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By D. R. Babich, R. A. Allwes, L. V. Wade

The design of a longwall entry system is discussed in this Bureau of Mines paper. This is done primarily through the results of an in-mine case study made of two sets of longwall entries utilizing the stiff- yield pillar design concept. The rock mechanics instrumentation plan used in this case study is shown, including a description of the instrumentation layout and the types of instruments used. The analysis of the stress changes in the abutment and yield pillars is presented in detail as the longwall panels were mined. Conclusions concerning when the pillar first started to experience significant stress, pillar stress history as the longwall face approached and moved past the pillars, stress distribution within the pillars and relative stress changes between yield and abutment pillars are discussed. The paper concludes with a discussion of the redistribution of stress in the vicinity of the long- wall panel.

Jan 1, 1982

By N. A. Gjostein

The formal descnption of the decay of an isolated scratch can be written in terms of an appropriate Fourier integral. With the application of certain approximations, this description leads to the second-moment analysis developed by King and Mullins. It is shown that the second-moment analysis does not adequately describe the behavior of a decaying, isolated scratch, and that it is difficult to obtain internally consistent values of the surface self-diffusion coefficient, D,,from this analysis. This inconsistency arises from contributions of higher-order moments to the decay process. Two new analytical methods, based on the Fourier integval representation of a scratch profile, have been developed for determining values of D, from the decay kinetics of isolated scratches. In the profile-matching method, a given initial profile is resolved into its Fourier components, the components are allowed to decay exponentially over an annealing time interval, At, and finally they are synthesized to form a decayed profile. The predicted profile is adjusted to fit the experimental profile by varying only the parameter, D,At; the contribution from volume diffusion is directly taken into account and the integrals involved in the Fourier analysis are evaluated by numerical integration on an electronic computer. In the kinetic method, the widths, W, of a series of predicted profiles are determined for various volume-diffusion contributions, and the results are plotted in the form W vs DSAt. For a fixed ratio of surface to volume diffusivities, R, these plots are linear; the slope of the lines increases as R decreases. A simi-lar analysis can be performed on the depths of the predicted profiles. In this case, plots of (l/df3 vs D,At are found to be nonlinear. The proper value of Ds is found by superimposing the data for the experimental widths and depths on Plots of this kind and adjusting Ds until a fit is obtained with the line having the appropriate value oj R. An analysis of the slopes of these plots for R —= (surface diffusion only) reveals that they do not give the correct value, 2276, for width tf second-moment standard profile. This finding allows one to modify the second-moment analysis in such a way as to obtain internally consistent values of Ds. ThERE are several processes, involving a flow of matter along a surface, due to gradients in curvature of the surface, that may be used to determine the surface self-diffusion coefficient, Ds. These processes are commonly known as 1) thermal grooving, 2) single and 3) multiple scratch decay, 4) blunting of field-emitter tips, and 5) sintering. In this series of papers, the first three of these processes are examined in detail in an attempt to subject the phenomenological theories governing these processes to a critical test and, furthermore, to make a critical comparison of the values of D, obtained from these techniques. Although the thermal grooving technique has been established'' as a reliable method for determining D, , this has not been the case for the process of scratch flattening. Mullins and coworkers374 have proposed phenomenological laws governing the growth of the width and the decay of the amplitude of an isolated scratch, but only in one study5 has the width-growth law been supported by experimental evidence. In paper I of this series detailed experimental evidence is presented that points up the deficiencies of the second-moment analysis; the origins of these deficiencies are also discussed. Following this development, some new analytical procedures, based on representing the scratch profile by Fourier integrals, are presented as a means of obtaining reliable values of D, from the kinetics of the scratch-flattening process. Further applications of the Fourier integral approach are reported in papers 11' and 111,~ where the method has been useful in interpreting the anisotropy of flattening rates of isolated scratches (paper 11) and in describing the multiple scratch decay process (paper 111). THEORY OF SCRATCH DECAY Following ~ullins" approach we consider an arbitrarily shaped scratch profile, Fig. 6, at some time, t. The profile is designated by a function z(x,t) which can be expressed in terms of a Fourier integral as follows:

