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By E. J. Hammer

Crushing and grinding of gypsum demands con- trolled processing to a fineness suitable for further treatment of the mineral into end products, and into various sizes of material which are themselves saleable products. The majority of gypsum tonnage ultimately ends up in stucco for wallboard. Therefore, mineral reduction is normally designed toward this end, but it is done in a manner that permits drawing off intermediate products to meet various customer requirements. This forces companies into compromises at times in equipment installations. Normally, 5 to 6 different sizes intermediate to the end product are marketed and these are generally the fineness of material to be used as stucco for wallboard. These sizes are produced by controlled crushing, grinding and sizing. How Ore Characteristics Guide Processing First, gypsum as a mineral (CaS0;2H,O) is number two on the Mohs scale two of hardness; only talc is softer, Despite being soft, gypsum is tough, a factor which is of critical importance when developing equipment specifications. In addition, of the increasing volumes of rock handled, the associated and included impurities such as anhydrite, silica or lime- stones are found to be relatively abrasive.

Jan 1, 1970

By R. W. Wittkopp, J. D. Stephens

In a device known as the electron-beam microprobe, the mining industry has lately acquired a sophisticated new analytical tool that can dig out answers to a broad range of questions spanning all phases of mining activity. Essentially, the microprobe is a specialized X-ray fluorescence unit that makes it possible to obtain chemical analytical data for volumes as small as 1 cup. With this capability, it can be used both for determining the composition of small inclusions in rocks or metallic products and for monitoring changes in composition that proceed from a reacting surface. At the Research Center of Kennecott's Metal Mining Division, this versatile probe has successfully solved problems in mineral operations ranging from exploration through refining. A few instances of how the probe has been applied at the Center are presented here. In Mineral Exploration-A Good Look Before Leaping Since the objective of mineral exploration is to locate deposits of materials which can be processed at a profit, the mode of occurrence of elements or minerals in the deposits is important.

Jan 1, 1970

By James C. Patterson

Sintered fly ash was shown to have promise as a modifier for poorly drained soils. Turf grown in mixtures of sintered fly ash and soil benefited from increased water-infiltration rates, greater total pore space, and higher moisture availability, The result was an improved turf stand with increased grass yield and root density.

Jan 1, 1970

By Fathi Habashi

Precipitation of a metal from an aqueous solution of its salts by another metal is known as cementation, because the precipitated metal is usually cemented on the added metal. This phenomena was once described by the alchemists as "transmutation," when they dipped a piece of iron in a solution of copper sulfate and the iron was coated with a layer of metallic copper. The process can be predicted in terms of electrode potentials. The metal with the more positive (oxidation) potential, as given in Table 13-1 of the electromotive series, will pass into solution and displace a metal with a less positive potential.

Jan 1, 1970

By Edward L. Burwell

The Bureau of Mines investigated the use of dilute polymer in brine solutions to increase the efficiency of air in gas flooding model oil reservoirs. Slugs (0.23 pore volume) of 500 ppm polyacrylamide were injected into a model, consisting of a high- and a low-permeability core, that had been previously gas flooded to residual oil. Gas flooding was then resumed. Of the total gas volume injected, the percentage entering the high-permeability zone was greatly reduced after polymer injection but remained unchanged when slugs of water without polymer were used.

