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By Frank W. Clinard, Oleg D. Sherby

The effect of multiple an transformations on diffusion in a dilute iron alloy was studied. Inter-penetration between iron and an Fe-Co alloy was evaluated, under thermal-cycling conditions chosen so as to transform only the iron-rich side of the diffusion couple. It is shown that a small but consistent diffusion enhancement by a factor of two results when data from the transforming side of thermally cycled specimens are compared with predicted inter diffusion coefficients based on isothermal data. No enhancement is found when data from the mntransforming side of such couples are compared with predicted diffusivities. It is suggested that short-circuiting by moving pain boundaries is the most likely mechanism contributing to the observed diffusion enhancement from multiple phase transJormations in iron. Transformation-induced Point defects, dislocation-pifie short-circuiting, and point defects generated by dislocation motion are less effective in contributing to enhanced diffusion under the experimental conditions utilized. SO far as is known, no studies have been made of the effect of allotropic transformation on diffusion. previous to this investigation. Studies have been made, however, of the influence of transformation on the diffusion-controlled processes of spheroidization and sintering. Cullen1 has described a method of accelerating spheroidization in an AISI 1030 steel. Partial transformation between a and ? phases was uti-

Jan 1, 1965

The structure of the Bulli coal seam at Appin Colliery was detailed by the seismic reflection method. This unusual application of the seismic method was possible because there is a reflector near the seam as was revealed during exploration for petroleum in an area north-west of Appin. The reflector, which was at a depth of 1,500 ft, was shallow by normal reflection survey standards. Measurement of the seismic velocity at two ventilation shafts showed that the reflector was probably the Bulli coal seam. Accurate depth control was established from previous drilling results.INTRODUCTIONAppin Colliery, situated on the Southern Coalfield of N.S.W. (Fig. 1), is being developed to supply coking coal to the Port Kembla steelworks of Australian Iron and Steel Pty. Ltd. The colliery is mechanized and a detailed knowledge of structure, particularly faulting, is important in planning the workings.The Bulli seam, which is approximately 9 ft thick, and between 1,500 ft and 1,800 ft below the surface, is worked in the colliery. It is the uppermost member of the Permian Coal Measures and is overlain by Triassic rocks, which consist of thick sandstone beds containing beds of coloured shales, and which are subdivided into the Narrabeen Group, the Hawkesbury Sandstone, and the Wianamatta Group.In the early stages of development of the colliery, surface geological mapping and diamond drilling provided information on structure. Generalized results of the mapping are shown on Fig. 2. Drilling indicated that the physical and chemical properties of the Bulli seam are relatively constant, and that the seam is nearly horizontal, the average dipbeing about 1 in 25 to the west.

Jan 1, 1965

The Cowarra gold mine is at latitude 36°O'S. and longitude 149°19'E. which is roughly 20 miles north-north-east of Cooma.The deposit was· originally worked towards the end of the last century, but the presence of sulphides associated with the gold in the primary zone caused cessation of work when that zone was reached.GEOLOGY AND MINERALIZATIONThe principal country rocks are sandstones and shales of Silurian and Ordovician age, both very strongly folded with structural pitches ranging from a few degrees to almost vertical. The mine proper is within Silurian rocks and the main orebody (there are several minor parallel bodies) is developed within a shear striking approximately north, dipping approximately 70° east, and ranging in width from 2 ft to 15 ft but averaging about 4 ft.This shear is impregnated with quartz and sulphides with which the gold is associated. The predominant sulphide is pyrite though pyrrhotite is commonly present in quantity.Arsenopyrite and bornite are present in smaller amounts.Stillwell (1936, 1937a, 1937b, 1938, 1941) has published five mineragraphic reports on the ore.The various levels have been mapped in detail (Figs. 1-3) and the No. 2 level plan (Fig. 1) shows the general relationship of shearing, as now indicated by mineralization, and faulting. There is no apparent connection between the fold structures and mineralization.Fig. 3 is a longitudinal projection showing the distribution of gold expressed as inch-ounces. The estimation of...

