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By Debbie Marshall

Nickel and cobalt in lateritic ores can be extracted by either a hydrometallurgical or a pyrometallurgical route. The high-iron limonitic fraction of a deposit is best processed' hydrometallurgically while the magnesium-rich transitional and saprolitic fractions are more suited for pyrometallurgical processing. During hydrometallurgical processing, it may be attractive, for economic reasons, to blend the limonitic component with transitional and saprolitic ores, which contain higher nickel levels. However, blending increases the concentration of magnesium in the feed, leading to increased acid demands. The decision on how much ore to process then becomes an economic one. Ore samples with different magnesium contents were prepared for the leach test program by blending limonitic and transitional ores. The ore samples were slurried in seawater and tested in the Falconbridge Hydrometallurgical Pilot Plant. As expected, acid consumption increased with increasing magnesium content of the ore. For target extractions of 95% nickel and 92% cobalt, the required residual free acid concentration increased from 30 g/L at 1.7% magnesium to 50 g/L at 2.7% magnesium. When the magnesium content was raised to 3.8% and 4.6% in subsequent pilot plant testing, the final free acid requirements did not increase beyond what was observed at 2.7% magnesium. Thus, the cut-off ore composition to maximize nickel units and minimize acid requirements is between 1.7- 2.7% magnesium. Keywords: high pressure acid leaching, laterites, magnesium

Jan 1, 2004

By R. F. Neider, W. R. Bain

"Expanding upon one aspect of a recent paper on ""Fluid Column Roasting at Sherbrooke Metallurgical Co. Ltd.,"" the present paper deals with the operation of the fluid column process to achieve substantial elimination of cadmium and lead during the roasting of pelletized zinc concentrates. Designed to meet the need for additional feed for Matthiessen and Regeler Zinc Company's vertical retort zinc smelter in West Virginia, without recourse to a sintering operation, the plant is capable of simultaneously attaining very low lead and cadmium levels on demand, through operation in the manner described. Fluidizing air admitted via the wind box is supplemented by natural gas admitted via a tuyere bank 15 ins. above the hearth, in quantities adjusted to maintain a reducing atmosphere within the interstices of the bed. In addition, careful attention is paid to bed temperatures, which run from 1,080° to 1,100°C. Under these reducing conditions, 90 per cent of the cadmium and 92 per cent of the lead in the feed are eliminated, the sulphate sulphur content is decreased by 0.5 per cent, sulphide sulphur is held at 0.6 to 0.08 per cent, and the zinc content correspondingly in-creases. The fuel value of the natural gas is recovered as extra steam, which carries a credit. There are some added difficulties with fume accretions, gas conditioning and gas -cleaning, some of which have yet to be overcome."

Jan 1, 1967

By K. Lagnese, C. Robinson, S. Muddasani

"Mine water generated from underground coal mining operations contains both dissolved and particulate solids. Dissolved solids primarily consist of sodium, calcium, magnesium, potassium, chlorides and sulfates. When discharged to a receiving stream without treatment, these constituents create a potentially toxic environment for aquatic life. A case study is presented to discuss how a centralized treatment plant treats mine water from six locations to meet discharge limitations for chlorides. Located in West Virginia, this facility consistently achieves less than the NPDES permit limitation of 218 mg/L chlorides in the discharge while generating almost zero liquid waste. The dissolved solids concentration in the influent ranges between 5,000 and 10,000 mg/L, with chloride concentrations of 1,000 to 2,000 mg/L and sulfate concentrations of 2,000 to 6,000 mg/L. The mine water is treated using advanced treatment technology to produce clean water for discharge or reuse. The treatment process comprises aeration, softening, filtration, reverse osmosis, RO reject softening, evaporation, crystallization, final effluent remineralization and sludge dewatering. The solid waste generated in the treatment process is landfilled on site. The leachate is sent back to the facility’s thermal treatment process. Because no liquid waste leaves the property, this plant is termed a “Zero Liquid Waste” (ZLW) facility. INTRODUCTION The advanced water treatment system was built to meet a new 218 mg/l regulatory limitation imposed by the West Virginia Department of Environmental Protection for chlorides discharged to surface waters. The system is designed to treat a maximum flow of approximately 5 million gallons per day (795 m3/h) of mine water. The treatment process utilizes reverse osmosis (RO) membrane treatment to achieve the effluent criteria, and evaporation and crystallization technology to manage the RO concentrate from the water treatment process. As a result, the system produces clean water for discharge while generating zero liquid waste. The effluent water can be used for industrial purposes or discharged to a receiving stream. A Water Impact Index (WIIx) study indicated that discharge of this high-quality water into the Monongahela River watershed may improve the water quality for downstream water users. The waste produced in the treatment process, including softening sludge and salt, is disposed of in an on-site landfill."

