressed by the desire of the Imam to develop his country. The Imam stated that he had heard that there were minerals in his country and that he would like to secure engineers to advise him about them and other natural resources.. This seemed such a practical idea, and so greatly appealed to Mr. crane, that he offered to furnish an engineering 'expedition. Naturally the Imam gratefully accepted. This expedition was to study (as far as possible in 'the limited time) the natural resources of the ,Yemen, advise the Imam of what these consisted, and make suggestions regarding the most practical methods for their development. As agriculture is always such a fundamental part of a country's wealth, I first went to Indio, California, to study water-well drilling and the date industry, and eventually arrived at Hodeidah, the principal Yemen seaport, on Oct. 21, 1927.

Jan 1, 1929

By John W. Padan, John E. Crawford

Beginning with a small but positive participation in undersea mining, the Bureau of Mines continues its active investigations into this potentially tremendous field. The Bureau began its active role in undersea mining in September 1963, with a small task force of three dedicated scientists and a secretary, establishing headquarters at the old Tiburon Naval Net Depot about seven miles up the coast from San Francisco. The past months have been both busy and productive. With 22 Federal agencies involved in oceanography, it logically was the intent of Congress that the Bureau of Mines undertake research concerned only with the technology of marine mineral production and utilization. The Bureau has maintained this purpose in its activities at Tiburon, for while institutes, universities, the Navy and other Government agencies have developed exceptional programs in the fundamental science of the oceans, commonly called oceanographic research, little has been done toward advancing man's ability to exploit the ocean floors other than by drilling for oil and gas and sulfur.

Jan 3, 1965

By H. A. McKinstry, F. F. Lange

A vector analysis of orientating single crystals using the Laue back-reflection X-ray technique is given. Briefly, the analysis involves using a few data taken from a Laue photography and defining the crystal co- ordinate axes in a reference coordinate system. After a few matrix multiplications, the proper goniometer angles can then be determined to orient the crystal coincident with the reference frame. This analysis is easily programed for a digital computer to provide a fast, precise, and efficient method of orienting many crystals which are identical. The general procedure is as follows. The crystal is mounted on a goniometer. Laue photographs are taken until an array of diffraction spots is observed that includes a Laue spot that represents a rotational axis of symmetry. The rotation angles of goniometer are recorded. These angles are defined as positive for a counterclockwise rotation. When the axis of symmetry is located on the Laue photograph, the crystal coordinate axes can be defined in the reference coordinate system* as follows. Two Laue spots are chosen, one of which corresponds to the rotational axis of symmetry and the other to a set of planes whose zone axis is a known crystallographic direction and normal to the rotation axis of symmetry. The Laue spots are used to determine these two crystal directions in the reference coordinate frame. This is done by placing the Laue photograph on a sheet of polar coordinate graph paper and determining the polar coordinates (r, o) of these two diffraction spots in the reference coordinate frame. Their third coordinate is the distance between the crystal and the film (-D). The coordinates Xni of the two crystal directions Nn, (n = 1, 2) in the reference frame are then calculated by the following equations: Xn1 = -D X2n = Ancos on X3n = A, sin on where -tan- 1 rn/D An =Dtan(tan-1rp/D/2) By taking the proper cross products of these two directions (normalized to unit vectors), the crystal coordinate axes 3 (i = 1, 2, 3) can be determined in the reference frame. This is illustrated in Fig. 1. The next step is to determine the relation between

Jan 1, 1969

By Floyd C. Kelly

A. HUltgren, .Söderfors, Sweden (written discussion*).—From the results obtained in his own experiments as well as those of Austin and of Grube Mr. Kelley derives a general law, expressed tentatively in the following words: "whenever two metals are brought into intimate contact at a temperature at which diffusion takes place, a comparatively rapid, or abnormal, grain growth results." It is suggested that,, in order adequately to represent the facts, this definition should he restricted by the following qualifications: a and b are the two metals, b diffusing into a. A. At the temperature in question a should exist as phase a 1 having a limited solubility for b. B. The supply of b by diffusion should be sufficient, in view of the rate of diffusion into a 1, to increase the concentration of b above the saturation value in a 1 so as to cause a new phase a2 to form. (7. The phase a2 should have a range of solubility for 6, thus rendering continued diffusion possible. D. In order that the columnar grains may be preserved in the structure the phase a2 should, of course, not suffer transformation on cooling. The phenomenon thus defined may be described as progressive transformation by diffusion. Its mechanism would appear to he as follows: Fig. 17 shows a portion of the equilibrium diagram a-b, Fig. 18 the distribution of b in solution after various periods of diffusion, Fig. 19 represents the structure in cross-section of a cylindrical rod of a at the end of heating period 3. 1. The first effect of diffusion of b into a will be to establish a concentration gradient in phase a1 (1, Fig. 18). When the saturation value for the temperature of the experiment (m, Fig. 17) is reached at the surface, nuclei of, a2 of composition n will form here, and later develop into a continuous layer. Assuming that diffusion proceeds without irregularities and that transformation at any point sets in without lag—i. e., in the moment saturation is exceeded—the transformation a1-a2 will advance inwards on a cylindrical surface concentric with the surface of the rod. The discontinuity of composition at the transformation surface in the position it happens to have at the end of the treatment (3, Fig. 18) will be preserved at room temperature, if the cooling is not particularly slow, and be recorded in the structure as a marked, smooth line, in agreement with Grube's and the author's observations. The shape of the distribution curves in Fig. 18 is also corroborated by the analyses given by Grube. 2. During diffusion, since the secondary phase a2 is always in immediate contact with the saturated part of the primary phase a1, there should be very little lag in the transformation. This means that the first a2 grains formed should grow in preference to the formation of independent nuclei; in other words, columnar growth results. It does not seem necessary to assume, with Green,' whose conception of the phenomenon

