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By Keith E. Meyers

Condition monitoring is a viable troubleshooting practice among many industries to extend equipment performance, minimize unplanned downtime, reduce maintenance and repair time and costs, and increase related aspects of plant safety. But obstacles abound for mining, mineral-processing and cement operations striving to implement the technologies. Harsh machine environments can muddy efforts. High vibration in machinery can interfere with wide-spread rollout. Staff expertise or skills may be lacking. And costs may be prohibitive. Fault detection has emerged as a practical and cost-effective solution to identify process and machinery faults before failure interrupts productivity or jeopardizes worker safety. Fault detection can be a stand-alone system or connected to plant automation.

Jan 1, 2005

By W. D. Keller

Scan electron micrographs, SEM's, will be shown of representative refractory clays from Missouri deposits, with counterparts from other localities. The story is in the pictures, ("1000 words in each picture"), but clay types include the following. Plastic, semi-plastic, and semi-flint "fire clays" of Missouri have textures which appear to retain certain relic texture of ball clay. Flint clay is composed of tightly interlocking packets, sheaves, and books of kaolinite. Diaspore and boehmite mineral textures characterize those "clays". Surface-boulder diaspore shows very pronounced recrystallization and crystal enlargement from original, unexposed first-grade diaspore.

Jan 1, 1977

By Yasuo Ojima

The mainstream of copper smelting processes in the world today is a combination of Outokumpu type Flash smelting and PS (Pierse Smith) converting process. Presently it can be estimated that about 50% of the worldwide copper production is produced by the Flash smelting process and 80% by the PS converting process. PS converting process due to its operational flexibility and despite its batch character of operation has been widely used in many smelters for more than 100 years. However, an environmental issue has been pointed out related to this process because of the difficulty of handling the fugitive gases. Recently several copper smelters in the world have been newly construeted and others have executed major modification and modernization. The continuous converting process has been applied in many of them instead of PS converting process. This paper compares PS to the emerging continuous converting process and makes a prospect of the future of the copper converting process.

Jan 1, 2003

By D. A. Kraai, S. Floreen

The effect of 1 to 50 ppm S on the ductility of nickel at 800° to 1400°F was studied. Results at each temperature showed a decrease in the reduction of area from approximately 95 to 5 pet over the sulfur range studied. Ductility varied with grain size, but only to a minor extent relative to the sulfiw effect. The effects of sulfur were completely offset by the addition of small amounts of magnesium. The results indicate that the "hot-short" loss in ductility is not an inherent property of nickel. Some possible mechanisms which cause the loss in ductility are described. MANY metals or alloys that normally possess high ductility exhibit a ductility loss at intermediate temperatures. This loss in ductility is often called "hot-shortness". Numerous examples of this phenomenon have been reported in the literature. Much of this work has been reviewed by McLean1 and by Rhines and Wray.2 To date there is no fully satisfactory explanation of the cause of this intermediate-temperature hot-shortness. It is generally recognized that impurities, and particularly impurities that form low-melting phases, can cause embrittlement. Examples of hot-shortness have been reported, however, where there were no obvious impurities present which would lower the ductility. Thus there has been some basis for believing that hot-shortness is an inherent property, and that even the purest metal would display a hot-short loss in ductility. This latter hypothesis was recently put forward by Rhines and wray2 based on studies of nickel and nickel alloys. In the discussion of this paper, however, Guard noted that high-purity nickel showed no hot-shortness.3 Thus there is reason to doubt whether pure nickel, or by inference any other pure metal, will inherently exhibit hot-shortness. The present work was initiated to determine the extent to which hot ductility was sensitive to very small amounts of an impurity element. If it could be demonstrated that hot-shortness could be induced by only minor amounts of an impurity, then it might be argued that hot-shortness in general is an impurity effect, and not a fundamental property of pure metals. The particular impurity studied was sulfur in nickel. The deleterious effects of sulfur are well- known. It is also well-known, and will be shown below, that additions of magnesium will render sulfur innocuous. When no such refining agents are added, however, the Ni-S system is a very useful one for studying the influence of small amounts of impurities. EXPERIMENTAL PROCEDURE Two heats containing -24 ppm S were vacuum-melted and small amounts of magnesium were then added under an argon atmosphere. These alloys were used to show the effectiveness of the normal magnesium treatment in overcoming the influence of sulfur. A second series of alloys with a sulfur range of 1 to 50 ppm was then prepared by vacuum melting nickel in alumina crucibles. No elements, such as magnesium, which tend to combine with sulfur were added. The higher sulfur contents were attained by adding nickel sulfide. Lower sulfur contents were prepared using a method in which the melt was oxidized under vacuum to produce the reaction S + 2O = SO2 These heats were subsequently deoxidized with carbon. Ten- to twenty-pound ingots were cast of all of the alloys studied. The compositions are given in Table I. The ingots were forged and hot-rolled to 3/4-in. bar. They were then annealed at either 2000" or 1600°F to produce different grain sizes. One-quarter-in.-diam tensile specimens were machined from the bars. These were tested at 800°, 1000o, 1200°, and 1400°F. The specimens were held at temperature approximately 45 min before testing. The strain rates were 0.005 min-1 to yielding, and 0.05 min-' after yielding. No extensometers or gage marks were placed on the specimens because the higher sulfur heats tended to fracture at the knife-edge indentations or gage marks. The properties measured were ultimate tensile strength and reduction of area. The analytical technique for determining sulfur at low levels was that developed by Burke and Davis.4 They reported a standard deviation of 1 ppm at an average sulfur level of 4 ppm in NBS standards. A standard deviation of 3 ppm is probably more realistic for the alloys used in this investigation considering the possibility of some segregation in the ingots. RESULTS A summary of the tensile results is given in Table I. As shown in the table, both heats to which