Jan 1, 1967

By R. D. Carnahan, J. E. White

A study of dispersion strengthening in TD-Nickel (nickel plus 2 vol pct Tho2) was conducted employing microstrain techniques at ambient room temperature. It was found that optimum strength was due primarily to the incorporation of stored energy developed by a variety of thermal-mechanical treatments. The relatively low strength of the recrys-tallized condition implies that the dispersed particles themselves offer only token resistance to deformation. The development of resistance to large-scale recovery or recrystallization at temperatures near the melting point requires a more extensive sequence of strain-anneal cycles than does the development of optimum strength. A micro-Bauschinger effect was observed which appears to be related to the lattice resistance to the movement of free dislocations. The effect was nearly identical to that in pure nickel indicating that the presence of the dispersed phase and considerably increased dislocation density (stored energy) only alters the number or effectiveness of barriers. THE early stages of deformation of engineering materials can be conveniently studied by utilizing strain-gage techniques which permit resolution of strains less than 5 X 10-7 in. per in. for testing in four-point bending (Carnahan and white1). The present investigation, part of a continuing study on the very early stages of deformation, was designed to reveal the true role of a dispersed phase in promoting high strength in a commercially available dispersion-strengthened alloy. Although this technique has been used for some time to study microdeformation in pure metals and alloys, it has just recently received attention as a means of investigating dispersion strengthening. Studying the very early stages of deformation in alloys which depend upon a finely dispersed inert phase for strength may prove to be a very important method for a better understanding of these materials. It is essential to obtain considerable clarification of actual dislocation movement and the kinds of deformation barriers which exist before optimum properties can be designed into this type of material with any degree of confidence. Considerable research on a variety of dispersion-strengthened materials has resulted in two different schools of thought regarding the strengthening mechanism. One faction2-4 favors the idea that the particles themselves resist the motion of dislocations. The criterion for yielding is the fracture of the dispersed second-phase particles due to an array of piled-up dislocations. Other invesfigators5-a have shown that particles are effective primarily by allowing a greater buildup of stored energy or dislocation density through thermal-mechanical treatments in the composite than the pure matrix material. The particles themselves, then, are not exclusive obstacles, but the complex network of particles, dislocation tangles, subboundaries, and grain boundaries are strength determining. The development of such a complex dislocation network in SAP has been studied recently in some detail by Goodrich and Ansell. The ability of dispersion-strengthened alloys to resist softening or recrystallization is also of considerable importance; however, the criteria for maximum stability may not necessarily be those for maximum strength. In this study, in addition to the evaluation of the microstrain properties of TD-Nickel, it is felt that considerable clarification of the true dependence of strength and stability on the dispersed phase is shown. I) MATERIAL AND PROCEDURE TD-Nickel is a dispersion-strengthened alloy developed by the E. I. DuPont de Nemours Co., which contains 2 vol pct thoria (Tho2) in a pure-nickel matrix. The average ThO2 particle size is approximately 0.1 p and the interparticle spacing is less than 1 u. The material was supplied by DuPont in two conditions: hot-extruded bar stock, and stress-relieved cold-rolled sheet 0.025 in. in thickness. The bar was extruded at 2200°F from a cold-pressed and sintered billet. The sheet stock was prepared from the extruded material by a process involving ten or more 50-pct cold reductions by rolling with intermediate anneals at 1800° to 2000°F. Test specimens used in this study were prepared in the form of rectangular parallelepipeds measuring 0.375 by 1.375 in. in thicknesses ranging from 0.025 to 0.040 in. Samples prepared from sheet and extruded stock were mechanically polished before heat treatment and were handled with extreme

Jan 1, 1964

Who is ArcelorMittal Mines Canada ?One of Canada's leading suppliers of iron ore to steel markets around the world ?Past company name = ??Quebec Cartier Mining?? ?Operator of one of North America's largest open-pit mines ?Mont Wright Mines ?Fire Lake Mine ?Largest ArcelorMittal iron ore mining subsidiary ?Annual production of 15 million tonnes of concentrate ?Major expansion program to 24 MT/Y ?Internationally competitive pellet plant ?9.0 million tonnes annually

