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By Dapeng Zhang, Brij Moudgil, Shibo Zheng, Chunhui Feng, Wenyi Song, Wending Xiao, Patrick Zhang

Separation of dolomite from phosphate is the most challenging problem in phosphate mineral processing. Over 50% of the future phosphate reserve in Florida contains too much dolomite to process using the current industry practice. The current phosphoric acid production practice requires less than 1% MgO in the phosphate concentrate as the feed material. The Florida Industrial and Phosphate (FIPR) Institute has collaborated with worldwide experts in the field to address this issue. As a result, the industry is now offered three feasible options. Option 1 offers three methods for reducing MgO content in the concentrate from the Crago process, including adding a dolomite depressant in the rougher flotation step, dolomite flotation of the cleaner concentrate, and scrubbing the cleaner concentrate in quartz sand. These methods could reduce MgO content in the final concentrate by 20–40%. Option 2 involves crushing and grinding of high-dolomite phosphate pebbles followed by dolomite flotation at slightly acidic pH using a new collector that does not require phosphoric acid as a phosphate depressant, achieving a final concentrate analyzing less than 0.9% MgO at about 87% P2O5 recovery. Option 3 is a gravity separation technique using an innovative separation jig, and its full potential remains to be demonstrated.

By Derrick Dasenbrock, Mary C. Nodine, Benjamin Rivers

Up to 50 percent of major infrastructure projects suffer impacts to schedule or cost due to geotechnical issues, many of which correspond to risks related directly or indirectly to the scope and quality of site characterization work. The Federal Highway Administration (FHWA) in coordination with industry organizations seeks to address this issue through Every Day Counts (EDC), a program that identifies and deploys proven, yet underutilized innovations at the project level to save time, money and resources. The A-GaME (Advanced Geotechnical Methods in Exploration) is one of the innovations supported under EDC.

By Carmel Bofinger, Maureen E. Hassall, David Cliff, Eric Stemn

Incident investigation is of utmost importance in most high-risk industries and is often used to improve organisational safety. This study was undertaken to examine the content of past incident investigation reports to determine the effectiveness of the incident investigations. The study uses a semi-quantitative method to assess the effectiveness of incident investigations in the Ghanaian mining industry by evaluating the quality of past investigation reports. The assessment tool consists of five elements with several indicators and rating scales for assessing the quality of an investigation report as a measure of the effectiveness of the investigation. The method was applied to 304 investigation reports of three Ghanaian large-scale gold mines, and the results correlated with incidence rates of the mines to determine if any relationship existed. The results showed that the mines differ significantly in the quality of their investigation reports, suggesting differences in the effectiveness of their investigations. In addition, the incidence rates of the mines negatively correlated with some elements of the assessment tool. In general, the method was found useful and revealed areas where improvement is needed.

By Mokhinabonu Mardonova, Yosoon Choi

Open-source technology for supporting the Industry 4.0 has become the target of academic research in many sectors. This study reviewed the trends of open-source technology, its forms, and some industrial applications. As a case study using open-source hardware and software for the mining industry, this study proposed a low-cost environmental monitoring system for non-metallic underground mines to support mine safety and occupational health issues. The system was developed using open-source hardware, Arduino and 3D printer, to design the monitoring device. An open-source software, MIT App Inventor, was used for developing an Android application for smartphones to enable remote communication with the system. Field experiments were conducted at an underground tunnel and a non-metallic underground mining site to assess the performance of the system in both mobile and static modes, respectively. Although a few limitations related to the precision of the low-cost dust and gas sensors still exist, the findings of the experiments show that the mining industry can benefit from open-source technology deployment when considering cost factors

