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By W. M. Lehrer

RECENT development of high-temperature brazing alloys has required information regarding the eutec-tic temperature and composition of the Pd-rich section of the Pd-B system.. Literature on this subject was found to be scanty with no complete system yet determined. Buddery and welch1 report an inter-metallic compound occurring in the Pd-B system at 6.33 wt pct B (PdsBz). Another source, Sieverts and Bruning,2 indicates that after annealing at 700°C, a 1.6 and a 2.0 wt pct B alloy were two phase whereas a 0.75 pct B alloy was single phase. Recent work3 using a hot-stage microscope has proposed a eutectic temperature of 743OC. This method utilized the observation of the onset of incipient melting at grain boundaries. The eutectic composition, however, was not determined. METHODS AND PR0CEDURES Five alloys were prepared by triple inert arc-melting high-purity palladium (95.98 pct) with additions of 2 to 6 pct purified amorphous boron. The alloys were crushed within a hardened steel mortar with a steel pestle. The 2 pct alloy, however, was too tough to be crushed in the above manner so was crushed by successive reductions through a rolling mill. Approximately 17 to 18 g of the crushed alloy was used in the thermal analysis. The alloys were melted in pure quartz crucibles. The thermocouple protection tubes were also of quartz and fused along the inside wall of crucibles to prevent floating of the thermocouple. This was an expediency as centering of the thermocouple in the melt would have been preferable. Melting was done in a tube furnace with a slow flow of tank helium maintained as a protective atmosphere. Heating and cooling rates were maintained at 3.5OC per min through the critical temperature ranges by means of a synchronous motor hook-up to a furnace controller. All specimens were heated to 100°C over the indicated liquidus on heating prior to reversing to the cooling cycle. Specimens emerged from the furnace with mirrorlike brightness attesting to the protective quality of the helium atmosphere. Thermal arrests were detected by the differential thermocouple technique using chrome l-alumel couples and nickel as the reference specimen. Arrests were recorded on a Leeds-Northrup automatic X-Y recorder. The specimen temperature and temperature difference were read to + 7.5OC and ± 1.5OC, respectively. These readings were well within the sensitivity of the instrument amplifier. Chromel-alumel couples were used in lieu of Pt-Rh as very few arrests were contemplated in excess of 1200" to 1300°C, the approach of instability. No standardization was performed on these thermocouples subsequent to their use. RESULTS The thermal arrest temperatures obtained are plotted in Fig. 1 as a function of wt pct B. The composition function was obtained by chemical analysis of portions of the specimens after the thermal analysis was completed. The 2 to 6 pct nominal alloys were found to have 1.80, 2.35, 3.65, 4.18 and 5.90

Jan 1, 1960

By H. F. Weaver

The 18th National First-Aid and Mine Rescue Contest was held in the Memorial Auditorium, Buffalo, New Vork, October 5, 6, and 7, 1959. The meet was sponsored by the Federal Bureau of Mines and the Joseph A. Holmes Safety Association, in cooperation with State mine inspection agencies, management and labor of the mineral extractive industries, and other safety minded groups. The Arrangements Committee, as authorized by the General Committee, made a11 the necessary arrangements for conducting the 1959 contest. Members of the Arrangements Committee were: Harry Gandy, Jr. (chairman), National Coal Association; James B. Benson, Southern Coal Producers' Association; Charles Ferguson, United Mine Workers of America; George C. Trevorrow, Bituminous Coal Operators' Association; and James Westfield, Federal Bureau of Mines.

Jan 1, 1960

By H. D. Hess

This report describes in detail a unique occurrence of fersmite, (Ca, Ce, Na) (Cb, Ti, Fe, Al)2 (0, OH, F)6, which occurs as small anhedral inclusions and intergrowths with a tantalum-free columbite found in the metamorphic complexes of Ravalli County, Mont. Chemical and crystallographic data along with the physical and optical properties agree in general with those given in the original description of fersmite from the Ural Mountains of Russia. X-ray diffraction data not given in the original description and more specific optical data have been determined. The Montana fersmite, now established as the second occurrence of this rare calcium-columbate mineral, was discovered during a routine Bureau of Mines mineralogical examination of a prospector's sample.