May 1, 2011

By C C. Souza, S C. Amarante, A C. Arauj

All major companies now producing iron ore in Brazil currently employ or are planning to employ some sort of concentration method to upgrade their fine sized products (sinter feed fines and pellet feed fines). The criteria for the selection of the most suitable concentration method for each application include a series of parameters; the most important among them being related to ore mineralogy. This paper reviews the concentration operations currently employed in Brazil and shows how ore mineralogy plays a fundamental role in the selection of a given method. Examples involving gravity concentration (jigs and spirals), magnetic separation (Rare Earth wet drums, ferrous wheel, and Jones type magnetic separators) and flotation (especially column flotation) are discussed. Fundamentally important for the selection of a concentration method is the mineralogy of iron-bearing minerals and gangue minerals presented to the feed to the concentration unit operation. For instance, the presence of liberated quartz as the major gangue mineral for a pellet feed size stream generally indicates that flotation will be the best selection for the concentration of that stream. However, even if magnetite is present only in the form of crystal relicts within hematite grains, it may lead to the selection of either magnetic separation alone or a combination of magnetic separation and flotation for concentrating such material. Presence of gibbsite and/or kaolinite as the major phase containing alumina will also affect the selection of the concentration method in all cases. Again for the case of pellet feed size streams, kaolinite does not interfere with flotation whereas gibbsite tends to contaminate flotation concentrate (pellet feed fines) as it is depressed together with iron oxides and hydroxides during the reverse cationic flotation process.

Jan 1, 2002

By S. P. Taite, A. R. Charest, P. D. Lewis

The El Sauzal deposit is a classic, high sulfidation, epithermal gold system located in southwestern Chihuahua State, Mexico. The prospect was discovered by a Francisco Gold Corp. geologist in1995. El Sauzal was encountered as a result of an extensive grass-root exploration program in the rugged, dissected volcanic terrains of the Sierra Madre Occidental, around the historical Batopilas Silver Camp. At El Sauzal, high grade gold is hosted within a series of more permeable, low-dipping, lithic and fine-grained dacitic rocks of early Tertiary age. The mineralization appears to be both structurally and lithologically controlled. The alteration characteristics are typical of a high sulfidation system including kaolinite, illite, alunite, dickite and pyrophyllite. The deposit’s gold distribution, as recorded from drill-hole data and surface samples, varies from 0.2 to 650.0 g/t. The estimated geological resource, as calculated from an independent study completed in 1998, was 3.0 million oz @ 2.03 g/t including a minable reserve of1.8 million oz @ 3.3 g/t.

Jan 1, 2004

President elect Ralph Moore opened the business meeting at 9:30 a.m., he called on the Auditing Committee to present its report on the financial statement of the treasurer. Gabe Ishley read the report and asked for its approval. A motion was made, seconded and carried. The Resolutions Committee was called upon to make its report. William A. Bear submitted the following: (1) WHEREAS, the 72nd Regular Meeting of the Rocky Mountain Coal Mining Institute celebrates sixty-four years of most successful service to the coal industry, and WHEREAS, this success is largely due to the faithful and devoted service of our Secretary-Treasurer, Augusta Whiteside, during the last fifty years of its existence, NOW THEREFORE BE IT RESOLVED, that we commend and express our sincere thanks to "Gussie" for her outstanding devotion in per- forming a job well done. (2) RESOLVED: WHEREAS, in the year since the last convention of the Rocky Mountain Coal Mining Institute, the Institute and the coal mining industry have suffered the loss through death of the services of:

Jan 1, 1976

By Hongling Wang, DI WU, Shuai Li, Hui Shu

Isothermal reduction experiments on carbon-bearing pellets of copper slag were investigated by the thermogravimetric method with biomass carbon as a reducing agent. The results indicated that the reduction process of copper slag‑biomass composite pellets was dominated by gas phase diffusion, and the apparent activation energy was 88.44 kJ/mol. In the temperature range from 1000 to 1200 °C, the metallization rate of pellets increased with increasing temperature, and the maximum metallization rate was 78.4%. The optimal reduction temperature of CSBCP (copper slag-biomass composite pellets) was 1200 °C.

Nov 23, 2022

Particles finer than 10 um often cause problems in flotation. The current under- standing of the nature of the following effects is discussed: slime coatings on particles, carrier flotation, increased froth stability, entrainment of ultrafine gangue, excess reagent consumption, slower rate of flotation, more reactive surfaces. The review emphasizes the principles underlying these effects rather than details of progress in practical solutions to the problems they cause. The princi- ples of selective flocculation and floc flotation and the various approaches to achieving selectivity are discussed. Hydrodynamic effects on floc growth are reviewed. The evidence suggests that satisfactory performance in the ultrafines fraction will be achieved only by simul- taneously increasing the rate of flotation of the ultrafine valuable mineral and de- creasing the rate of entrainment of ultra- fine gangue.