By Rambabu Pothina, Rajive Ganguli

The economics of a mineral processing circuit is dependent on the numerous sensors that are critical to optimization and control systems. The sheer volume of sensors results in mines not being able to keep the sensors calibrated. When a sensor goes off calibration, it results in errors which can severely impact plant economics. Normally, these errors are not detected until the error grows and becomes a large (“gross”) error. Undetected errors are not remedied until the next calibration, which on average are a year apart Beamex (2019) [1] across all industries. Classical statistical methods that depend on linear relationships between input and response variables are typically used to find gross errors, but are not effective for highly non-linear and non-stationary operations in mining and mineral processing industries. Calibration of sensors is time-consuming and generally requires physical intervention that results in equipment downtimes causing production losses. Therefore, in situ detection methods are warranted that do not require physical removal of sensors to compare with standard measurements or well-calibrated sensors. Data-mining based techniques and algorithms have high success rate in tackling such problems. This paper presents results from a groundbreaking multi-year big data research project whose goal was to develop data-mining-based original techniques in a multi-sensor environment to identify when sensors start to stray, rather than wait for errors to grow. The carbon stripping (gold) circuit in the Pogo Mine of Alaska was selected for this project. Maintaining strip vessel temperatures at optimum levels is crucial for maximizing gold recoveries at Pogo, and hence the focus was on the temperature sensors of the two strip vessels. An automated algorithm to detect errors in strip vessel temperature sensors was developed that exploited data from multiple sensors in the strip circuit. This algorithm was able to detect with a high success rate when bias errors of magnitude as low as ± 2% were artificially induced into strip vessel temperature data streams. The detection times of about 1 month were much less than the industry average calibration frequency of 1 year. Thus, the algorithm helps detect errors early, without stopping the circuit. The algorithm alarms can serve as triggers when calibrations are done. Experimental methodology along with results, limitations of algorithms, and future research are also presented in this paper.

By C. D. Ashley, X. P. Garzon-Villalba, R. M. Lopez, T. E. Bernard

Federal standards for refuge alternatives (RAs) mandate that they not exceed a Steadman apparent temperature (AT) of 95 °F (35 °C) at an assumed metabolic rate of 325 W, a limit that appears to be arbitrary. Occupants in an RA spend most of their time at rest (a metabolic rate less than 325 W), and thermal equilibrium can likely be maintained at an AT > 35 °C. The purpose of this study was to examine the upper limit of sustainable heat stress during 4- and 8-h exposures at rest. Five men underwent five 4-h trials (phase 1: AT range 39 to 49 °C, 90% rh) and five 8-h trials (phase 2: AT range 46 to 56 °C, 90% rh) in a semi-recumbent position. Descriptive statistics for gastrointestinal temperature (Tgi), heart rate (HR), systolic and diastolic blood pressure (SBP and DBP), sweat rate, fluid intake, urine color, urine specific gravity (USG), and changes in body mass are reported. Mean Tgi for all trials ranged from 36.9 to 37.3 °C, and mean HR for all trials ranged from 61 to 75 bpm. To determine the effects of increased heat exposure, differences in heat strain between 4- and 8-h trials were examined via repeated measures analysis of variance (ANOVA). As AT increased, there were no significant changes in ΔTgi and ΔHR from 1 to 4 h in the 4-h and 8-h trials. During the 8-h trials, as AT increased, there was a difference in ΔTgi between 4 and 8 h. In conclusion, there was support for sustainable exposures resulting in no significant increase in physiological strain at an AT greater than 35 °C AT, with a sustainable limit (no increases in Tgi due to increases in AT) below 46 °C AT. Although the participants were not representative of coal miners, the results provide support for sustainable exposures greater than 35 °C AT at an average metabolic rate of 155 W.

By Kritika Baxla, M. Mustafa Kahraman, Frank A. Drews, Yaxue Wang, Joel M. Haight, Kody Powell, Mohit Sobalkar, W. Pratt Rogers

In the opinion of these authors, technology alone can never give an organization an edge over competitors or provide an industry step change. However, history has shown that technology applied with correct logistics and strategy makes a significant difference. Never has the minerals industry faced such daunting challenges and been in such need of a step change. Application of autonomous systems has been steadily increasing in the minerals industry. Automation technology has changed the mining value chain from exploration to mineral processing and refining. The future state will only see additional in-roads of automation into more processes and the whole system design. To better understand the near-future potential of automation, it is useful to explore and review the current state of automation in minerals development. A review of the state of automation research is given. The review will consider three critical areas: automation technology, system’s engineering and management processes around automation, and the role of human factors engineering in automated and semi-automated systems. The review ends with a discussion on the social and political risks of automation in terms of shared value and sustainable development.