Jan 1, 1960

President W. K. Dennison, Jr., called the final session of the Rocky Mountain Coal Mining Institute to order, and introduced H. A. Cornell, Portland Cement Association, Ft. Collins, Colorado. Mr. Cornell explained that the Portland Cement Association was not a sales organization, but is supported by the major manufacturers of portland cement. The research laboratories of the association are constantly endeavoring to improve the quality of cement, as well as promote new markets, new uses, and new ideas. The association works with engineers, contractors and universities, making available to them the results of their research. Mr. Cornell stated that numerous booklets and bulletins were available on request for any phase of construction with concrete. Mr. Cornell presented a film, "How to Make Quality Concrete," to the members of the Institute. D. W. Lyke, General Electric Apparatus Service Shop, Denver, Colorado, was introduced by President Dennison, who presented a film, "A-Hunting He Would Go." Following the film, Mr. Lyke stated that his firm was not confined to electrical equipment, but to all types of equipment, and asked the members to feel free to call for assistance at any time. These two films concluded the Manufacturer's Hour, and President Dennison opened the final business meeting of the session. Robert F. Bowie, of the Auditing Committee, read the Treasurer's Report, and complimented Mr. Whiteside on the commendable state in which the books were found. The Treasurer's Report is as follows:

Jan 1, 1960

"M bed, Matanuska valley, Alaska, coal carbonizingproperties B 510M spectral lines, low-energy, study RI 5538Mab shaft, Leadvile district, Colo., investigation RI .1518Maberry process, for aluminum chloride TP 321"

Jan 1, 1960

By C. R. Ross

"THE ASSESSMENT of pneumoconiosis-producing dusts in mines and other industries is usually undertaken for one or more of three reasons: (1) To compare dust exposures at particular operations with standards of permissible dustiness in order that hazards may be evaluated and preventive procedures initiated where required.(2) To study particular operations with the objective of improving dust control devices or procedures by locating dust sources. (3) To obtain data which, along with the results of medical investigations, may assist in understanding the causes of dust-induced diseases or aid in the establishment of permissible standards of dustiness. Most dust measurements are made for the first of these reasons -to evaluate dust hazards so that they may be controlled. For this purpose, four quite different assessment techniques have been in widespread use for many years. One of these is based on the konimeter, an instrument familiar to most .Canadian mining men; a second on the impinger, which is also widely used in Canada, and almost exclusively so in the United States; a third on the thermal precipitator, used extensively in Britain and South Africa; and a fourth on the tyndallometer, a light-scattering instrument used in Germany."

Jan 1, 1960

By R. E. Reed, R. D. Leggett, Paxton, H. W.

TECHNIQUES have been developed for growing monocrystals and bicrystals of Fe-20 Cr, Fe-20 Cr-20 Ni, and Fe-18 Cr-8 Ni alloys by both the strain-anneal and the Bridgeman techniques. None of the techniques are new but since they are simple and many people have expressed interest, they are described here quantitatively as they could be modified for other single-phase "commercial" materials of high melting point. CRYSTAL GROWTH BY STRAIN ANNEAL Flat tensile specimens with a tapered gage length were initially studied to deduce the approximate critical strain. Normal flat tensile specimens were then used. The optimum procedure for the austenitic steels (Fe-Cr-Ni) deduced from a variety of cold reductions, recrystallization treatments, tensile strain, and growth anneals was as follows: cold reduce 70 pct, recrystallize (after machining tensile specimens) at 1000°C for 1 hr, strain in tension 2.5 pct, and then heat to 1350°C as rapidly as possible. A time of 100 hr at 1350°C is usually sufficient to pro-