Jan 1, 1964

By Lucien Eaton

VENTILATION in the iron mines of the Lake Superior region in nearly all cases is natural; that is, it is induced by the difference in elevation between different outlets in the mine and by the difference in temperature of the air in the mine and that outside. This difference in temperature is frequently augmented by placing a steampipe in the upcast shaft; but aside from this, artificial aids to ventilation have been rare until - recent years. In some of the older mines, as at the Cliffs Shaft mine at Ishpeming, Mich., in the 80's, fans have been used when there was only one opening to surface, but their use was abandoned as soon as a natural circulation of air started. In recent years, the Newport mine at Ironwood, Mich., was the first to use positive mechanical ventilation. The installation was not large enough, however, to give definite results, reliance being placed largely on natural ventilation. With the coming of warm weather in the spring of 1914, the necessity of positive mechanical ventilation at the Lake mine of the Cleveland-Cliffs Iron Co. at Ishpeming, Mich., became evident. The workings of the Lake mine are under the bed of old Lake Angeline, which was pumped out in 1894, and the mine had been in operation for 6 years prior to that date making a total of 26 years of continuous operation. The total production, up to 1914, amounted to over 8,000,000 tons. The ore was first mined by square-set rooms and pillars, but this was later changed to top slicing and caving. Both methods required the use of large amounts of timber, probably 80,000,000 board feet in all, practically all of which remained in the timber mat. The slow oxidation of this timber was one of the principal causes leading to the installation of mechanical ventilation. The mine was served by only one working shaft, called No. 4, a second outlet being provided by a raise to the surface from the old workings on the south side of the mine. This raise was the "down cast;" but it was very small and the drifts and raises leading to it were too small and crooked to permit an adequate amount of air to enter the mine, especially during the warmer weather. Measure-