Jan 1, 1970

By J. Szekely, G. P. Martins

A formulation is given and a general analytical solution is presented for the problem of spherical phase growth in multicomponent systems. The results are valid for describing the rate of bubble growth in the absence of translational motion and, therefore, should be relevant to heterogeneous nucleation processes. Typical worked examples are given, which include bubble growth due to the simultaneous diffusion of hydrogen and nitrogen in molten steel, and the growth of CO bubbles in steel, due to the reaction: C + 0 = CO. The calculations predict that the presence of additional components would enhance the growth rate and also increase the absolute rate at which the individual components are transferred into the bubble. These findings should be relevant to degassing processes. THE problem of spherical bubble growth in the absence of translational motion is appropriate to the description of the heterogeneous nucleation and subsequent growth of gas bubbles while attached to a solid surface. Such problems are of considerable practical relevance to various vacuum degassing and steelmaking processes where bubble nucleation and subsequent growth play an important part in the overall reaction mechanism. A definitive formulation of spherical phase growth has been given in the now classical paper by Scriven1 and the analogous problem for solid phase growth has been discussed by Horvay,2 furthermore a thorough review of the relevant literature has also become available.3 All this previous work was concerned with one component or binary systems. The purpose of this paper is to show that the technique developed by Scriven may be generalized to alow the consideration of multicomponent systems. The results of this generalization would be particularly relevant, as gas bubble nucleation in the metallurgical systems previously mentioned frequently involves the simultaneous diffusion of several components. In the following a general formulation is given and typical worked examples are presented. FORMULATION Consider the growth of a spherical gas bubble due to diffusion in a quiescent liquid of infinite extent, as sketched in Fig. 1. The formulation of such problems requires the statement of the following conservation equations relating to the liquid phase: Equation of continuity Equation of motion Conservation of the diffusing species—Diffusion Equation. The following assumptions are made: a) The fluid is incompressible, quiescent, and of infinite extent b) The bubble is stationary, i.e., it undergoes no translational motion c) Spherical symmetry is observed throughout d) The mass diffusivity is constant e) Chemical equilibrium exists at the surface of the bubble, and any reactions occurring there are fast compared to the diffusion process f) Inertia and surface tension effects are neglected. Equations derived on the basis of these assumptions by previous investigators were found to provide a reasonable representation of bubble growth while attached to a surface in organic and aqueous systems4,5 For gas bubble growth in molten metal systems assumptions a) to d) chould hold reasonably well. The exclusion of chemical kinetics as a possible rate limiting step may not be universally valid, but should hold for many systems operating at high temperatures. The effect of hydrodynamic inertia may be neglected for moderate growth rates; finally, the assumption neglecting the effect of interfacial tension on the bubble growth was made for the sake of mathematical convenience; its inclusion would have required the use of quite cumbersome numerical techniques. While surface tension effects could be appreciable on the initial values of the overall growth rate, especially at low absolute pressures and in case of small bubbles, they are not thought to modify the relative effects present in multicomponent systems, the study of which is the objective of this paper. Within the framework of the above assumptions

Jan 1, 1970

By A. Blake Caldwell

In 1936 the Ertsberg story began and its development is a classic example of the courage it takes to discover one mining prospect and bring it into production. Truly, the finding and working of this mine is a modern exception to the overwhelming odds every modern prospector must surmount to be successful. Today, it takes lots of time, plenty of money and the tenacity of a bulldog to whip the laws of nature. Ertsberg ("ore mountain" in Dutch) is literally an elliptically shaped plug of magnetite which erosion has exposed for 560 ft above ground level. The deposit has been likened to an ice cream cone with the outcrop the ice cream, which is above ground, and with the cone buried below the surface. Assaying about 2.5% Cu, the 33 million tons of ore also carry 0.025 oz Au and 0.265 oz Ag per ton.

Jan 1, 1970

Jan 1, 1970

By Charles E. Carlsen

Underground construction involves all the legal problems common to the construction industry and adds a nice little group of its own. Elements which will ultimately affect contractor-owner relationship commence to form almost as soon as the owner conceives of the project. A few of these with emphasis on their application to underground construction will be mentioned. (1) During the design stage, determination must be made as to whether the specifications will be general or restrictive. To what extent will the operations of the contractor be controlled? Can he proceed to use any method of tunnel excavation that he desires and only be responsible for the end result or will specific excavation procedures be required? Can explosives be used? Under what restrictions? Are tunnel supports required? How long can the crown behind the heading remain unsupported? What kind of supports are required? What restrictions on the placement of tunnel-lining concrete will be required? Each of you could extend this list for many pages but these illustrations are indicative of decisions that must be made in advance of bidding, and the ultimate decision on each question can have a significant effect on the legal relationships that exist between the contractor and the owner. The owner wants a good job at a fair price. On the other hand, nothing is worse than having a tunnel collapse during the construction period, with its extra costs, loss of life, and delay to the entire project. If the specifications are too restrictive, increased costs of performance are bound to occur. Owners save tremendous amounts of money by obtaining a contractor who has been ingenious in devising the most economical construction procedure. Care must be taken in drafting the specifications so that the benefits of such ingenuity will not be lost. (2) HOW is the contract to be awarded? Will there be open bidding, a restricted list of bidders, or will there be negotiations with a comparatively few contractors? If it is a government project, whether Federal, state, or

Jan 1, 1970

By Gerry Doeksen

The paper deals with three case studies: (a) the handling of wet concentrates (5 to 8 per cent moisture) through feed bins; (b) the handling of the same product in rail cars; and (c) the handling of dry concentrates (less than 0.5 per cent moisture) through feed bins. In each case, the paper discusses the problems of rat-holing. In each of cases (a) and (c), there is a discussion on the consequent extreme variations of feed rates coming from the feeders, making automation of process control difficult to impossible. Currently available bin-flow theory and flow property tests are used as aids in redesigning the bins. The paper concludes with illustrations of the final results after the redesigned hoppers were installed and tested. There is also a discussion on the advantages of the new mass-flow bins on adjacent feeder performance.