Jan 1, 1960

By J. W. Rutter, K. T. Aust

The motion of individual grain boundaries under a constant driving force was investi,qated for zone-refined lead, with and without solute tin additions. The rate of boundary migration was found to depend strongly on tin content and on the orientation relationship between the adjacent grains. The results are compared with the theory of impurity-controlled grain boundary miqration developed by Lucke and Detert. Evidence was found that grain boundaries separating grains which have the Kronberg-U&apos;ilson orientation relationships of 38 and 22 deg about <Ill> and 28 deg about <100>, correspond to boundaries of high mobility. The results are discussed in relation to the formation of annealing textures in metals and the structure of high-angle boundaries. It is generally known that small amounts of impurities in solid solution greatly influence the re-crystallization behavior of metals. For example, the addition of 0.005 at. pct of tellurium to copper,&apos; or 0.005 at. pct of silver to lead,2or 0.01 at. pct of manganese or nickel to aluminum3 greatly decreases the rate of recrystallization of these metals. However, this effect may be the combined result of a decrease in the rates of both nucleation and growth; recrystallization experiments do not separate these two factors. Bolling and winegard4 determined the effects of small quantities of tin, silver, and gold on grain growth in polycrystalline zone-refined lead.

Jan 1, 1960

By R. O. Williams

A recent article by Chernock, Singer, Mueller, and Beck 1 which supports the use of the integral of I sin $ d$ for comparing fiber texture data does not settle what happens to I sin ø as ø approaches zero, where I is the diffraction intensity for poles oriented 0 deg from the fiber axis. They indicate that they believe that it should approach some constant value (that is, I increases without bound) and the fact that in reality it does not was a result of the diffraction

Jan 1, 1960

By W. J. Wenger

THIRTY-FOUR analyses of crude oils from the fields of the Four Corners Area of Arizona, Colorado, New Mexico, and Utah are presented and compared. The samples, taken from formations in four geological time periods, have high gravity and low-sulfur, -nitrogen, and -asphalt content. Generally, the oils are paraffinic in the low-boiling fractions, with increasing naphthenicity in the higher-boiling fractions. Oils from Cretaceous formations resemble other Cretaceous oils in the Rocky Mountains, but oils from Permian and Pennsylvania formations are unlike other oils of these ages in the Rooky Mountains. The differences in the oils are minor and cannot be used to distinguish between fields or between producing formations. With minimum special processing, the oils should yield large amounts of good-quality motor fuels. INTRODUCTION The only place in the United States where four States have a common junction is known as the Four Corners Area. This area (fig. 1) includes the northeast corner of Arizona, the southwest corner of Colorado, the northwest corner of New Mexico, and the southeast corner of Utah. It includes three major geological basins: The Black Mesa, the San Juan, and the Paradox. Major oil developments have occurred in both the San Juan and Paradox basins, but no discovery of commercial importance has been made in the Black Mesa basin.

Jan 1, 1960

By H. H. Heady

A naphtha obtained by destructive, recycle hydrogenation of crude shale oil, produced by gas-combustion retorting of Colorado oil shale, was found by the Bureau of Mines to contain 49.1 percent paraffins, 20.3 percent cycloparaffins, 7.8 percent olefins, and 22.8 percent aromatics. The naphtha contained only minor amounts of sulfur, nitrogen, and oxygen compounds. Compounds containing less than 5 carbon-atoms per molecule were removed by distillation before analysis. The paraffins where predominantly straight-chain compounds; n-Hexane was present in the largest quantity, and the other straight-chain paraffins decreased in amount as the molecular weight increased. The cycloparaffins, which contained both cyclopentanes and cyclohexanes, were evenly distributed throughout the boiling range. Although the naphtha had been produced by hydrogenation, it contained a small quantity of olefins. Straight-chain olefins with a terminal double bond comprised about two-thirds of these compounds. Among olefins with an internal double bond, those having trans configuration were present in three times the quantity of those in the cis form. In the aromatics all but one of the alkylbenzenes having nine or less carbon-atoms per molecule were identified; toluene was present in the greatest quantity. Only a few of the higher molecular-weight homologs were identified. The composition of the naphtha was computed from analyses of 105 narrow¬boiling distillation fractions. Volume, density, refractive indices, bromine number, and an ultraviolet spectrum were determined on each fraction. From these data the hydrocarbon-group composition of each fraction was estimated. A silica gel adsorption analysis was used to check the values of nearly one-third of the fraction calculated from physical-property data. Mass and infrared spectra were obtained on some fractions for identifying individual compounds or types of compounds, such as terminal olefins.