Jan 1, 2015

By Tim J. A. Smith

Fundicion Refimet S.A. has operated a custom copper smelter at La Negra, near Antofagasta in northern Chile since 1993. From an initial operation based on Reverb smelting and Peirce-Smith, converting, the plant was expanded from 90 000 t/y to 160 000 t/y copper production in early 1997, by conversion to oxy-fuel smelting and use of concentrate injection on Converters. As part of this expansion a novel reverb gas cooling and cleaning system was developed and designed by Kilborn SNC-Lavalin Europe, the London, UK-based mining and metals; Office of Canada's SNC-Lavalin group. The reverb gas cooler needed to satisfy several very specific requirements including low cost, flexibility, robustness and simplicity of operation. Of particular importance was the requirement to cool and clean the ,oxy-fuel reverb gases and render them suitable for subsequent treatment in a conventional sulphuric acid plant. It was also important to avoid accretion or dust handling problems. This paper describes the key design features and subsequent successful installation, commissioning and operation of the unit.

Jan 1, 1998

By B. VISWANATH

T HE Mysore iron works, at Bhadravati, about 2000 ft. above sea level in the Shimoga district of Mysore, British India, is served by a meter gage branch line of the Mysore State Railways. The works which were designed and erected by Perin & Marshall, who still act as consulting engineers, are surrounded by a thickly wooded country which sup- plies about 400 tons per day of wood for fuel. The ore deposits lie 20 miles to the south, and limestone quarries are close by the works. The Bhadra river sup- plies the works and the town with the necessary quantity of water. Dwelling houses for the employees

Jan 1, 1930

By Cristiana dos Santos Nunes

A soldagem de uniões dissimilares é muito comum em sistemas usados na exploração de petróleo e produção em águas profundas no mar. Comumente envolve soldagem de tubos de aço de baixo carbono com aços forjados baixa liga, muitas vezes, com revestimento interno de Inconel com o objetivo de reduzir o nível de tensões residuais seguidos de tratamentos térmicos de pós-soldagem. Uma técnica alternativa para reduzir as tensões residuais é utilizar um eletrodo que, durante o processo de resfriamento passa por uma transformação martensítica em uma temperatura relativamente baixa, de modo que a deformação resultante da transformação compense a contração durante o processo de resfriamento. Desta forma, o objetivo deste trabalho é avaliar o emprego do maraging como metal de solda em união dissimilar de materiais aplicadas na indústria do petróleo. Foram usados amostras de aços estruturais chanfradas em meio-v e soldadas utilizando varetas. Os níveis de tensões residuais e microestruturas da zona afetada pelo calor (ZAC) foram investigados. Uma verificação importante foi que a junta soldada apresentou tensões compressivas no metal de solda.