Jan 1, 1970

By P. LaRochelle, K. Y. Lo, A. L. Tamuly Phukan

In many civil or mining engineering works, the stresses and deformations of natural or excavated slopes due to the combined effect of self-weight and initial stresses are of interest. Because of the mathematical complexities of this problem, however, no complete exact solution exists for the simplest case, that of assuming the stress-strain relation of the rock to be perfectly elastic. Efforts have therefore been directed toward numerical and experimental technique. The stresses within an elastic slope have been obtained by LaRochelle,1 using the photoelastic and finite difference method to determine the difference and sum of principal stresses. Subsequently, Finn,2 Hoyaux and Ladanyi,3 and Duncan and Dunlop4 attempted to solve the same problem by using the finite element method. The problem was also investigated by Brown and Goodman5 and Brown and King6 who emphasize the importance of the effect of loading or unloading procedure on the stress distribution within the slope. Although the geometry of the slope and the boundary conditions involved are identical or similar, the results obtained by these various authors by no means agree. It is therefore necessary to review briefly the results of elastic analysis in order to lend credence to the methods used in the solution. Although the stress-strain behavior of some rocks may be reasonably approximated by the elastic modrl, other rocks generally exhibit an elasto-plastic behavior with strain hardening or strain softening as shown in Fig. 1. Experiments show that for most rocks, the stress-strain relationship is approximately linear from the origin to the point P (neglecting the small concave region under low stresses). At P, the curve deviates

Jan 1, 1970

Samples weighing O·25 g are fused with 1 g potassium hydrogen sulphate, leached with 5 ml. of hydrochloric acid, and then diluted with another 5 ml. of acid. After settling, an aliquot of the clear solution is reduced with stannous chloride, and then a zinc dithiol solution is added to form a coloured tungsten complex which is extracted with petroleum spirit for comparison with standards.Concentrations down to 4 p.p.m. may be analysed at a rate of 100 determinations per man-day of 8 hr.

Jan 1, 1970

By J. Kitagawa

INTRGDUCTION The Paragsha concentrator is the largest of Cerro de Pasco Corporation's base metal beneficiation plants operating in Peru. At present, this plant is treating an average of [ ]

Jan 1, 1970

By Jose Luis de Valle Alonso

Although present electrolytic zinc manufacturing processes are aimed at the direct wet process recovery of the metal, and, with this end in view, several industrial scale patents have been applied for during the last few years, the object of this paper is to enhance the possible metallurgical interest in the conventional recovery of zinc and other metals from leaching residues. Therefore, its main end is the description and discussion of the recovery process of zinc, lead and cadmium from leaching residues. Fundamentally, the process consists of the following: Flotation processing to recover the non-roasted blende still contained in the residues. Pyrometallurgical processing of flotation tails in low-shaft furnaces (kilns) and open-flame rotating furnaces and the ensuing recovery of zinc, lead and cadmium as a mixture of their oxides through volatilization.

Jan 1, 1970

As part of a continuing program of evaluating the Nation's crude-oil resource, this report presents information pertaining to resource, primary reserve, and potential waterflood reserve for 3,209 selected reservoirs contained in 24 oil-producing States, as of January 1, 1968. To that date the selected reservoirs had not been subjected to pressure-maintenance or secondary-recovery operations. These reservoirs also met the following parameters: (1) a minimum of five oil-producing wells on January 1, 1968, (2) a minimum of 50 acres areal extent, (3) a minimum of 50,000 bbl of oil ultimate primary recovery, and (4) the principal reservoir energy was other than active water encroachment. The selected 3,209 reservoirs produced 527 million bbl of oil in 1967, about 17 pct of U.S, total production. Primary oil reserve was 4,983 million stb; in addition, there was 6,043 million stb of potential water- flood oil reserve. Oil resource in the selected reservoirs was 59,547 million stb. A brief history and outlook of waterflooding are presented for each State. Depth and producing rate statistics and geologic distributions of production, resource, reserve, and potential waterflood reserve for the selected reservoirs are presented by States in the appendix. Also included in the appendix are description, history, and technique modifications of waterflooding, and a preliminary cost estimate of a closed-system water-injection project.