Jan 1, 1929

By Floyd C. Kelly

A. HUltgren, .Söderfors, Sweden (written discussion*).—From the results obtained in his own experiments as well as those of Austin and of Grube Mr. Kelley derives a general law, expressed tentatively in the following words: "whenever two metals are brought into intimate contact at a temperature at which diffusion takes place, a comparatively rapid, or abnormal, grain growth results." It is suggested that,, in order adequately to represent the facts, this definition should he restricted by the following qualifications: a and b are the two metals, b diffusing into a. A. At the temperature in question a should exist as phase a 1 having a limited solubility for b. B. The supply of b by diffusion should be sufficient, in view of the rate of diffusion into a 1, to increase the concentration of b above the saturation value in a 1 so as to cause a new phase a2 to form. (7. The phase a2 should have a range of solubility for 6, thus rendering continued diffusion possible. D. In order that the columnar grains may be preserved in the structure the phase a2 should, of course, not suffer transformation on cooling. The phenomenon thus defined may be described as progressive transformation by diffusion. Its mechanism would appear to he as follows: Fig. 17 shows a portion of the equilibrium diagram a-b, Fig. 18 the distribution of b in solution after various periods of diffusion, Fig. 19 represents the structure in cross-section of a cylindrical rod of a at the end of heating period 3. 1. The first effect of diffusion of b into a will be to establish a concentration gradient in phase a1 (1, Fig. 18). When the saturation value for the temperature of the experiment (m, Fig. 17) is reached at the surface, nuclei of, a2 of composition n will form here, and later develop into a continuous layer. Assuming that diffusion proceeds without irregularities and that transformation at any point sets in without lag—i. e., in the moment saturation is exceeded—the transformation a1-a2 will advance inwards on a cylindrical surface concentric with the surface of the rod. The discontinuity of composition at the transformation surface in the position it happens to have at the end of the treatment (3, Fig. 18) will be preserved at room temperature, if the cooling is not particularly slow, and be recorded in the structure as a marked, smooth line, in agreement with Grube's and the author's observations. The shape of the distribution curves in Fig. 18 is also corroborated by the analyses given by Grube. 2. During diffusion, since the secondary phase a2 is always in immediate contact with the saturated part of the primary phase a1, there should be very little lag in the transformation. This means that the first a2 grains formed should grow in preference to the formation of independent nuclei; in other words, columnar growth results. It does not seem necessary to assume, with Green,' whose conception of the phenomenon