Jan 1, 1984

By A Frydrychewicz, J. Mirza, J. Lipkowski

The objective of this work was to understand the mechanisms of action of additives, such as thiourea, that enhance gold leaching in thiosulfate solution. The leaching reaction and surface passivation were investigated using linear sweep voltammetry. Leaching currents were determined using analysis of current-potential curves and the mixed potential theory. The gold-electrolyte interface was further characterized with surface enhanced Raman spectroscopy. The results show how thiourea prevents formation of oxysulfur compounds, which passivate the gold surface. Other molecules such as 3- m ercaptopropionic acid and L-cysteine were also studied as possible additives to prevent passive layer formation.

Jan 1, 2011

THOSE MARKED THUS * ARE MEMBERS, MARKED THUS ?ARE ASSOCIATES. THESE SIGNS DOUBLED INDICATE LIFE MEMBERS AND ASSOCIATES RESPECTIVELY. THE FIGURES AT THE END OF THE ADDRESS INDICATE THE YEAR OF ELECTION. HEAVY-FACED TYPE SIGNIFIES HONORARY MEMBERSHIP. *AARONS, J. BOYD, Vivian Gold Mining Co., Ltd., Harris, West. Australia. '05 *ABADIE, EMILE R., Cons. and Min. Engr., 214 Union Savings Bank Bldg., Oakland, Cal. '76 ?ABBÉ, MAX F., Prest., Abbé Engineering Co, 220 Broadway, New York, N.Y. '07 ? ABBÉ, PAULO., Secy.,Abbé Engineering Co., 220 Broadway, New York, N.Y. '07 *ABBOTT, AI ARTHUR Morococlia, Peru, So. America. '95 *ABBOTT, CLARENCE Chief EDgr., Iron Mines, Dic Tennessee Caol, Iron & R. R. Co., Bessemer, Ala. '04 *ABBOTT, JAMES W., Min. Engr: Ploche, Lincoln Co., Nev. '94 *ABE, MASAYOSHI, Prof. of Mining, Imperial University Kyoto, Japan. '05 ? ACKER, E. O'C., Supt., Treatment Dept., Bethlehem Steel Co., So. Bethlehem, Pa. '86

Jan 1, 1910

By H. Rush Spedden, A. M. Gaudin

IN the belief that a critical study of its operating problems might be a sound investment, the Cuban American Manganese Corporation initiated an ore-treatment research in cooperation with the Massachusetts Institute of Technology One of the early objectives of this research naturally became the relationship of the microscopy of the Cuban ores of the Corporation to their flotation treatment The operations in Cuba have already been described by F S Norcross, Jr 7 and the laboratory study of manganese oxide flotation goes back a number of years 4 Broadly speaking, the difficulties encountered in the flotation of manganese ores are that the consumption of reagents is extremely high, the concentrate contains more silica than is desirable and the tailing losses are relatively high An appreciable betterment on any of these scores would achieve a definite betterment in costs, quantity of minable ores, and quality of product The microscope study discussed in this paper was made on samples from the Quinto mine, from the Ponupo mine, and from mill products at various stages of passage of the ore through the mill The writers have had access to Company records and in particular to the petrographic studies made on thin sections of ore by the late Professors R J Colony and Philip Krieger, of Columbia University They acknowledge their debt to both of these men for the help derived from the reports Manganese oxides are black, friable, smudging It is therefore, very difficult to judge operations by inspection The mineralogy of manganese compounds seems to be confused, and the authors believe that many more minerals have been described than actually exist Much of this difficulty is due to the prevalence of the structural conditions that will be discussed further in this paper, namely, the porosity and the friability of the ores, and the extremely intimate association of minute manganifeous mineral crystals with impurities of various sorts By all odds the most important manganese mineral in Cuba is the one that in this paper is called "psilomelane " The name "psilomelane" has been used in so many different ways that the choice of it for this ore may not be approved by all However, it seems to be the best under the circumstances This mineral accounts for about 97 per cent of the manganese in the ores of the Quinto and Ponupo mines and in the mill feed The remaining odd 3 per cent consists mostly of pyrolusite together with minor amounts of other manganese oxide minerals DESCRIPTION OF PSILOMELANE Aggregate Structure In grains or lumps, psilomelane has a characteristic fibrous appearance and seems