Jan 1, 1970

By Eckhard Nembach

The phase diagram of the system Pb-In has been investigated between -27° and + 40°C, using nzainly X-ray dijfraction. In accordance with t her mo dynamic measurements by Heumann and Predel, a segregation occurs at low temperatures, though not in the form of a nziscibility gap. THE phase diagram of the system Pb-In has been the subject of extensive investigations,1&apos;1 but recently Heumann and prede13 concluded from their thermodynamic data that a new feature should occur below room temperature. These authors observed that the maximum values for the enthalpy and entropy of mixing, which occurred at a composition of 50 at. pct Pb, were +400 and —1.7 cal per g-atom deg, respectively. From this the authors estimated that a miscibility gap should occur below 30°C, centered at 50 at. pct Pb. Resistivity measurements seemed to support this view. These authors proposed the phase diagram outlined in Fig. 1. Three phases exist at 30°C: the tetragonal indium phase with c/a > 1, the tetragonal intermediate phase a, with c/a < 1, and the fcc lead phase. During an investigation of the superconducting properties of Pb-In alloys. it has been observed4 that aging a specimen with 50 at. pct Pb for 14 days at -18°C decreased the superconducting transition temperature about 0.13"K and tripled the transition width. In this paper, the results of an investigation of the Pb-In phase diagram in the temperature range from — 2T to +40°C are reported. Superconductivity and X-ray methods have been used. 1) SPECIMEN PREPARATION The materials were provided by the American Smelting and Refining Co. According to the manufacturer their purity was 99.999 pct. The weighed amounts of the constituents were sealed in quartz tubes under an atmosphere of 10 torr helium, mixed for 24 hr in a rocking furnace at 380°C, quenched in ice water, and homogenized at 20" to 30°C below the solidus line, established by Heumann and Predel. The annealing times were 144 hr for specimens containing Less than 30 at. pct Pb and 36 hr for the remainder. 2) SUPERCONDUCTIVITY EXPERIMENTS The specimens were quenched from the homogeniza-tion treatment into ice water and their superconducting transition temperatures T, measured. The procedure used has been described in Ref. 4. The transition was detected by the change of the mutual induc- tance of two coaxial coils containing the sample. T, was defined as the temperature at which 50 pct of the total change in inductance had occurred. The repro-ducibility with which T, could be measured was i0.002"K. Then the specimens with lead contents between 38 and 75 at. pct were aged for 7 days at temperatures between -30" and 40°C. If this treatment caused T, to change by more than 0.005"K or the width of the transition to increase by more than 0.002"K, it was concluded that the specimen had undergone a phase change and no longer consisted only of the fcc lead phase: as it did immediately after homogenizing. The result is shown in Fig. 2. From this one can estimate at what temperatures and concentrations phase changes occur. The X-ray measurements were based on these preliminary results. 3) X-RAY EXPERIMENTS Because of the softness of the material, relatively coarse powders. 75 p, had to be used, which were filed in a helium atmosphere from homogenized specimens. The powders were annealed at least 30 min at temperatures between 120" and 16OJC, depending on their concentration, and quenched in ice water. Then their X-ray patterns were taken at -178°C with a Picker diffractometer, model 3488K, and a cold stage. on which the specimen was in thermal contact with a liquid-nitrogen reservoir. In this way the following relation was established for the fcc lead phase: a = 4.697 + 0.00247C for 40 5 C 5 75 11 where n is the lattice constant (A) and C is the at. pct of lead. The coarseness of the powder made it impossible to use lines with 0 > 75 deg; therefore n was averaged from lines with 45 deg 5 0 5 75 deg. The results were reproducible to within i0.05 pct. Relation [I] is very similar to the one found by Heumann and Predel at room temperature. Following this, homogenized specimens with compositions between 15 and 56 at. pct Pb were aged for at least 10 days at temperatures between -27" and