Aug 16, 2017

By Aline Silva Magalhães

Os aços rápidos são assim chamados por sua capacidade de reter elevadas durezas mesmo quando submetidos a altas temperaturas, em geral decorrentes de elevadas velocidades de corte no processo de usinagem. No entanto, para que esses aços apresentem as propriedades mencionadas, faz-se necessária a combinação adequada da composição química e dos parâmetros dos tratamentos térmicos. Dentro deste contexto, o objetivo do trabalho é avaliar os efeitos da temperatura de austenitização e do tempo de encharque na têmpera na microestrutura e na dureza do aço rápido AISI M2, ligado ao tungstênio e ao molibdênio. As análises foram conduzidas através de testes de dureza e microscopias óptica e eletrônica de varredura, além de difração por raios-x, considerando três temperaturas e três tempos de austenitização. Foi observado que, de maneira geral, os valores de dureza aumentaram com a elevação da temperatura de austenitização para os três diferentes tempos de encharque utilizados, de forma concomitante com a redução na quantidade de carbonetos dispersos na matriz martensítica.

Aug 8, 2018

"Mechanical alloying (MA) synthesizing technology and thennohydrogen processing (THP) were utilized to produce nanocrystalline Ti-MMC's reinforced by TiB intermetallic compound by using TiH2-B powder mixtures. Powders MA'ed up to 8 hours were examined by X-ray diffraction and SEM study. All MA'ed powders afterwards were HIP'ed at 700, 800 and 950EC for 1 hour. Detailed XRD, SEM and TEM study of the samples were carried out to determine the structure and micrography of the Ti-TiB MMC material processed by MA+THP approach followed by HIP'ing at high temperatures.IntroductionThe fiber reinforced titanium base composites [1,2] which possess a great resistance to high temperature have been investigated. In these studies fibers of C and SiC were used as reinforcing materials. However, these fibers react with Ti-matrix at elevated temperature resulting in product formation at the interface between the matrix and the fiber. Because of the chemical reactions, strength of the product MMC material diminishes.In conventional techniques of whisker reinforced composite material production, the mixtures of matrix metal powders and dispersed fibers are consolidated by hot pressing, HIP and/or hot extrusion. These techniques, however, have some shortcomings. Hard and brittle fibers could be broken during mixing cycle of the processing. Consolidation techniques could also be the cause for fiber breakdown. Attaining of the uniform dispersion of fibers into the metal matrix is not an easy process. The chemical reactions at elevated temperature exposures in the interface between the matrix material and fiber reinforcement cause product formations leading to poor mechanical properties."

Jan 1, 1998

By L. D. Tracy

For many yeirs natural gas has been the principal fuel used in the he·1 ting furnaces in those mills located in the. Pi t-c;s. b.urgh district· \7hich manufacture bolts ., nuts, rivets, pick$, mattocks and srr.&11 for6ine;s. For a nUI.1"'.::>er of years the steady supply of this fuel has been more or less interrupted owing to the increased4and f·or d9mes tic use and to the increasing difficulty in securing an ad.eq_ua te c.1mount of natural gas. This condition has led a number of the steel compa.nies to substitute -oulvsrized coal a.s a fuel for the.furnaces. Elaborate irista.llations have been made for pulverizing tne coal ar!d _ coriveyi16 i -c to the fur:waces. • Soon after the furnaces ·-:commenced .. to operate ·,Vi th :pulverized coal, large quanti ties O::f.' fine dust beg.::in to accumulate on the platforms over the fu:rna. ces, the. roof trusses, on the outside of the va.rious· pip·e ·line electric cables a.i.1.d even on the roofs of the buildings. Some of tha comi:,a.n:;.0s, becomin·g alarmed, requested the Bureau of ;Unes to rr.c1ke an investigation to ascertcliin the.· licibili ty of this dust to cause an explosion.· Nhi le conducting this inves ti ga ti on,· an explosion· occurr-2! d in a.nothe:2 nill ·,7hich caused he death of one man and severely burned t;io others. Eleven sc1nrcles of the dust (which for convenience has been termed "mill d.ust 11 ) from various locations in the different mill' buildings were taken and submitted to chemical analyses, microscopic examination and also to flame and explosion tests. From the chu,1ica.l analyses it was found that· the volatile matter in th..:: dusts xanged -from 6.3 per cent to 23,54 per cent, fixed carbon from 50.88 per cent to 67.08 per cent and ash from 32.29 per cent to 32.16 per centw