Jan 1, 1965

By William R. Hess

Volcanic ash, although a little-used Kansas resource, is available in forty counties with estimated, reserves of more than 20 million tons. It was first produced in Kansas in the early 1900?s but not until the early 1920 is did it become an important abrasive material. Total production to date is estimated at 2 million tons, the major use being as an abrasive in scouring compounds and soaps, additional uses include ceramic glazes, an additive in cement, and a filler and stabilizer in hot mix asphalt for paving. Unrecorded tonnages have also been used in construction of black-top (macadam) roads. From 1916 through 1944, Kansas ranked first among the states in volcanic ash production; peak production was about 52, 000 tons in 1923. Since 1945, production has steadily declined, primarily because materials other than volcanic ash are now being used for abrasives; only two producers operated in 1964.

Jan 1, 1965

By D. G. Westlake

Polycrystalline tensile specimens of various Zr-0-H alloys have been tested at 298°, 178°, and 77°K. Solute oxygen and hydride precipitates in quenched alloys made individual contributions to the yield strength at 0.2 pct strain which combined to produce a resultant strength increment, a,., Ductility changes which were ohserved can he interpreted in terms of the various oxygen and hydrogen concentrations, testing tem -peratures, and dispositions of the hydride. ADDITIONS of oxygen in solid solution were known to increase the yield and tensile strengths of polycrystalline zirconium as early as 1951.' More recently, the critical resolved shear stress (CRSS) for prism slip in zirconium single crystals was also shown to be affected by the solute oxygen impurity.' This latter work also demonstrated that large increments of strength could be contributed by the finely dispersed zirconium hydride precipitates that are present in quenched Zr-H alloys.3 It was concluded that the combined strengthening due to alloying could be expressed by where to is the increase in the CRSS due to solute oxygen alone and TH is the increase due to finely dispersed hydride precipitates. Eq. [I] is analogous to one used to express the combined strengthening effects of work hardening and neutron radiation damage.4 Eq. [1] was verified only indirectly and for only small amounts of the impurities—up to 0.14 at. pct 0 and 0.63 at. pct H. The present investigation was undertaken to obtain a more direct verification of the validity of the form of Eq. [1] for this system and also to determine the combined effects of oxygen and finely dispersed hydride precipitates on the tensile strength and ductility of polycrystalline zirconium. EXPERIMENTAL PROCEDURE Tensile specimens were machined from the same rolled billet of Kroll zirconium used in the earlier study.' These measured 38 by 4.7 by 0.5 mm and had 10-mm gage lengths which were 2.8 by 0.5 mm. Each specimen was ß-annealed in vacuo at 1173°K for 15.5 hr and a-annealed at 1073°K for 4 hr to D. G. WESTLAKE, Member AIME, is Associate Metal l ur-gist, Metallurgy Division, Argonne National Laboratory, Argonne, III. Manuscript submitted July 17, 1964. IMD______________ give an equiaxed structure with grain diameters averaging 0.06 mm. Oxygen was added by allowing the metal to react with a known quantity of oxygen during the 0 anneal and known quantities of hydrogen were added during the a anneal. Each alloy was encapsulated in Pyrex under vacuum, annealed at 873°K for 4 hr, quenched into ice water, and polished by immersion in a solution of 46.75 vol pct H2O, 46.75 vol pct concentrated HNO3, and 6.5 vol pct HF (49 pct) at 298°K. Special heat treatments given to a few specimens are described in the results below. Tensile tests were done on an Instron machine and were begun within 20 min after the quench, except where specified otherwise. Tests at 298°K were in air, at 178°K in acetone, and at 77°K in liquid nitrogen. All tests were at a strain rate of 8x sec-1. RESULTS AND DISCUSSION Yield Stress at 298°K. The compositions of alloys and the corresponding yield stresses (0.2 pct strain) are given in Table I. A plot of the yield stresses of the oxygen alloys, A, B, C, and D, indicates that varies linearly with CO1/2, where Co is the oxygen concentration, Fig. 1. This is in accord with Fleischer's6 theory for solution strengthening if the oxygen atoms do not cluster, or the cluster size remains constant with increasing oxygen concentration. In Fig. 1, it appears that if one could prepare some oxygen-free zirconium its yield stress would be very low. Therefore, we shall assume that for the oxygen alloys is equivalent to O0, the strength increment contributed by the presence of oxygen. The relationship between0.2and Co is expressed by 0.2 = 31.3 CO1/2, when the yield stress is in kg per sq mm and the concentration is in at. pct. Each of the hydrogen alloys, Al, A2, A3, and A4, contained 0.081 at. pct 0 as an impurity. In Fig. 1, it appears that this small amount of oxygen makes a significant contribution to the strength which cannot be ignored when we evaluate the contribution of the finely dispersed hydride. Let us assume the validity of the following equation: a0.2 = (a2o+a2R)1/2 [2] which is analogous to Eq. [I] for single crystals, and calculate values of UH for the hydrogen alloys by using the experimental values of 0.2 and o (0.081 at. pct) = 8.9 kg per sq mm. For 0.36 at. pct H, oH = 6.47; for 0.72 at. pct H, OH = 11.30; for 2.16 at. pct H, OH = 19.4; and for 3.60 at. pct H,

