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By Gerald Edmunds

Castings of pure metals and many alloys usually have a coarse-grained structure characterized by long columnar grains throughout the main body of the casting. Frequently, the surface exhibits finer, sometimes nearly equiaxed grains, and such grains may also compose other parts of the casting. This paper deals .primarily with determinations of the grain-orientation textures of the columnar and surface grains of polycrystalline zinc castings. It includes some results upon a cadmium casting and a magnesium casting. A hypothesis is developed to account for the observations on columnar grains and to use as a basis for predicting orientations in other cast metals. A general description of the position of the columnar grains in castings is that their long axes are approximately parallel to the direction of the thermal gradient during crystallization. Thus, in cylindrical castings the columnar grain axes tend to be radial, and in large flat castings where most of the cooling is through one or both of the large mold surfaces they tend to be perpendicular to the mold surfaces. At the edges and corners the direction of heat flow and therefore the position of the grains is more cornplex. Actually observation shows that even in castings made in flat molds the cooling seems to be somewhat irregular, since columnar grains tend to emanate from certain areas of the cooling surface, indicating that thermal contact was better there than in neighboring areas. The nucleus from which a columnar grain grows may be so oriented that its direction of maximum growth rate does not coincide with the direction of the thermal gradient. In this case the long axis of the grain probably assumes an intermediate position. Notwithstanding these minor irregularities, the situation does exist that the long axes of the columnar grains are generally disposed approximately perpendicular to the mold surface. Schmid and Wassermanl and Nix and Schmid2 have determined the orientation texture of columnar grains in castings of several cubic, tetragonal, hexagonal close-packed and rhombohedra1 metals. For zinc and cadmium, they report the basal plane to be parallel to the columnar grain axes, with no preference for any particular direction in this plane to coincide with the grain axes. This texture, termed a ring fiber texture,3 is uncommon in metals; zinc and cadmium are the only ones reported to exhibit it. Generally, it is stated, a simpler texture exists in which a principal, though not necessarily the most closely packed, crystallographic direction is parallel to the direction of heat flow. In cast magnesium (also hexagonal close packed) they report a digonal axis I, [100] direction, parallel to the direction of heat flow. The writer is not aware of any other orientation-texture determinations on cast polycrystalline hexagonal metals. In view of the observations reported in the present paper it is of interest also to note that Nix and Schmid stated that a

Jan 1, 1941

By W. Rostoker, R. P. Elliott

TWO intermediate phases enter into equilibrium with the primary solid solutions of titanium.' The TiMn2 phase was identified by Wallbaum2 as of the C14 type isomorphous with MgZn2. Contrary to Maykuth, et al.,¹ the phase occuring at about the 50-50 atomic proportion has been shown to derive from a peritectoid reaction.:' A 30 day anneal at 900°C of an alloy containing 52 wt pct Mn developed sufficient of the new phase to give a clear and predominant diffraction pattern. The powder pattern was taken in a 14 cm diameter powder camera using filtered Cu Ka radiation. In all, 75 lines were recognized and measured. Interplanar spacing and observed intensities for the first 26 of these are given in Table I.