Jan 1, 1960

By J. R. Mihalisin, J. S. Iwanski

The response of Inconel "700" to heat treatment has been studied by light and electron microscopy combined with X-ray and electron diffraction techniques. A heat treatment which vesults in low ductility for this alloy appears to be associated with the formation of MC carbide in a Widmanstdtten distribution. This type of precipitation can be suppressed by suitable heat treatment with concurrent increase in ductility. Various other phases precipitated in this alloy are also identified. RECENT studies of commercial nickel base su peralloys have demonstrated the importance of the morphology of carbide phases upon physical properties.&apos; For example, empirical heat treatment studies applied to Nimonic "80" and Inconel "X" have resulted in prescribing double aging treatments for optimum physical properties. These treatments have subsequently been related micro-structurally to grain boundary carbide morphology.2 The purpose of this study was to obtain information about the morphology and identity of some of the phases precipitated in Inconel "700" after heat treatment. It was hoped that some correlation could be made of micro structure with heat treatment similar to that observed with Inconel "X" and Nimonic "80." EXPERIMENTAL PROCEDURE Specimens were obtained from a hot-rolled bar of Inconel "700" of the following composition: C Mn Fe S Si 0.10 0707 0.42 0.007 0.12 Cu Cr -A1 -Ti- Co Mo Ni 0.02 -14.90 TM 2.22 27.61 2.92-- Bal. Specimens were prepared in the following heat-treated conditions: (A) 2275°F for 2 hr WQ (B) 2275°F for 2 hr WQ + 2000°F for 1 hr (C) 2275°F for 2 hr WQ + 1600°F for 48 hr. (D) 2275°F for 2 hr WQ + 2000°F for 1 hr + 1600°F for 48 hr. Empirical stress-rupture studies had shown that treatment (D) resulted in optimum stress-rupture life and ductility. Treatment (C), although giving a good aging response, resulted in low ductility. Treatments (A) and (B), respresenting individual. steps in treatments (C) and (D) were added here for microstructural comparison studies. The procedure was to make an optical and electron microscopic investigation supplemented by X-ray diffraction analysis of electrolytically extracted residues. Electron diffraction studies were made utilizing selected area diffraction techniques with extraction

Jan 1, 1960

By C. G. Dunn, J. L. Walter

SILICON-iron .under certain conditions of processing and annealing will form a cube texture. The occurrence of this texture in thin tapes of silicon iron was first reported by Assmus, Detert, and Ibe.&apos; They concluded that the cube texture in their material formed by a secondary re crystallization process. In the course of present investigations on the development of the cube texture and the mechanisms involved in its formation by secondary re-crystallization it was found that under certain conditions the cube texture was replaced by a cube-on-edge or (110) [001] texture. We call this phenomenon tertiary re crystallization since it follows secondary recrystallization. The secondary recrystallization occurs after primary recrystallization and a substantial amount of normal grain growth. It is the purpose of this paper to describe briefly the occurrence of tertiary recrystallization and the structure and texture prior to and after tertiary recrystallization. The primary and secondary recrystallization structures and textures are the subject of another study and will be referred to briefly in the discussion of results. Evidence will be presented for the view that the dominant driving force for tertiary recrystallization is derived from the surface free energy which depends on the crystallographic planes presented to the gas-metal interface. In the absence of boundary restraining forces (dispersed phases, thermal grooves, and so forth) a sufficiently large difference in surface free energy across a grain boundary would produce boundary migration away from the center of curvature of the boundary intersection line in the surface of the sample according to risher.2 Therefore, particular attention was paid to observation of the direction of motion of these surface boundary lines. Furthermore, measurements of the actual boundary curvatures could be used to estimate the driving force supplied by surface free energy. EXPERIMENTAL PROCEDURE Samples were prepared by hot and cold-rolling vacuum-melted ingots of iron containing 3 pct Si to strips 0.012 and 0.006 in. thick. The ingots contained less than 0.005 wt pct impurities. The rolled strips were cut into samples approximately 1 in. wide by 3 in. long and were electropolished to remove surface imperfections. All samples were annealed in a vacuum at a pressure of approxi-

