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By J. T. Burwell, J. Wulff

As is well known, the alloys of iron containing 18 ± per cent chromium, 8* per cent nickel and less than 1.2 per cent carbon exhibit the same allotropic modifications as iron. The face-centered cubic or gamma phase is stable at high temperatures and the body-centered cubic or alpha ferrite is presumably stable at room temperature. The transformation from the gamma phase to the alpha phase in alloys of the above composition (18-8 or stainless steel) is sluggish; even moderately rapid cooling permits the retention of the gamma phase. Cold-work, however, causes the transformation from gamma to alpha to occur at room temperatures. It is difficult, nevertheless, to induce complete transformation regardless of the method of cold-working. Since metallographic polishing is very effective in transforming the surface austenite to ferrite, as indicated by the magnetic studies of Buehl and Wulff,1 it was decided to investigate the phenomenon by electron diffraction methods. Apparatus The apparatus used (Fig. 1) was a hot-filament type employing movable slits, similar to that described by Germer.2 The sample-to-photographic plate distance was 69 cm. and the accelerating voltage 30 kv. Since electrons do not in general follow geometrical paths, it is necessary that either the electron source or the sample be movable in a plane normal to the beam. In this case the sample is fixed and the electron source is movable. The source is adjusted until the shadow of the sample appears in the brightest part of the beam as viewed on the fluorescent screen, then the slits composing the two pinholes are inoved into position one by one. The system is evacuated by means of a mercury diffusion pump backed up with a Cenco Hypervac oil pump. Pressures lower than 10- mm. of Hg are read on a calibrated ionization gauge.

Jan 1, 1939

By J. T. Burwell, J. Wulff

As is well known, the alloys of iron containing 18 ± per cent chromium, 8* per cent nickel and less than 1.2 per cent carbon exhibit the same allotropic modifications as iron. The face-centered cubic or gamma phase is stable at high temperatures and the body-centered cubic or alpha ferrite is presumably stable at room temperature. The transformation from the gamma phase to the alpha phase in alloys of the above composition (18-8 or stainless steel) is sluggish; even moderately rapid cooling permits the retention of the gamma phase. Cold-work, however, causes the transformation from gamma to alpha to occur at room temperatures. It is difficult, nevertheless, to induce complete transformation regardless of the method of cold-working. Since metallographic polishing is very effective in transforming the surface austenite to ferrite, as indicated by the magnetic studies of Buehl and Wulff,1 it was decided to investigate the phenomenon by electron diffraction methods. Apparatus The apparatus used (Fig. 1) was a hot-filament type employing movable slits, similar to that described by Germer.2 The sample-to-photographic plate distance was 69 cm. and the accelerating voltage 30 kv. Since electrons do not in general follow geometrical paths, it is necessary that either the electron source or the sample be movable in a plane normal to the beam. In this case the sample is fixed and the electron source is movable. The source is adjusted until the shadow of the sample appears in the brightest part of the beam as viewed on the fluorescent screen, then the slits composing the two pinholes are inoved into position one by one. The system is evacuated by means of a mercury diffusion pump backed up with a Cenco Hypervac oil pump. Pressures lower than 10- mm. of Hg are read on a calibrated ionization gauge.