Jan 1, 1929

By M. J. Marcinkowski, D. Koskimaki, A. S. Sastri

THIS is the second in a trilogy of investigations carried out in order to understand the solid state transformations and their accompanying effects on the deformation behavior of near-equiatomic Ni-Ti alloys. The first stage of this effort has dealt with the strictly martensitic structures obtainable in these alloys, i.e., those in which diffusion processes were not involved.1,2 These martensites could be produced either by rapid quenching or by plastic deformation of the originally B2 type phase. The present investigation, on the other hand, will deal with those transformations in Ni-Ti which do involve diffusion. A majority of investigators3-10 have shown that the B2 modification of TiNi, which is stable at elevated temperatures, decomposes into one or both of the intermetallic compounds NiTi2 and Ni3Ti below about 650°C. On the other hand, this has been disputed by several Workers was undertaken in order to resolve this discrepancy, as well as to shed more light on the nonmar-tensitic decomposition of B2 NiTi. EXPERIMENTAL PROCEDURE Sample preparation, fabrication, and examination were the same as those described previously in Ref. 2. In addition to the 50 at. pct Ni (55.06 wt pct) hypoeu-tectoid alloy used previously, a second hypereutectoid alloy containing 54.4 at. pct Ni (60 wt pct) was also prepared for this study. RESULTS AND DISCUSSION The equilibrium diagram for the Ni-Ti alloy system in the vicinity of Ni-Ti is shown in Fig. 1. The solid lines have been established by the work of Poole and ~ume-Ftothery4 whereas the dotted lines are based on findings obtained in the present investigation as described below. Structure and Morphology. Fig. 2(a) shows a bright field transmission electron micrograph of a two-phase structure obtained in a polycrystalline Ni-Ti alloy that was furnace cooled (approx 200°C per hr) from 1050' to about 300°C. Large plate-shaped precipitates can be observed in a matrix which was found by electron diffraction to possess the high temperature B2 structure. A selected area diffraction pattern of the region covered by Fig. 2(a) is shown in Fig. 2(b), while Fig. 2(c) is a detailed schematic interpretation of Fig. 2(b). The B2 matrix reflections are illustrated by squares while those of the precipitate are shown as circles. The d values associated with the precipitate reflections could be determined quite accurately since the reflections from the B2 matrix, for which the lattice constant is known precisely, were simultaneously present in the diffraction patterns. All of the reflections

Jan 1, 1970

By D. S. Eppelsheimer, D. N. Williams

The cold rolled textures of iodide titanium and of three samples of commercial titanium were examined using the Schulz-Decker Geiger counter technique. The iodide titanium and two of the three samples of commercial titanium showed a (0001) [1010] texture rotated 30' toward the transverse direction about an axis in the rolling direction. The third sample of commercial titanium showed a double texture. THE metals of the hexagonal system tend to deform similarly if the c/a ratios are similar. Thus titanium, zirconium, and beryllium, with c/a ratios of 1.601, 1.590, and 1.570, respectively,l should have similar cold rolled textures. The cold rolled texture of high purity iodide titanium has been described as (0001) [1010] rotated 30" toward the transverse direction about an axis in the rolling direction.' The texture of zirconium has also been reported as (0001) [1010] with a transverse rotation from the ideal position of approximately 30" about an axis in the rolling direction." This texture differs from that reported for titanium however since a continuous spread of (0001) poles toward the transverse direction was reported rather than distinct (0001) maxima 30" from the rolling plane normal. Beryllium has a texture similar to that of zirconium although the angle of transverse rotation of the (0001) poles is much less.' These three metals thus show a common type of cold rolled texture, as yet unexplained, which can be described as (0001) [1010] with various degrees of rotation toward the transverse direction about an axis in the rolling direction. Since titanium showed the greatest degree of rotation from the (0001) [1010] position, the cold rolled texture of titanium was re-examined using a semiquantitative Geiger counter X-ray technique to obtain more accurate experimental data from which a theoretical interpretation of this new type of hex- agonal rolling texture could be developed. The cold rolled textures of iodide titanium and of three samples of commercial titanium were determined. Table 1 gives the analyses of the titanium samples. Experimental Procedure Preparation of Samples: Prior to the final rolling operation each of the samples was given an initial reduction of approximately 50 pct and annealed to remove the gross effects of any previous treatments. Samples were annealed in vacuum, high purity helium, and air to determine whether annealing atmosphere had any effect on the cold rolled textures developed. All samples were annealed 1 hr at 800°C. Grain size determinations were made using the formula, 1.075 in which n is the number of grains counted in an area A (in sq mm) and M is the magnification of the area counted.' This formula gives the diameter between opposite flats assuming hexagonal grains. At least three areas containing more than sixty grains each were counted in each grain size determination. Rockwell B hardness readings were made on the annealed samples. The results of the measurements of