Jan 8, 1920

At a regional scale, the Otago Schist has been divided into textural zones, metamorphic zones, structural transposition zones, and terranes and lithologic associations. Each of these subdivisions reveals aspects of the internal structure of the lithologically monotonous Otago Schist but, to date, a map of the schist derived directly from structural data has not been made. In the present study, digitised structural data from the QMAP GIS were used to make a form line map of Schist foliation which, in turn (and using certain non-unique guiding assumptions), was used to construct a provisional foliation thickness map of the Otago Schist. Contours of dominant foliation (Sp) thickness have been drawn from 4 kIn above to 16 km below the reference level of the Caples-Torlesse terrane boundary in the schist structural pile. A recent revision of the Otago Schist textural zone classification has shown that the grain size of metamorphic white micas increases progressively with textural grade. There also appears to be a correlation between schist mica grain size and foliation thickness. Using mica grain size, it may eventually be feasible to establish the vertical structural position of samples in greenschist facies parts of the schist pile to a precision of ¦ 1 km or better, even if they are in inliers or fault-bounded blocks. Foliation thickness and mica grain size are thus potentially useful tools for research and exploration in the Otago Schist in that they assist with structural interpolation and extrapolation. Even at this early stage of application they can be used to provide hitherto unobtainable, semi-quantitative estimates of displacement on Mesozoic and Cenozoic faults and folds.  

Jan 1, 2001

By F. A. Rutledge

"The W. E. Dunkle mine, sometimes called the Costello Creek coal mine, is 8 miles N. 20° W. of Colorado Station on the Alaska Railroad. The presence of coal in this area has been known since the district was extensively pros¬pected for gold between 1911 and 1915. At that time, coal from this deposit was used by miners for blacksmithing. The increased demand for coal resulting from government defense projects in Alaska led to exploitation of this deposit in 1941.The inability of Alaska coal mines to supply the quantity of coal required by public and private consumers and by the armed forces in Alaska was responsible for establishment by the Army of the Coal Procurement Section of its Alaska Department. It proposed to investigate the deposits and to expedite production from the Alaskan coal fields. The Bureau of Mines closely cooperated in this program.The quality of the Dunkle coal and the favorable location of the deposit caused it to be one of the properties chosen for investigation under a joint Army-Bureau of Mines-Geological Survey program.During July 1943, the coal area in the immediate vicinity of Costello Creek was geologically and topographically mapped. by Clyde Wahrhaftig and Jacob Freedman, geologists, U. S. Geological Survey. F. A. Rutledge, mining engineer of the Bureau of Mines examined the property July 18 to 22, 1943, and a project of trenching, diamond drilling, and sampling was initiated on August 4, 1943. During the project Clyde Wahrhaftig remained at the Dunkle mine to interprets drill cores and assist the author in planning the explora¬tory program. The project was completed October 7, 1943.Field investigations were under the general direction of R. S. Sanford, acting chief, Alaska Branch, Mining Division. Coal analyses were made by Maurice L. Sharp, coal analyst for the Alaska Railroad.Special mention is made of the cooperation and assistance received from Clyde Wahrhaftig, geologist, U. S. Geological Survey.The many courtesies received from the owner, W. E. Dunkle, and the members of the Army Coal Procurement Section, Alaska. Department, also are acknowledged.The W. E. Dunkle coal mine is in the Broad Pass region on the south slope of the Alaska Range at an altitude of 2,800 feet (fig. 1). It is situated within the Third Judicial Division, headquarters of which is Valdez, Alaska. The area is situated approximately at latitude 63° 15' N. and longitude 149° 30' W. and is connected with the Alaska Railroad at Colorado Station by an 11-mile gravel road that is passable throughout the year. This road is maintained by the Alaska Road Commission. A private telephone line to Colorado Station connects with the telephone and telegraph service of the Alaskan Railroad.The passenger rate from Anchorage, Alaska, to Colorado station is $12.10. Freight rates are $1.60 a hundred pounds for heavy machinery and $2.66 a hundred pounds for first-class freight.The Costello Creek coal basin is in an area of low relief and has been dissected by numerous creeks flowing down the south flank of the Alaska Range. The Dunkle coal mine is on Coal Creek, a small tributary of Camp Creek, 1,000 feet from their junction. About 700 feet below this junction, Camp Creek joins Costello Creek, which in turn empties into Bull River 1/2 mile above the latter's confluence with the West Fork of the Chulitna River. The location of the mine is shown on figure 1."