Jan 1, 1965

By C. O. Hawk

Distillable oils derived from coal were desulfurized and hydrogenated at 2,500 psig in a two-step vapor-phase catalytic operation to give a product rich in saturated cyclic hydrocarbons. The first step was mainly a desulfurization at 400 C, the second a saturation at 300 C. One of the oils used as feed stock was from low-temperature carbonization of a bituminous coal, the other was from the liquid-phase hydrogenation of coal in the Bureau's pilot plant. The product from the saturation step was distilled to remove the light ends and high-boiling residue and to recover a fraction having acceptable properties with respect to heating value, density, freezing point, viscosity, and boiling range according to specifications suggested by the Air Force for ultra-high-speed aircraft fuel. Quantities of the fuel fraction available were too small for the thermal stability test approved by the Air Force. The experiments, performed on laboratory scale, comprised mostly a study of the effect of varying the oil feed rate (at constant oil-to-hydrogen ratio) on the yield of the desired fuel fraction. The yield of the fuel fraction made from low-temperature carbonization oil was a little more than 1 percent of the weight of coal carbonized; that from coal-hydrogenation oil was about 12 percent of the weight of coal hydrogenated. A few attempts to do both desulfurization and saturation in one operation with sulfur resistant catalysts, developed for vapor-phase hydrogenation or hydroforming, were unsuccessful. By leaving the low-boiling ends in both feed stocks to desulfurization, another product was obtained: a low-sulfur aromatic cut boiling below 200 C. This material would be suitable as a solvent or a chemical raw material.