Jan 1, 1942

By M. Suzuki, M. Dobashi, M. Kahata, T. Yoshida

Almost 30% of steel in Japan is produced by electric arc furnace (EAF) treatment of iron scrap. EAF dust includes approximately 20 wt % of Zn and 3- 5 wt % of CI and is treated by the pyrometallurgical processes to recover Zn as Zn oxide. Direct hydrometallurgical processing is one of the most effective methods to recover high purity Zn. In this case, CI in the EAF dust is dissolved in the liquid phase by leaching, and the CI anion in electrolyte attacks anodes which are commonly made of a lead base alloy. Several processes have been proposed to remove CI anions from acidic sulfate solution. In this study, an electrolytic process was examined to eliminate CI anions from Zn sulfate electrolyte. From our study it can be said that the elimination rate of CI anion depends on the anode material ( i.e., the elimination rate is Pb-Ag alloy == Pb > DSE== Pt). In industrial Zn electrowinning process, the electrolyte contains Mn, which means the influence of Mn should be considered in the elimination of Cl. Mn dioxide deposition on an anode plate reduces the efficiency of CI removal. A periodical reverse current electrolytic system was examined to prevent this efficiency decrease, and deposited Mn dioxide could be removed very rapidly when the current is reversed. More than 95% of CI anion could be removed by this method in a shorter period than direct current method.

Jan 1, 1997

By Brunno Spinelli Pimentel

Ambientes contendo H2S e CO2 impõem condições severas a componentes fabricados em aços, já que estes podem sofrer corrosão com perda de propriedades mecânicas e falha das instalações. Uma preocupação é a quantificação dos fenômenos envolvendo difusão do hidrogênio atômico, o qual (seja pelo gás H2 em interfaces ou pela interação com ligações atômicas ou discordâncias) pode causar redução nas energias superficiais de fraturamento prejudicando ductilidade e tenacidade. Neste cenário, este trabalho investiga a fragilização por hidrogênio em um aço microligado API 5L X65 sour obtido de um tubo de diâmetro externo 32” e espessura de parede 20,6 mm fabricado pelo processo UOE. Amostras longitudinais e transversais de tração (ASTM E8/E8M) foram extraídas e imersas em solução saturada com H2S. O eletrólito empregado foi a solução A (ácido acético contendo cloreto de sódio) da norma NACE TM0284-2011, fazendo-se purga com N2 e injeções de H2S. Os tempos de imersão foram de 0, 96 e 360 horas, sendo os ensaios de tração realizados após doze dias do término da imersão. Os resultados não revelaram efeito estatisticamente relevante na resistência mecânica, na evolução tensão-deformação e tampouco no módulo de tenacidade. Entretanto, foi observado maior espalhamento dos resultados advindos de amostras submetidas a H2S. Esse comportamento sugere que o hidrogênio influenciou no micromecanismo local de fraturamento, mas com inexpressivo comprometimento das propriedades monotônicas macroscópicas. Tal desempenho pode ser fruto da microestrutura com grãos refinados e do baixo nível de inclusões encontrado, indicando poucos e uniformes sítios de ancoramento de hidrogênio irreversível.

Aug 8, 2018

Crystalline silica is the scientific name for a group of minerals composed of silicon and oxygen. The term crystalline refers to the fact that the oxygen and silicon atoms are arranged in a three-dimensional repeating pattern. This group of minerals has shaped human history since the beginning of civilization. From the sand used for making glass to the piezoelectric quartz crystals used in advanced communication systems, crystalline silica has been a part of our technological development. Crystalline silica's pervasiveness in our technology is matched only by its abundance in nature. It's found in samples from every geologic era and from every location around the globe. Scientists have known for decades that prolonged and excessive exposure to crystalline silica dust in mining environments can cause silicosis, a noncancerous lung disease. During the 1980's, studies were conducted that suggested that crystalline silica also was a carcinogen. As a result of these findings, crystalline silica has been regulated under the Occupational Safety and Health Administration's (OSHA) Hazard Communication Standard (HCS). Under HCS, OSHA regulated businesses that use materials containing 0.1 or more crystalline silica must follow Federal guidelines concerning hazard communication and worker training. Although the HCS does not require that samples be analyzed for crystalline silica, mineral suppliers or OSHA-regulated businesses may choose to do so if they wish to show that they are exempt from the requirements of HCS. Because crystalline silica is an extremely common mineral and the HCS will affect many mineral commodities, it is important then, that there be as clear an understanding as possible of what is and what is not crystalline silica, and where it is found and used, and how it is qualitatively and quantitatively identified. This primer is an attempt to accomplish this in as nontechnical a manner as possible. This primer will examine crystalline silica. Part I will describe, in nonscientific terms, what crystalline silica is and how we come in contact with it. Part" will discuss the regulatory decisions that have created new interest in this ancient and widespread substance and will present a nontechnical overview of the techniques used to measure crystalline silica. Because this primer is meant to be a starting point for anyone interested in learning more about crystalline silica, a list of selected readings and other resources is included. The detailed glossary, which defines many terms that are beyond the scope of this publication, is designed to help the reader move from this presentation to a more technical one, the inevitable next step.