Oct 1, 1948

By Samuel M. Brock

In recent years society has become increasingly concerned with maintaining and improving the quality of environment. Thus, public interest and concern with pollution problems is now high. This is reflected in recent federal and state efforts to formulate new legislation to prevent pollution and strengthen existing pollution laws. In reviewing literature pertaining to pollution problems, it is possible to distinguish many common elements. The most outstanding of these is the failure of the market to guarantee that private firms responding to price signals generated in the marketplace will make decisions leading to optimal resource use. Cases of market failure in allocating natural resources according to the wants of society frequently are due to the presence of technical externalities, or side-use effects.59 These roughly and generally can be defined as interdependencies among production and consumption units, the impacts of which are exerted other than through the market. They are, in other words, extra-market relationships. The economic unit generating external effects does not take them into account in decision-making. Thus, the tendency is for the unit to produce either more than society desires or not enough. In such cases society often has intervened in the decision-making process. This intervention frequently has taken the form of legislation to regulate production and consumption activities. Thus, a body of institutions, which acts as a constraint in decision-making processes, has materialized. These institutions are often far more influential in their effect upon resource use than are the forces of supply and demand acting in the marketplace. The problem of environmental pollution is essentially the problem of handling residuals which are the byproduct of all production and consumption activities which take place in the economy.2 These residuals are emitted into the air and water and disposed of on the land. They are interrelated, in that efforts to control emissions into the air or water can result in the production of solid wastes, which then present disposal problems. It is convenient to separate residuals by the type of pollution they cause-air, water, and land while remembering that these problems are related and that solutions may require coordinated effort.1 Residuals may be produced in both production processes and consumption. Residuals produced in production by the mineral industry, or firms utilizing its products, range from emission of sulfur dioxide by steam generating plants to radioactive mill tailings produced in the course of mining uranium.. Residuals associated with consumption are generated mainly through transportation of members of the household, space heating, and in the disposal of solid wastes, including refuse and junk autos. Residuals associated with both production and consumption receive attention in ensuing sections of this chapter.

Jan 1, 1976

By G-L. Wu, S-W. Wu

"The hot deformation behaviour of Nb-Ti microalloyed high-strength steel was investigated. Hot compression tests were conducted in the temperature range 900 to 1100°C under strain rates of 0.1, 1, and 5 s-1. Dynamic recrystallization (DRX) occurs as the main flow softening mechanism at high temperature and low strain rate. The hot deformation activation energy was calculated to be about 404 699 J/mol. The constitutive equation was developed to describe the relationship between peak stress, strain rate, and deformation temperature. The characteristics of DRX at different deformation conditions were extracted from the stressstrain curves using the work hardening parameter. The Cingara-McQueen equation was developed to predict the flow curves up to the peak strain. The processing maps were obtained on the basis of a dynamic materials model. The results predict an instability region in the temperature range 1010 to 1100°C when the strain rate exceeds 0.78 s-1. IntroductionThe 700 MPa grade HSLA steel is widely used in engineering machinery, automotive beams, carriages, and axle tubes, etc. (Pan et al., 2017 ). Generally, such grades contain a moderately high amount of Mn (approx. 1.4% and above), and microalloying elements like Nb, Ti, V, and Mo to impart the desired strength and toughness through solid-solution strengthening, precipitation hardening, and grain refinement dislocation strengthening (Chen and Yu, 2012; Opiela, 2014). However, the production costs can be greatly reduced by replacing part of the Nb, V, or Mo with inexpensive Ti and adopting the compact strip production CSP process (Opiela, 2014; Chen et al., 2015). Furthermore, the microalloying technology coupled with new-generation thermomechanical control processing (NG-TMCP) has proved efficient for achieving the proper balance between strength, toughness, ductility, and formability by means of a suitable combination of chemical composition and thermomechanical treatment parameters (Shukla et al., 2012; Wu, Zhou, and Liu, 2017).In hot forming processes, the complex microstructural evolutions are often induced by multiplicative hot deformation mechanisms, such as work hardening (WH), dynamic recovery (DRV), and dynamic recrystallization (DRX) (Zhang et al., 2014; Liang et al., 2015). Dynamic softening behaviour during hot processing has generated considerable interest because component properties are influenced significantly by its corresponding microstructural evolution (Wu et al., 2010). During deformation in the DRX process, deformed grains are replaced with substructures and newly formed fine and uniformly distributed grains. This occurs only when a critical strain for the onset of DRX is reached, and at the same time, the minimum rate of energy dissipating is reached (Ferdowsi et al., 2014). DRV occurs at a high strain rate and low temperature, reducing the stored energy greatly and making DRX difficult (Liang et al., 2015). The microstructural changes during DRX are sensitive to the processing parameters, such as strain rate, deformation temperature, and strain (Zhang et al., 2014; Ferdowsi et al., 2014). Therefore, in order to optimize the hot processing parameters, it is important to understand the behaviour of hot deformation visà- vis control of microstructural evolution."