Jan 1, 1965

By R. T. DeHoff

A new approach to the measurement of the size distribution of particulate structures imbedded in opaque bodies is developed. The method is based upon the assumption of a general two-parameter distribution curve, and the estimation of these two parameters from three well-known counting measurements made upon metallogvaphic sections. The total number of particles in the system is also a product of the analysis. Application of the method with the assumption of the logarithmiconorma1 disfribution function is developed in detail. A complete description of the geometry of a particulate structure requires the determination of the size distribution of particles. The problem of estimating the size distribution of particles of a particular phase in a multiphase system, or the grain-size distribution in a homogeneous system, has been approached by many investigators.'-'0 All of the solutions proposed by these investigators share the following characteristics. a) A minimum of several hundred particle sections in the microstructure must be examined, and some characteristic dimension recorded, such as area,3'5 intercept length,6"9 or diameter.1'2'4'10 b) The resulting data must undergo a series of fairly complex calculations to generate the empirical histogram which describes the size distribution in three dimensions. c) In order to manipulate the result, the histogram must be fitted to some assumed mathematical formula, using the attendant statistical procedures. d) With two notable exceptions,8,10 the particles must be spherical. The measurements and calculations involved are in general very tedious and time-consuming, with the logical result that much effort has been expended in the development of equipment which will perform these tasks automatically and semiautomati-cally.9,11-15 considerable success has been achieved in this area, but the equipment is in general expensive, and usually places stringent requirements On the quality of microstructure which can be reliably analyzed. In laboratories which do not possess such equip- ment, the analysis of geometry is usually limited to measuring total properties of the microstructures, such as volume fraction and interfacial area, because the measurements required are much simpler to make. The determination of size distributions rarely is undertaken. The development which is presented in this paper permits the estimation of size distributions of three-dimensional structures from the same simple counting measurements which are required to determine the surface area and volume fraction of the particulate structure, and one other counting measurement. The basic approach that is used is to assume a general mathematical form for the distribution, which is described by two parameters (as the normal distribution is described by assigning values to the mean and the standard deviation), and then estimate these two parameters from the results of the counting measurements. The introduction of a third counting measurement also permits the evaluation of the number of particles per unit volume, Nv.

Jan 1, 1965

By R. A. Meussner, R. J. Goode

Six intermediate phases occur in the Nb-Zn sysThese phases form by peritectic reactions at 1120°, spectively. The Nb Zn 15 phase appears as the minor phase in the eutectic structure, and the terminal phases remain nearly pure niobium and zinc even at high temperature. Vapor -pressure measurements on the four high-temperature phases (Nb Zn to Nb Zn 3) permitted estimates of the composition limits of these phases and the calculation of approximate values of AFO, AH°, and AS°. 1 HE present study of the constitution of the binary Nb-Zn system was a part of an analysis of the mechanism by which coatings of the Nb-Zn intermediate phases protect niobium against oxidation at high temperature.' Since the primary interest in these phases was in coating service, attention in this study was given principally to the four phases stable at high temperature with only cursory attention to the two low-temperature phases. The solubility studies of niobium in zinc by Martin, Knighton, and Feder2 and the reports from the present study of the Nb-Zn coating represent the only published data pertaining to this system. Previously Hodge, Evans, and Hoskins, in an experimental survey, had noted that niobium was not resistant to attack by molten zinc, but no further observations were reported. EXPERIMENTAL PROCEDURES a) General. The nature of the binary Nb-Zn system precluded the use of more conventional methods of determining the phase equilibria such as thermal analyses of a series of cast alloys. An extrapolation of the liquidus data of Martin, Knighton, and Feder2 to higher temperatures suggested that the solubility of niobium in zinc would remain low in the entire temperature range of interest. The preliminary results of the present studies showed that all of the high-temperature intermediate phases form by peritectic reactions. Thus the sluggish nature of this type of reaction and the steepness of the liquidus indicated that thermal analyses would not yield reliable data. The peritectic reactions, of course, precluded the direct formation of samples of the individual phases from the melt. b) Materials. The niobium and zinc used in the present studies were of high purity. The niobium, in the form of 0.1-in.-diameter rods, contained 30 ppm 0, 30 ppm N, and 15 ppm C. Aside from 0.05 pct Ta, the metallic impurities (iron, titanium,