Jan 1, 1954

By Allen Garrison

THE chemistry of clays and shales has been assuming increasing importance in the petroleum industry, and two factors have greatly influenced this trend. The first has been the growing evidence that the marine shales are source beds, and that the petroleum compounds have migrated to the sand reservoirs overlying or underlying these shales: the second has been the demand for drilling, fluids better adapted to penetrate these marine shales without difficulty and expense. ORIGIN AND GENERAL COMPOSITION OF CLAYS AND SHALES Clays, shales and surface soils are all closely related materials. They are mixtures of finely divided compounds formed during the weathering of the solid crust of the earth. Their nature is essentially colloidal; that is, their behavior is determined by the state of division of the materials and the surface reactions of the smallest grains. Many of their chemical changes affect only the exposed areas and do not involve the interior of the grains of matter. The extent of these reactions is more nearly proportional to the area of the substances than to their mass, therefore it is possible for a small. amount of a material in an extremely fine state of division to completely dominate the character of the mixture. More than 83 per cent of the crust of the earth is composed of three elements-oxygen, silicon and aluminum. Consequently, the corrosion products of the crust are predominantly aluminosilicates, or compounds of aluminum, silicon and oxygen. If we add the compounds of six elements-iron, calcium, sodium, potassium, magnesium and hydrogen-more than 98 per cent of the crust has been accounted for. These six elements, together with the first three, also appear in soils, clays and shales. But direct chemical analysis is of little value in describing the nature of such materials. Many chemical individuals may be present in variable amounts,. and the extreme subdivision of any one of the individuals may contribute qualities that dominate the mixture.

Jan 1, 1939

By D. A. Rice, R. L. Stone

Studies of the possible effect of plant water chemistry on the strength of unfired iron ore pellets apparently have not been reported in the literature. Naturally occurring soluble salts were removed from magnetic concentrate filter cakes obtained from several iron ore concentrators. Laboratory balling tests showed that unfired pellets made from these "clean" filter cakes were 50-100% stronger than the usual unfired pellets containing the salts. The fact that certain chemical additives dissolved in the water used for balling "clean" concentrates decreased the strength of unfired pellets indicates that salts in the plant process water may be responsible for lower strengths. According to chemical analyses of plant process waters at these plants, calcium and magnesium are probably the most detrimental salts in the plant circuits. It is suggested that calcium, magnesium, and other polyvalent cations in the mill process waters ion-exchange for lower-valence cations in the bentonite and thereby destroy the electrostatic-charge bonding in the green pellet. Some practical guidelines are also included for plant balling practices.

Jan 1, 1973

By Fred Porter

Pollution problems from smelters may be unique in industry since the pollutants cover the wide range of SOx, particulates, carcinogens (arsenic), plus a number of heavy metals, the health implications of which are not clearly understood. In addition to this wide range of pollutants, many of the plants are extremely old; and fugitive emissions may, in fact, be the most significant air pollution problem. The Environmental Protection Agency, both in an in-house and contract effort, has assessed the quantity of pollutants emitted and evaluated the health impact. This paper will review the status of EPA's regulatory efforts in both new and existing smelters in light of these pollutant assessment studies.

Jan 1, 1976

By J. Bruce Clemmer, P. E. Churchward, Carl Rompacek

The paper describes a cyclic method for processing manganese ores using sodium sulphate as the basic reagent. Sodium sulphate is electrolyzed in a diaphragm cell to give an anolyte sodium sulphate acid and a catholyte containing caustic soda, a part of which is carbonated in a cyclic manner to form soda and reduced ore is leached with the anolyte to dissolve the manganese and the impurities are precipitated by addition of catholyte. Manganese in the pregnant solution is precipitated as synthetic rhodochrosite with a carbonated catholyte, and sodium sulphate is regenerated. Calcining the manganese carbonate site a high-grade product and the carbon dioxide is returned to the carbonation step. the results of laboratory tests using cells equipped with synthetic fiber diaphragms and permselective membranes which permit transfer of using or cations during electrolysis are described. The article from which the above abstract is reprinted appears in Trans. AIME (1955) 203, p. 51; Journal op Metals (January 1955).

Jan 1, 1956

By A. Wahab Khair

This paper presents an analysis of fracture mechanisms in coal subjected to bi-axial state of stresses, indentation of laterally con- fined coal specimen. Coal specimens were loaded to failure by the straight wedge indenters at various lateral confinement pressures. Strain distribution and acoustic emission characteristics of coal specimens under stress were recorded. The influence lines of vertical forces acting on the horizontal straight boundary of the coal specimen for each type of wedge indenter have been established using holographic interferometry technique. The effects of wedge indenter angle, confinement pressure, and coal anisotropy on fracture types, failure modes, and post-failure conditions were studied. The results indicated that combined application of holographic interferometry and acoustic emission monitoring techniques is not only suitable for studying deformability of heterogeneous and microscopically discontinuous material under stress but it also enhances the mode of fracture during the post failure stage.

