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By AIME AIME

MODERN metallurgy is an art and a science. The art is process metallurgy-extracting metals from their ores, refining them, and alloying them with one another and with certain nonmetals to produce thereby a variety of metallic materials which, owing to a wide range of useful properties, are for many purposes more valuable to man than the individual metals themselves; process metallurgy also includes shaping or otherwise treating metals and alloys to form objects useful to a complex industrial world. The science is physical metallurgy-organized knowledge of the constitution and internal structure of metals and alloys, of the relation of their composition and structure to properties, and of the laws, theories, and hypotheses that purport to explain this relation.

Jan 1, 1942

By Allan T. Gwathmey, J. Bruce Wagner, Kenneth R. Lawless

Between 250°and 550°C in oxygen pressures of 10 to 760 mm Hg, the relative oxide thicknesses formed per unit time on the (100), (111), (110), and (320), decreased in this order. The predominant oxide orientation was (001)Fe3O4 and [110] Fe304 A small amount of a-Fe2O3 which exhibited a fiber pattern was observed in all oxides except those formed at 250°c in low oxygen pressures. IN order to understand the properties and behavior of thin films, particularly their role in oxidation reactions, there is needed more experimental information on their structure, composition, and kinetics of formation on clean surfaces of known geometry. The present study was undertaken to obtain such information for thin oxide films formed on single crystals of a body centered cubic metal, iron. Crystals in the form of spheres were used in order to expose all possible crystal planes to the reactant gases simultaneously. Using this procedure the relative rates of oxidation of all planes could be estimated, and those exhibiting, maximum or minimum oxidation rates could be selected for a more intensive study of composition and expitaxy. Since the three types of information were obtained from the same experiment using a single crystal substrate, any differences between rate, composition, and expitaxy on the several planes may be attributed to the influence of the substrate structure. EXPERIMENTAL The starting material for this study was Armco iron rods, 6 in. long and 3/8 or 1/2 in. in diam. The analysis was reported to be 99.8 pct Fe, with major impurities listed as carbon 0.018 pct, manganese 0.027 pct, phosphorous 0.005 pct, sulfur 0.029 pct, silicon 0.005 pct, and copper 0.11 pct. These rods were cleaned with ether and heated in an atmosphere of moist hydrogen at 950°C for three days. The purpose of this treatment was to decarburize the iron and to provide a consistent, uniform grain size for the growth of single crystals. Crystals in the form of rods, up to 1/2 in. in diam and 2 in. long, were prepared by a method similar to that reported by Leidheiser and Buck.2 Spherical crystals, 3/8 and 1/2 in. in diam and having a handle about 1/4 in. in diam by 112 in. long, were machined from the single-crystal rods. After machining, each crystal was etched in aqueous nitric acid to remove the cold-worked metal at the surface. Before each experiment, the crystal was polished mechanically with metallographic papers through number 4/0, and electropolished in a perchloric acid-acetic anhydride mixture by the method of Jacquet and Rocquet.3 The crystal was washed in running distilled water for at least 5 min. The excess water was blotted with a soft paper tissue, and the crystal was placed in an all-glass reaction vessel (See Fig. 1). The crystal was heated at 550°C in hydrogen for at least 8 hr prior to the oxidation in order to reduce any surface oxides and to help relieve any stresses in the metal. For the structure and composition studies, flat faces were cut parallel to (loo), (111), and (110) planes on the iron crystal spheres. The orientation of these faces was checked by a back-reflection X-ray diffraction technique. The faces were within 2 deg of the desired orientation. The flat faces were treated as described above except that prior to electropolishing they were given an additional polish on metallographic felt saturated with twenty-minute levigated alumina. After the crystal was heated in hydrogen for at least 8 hr, the temperature was adjusted to the desired value, and the hydrogen was evacuated. Commercial oxygen which had been purified by successively passing through tubes containing magnesium perchlorate, Ascarite and magnesium perchlorate was admitted to the desired pressure as measured by a mercury manometer. A resistance-wound furnace surrounded the oxidation chamber, and a temperature controller maintained the temperature within ±3°C. The furnace was provided with a small window for observing the crystal. The changes in thickness of the oxide films were followed by observing the interference colors. The oxidation was allowed to proceed until the desired oxide thickness was attained on a given crystal plane. The experiment was terminated by evacuating the oxidation