By Andrew B. Cecala, Emily J. Haas, Jay F. Colinet

A sociotechnical system (STS) creates a framework that allows an examination of how social and technical factors affect organizational outcomes within a specific environmental context. STS has been rigorously studied with a primary research focus addressing worker-technology interactions. Although these interactions are important, the social processes and interactions that occur whenever any technical or environmental change is introduced into the system have been undervalued. If social processes are better understood, mining organizations could efficiently prepare and stabilize for such changes. With this goal in mind, we sought to extend STS theory through applying principles of meta-design to analyze the results of two case study interventions. Specifically, we studied the impact of an unregulated dust control technology (the Helmet-CAM) and a regulated dust control technology (the Continuous Personal Dust Monitor) on factors within an STS including employees’ knowledge of, communication about, and use of technology to mitigate respirable dust sources. The results are presented in a way that first, addresses the overarching principles of meta-design STS including organizational participation, flexibility, and communication and second, examines how technology implementation processes differ when the organization is complying with a formal, higher-level requirement. Results show that a prominent focus on the social factors within an STS framework could help reduce unpredictability on the technical side and may improve communication within the system to help reduce adoption time, especially if and when accompanying a new, formal work process.

By Tyler Acorn, Brandon Wilson, Jeff Boisvert

Scenario-level uncertainty is a representation of large-scale differences encountered when considering ultimate mining pits optimized over various subsets of stochastic realizations. Accounting for scenario-level uncertainty allows mine plans to be assessed against several probabilistic subsurface interpretations. Scenario-level uncertainty is found through clustering stochastic geostatistical realizations and optimizing final pits across the realizations in each cluster. Where these pits are geometrically different, plans for each scenario differ. Knowing these differences allows the value of each planning alternative to be assessed based on the value and relative probability of each scenario. These results also facilitate the use of formal decision-making frameworks for planning, leading to optimization that better represents the full statistical characterization of the deposit. An example utilizing this approach evaluates both infrastructure placement and drilling program requirements. In both cases, scenario-level uncertainty improves initial plans by limiting opportunity costs and identifying additional potential.

By Chen-Luh Lin, Jan D. Miller, Sindhoora Puvvada

The depletion of good-quality phosphate resources, coupled by a need to supply acceptable products at a rapid rate, while meeting the specifications of fertilizer chemical plants, is of significant concern to the phosphate industry, particularly the production of concentrates with tolerable dolomite content. Tremendous efforts have been made in the past to develop an efficient and economical process that can effectively reject dolomite. However, dolomite removal continues to plague the phosphate industry due to several process-specific challenges being encountered with various beneficiation technologies. In this regard, detailed characterization of phosphate reserves is crucial to understand textural limitations and help design appropriate strategies to achieve quality products. In this paper, the development of procedures to establish dolomite rejection/francolite recovery curves for gravity preconcentration of pebble phosphate from Central Florida is described using high-speed X-ray computed tomography (HSXCT). The developed procedure is illustrated with the analysis of high MgO pebble phosphate samples (10.39 mm × 1 mm) received from South Pasture and Four Corners locations operated by the Mosaic company. The rejection/recovery curves were calculated for each sample for five different particle size classes to observe the trend in rejection/recovery with variation in particle size. In order to evaluate the reliability of the HSXCT data, analysis using the high-resolution X-ray computed tomography (HRXCT) technique was performed on one particular sample (FC-3-1). Finally, to assess the separation efficiency, the HSXCT and HRXCT rejection/recovery curves obtained were compared to experimental gravity preconcentration results reported in the literature. In this way, liberation limitations for gravity preconcentration in the processing of pebble phosphate have been established based on X-ray computed tomography analysis.