Jan 1, 1984

By R. Schuhmann

PROBLEMS in expressing, interpreting, and using size-distribution data recur in many phases of mineral dressing; therefore it is desirable that size analyses be expressed in such a form, either numerically or graphically, that comparisons can be made readily. The size distribution of comminuted material is a result of a specific physical operation on the material and therefore should be governed by some definite physical principle, or cause-effect relation. Although this principle has not been discovered, it has been found that the size distribution of comminuted, homogeneous solids may be expressed by relatively simple mathematical equations. Two equations in particular, proposed by Gaudin1 and by Rosin and Rammler,2 respectively, have stood out, both having wide demonstrated ranges of application. The form and the method of application of the two appear almost irreconcilably different on the surface, but, as will be shown, they are asymptotic in the fine sizes when expressed in the same units. This paper gives the results of a further study of the Gaudin and Rosin-Rammler relations, made with the object of developing a form of size-distribution equation that will be more usable and more significant-particularly in comminution studies, both for interpreting the nature of size distribution and for evaluating surface. The work is summarized in the following: I. An equation relating cumulative per cent finer to particle size in the fine sizes is derived from Gaudin's original equation. That equation relates weight per cent retained on one size and through the next larger size in a geometric series of sizes to size (of the retaining screen, for example). 2. Comparisons with Gaudin's equation and with the Rosin-Rammler equation show that the cumulative equation applies to the fine sizes of all size distributions that fit either of these earlier relations, and, furthermore, has some advantages over each. 3. A simple graphical method of surface calculation based on the cumulative-equation plot is evolved and illustrated. 4. Additional confirmation of the cumulative equation was obtained in the more severe test of sizing down to the limit of a sedimentation balance a sample of jaw-crushed quartz. The equation was closely followed over a 20o-fold range in size, from approximately 0.4 mm. (35 mesh) down to 0.0023 mm. (2.3 microns), the lower limit of the size analysis made. There is no indication that the equation will not hold further to well below 2.3 microns. 5. Calculations of the surface produced in the jaw-crushing test mentioned above showed that at least 8o per cent of the total new surface was on particles finer than 35 mesh (about ½ 5 of the crusher setting). The minus 35-mesh portion was only

