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By David A. Edgecombre

This paper discusses modern practices in the extrusion of steel. Particular emphasis is given to a description of the Ugine Sejournet method of extrusion, involving the use of glass as a hot work lubricant. Other methods are also mentioned. A brief history of extrusion is presented; present practices in the quality extrusion of tubing and solids are described; and the future potentials of the) process as a tonnage producer are briefly discussed. The advantages of extrusion and the reasons for the use of a glass lubricant, as well as the various methods of using glass, are given. The process, as described, is being used in the manufacture of large commercial quantities of stainless steel tubing and sections. This extrusion process is an essential and unique means of forming such atomic-age materials as titanium, zirconium, molybdenum and other super alloys all of which are materials required in the creation of nuclear installations.

Jan 1, 1963

By Ganesh P. Mohanty, James J. Wert

THE brittleness of the intermetallics usually render their deformation studies at ordinary temperatures using conventional techniques inadequate. On the other hand, although X-ray line broadening measurements is not a complementary technique, it provides a means for gaining limited but useful information on the cold worked state of these materials. In the present instance, a study of the effects of cold work in the lead telluride intermetallic compound was carried out by analyzing the diffraction profiles of the deformed and the corresponding annealed samples. An ingot of PbTe was prepared by induction melting high-purity lead and tellurium in a quartz crucible under an atmosphere of argon. After homo-genization, the ingot was ground to -325 mesh at room temperature, and using a polished die the cold- worked powder was pressed into the form of flat faced briquets for diffraction measurements. A spectrometer with 0.125 deg per min scanning velocity, CuKa radiation, pulse height analyzer, and a proportional counter were employed in the X-ray measurements, and the powder peaks were collected from the sample in fully cold-worked state and after it had been annealed to relieve the effects of cold work completely. For reliable estimates of the peak extremities, small angular ranges where the tails merged into the background were point counted. Fourier inversions of the experimental peaks were carried out in an IBM 705 computer using the procedures introduced by stokes.' Both the cosine and sine components of the Fourier series were used to take into account any peak assymetry arising

Jan 1, 1963

By C. H. Li, J. A. Sarteli, W. Bonfield

The stress to cause a permanent micros train of 2 x 10-6 in. per in. (defined as the microscopic yield stress) in beryllium is found to be very sensitive to surface condition. The initiation of plastic flow in as-machined specimens, which contain a high density of twins and large residual compressive stresses to a depth of about 0.010 in. from the surface, occurs by the nucleation of slip from high stress fields around twin tips in the surface layers. Removal of the damaged surface layers by chemical polishing results in an appreciable increase in the microscopic yield stress, which is attributed to the remoual of stress raising twins rather than to the release of residual stresses. IT is well known that the macroscopic mechanical properties of beryllium are very sensitive to the nature of its surface finish. Matthews and coworkers1 have shown that the tensile strength of rolled beryllium sheet can be considerably enhanced by chemical polishing, presumably due to the removal of the high concentration of notches, twins, and large residual compressive stresses normally found in the surface layers of ground specimens. There was no similar effect of surface condition on the macroscopic yield stress (the stress to produce 0.2 pct strain), a point to which we shall return. To date there have been no extensive studies on the effect of surface condition on the microstrain region of beryllium. Recent measurements2 of the stress to cause a permanent microstrain of the order of 10-6 in. per in. on machined hot pressed QMV beryllium, gave values ranging from about 600 to 3500 psi. Reasons for the considerable scatter in the results were not discussed. In this paper, we wish to show that the microstrain region of polycrystalline beryllium is, in fact, very sensitive to surface condition. The stress to cause a permanent strain of 2 x 10-6 in. per in. which for convenience we will refer to as the microscopic yield stress, can be increased by almost a factor of 2 by minimizing the amount of surface damage. The variation of microscopic yield stress is attributed to the presence of twins in the surface layers, rather than to residual compressive stresses. EXPERIMENTAL PROCEDURE The starting material for this investigation was commercial purity hot pressed QMV beryllium, with an average grain size of about 20 . The effects of surface treatment were assessed by comparing the microstructure with residual stress measurements and microstrain properties. Specimens were prepared for metallographic examination by wet grinding with 240, 400, and 600 papers, followed by polishing with a suspension of fine alumina in warm 20 pct oxalic acid. After this treatment, the surface could be examined, either in the unetched condition with polarized light, or after etching in 2 pct hydrofluoric or boiling 20 pct oxalic acid with normal light. Thin films of beryllium suitable for electron transmission study were prepared from bulk specimens by chemical polishing with hydrofluoric and phosphoric acids, and were examined in an RCA-EMU-3 electron microscope. Residual stress measurements were made by a procedure similar to that of Treuting and Read.3 Specimens 4.0 in. by 0.625 in. by 0.080 in. were prepared by three different machining procedures, namely: turning, grinding, and sawing, in order to introduce different levels of residual stresses. An electrical resistance strain gage was attached to one side of the specimen, and that surface was then protected by an acid-resistant enamel, while the opposite surface was removed by etching approximately one thousandth of an inch at a time. The change in specimen curvature in the longitudinal direction was noted and the residual stress was calculated by the following formula:

Jan 1, 1963

Jan 1, 1963

Calculations of the temperatures of metal, coke, and gas at any level in the cupola furn~ce can be carried out by means of heat balances, using data obtained from experiments with an 18 in. experimental cupola. The results can, to a certain extent, be verified by means of heat transfer calculations.The curves thus obtained, showing the variation of temperature with height in the cupola, provide a valuable picture of the heat transfer processes in a shaft 'furnace.INTRODUCTIONThe Brown Coal Research Laboratory, of the University of Melbourne, has been engaged in recent years on a programme of iron-melting tests in an experimental cupola furnace.Although the ultimate aim of this work is to develop brown coal char as a cupola fuel, most of the experimental work so far has been with conventional coke. The testing programme was designed to provide information on the effect of variables such as blast rate, metal-coke ratio, and coke size on the overall melting process, e.g. melting rate, temperature of metal tapped, and stack gas composition.However, in many cases data were obtained on conditions inside the furnace by measuring temperatures and gas compositions. The aim of the work described in this paper was to qevelop a method for using this data to obtain information on the processes taking place in the cupola.Very little research has been done on the combustion of fuels in shaft furnaces. Early work on this subject, as well as the initial stages of the Brown Coal Research Laboratory's programme, has been discussed by Evans (1959). The use of probes for obtaining information on conditions in the interior of a shaft furnace was pioneered by Belden (1913)...

Jan 1, 1963

By H. R. Ogden, E. S. Bartlett, A. G. Imgram

Notched and unnotched tensile specimens of wrought and recrystallized, oxygmted and hydro-genated tantalum and columbium were tested over a range of temperatures selected to encompass the ductile-to-brittle transition. Increasing the oxygen content of tantalum and columbium increased their strength, and raised their ductility transition temperature, but did not cause a marked deterioration of notch properties below that of commercially pure material. The adverse effects of oxygen were more pronounced for recrystallized structures than for wrought material. The effects of hydrogen are complicated by strain aging or slow strain rate hydrogen embrittlement at -105°F. However, in general, hydrogen had only a minor effect an strength, but markedly increased the effective transition tem-terature and caused a deterioration of notch properties . BCC metals including the refractory metals in Groups Va and VIa (V, Cb, Ta and Cr, Mo, W) can be expected to undergo a ductile-to-brittle transition and exhibit brittle fractures at low temperatures.' Notch embrittlement is associated with this phenomenon, and can be a serious design problem. Table I compares the tensile transition behavior and notch sensitivity of commercially pure Group Va and VIa refractory metals. The Group VIa refractory metals have considerably higher transition temperatures, and become notch sensitive at higher temperatures, than do the Group Va refractory metals. In addition, the Group VIa refractory metals are sensitive to metallurgical structure. Recrystallized structures generally have higher transition temperatures than wrought material of the same composition. The relatively poor transition behavior of the recrystallized structures of these metals is generally attributed to the segregation of interstitial impurity atoms at grain boundaries. Pronounced sensitivity to structure is not evident with commercially pure Group Va refractory metals, however. Since these metals have higher solubilities for interstitial elements than do the Group VIa metals ,4 it can be expected that higher total interstitial concentrations are necessary to develop a comparable degree of grain boundary segregation and to produce a similar sensitivity of transition temperature to structure. Increasing only the concentration of interstitial atoms in solution would tend to increase the flow stress of a metal in relation to its cleavage fracture stress and thereby raise its transition temperature, but would not be expected to cause a marked sensitivity of transition temperature to structure. A research program has been conducted at the Battelle Memorial Institute to evaluate the effects of interstitial oxygen and hydrogen on the transition behavior and notch sensitivity of tantalum and columbium, and to evaluate the effects of structure on "contaminated" material. EXPERIMENTAL PROCEDURES Notched and unnotched tensile specimens of oxygenated and hydrogenated tantalum and columbium with both wrought and recrystallized structures were tested over a range of temperatures selected to encompass the ductile-to-brittle transition Oxygen levels selected for study in both tantalum and columbium were nominally 500 and 1000 ppm, whereas nominal hydrogen contents were 150 and 500 ppm in tantalum and 150 and 300 ppm in columbium. Oxygen and hydrogen additions were made directly to 6-in. lengths of 1/2-in.-diam electron beam melted wrought bar stock, in a Sieverts Apparatus. Subsequent high-temperature annealing was required for homogenization of the oxygenated material, but was not necessary in the case of hydrogenated stock. The oxygenated and hydrogenated bars were then swaged to 1/4-in.-diam rods. Tensile specimen blanks were cut from the 1/4-in.-diam rods and annealed to achieve stress-re-