May 1, 2019

By Wm. Reisz, Raphael Trousselle

We are now well into our second decade of commercially available electronic initiation systems. Over this time, the technological advances have made electronic systems a very practical option for a wide variety of blasting applications.

Jan 1, 2011

By M. A. Llavona

In Spain, as in many countries, the gold content of jewellery must be officially hallmarked. The official methods of assay are gravimetnc cupellation (a method which is highly accurate but both time and sample consuming), potentiometry, gravimetry and volumetry. In this paper, a procedure for measuring gold by flame atomic absorption in jewellery samples is described. The method is based on the acid digestion of a 40 mg sample. The quantity of aqua regia necessary for dissolving the gold, the ideal weight of a sample in order that the error may be minimal, the effect of the acids employed, the type of material used for its storage, and the necessity of employing a buffer to avoid the ionization of the solution are described. The method proposed is simple, highly accurate and causes little damage to the jewellery.

Jan 1, 1999

By R. V. Ramani, R. Bhaskar

"One of the primary means of control of health hazards from respirable contaminants in mine atmospheres is through design and operation of mines to meet mine health and safety regulations and recommended practices. A U.S. National Academy of Sciences study concluded that for significant progress in coal mine dust control, research should be directed more toward obtaining fundamental understanding of the origin, transport and characteristics of respirable coal mine dust. Theoretical and experimental studies on transport of dust · in mine airways, particularly coordinated efforts to validate theory with practice, are scarce. Some empirical models, developed on the basis of experimental data, are available but these models cannot be applied to new conditions. The purpose of this paper is to present the results of theoretical and experimental studies on the transport and deposition of dust in mine airways. This study is a part of an ongoing research project in the Generic Mineral Technology Center on Respirable Dust.In the paper, the assumptions of the modeling phase of the project and the development of a convectiondiffusion equation for dust transport in mine airways are outlined. The important aspect of the modeling effort is the capture of the deposition phenomenon. The experiments performed under controlled conditions in a typical mine airway, as well as under normal mine operating conditions, are discussed. The comparison of the model predictions with experimental results are made to identify critical areas of agreements and deviations. The implications of the findings and areas for further research and development are presented."

Jan 1, 1990

In setting out to describe the methods and machinery employed at Iron Knob the writer does not attempt to give any information as to the situation, topography or geological features of the locality. This, together with estimates of the quantities of ore still available, has been carried out in a most thorough manner by R. L. Jackr and F. R. Hockey. This essay is intended to deal with working methods as they exist to-day, beginning with drilling, blasting, quarry traction, etc., and touching on such details as the supplyof electricity, water and compressed air.At the present time almost the entire output of ore is won from the hill known as Iron Monarch. The form of the hill, a smooth, rounded dome, rising some 640 ft. above the plain and having a base diameter of n miles, lends itself ideally to the "bench" system of open-cut quarrying.Fig. 1 shows the relationship of the benches "A," "B" and "E" in their order of development. Bench "E" is at present the principal working, but, as the greater part of the ore above this level has now been removed, bench "A," some...