Jan 1, 1940

By Narendrakumar A. Chevli

Exploratory work was conducted in the fabrication of integrated circuitry, specifically linear amplifier circuits, by three general methods: 1) monolithic diffused silicon; 2) a combination of metal thin-film and monolithic diffused silicon; and 3) a hybrid of metal films and diffused silicon on an alunina substrate. In these linear amplifier integrated circuits the followzng conditions were desired: very high-frequency response, high voltage gain, and good thermal tracking stability of electrical characteristics. The resulting circuit designs imposed problems of isolation between elements, layout and smallness of size of active elements, and close tolerances on electrzcal characteristics of the passive elements. Interconnection problems for specific designs resulted from the small dimensions involved and the topography of the hybrid fabrication techniques. The desired integrated-circuit characteristics were achieved with the technologies of categories 2 and 3 above. Solutions to the problems imposed by these characteristics lay in the ability to isolate czrcuit elements of small size while providing a layout designed to minimize element-to-element variations. Sufficient freedom in the formation of passive elements was achieved by uniting the metal film and the monolithic silicon technologies. The most satisfactory designs were based on the beam-lead interconnection and isolation technique. SINCE the advent of integrated circuits, major emphasis has been on fabricating digital integrated circuits. Linear circuits require high performance, high voltage, and tighter tolerance components which are not always compatible with the capability of process technology available for fabrication of these circuits into integrated form. Fortunately the growth of newer and improved processes and materials for fabricating integrated circuits has been an accelerated one. This has now made possible the translation of stringent performance requirements of the linear circuits into microminiature integrated circuits of the same performance. In the exploratory work of fabricating high-performance Linear Integrated Circuits—LIC, the following objectives were formulated: i) fabrication of high-frequency transistors such as the type 2N918 isolated on a single silicon substrate; ii) fabrication of medium-frequency transistors having a very high gain at low collector currents such as the types 2N930/2N2484 isolated on a single substrate ; iii) fabrication of tight-tolerance, high-valued resistors having low temperature coefficients of resistance and stable thermal tracking characteristics, these resistors to be fabricated on an active or passive substrate; iv) simultaneous fabrication of complementary transistors—pn and pnp-on the same silicon substrate; v) fabrication of newer active elements such as MOS, FET transistors along with the conventional active and passive elements on the same silicon substrate. State-of-the-art assessment f all the available processes, materials, and technology to meet above objectives indicated that economic fabrication of LIC cannot be achieved by a single technology for all types of linear circuits. Where design and performance of a given linear circuit can be modified and tolerated to the extent of a particular technology, then alone is it possible to fabricate a LIC using a single process technology such as all diffused, planar technology. In order to evaluate this economic breakpoint with design and performance compromise in fabricating LIC, it is essential that a thorough understanding be obtained of techniques, potentials, and limitations of all the various process technology and materials

Jan 1, 1967

By Ray W. Carpenter, Ralph Hultgren, Raymond L. Orr

Heats of formation of Au-Zn alloys of compositions Au3Zn and AuZn were rneasured at several temperatures by liquid tin solution calorimetry. The data for Au3Zn show that much smaller heat and entropy effects are associated with the a2- a1 transformation than for the a1 - a transformation. This result is consistent with reported X-ray diffraction studies which indicate that the a1 and (a2 phases have ordered structures which only slightly differ, whereas the a phase is disordered. The heat of formation of AuZn(ß') does not change significantly between 322o and 8000 K, confirming that the ß' alloy remains highly ordered to high temperatures. Not many measurements have been made of the energies of order-disorder transformations in alloy phases. In many cases these energies may be conveniently determined by measuring heats of formation as a function of temperature. Many alloy phases approximately obey Kopp's law of additivity of heat capacities; as a consequence their heats of formation do not change with temperature. In ordered alloys, however, a decrease in degree of order with increasing temperature will contribute an endothermic component to the heat of formation. Thus, for ordered phases where other anomalous contributions to heat capacity in the alloy or its pure components are absent, a measured change in the heat of formation may be attributed to the energy of disordering. A portion of the Au-Zn phase diagram1" is shown in Fig. 1. The composition AuZn(ß') has a well-ordered superlattice structure of the CsCl type at room temperature. The alloy is considered to remain ordered to its melting point,1 although, from X-ray diffraction data and electromotive force measurements of zinc activities, Terpilowski3 concluded that considerable disordering began at -673°K. The Au3Zn composition is a disordered fee solid solution (a) at high temperatures. Between 693o and 543oK, the ailoy orders to form the a1 phase, having a structure based on the L12(AuCu3) type, but with a regular distribution of ordering faults in the c direction, making it tetragonal. Below 543oK, the alloy orders further by means of slight atomic shifts, without diffusion, yielding a complex long-period orthorhom-bic superlattice structure, a2.4-7 Heats of formation of Au3Zn(a2) and AuZn(ß') were measured at 363°K by Biltz et al.8 by aqueous solution calorimetry. Heat capacities of several alloys between 14.9 and 38.4 at. pet Zn in the range from 373" to 723°K were measured by Iwasaki ef al.6 Stoichiometric Au3Zn, however, was not included in the alloys measured, the nearest composition being 26.1 at, pet Zn. Also, the heating rate used for the measurements, 2 deg per min, may not have permitted equilibrium to be reached in the neighborhood of the transformations. Heat contents of solid and liquid AuZn were measured between 488o and 1138°K by Kubaschewski.9 It was decided to determine the ordering energies of Au3Zn and to check on the possible disordering of AuZn by measuring the heats of formation of these alloys at several temperatures. The present paper reports measurements by liquid tin solution calorimetry of the heats of formation of the three phases of Au3Zn at temperatures within their regions of stability, and of AuZn at a low (322°K) and a high (800°K) temperature. EXPERIMENTAL Alloy Preparation and X-Ray Examination. Ten-gram ingots of Au3Zn and AuZn were prepared by melting weighed amounts of gold (99.95 pct Au) and zinc (99.99 pet Zn) together in sealed evacuated Vycor tubes at 1060°K, followed by rapid quenching. The resulting ingots were homogenized at 900°K for 10 days. The Au3Zn alloy lost no weight in preparation, the loss from the AuZn alloy was enough to introduce an uncertainty of only 0.1 at. pet in its composition. Filings for X-ray examination were taken from various parts of each ingot and strain-annealed at 723°K for 20 min in vacuo. The Au3Zn filings were quenched rapidly to retain the disordered phase. Diffraction patterns were determined with an X-ray dif-fractometer using copper Ka radiation.