Dec 1, 1919

By Lu Lin, Yanping Bao, Xiang Li, Linzhu Wang, Xiaobai Yan

The results showed the microinclusions were mainly Al2O3 and sulfide inclusions from tapping to the beginning of LF refining. Al2O3 inclusions were modificated into calcium aluminates after calcium treatment. Lots of spherical calcium aluminates composite inclusions containing MgO, TiO2 and MnS were found after soft blowing and during tundish metallurgy and left in the slab which caused the defects of beam plates. Pure Al2O3 inclusions were observed again after soft blowing 8min. Average sulfur content in inclusions decreased because of the high desulfurization ability of refining slag. Average Ca/Al ratio value in inclusions increased during LF refinging because of the reduction of CaO in slag by carbon and it increased obviously during the process of soft blowing 8min because of the dissolusion of calcium wire.

Jan 1, 2015

By Maria Leikola, Joseph Hamuyuni, Petteri Halli, Fiseha Tesfaye, Mari Lundström

In a race to save the planet of its rapidly depleting natural resources, the use of Secondary Raw Materials (SRMs) as replacements in several processes is currently intensively pursued. In fact, this is currently one of the European Union (EU)’s mandates. Valorization of SRMs is consistent with circular economy, where resource efficiency is maximized for the benefit of both businesses and the environment. In line with this mandate, this paper focuses on investigating process phenomena related to hydrometallurgical recycling of Electric Arc Furnace (EAF) dust. In the experimental study, selective dissolution of zinc and other metals is investigated to acquire a recyclable leach residue. Based on the experimental and theoretical investigations, zinc could be extracted from the EAF dust and a recyclable leach residue produced, having chemical composition suitable as a feed material into electric arc furnace.