By Andre Vien, Frank Laroche, David Di Sandro

Back in 1994, Claude Bazin presented a novel method for linking size data from milling models to the feed input of flotation models. It was achieved with the simple addition of a metal/mineral distribution—size distribution relationship. This allows grade and recovery predictions from a varying mine plan via product size distribution predictions. This paper presents a case study where this elegant method has been used to build a very powerful forecaster at a process plant, built from historic operating data. The methodology has been used by this operation to forecast production on a quarterly, annual, and life-of-mine basis since the late 1990s. It has been upgraded several times to incorporate new drivers as the complexity of feedstocks has increased over the years.

By S. K. Sahoo, S. K. Sharma, A. Yadav, B. Behera, G. S. P. Singh

A field representative modeling of the gob behavior is critical for the understanding of the associated mechanics of strata behavior in longwall workings. The findings of theoretical models and laboratory tests on the simulated gob material have shown the strain hardening behavior of the gob material. The double-yield material model, which is a built-in constitutive model in FLAC3D, has significant potential to simulate the gob compaction process as it represents materials which undergo irreversible compaction in addition to shear yielding. Apart from this, several researchers have attempted using modified elastic model or applied nodal force in reaction to the strain in the gob area as per the well-known theoretical relations to meet this requirement. Although these models can simulate the mechanical response of the gob for subcritical and critical extraction widths, they do not apply to supercritical extraction width as the gob stress may exceed the in situ stress level in such cases. For overcoming these limitations, a standard approach has been developed and validated in this paper, which can be used for simulating the gob behavior in supercritical longwall workings as well. The complete study is divided into two stages wherein the laboratory scale compression test on the simulated gob material has been numerically replicated to develop preliminary confidence followed by a parametric study of the double-yield constitutive parameters for a rational estimation of their values in different conditions. The calibrated model has been used for verifying its results by plane strain modeling of two different longwall workings, using well-established empirical and analytical findings and field observations. The approach suggested in this study can be used for the efficient modeling of the gob behavior of longwall panels under varying geo-mining conditions without compromising the accuracy of the numerical model. The meticulously validated model can be helpful in rational estimation of stress redistributions around the gob area apart from load transfer on the barrier pillar.

By Edward C. John, Wilbur H. Smith

At the Bingham Canyon pit operated by Kennecott's Utah Copper Division, the demand for geology has recently grown and diversified so rapidly that it has necessitated a revolution in geologic mapping techniques. The most significant changes in method have been in the preparation of the base map and in the computer application of collected data. Formerly maps were prepared by surveying with a transit or plane table. Now, however, a photogrammetric map with a scale of l in. to 200 ft is prepared semiannually and updated continuously to keep pace with the removal of more than 350,000 tons of material a day. Larger-scale bases of areas with specific problems such as un- stable slopes are prepared with aerial and terrestrial photography and photo-mosaics. Note sheets designed for computer application speed the processing of data. The multiplying applications of geology at the Bingham mine now include studies of the effect of structure, rock type, and alteration on slope stability, the relationship of sulfide mineral distribution to concentrating results, the effect of rock and mineral types on waste dump leaching, and the requirements of a reliable internal source of silica flux for smelting, as well as many others.

Jan 9, 1969

By K. Tajrych

Time and again, lives are lost in underground cave-ins only be- cause there is no quick, sure way of locating the victims. When such accidents happen, rescuers must usually depend on the testimony of eye- witnesses for information on the whereabouts of trapped miners. Seldom is this information reliable. The witnesses themselves have just been through a traumatic experience that has distorted or destroyed their sense of time and place. A far more reliable method of finding men underground has recently been developed by the Coal Mining Research Institute of Ostrava, Czechoslovakia. With this system, a miner can be located with adequate precision even if he shows no sign of life. For the system to work, the miner need only have his electric cap lamp somewhere nearby. The system consists of a minute radio transmitter operated by the lamp battery (Fig. 1). This tiny transmitter continuously emits high- frequency electromagnetic waves that can be picked up by a sensitive direction-finder receiver in case of accident.