Jan 1, 1970

By Robert S. Shoemaker

Recently we read a short article which stated that Marcona Corp. was studying the use of 25,000-hp autogenous grinding mills for an iron ore project in Alaska. As if that weren&apos;t enough, they were going to dispense with the primary crusher and feed run-of-mine ore to the grinding mills which were to be driven by wrap-around seven-cycle motors. We see also that Bougainville Copper Co. will be grinding 90,000 tpd of ore in only eight 4250- hp ball mills. At Bougainville too, their float section will be the first large one to be completely equipped with the new 350-cu ft flotation cells. After a half century of relatively peaceful growth in the minerals industry, we are now seeing almost exponential advances in both equipment and plant size. At the same time, we are seeing a constant blending of hydro and pyrometallurgical techniques and processes into minerals beneficiation until the sample grind-&apos;em-up-and-concentrate-&apos;em plant is becoming a rarity.

Jan 1, 1970

By C. S. Giggins, F. S. Pettit

The oxidation properties of Ni-Cr alloys with fine grains, coarse grains, and deformed surface layers have been studied at temperatures of 900" and 1100°C in 0.1 atm of oxygen. The oxidation rates of alloys containing between 10 and 30 wt pct Cr have been found to be dependent upon the grain size of the alloy. Finegrained alloys had smaller oxidation rates than coarsegvained alloys because of the selective oxidation of chromium at alloy grain boundaries. In this compositional range alloys with deformed surface layers behaved similar to fine-grained alloys due to recrys-tallization of the deformed surface layer. In the preceding paper1 it was found that during the oxidation of Ni-Cr alloys, the volume fraction of precipitated Cr2O3 could be greater at alloy grain boundaries than at other areas of the alloy surface. In the case of alloys with chromium concentrations equal to or greater than 30 pct,* the volume fraction of Cr2O3 *AIL compositions are given as weight percent unless specified otherwise. precipitated at grain boundaries and within grains on the alloy surface both exceeded the critical amount required for lateral growth of the Cr2O3 particles and the surfaces of these alloys were completely covered with a continuous, external layer of Cr203 during oxidation. However, in the case of alloys with chromium concentrations between approximately 5 to 30 pct, the volume fraction of precipitated Cr2O3 exceeded the critical value required for external scale formation only at grain boundaries.but not within the interior of the grains. Consequently, the surfaces of these alloys had external scales of Cr3O3 over the grain boundaries but internal Cr2O3 subscales with external scales of NiO away from the grain boundaries. Under these latter conditions, it was found that chromium could diffuse laterally in the alloy from those areas covered with an external layer of Cr2O3, i.e., grain boundaries, to areas where the Cr2O3 was present as a subscale. This diffusion of chromium resulted in an increase in the volume fraction of Cr2O3 precipitated in the sub-scale zone and continuous layers of Cr2O3 could be formed at the subscale front in these regions. For the alloys used in the previous studies,&apos; continuous layers of Cr2O3 were formed on Ni-20Cr alloys in the subscale regions after approximately 30 hr of oxidation at 900°C. For shorter periods of oxidation, the Cr2O3 layer was semicontinuous with the continuous portion at the subscale front emanating from points where the Cr2O3 had been formed as an external scale over alloy grain boundaries. Some lateral growth of a Cr2O3 layer in the subscale region was observed on Ni-15Cr and even Ni-10Cr alloys but this layer was never continuous after 30 hr of oxidation. These results indicate that the selective oxidation of chromium in Ni-Cr alloys with chromium contents between 5 to 30 pct may be dependent upon the grain size of the alloy. Fine-grained specimens in this compositional range should have a larger fraction of the surface covered with external Cr2O3 than coarsegrained specimens and the subscale areas required to be sealed via lateral diffusion of chromium should be smaller. It is therefore to be expected that a continuous layer of Cr2O3 can be formed on alloys in this compositional range after short periods of oxidation providing the alloy grain-size is sufficiently small. bo studieS2,3 have established that the oxidation behavior of alloys can be significantly influenced by pretreatments which produce mechanically deformed surfaces. It has been found that deformed surfaces usually promote the selective oxidation of elements in alloys and it is believed that these effects are due to rapid diffusion of elements in the deformed layer. In view of the previous results,&apos; which showed that alloy grain boundaries may play an important role in the selective oxidation of chromium in Ni-Cr alloys, deformed surfaces may promote the selective oxidation of elements in alloys as a result of the numerous grain boundaries formed on the alloy surfaces via recrys-tallization during heating to the oxidation temperature. The purpose of the present studies was to determine the effect of alloy grain size and surface deformation on the selective oxidation of chromium in Ni-Cr alloys at temperatures of 900" and 1100°C in 0.1 atm of oxygen. EXPERIMENTAL The average grain diameter of the alloys used in the previous studies1 was not less than 0.04 mm and alloys with compositions between 5 and 30 pct chromium had average grain diameters between 0.04 and 0.14 mm. Since the oxidation kinetics were already available for these relatively coarse-grained alloys, it was desirable to use these same alloys in the present studies. The surfaces of the alloys listed in Table I of the previous paper were deformed by using a Model F S.S. White Industrial Airbrasive Unit, which delivered a controlled mixture of 25 µ Al2O3 particles in a stream of dry air at high velocity against the surface of a specimen. The amount of surface deformation produced by this treatment was not determined but a re-crystallized layer about 15 µ thick was formed upon annealing deformed specimens. The grain size at the surface of the specimens was reduced to an average grain diameter of 0.01 mm by annealing the deformed specimens, i.e., grit-blasted,