Jan 1, 1936

By C. Ayora

The Iberian Pyrite Belt (SW Spain and Portugal) contains one of the largest reserves of pyrite in the world with mining activities dating back to prehistoric times. About one hundred abandoned mine wastes and galleries release a huge acidity and metal load to the Tinto and Odiel rivers. Once the mining activity is over, polluting discharges can persists for decades or even centuries with no specific responsible entity. In-situ passive remediation technologies are especially suitable for these orphan sites. The concept is to insert a reactive porous material in the natural flow path of contaminated surface and ground waters, and it is implemented through infiltration ponds and reactive barriers, respectively. Calcium carbonate pea-size gravel is the common alkalinity supplier to neutralize acidity and precipitate metals. These remediation systems have been traditionally implemented in coal mines. However, the acid drainages from the Iberian Pyrite Belt contain metal concentrations one to two orders of magnitude higher than those from coal mines and require special designs to avoid quick clogging or passivation (coating) of the grains of reactive material. To overcome these problems, a Dispersed Alkaline Substrate (DAS) mixed from fine-grained limestone sand and a coarse inert matrix (e.g. wood chips) was developed. The small grains provide a large reactive surface and dissolve almost completely before the growing layer of precipitates passivates the substrate. The high porosity and the dispersion of nuclei for precipitation on the inert surfaces retard clogging. However, limestone dissolution only raises pH to values around 6.5, which is sufficient to precipitate the hydroxides of trivalent metals (Al, Fe), but it is not alkaline enough to remove divalent metals. Magnesium oxide, which hydrates to Mg hydroxide upon contact with water, buffers the solution pH between 8.5 and 10. A DAS system replacing limestone with caustic magnesium oxide has been tested to be very efficient to remove divalent metals (Zn, Cd, Mn, Cu, Co, Ni, Pb) from drainage previously treated with limestone.

Aug 1, 2013

By DALE MacGREGOR, VERA TUREK

The Blue Mountain nepheline syenite deposit has been the subject of several detailed studies. It has been variously referred to as an intrusive stock, a metasomatic deposit, an intrusive sill and a metamorphic-metasomatic body. The body is divided into six mineralogical zones, the first five being based on the characterizing accessory mineral; muscovite, muscovitemagnetite, biotite-muscovite, biotite, hornblende and pink syenite. Mining currently takes place only in the biotite zone. Foliation is particularly prominent in the central (hornblende) zone and near the margins of the nepheline syenite. Majic bodies within the nepheline syenite may represent basic rocks that have been less altered by metasomatism, metamorphosed basic dykes or sloped blocks of metasediments. The most prominent structural features are the northeast-trending folds that have been modified by later north west-trending folds.

Jan 1, 1984

By Itavahn Alves da Silva, Jose Dimas de Arruda, Amanda Aparecida Fátima Arruda, da Silva de Souza, Carlos Antonio da Silva, Varadarajan Seshadri, Samuel

The knowledge of the flow field inside a continuous casting mold is essential to improve operational efficiency of the process and also to achieve better inclusion control. Physical modeling, PIV technique and CFD have been employed to assess the velocity distribution in the metal- slag interface region in a slab mold. The analysis of results shows how higher casting velocity and lower immersion depth of submerged nozzle can lead to higher turbulence in the slag-metal interface. The effects of density difference between slag and metal and interfacial tension between the phases have been highlighted.

Jan 1, 2016

By Clark F. Grain

The monoclinic to tetragonal inversion of zirconium dioxide was studied by single-crystal X-ray methods, high-temperature X-ray diffractometry, and differential thermal analysis. The unusual features of the inversion, such as no definite transition Lperature, hysteresis, and athermal kinetics, were confirmed for powders who mean crystallite size was greater than 1,000 A. Samples of mean crystallite size below 1,000 A displayed classical kinetics, obeying a logarithmic rate law. A detailed mechanism based on Ubbelohde's theory of continuous phase transformations was proposed which is consistent with all the experimental facts.