Jan 1, 1939

By P. H. Lindon, J. C. Billington

Fe-O melts containing 0.045 pct 0 were deoxidized with Mn-Si-A1 alloys. Product compositions were reluted to the melt and alloy compositions and were found to be most sensitive to the aluminum content of the alloy. Low residual oxygen contents could be obtained when aluminum oxide was present in the Products because of the reduction of silica and manganese oxide activities. Flotation of the Products from a quiescent melt was followed both by analysis of the oxygen content and metallographic measurement of inclusion concentration. MnO-SiO2-A12O3 products were found to float most rapidly when their composition was such that their viscosity may be expected to be low. Changes in the particle size distribution indicates that particle coalescence occurred and differences in the degree of coalescence are thought to be responsible for the different flotation rates observed between products 0f differing composition. Measured flotation rates were slower than those Predicted from a model based on Stoke's Law, although alumina flotation might be reasonably accounted for by this model. Interfacial effects between oxide particles and the melt are believed to be responsible for the discrepancy. It has been recognized that deoxidation products constitute a large proportion of the nonmetallic inclusions present in killed steel. The amount of oxide inclusions which originate as deoxidation products depends largely upon three factors. These may be summarized, according to P16ckinger1 as: 1) Amount of primary products remaining in the steel prior to cooling. 2) Residual dissolved oxygen content of the steel after deoxidation. 3) Amount of secondary products, formed during cooling and solidification, which remain entrapped in the solid steel. In a well-deoxidized steel containing residual aluminum and/or silicon, the equilibrium dissolved oxygen content is usually very low and so the maximum amount of oxide which may be produced as secondary deoxidation products is small in comparison with the amount of primary products. It may be seen, therefore, that the amount of indigenous nonmetallic inclusions may be minimized if a low dissolved oxygen content is achieved by deoxidation and if the primary deoxidation products are efficiently removed. Oxides which originate by reaction of the metal stream with the atmosphere during teeming are not considered in the present study. It is known that two or more deoxidizers may result in a lower equilibrium oxygen content when used in conjunction with one another than when any of the individual deoxidizers are used alone. Equilibrium studies by Hilty and crafts2 and by Bell3 have shown that manganese increases the effectiveness of silicon as a deoxidizer, and Walsh and Ramachandran4 relate this to a reduction in the activity of silica in the products as the manganese :silicon ratio in the steel increases. It was also shown by Herty's work on deoxidation of steel by silico manganese alloys,5 that there existed an optimum ratio of manganese to silicon which gave a minimum inclusion content. This ratio was in the range 4:l to 7:l and the (FeO-MnO-SiO2) products formed by such deoxidation practice were found to lie in a composition range having very low liquidus temperatures (1170 to 1250°C approx). The optimum manganese:silicon ratio was then explained by postulating that these fluid products were able to coalesce and that the larger particles formed floated out of the steel very quickly as predicted by Stoke's Law. The present work examines the effectiveness of various Mn-Si-A1 alloys as deoxidizers and their effects on the composition and removal of primary deoxidation products from a quiescent melt. EXPERIMENTAL TECHNIQUE Approximately 250 g of prepared Fe-O alloy, containing 0.045 to 0.055 pct O, were melted in an alumina crucible and deoxidized at 1550°C by plunging a thin steel cartridge containing the deoxidizer below the melt surface. A high frequency induction furnace supplying current at 8.5 kHz was used to heat a graphite susceptor, the interior of which had been machined to give a wall thickness of 0.85 in. to form a receptacle for the alumina crucible. The iron melt was essentially quiescent as the induced current was concentrated at the external surface of the graphite susceptor by the skin effect. A nonoxidizing atmosphere was maintained over the melt by passing a continuous stream of argon through the lid of the susceptor. The melt temperature was measured before deoxidation, and again at the end of an experiment by means

Jan 1, 1970

By Charles Law McCabe, Lyndon H. Everett, Edna A. Dancy

It has been found that the carbide phase present at equilibrium in the system M-H2-CH4, at about 600°C, is MC for the rare-earth metals Ce and Pr. X-ray diffraction analysis showed that the monocarbides have fcc structures with lattice constants of 5.036 + 0.009Å and 5.131 + 0.001Å for CeC and PrC respectively. Gaseous equilibrium measurements were used to calculate the standard free energy of formation of the monocarbides from the elements. for the formation of (+ 1300) for the formation of PrC. THE rare-earthdicarbides, and their crystal structures, have been known for some years,l but only more recently were the carbides CeC,2,3 Ce2C3 2 and CeCS3 reported. In 1958 to 1959, Spedding et al. published work on the lanthanum-carbon system4 and other rare-earth metal-carbon systems,5 proving the existence of M2C3 and MC2, and measuring the lattice constants. They also demonstrated that tri-rare earth carbides, M3C, exist for the rare-earth metals samarium through ytterbium. However, they concluded that the cerium monocarbide reported by Brewer and Krikorian2 and by Warf,3 and given a fcc structure with a lattice constant of 5.130Å bythe former workers, was, in fact, cerium metal with carbon dissolved in it. They were also unable to find any evidence for the existence of Warf's CeC3, for which no structural details had been given. Even more recently, Palenik22 reported the existence of only M2C3 and MC2, having been unable to find any evidence for the existence of any other rare-earth carbides. There are no published experimentally derived thermodynamic data for the formation of any of these carbides, although Brewer and Krikorian6 have estimated values of for CeC, Ce2C3 and CeC2. The objective of the present investigation was; to determine experimentally the free energy of formation of any of the reported carbides of cerium and praseodymium, through a study of the rare-earth metal-hydrogen equilibrium. EXPERIMENTAL A methane-hydrogen mixture was circulated, in a closed system over previously prepared cerium or praseodymium hydride, and when equilibrium had been attained, the gas mixture was analyzed by selectively oxidizing the hydrogen and condensing out the water formed. The metal hydrides were used as starting material for convenience because, otherwise, the hydrogen in the gas mixture would immediately dissolve in the metals; in addition, the metals would not react with methane alone at the experimental temperature (around 600°C). The circulating system was based on that used by Browning, DeWitt, and Emmett7 for similar studies on iron carbides. It consisted of a quartz reaction vessel, all-glass circulating pump, analysis tube containing copper oxide that could be heated to 300" C by means of a small furnace, a solid CO2-methanol trap, and a double limb absolute manometer, Fig. 1. A cathetometer, capable of reading to 0.005 cm, was used to measure the difference in height between the two columns of mercury. In its final form, the reaction vessel was enclosed in an outer jacket, containing approximately the same pressure of hydrogen as that within, to reduce errors due to diffusion of hydrogen out through the fused silica of the reaction vessel., The circulating system was supplied with