Mar 1, 2018

By D. W. Lillie

It has been demonstrated that considerable bend ductility exists in bulk specimens of polycrystalline high-purity silicon. The possibility of hot-forming at 1200°C is suggested. EXCELLENT corrosion resistance in many media and low cross section for absorption of thermal neutrons (0.13 barn) would make silicon of interest to nuclear engineers were it not for extreme brittle-ness and the difficulty of fabrication by any reasonable means. The use of silicon for structural purposes also has been considered in view of its light weight and oxidation resistance. Johnson and Han-sen' have investigated the properties of silicon-base alloys and concluded that there was no way of making pure silicon or silicon-rich alloys ductile at room temperature. In view of reports of appreciable ductility in germanium single crystals above 550°C'." and some plastic deformation in single-crystal silicon above 900oC,' the present investigation was undertaken to define more precisely the limits of high-temperature ductility in pure silicon. After this investigation was begun torsion ductility in both germanium and silicon was reported by Greiner." Through the courtesy of F. H. Horn, a small bar of cast extra high-purity silicon was obtained and small bend specimens were made from it by careful machining and grinding. All of the reported tests results were obtained from samples from this bar (bar No. 1) and one other of similar source (bar No. 2). No complete analysis was obtained but, based on analysis of similar semi-conductor grade material, metallic impurities were under 0.01 pct total. Vacuum-fusion analysis for oxygen showed a value of 0.0018 2 0.0003 pct for the first bar tested and metallographic analysis showed no evidence of a second phase. Bend tests were carried out on an Instron tensile machine using a bend fixture with a 1 -in. span loaded at the center. Supporting and loading bars were 0.250 in. round and the load was applied by downward motion of the pulling crosshead of the machine. Specimen thickness and width were approximately 0.10 in. and % in. respectively. Loading rate was controlled by holding crosshead motion constant at 0.02 ipm. In some cases a smaller specimen was used on a 5/8-in. span with a 0.129-in.-diam loading bar. The entire bend fixture was surrounded by a hinged furnace and all heating was done in air atmosphere. Temperature measurement was made with thermocouples fastened directly to the bend fixture within less than 1 in. from the specimen. Autographic stress-strain curves were recorded during each test, and breaking load, total deflection, and plastic strain could be obtained from these curves. Stress was calculated from the beam formula S = 3PL/2bh2, where P is the load in pounds, L the span in inches, b the specimen width in inches, and h the specimen thickness in inches. This formula is strictly correct only in the elastic range but has been used to calculate a nominal stress for convenience in the plastic range. The stress given is the maximum stress in the specimen. Results The results of the complete series of tests are shown in Table I. The first group of tests (specimens Nos. 1-6) showed the beginning of plastic flow at a test temperature of 900°C, so two additional tests (Nos. 8 and 9) were made at 950°C on small-size specimens from bar No. 2. Specimen No. 8 was tested in the as-machined condition, and No. 9 was heat-treated in hydrogen at 1300°C for 2 hr, cooled to 1200°C and held 1 hr, cooled to 1000°C and held 1 hr, cooled to 900°C and held 1 hr, and finally cooled to a low temperature before removal from the hydrogen. It is apparent that the heat-treatment had a significant effect on yield strength and ductility. In addition, the magnitude of the yield point was conslderably reduced in the heat-treated specimen as is shown m Fig. 1 by tracings of the stress-strain curves. After obtaining a furnace capable of reaching higher temperatures specimens Nos. 10 to 13 were tested at 1100 and 1200°C. Strain rate was increased by up to a factor of 10 to see whether the ductility observed was excessively strain sensitive. Specimen NO. 10, strained at 0.02 ipm and 1100oC, was still bending at a deflection of 0.322 in. when the load rate was increased to 0.2 ipm, resulting in immediate

Jan 1, 1959

By F. R. Cattoir

This Bureau of Mines study investigated molten salt electrorefining for beneficiating low-grade, high-carbon ferrochromium products which can be readily produced from domestic chromite concentrates. A second objective was to refine commercial ferrochromium into low-iron chromium products. Electrorefining of both types of ferrochromium in molten CaC12-NaCl-CrC12, CaCl2-MgC12-CrCl2, or KC1-LiCl-CrCl2 electrolytes produced chromium-iron products with virtual elimination of other impurity elements and some lowering of the iron content, Over 90 percent of the chromium present in the feed materials was recovered. The electrodeposited products were upgraded further by magnetic separation techniques into chromium containing less than 5 percent iron. The technical feasibility of preparing a premium chromium product from a low-grade, high-carbon ferrochromium made from domestic chromite was demonstrated. Chromium virtually free of carbon, oxygen, and silicon from high-carbon ferrochromiums was produced. In addition, the amenability of three commercial grades of ferrochromium to electrorefining and magnetic separation for preparing chromium metal containing less than 5 percent iron was determined.

Jan 1, 1969

By G. L. Oldright

The past reputation of zinc as an ingredient in lead blast furnace slags has been bad. Zinc is thought of as a cause of accretions in the shaft of the blast furnace, of hot tops, of the formation of "zinc mush" in the crucible and forehearth, of leach rich slags, of viscous slags, and of low capacity in smelting.