Jan 1, 1965

By A. Bobet

Design of a new underground laboratory is underway through the auspices of the United States National Science Foundation. The Deep Underground Science and Engineering Laboratory (DUSEL) is scoped to provide a diverse group of researchers with a dedicated underground facility capable of supporting a broad spectrum of fundamental and applied research at depth in the Earth?s crust. Key research partners in the endeavor are physicists, biologists, geoscientists and engineers. Engineers are not only designing the underground facilities, but are also actively involved in developing research initiatives. This paper will introduce the DUSEL engineering research program to the mining community, provide an overview of the site, geology, and laboratory facilities, and describe some key program initiatives. The particular technical challenges and opportunities afforded by the construction of DUSEL and the performance of the integrated science-engineering program will be discussed by reference to a subset of research initiatives that are currently under development: Cavern Design, CO2 Sequestration and Transparent Earth. These research initiatives target the development of new techniques that can support improved subsurface investigation, design and construction procedures. An increased use of the subsurface can actively contribute to the development of new, more sustainable solutions for use in mining and civil engineering practice.

Jan 1, 2011

By H. R. Peiffer, R. Geckle

The silver phase of silver and finely divided alumina composites is shown to grow as single crystabs upon solidification from the melt. These crystals grow without the aid of an externally applied thermal gradient or a mold. The single-crystal growth is more readily disrupted as the alumina content varies from the optimum concentration of 20 wt pct. Pretreatment such as variation of fabrication pressure, and presintering of the specimens appear to play a lesser role in this phenomenon. In actual practice the growth of single crystals of metals from the melt is a tedious, painstaking process.' Care must be taken to insure the proper thermal gradients and rate of growth in a vibration-free environment. Excellent single crystals can be grown when these variables are controlled. When a second insoluble and finely divided phase is present in the melt the growth of single crystals is difficult, if not impossible, even under the most favorable conditions outlined above. During the past few years, a composite of silver and alumina has demonstrated an ability to resist flow even though the major phase, silver, is mo1ten. 2 A more surprising feature of this material is the ease with which single crystals of silver grow upon cooling the composite from temperatures above the melting point of silver to temperatures near room temperature. Observations have been made that demonstrate that single crystals of silver will grow even when conditions most unfavorable for growth of pure silver crystals exist. The crystals grown in this manner are imperfect in that a great deal of subgrain structure exists. It is the purpose of this manuscript to qualitatively describe this process and to attempt to isolate the influencing factors of this behavior. MATERIAL PREPARATION The composite material is prepared by powder-metallurgical techniques. Two items of great importance are the introduction of oxygen into the system and the obvious need for a thorough mixing of the metallic and refractory oxide phases. The oxygen is necessary in order that the silver wets the alumina. Without oxygen the phases separate and the material shows no unusual properties. In order to supply the needed oxygen the silver is added in the form of silver oxide which is readily decomposed to oxygen and silver upon heating. The silver oxide is readily obtained in a finely divided form that allows a uniform mixture of the alumina and silver oxide to be prepared. The correct ratio of alumina to silver oxide is mixed in the presence of alcohol in an ordinary food blender. The mixture has the consistency of a thin slurry and after mixing for approximately 20 min is dried and pressed into billets at various pressures. As is shown in Fig. 1, there is no limit to the shape of the specimens obtainable as single crystals. These billets are heated in air in a predeter-