Jan 1, 1962

By L. Burris, G. A. Bennett, P. A. Nelson

Staznless steels ave rrzuch less seuel-ely attacketl by zinc lapov than by molten zinc systems. To determine the applicubility of stainless steels fov equipment items which would be exposed only to zinc vapor, the corvosion resistance of several stainless steels to zinc vapor was investigated in 500-hr- exposuves at 900° C. Two austenilic stainless steels, Types 304 and 3-17, suffered severe intergranular attack. Loss of nickel from these steels and micro-probe crnalyses indicated the probable formation of low-melting zinc-rich phases. Good vesistance to attack by zinc vapor, as determined by metallo-9-rpaphic excr)rtination and physical testing, Loas exhibited by Type 405 stainless steel, a jevvitic steel. Type 440C stainless steel, a tnartensitic steel, although suffering considevable loss in weight, was not structurally weakened. At Argonne National Laboratory liquid zinc and zinc-rich alloys are being employed as solvent media in pyrometallurgical processes under development for recovering and purifying discharged reactor-fuel materials.' Because of the high solubility of most metals in liquid zinc,' there are few metals which can serve as container materials for liquid zinc at temperatures much above the melting point. The poor corrosion resistance of the common metals and alloys to molten zinc has been discussed by Eldred.3 DeKany, Lavendel, and Burris4 tested some of the less-common alloys of the nonrefractory metals and found that they also have poor resistance to attack by liquid zinc and Zn-Mg solutions. Of the metallic materials, only some of the refractory metals such as tantalum, tungsten, and molybdenum and their alloys have shown resistance to attack by liquid zinc.4-7 In the process-development work at Argonne National Laboratory, tantalum and tungsten vessels have been used to hold liquid-zinc alloys. These vessels are housed in stainless-steel equipment, principally to permit maintenance of an inert atmosphere and operation at various pressures. In this experimental work, it has often been observed that Type 304 stainless steel suffers little attack by zinc vapor at temperatures up to about 800 °C. In contrast, severe attack occurs in areas where zinc condenses as a liquid. The extent of attack by zinc vapor on several stainless steels was investigated because there are possible useful applications of stainless steel for equipment items which would be exposed only to attack by zinc vapor. These applications include, for example, housings around processing equipment as indicated above and vapor lines leading from zinc stillpots or retorts to condensers. EXPERIMENTAL EQUIPMENT AND PROCEDURE The experimental procedure consisted in exposing stainless-steel test coupons to static zinc vapor for 500 hr at a temperature of about 900°C. The apparatus, shown in Fig. 1, consisted of a 12-in.-long closed tantalum tube jacketed in Type 304 stainless steel to prevent oxidation of the tantalum. A Zn-10 wtpct Mg* alloy charge of 293 g in the bottom of the

Jan 1, 1965

By Robert H. Leach, C. H. Chatfield

This paper gives a brief summary of the process of manufacture of sterling silver, and some of its more important physical properties, as observed in conlmercial production of rolled sheet and wire. Although papers have been published by Turner and Smith,1 Rose,2 Sperry3 and Jordaq4 there are few technical data available, and unfortunately the time allowed for the preparation of this paper has not been sufficient to make it as comprehensive as the title might indicate. Analysis of Steeling Silver Fine or pure silver is too soft for coinage and the manufacture of articles in which strength and resistance to wear are desired. From the earliest times of which we have record, copper has been the metal generally used to harden silver. Analyses of coins and silver articles from ancient tombs show varying amounts of copper, and old Roman silver objects in the British Museum have approximately the same ana,lysis as our sterling. The first authentic record of the establishment of a standard alloy is during the reign of Henry I1 in England. During the twelfth and thirteenth centuries, the people in the Eastern Provinces of Germany had a reputation for the standard and purity of their silver coinage, and it is said that Henry II employed some of these Easterlings, as they were called, to improve and standardize the English coinage, which had become debased. The peculiar standard adopted is probably accounted for by the system of weights used. A troy pound contains