Jan 1, 1963

By James S. Browning

The Bureau of Mines conducted laboratory batch and small-scale continuous selective flotation tests of barite-fluorspar ores from two deposits near Marion, Ky., to determine the technical feasibility of recovering commercial grade fluorspar and barite concentrates. The lignin sulfonate-sodium fluoride method of floating the fluorspar successfully produced acid-grade fluorspar concentrates. Flotation of the barite from the fluorspar tailing using petroleum sulfonate collector yielded concentrates suitable for use in compounding oil-well drilling mud. The fluorspar and barite recoveries were about 82 and 85 percent, respectively.

Jan 1, 1963

By M. Bevis, A. G. Crocker

A. G. Crocker and M. Bevis (Battersea College of Technology)— Richman and Richman and conard17 have recently published the very interesting results of their studies on the plastic deformation of Fe-Ni-C martensites and of an Fe-5 wt pct Be alloy. Other work on the range of Fe-Be alloys containing between 16 and 27 at. pct Be has also been reported by Richman." One of the fascinating features of this work is that the materials investigated deform primarily by means of twinning and that several twinning modes are operative in addition to the well-established (112 ) mode of bcc materials The composition planes of these unusual twins were determined using a single-surface analysis and reported as (0131, "{045)" or "{089)", and It is now thought1' that the "{0,1,13)" habit reported for the Fe-Ni-C alloys'' is more likely to be near "{127)". Although the full twinning elements of these unusual twinning modes could not be determined directly from the experimental results, the authors attempt to deduce the elements by considering twin intersectionslQ and by using the projection technique of Jaswon and Dove. The basic assumption of their approach is that the (013) habits are truly rational planes but that the other habits are irrational and merely approximated to by the indices quoted above. They thus deduce that the twinning mode describing the (013) habit is either Type I or compound and that the modes describing the other habits are Type 11. This deduction must however be false as all twinning modes in cubic structures obeying the classical orientation relationships of deformation twinning must be compound. Type-I and Type-I1 modes can occur in all of the other crystal systems (indeed in the triclinic system compound modes are not allowed), but in the cubic system only compound modes can arise. This fact, which does not appear to be well-known, fol- lows immediately from the relations between the four twinning elements defining a twinning mode. Thus for a Type-I mode which is uniquely defined by the rational twinning elements K1 = hi and given by: where the summation convention of the tensor calculus has been adopted. For cubic materials the metrics and reduce to the unit tensors and j so that we have It is clear from these equations that both ki and ui must take on integral values; i.e., Kz, and ql must be rational, if hi and vi are integers, i.e., if K1 and are rational. Thus for cubic materials a Type-I mode must degenerate into a compound mode and the same result also arises for Type-II modes. The apparently irrational habits observed by the authors can thus not be explained in terms of Type-I1 twinning if the classical laws of deformation twinning are to be obeyed. An alternative explanation of the irrational habits is that they may arise from twinning modes with four irrational twinning elements. These modes, which do not obey the classical orientation relationships associated with deformation twinning, have been shown to arise as the result of double twinning processes in magnesium,22 but may also describe a simple shear on an irrational plane in an irrational direction. Indeed double twinning processes in bcc