Jan 1, 1954

By A. D. McMaster, M. L. Gimpl, N. Fuschillo

Low-power, high-speed, radiation-resistant, monolithic thin-film integrated circuits require thin-film resistors of high sheet resistance which are compatible with the processing requirements for monolithic silicon devices. For this purpose the structure and electrical resistance as a function of temperature were investigated for Nichrome-silicon monoxide cermet films on passivated single-crystal silicon substrates. A suitable material was found to be a mixture of 50 vol pct Nichrome-50 vol pct silicon monoxide. This mixture, when evaporated onto 300°C substrates. showed a low temperature coefficient up to 400°C, at both 270 and 1100 ohms per square. Resistors deposited on room-temperature, 300°, and 500°C substrates were heat-treated at 600°C in air for short periods of H- seed, low-power, radiation-re sis tant, monolithic thin-film integrated circuits'-3 require thin-film resistors of high sheet resistance and low temperature coefficients of resistance which are compatible with the processing requirements for monolithic silicon active devices. The present investigation is directed towards the replacement of the Nichrome in the sandwich-type SO2-Nichrome-SiO resistors, currently used for DTL monolithic thin-film integrated circuits, with codeposited Nichrome-SiO cermet resistors. These Nichrome-SiO resistors are provided with an overcoat of SiO and are deposited onto thermally oxidized silicon wafers used in monolithic mi-crocircuit technology. The cermet resistors are shown to provide a lower temperature coefficient of time totaling up to 45 min. Electron nzicrogvaphs and diffraction patterns were taken of the as - deposited and heat-treated films. These results were then compared with electrical-resistance measurements for each condition. The room-temperature and 300°C substrate films showed a large decrease in resistance. The 500°C substrate film remained stable throughout the entire cycle. Electron-microscopy results show that the increased stability after heating to 600°C is largely due to crystallization of the films which begins in the vicinity of 400°C. The slight oxidation of the films when heated in air had a negligible effect on the resistance. The resistance of the film was a function of the substructure. resistance and a more versatile compatibility with silicon monolithic processing. Previous work3, on chromium-SiO coevaporated cermet resistors on glass and ceramic substrates without overcoats of SiO has been reported. For the present application, the thin films should possess the following ideal requirements: a) a temperature coefficient of resistance as near zero as possible up to 300°C; b) have a sheet resistance higher than 200 ohms per sq to conserve space on the chip; c) be easy to evaporate; d) be oxidiation- and radiation-resistant; e) show long-time stability at 100°C; } be stable in N2 atmospheres up to 600°C for short periods of time (5 to 45 min). Requirements a to e are well-known. The last requirement was optional and was due to a mask elimi-

Jan 1, 1967

Jan 1, 1943

Jan 1, 1943

Jan 1, 1936

Jan 1, 1936

By S. D. Michaelson

[CONTENTS PACE See TP 2377, Min. Tech, May 1948 for discussion of A Technique for Photographing Difficult Subjects through a Petrographic Microscope (TP 2092 by DONALD W. SCOTT, Min. Tech., Nov. 1946. Discussion by HORACE WINCHELL). Metallurgical Efficiency-a Yardstick in Lead-zinc Flotation Metallurgy (TP 2141 by R. A. ....... PALLANCH, Min. Tech:, March 1947. Discussion by S. D. MICHAELSON). I Symposium on Milling Devices and Practices. (TP 2162 by J. F. MYERS and R. J. TOWER, Min. Tech., May 1947. Discussion by HARLOWE HARDINGE). ............ 2 Rod Milling-Plant and Laboratory Data. (TP 2175 by J. F. MYERS, S. D. MICHAELSON and F. C. BOND, Min. Tech., July 1947. Authors' supplement and discussion by HARLOWE .......................... HARDINGE, and B. H. IRWIN) 2 A New Separating Vessel for Sink-float Concentration. (TP 2182 by E. C. BITZER, Min. Tech., May 1947. Discussion by E. H. CRABTREE, JR.) .................. 5] Metallurgical Efficiency-a Yardstick in Lead-zinc Flotation Metallurgy S. D, MICHAELSON*-The method of determining the efficacy of a separation described in this paper, gives the metallurgist a most useful guide for keeping his ship on an even keel When the ore Waves vary from placid seas to high breakers. Now that such a method of evaluating metallurgical efficiency has been developed and proven practical, it Would seem logical to introduce the next, and more final, factor of Economic Efficiency. I choose to define this term as the percentage ratio of net return from milling to the theoretical maximum net return. The actual operating cost subtracted from the actual mill return represents the net actual amount received for the material treated. Experienced operators of most plants Would ordinarily have enough data on hand to estimate a theoretical milling cost per ton, based on labor, power, supplies and maintenance When operating at maximum tonnage With minimum trouble and under ideal ore conditions. When this theoretical estimated cost is subtracted from the theoretical maximum ore return (calculated by Pallanch's method) the resulting figure is the maximum theoretical net amount the mill operator could hope to realize in processing the ore. The percentage ratio of these sums, of actual to theoretical, is the economic efficiency of the operations. This economic efficiency, if determined on the basis of a fixed market price for metal and similarly fixed base rates for labor, power and supplies, Will reflect the effect of changes in milling practice, labor efficiency and equipment condition. When computations made on the basis of actual current rates for labor, power and supplies are compared With similar actual figures for past periods they will show forcefully how energetic our hunt must be to develop man saving controls, more effective metallurgy, and better equipment to maintain profitable operations. Such computations also offer a simple means of determining how much more labor, supplies and power can be put into the mill operation to obtain an increase in metallurgical recovery at a profit.

Jan 1, 1947