Jan 1, 1962

Jan 1, 1893

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION TO OCTOBER, 1904 Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

By J. E. Burke, C. W. Mason

IN attempting to study precipitation from a tetragonal lattice using solid solutions of bismuth in tin, it was found that although a Widnmanstatten pattern is observed 1 only a qualitative analysis of the orientation relationships is possible, because of the unusual structural changes that accompany the precipitation process MICROSCOPICAL STUDIES Alloys were made from Chempur tin (Standard samples 42b and 42c, National Bureau of Standards), and bismuth (Kahlbaum C P ) by melting neighed quantities together under palm oil, stirring well, and casting in a heated graphite mold The polishing and etching techniques employed largely govern the visibility of the structural changes The preliminary surfacing operations were similar to those recommended by Villela and Bergekoff,5 through BehrManning 3/o abrasive papers, lubricated by a solution of paraffin in kerosene A rough metallographic polish was next given, using a thin cotton cloth charged with relevigated alumina (maximum particle size of about 4µ) and soap solution, repeated etching and polishing served to remove disturbed metal For high-power examination better preparation was necessary It was found that on such soft metals the threads of the fabric, rather than the abrasive, cause most of the scratching Cotton outing flannel, which had been brushed so that the nap lay down, was fairly satisfactory, but a Heavy grade of silk velvet (not the noncrushable kind) was found to be better, especially after some use A better procedure was as follows The metal lap was warmed slightly, and a 4-in circle of woolen broadcloth was cemented to its center by a thin film of melted paraffin The broadcloth was then moistened with water, and a 30 to 40 per cent solution of sodium hydroxide heated to about 50°C was poured over it, allowed to stand for 1 to 2 min and then washed off It was neither necessary nor desirable to remove all the sodium hydroxide from the cloth, since its etching action aided in the removal of the flowed layer from the sample The cloth was then charged with a paste of the relevigated alumina in water Since this lap did not remove deep scratches, it was necessary previously to polish the specimen on some material such as the silk velvet The sodium hydroxide softens and partly gelatinizes the woolen lap covering, permitting a scratch-free polish, but its action continues, and the cloth deteriorates after about 24 hr This is not serious, because a new lap can be prepared in about 5 min, and only small pieces of cloth are used Etching with a strongly acid solution of ferric chloride was found satisfactory for removing the flowed layer For the final etching, the most satisfactory reagent was that of Taffs,7 the formula for which is FeC13 6H20, 2 grams, HC1, 5 c c , H2O, 30 c c , C2H5OH (95 per cent), 60 c c This etchant reveals differences in com-