By Glenn C. Waterman, Scott Hazen

3.1-1. Purpose. Development drilling is directed towards determining the grade, volume, and three-dimensional outline of a mineralized zone previously located by exploration. It is distinguished from exploration or reconnaissance drilling, which has as an objective the discovery of new mineralized areas. A development drilling and bulk sampling program should furnish the following information: 1. Geology of the mineralized zone. 2. Quantitative data on grade and tons of material within pertinent cutoff limits. 3. Physical size and shape of the deposit. Areas underlain by waste as well as ore. 4. Mineralogica1 and metallurgical characteristics of the ore. 5. I1hysical characteristics of the ore. 6. Hulk samples for metallurgical testing and grade check. 7. Data on other factors that could affect mining operations, such as ground water, ground conditions, etc. 3.1-2. Procedures. There are numerous methods and techniques that are used to acquire pertinent data on a potential ore deposit. The total cost and accuracy of a development program depends on significant evaluation of the geology, proper selection of a drilling method, thorough analysis of sample data, and accurate evaluation of all the information. Knowledge of the geology of the mineral deposit is important in planning the development testing program and in evaluating the data obtained from such a program. Exploration work usually provides some significant information on the general size, shape, thickness, grade, and geology of the deposit. In some cases no further data are needed; in many cases geological complexities suggested by the preliminary work require further geological study. Of considerable importance may be the following:

Jan 1, 1968

By Arthur Phillips, E. S. Davenport

The purpose of this paper is to present certain data and observations resulting from a series of experiments dealing with the heat treatment and microstructure of commercial white cast iron and its derivative, malleable iron. In planning the experimental work, particular pains were taken to secure for the tests white cast iron of "normal" composition; i.e., within the composition limits commonly prescribed by manufacturers of malleable castings. A review of the literature leads us to believe that much data of a fragmentary character treating of the graphitization of white cast iron have been of little value, mainly because of the diversity in chemical composition of the materials employed in the tests. Moreovcr, when feasible, annealing periods at least comparable to those of current practice have been adopted. We wish to acknowledge our indebtedness to the members of the research department of the Eastern Malleable Iron Co. for the white cast iron used in the test's and, particularly, for their active cooperation during the experimental stage of the work. In this paper the following subjects will be discussed in the order indicated: Data on the thermal critical points of white cast iron and malleable iron. Changes produced in tensile properties and microstrue.-ture of white cast iron by annealing at different temperatures within the, range, 760 to 1100° C. Relation of thickness of wall section of hard iron to microstructure and tensile properties of malleable iron obtained under normal annealing conditions. Notes on mechanics of graphitization of normal white cast iron as observed in specimens quenched after various periods of anneal at approximately 800" C.

Jan 1, 1922

By Arthur Phillips, E. S. Davenport

The purpose of this paper is to present certain data and observations resulting from a series of experiments dealing with the heat treatment and microstructure of commercial white cast iron and its derivative, malleable iron. In planning the experimental work, particular pains were taken to secure for the tests white cast iron of "normal" composition; i.e., within the composition limits commonly prescribed by manufacturers of malleable castings. A review of the literature leads us to believe that much data of a fragmentary character treating of the graphitization of white cast iron have been of little value, mainly because of the diversity in chemical composition of the materials employed in the tests. Moreovcr, when feasible, annealing periods at least comparable to those of current practice have been adopted. We wish to acknowledge our indebtedness to the members of the research department of the Eastern Malleable Iron Co. for the white cast iron used in the test's and, particularly, for their active cooperation during the experimental stage of the work. In this paper the following subjects will be discussed in the order indicated: Data on the thermal critical points of white cast iron and malleable iron. Changes produced in tensile properties and microstrue.-ture of white cast iron by annealing at different temperatures within the, range, 760 to 1100° C. Relation of thickness of wall section of hard iron to microstructure and tensile properties of malleable iron obtained under normal annealing conditions. Notes on mechanics of graphitization of normal white cast iron as observed in specimens quenched after various periods of anneal at approximately 800" C.