Jan 1, 1965

By A. P. Herring, S. F. Ravitz

Manganese dioxide reacts with sulfur dioxide solution in the absence of oxygen to form manganous ion and dithionate ion, together with a small amount of sulfate ion. The effects of SO, concentration, hydrogen ion concentration, stirring speed, and temperature on the rate of the reaction were studied. If it is assumed that undissociated SO2 molecules react rapidly with MnO, at active surface sites and that bisulfite ions react slowly, an equation can be derived that satisfactorily represents the observed reaction rates. For solutions in which the reaction with undissociated SO2 predominates, reaction rates and activation energies estimated from diffusion theory agree well with those found experimentally. Manganese dioxide dissolves readily in aqueous solutions of sulfur dioxide. The nature of the dissolution reaction was first investigated by Gay-Lussac and welter1 in 1819; they identified a new oxysulfur radical, the dithionate ion, S2O6, as one of the reaction products. Since then, the reaction has become a standard method of preparing dithionates in the laboratory and one of the more promising methods of leaching manganese from low-grade ores. In the "dithionate process" developed by the U.S. Bureau of Mines2,3, manganese-dioxide ore is suspended in a solution of calcium dithionate and leached with gas containing sulfur dioxide. The manganese is dissolved and the sulfur dioxide is oxidized according to the reactions:

Jan 1, 1965

By Douglas J. Lootens

Geologic mapping was undertaken in the Sierrita Mountains as part of a Doctoral program at the University of Arizona, Tucson. During the study, approximately 35 square miles was mapped in detail, with particular attention given to specific areas of great or significant structural complexity and their relation to mineralization in the vicinity. A combination, of field studies and photogeologic interpretation was used in order to define regional and local structural controls for disseminated copper-molybdenum mineralization in and adjacent to the study area. Gratitude is expressed to the faculty of the University of Arizona, Department of Geology for their assistance in this work and to Bear Creek Mining Company for making numerous reports and drill cores available for study.

Jan 1, 1965

By Roger Bell

Most modern mines can profit from improvements in information handling. Recording systems in many cases were designed to satisfy certain necessary legal requirements, but not specifically to provide management information. As a consequence, the top managements of these properties work with cost data and production information that is dated, lacking in detail and clouded with supposition. It is the intent of this paper to describe an information system for a mine-plant complex in terms of the type of data, application areas and the existing equipment technology that may be applied to improve this situation. The economics of information processing and data handling will not be discussed in detail. This paper is based on the premise that information is something of value and that information processing like a manufacturing operation works for and is subject to management control. Information, the product, must be of quality, and the cost must be favorable in terms of its use.

Jan 1, 1965

By H. A. Schrecengost

Information presented herein was gathered by examination of 29 fluidized- bed thermal coal dryers and by conferences with manufacturers and users of such equipment to determine what safety features could be incorporated in design, installation, and operation to minimize fire and explosion hazards. Fire and explosion hazards are inherent in certain types of coal dryers in that high temperatures are employed; the sizes and volatility of material handled are capable of propagating explosions; and drying gases are seldom, if ever, low enough in oxygen content to prevent ignitions of dust clouds, distilled gases, or their combinations. This is especially true for fluidized- bed dryers in which the coal is dried in air suspension and in which atmospheric air is constantly introduced to temper the heated furnace gases. Occurrence of fires on heated bedplates, in dust collectors, and in hot gas inlets was common in nearly all the dryers examined. Forceful explosions which produced external effects had occurred in 11 (39 percent), and internal "puffs" or "bumps" had occurred in at least 24 (79 percent) of the plants examined in the study.

Jan 1, 1965

By J. G. Donaldson

Cobalt-tungsten binary deposits were formed in laboratory experiments by hydrogen reduction of the anhydrous mixed vapors of cobaltous chloride and tungsten hexachloride. The materials were sublimed in seperately heated zones of reaction tube and were transported in a stream of purified helium into the deposition section of the tube where the chloride gases were reduced to metal by a countercurrent flow of hydrogen. Heattreating of the near stoichiometric binary metallic deposits converted nearly all to the intermetallic compound Co3W, however, small quantities of both cobalt and tungsten remained. Mechanical tests showed that the tensile strength of heat-treated 75 percent cobalt-25 percent tungsten deposits was twice as high as that of similarly treated deposits of cobalt.