Jan 8, 1969

By F. F. Aplan

Mineral processing engineers have recorded an- other year of active research and development work. Most gratifying was the broadly based attendance at the Mineral Processing Fundamental (formerly Basic Science) Committee sessions at the 1968 Annual Meeting of the AIME. Because of the availability of good papers, the active discussion and the growing attendance, sessions have grown from one to three at the annual meeting. Prof. M. C. Fuerstenau of the University of Utah will chair the Mineral Processing Fundamentals Committee for the next two years and we may thus be assured of continued active leadership. The name change from "Basic Science Committee" to the more descriptive "Mineral Processing Fundamentals Committee" approved by the MBD executive council is a welcome improvement. Our profession continues to attract the interest and cooperation of those in other professional groups. The 1968 Engineering Foundation Particulate Matter Conference, under the chairmanship of John Karpinski of Bethlehem Steel, was devoted exclusively to comminution this year. It attracted conferees from five continents and served as a particularly stimulating source of interchange of knowledge from many technical fields. Next year's conference will be under the chairmanship of Professor L,. G. Austin of The Pennsylvania State University. This conference plus the Symposium on Wettability and Flotation to be held at the annual American Chemical Society meeting in Minneapolis in April indicates the success achieved in the inter-disciplinary approach to problems. Other evidence of this spirit of professional cooperation is the forth- coming book on Size Reduction edited by D. W. Fuerstenau. This is the outgrowth of an AIChE symposium on size reduction held in 1965.

Jan 2, 1969

By O. T. Berge

Development and production from open cut mines continued its vigorous growth trend during the year 1968. Material handling and transportation were again exposed to the use of larger equipment with shovels, trucks and front end loaders leading the way. Highlights of World Mining Activities Africa: The Anglo American Corp. opened a new high-grade copper mine in Zambia during the year. In Angola, the Companhia Minera do Lobita planned a 3 million ton iron ore production for 1968 from new mines which will ultimately produce 5 million tons per year. A feasibility study of Bethlehem Steel Co., for the development of large high- grade iron ore reserves in Gabon, was in final stages of completion this year and Pickands Mather and Co. continued its investigation of iron ore deposits along the Ivory Coast.

Jan 2, 1969

By C. E. Violet, R. J. Borg, E. M. Howard

The miscibility gap in the Au-Ni system has been determined by Mossbauer spectroscopy, with used as a probe. The phase boundaries were determined from the compositional dependence of both the isomer shift and Curie temperature. X-ray diffraction measurements were also used to confirm the Mossbauer results. 1 HE purpose of this research is to demonstrate the application of Mbssbauer spectroscopy to the determination of phase boundaries and to redetermine the miscibility gap by an independent and novel technique. The techniques evolved in this study are readily applicable to other polyphase systems and are generally as quick and accurate as the more conventional methods, e.g., metallography, X-ray diffraction, thermal analysis, and so forth. To be sure, not all polyphase systems will lend themselves favorably to Mijssbauer investigations, but this is a problem met in the use of conventional methods as well. The Mbssbauer spectrum responds to a different set of physical parameters, and consequently provides an entirely independent method of analysis. It is especially useful if the system has either a ferromagnetic or an antiferromagnetic transition. The Au-Ni system was selected because alloys containing more than -60 at. pct Ni become magnetically ordered at low temperatures; also the miscibility gap is quite well established (see Ref. 7 for a compilation of pertinent references, also Fig. 11, and thus provides a reliable test of this novel procedure. As Fe is the most commonly used Mijssbauer isotope, there exists a wealth of information concerning its behavior in iron-containing alloys and compounds. However, as yet there have been relatively few experiments using it as a probe to investigate nonferrous systems. By choosing a nonferrous alloy system, we are able to demonstrate that its use is not restricted to systems containing iron as one of the major constituents. Wertheim and ~ernick' have used the same method to investigate Cu-Ni, and demonstrated that one can obtain a systematic variation in the isomer shift and magnetic hyperfine field. However, we believe this to be the first time these techniques have been used to establish phase boundaries. Two hyperfine interactions were measured and used to determine the phase boundaries, viz., the magnetic hyperfine splitting and the isomer shift which in this alloy system are both strong functions of composition. Calibration curves were established based upon single-phase solid solutions obtained by quenching from temperatures well above the maximum of the miscibility gap, see Fig. 1. Solid solutions containing 25, 50, 65, 75, 85, 92, and 96 pct Ni as well as pure nickel were used in the calibration procedure. Fig. 2 shows the Curie temperature, TC, and the isomer shift, v,, as determined from the Mbssbauer spectra, and variation in lattice parameter as determined by X-ray diffraction, as functions of composition. The compositions of the two-phase systems quenched from temperatures within the miscibility gap are obtained by comparing their respective values of TC and v0 with the calibration data. I) EXPERIMENTAL Mbssbauer sources were made by fusing the component metals in a tungsten arc melter, which has a water-cooled copper hearth. Both nickel and gold were 99.999 pct pure, and the melting was done in an atmosphere of purified argon. The alloys were rolled, diced,