Jan 1, 1970

By J. A. Roberson, A. M. Adair

A plate of an 18 pct Ni (250 grade) maraging steel was homogenized, cold rolled, and re crystallized to produce a fine grained, homogeneous structure. The strength properties were then measured as a function of cold rollinq prior to aging. Material in the solution heat treated condition exhibited substantial strengthening from cold rolling. The strength increase and the rate of strengthening were proportional to the amount of cold work. This benefit, of up to 50 ksi, was retained during aging for 3 hr at 900°F. The structures produced by cold rolling and aging have been systematically investigated by transmission electron microscopy. The dislocation debris produced by cold work influences the morphology and distribution of precipitate particles as well as the rate of precipitation. An essential feature of the high nickel maraging steels is a martensitic transformation from y to a with the resultant production of a supersaturated bcc solid solution. This solution decomposes to form precipitates during a subsequent aging treatment.&apos; The martensitic transformation in low carbon Fe-Ni alloys and the mechanical properties of these alloys have been studied extensively.2"4 The carbon content of maraging steel is kept very low to avoid the embrittling Fe3C phase and to minimize the acicular, or twinned martensite common to high carbon steels. Maraging steels are usually strengthened only by heat treatment, but cold working is also quite effective in this respect as was shown by Decker, Eash, and Goldman,&apos; Kula and Hickey,5 and the present work. There is, however, some disagreement between the present results and those of Kula and Hickey. Because of their unusual combination of strength and toughness, the maraging steels are suitable for applications where reliability at high stress levels is required. The strength level is achieved through a combination of solid solution hardening,&apos; substructure hardening,3 and precipitation hardening,6 of which the last is the most important. The toughness of these steels has been reported to be a result of the absence of brittle grain boundary precipitates,7 and the fact that the matrix is a massive martensite rather than a twinned martensite.&apos; One of the problems in the manufacture and use of maraging steel has been its tendency to develop laminations in sheets parallel to the rolling plane.9,10 The present investigation was intended to determine whether or not an improvement in the microstructure of this steel by thermomechani-cal processing would improve mechanical properties. I) EXPERIMENTAL PROCEDURES A plate ($ in. thick) of an 18 pct Ni-250 grade maraging steel* was obtained and examined metallo- "Analysis, wt pct: 18.1 Ni, 8.6 Co, 5.3 Mo, 0.4 Ti, 0.07 Mn, 0.05 Cr, 0.05 Si, 0.002B. 0.1 Cu. 0.05 Al. 0.002 Zr, 0.016 C, balance Fe. graphically. It was found to contain laminations as described by previous investigators. This plate was then annealed at 2100°F for 24 hr to promote homogeneity. Pilot studies on small coupons had shown that this was the minimum temperature required to accomplish homogenization in 24 hr. Since this treatment caused excessive grain growth, the steel was subsequently cold rolled and recrystallized. Cold rolling was accomplished at about 5 pct per pass to a total reduction of 66 pct. The standard solution annealing treatment (1 hr at 1500°F) was adequate to cause recrystallization of the cold worked steel. The recrystallized steel was then cold rolled and ground by various amounts to produce specimens with uniform thickness and selected amounts of cold rolling. All tensile specimens with less than 90 pct cold reduction were ground to a thickness of 0.050 in. Specimens with 90 pct cold reduction were 0.025 in. thick. All