Jan 1, 1965

By John L. Miles

John L. Miles (Arthur D. Little, 1nc.)—Pollack and orris" have reported measurements on electron tunneling through A1-A12O3-A1 sandwiches in which the oxide was formed by gaseous oxidation in a glow discharge. From these measurements they deduced the asymmetry of the barrier and, since this is small, conclude that the mechanism suggested by Mott19 for the growth of oxide in thin A12O3 films is inapplicable. In earlier papers20 Pollack and Morris report similar work for oxide films grown thermally. In this case they find a greater asymmetry and conclude that the Mott mechanism is valid. I would like to point out that both these conclusions are quite unjustified. Mott suggests that the growth of the oxide film on aluminum results from the passage of ions through the already present film of oxide under the action of an electric field. This field results from a constant voltage which is in effect a contact potential between metal on one side of the barrier and adsorbed oxygen ions on the other side of the barrier. The theory does not require that the oxide grown is nonuniform either in stoichiometry or structure. It does however specifically assume that the partial layer of ionized oxygen on the surface remains adsorbed on the surface of the growing oxide. In other words, the so-called "built-in field" remains in the oxide only as long as the ionized oxygen is present. When a counter electrode of aluminum is deposited on the oxide, it will react with the adsorbed oxygen on the surface of the oxide, thus forming a small additional amount of oxide. It is clear, then, that there is no requirement in the Mott theory of oxide growth which would necessitate tunneling currents through an Al-A1203-A1 sample to be different when the polarity is reversed. Neither does the theory eliminate the possibility that some additional mechanism could cause the tunneling barrier to be asymmetric and hence tunneling currents to be a function of polarity in such a sandwich. Thus these tunneling-currents measurements are not germane to the question of whether the Mott mechanism is the true method of growth of aluminum oxide films. In fact, it is not surprising that there should be a difference between the oxide properties at the two interfaces (with resulting asymmetry in the tunneling barrier) since the growth conditions and growth rates must have been quite different at these two positions. S. R. Pollack and C. E. Morris (authors' reply)— The point raised by Miles above is one has caused some confusion in the past. The following is an attempt to clarify this point. The built-in field which is responsible for the growth of the thermal oxide at low temperatures arises, according to Mott, because of the passage of electrons from the Fermi surface of the oxidizing metal to surface states introduced by the adsorbed oxygen. It is assumed that the energy of these surface states lies below the Fermi energy of the metal. Electrons therefore continue to flow from the metal to the surface until the built-in electric field raises the potential energy of the surface states to the value of the Fermi energy in the metal, at which time equilibrium is obtained between the surface states and the metal. That is in equilibrium as many excess electrons pass from the metal to the surface per unit time as vice versa. The surface of the oxide prior to deposition of a metallic counterelectrode can then be pictured as follows. The Fermi energy lies in the energy gap of the oxide and is essentially pinned at the energy of the oxygen surface states. The vacuum work function of the oxide is then given by the sum of the electron affinity of the oxide (i.e., the difference in energy between the vacuum and the conduction-band minimum) plus the energy difference between the conduction-band minimum and the Fermi energy. The deposition of a metal onto the surface of the oxide can result in a transfer of electrons across the extremely thin oxide only if there is a contact potential difference between the deposited metal and the parent metal or oxide. That is if the vacuum work function of the deposited metal differs from that of the parent metal, then charge can be redistributed across the oxide in order to equilibriate the Fermi energy across the structure. (It should be