Jan 1, 1968

By Richard P. Rothwell

Though coal has been mined in this country for more than a century, no systematic effort was ever successfully made to ascertain the total amount produced. The production of the Cumberland Basin, Md., and the shipments from the anthracite fields of Pennsylvania, have been placed upon record, thanks to the intelligence and foresight of Mr. C. Slack in the former case, and to the late Mr. B. Bannan in the latter. For some of the years between 1822 and 1842, the production of the Richmond Basin was reported by Mr. R. C. Taylor, but since that date till the author undertook this work it was impossible to obtain any statement of the production of this field. A few of the newer fields, such as that of Mt. Diablo, Cal., have been fully reported, and a few of the newer States have also had this service performed by some intelligent private individuals; but no statistics of coal production have ever been collected either by the State or General Government, if we except the returns for the years 1869—70 of the census report. During the year 1875, by great exertions, I succeeded in obtaining, and July 3d, 1875, gave in the Engineering and Mining Journal what, " though not an accurate statement of our coal production," was " by far the most full and reliable that had ever been published." Though that report showed the production of bituminous coal to be 23,630,094 gross tons, or about six million tons more than had ever before been reported, it was in reality two and a half million tons below the actual output. The more full returns I obtained for 1875 gave many figures for 1874

By Kendall E. Born, Walter F. Pond

Production of crude oil in Tennessee during 1935 approximated 20,000 bbl., an increase of about 5000 bbl. over 1934. The total production for the state is an estimate, since the only definite figures available are those for Scott and Morgan counties, where 12,377 bbl. were marketed during 1935, an increase of 4305 bbl. over the preceding year. The oil fields of Scott and Morgan counties are near the eastern margin of the Cumberland Plateau where Pennsylvanian sediments rest uncon-formably upon the Mississippian. Near Glenmary, in Scott County, the production is from the middle Mississippian, probably near the top of the St. Louis limestone. Accumulation is due to a low, east-west anticline which has been cut by a fault. This field is now 20 years old and only a few wells are pumped at present. Oil was Struck along Boone Camp Creek in Morgan County in 1924 and there has been small production since that time. The oil comes from the middle of the Fort Payne formation of lower Mississippian age at a depth of 1400 ft. Geologic work in the area has shown that a terrace and porosity conditions in the Fort Payne formation account for the accumulation. The production figures on a number of small producing wells in Clay and Overton counties are not available. As pointed out by Glenn1, the installation of small local skimming or topping plants in the fields has curtailed the shipment of crude oil out of the state and as a result it has been impossible to secure accurate production figures in these counties. The operators, in most cases, are reluctant to give information, and there is no state law requiring them to do so. Based upon information available to the writers, it is believed that between 7000 and 8000 bbl. is a fair estimate of the production in Clay and Overton counties during 1935. More than 500 wells have been drilled in Clay County, the majority of which were drilled east of Cumberland River. Some eight small oil fields have been developed in the county within the past 12 years, a