Jan 1, 1969

By A. P. Page, G. E. Alexander, L. L. Sirois, A. A. Winer

A knowledge of the electrical surface characteristics of minerals is all-important in the choice of treatments to up-grade and beneficiate them. At their solid-liquid contacts, there are transfers of ionic species, which for insoluble oxide minerals are the H+ and OH-ions. The adsorption density of these ions can be detected by carrying out potentiometric titrations, and this paper describes the automation of such an apparatus. The details are discussed fully and the validity of the method is demonstrated by flotation tests.

Jan 1, 1969

By P. C. J. Gallagher

A number of recmt determinations for the ratio of extrinsic to intrinsic stacking fault energy in fcc solid solutions are examined. Some of these arise from incomplete analyses which can yield only approxi?nate values for the ratio. Reliable results, on the other hand, obtained using extrinsic-intrinsic fault pairs, show that the extrinsic and intrinsic fault energies are essentially equal in several materials. There is some reason to believe that this finding is of general applicability to fcc elements and alloys. A wide range of values has been obtained for the relative magnitudes of the extrinsic and intrinsic stacking fault energies (yext and yint, respectively) in recently published studies in a variety of materials. In contrast, Hirth and Lothe' using a central force model have shown that out to tenth nearest-neighbor interactions the perturbation in energy caused by both types of fault is the same. Although the model used is not completely valid in metals, there is nevertheless some indication that marked variations of yext/nnt should not be observed from one material to another. In early work in Cu-A1, Cu-Ge, Ni-Co, and stainless steel all the deformation faults observed in the electron microscope were found to be intrinsic in nature, which led to an attitude that the extrinsic fault energy must be considerably greater than the intrinsic. Extrinsic faulting arising from deformation has, however, more recently been directly observed in Au-4.8 at. pct n;~ Ag-6 at. pct Sn and Ag-8 at. pct sn; Ag-7.5 at. pct In and Ag-11.8 at. pct 1n;"' pure silwer and Ag-0.5 at. pct ~n;' and Cu-22 at. pct Zn, Cu-30 at. pct Zn, and Cu-7.5 at. pct ~1.l' Multilayer loops containing extrinsic faulting have also been observed in quenched aluminum." While peak asymmetries in X-ray faulting probability studies were generally attributed to the presence of twins,Lelel2 has recently reinterpreted earlier X-ray data in Ag-Sb alloysU in terms of the presence of extrinsic faulting. The determinations of yeXt/yint made from the above studies are shown in Table I, with a brief description of the techniques employed. A number of the methods utilized are deficient in one or more respects, and the reliability of the values listed will be discussed. ~ele'~ recognizes that his approximate determinations of yext/yint assumes equal numbers of extrin-sically and intrinsically faulted dislocations. It is well-known, however, that such an assumption is not at all justified since extrinsic faulting has but rarely been observed in samples studied in the electron microscope. The only conclusion that should be drawn from the X-ray results at present is that the total intrinsic scattering cross section (i.e., the product of the width of the intrinsically faulted dislocations with their density) is approximately ten times greater than for extrinsic faulting in these particular samples. An important point is that the relative magnitudes of the energies cannot be inferred from results of this type, unless the intrinsic and extrinsic faults form with equal ease. One must recognize that, although a formation barrier may restrict the amount of extrinsic faulting which occurs, this in no way implies that the extrinsic and intrinsic energies should be different. It is unlikely that a worthwhile estimate of the relative densities of extrinsically and intrinsically faulted dislocations can be made at the high deformations present in X-ray samples. ~oretto,'~ from a statistical argument applied to the nonobservation of extrinsically faulted tetrahedra out of a large sample, concluded that yeXt/yint could not be less than -4.5. However, the present author feels that a high-energy formation barrier as just supposed also explains this finding satisfactorily and that no conclusion can possibly be drawn concerning the actual extrinsic stacking fault energy. The same argument also serves to explain the fact that extrinsic faulting has been relatively little observed in the electron microscope. Extrinsic-intrinsic node pairs and isolated extrinsic nodes were first reported by Loretto~ and subsequently by Ives and Ruff,' Gallaher,' and Gallagher and Wash-burn.' Ives and Ruff' found a wide spread in the ratio of extrinsically to intrinsically faulted area in the node pairs they observed, and drew the very tentative conclusion that yeXt/yint 2 2. They recognized that a straightforward comparison of the size of the faulted areas could provide no more than a qualitative result without a theoretical analysis of the dislocation geometry associated with extrinsic faulting. A theoretical