Jan 1, 1934

If it had not been for the almost unbelievable adventures that came before and after, the last ten months of 19 15 would have been exciting enough for anyone. As it was they were a cheerful interlude. I spent most of the time on our Warren operations catching up on a lot of underground work and visiting Ajo every few weeks to see if my Chuquicamata visit might help solve the New Cornelia problem. While the difficulties were finally solved, at times they seemed almost hopeless. About all I could do to help was to make sure that the ore sent to the pilot plants represented the average ore that must be treated in the final 5000 tpd mill. Dr. Ricketts and John Greenway worked tirelessly with the best consulting advice they could obtain. Credit for the final success was due chiefly to their efforts. Since our old group had given up its "Merry Widow" home in Warren, a few of us got rooms in the company-built Cole Building over the Warren grocery store. This included Jim Lewis, Roy Mitchell, Steve Landon, Paul Stevens, and Hubert d'Autremont who came from Duluth to join our legal staff. Later we rented a small house two blocks from the Calumet and Arizona office. With the now flourishing country club only a 10-min walk away, and an electric car running to it every half hour or so, we were able to give parties in return for the hospitality of our friends. One of the most pleasant episodes came by luck a few days after I got back from Chile. Chester Congdon, a leading director in Calumet and Arizona, with his wife and their daughters, Elizabeth and Helen, spent a couple of days at the Greenway house before making an auto- mobile trip across the desert from Tucson to Ajo. At the same time I arranged to examine the small but rich Bush and Baxter copper mine a few miles from Tucson. At a party in Warren we found we would all be staying at the Santa Rita Hotel in Tucson, and I took my South

Jan 1, 1976

By Larry M. Southwick, Phillip J. Mackey, A. E. (Bert) Wraith, Albert Pelletier

In 1881, the first commercial pneumatic Bessemer-type converter treating copper matte was successfully introduced by Pierre Manhes at the Eguilles copper plant near Vedène in France. This development followed over a year of testing on a smaller scale at a foundry in Vedène, during which the vertical tuyeres of the conventional Bessemer converter had been successfully replaced by horizontal tuyeres in an effort to avoid the freezing of copper which had occurred in the bottom of the vessel having vertical tuyeres. The Manhes Converter, as it became known, was the first successful large-scale adaptation of the Bessemer concept of using compressed air blown into a melt for metal refining and treatment. Within a few years, Manhes Converters utilizing horizontal tuyeres in either the original type of vertical converter, or a later and more enduring horizontal barrel converter, were in operation at over a dozen copper smelters around the world. It was this process that Messrs Peirce and Smith essentially improved with the introduction of the larger converter which bears their name and the development celebrated at this Symposium. The present paper briefly traces the original development by Pierre Manhes in the early 1880s and which set the stage for the later Peirce-Smith adaptation. The paper observes that the original development by Manhes was in part driven by the need to reduce coal (energy) consumption and hence the production cost in order for Eguilles to remain competitive with the larger plants in Swansea, Wales, where a ready supply of cheap coal helped keep smelter treatment terms of the day low. These themes are eerily resonant of today where booming copper production in China has impacted the industry, and also where energy consumption, closely linked to today’s more familiar theme of ‘climate change’ remains an important challenge currently confronting the entire industry. The paper concludes with comments on these seemingly parallel situations today and offers some thoughts for the future.

Jan 1, 2009

By J. A. Eisele

The Bureau of Mines conducted bench-scale cyclic tests to determine the composition of recycled leach liquor in the Bureau?s proposed clay/HCl leach/ HCl sparge process for producing Al203 from clay. The data developed from these tests make it possible to synthesize leach liquors for predetermined steady-state operating conditions when conducting large-scale crystallization tests. The results of two sparge tests were compared. One was a 20-cycle test with a 36-pct-HCl concentration in the mother liquor; the other was a 10-cycle test with a 26-pct-HCl concentration in the mother liquor. The effect of impurity concentrations in the leach liquor on the purity of aluminum chloride (AlCl30?6H20) crystals was determined, but there was poor correlation between this data and results that have been obtained from miniplant-scale work.

Jan 1, 1980

By Frank L. Hess

In the first cart of that little space of time that we have designated as the nineteenth century, chemistry had reached a wonderful stride. Viewed from the present heights attained by the efforts of innumerable chemists with perfected apparatus, mire reagents, air under pressure, water, gas, and electricity conducted to the desk, and. numberless other helps, it seems marvelous that chemists of that day obtained such results. In 1820, about half of the elements had. been discovered; of these discoveries, Swedes had made 15 or more, about once-third of the elements then known and nearly half of those discovered after 1700.