Jan 1, 1936

By Nicholas J. Grant, Olaf Troili, John Chipman

IN recent studies of the factors which affect the rate of desulphurization and its equilibrium, it became apparent that certain concurrent reactions were operative which had a significant effect on desulphurization. This is emphasized in the experiments of Hatch and Chipman1 and of Grant, Kalling, and Chipman' by the slow approach to a final state of equilibrium which is in marked contrast to the initial rapid transfer of sulphur from metal to slag. Since the removal of sulphur is of such profound importance in iron and steelmaking, it appeared necessary to investigate the reactions responsible for this behavior. It is now known that the presence of iron oxide in the slag interferes seriously with the principal reaction of blast-furnace desulphurization: CaO (slag) +-S + C - CaS (slag) + CO [l] The interfering reaction is most simply expressed as: CaS (slag) + 0 = CaO (slag) +-S 121 and a small concentration of oxygen (or FeO) is sufficient to hold a considerable amount of sulphur in the metal. It has been shown by Grant, Kalling, and Chipman2 that the addition of MnO to blast-furnace slag slows the removal of sulphur from the metal. This effect overshadows the contribution of MnO to basicity and is ascribed to its oxidizing power. It will be shown in this paper that SiO, also has sufficient oxidizing power to interfere with blastfurnace desulphurization. This is, of course, only one of its several effects. Primarily it is an acid and therefore reduces the concentration of excess lime. But when silicon is reduced to the metal the oxygen to which it was previously bonded becomes in part available for reaction 2. The proof of this statement is found in the following experiments. Experimental Procedure and Results Utilizing the same procedure and apparatus described by Grant, Kalling, and Chipman' five additional heats were made using slags IV and 11, the starting compositions of which were: slag IV—40 CaO, 10 MgO, 35 SiO,, 15 A1,0,; and slag 11—50 CaO, 10 MgO, 25 SiO,, 15 Al3O3. An important difference between these heats and those previously reported was that silicon to the extent of 1 to 4 pct was added to the present heats whereas the starting silicon content was formerly about 0.2 pct. Table I shows the slag and metal analyses for heats 82 to 87, and Table I1 shows the silicon addi- tions made to the charge. These additions are based on 400 g of metal and 400 g of slag. All heats had 1.65 400pct S charged before the cold slagadditions. The temperature was maintained at 1525°C. Rate of SiO, Reduction: Fig. 1 shows the silicon content of the metal in contact with slag IV at 1525°C as a function of time. Heat 70 from the work of Grant, afunctionKalling,of and Chipman is included as the lowest starting silicon. It will be noted that eeven with 4 pct Si in the starting metal, there is an increase in silicon content with time. Heat 84 is apparently approaching silicon equilibrium very slowly. Heats 70 and 82 with very much lower slowly.starting silicon show a more rapid initial rise in startingsilicon content but do not reach equilibrium during a long holding period. Fig. 2 shows 3 different initial silicon contents for Fig.2shows3differentheats 73 (from Grant, Kalling, and Chipman) 86 and 87, in contact with slag II, the most basic slag. Heat 73 is increasing in silicon with time, whereas heat 87 with an initial silicon content of 3.7 pct shows a decrease with time. Heat 86 shows a very close approach to equilibrium. The rate of transfer of silicon from slag to equilibrium.metal is very slow in all of those heats, even those which are initially far from equilibrium. ____