Jan 1, 1922

By H. I. Aaronson, C. Laird

Although the past results of X-ray experiments indicate that the broad faces of 0' plates are coherent with their matrix, dislocations lying in arrays have frequently been observed at these boundaries by transmission electron microscopy. Critical experiments employing the latter technique have been carried out in order to determine the origin of these dislocations. It is concluded that 8' plates are essentially coherent with the matrix at their broad faces throughout the aging temperature/time envelope studied. Virtually all of the dislocation arrays observed are deduced to have been formed by plastic deformation accompanying transformation. The proportion of dislocations arising from convexity of the plates is shown to be negligible by comparison with that from plastic deformation. At the higher aging temperatures, a[001] dislocations appeared in moderate numbers. These dislocations were traced directly, however, to the ledgewise dissolution of 0' occasioned by the formation nearby of 0 crystals. On the other hand, since there is a parametric difference normal to the broad faces of the ?' plates, mismatch dislocations do form at their edges. A previous conclusion that these dislocations have Burgers vectors of type a[001] was confirmed directly. The edges of 0' plates were observed to develop octagonal shapes when growing, but circular shapes during dissolution. 1 HIS paper presents the results of an investigation of the interfacial structures of plates of the transitional phase, 8', formed in an A1-4 pct Cu alloy. In a companion paper, Part 11, the effects of these structures upon the migration kinetics of a:?f boundaries are reported. This work is pa.rt of a general program designed to establish the basis of precipitate morphology. The present authors in Al-Ag,1 and whitton2 previously in U-C alloys, have used transmission electron microscopy to examine directly the vander Merwe3-6 networks of dislocations anticipated7 to compensate the small amount of lattice misfit normally founda at the broad faces of Widmanstatten plates. Since the broad faces of 0' plates are considered to be perfectly coherent with the corresponding habit planes in the a matrix,' no dislocations should be present at these faces. Many reports have been published, however, giving evidence to the contrary.10-18 The primary objective of this investigation was therefore to ascertain the nature of these dislocation structures. An attempt to do this is described in the first three sections of this paper. Inspection of the matching of the a and 8 ' lattices at the orientations of the 0:0' boundary corresponding to the edges of 0' plates raises the possibility that these edges may be made up of rather closely spaced edge- type misfit dislocations oriented so as to be sessile with respect to the lengthening or shortening of the plates. Since this structure should severely inhibit migration of the plate edges (Ref. 7, Part II), a situation not originally anticipated,' an experimental determination of the interfacial structure of the edges of 8' plates was clearly in order, and is reported in Section III. Those aspects of the experimental procedure applicable to both Parts I and I1 are presented in the next section. Specific procedures applicable to individual aspects of each investigation, and also the relevant surveys of the literature, are then individually reported in the appropriate sections. I) GENERAL EXPERIMENTAL PROCEDURE The material used in both parts of these studies was the same as that of a previous investigation:" strips of A1-3.93 pct Cu, 0.009 in. thick, prepared as before, solution-annealed at 548°C for 6 hr, and quenched. Details of subsequent aging, and in some cases deformation treatments, are given in the Experimental Procedure sections of the individual parts of both papers. Specimens of the heat-treated strips were electro-thinned as beforeLg and examined in a Philips EM 200 microscope equipped with a goniometer stage. A commercial hot stage, of the grid-heater type and capable of * 30-deg tilt about one axis in the plane of the specimen, was also used for kinetic studies. The usual precaution of calibrating for the additional heat supplied by the electron beam was taken.19 A 16-mm cine cam-I era mounted outside the viewing window was frequently used to record the transformations. Conventional selected-area diffraction and dark-field viewing techniques were used to identify the precipitates in the foils. Normal bright-field images corresponding to two-beam diffracting conditions or dark-field images were employed to characterize the dislocations observed at the interfaces of the precipitates. The application of these techniques to the study of an interphase boundary, and the interpretation of the images,20'21 has been fully described in a previous paper.'

Jan 1, 1969

The Committee on a Standard Gauge have been constantly engaged, since their appointment, in the duties assigned to them.§ They have corresponded with different persons interested in the manufacture and use of gauges in this country, and have received from several of them important information. They have also entered into correspondence with the governments of England, France, Gerniany, and Russia through their Consuls, ant1 with Austria directly. The Consuls of Germany and France

Jan 1, 1879

By Richard Klimpel

In this paper various formulae are developed which can be used to estimate stream flow rates or weight ratios given information on the stream components. The type and level of experimental error present in the stream component analyses does have an important bearing on the numerical values (and reliability) of the weight ratios calculated by the various formulae. A simple but theoretically sound method is shown for selecting appropriate estimation formulae for any given engineering operation. The derived formulae are applied to sets of experimental classification data for illustration purposes.