Jan 1, 1960

By M. M. Wong

A brief investigation was made to determine the feasibility of electro-refining beryllium in a KCI-LiCI-BeC12 bath. Thin, platelike crystals of beryllium metal were produced by electrolyzing technical-grade beryllium metal beads (about 94-percent purity) as the soluble anode. Operating cell conditions were: Temperatures of 450° to 600° C.; an inert atmosphere; bath compositions of (1) 38.1 mol. percent KC1, 54.8 mol. percent LiCl, and 7.1 mol. percent BeC12 and (2) 36.7 mol. percent KC1, 52.7 mol. percent LiCl, and 10.6 mol. percent BeC12; cell voltages of 0.30 to 0.80; and initial cathode current densities of 50 to 435 a./sq, ft. Current efficiencies ranging from 87 to 96 percent were obtained. Qualitative spectrographic analyses of the metal products indicated that impurities were reduced. This technique offers the possibility of producing a grade of beryllium purer than that now generally available, which may have better mechanical properties.

Jan 1, 1960

By G. R. Wilms

In a recent investigation1 on the properties of chromium, and of Cr-10 wt pct W and Cr-5 wt pct Mo alloys at elevated temperatures, it was found that intercrystalline cavities developed in all of these materials during tensile creep at 950°C, and that the cavities led to intercrystalline fracture. There were some interesting differences, however, between the cavities produced in the pure metal and those in the alloys; these differences, moreover, were associated with a difference in ductility. The relevant conditions of creep testing are specified in the captions to Figs. 1 and 3. Chromium showed the presence of quite large intercrystalline cavities, Fig. 1, and these were more or less randomly distributed around the boundaries. The chromium alloys, on the other hand, showed the presence of both small cavities and cracks at the grain boundaries, Fig. 3; it is apparent that the cracks are formed by the linking together of the small cavities. Moreover, the cavities and

Jan 1, 1960

By Harold W. Lipper

BUREAU OF MINES helium plants produced a. record-breaking 477 million cubic feet of this essential element in 1959. The supply of helium was less than the demand before operations were resumed at the Navajo plant in July and begun Sit a. new plant at Keyes, Okla., in August. Helium was in abundant supply after August, and the informal allocation system which had been in use intermittently since 1955 was discontinued Delivery of 26 new tank cars in August and September increased the total in the tank-car pool to 163. Defense and space agencies and the Atomic Energy Commission continued to use more helium in their operations and research.

Jan 1, 1960

By F. C. Langenberg, J. Chipman

New data on the distribution of silicon between slag and carbon-saturated iron at 1600oand 1700oC are presented which, in combination with previously published data, permit the determination of silica activities over a broad range of compositions in the CaO-Al2O3-SiO2 system. The distribution of silicon between graphite-saturated Fe-Si-C alloys and blast furnace-type slags in equilibrium with CO has been described in previous publications.1"3 In this past work the silica-silicon relation was established at temperatures of 1425" to 1700°C for slags containing up to 20 pct Al2O3. This paper presents the results of additional studies at 1600" and 1700° C which extend the silicon distribution data at these temperatures for CaO-A1203-SiO2 slags over a range from zero pct A12O3 to saturation with A12O3, or CaO.2A12O3. The upper limit of SiO, is set by the occurrence of Sic as a stable phase when the metal contains 23.0 or 23.7 pct Si at 1600" or 1700°C, respectively. The activity of silica over the expanded range is determined directly from the distribution data.3 Recently, 4-7 other investigators have studied the activities of SiO, and CaO, principally in the binary system, using different methods and obtaining somewhat different results. EXPERIMENTAL STUDY The experimental apparatus and procedure have been fully described in previous publications.1, 3 Six new series of experimental heats have been made, four at 1600° and two at 1700°C. Master slags of several fixed CaO/A12O3 ratios were pre-melted in graphite crucibles, and these were used with additions of silica to prepare the initial slag for each experiment. Slag and metal were stirred at 100 rpm and CO was passed through the furnace at 150 cc per min. The initial sample was taken 1 hr after addition of slag at 1600°C or 1/2 hr after addition at 1700°C. The run was normally continued for 8 hr at 1600°C or 7 hr at 1700°C, and the final sample was taken at the end of this period. Changes in Si and SiO2 content indicate the direction of approach to equilibrium, and in a series of runs where the approach is from both sides this permits approximate location of the equilibrium line. Fig. 1 shows the results of such a series of 15 runs at 1600°C for slags of CaO/Al2O3 = 1.50 by weight. Figs. 2 and 3 record other series at 1600°C and Fig. 5 a series at 1700°C with fixed CaO/Al2O3 ratios. The results of the experiments at 162003°C have been reported in part in a preliminary note.3 In the experiments recorded in Figs. 4 and 6, the slags were saturated with A12O3 (or with CaO.2A12O3 within its field of stability) by suspending a pure alumina tube in the melt during the course of the run. The final slag analyses were used to establish the liquidus boundaries8 in the stability fields of CaO.2Al,O3 and of A120,. ACTIVITY OF SILICA The free-energy change in the reaction has been calculated by Fulton and chipman2 from recent and trustworthy data including heats of formation, entropies, and heat capacities. The more recent determination by Olette of the high-temperature enthalpy of liquid silicon is in satisfactory agreement with the values used and therefore requires no revision of the result which is expressed in the equation: SiO, (crist) + 2C (graph) = Si + 2CO(g.) [1] &F° = + 161,500 - 87.4T The standard state for silica is taken as pure cristobalite and that of Si as the pure liquid metal. Since the melts were made under 1 atm of CO and were graphite-saturated, the equilibrium constant for Eq. [I] reduces to K1 = asi /asio2 The value of this constant is 1.77 at 1600°C and 16.2 at 1700°C. Through K1, the activity of silica in the slag is directly related to the activity of silicon in the equilibrium metal.