Jan 1, 1952

By H. C. Jennison

Two distinct types of defects occur at times in copper wire as a result of the use of dies of improper design or undesirable wire-drawing practice. The conditions under which these defects may be produced, as well as precautions to be taken in order to prevent them, have been known to The American Brass Co. for many years. The quality of the copper wire bars and rods has too often and unjustly been held responsible for these particular defects and it is to correct any such belief that this paper is presented. An extremely high quality of electrolytic copper has been supplied to the trade by all refineries for the last 20 years at least. The purity of the copper would average well above 99.900 per cent. The casting of the wire bars has been handled in a generally satisfactory manner. The bars have been cast sound, with a flat to slightly crowning set and have been free from sloppy edges, cold sets, etc. In other words, the wire bars have met A. S. T. M. specifications and have been generally satisfactory. For the most part, they have been everything that could be desired from a quality standpoint yet most of the wire mills in this country and in Europe have at times held the quality of the copper responsible for the two types of defects described in this paper. As a matter of fact, these defects are produced entirely in the wire mills. The author has visited many of the large wire mills in the United States and in Europe to investigate these defects. In some cases the trouble has been so serious that the wire mill has ceased operations. At times the wire mills are reluctant to believe that they are responsible for the defective product. The effect of die design, wire-drawing practice, etc., upon the quality of copper wire has received' little study on the part of wire mills, particularly those that have commenced operations in the last few years.

Jan 1, 1930

By Newell Hamilton

Some years ago, in the manufacture of seamless tubing from an alloy steel containing 0.07 per cent maximum carbon, 18 per cent chromium and 8 per cent nickel, at the plant of The Babcock & Wilcox Tube Co., a peculiar type of piercing defect was noticed. This defect was definitely associated with certain heats of the alloy and was independent of any of the variables of mill operation and billet-heating condition. A thorough analysis of the defective material yielded but one clue to the reason for its abnormal behavior in piercing and that was its oxygen content as determined by the vacuum fusion method. The oxygen content of the defective 18-8 alloy was found to be from two to three times that of the material that had pierced satisfactorily, and this incited an active interest in the vacuum fusion method for the analysis of alloy steels. After a critical survey of the literature on this subject, and considerable experimentation, an apparatus and technique were evolved that gave a fairly rapid, simple and reliable method of analysis. Samples selected from six years of tube production of 18-8 and other corrosion-resistant alloys were analyzed by this method. This paper describes the procedure and gives a correlation of the oxygen, hydrogen and nitrogen contents of a number of alloy steel samples representative of good and bad tube-piercing quality. The Apparatus Basically the apparatus used in this work was that of Jordan and Eckman,' employing a high-frequency induction furnace and the gravimetric method of analyzing the evolved gases, nitrogen being excluded from the determination. In addition, a magazine-type cap and a large-

Jan 1, 1934

By R. H. Ernst, H. R. Ogden, D. J. Maykuth

AT present, no theories exist which allow prediction of the effect of alloying additions on the thermoelectric properties of metals. Nevertheless, Battelle and others1 have observed that, at high temperatures, the peak thermal electromotive-force output (relative to a platinum standard) occurs with metals in Group VI of the Periodic Chart. The authors suspected that this peak was associated with the fact that maximum electronic bond stability is achieved with these metals which have six bonding electrons per atom. On the basis of current electron-concentration theory for transition metals and alloys:' it was surmised that the addition of valency electrons to metals of Groups IV and V (accomplished by the addition of metals from Groups VI, VII, or VIII) should progressively increase the thermoelectric-power output of the resulting alloys until an alloy composition is reached at which the number of valency electrons per atom is six. A further increase in the ratio of valency electrons per atom should then decrease the thermoelectric power. In contrast, the addition of bonding electrons to Group VI, VII, or VIII metals should decrease their thermoelectric power since the electron per atom