Jan 1, 1970

By F. H. Froes, D. H. Warrington

Electron microscope evidence which indicates that TaC may precipitate at random sites in the matrix is presented. Initially the particles are almost spherical and coherent with the matrix. However, as they grow in conditions in which there are insufficient vacancies to relieve lattice strain, the particles rapidly lose coherency in two directions and continue to grow as plates with approximately the full lattice mismatch strain present perpendicular to the plane of the plate. The necessary relief of strain comes from dislocations loops which do not become visible until the later stages of aging. The rapid decrease of apparent strain to low values of appoximately 1 pct at small particle sizes arises not from a complete incoherency but from applying a model wrong for the particle shape and strain distribution. PREVIOUS work has shown that MC-type carbides may precipitate intragranularly in austenitic stainless steel on dislocations,1&apos;2 in association with stacking faults,3&apos;4 and randomly through the matrix,5-7 In investigations of the matrix precipitate by thin-foil electron microscopy, considerable lattice strain has been found to occur around the precipitating phase.7&apos;8 Attempts have been made to evaluate the amount of lattice strain by using the methods developed by Ashby and brown.9,10 Values of the linear strain, much less than the 17 pct theoretical mismatch (for TaC), have been reported; it has been suggested that this is due to either a loss of coherency1&apos; or vacancy absorption which occurs during either the initial nucleation or growth of the precipitate." This report is an extension of earlier work7 that dealt with the precipitation of TaC from an 18Cr/12Ni/ 2Ta/O.lC alloy after it had been quenched from 1300°C and aged between 600" and 840°C. In particular, the shape of the precipitate particles and the amount of strain in the matrix, due to the precipitate, have been studied. The work described here is part of a wider investigation of factors that affect carbide precipitation in austenitic stainless steel," details of which are to appear elsewhere. RESULTS The present investigation can be conveniently split into two aspects of the strain-fields surrounding the matrix particles: 1) information derived from the strain-field which indicates the shape and habit plane of the precipitate particles and 2) the magnitude and sign of the strain-field. The Shape and Habit Plane of the TaC Precipitate. In the early stages of aging twin lobes (normally black F. H. FROES, formerly at the University of Sheffield, Sheffield, England, is Staff Scientist, Colt Industries, Crucible Materials Research Center, Pittsburgh, Pa. D. H. WARRINGTON is Lecturer, Department of Metallurgy, University of Sheffield. Manuscript submitted November 1, 1968. IMD on white background, i.e., for the deviation parameter, S > 0) that indicate the strained region of the matrix define the position of the particles by bright field transmission electron microscopy. The actual particles were not detected until they were approximately 120Å diam; below this size they were too small to be imaged in the electron microscope. This meant that particle growth that had occurred before this stage had to be inferred from the matrix strain-field contrast. In all cases when diffraction effects were observed from the precipitate particles, a cube-cube orientation relationship (i.e., (llO)ppt Il<llO>matrix and {1ll }ppt {III} matrix) existed between the precipitate and the matrix. From the matrix precipitate particles lying along edge-on {111} planes (e.g., at A, Fig. I), the precipitates are seen to be plate-like with their diameter being roughly 18 times their thickness after 5000 hr at 650°C. However, the exact shape of the particles cannot be determined because of the masking effect of the strain-field contrast. If a dark-field micrograph, using a precipitate reflection, is studied, Fig. 2, a number of the projected images of the TaC particles [on the (110) foil surface] apear to have straight edges parallel to projected f111) planes. Thus, it appears that in the later stages of aging the TaC particles are plate-like with some tendency for the edges of the plate to be bounded by the matrix close-packed {ill} planes (though the general shape of the particles in the plane of the plate is circular and thus the "diameter" of the particles has a real physical significance). It should be noted that the bands of fine discrete particles observed in Figs. 1 and 2 are not the matrix precipitate discussed in this paper but are precipitates associated with extrinsic stacking faults3j4 occurring on (111) matrix planes. **£** ****** \ *x 23 Fig. 1—18/12/2~a/0.1~ alloy. Solution treated at 1300°C for 1 hr, water quenched, and aged 5000 hr at 650°C. The (112) directions shown are the traces of the e&e-on (111) planes. Foil normal [110]; operating reflection (331); bright field micrograph.

Jan 1, 1970