Jan 1, 1992

By E. K. Stanek

This report contains results of two major efforts related to electrical transients on mine electrical power systems. The first area concerns the use of digital computers to model mine electrical power systems and predict transients or duplicate field recordings of transients. Two existing general purpose circuit analysis programs were used. The first was the TRW Engineering System Simulator or TESS. The second was Electronic Circuit Analysis Program or ECAP. TESS proved to be superior to ECAP in several important characteristics, including system size limitations and modeling nonlinear elements. The second major topic covered in this report is the evaluation of commercially available surge suppression devices. These devices were found to be quite acceptable and guidelines for the selection and placement of surge suppressors were included. The final important item is a listing of the worst-case transients, from a design point of view, for ac and de utilization systems and ac distribution systems.

Jan 1, 1979

By George Fancher, R. L. Whitting

A typical drilling mud from the Hastings oil field, Brazoria County, Texas, containing only 8 per cent (dry basis) of material of colloidal dimensions, which is largely illite, was concentrated to a density of 10.2 lb. per gal. and used in this study. The effects of water dilution, treatment with complex polyphos-phates, temperature and the time of heating upon the rheological properties of the mud were investigated. It was found that water plays an important part in chemical treatment and that sodium acid pyrophosphate and sodium tripolyphosphate were more efficient than other complex polyphosphates for chemical treatment. Muds treated with either of these chemicals manifested maximum reduction in viscosity and minimum filtration rates at low concentrations. Furthermore, .mud treated to minimum viscosity with either of these two chemicals was virtually unaffected by heat-treatment. Introduction The drilling of deep wells is dependent upon the use of drilling mud, and problems frequently arise concerning the effects on mud of temperature, prolonged heating and aging. The use of chemicals to control the rheological properties of mud is a well-established practice. Salts of weak organic acids such as sodium tannate or gallate were used at first until the complex phosphates of sodium were found to be more efficient. Consequently, it seemed important to investigate the reaction of a mud to chemical treatment with phosphates, temperature, heat-treatment and aging, particularly since previous work in the laboratory at the University of Texas had provided the particle-size distribution and mineral composition of Hastings mud. Properties or Mud Used in Experiments A large sample of the mud from a drilling well in the Hastings field, Brazoria County, Texas, was obtained directly from the circulatory system. Some of the general physical characteristics of the mud and other data are presented in Table I. Table i.—General Properties of Hustings Drilling Mud Alex- Cur-ander keet Well Well Depth when sample was taken, It.. 5720 5700 Weight. lb. per gal............... 9.5 0.8 Viscosity, sec. A.P.I.............. 47 60 Viscosity, Stormer, grams......... 80 Viscosity, centipoises............. 13 Filtration rate, c.c. per 30 min.a. . . 19.6 22.8 Salt content (chlorides), per cent... 0.13 0.12 pH............................. 8.9 8.9 The Alexander mud was used for the experimental work. Comparison with Curkeet mud indicates a considerably greater dilution but otherwise suggests similarity. The mineral composition and particle-size distribution of Curkeet mud (Table 2) are available (Fancher and Oliphant6). It is suggested that Alexander mud would have a similar composition.