Jan 1, 1965

By C. W. Spencer, B. F. Addis, G. H. Bishop, C. A. Steidel

STUDIES of the inter granular attack of metals by liquids have generally been confined to polycrys-talline specimens. This note reports the results of preliminary studies of the penetration of bismuth-rich Ni-Bi liquids into oriented bicrystal specimens of nickel. It is found that isothermal penetration follows a parabolic rate law and shows a definite anisatropy with respect to direction on the grain boundary surface. Nickel bicrystals containing < 100> tilt boundaries were grown using the Czochralski method. Relative misorientation of the parent crystals was controlled to ± 1deg. The boundaries are straight in the growth direction, i.e., the common <100>, and generally straight in the transverse direction, as shown in Fig. 1. The starting material, Inco HPM grade nickel was contained in a recrystallized alumina crucible and maintained under argon. Bicrystals typically contain 30 ppm C, less than 10 ppm S, O, N, and 50 ppm residual metallics, principally iron and silicon. Specimens, as schematically illustrated in Fig. l(c),were cut from bicrystal ingots using a thin water-cooled abrasive wheel. To insure removal of all residual strain, which accelerates the penetration, specimens were round through 600 grit silicon-carbide, chemically polished, and annealed for 4 hr at 1375°C under argon. The procedure described by Cheney et al.1 for exposing specimens to

Jan 1, 1962

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&apos; 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.&apos; 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.&apos; 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

By Walter Weeks

THERE is very little useful material in the litera-ture on the construction of manometers, so each experimenter must devise his own instrument. I have experimented for a number of years and have finally built one that is satisfactory. If we are to obtain accurate friction factors in mine-ventilation problems we must use accurate instruments. The most simple and convenient instrument for the mea-surement of small pressures is the inclined manometer or U-tube. By changing the angle at which the tube is set, any desired magnification of the pressure reading may be obtained. The first question in regard to the manometer is: What liquid shall be used? Alcohol, in my opinion, is the best. It does not cling to the glass and it does not attack the rubber tubes. The next problem is the setting of the instrument at the proper angle. One method is illustrated in Fig. 1. The base plate AC is made horizontal by a level bubble. The plate AB, which carries the U-tube, is hinged at A. The angle z which AB makes with the horizontal may be made any value by pinning the end B at the calculated position on the arm CD. Such an instrument may be designed to read directly in inches of water if a liquid of constant specific gravity is used. If the specific gravity varies, a calculation is necessary to convert the reading into inches of water.

Jan 1, 1923

By Wm. R. Webster

This is a contribution for the proposed new discussion on the physics of steel. The former discussion on the subject started with the consideration of five papers presented at the Chicago meeting in 1893, and continued for several years. The Suggested Lines of Discussion, prepared by Doctor Howe, covered a wide field and added greatly to the success of the work. Naturally, the first step in a new discussion will be to remodel and bring up to date the old Suggested Lines of Discussion so as to embody all the important advances in the metallurgy of steel that have a bearing on the physics of steel and keep the papers and discussions within the field of work undertaken. This paper will be devoted to the practical application, in rolling steel, of the effects of carbon, phosphorus, and manganese on its tensile strength, with some suggestions on further research work. Dr. J. E. Stead, in his paper Influence of Some Elements on the Mechanical Properties of Steel,&apos; gave a complete review of all that had been done during the past thirty years. He gave full credit to all investigators who worked on these lines, also their results, with his views on same, and in many cases his own results. All of this data and much new valuable information were put in convenient shape for reference and study. To do this required a great deal of work, which is fully appreciated by the steel manufacturers and investigators. The variations in the values given by the different investigators for the increase of the tensile strength of steel for each 0.01 per cent. of carbon, phosphorus, and manganese were largely due to the steels they worked on, the large or small variations in the amount of the elcments present, and the omission to take into consideration all the factors, from the blast furnace through to finished rolled material, that affect the character of the steel. For instance, a poorly made dirty steel requires considerably more carbon to give the same ultimate strength than a well-made clean steel with the same phosphorus and manganese content.

Jan 1, 1922