Jan 1, 1969

By W. H. Herrnstein, F. H. Beck, M. G. Fontana

Sulfur solubility in a iron was measured in the 750 to 890°C temperature range and was found to be insensitive to ferrite purity within a limited composition range. The permeability of sulfur in ferrite was determined from the internal sulfidation of Fe-Mn alloys. From the solubility and permeability results, the diffusivity of sulfur in ferrite could be calculated. These results are summarized as follows: Dissolved sulfur decreased the lattice parameter of ferrite. The effect of dissolved sulfur on the tensile properties of ferrite at low temperatures was also determined. SINCE sulfur is an important residual impurity in commercial irons and steels, effects associated with the presence of sulfur as a solute in iron are of considerable practical interest. Unfortunately, certain basic information relative to the Fe-S system appears to be lacking in the literature, e.g., the effect of dissolved sulfur on the lattice parameter and mechanical properties of ferrite. In addition, discrepancies exist in previously reported results for the solubility of sulfur in ferrite. These discrepancies raise questions regarding the sensitivity of sulfur solubility to the purity and microstructure of iron. This study was undertaken primarily in an effort to obtain reliable data on the solubility of sulfur in ferrite. Additional objectives included determination of the permeability and diffusivity of sulfur in ferrite by the internal sulfidation method and determination of the effect of dissolved sulfur on the lattice parameter and tensile properties of ferrite. EXPERIMENTAL METHOD Three grades of iron, encompassing a range of impurity levels, were employed in the study. The grades were designated VME (vacuum-melted electrolytic), SPZR (single-pass zone-refined), and MPZR (multipass zone-refined). The composition of each grade is given in Table I. Poly crystalline and single-crystal strip specimens were employed in the solubility experiments. Uniform grain size strip (ASTM 3 to 5) of 0.005 to 0.020 in. thickness was obtained by alternate cold reductions of 60 thickness 60 to 80 pct and recrystallization at 650°C for i hr in pure, dry argon. Single-crystal specimens were produced in 0.010-in.-thick SPZR iron strip by the strain-gradient anneal technique. Recrystallized strip 0.25 in. wide was strained until a Luders band or bands had propagated over the length of the strip; the strip was then annealed by drawing it through a 150°C per in. gradient (890°C peak temperature) at 1 in. per hr in an atmosphere of pure, dry argon. Laue photographs of the crystals produced exhibited no discernible asterism. Specimens were equilibrated with H-H, atmospheres at temperatures between 750" and 890" by one of two methods, each of which makes use of the reaction: The encapsulation sulfurization method was employed in the majority of the solubility experiments. A strip

Jan 1, 1969