Jan 1, 1965

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The room-temperature Knoop hardness of single -crystal titanium diboride has been determined. Variations in microhardness have been correlated with orientation and structural imperfections in the crystals. Maximum differences in hardness values of 750 kg per sq mm with respect to orientation and 450 kg per sq mm with respect to substructure were found. The effects of etchants, load on indenter, and degvee of cracking of indentation were studied. The average hardness was determined as 2800 kg per sq mm on the as-grown crystals. Annealing increased the average hardness to 3375 kg per sq mm. ThE microhardness of polycrystalline titanium diboride approximating the stoichiometric composition TiB, has been studied by several investigators. The values for the Knoop hardness number range from 2710 kg per sq mm (Khn = 2710 kg per sq mm) to 3400 kg per sq mm.'-4 Samsonov et al.' reported a Vickers hardness number of 3400 kg per sq mm (Vhn = 3400 kg per sq mm) at 120-g loads for a 98 pct Ti + B material of 96 pct theoretical density. Recently Dunegan measured the Vickers hardness and obtained 2060 kg per sq mm with a 10-g load (Vhnlo = 2060 kg per sq mm), 1425 kg per sq mm for Vhnloo, and 1320 kg per sq mm for Vhnlooo. We have obtained a Khnloo = 3000 * 350 kg per sq mm for hot-pressed polycrystalline TiB2 that was 99.1 pct Ti + B and 96.6 pct of theoretical density. The present investigation has been made on single-crystal titanium diboride boules, and is believed to be the first such study on TiB, crystals of known orientation. EXPERIMENTAL The single crystals were prepared by a Verneuil-type process using an electric arc by the Linde Division of Union Carbide Corp. The largest specimens were 6 mm in diameter by 12 mm long. The crystals were of theoretical density (4.50 g per cm3) with a Ti + B content of 99.8 pct. The major impurities present were: 0.03 pct (by weight) 0, 0.06 pct C, 0.01 pct Si, 0.05 pct Fe, 0.01 pct Cr, and 0.01 pct Ni. The crystals were boron-rich, the average boron content being 31.S7 wt pct (stoichiometric value is 31.12 wt pct), and titanium-poor, the average titanium content being 68.2 wt pct (stoichiometric value is 68.88 wt pct). Titanium was determined gravimetrically by cupferron precipitation and boron by titration of H3B03 from a NaOH-fused specimen after removal of titanium with BaC03. The outer edge of the boule accounted for some of the excess boron. An electron-microprobe analysis showed that the titanium content increased from 60.0 wt pct at the edge to 68.5 wt pct at D, ~ 1000 p, where D, = distance from outer edge (see Fig. 5). X-ray measurements indicate that the boules are single crystals with considerable substructure. Upon etching this structure is seen in the form of a Widmanstatten-type rhombohedral line pattern in the basal (c) plane and a parallel "lines" pattern in the prism (a) planes. A typical WidmanstHtten-type pattern is seen in in Fig. 1. Electron microscopy reveals that the lines are less than 1 p across, which does not allow direct electron probe or microfocus X-ray determination of their composition. The identity of the second phase has not been established. It might be a higher boride or a nonstoichiometric TiB2. On annealing above 2200°C the precipitate is dispersed and dissolves in the matrix. The best etchants found were HF/HNO/HO, KF(CN)$NOH/HO (Murakami's Etch), and A large number of other etchants were previously Studied. The acidic etchant produced an acicular or "needles" pattern in the (a) planes which is an etchant effect on the "lines" pattern.

Jan 1, 1965

By Wallace W. Key

The California pesticide industry in 1962 consumed about 30,000 tons of clay, talc, limestone, diatomite, sulfur, and other minerals as fillers (carriers and diluents) in pesticide formulation. This was 10 percent of the U.S. filler requirement for pesticides. About two- thirds of the California total was supplied by a few local mineral producers; the remainder came mainly from Florida, Georgia, and Wyoming. The objectives of this report are to provide data on quantities, sources, specifications, and market conditions for minerals used as fillers by California pesticide formulators. The study disclosed that specifications for mineral fillers have become more rigid and formulators have become more numerous in recent years. During 1962 over 1,200 firms registered 16,000 pesticide products with the Bureau of Chemistry in California. Factors which will tend to diminish future need for mineral fillers include the trend toward greater use of organic sprays rather than dusts and further development of biological controls, such as the development of sterile insect strains.