Jan 1, 1941

By B. C. Allen

The solubility of chromium in liquid silver and that of molybdenum and tungsten in liquid tin have been determined by equilibrating Ike Liquid in a crucible of the solule metal. Generally the weight of solute in solulion was delermined both chemically and from crucible weight losses. The resulting weight percent solubilily of chromium in silver as a function of absolule temperature T is given by log w = -6660/T + 4.02 in the range 960° to 1445°C, and that of molybdenlttrl in tin by log w = —5050/T + 1. 79 in the range 1200° to 2200°C. The values appear unaffected by minor changes in solute composition. Calculations aye made of the parlial molar heal and excess entropy of mixing. The estimated solubility of tungsten in tin is 0.001 pct at 2000°C. Evidence is presented that molybdenwm dissolves in tin without compound for mation and that tungsten and tin form W10Sn. RECENT developments in coatings, heat transfer, and brazing require a knowledge of equilibrium solubilities in a variety of systems at elevated temperatures. Of particular interest are solid-liquid interactions in metal systems involving dilute solutions. This investigation was undertaken since little is known about the phase relations or solubility of chromium in liquid silver or of molybdenum and tungsten in liquid tin.1,2 EXPERIMENTAL WORK As indicated in Table I, high-purity metals or those of known impurity levels were used. Crucibles were machined from chromium, molybdenum, and tungsten bar stock 1.3 cm diam and 2.2 cm long. Chromium rod was prepared by arc melting and extruding iodide process crystals.3 The five chromium impurity alloys were in the form of 0.6-cm-diam swaged rod. A Cr-0.06N* alloy was prepared by exposure to NH3 at 1150°C in a closed quartz capsule for 24 hr. Because significant nitrogen was lost during annealing in argon at 1600°C,4 the estimated level was 0.01 pct N. Chromium and Mo,W crucibles were outgassed at 1200" and 1600°C, respectively, at 3 X 10-5 mm. The solvent was placed In crucibles of the solute metal- 6 g Ag in chromium, 0.4 g Ag in the five chromium impurity alloys, and 4 g Sn in Mo,W crucibles. The silver and tin series were outgassed at 900" and 110O°C, respectively, and held at the desired solution temperature in a tantalum resistance furnace under 1.05 atm 99.995 pct Ar. An equilibration time of 0.5 to 1 hr was chosen since 0.3-, I-, and 4-hr anneals at 1235°C for Cr-Ag yielded similar results. Temperatures were measured optically to +10°C under essentially black body conditions which were checked against the melting point of silver. The Cr-Ag and Mo-Sn,W-Sn series were respectively equilibrated at 990° to 1400°C and 1200" to 2000°C. Vaporization losses were generally held to <1 pct by the argon. In the 1800" and 2000°C anneals for 0.5 hr, the crucibles were placed in tightly sealed tantalum cans which kept tin losses to <5 pct. After the anneals, the specimens were furnace-cooled. One anneal was made on small Mo-0.02 C, Mo-0.5Ti-0.lZr, and tungsten crucibles containing tin at 2200°C. The metals were sealed in an electron-beam-welded tantalum can of minimum volume. After the anneal, tin was still present in each crucible, none of which was severely attacked. After equilibration, the saturated solvent metal was selectively removed from the crucible by acid leaching. Weight losses sustained by the crucibles were determined from the initial weight minus the final blank-corrected weight after acid leaching. Chemical analyses were performed on some of the samples. Hot 1:l HNO3-H2O removed silver from chromium with the blank running <0.1 mg or <0.002 pct on measured solubility. Tin was removed from molybdenum and tungsten by hot concentrated HC1 with the respective blanks amounting to -0.004 and -0.0004 pct in the presence of tin. The insoluble residues were weighed and checked for composition. The leaching solutions contained traces of the solute metals which were analyzed by colorimetric methods, Diphenyl Carbazide for chromium, Thiocyanate for molybdenum, and Dithiol for tungsten. The total of the two percentages found from the residue and leaching solution minus the blank gave the desired solubility values. On the basis of annealing empty molybdenum and tungsten crucibles, weight losses due to MoO3 or WO3 volatilization were found to be generally 10.4 mg and affect measured solubilities by <0.01pct. RESULTS AND DISCUSSION Chromium-Silver . Since no intermediate compounds are reported to form in the Cr-An system,&apos; crucible weight losses and chemical analysis of the entire melt should provide reliable measures of the chromium in solution. Values obtained by the two methods are in agreement as shown by the results for unalloyed chromium in Table II and plotted in Fig. 1. Furthermore, the results are consistent with those previously determined by melting equilibrated silver out of the crucible and analyzing calorimetrically for chromium.&apos; On the basis of limited thermal analysis data, the solubility of chromium in silver has been quoted as 8 pct at the monotectic temperature of -1445°C.1 This investigation indicates an extrapolated solubility of 1.38 pct which is believed to be more reliable. At the eu-

Jan 1, 1968

By E. J. Eisenach, Edward Matsen

AT the present time the Climax Molybdenum Co. is the largest molybdenum producer in the world and the operator of the largest underground mine in North America. It has grown steadily and rapidly since its beginning in 1917. Only 250,000 lb of MoS2 were produced during the first year from 1917 to 1918 when the company was formed. Operations were suspended shortly thereafter because of the lack of a market and knowledge of the uses of molybdenum. During World War I it was used as a substitute for some rare metals and for minor chemical purposes. After 5 years of intensive research and sales promotion, Climax metallurgists succeeded in finding proper applications for the newly discovered metal and the mine was reopened in 1924. Demand for molybdenum increased gradually and in 1930, 3.5 million lb of MoS2 were produced. In the meantime, research work for additional uses of molybdenum continued until it had established itself as one of the most important alloying elements in producing high quality steels. After the start of World War 11, from January 1942 to October 1953, 43 million tons of molybdenum ore were mined and 484 million lb of MoS2 were produced. Climax mine is located in Colorado, 100 miles southwest of Denver and 12 miles northeast of Leadville on the Continental Divide of the Rocky Mountains. The principal mine workings range from 11,170 to 12,000 ft in elevation. Topographically, it lies in the base of a large cirque that is surrounded by Mt. Bartlett to the north, Clinton Peak and McNamee Peak to the east and Ceresco Ridge to the south. This cirque opens to the west and to the Ten Mile Valley.