Jan 1, 1963

By H. B. Aaron

DIFFRACTION micrography provides a useful tool for studying complex strain fields. Newkirk1 observed an X-ray diffraction effect due to strain interactions at the intersection of slip lines in LiF and attributed this effect to a reduction of primary extinction due to strain-gradients. It is the object of the current study to correlate the observations and rationalize the appearance of the strain fields around intersecting slip planes in x-ray extinction contrast studies by a semiempirical method. Fig. 1 shows typical strain patterns observed by Newkirk on (200) reflections in LiF using chromium radiation and a variation of the Berg-Barrett (B-B) technique. In other reflections (e.g., {220}) the strain patterns are absent. If one defines a vector 3 along the striations from the more to the less dense portion, and a vector v in the direction of the X-ray beam parallel to the reflecting plane, such that both 3 and v lie in the reflecting plane of the crystal, Fig. 1, then the positions of the striations on (200) reflections appear to be confined such that where is the angle between v and 3, Fig. 1. It will be seen later that 3 is the projection of Sb on the reflecting planes. In some instances the strain effects are observed only above the slip plane, Fig. l(C), in others only below, Fig. l(D). Where the strains appear to be both above and below the slip line, Fig. l(E), one sees that there are actually two slip lines present, Fig. 1(F) and (G). Furthermore, the strain patterns are observed in the vicinity of the intersection of emergent edge dislocations (diagonal lines on the micrograph) with emergent screw dislocations (horizontal lines on the micrograph), e.g., Fig. l(HJ) and (MN), but not in the vicinity of the intersection of two emergent edge dislocation arrays, Fig. l(HJ) and (KL). However, in the latter case the contrast of the dislocation array itself is reduced along (KL) and increased along (HJ). Line (AB) in Fig. 1 is the edge of the crystal, and the material to the left of (AB) is the side of the sample. Any empirical correlation will have to include most, if not all of the aforementioned observations. Lang2 and Newkirk1 determined that the condition for contrast is given by g-b#0 [2] where b is the Burgers' vector and g the diffraction vector (normal to the reflecting planes). If one assumes that the direction of the observed strain fields is given by the vector sum of the slip vectors (Sb1) of the intersecting slip planes, then Eq. [2] may be generalized to g-S#0 [3]

Jan 1, 1963

By H. L. Burmeister

This report describes the mining and milling practices used by the Eastern Magnesia Talc Co. at its Johnson, Vt., operation. The report also contains a description of the local geology and all available information on cost and performance data. Since 1925 the mine has produced continuously at an average annual rate of 54,000 tons, and the ratio of ore hoisted to finished product is roughly 2 to 1. Ore is stoped by a combination of shrinkage and sublevel methods. In any 24-hour period the mill produces an average total of 14 grades of finished talc product, 9 by dry grinding and air classification and 5 by wet grinding and flotation methods. The mine operates one shift per day, 5 days per week and the mill operates on a 3-shift, 5-1/2-day-per-week basis. Operating costs for 1958, on a percentage basis, were mining, 22.34; milling, 54.77; ore haulage, 2.89; and all other, 20.00 percent.