Jan 1, 1965

By J. Buchwald, R. W. Heckel

THE DeHoff method' of analysis of ellipsoids of constant shape provides a quantitative metallo-graphic technique whereby the actual size distribution of the ellipsoids may be determined from polished and etched random planar sections. This method provides a useful metallographic tool since it appears to be the only method available for determining the size distribution of nonequiaxed second-phase particles. This method, however, assumes that the type of particle being studied is known to be either oblate or prolate of a fixed minor to major axis ratio, q. This, in general, means that one assumes either oblate or prolate ellipsoids of a given q and checks the total volume and surface area of the second phase as determined from the particle size distribution to values of these quantities determined by other techniques. Suitable check methods may be point counting, lineal fraction, and areal fraction methods for obtaining the total volume and the Smith and Guttman2 method of intercepts for obtaining the total surface area. If the initial guess at particle shape and q were incorrect, i.c., the volume and surface information obtained from the particle size distribution data does not agree with those values obtained by other techniques, another assumption must be made and the particle size dist distribution must be recalculated. A current study in this laboratory has involved a large number of these calculations. To facilitate the handling of the calculations, the DeHoff method was programmed in the FORTRAN language for an IBM 1620 computer. The purpose of this note is to briefly describe this program. The complete program along with a list of variable names, a sample input, and a sample output may be obtained from the senior author. Basically, the program provides for the calculation of particle size distributions for a series of q values for both oblate and prolate ellipsoids for each set of input data. The total volume of second-phase particles per unit volume are calculated for each calculated particle size distribution. The output of the program is arranged to allow a rapid comparison of the calculated volume and surface values to data obtained by independent check measurements. A condensed flow chart of the program in the notation of DeHoff1 is given in Fig. 1 The calculation of the number of particles per unit volume in the jth size class, Ni, according to the DeHoff method' is: where k(q) is the shape-correction factor given by DeHoff as a function of q for both oblate and prolate ellipsoids, A is the size-class increment, k is the number of size classes, ni is the number of particles in the ith class on the planar measurement surface, and B(j,i) are the saltykov3 coefficients which correct for measurement surfaces which do not pass through the major and minor axes of the particles. The values of /3(j,i) are included as a two-dimensional array in the program. Particular values of k(q) are included in the program in increments of q of 0.05. The first calculation is carried out for q = 1 (spheres), the second for q = 0.95 oblate, the third for q = 0.95 prolate, and so forth. The number of q values chosen for the calculation is determined by a control card in the input for each set of data.

Jan 1, 1965

By D. R. Mathews

Electrorefined vanadium was evaluated with respect to tensile properties and the effects of interstitial contaminants in the temperature range of 77° to 273° K. The yield strength of 18,500 psi and hardness of 63 diamond pyra-mid hardness (DPH) of electrorefined vanadium are approximately equal to that of iodide crystal bar vanadium. The ductile-brittle transition temperature was found to be below 77° K, but with 0.175 weight-percent oxygen or 0.10 weight-percent nitrogen, it increased to between 123° and 190° K. With carbon content up to 0.11 weight-percent, the transition temperature remained below 77° K. The yield strength of the interstitial-containing alloys can be expressed by: au = 7.5 + 480 (pct N) + 290 (pct 0) + 280 (pct C), where au is the upper yield stress in 1,000 psi at 273° K. Profuse deformation twinning occurred in the alloys tested at 77° K. However, twinning could be suppressed by dissolved oxygen or nitrogen in excess of 0.15 and 0.086 weight-percent, respectively. Carbon, even though present in excess of the solubility limit, did not affect twinning.

Jan 1, 1965

By P. E. Palmer, A. H. Daane, C. E. Habermann

Jan 1, 1965

By Joseph Grumer

The range of composition of gases synthesized from solid fuels which are exchangeable with natural gas on current gas appliances was evaluated by theoretical principles. These principles consider primarily the flashback, blowoff, and yellow-tipping characteristics of air-entraining burner flames. It was found that complete identity between the synthetic and natural product is not necessary. Gases such as may be obtained by hydrogasification of coal and other solid fuels without the removal of unreacted hydrogen offer advantages in flame characteristics. Between 25 to 37 percent hydrogen can be tolerated in the sendout gas.

Jan 1, 1965