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By J. L. Fitch, B. G. Hurd

The presence of gypsum in samples subjected to standard core analysis introduces serious errors in the measurement of water saturation and porosity. The magnitude of these errors, depending upon the type of analysis procedure used, has been evaluated experimentally and theoretically. Water-saturated pore volumes determined by vacuum distillation or retort procedures may be too high by as much as 48 per cent of the volume of gypsum present. The maximum error in this value determined by Dean-Stark extraction with toluene is 36 per cent of the gypsum volume. If pore space is measured by a Boyle's law type porosimeter the maximum erorr due to gypsum is 38 per cent of the original gypsum volume present. The conscientious core analyst may eliminate the errors caused by gypsum by either of two methods. He may apply suitable corrections for the water of crystallization removed from gypsum, or take special precautions to prevent dehydration of gypsum during core cleaning and alzalysis procedures. These alternatives are discussed and methods for obtaining reliable core analysis data are proposed. Gypsum (CaSO4 . 2H2O) occurs as a common mineral in many of the world's sedimentary basins. In addition to its presence as primary bedded evaporitic deposits, it is often found as secondary replacement zones and pore-fillings in host rocks. That it may cause false indications in porosity, both on neutron logs and in standard core analysis, has been generally recognized. False porosity interpretations from neutron logs result because the chemically bound water in gypsum attenuates neutrons as effectively as free water. Errors in core analysis result when gypsum is dehydrated prior to or during the analysis. Vacuum retort procedures used by many laboratories to determine fluid saturation and porosity effect a complete removal of water of crystallization from gypsum. The crystal water, distilled and collected with free water from the sample, is counted as water-sat11rated pore space. Dehydration of gypsum results in a decrease in volume occupied by calcium sulfate and a corresponding increase in pore volume. Thus, if gypsum is dehydrated by sample cleaning and drying procedures, subsequent porosity measurements with gas expansion or compression instruments will be high. The qualitative effect of gypsum on porosity determinations by retort procedures was discussed in a recent article by Bynum and Koepl3. They concluded that since false porosity was interpreted as being water saturated, determinations of oil content were not affected. Others in the industry, however, have pointed out that porosity values are often used with values of water saturation determined independently, e.g., from electric resistivity logs in making reserve estimates. Values of water saturation calculated from the formation resistivity using the Archie equation, S4= are actually low if values of are high due to gypsum. In this case, false porosity values due to gypsum could cause serious errors in calculations of oil-in-place. This investigation was made to determine quantitatively the effect of gypsum on porosity values determined by different core analysis procedures. EXPERIMENTAL PROCEDURES Dehydration of Gypsum The extent and rate of removal of water of crystallization from gypsum under conditions encountered in core analysis procedures were studied. Taken for the experiments were three types of relatively pure, naturally occurring gypsum, viz. selenite, satin spar and massive gypsum. Although all samples probably contained trace chemical impurities, each type lost the theoretical amount of water upon complete dehydration. An automatic recording thermobalance, similar to one described by Mauer2, was used to obtain dehydration rate data for samples heated in dry air. Water

By James T. Gow, Oscar E. Harder, Anton de S. Brasunas

THIS paper deals with the results obtained and the techniques employed in determining: I. Liquidus and solidus temperatures of the HH and HT type heat-resistant alloys. † 2. The relation of true temperatures (thermocouple) to apparent temperatures (optical pyrometer) for the molten HH and HT type alloys. This work was the outgrowth of needing to know something definite about these temperatures in order to study the effect of pouring temperatures, shake-out times, and heat-treatments on the properties of some heat-resistant alloys. The information developed is thought to be of interest to industry for guidance in foundry practices and the industrial heat applications of the alloys. This paper is based upon work that has been done for the Alloy Casting Institute at Battelle Memorial Institute. LIQUIDUS AND SOLIDUS TEMPERATURES OF HH AND HT TYPE ALLOYS Experimental Procedures Temperature-time curves were obtained during the cooling and solidification of several HH and HT type alloys. The metal was melted in an Ajax high-frequency induction furnace and poured into a coresand mold for cooling. The temperature measurements were obtained by means of a platinum, platinumrhodium thermocouple contained within a fused silica sheath, which was extended through the side wall of the dry core-sand mold to a point at about the center of the mold cavity, which was 3 in. in diameter by 5 in. deep. The cold junction of the thermocouple was kept in an ice bottle, and the temperature was recorded automatically on a direct-reading potentiometer recorder. Through a switching arrangement, the temperature recorded was checked occasionally with a portable Leeds and Northrup potentiometer indicator. Less than a 5°F. variation in the two instruments was always found. This is within the limit of accuracy of readings. The thermocouple used was checked for accuracy against a standard couple, both before use on this work and after completion of the work, by the instrument laboratory. Temperature-time Cooling Curves Fig. I is an enlarged reproduction of a part of one of the cooling curves over the temperature range of 2600° to 2200°F. for an alloy of the HT type with 0.45 per cent carbon, 16 per cent chromium, and 36 per cent nickel. This is a typically shaped cooling curve as obtained for the alloys. It will be noted that two temperatures are shown on Fig. r for the liquidus temperature. It is thought likely that the higher temperature, A, at the point at

Jan 1, 1945

By S. Zaman, F. F. Aplan, Franklin T. Davis

This section deals with the oxides of heavy metals, namely, columbium and tantalum, rare earths, chrome, manganese, titanium, tin, and tungsten. Table I contains the production figures for each of these commodities in the US and in the world in 1977. Specifications for concentrates are also summarized as well as prices for concentrates in 1977. In each chapter an attempt has been made to describe the more common commercial mineral involved with the commodity and the processes used to recover and concentrate the minerals, as well as geographical areas where these processes are utilized.