Jan 1, 1963

By Lawrence A. Shepard, Richard H. Krock

A series of ductile, two phase W-Ni-Fe composites, sintered in the presence of a liquid phase, were tested in tension. Identical room temperature stress-strain curves were obtained for specimens containing from 80 to 92 wt pct W (58 to 75 vol pct W particles). The composites exhibited a maximum elongation of 29pct at room temperature, and 10.7 pct at 77 °K. The tungsten particles in the composite elongated by the same amount at these temperatures. Single-phase alloy specimens matching the composition of the composite matrix showed about one half the flow stress of the composites. The test results demonstrated that the mechanical properties of W-Ni-Fe composites are determined by the tungsten particles alone and are independent of matrix volume fraction or mean free path over the composition range studied. A general prediction of the plastic behavior of two-phase alloys or composites from a knowledge of the properties, size, shape, and dispersion of the individual components is not, at present, possible. The excellent theoretical and experimental exposition of the dispersion-strengthening problem applies only to cases where the stronger phase is present as fine particles and in volume fractions of a few percent. Materials in which the stronger phase constitutes a significant fraction of the volume, although of broad engineering interest, have received comparatively little analytical attention. This important group of materials is the concern of the present study. The degree of deformation of each phase during the plastic working of a ductile two-phase alloy has been established by Boas and Honeycombe,1 Clare-brough,2 and Clarebrough and berger.3 These workers empirically correlated the recrystallization temperature of the individual phases with the degree of cold work sustained by each. It was shown that the deformations of both phases are equal and therefore the same as that sustained by the composite whole when the volume fraction of the stronger phase exceeds 35 pct. At yielding, however, deformation begins in the weaker phase. A direct correlation of composite strength, as a function of deformation, with the strength of the individual components cannot be made. In the presence of stronger phase particles, the flow stress of the weaker matrix phase is enhanced by an additional hydrostatic component. The development and potential magnitude of matrix strength promotion upon straining has not even been experimentally established. Quantitative work in this field has been confined to ceramic-metal composites. These materials fracture at strains considerably below 1 pct by cracking of the ceramic particles.4-6 An indication of the potential constrained matrix strength capacity is given by the observation by Nishimatsu and Gur-land4 that the maximum tensile strength of a WC-Co composite is almost double the bulk strength of the cobalt matrix. The relationship between composite strength and geometry is ordinarily expressed in terms of the mean-free matrix path (referred to subsequently as MFP) between the stronger particles.* This factor takes into account both the volume fraction of matrix phase and the average size of the particles. unke17 concluded that composite strength varied directly with the decreasing log MFP, following the Gen-samer8 relationship. However, Gurland and ~radzil~ reported a strength maximum at an MFP of the order of 1 p in WC-Co composites. A ductile two phase metallic composite was chosen for the present investigation of composite mechanical properties with the view of avoiding the difficulties and ambiguities noted above. The W-Ni-Fe heavy alloy of Green, Jones, and pitkin9 contains 80 to 94 wt pct W, and nickel and iron in a weight ratio

Jan 1, 1963

By C. Chiou, D. P. Seraphim

The effect of clustering on the superconducting properties of Al-Zn alloys has been studied by the ballistic induction techniques. The superconducting critical temperature, T,, changes when zinc-rich clusters are formed. The change in T, depends on the concentration and may be positive or negative, but always correlates with an effective decrease in the solute concentration of the alloy. Reversion after clustering effectively returns a 5 at. pct Zn alloy to the quenched state. These methods might be use&lly extended to the Al-Mg system, where X-ray data are difficult to obtain. In very dilute Al-Zn alloys, as in other tin,' indium, aluminum,2 or tantalums base solid solutions, there is a decrease in the superconducting critical temperature, Tc, roughly proportional to the temperature independent resistivity, i.e., -0.2°K per pS2cm. With increasing solute concentration, the T, generally reaches a minimum and then increases4 to a value well above that for the pure solvent. The change of T, with solute concentration follows an empirical formulation involving two constants which correlate with the scattering cross section of the impurities. As will be shown below, the Al-Zn alloys more concentrated than 1or2at. pct do not follow the empiricism, probably because they are unstable even when rapidly quenched.5 However, it seems possible to study at least the later stages of solute clustering by precise measurements of the 1', following various thermal treatments. A few experiments on quenched alloys, aged alloys, and tests on reversion are reported here. The heat treatments selected for obtaining the quenched and aged states were mainly deduced from the work of Dash and Fine.6 For the quenched state, specimens were homogenized at 480°C, quenched to -160°C, and immediately transferred and mounted in liquid nitrogen. Measurements on the superconducting properties and residual resistivities were then made at helium temperatures, after which the specimens were aged at room temperature for 3 to 5 hr, i.e., much longer than the time required for clustering to be essentially completed. The superconducting properties and residual resistivities were once again examined. To reach the reverted state of the A1-5at. pct Zn alloy, the aged specimen was heated for 5 min at 200°C and then tested as above.