Jan 1, 1939

By S. M. Purdy

Under certain conditions of hot rolling and air cooling from the hot-rolling temperature, bars of a high carbon (0.40 pct C) chrome-nickel austen-itic alloy were found to show magnetism even though no ferrite or martensite could be detected by microscopic or X-yay methods. The appearance of magnetism in such alloys may come from chromium impoverishment of the austenite grains near the precipitated carbide particles. SPORADICALLY, hot-rolled bars of Silchrome 10, an exhaust valve steel, have been found to be magnetic. Because of the analysis of the alloy—0.40 pct C, 18 pct Cr, 8 pct Ni, 3 pct Si —magnetism is unexpected. Preliminary investigation showed neither martensite nor ferrite to be present; only austenite and Cr23C6. Since a literature search was fruitless, a brief study was made of the appearance of magnetism in this alloy. The only basic difference between the two heats is the nitrogen content. Permeability was measured using a Severn magnetic gauge. This instrument consists of a magnet mounted on a counterbalanced arm. A set of calibrated plugs is placed in contact with one pole of the magnet. The specimen is placed close to the other pole of the magnet. If the specimen pulls the magnet away from the plug, it has a permeability greater than that marked on the plug. This technique is swift and reproducible. Previous experience has shown that the permeabilities obtained corresponded to those obtained on a permeater with a field strength of 100 oe. Specimens from both heats were annealed at temperatures between 1700 and 2300°F. One set of specimens was water cooled and another furnace cooled. All the water-quenched specimens were non-magnetic; the furnace cooled ones were magnetic as shown in Table I with no difference being observed between the two heats. Microstructural examination of the specimens showed the expected increase in carbon solubility with increasing temperature. Carbide solution was complete at 2200°F. The specimens heated to 1900°F or below showed some carbide precipitation from the hot-rolled structure. A furnace cooled specimen from a given temperature showed less carbide out of solution than the water-quenched specimen from the next temperature below; e.g., the specimen furnace cooled from 2100°F showed less carbide out of solution than the water-quenched specimen from 2000" F. These studies indicated that the appearance of magnetism was not related to the quantity of carbon in or out of solution and it was related to precipitation at temperatures below 1700" F. A set of samples annealed and water-quenched from 2100° F was aged for 4 hr at temperatures between 1000" and 1600°F; all were non-magnetic. A second set of samples, similarly annealed, was aged 1 to 24 hr at 1200°F with the results shown in Table II. None of the latter set of specimens showed magnetism until they had been aged about 8 hr. Magnetism was quite strong after aging 24 hr. X-ray diffraction studies on several of the magnetic specimens showed that the austenite had a lattice parameter of 3.58A and that the carbide was Cr23C6. Several of these samples were electrolytically digested in 10 pct HCl in ethanol, with a current density of 0.1 amp per sq cm. None of the particles in the residue were magnetic. Accidentally, one cell was run at 1 amp per sq cm; e.g., magnetic particles were found in this residue. After careful separation, the magnetic particles were mounted on a quartz fiber and their diffraction pattern determined using a 5.73-in. Debye-Sherrer camera with CrK radiation. These particles showed a fcc structure with a lattice parameter of 3.57A. Prolonged exposure, up to 16 hr, produced no other lines on the film. The following facts seemed to be established at this time: 1) Austenite was the magnetic phase. 2) Neither ferrite nor martensite could be detected. 3) Magnetization could be produced by aging at 1200°F. One explanation of these data is that the carbide precipitation impoverishes the region immediately around the carbide particle of carbon and chromium and increases the proportion of nickel. All of these serve to increase the Curie temperature of the region around the carbide particle. If the composition change is enough, the Curie temperature will rise above room temperature. If the volume of the affected region is great enough, the magnetism will become detectable. At low aging temperatures, composition changes are great enough but the overall volume of impoverishment is quite small