Jan 1, 1943

By R. L. Whitting, George Fancher

A typical drilling mud from the Hastings oil field, Brazoria County, Texas, containing only 8 per cent (dry basis) of material of colloidal dimensions, which is largely illite, was concentrated to a density of 10.2 lb. per gal. and used in this study. The effects of water dilution, treatment with complex polyphos-phates, temperature and the time of heating upon the rheological properties of the mud were investigated. It was found that water plays an important part in chemical treatment and that sodium acid pyrophosphate and sodium tripolyphosphate were more efficient than other complex polyphosphates for chemical treatment. Muds treated with either of these chemicals manifested maximum reduction in viscosity and minimum filtration rates at low concentrations. Furthermore, .mud treated to minimum viscosity with either of these two chemicals was virtually unaffected by heat-treatment. Introduction The drilling of deep wells is dependent upon the use of drilling mud, and problems frequently arise concerning the effects on mud of temperature, prolonged heating and aging. The use of chemicals to control the rheological properties of mud is a well-established practice. Salts of weak organic acids such as sodium tannate or gallate were used at first until the complex phosphates of sodium were found to be more efficient. Consequently, it seemed important to investigate the reaction of a mud to chemical treatment with phosphates, temperature, heat-treatment and aging, particularly since previous work in the laboratory at the University of Texas had provided the particle-size distribution and mineral composition of Hastings mud. Properties or Mud Used in Experiments A large sample of the mud from a drilling well in the Hastings field, Brazoria County, Texas, was obtained directly from the circulatory system. Some of the general physical characteristics of the mud and other data are presented in Table I. Table i.—General Properties of Hustings Drilling Mud Alex- Cur-ander keet Well Well Depth when sample was taken, It.. 5720 5700 Weight. lb. per gal............... 9.5 0.8 Viscosity, sec. A.P.I.............. 47 60 Viscosity, Stormer, grams......... 80 Viscosity, centipoises............. 13 Filtration rate, c.c. per 30 min.a. . . 19.6 22.8 Salt content (chlorides), per cent... 0.13 0.12 pH............................. 8.9 8.9 The Alexander mud was used for the experimental work. Comparison with Curkeet mud indicates a considerably greater dilution but otherwise suggests similarity. The mineral composition and particle-size distribution of Curkeet mud (Table 2) are available (Fancher and Oliphant6). It is suggested that Alexander mud would have a similar composition.

Jan 1, 1943

By J. W. Sandelin, L. S. Birks

The group five metals, vanadium, niobium, and tantalum all show cold-rolled textures of {100)(011) and {112)(0ll) with a preference for the (100) in vanadium and niobium and for the {112) in tantalum. Recrys-tallization texture of (100) and (111) was reported1 for vanadium after annealing (no temperature stated). For tantal~m ,~ annealing below 1200°C strengthened the (112) texture but the (111) texture increased and was predominant as the annealing temperature was raised to 2500°C. Annealing niobium up to 1100°C strengthened the ( 100) texture and developed a weak (111) texture.' In the present work niobium has been annealed up to 2000°C. Nearly 70 pct of the grains showed {111) texture with only a weak (112) component and an insignificant (100) component remaining. In addition, double-crystal rocking curves were used to follow the increase in crystal perfection of the grains with increased annealing time. Material and Treatment. Samples i by 4 in. were sawed from & -in.-thick cold-rolled niobium sheet obtained from Wah Chang. Chemical analysis of the material showed it to be 99.4 pct pure with tantalum as the major impurity. Individual pieces were annealed for 2, 15, 30, and 60 rnin in a vacuum of 10'* Torr using an rf generator. They were etched until the grain boundaries were well-defined, Fig. 1. Average grain size varied from 1 mm for 2 min annealing to 2 mm for 60 rnin annealing. Experimental Results. Preferred Orientation. The orientations of 97 of the 117 grains in the specimens of Fig. 1 were determined by back-reflect ion Laue patterns. A General Electric 10-cm-diam cylindrical camera was used rather than the conventional flat camera in order to record more of the low-index spots. The method proposed by Forest, Barton, and schieltz4 was used to transform the cylindrical film patterns to standard stereographic projections. Table I gives the compilation of data. Even 2 rnin anneal at 2000°C is sufficient to yield a strong (111) preferred orientation, and the percentage of grains with this orientation increases steadily with annealing time at the expense of all other orientations. Crystal Perfection. X-ray topographs were taken of each specimen in both the (111) and (112) orientation using the method described by Birks and Grant.' As the anneal time increases, the grains become larger and the individual reflections become slightly more uniform in intensity, indicating an increase in crystal perfection. For a more quantitative measure of crystal perfection, it was necessary to measure the double-crystal rocking curve. The spectrometer employed was a Gaertner instrument of Compton design. LiF was chosen for the first crystal because the (400) reflection with d spacing of 1.05 AU is a good match to the (222) niobium reflection with d spacing of 0.95 AU. CuKp radiation was used in order to further reduce the d spacing mixmatch correction.' A variable aperture was placed between the LiF and the niobium specimen so that a single grain or even a small portion of a grain could be examined. Fig. 2 shows typical rocking curves for the four annealing times. For the 2-min specimen, a single peak is observed with 10' of arc full-breadth at half maximum. As the annealing time is increased to 15 or 30 min, several sharper peaks of 40 to 80" breadth can be seen within a single grain. After 60 rnin anneal only a single peak of about 30" is observed. Table I1 shows the corrected rocking curve breadths and the dislocation densities, ND. The latter were calculated from the equation7 where W is the corrected rocking curve breadth at half maximum in radians and b is the effective Burger's vector. For (110)(111) slip in niobium, b is 2.86 AU. Discussion. The annealing of cold-rolled niobium at 2000°C causes rapid preferential growth of grains with {ill} orientation. After only 2 rnin annealing time, 35 pct of the grains have the (111) orientation, and after