Jan 1, 1963

By R. W. Borio, T. S. Spicer

Inflammability and crossing point apparatus were used to study the influence of increasing amounts oi such inerts as ash, fly-ash, pyrite, limestone and Portland cement with several pulverized bituminous coals. The results indicate that it requires large proportions of inerts to substantially suppress the ease of ignition. The ignition phase of the combustion of solid fuels has been under study periodically since 1900. With the advent of pulverized coal firing some 60 years ago, a technique now dominating the coal utilization field, the ignitibility characteristics have become increasingly important. Much of the early work was directed toward the prevention of coal dust explosions and improved mine safety rather than combustion. Many factors affecting ignitibility have been studied and numerous methods devised in an effort to measure the ignition temperature and these have been reviewed by other authors. A recent survey was made by Finney and Spicerl in 1959, so a discussion of previous work will be omitted. Despite these efforts, the initial stage of combustion, termed ignitibility, is still a little understood phenomenon. In fact, no ASTM method has been adopted for the calibration of this illusive property. However, a D-5 Subcommittee XVI on Ignitibility of Coal and Coke of ASTM (now inactive) defined ignitibility:' "The ignitibility of a fuel is that char-

Jan 1, 1963

By J. Laganiere

A considerable part of the sulphuric acid requirements of the Aluminum Company of Canada's Arvida smelter comes from the burning of 180-200 tons per day of zinc '"'sulphide concentrates in a 22-ft.-diam-eter fluidized bed roaster. The plant and its operation were fully de-scribed in a publication that appeared about ten year ago (1). A simplified flowsheet of the roasting and gas-cleaning sections of the plant is given in Figure 1. The wet zinc sulphide concentrates are un-loaded into a pug mixer, by means of a Pay loader, and mixed with water in a mixing tank to make a slurry of 80 per cent solids. The slurry is transferred to a .feed tank and then introduced into the roaster at a point four feet above the constriction plate, which is the height of the settled bed of zinc calcines. The roasting temperature is con-

Jan 1, 1963

By M. R. Louthan

The susceptibility of titanium to stress orientation of hydride precipitates was investigated. It was determined that, when hydride precipitation occurred in titanium under an applied tensile stress of 30,000 psi, the hydrides precipitated on the titanium habit plane oriented most nearly perpendicular to the stress axis. Stress orientation of the hydride platelets occurred because the precipitation of the lower density hydride phase perpendicular to the stress axis caused expansion of the matrix in a direction that tended to relieve the applied stress. The Ti-H system has received considerable study in recent years, mainly because of concern over the effects of hydrogen on the mechanical properties of titanium. The amount of hydrogen present in commercial titanium is now quite low and should have no appreciable effect on its mechanical properties; however, many titanium applications require ex- posure to hydrogenous atmospheres under conditions in which hydrogen pickup is likely. In such cases continued exposures may cause the hydrogen content to increase to the extent that titanium hydride does precipitate as a second phase. The hydride phase has been shown 1,2 to have an adverse effect on the mechanical properties, particularly the impact properties, causing reductions in strength and ductility. BACKGROUND The behavior of titanium is often quite similar to that of zirconium and zirconium-base alloys, and the technology developed on one metal can often be applied to the other. Marshall and Louthan3,4 have shown that Zircaloy is susceptible to stress orientation* of zirconium hydride platelets, and that the platelet orientation has a pronounced effect on the mechanical properties of Zircaloy. They showed that when zirconium hydride precipitated in Zircaloy under an applied stress the hydride platelets tended to be aligned parallel to a compressive stress and perpendicular to a tensile stress. They also showed

Jan 1, 1963

By J. C. Borland, J. H. Rogerson

Jan 1, 1963

By James H. Gary

Data regarding the composition and physical properties of Florida land-pebble phosphate-waste slime are presented, and the feasibility of dewatering and beneficiating the slime by several different methods is discussed. Chemical analyses, electron micrographs, and X-ray diffraction data showed that principal constituents of the slime included quartz, attapulgite, and flaorapatite. Viscosity of the slime changed with pH; thixotropic, Newtonian, and rheopectic states were observed as the pH increased. Use of various flocculating agents was not effective in improving thickening properties of the slime. Dewatering tests using pressure filtration showed that temperature influenced the filtration rate more than pressure; the filtration rate at 165° C was tenfold that at room temperature. Selective flotation of the slime, using two different processes, gave promising results. About 25 pct of the phosphate was recovered in a concentrate assaying 31 pct P205, Other tests demonstrated that the slime could be successfully fractionated at 20-microns using a hydrocyclone. In hydrometallurgical tests about 80 pct of the phosphorus and alumina were chemically extracted from the slime using sulfuric acid. Limited bacteriological studies made of the slime showed that several types of microorganisms were present and grew in the material despite the presence of fluorine-bearing minerals.