Jan 1, 1960

By John W. Barnes

In seeking cost reductions, control methods are a fertile field because they significantly affect labor and other costs. While process control in uranium mills is excellent by the evidence of high recovery, the costs seem high to those familiar with extractive operations for other metals. To some extent this high cost is inevitable, because of exacting quality control-, the technically complicated recovery processes; poor control over grade and nature of mill feed- special problems arising out of the radioactive property of the material. Practices used in uranium mills and the limitations indicated for instrumentation and automation are discussed. It is concluded that any large investment in automatic controls should be preceded by a careful study of their reliability and maintainability, and an estimate of the net income after taxes smaller plants my find it more profitable, or at least less risky, to concentrate their efforts on the possible reduction of some control problems and to development of a stable force of skilled employees. The observed experience does not inspire optimism that ore-dressing plants can be extensively automated although certain unit operations offer a challenge for improvements in instrumentation and machine design.

Jan 1, 1960

By T. A. Henrie

The Federal Bureau of Mines has investigated methods of sodium reduction of titanium chlorides to produce high purity titanium metal (14).4/ This investigation was made to obtain a better understanding of the reactions involved in sodium reduction of titanium chlorides and was part of the Bureau&apos;s activities toward improving the technology of titanium. Theoretical and experimental evidence show that sodium reduction of titanium tetrachloride occurs by stepwise reactions. The first stage reduction between sodium vapor and vapors of titanium chlorides produces titanium di-and trichlorides which subsequently condense with sodium chloride to form a salt mixture. The second stage reduction takes place in the condensed salt mixture between sodium and titanium subchlorides. Final reduction is a heterogeneous reaction between two separate phases, the a phase which consisted of sodium dissolved in sodium chloride and the ß phase titanium subchlorides dissolved in sodium chloride. The mechanism of the heterogeneous reaction between these phases is electrochemical in nature. The model proposed is a galvanic reaction at the interfacial region.

Jan 1, 1960

By Niles E. Grosvenor

Several methods have been proposed for determining the tensile strength of rock. These have been tried out over the past several years, but the results have been erratic and of doubtful value. The tensile strength of rock is its weakest property, and this property apparently enters into all failure phenomena whether underground or on the slope of an open pit. Therefore, it is essential that detailed quantitative information is known about the tensile strength of rock if the design engineer is going to select the proper pit&apos; slope, pit orientation, or orientation of underground workings so as to give the most economical and safest mining condition. This quantitative information may be used to orient the pit in such a manner as to allow steep slopes along two sides. This information may possibly be used to orient the direction of either underground workings or open pits so as to decrease powder consumption and to increase blasting efficiency. Hence it is of prime importance that a method of determining accurately the tensile strength of rocks be developed.

Jan 1, 1960