Jan 1, 1968

By M. A. Dayananda, R. E. Grace

Vapor-solid diffusion couples were employed in a study of ternary diffusion in the single-phase copper-rich corner of the Cu-Zn-Mn system Interdiffusion coefficients were measured at three different compositions corresponding to the intersections of diffusion paths determined at 850°C. Intrinsic diffusion coefficients were determined at two compositions by the Philibert-Guy method. New relations between the various intrinsic diffusion coefficients are also presented. MOST of the investigations of ternary diffusion have been made with "sandwich" couples formed by welding together two homogeneous solid solutions with or without markers placed at the interface. With such couples Kirkaldy and his coworkers1,2 have determined interdiffusion coefficients which describe ternary diffusion in the substitutional alloy systems, Cu-Mn-A1 and Zn-Cu-Al. Guy and Leroy3 have reported intrinsic diffusion coefficients for Co-Ni-Cr alloys as a function of composition using the analysis of Philibert and Guy.4 The use of semi-infinite diffusion couples, for example, vapor-solid couples, where the diffusing species are supplied from a vapor source in contact with a diffusion disk, has so far been confined to studies of binary diffusion. Balluffi et a1.5,6 have successfully determined the interdiffusion as well as the intrinsic diffusion coefficients in several binary metallic systems employing vapor-solid couples with markers initially placed at the vapor-solid interface. They have also discussed the general advantages and limitations of such couples. Vapor-solid diffusion couples can successfully be employed in ternary diffusion studies. The importance of such couples in ternary diffusion lies in the fact that inert markers lie close to the vapor-solid interface, and the composition of the marker plane is virtually known before experimentation begins. Another minor advantage is that the method of Philibert and Guy4 may be used with three alloys instead of four. Lastly, the diffusion paths need not be S-shaped, as pointed out by Meijering7 for "sandwich" couples. The Cu-Zn-Mn system is convenient for ternary diffusion studies because of the large single-phase field in the copper-rich corner. The vapor pressure of zinc above such alloys is known, and X-ray measurements indicate that the molar volume is nearly constant over a wide range of compositions.8,9 It is the purpose of this paper a) to extend the analysis of Balluffi and seigle5 to permit an evaluation of interdiffusion coefficients in ternary vapor-solid couples, b) to use the method of Philibert and Guy to determine intrinsic diffusion coefficients with such couples, and c) to present experimental data on both interdiffusion and intrinsic diffusion coefficients for the Cu-Zn-Mn system at 850°C. INTERDIFFUSION IN TERNARY VAPOR-SOLID COUPLES The analysis of Balluffi and seigle5 is extended in this section to a vapor-solid couple where two solutes diffuse from a vapor source into a ternary solid solution. To take into account the expansion of the diffusion disk caused by the absorption of mass from the vapor phase, the total fluxes are expressed on the basis of a coordinate system that moves with the velocity of the vapor-solid interface; thus. where D3ij are the intrinsic diffusion coefficients,4 v(x, t) is the local Kirkendall velocity of mass flow, and F(t) is the negative velocity of the vapor-solid interface (x = 0). Both these velocities are based on a fixed coordinate system far removed from the diffusion zone. Using the continuity relations and Darken's method1' for a ternary system in which components 1 and 2 diffuse from the vapor phase into a solid of negligible vapor pressure, one obtains

Jan 1, 1965