Jan 1, 1964

By Che-Yu Li, J. L. Gregg, W. F. Brehm

Oriented, oxygen-doped niobium bicrystals were tested in liquid lithium. The grain boundaries were attacked preferentially. The depth of the penetrated zone varies as (time)2. The penetration was aniso-tropic, had a high activation energy, and increased with the increased oxygen doping level. A possible model was proposed to account for the experimental observations. 1 HE grain boundary penetration of a metallic system by liquid metal has been studied by several investigators. Their results are summarized by Bishop.' Most of these works show that the penetration by liquid metal corresponds to the phenomenon of liquid metal wetting. In the case of a grain boundary, wetting will occur when twice the solid-liquid interfacial tension is smaller than the grain boundary tension resulting in the replacement of the grain boundary by two new solid-liquid interfaces. Other possibilities exist; for example, the atoms of the liquid metal may diffuse into the grain boundary region due to chemical potential gradient. The gradient can be produced by impurity segregation or simply be due to the increase in solubility in the grain boundary region. The penetrated grain boundary in these cases may remain solid at the test temperature. The Nb-Li system has been of considerable interest because of its possible technological applications. For fundamental interest it provides a possibility of studying the grain boundary penetration process which is not controlled by the wetting mechanism. The pure niobium is not attacked by the liquid lithium, but if niobium containing more than 300 to 500 ppm oxygen by weight is exposed to liquid lithium, corrosion occurs at the solid-liquid interface and preferentially at grain boundaries. Previous investigators2-' have proposed that this preferential corrosion at grain boundaries is caused by oxygen segregation there, with subsequent inward diffusion of lithium to form a Li-Nb-0 compound. These investigators also found that the corrosion could be retarded by adding 1 pct Zr to the niobium to precipitate the oxygen as ZrO2 upon proper heat treatment. However, there are no quantitative data on the kinetics of the grain boundary penetration process to test the validity of the proposed corrosion mechanism. In this work an investigation of this penetration process in oriented bicrystals was made as a function of the oxygen doping level in the bulk niobium and the grain boundary orientation. A possible model for the penetration process based on the experimental results was proposed. EXPERIMENTS Oriented niobium bicrystals were grown by arc-zone melting oriented single-crystal seeds.7 These bicrystals contained simple tilt boundary. The [001] directions in the two grains were tilted about a common [110]. The bicrystals were 31/2 in. long and 5 by 4 in. in cross section with the straight, symmetric, planar grain boundary longitudinally bisecting the crystal rod. The bicrystals were doped with oxygen by anodically depositing a layer of Nb2O on the surface in a 70 pct HNO solution at 100 v, using a stainless-steel cathode. The specimens were homogenized by annealing in evacuated quartz tubes at 127 5°C. Oxygen content of the niobium was measured from microhardness values, after DiStefano and Litmman.' Supplementary checks were made with vacuum-fusion analysis.7 Individual test specimens cut from the doped bi-crystal rods, about by by % in. in size, were tested inside double jacket sealed capsules. The inner jacket was niobium, the outer was stainless steel. The niobium inner jacket eliminated the problem of dissimilar-metal mass transfer.' The lithium (99.8 pct pure, obtained from Lithium Corp. of America) was handled only in a purified argon atmosphere in a Blickman stainless-steel glove box. After introduction of lithium, the capsules were sealed by welding. Further detailed experimental procedures are given in Ref. 7. The capsules were heat-treated in vertical Marshall resistance furnaces. Temperatures were controlled to When heating above 1100°C, it was necessary to seal the furnace work tube and flow argon through to prevent failure of the stainless-steel outer jacket of the capsule. Tests were made on 6" 2", 16" 2, and 33" i2" bicrystals at oxygen levels up to 2600 ppm by weight in the 6' and 16" crystals and with 1300 ppm oxygen in the 33' crystals. The oxygen levels were controlled to 100 ppm. Most of the quantitative data were obtained from 16" bicrystals between 800" and 1050°C. The capsules were quenched into water after the test and cut open with a water-cooled abrasive wheel. The capsules were then submerged in water, which dissolved the lithium and freed the specimen. Measurement of the depth of the penetrated zone in the grain boundary was done either on metallographically prepared surfaces or directly on the grain boundary plane after the specimen was fractured in tension in the grain boundary plane. The depth of penetration measured by both methods agreed well. Further details describing these techniques have been reported elsewhere.'p7

Jan 1, 1969