Jan 1, 1962

By C. W. Beattie, R. L. Solter

ALUMINUM-KILLED, low carbon steel sheets are used extensively for severe deep drawing and other difficult forming operations. They usually, but not always, have a characteristic grain structure in which the grains are elongated both in the lengthwise and in the transverse direction. As described by Burns and McCabe,&apos; a typical grain in the plane of the sheet has its two axes in that plane from 1 Y2 to 4 times as long as the axis normal to the plane of the sheet. Rickett, Kalin, and MacKenzieZ have also reported on the recrystallization behavior of such steel. The contrast in grain structures of fully processed sheets of aluminum-killed and rimmed steel is illustrated by Figs. 1 and 2. The elongated grain structure of the aluminum-killed sheet is not developed on all heats or lots of this metal, and studies of the factors controlling and influencing its formation are reported in this paper. Jeffries and Archerb tate that unstrained grains are normally equiaxed, but exceptions are common. For example, if a metal containing a material mechanically obstructing grain growth is subjected to considerable working followed by thorough annealing, it may exhibit grains consistently elongated in the direction of working. Our experiments demonstrate that aluminum-killed, low carbon steel is such a metal, and that the substance mechanically obstructing grain growth is aluminum nitride. The effectiveness of aluminum nitride in inhibiting grain growth has been found to be influenced by the degree of cold reduction, the rate of heating in annealing, the thermal history of the sample before cold reduction, and the residual aluminum content. A correlation between grain shape and austenitic grain coarsening temperature also was indicated and additional experiments demonstrated that aluminum nitride is also the principal cause for the fine grain characteristic of aluminum-killed steels. Manufacture In conventional practice, aluminum-killed sheet steel is manufactured from a low carbon steel containing approximately 0.02 to 0.07 pct residual (HC1 soluble) Al. With the exception of certain samples containing greater or lesser amounts of aluminum, the steels used in these investigations were within the following composition range: C, 0.03 to 0.06 pct; Mn, 0.28 to 0.38; S, 0.017 to 0.032; Al, 0.03 to 0.06; P, <0.01; and Si, <0.01. Properly heated ingots are rolled to slabs about 4 in. thick. After surface conditioning, the slabs are reheated to about 2300°F and hot rolled continuouslv to strip about 1/10 in. thick. The strip rolling is completed at a temperature of 1550°F or higher, and the strip is coiled, usually at a temperature near the lower critical transformation. After cooling, the strip is pickled to remove oxide, cold reduced 40 to 70 pet to final thickness, then annealed to 1250° to 1350°F in 20 to 80 ton charges, the size of which results in slow heating and cooling rates. Effect of Cold Reduction According to Sachs and Van Horn,&apos; the deformations of the individual grains in rolling are similar to those of the total volume. Thus individual grains would elongate in rolling according to the amount of cold reduction imposed. This is true theoretically, but as cold reduction increases the individual grains tend to fragment, and measured grain elongations become less than theoretical. The amount of grain elongation may be described by a numerical rating based on grain counts made by the intercept method. Specimens are polished normal to the plane of the sheet, with the polished surface extending parallel to the rolling direction. After etching, grain intercepts are counted along a 50 mm line on a micrograph of suitable magnification. In random locations parallel to the plane of the sample 20 counts are made and 20 are made in the thickness direction of the sample the average count in the thickness direction divided by the average count parallel to the plane of the sample gives a numerical rating of the grain shape called grain elongation. For example, a grain elongation of 2.00 means that the average grain is twice as long as it is thick. The average of both counts may be converted to grains per sq mm by a nomograph relating intercept counts and grain count. By the same procedure the grain elongation in the plane of the sheet but transverse to the rolling direction may be determined, using transverse metallographic samples. A comparison of theoretical and measured grain elongation was obtained on an aluminum-killed

Jan 1, 1952