Jan 1, 1963

By M. E. Wadsworth, I. B. Cutler, R. W. Bartlett

The oxidation kinetics of ZrC was studied between 450" and 580°C in oxygen pressures from 6.5 x 10-to 1 atm using a ther mogravimetric apparatus and sized powder samples. Two parallel rate controlling processes were observed. A surface reaction occurring at the ZrC-ZrO2 phase boundary accounted for most of the oxidation and had an activation enthalpy of 46 kcal per mole. The other process, believed to be diffusion of oxygen into the ZrC lattice partially replacing carbon, had an activation enthalpy of 53 kcal per mole. The enthalpy for chemisorption of O2 on ZrC was determined to be —13 kcal per mole. Water vapor in the presence of oxygen accelerated the surface reaction rate. THERE has been little reporting of formal rate studies or attempts to ascertain the mechanism of oxidation of carbides. MacDonald and Ransley1 studied the oxidation of titanium carbide which has the same structure as zirconium carbide, fcc. They observed an initial increase in rate with increasing temperature followed by a rapid decrease through a rate minimum and a subsequent second increase at higher temperatures. The discontinuity in the rate rise was attributed to a phase change in the oxide which changed the rate determining step from the surface reaction at the carbide-oxide interface to diffusion through the oxide layer. Samsonov and Golybera 2 studied titanium carbide and reported that during the initial period of oxidation a dense film of Tic-TiO was formed followed by the formation of less adhering layers of higher oxides. The purpose of this investigation was to study the kinetics of oxidation of zirconium carbide and to attempt to gain some knowledge of the mechanism by which oxidation occurs. EXPERIMENTAL PROCEDURE Measurement of the weight gain associated with the oxidation of ZrC was used to determine oxidation rates. The principal experimental parameters were surface area, temperature, and oxygen pressure. Although moderately sized crystals of ZrC can be grown by the Van Arkel method, the only commercially available ZrC is a powder. In using powders, the surface area must be controlled either by fabricating the powder into a sintered pellet with a measurable surface area, relatively fixed during oxidation, or by using sized unconsolidated powder and applying appropriate geometric considerations to the shape of the grains to correct for their diminishing surface areas as they oxidize. Both techniques involve some difficulties. pellets of binder-free zirconium carbide can be made by hot pressing, but it is difficult to obtain densities greater than 90 pct of

Jan 1, 1963

By Bruce E. Kester

The concurrent observation of the phenomena of alkali-aggregate reaction and development of efficient dust collection systems on rotary kilns made mandatory the process modifications to produce low alkali cements. Such low alkali cements as were available prior to these recent changes were either the rare result of low alkali raw materials, the loss of alkalies with dust loss from the kiln stack, or in some instances by the use of CaC12 in the kiln feed to increase volitalization of the alkalies and their subsequent loss or discard with the normal dust emission from the kiln. The relative slowly soluble nature of natural occurring alkali minerals in cement raw materials as compared to the very soluble nature of the alkali salts as present in cement kiln reaction products, either in clinker or in dust emission led to the development of the water leaching system. Two distinctly different problems of leaching are created by the two major systems of portland cement production, the wet and dry processes. The wet process is characterized by moderate dust loads and concentration of soluble forms of alkali in the dust. Further the return of the leached dust slurry does not materially change the characteristics of kiln feed on reintroduction and subsequently does not materially influence kiln operation. The dry process differs in high levels of dust emission and the presence in the collected dust of large amounts of unreacted kiln feed with its sparingly soluble alkali minerals. In the dry process reintroduction of leached dust slurry changes the dry process to what may be classed as a damp process. This change results in some decrease in kiln capacity and creates conditions of operation which are uncommon to either the wet or dry process.

Jan 1, 1963

By John C. Machisak

THIS INFORMATION CIRCULAR contains injury and employment data for all stone quarries in the United States for the Calendar year 1960. This publication contains statistical data on injuries and employment pertinent to the stone quarries and related operations, such as the manufacture of cement and lime, rock dressing etc., but excludes statistics for clay and sand and gravel operations. Data for these commodities may be found in other Bureau publications. Reports received from the operators are voluntary responses to the Bureau's request for information; therefore, the figures may not be complete for the industry. However, since these data contribute greatly to the promotion of safety, every effort has been made to make them representative of the industry.

Jan 1, 1963