Jan 1, 1980

By B. A. Wilcox

ThERE are several reports in the literature which indicate that both solid-solution hydrogen and hydride precipitates can promote low-temperature em-brittlement of tantalum.1-3 For example, Imgram et al.2 showed that hydrogen additions in the range of 140 to 580 ppm promoted a ductile-to-brittle transition at slightly above room temperature in both wrought and recrystallized tantalum. This contrasts with the observation that tantalum of norma1 purity is very ductile, even at liquid-nitrogen temperature. Imgram et al. also found that hydrogen additions caused a deterioration of notch tensile properties of tantalum. The purpose of this communication is to present some limited evidence that hydrogen can also cause fatigue embrittlement of tantalum. The material used in this investigation was wrought, stress-relieved (1000°C, 1 hr), are-melted tantalum rod (5/8-in. diameter) containing the following impurities in weight percent: 0.005 C, 0.007 02, 0.0005 H2, 0.003 N2, 0.08 Cb, 0.01 W, and 0.01 Fe. Hydrogen charging was done in an atmosphere of flowing dry hydrogen for 3 hr at 600°C, followed by an homogenizing anneal in purified argon for 15 min at 600°C, and cooling in an argon atmosphere. Typical micro-structures of the hydrogen-free and the hydrogen-charged materials are shown in Fig. 1(a) and Fig. 1(b), respectively. Fig. 1(b) shows the appearance of hydride precipitates which, in many cases, formed preferentially parallel to the rod axis. The hydride dispersion was uniform across the diameter of the specimen. The fact that the precipitate was a tantalum hydride was tentatively confirmed by X-ray diffraction on a metallographically prepared surface. After hydrogen charging, chemical analyses by vacuum fusion revealed the hydrogen content to be 0.0295 wt pct. In addition, the oxygen and nitrogen contents were slightly raised to 0.0095 O2 and 0.005 N2.

Jan 1, 1964

By H. Doi, Y. Fujiwara, K. Miyake

In order to throw light on the mechanism of plastic deformation of WC-Co alloys, compressive tests of WC-(7 to 43) vol pct Co alloys have been carried out at room temperature, and stress-micro strain relation has been investigated in detail. The analysis of the factors affecting the yield stresses reveals that the yield stresses can be predicted by modified Oro-wan's theory if one properly estimates the planar in-terfiarticle spacings. Conzpressive straining of some of the alloys by 0.066 to 0.17pct increases the decrements by a factor of as much as 3.4 to 14, whereas the corresponding increase in the electrical resistivities is less than 10 pct. The analysis of the decrement data in terms of -Gramto and Lücke theory shows that the marked increase is attributed to increased dislocation darnping itt the binder (cobalt) phase. By cornbilling the decrement data and the conzjwession duta, one obtains the relation between flow stress in shear (?t) and increase in dislocation density (p): At = const . v6 . This is interHeted to mean that the mechanism of strain hardening of CirC-Co alloys is essentially sarne as the one for dispersion strengthened alloys. The possible effect of bridge formations between the carbide particles has also been examined. OWING to the combination of hardness, strength, and other physical and chemical properties, WC-Co alloys have opened the way for unique fields of applications, the recent ones being, for instance, anvils for super-high-pressure generation apparatuses. In such applications, the alloys are frequently subjected to very high compressive stresses: these stresses may cause the alloys to deform plastically and eventually to fail. However, much remains obscure regarding the nature of the plasticity of the alloys. Evidently, the alloys owe their high strength to the hard carbide particles which frequently occupy as much as 80 to 90 pct in volume fraction, whereas the ductility required for practical applications is provided by the small amount of the binder phase between the carbide particles. When the volume fraction of the carbide phase is not very large, deformation behavior of the alloys may be described by some of the current dispersion strengthening theories. However, greatly increasing the carbide phase is thought to lead to some carbide skeleton structure or bridge formations owing to the increased chances for direct contacts between the carbide particles;1,2 this may appreciably affect the plasticity of the alloys. Regarding the effect of formation of the carbide skeleton structure, it is interesting to note the work by Ivensen et al.3 on compression tests of the alloys containing somewhat large carbide particles; they observe extensive generation of slip bands in the carbide particles after application of some preliminary compressive stresses. They interpret the results in terms of plastic deformatiot: of the carbide particles which are supposed to have formed a skeleton structure; the binder phase plays only a passive role, at least in the early stages of the deformation. That carbide crystals exhibit microplasticity at room temperature is apparent from the work of Takahashi and Freise4 and French and Thomas5 on indentation of WC single crystals. On the other hand, Dawihl and coworkers6-10 maintain that even when volume fraction of the carbide phase is very large (for instance, more than 90 pet), a very thin binder layer generally exists between the carbide particles. They interpret the results of the extensive mechanical tests in terms of the plasticity of such a layer. Gurland and Bardzil11 point out that decrease in ductility of the alloys with increase in the carbide phase is caused by the effect of plastic constraint exerted by the dispersed carbide particles. Drucker12 further develops this concept from a continuum-mechanics approach on an assumption that a continuous thin binder layer separates the carbide particles. A common feature of the studies reported so far on the plasticity of the alloys is that the information deduced is invariably qualitative in nature. Thus, very few systematic experiments for obtaining reliable and sufficiently detailed stress-strain curves of the alloys varying widely in the microstructural features have been carried out. In particular, it may be of special interest to investigate in detail the early stages of the plastic deformation of the alloys in order to shed light on the strengthening mechanism. However, such work appears to be extremely rare. Doi et al.13 recently reported a first brief account of the results of some quantitative analysis of the plasticity of the alloys in terms of dislocation theory. Their experiment was rather limited in the composition range covered (volume fraction occupied by the carbide phase: 79 to 83 pct), and thus they could not necessarily elucidate the controlling mechanism of plastic deformation of the alloys of a more general composition range. Consequently, in the present investigation, deformation behavior and some other physical properties of the alloys were investigated and discussed in more detail over a much wider composition range. SPECIMEN PREPARATION WC-Co alloys used in this experiment were prepared in cylindrical or rectangular form by sintering in vacuo compressed mixtures of tungsten carbide and cobalt