Jan 3, 1954

By R. F. Hehemann, Darrell W. Smith

The kinetics of alloying- in W-5 rot pct Re powder compacts were investigated at temperature about the upper limit for the formation of the x phase, such that a single intermediate phase was involved in the process. The rates and directions of motion of the a-o and o-b interface were assessed as functions of tinze at the sintering teri7peraticve by quantitative izetallog-ralhic techtziques. The iiotion 01 these interjuces could be specified approxitnate1.y by u Parabolic )-ate law and deviations from this ,rate law were attribuled to a complex interaction between surface dif&apos;fusion and volume diffusion during the initial stages of sintering. WHEN binary or more complex alloys are produced by sintering compacted blends of elemental powders, a complication is encountered which does not arise in the sintering of pure metals. In addition to concern for grain size and densification, the rate of inter diffusion of the component elements must be considered. The general problem of alloying during sintering has been treated by numerous investigators.&apos;-7 These investigations have been concerned only with systems that form continuous series of solid solutions and a concentric-sphere diffusion model4 provides a useful description of homogenization in these stems.&apos; Some controversy remains, however, over the contribution of surface and grain boundary diffusion to the homogenization process. Heckel% ePorts that homogenization can be described by volume diffusion at all temperatures, whereas other invetiators&apos;&apos; recognize the importance of surface and grain boundary diffusion, particularly at lower temperatures. Analysis of the homogenization process in partially miscible systems is complicated by the motion of the interfaces separating the individual phases. A simple analytical solution does not exist for such finite systems with spherical symmetry. It was the purpose of this work to examine the kinetics of the formation and dissolution of an intermediate phase in a binary system through an assessment of the motion of the interfaces separating this phase from the terminal solid solutions. PROCEDURE The W-Re system is an example of a partially miscible binary system and was selected for study because of its current importance in refractory-metal technology. The equilibrium phase diagram, Fig. 1, shows that the o phase will be formed by interdiffu-sion between tungsten and rhenium. At temperatures between approximately 2125" and 282O°C, the o phase will appear as the only intermediate phase in the diffusion system. In this work, a mixture of elemental powders containing 5 pct Re was employed. In such a mixture, the rhenium particles will be distributed randomly in a tungsten matrix. During sintering, a o-phase layer will form at the W-Re interface. The development and subsequent disappearance of the o phase are controlled by the relative rates and directions of motion of the 0-0 and a-p interfaces. The motion of these interfaces can be inferred from quantitative metallographic measurements of the average radii of the o shells surrounding rhenium particles. Elemental tungsten and rhenium powders of commercial purity were employed in these investigations. The rhenium powder was spheroidized from +200 mesh agglomerates by plasma-arc spraying and was then classified to yield a powder composed of essentially

Jan 1, 1967

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

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1917

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1917

By H. A. Doerner

PROPOSALS to use hydrocarbon or natural gases for the reduction of zinc from oxide materials may be traced back through Patent Office files to the early years of the present century. Natural gas at rates cheap enough to compete with solid fuels has been available at or near one major zinc district for more than a decade. That the seemingly meritorious and economically interesting applications of these proposals have not devel-oped into workable processes for direct production of zinc by natural gas cannot be completely ascribed to the proverbial conservatism of the zinc industry. It is possible to produce spelter commercially in normal times from zinc oxide and carbonaceous reducing agents without having a very precise understanding of the chemistry of the process. The reduc-tion by hydrocarbons is not, however, in this class, and the technical complexity of this reduction metallurgy and chemistry prohibits solution of the inherent difficulties by the "hit and miss" methods that are some-times thought to be practical. In a thermodynamic study of the chemistry of zinc smelting, Maier1 made a preliminary study of the chemistry of the use of methane for reducing zinc oxide by thermodynamic means, pointing out that the following reactions, the limits of which could be theoretically predicted, were important: ZnO + CH4 = Zn(gas) + CO + 2H2 [1] CH4 = C -I- 2H2 [2] ZnO + CO = Zn(gas) + CO2 [3] ZnO + H2 = Zn(gas) + H2O [4] Other possible reactions, not discussed in the reference quoted, are: CO2 + CH4 = 2CO + 2H2 [5] H2O + CH4 = CO + 3H2 [6]