Jan 1, 1970

By A. E. Gorum, J. Washburn, E. R. Parker

Experimental evidence was obtained in support of the idea that cleavage fracture can be initiated by dislocation pile-up. The high ductility of MgO crystals when tested in bending comPared to their relative brittleness in tension was explained on the basis that large pile-ups are more likely in a tension specimen. CLEAVAGE fractures have been a problem of major concern for many years. A number of large steel structures have failed in a brittle manner, usually suddenly and without warning; often the failures occurred for no obvious reason and at nominal stress levels well within the generally accepted range. A great deal of data have been collected about factors that contribute to failures,1 but the physics of the fracture process has never been revealed. cottrel12 has recently developed a theory of brittle fracture in ductile materials which was based upon the concept that dislocations moving on two intersecting planes can unite to form a crack nucleus. This theory accounts for the known effect of grain size and for the effect of testing temperature. There has, as yet, been no experimental evidence published that would substantiate this or the earlier theories based on stress concentrations due to piled-up dislocations. The study reported herein was conducted to obtain information that would either substantiate or disprove the

Jan 1, 1960

By AIME

WE produce Charles Van Ormer "Charlie" Millikan as living proof that man need not make a loud noise to be heard. His quietly affable, analytical, and soft-spoken manner in the face of all problems belies his ability to "get tough" when the situation demands it. As a chief engineer with many responsibilities for the success of a large producing company there must have been many occasions to tempt Charlie to excitement, but there are few, if any, who can say they saw him yield. He has an abiding faith in the benefits of hard and persistent work and will not admit the existence of a problem that cannot be reduced by it.

Jan 1, 1948

By M. Khorouzan, L. Thomas

Designers of semiconductor devices have been strivi,ng to resolve problems associated with Au-A1 alloys in bonded in.tercomzeclions. One approach now being- used is that of waintaining a physical seyav-atioz between the two metals in bond areas. This is accolrzplished by alunzincnz-plating a bonding area on the tips oJ the kovar leads and using alcminurn wires to join the senzicondictor device to the leads. The portion of the kovar lead which is on the externul side of the sealed package is gold-plated to provide an oxide-free surface for soldering or welding. A discoloration condition originally thought to be sinilar to purple plague, occuving in the yluled uluninur bonding area after package sealing, has been investigated to determine its efiects ipm bond integrity. Electron-micro-probe analysis determined that no1 only gold, but lead, zinc, and silicon were also present in the discolored area. A series of samples conlaining' conkrolled umonts of these inzpitrities weve prepared and subjected to a sil.zuluted sealing process. The investigations swcued that, of the contawiinants, only zinc toas detrinenlul to Lhe bond integily. The discoloration condition itself was found not to be detrimental to the bond integrity. DESIGNERS of semiconductor devices have been striving to resolve problems associated with Au-A1 alloys in bonded interconnections. One approach now being used is that of maintaining a physical separation between the two metals in bond areas. This is accomplished by aluminum plating a bonding area on the tips of the kovar leads and using aluminum wires to join the semiconductor device to the kovar leads. The portion of the kovar lead which is on the external side of the sealed package is gold-plated to provide an oxide-free surface for soldering or welding. Contamination as evidenced by discoloration of the aluminum-plated area was observed in a number of integrated circuits undergoing examination for defect characteristics which cause electrical failures.' This paper contains the results of an investigation to determine the nature of this discoloration, its cause, and its effect upon the integrity of the interconnection bond. I) THE NATURE AND EXTENT OF ALUMINUM-BOND CONTAMINATION The initial hypothesis in the investigation was that the discoloration was caused by reaction of the aluminum film with some unknown contaminants during the sealing of the hermetically sealed integrated-circuit flat package. The package is a rectangular ceramic container sealed with glass which surrounds the kovar leads as well as joining the top to the bottom. The seal is made hermetic by heating and cooling the package to devitrify the glass. In the case of the packages under investigation, the hermetic sealing had been accomplished with dry air as internal atmosphere. The apparent effect of contaminations as observed by microscopic examination was the formation of surface oxides having variations in color encompassing the whole spectrum of visible light. The contamination appeared to be related to one of the more notorious examples of these colorations, the so called purple plague.' In addition to purple plague, Fig. 1 shows the tarnish in the luster of the aluminized surface in the bond area which had been observed in many of the integrated circuits. To identify the contaminant in the bond area electron-probe microanalysis techniques were used.3 Fig. 2 shows the result of this analysis. The contaminants identified were gold, aluminum, zinc, lead, silicon, and cobalt. Fig. 2(a) is a back-scatter display of the area under study. The back-scattered electrons provide a general indication of the distribution of elements in the specimen surface. Elements with higher atomic number scatter more electrons back from the surface and are seen as light areas in the picture. The sample current, Fig. 2(b), is the amount of current conducted by the specimen as a result of electron-beam striking it and is an indication of element distribution. The Sample current is the reverse of back-scatter and complements it. Other pictures in Fig. 2 are produced by characteristic X-rays generated by the elements, allowing the isolation of the element of interest. The isolated element appears white and all other elements are dark. In this manner a comparative study provides a correlation between different surface areas and the elements which are in these areas. The area covered by the gold film, Fig. 2(c), shows that the boundary between the gold film and the kovar is not sharp as expected and that some sort of diffusion has taken place. Fig. 2(c) shows that some gold particles have been carried to the bond area and are in the proximity of the bonded wire in spite of the presence of a physical barrier in the form of the un-

Jan 1, 1967

Q: It is May 1961 at Bill Wrather's Washington house. Bill, think back to your first job after college. Wrather: Perhaps I ought to go back a little bit further than my first job. I entered the University of Chicago with the idea of studying law. My intention was to take a 4-yr liberal arts course and superimpose a law degree on that. But during my undergraduate work I fell under the influence of R. D. Salsbury. He decided I had some talent as a geologist and influenced me to take a geological course. Nevertheless, I did not give up the idea of law. While in school I took a spell of typhoid fever and almost died. The doctor recommended outdoor exercise, so a geological job seemed logical. W. H. Emmons was a graduate student in the University and he interceded with Dr. Hayes of the USGS. I went on the payroll as assistant packer at $60 a month. I had one of the most glorious summers I ever spent in my life. That fall and the following year I took law courses and became thoroughly convinced that I was cut out for a geologist rather than a lawyer. I finished up my law work in 1908 while waiting for a job with Bill Emmons, who was doing a careful study of Goldfield and Tonopah.

Jan 4, 1964

By Richard Franchot

IN the inevitable conquest of the blast furnace by metallurgical science in the solution of the problem of how to make more and better iron or to burn less coke, or both, it is highly desirable first to find out why the efficiency of the furnace generally is no better than it is. The immediate need would seem to be a theory to account for the existing facts. Explanation for the quantitative results obtained in current practice has been strangely lacking. One reason for this may be found perhaps in the custom of think-ing of efficiency in terms of coke consumption. Before efficiency can be explained there should be a fairly exact knowledge of what it is. A statement of the pounds of coke used per ton of iron made may have value in indicating comparative results in smelting similar ores with similar cokes, but it tells very little of the efficiency of the operation. When the materials are different, one practice burning 1800 lb. may be less efficient than another using 2000 lb. A better measure is the pig and slag per unit of coke. What is needed is a specific description of efficiency as a' definite quantity having an exact meaning. Such description is afforded by expressing efficiencies in terms of the respective proportions of the fuel energy absorbed in and chargeable to the various actions known to be -taking place in the furnace. Concretely, the energy value of a pound of coke having 85 per cent carbon blown with air heated to 1200° F. is about 7650 lb.-cal. (13,770 B.t.u.). And the work done in smelting a pound of average iron from hematite, comprising reduction and melting with production of a half pound of free running slag from an equal weight of limestone,

Jan 9, 1926

By C. W. Goodale

As an appendix to the above-mentioned paper, a drawing of the vertical projection of the Knoxville mine workings is here given. In my paper it was stated that the ore-chimneys are found along a crack or plane of cleavage in the limestone ; and as this crack is not parallel with the strata, it is safe to assume that the manganese was not deposited where it is now found before the tilting-up of the strata, but rather that the crack was caused by the folding, and that tile formation of the ore was entirely subsequent to the change of position of the limestone. There are here four chimneys, which have produced, as far as explored, over 12,000 tons of ore, containing at least 7000 tons of manganese oxides, and it is very difficult to apply Prof. W. P. Blake's theory of segregation from the surrounding limestone in accounting for the origin of this ore, as cross-cuts and drifts in the countryrock, even at short distances from the ore-chimneys, have not shown manganese in appreciable quantities. It is easier to believe that, in the language of .Mr. S. F. Emmons, in speaking of Leadville ore-deposits, there was a metasomatic interchange between the minerals brought in in solution and the limestone, and not a deposition in already existing cavities. This in-

Jan 1, 1890