Jan 1, 1933

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

By J. A. Clum, R. W. Heins, T. D. Tiemann

The use of Na-montmorillonite clay hinders (Western Bentonite) in the pelletizing of iron ore concentrates is well established as is the idea that alternative binders must be found. 1-6 This note summarizes work done7 in evaluating a Wisconsin montmorillonite clay binder. The clay occurs in irregualr beds overlying the Prairie du Chien Dolomite and the St. Peters Sandstone near Hersey, St. Croix County. The raw Wisconsin clay contained 65% quartz and 35% clay minerals. The Na20to CaO ratio was 0.234. Suspension viscosity tests of the raw clay gave results only slightly better than water alone, even after treatment with activator materials. Sedimentation treatment reduced the quartz in the decantate to 5% after 240 min (four hours). Twenty minutes of sedimentation produced a decantate with 27.5% quartz which was found as effective as the 5% quartz decantate in pelletizing behavior. The 20 min decantate was used in subsequent tests. The decantate was filtered and dried at 110°(230°F). The minus 200 mesh portion of this was added directly to the magnetite concentrate. Pellets were made in a laboratory sized disc pelletizer from pastes consisting of ore concentrate, balling water (9%) and binder (clay, or clay + resins, or resins). The pastes were premixed in a Waring blender. The binders were: (1) 1% of a commercially used Western Bentonite; (2) 1 % or 3% of the Wisconsin clay (raw, or 20 min decantate); (3) 20 min decantate washed with activator solutions, (to exchange Na for Ca in the clay); (4) decantate with activator added in the balling water; (5) decantate with organic resins; (6) organic resins. Measurements of the 0.46 m (18 in.) Green Drop Number, the Dry Strength and the Fired Strength (fired at 1260°C (2300°F) for 30 min) were made. The dry and fired compressive strengths were determined on an Instron testing machine using a C-load cell and a F-load cell, respectively. The cross-head speed was 0.004 m/sec (0.1 in./min) for both. The results of each measurement were averaged for 15 pellets. A summary of those results is presented in [Table 1]. More detailed results and procedures are presented in another report.7 In addition to the effects on pellet strength due to various binders the effect of varying magnetite concentrate characteristics is noted in [Table l]. There, a few comparative data are shown for Cornwall, PA Magnetite, which has a generally liner particle size than the Black River Falls magnetite which was used for most of the tests.

Jan 1, 1979

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1917

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1917

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1910

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page I Wilkes-Barre, Pa * May, 1871 I 3 II Bethlehem, Pa August, 1871 I 10 III Troy, N Y November, 1871 I 13 IV Philadelphia, Pa February, 1872 I 17 V New York, N Y * May, 1872 I 20 VI Pittsburg, Pa October, 1872 I 25 VII Boston, Mass February, 1873 I 28 VIII Philadelphia, Pa * May, 1873 II 3 IX Easton, Pa October, 1873 II 7 X New York, N Y February, 1874 II 11 XI St Louis, Mo * May, 1874 III 3 XII Hazleton, Pa October, 1874 III 8 XIII New Haven, Conn February, 1875 III 15 XIV Dover, N J * May, 1875 IV 3 XV Cleveland, 0 October, 1875 IV 9 XVI Washington, D C February, 1876 IV 8 XVII Philadelphia, Pat June, 1876, V XVIII Philadelphia, Pa October, 1876 V 9 XIX New York, N Y February, 1877 v 27 XX Wilkes-Barre, Pa * May, 1877 vi 3 XXI Amenia, N Y October, 1877 vi 10

Jan 1, 1917