Jan 1, 1985

By T. B. Braun

Cathode contamination is the principal factor affecting the quality of electrorefined copper. It is commonly accepted that annealability is unfavorably affected by the following elements, in decreasing order of adverse effect: tellurium, selenium, bismuth, antimony, and arsenic. Silver in cathodes has importance as it represents a nonrecoverable loss of silver to the refinery. Mechanisms for the contamination of cathodes by these elements are examined and the effect of operating variables on contamination, including anode composition, electrolyte composition, electrolyte temperature, addition agent practice, and electrolyte discard rate, are discussed.

Jan 1, 1976

By Hugh O?Neill

IN PREVIOUS papers,1 the author has reported the results of experiments on the straining in tension of a single crystal test piece, about 0.6 in. long, of vacuum-melted electrolytic iron containing 1.8 per cent. of silicon. The crystal was originally in the "as cast" condition, and was stressed slowly along a tetragonal axis so that slipping along conjugate gliding planes finally transformed the original cylindrical portion into a pair of fracture wedges. One of these fracture wedges was sectioned along the stress axis in a plane at right angles to the edge of the wedge. A metallographic study of this plane of -section led to the conclusion that slip had taken place in the (111) direction along (112) planes making a V shape with the stress axis. The present paper describes the results of scratch-hardness tests conducted on the same section, in order to determine the distribution of strain hardness therein, followed by annealing, and considers the resulting variations in hardness. These observations supplement those made by Krivobok2 on similar material reduced 25 per cent. by hammering (i. e., by impact) in the cold. In order to investigate ageing effects, two small crystals of the same alloy were also tested.

Jan 1, 1928

By G. W. Murrie

A geologic study of the Mary Lee Group of coalbeds in the Black Warrior coal basin was undertaken to examine coal stratigraphy and determine regional trends and extent of the coalbeds. The area investigated encompasses 835 square miles in Jefferson, Walker, and Tuscaloosa Counties, Ala. More than 700 core logs were used to construct a structure map, coal, interval, and overburden isopachs, and cross sections. There is evidence that structure affected sedimentation. Coalbed isopachs indicate the Mary Lee Group was deposited in fluvial-deltaic and low-lying coastal plain environments. The Mary Lee coalbed is the only coalbed which is continuous throughout the area, commonly with two benches which have a combined thickness of 2 to 12 feet. The Mary Lee coalbed changes rank in the basin from high-through medium-to low-volatile coal. The methane gas potential of the Mary Lee Group coals is estimated to be greater than 1 trillion cubic feet. There is an excellent correlation between the orientation of surface cleats with those measured underground in the Mary Lee coalbed. The face cleats roughly parallel the axes of the area's folds and trend northeast-southwest.

Jan 1, 1976

SINCE 1900, five underground fires of consequence have beenrecorded in the Broken Hill mines. These occurred at the Junction(1906), Proprietary (1906 and 1916), Block 14 (1906), and Centralmines (1923). All have been extinguished, but at an enormouscost; e.g., in the eleven months following on the 1923 Central mine fire the sum of £187,123 was expended in fire-fighting operations.To this series may be added others, as the South (1925) and British mine (1918) fires, which were extinguished before serious damage had resulted. All, however, have occurred within a period of 28 years, and in a district where spontaneous combustion, a prolific source of fire in the U.S.A., has been practically nonexistent. Therefore, definite fire risks exist in the underground workings of the Broken Hill mines, and, as a consequence, an active fire prevention policy is a necessity...

Jan 1, 1929

By Frank Wright

"The Icon Sullivan Joint Venture ore deposit was discovered in June, 1965 by Messrs. Paul Benard, Bob Galipeau and Mac Watson working under the direction of Mr. Andrew J. Troop, as employees of the Icon syndicate. The deposit is located on the Waconichici River as the south end of Baie du Poste of Lake Mistassini, approximately 45 miles north of Chibougamau. Property acquisition and Winkie drilling was followed by a diamond drilling program to evaluate the deposit. Stripping of the open pit area connnenced in the late fall of 1966 and the first test sample of ore was shipped to Chibougamau in December of that year.Regular ore shipments to the mill of Merrill Island Mining Corporation Limited for concentration commenced May 25, 1967. Production to December 31, 1970 amounts to 42,960,000 pounds of pay copper.The ore is chalcopyrite in white quartz dolomite, and it contains a very small amount of precious metals. The quartz dolomite assumes a flat to gently dipping attitude and is associated with a graphitic argillite contact zone on both hanging and footwall sides, in dolomitic limestone rocks. There is practically no other sulphide present in the ore.During the summer of 1969 a series of pre-concentration tests were completed and a Wemco heavy media sink float plant was installed in late 1969 and early 1970. This pre-concentrator eliminates at least one third of the ore mined in the form of barren quartz dolomite prior to ore shipment by truck to the concentrator in Chibougamau."

Jan 1, 1971

By Alexander Field

The hot-rolling properties of a series of high-sulfur steels are described. From a consideration of the sulfur, manganese, and zirconium contents of these steels, it is shown that zirconium reacts with the sulfur content of molten steel in accordance with the equation Zr + 2S = ZrS2. Zirconium disulfide appears in the finished state as gray-colored inclusions, similar to manganese sulfide in plastic behavior and general appearance. Zirconium completes its act of deoxidation before proceeding to combine with sulfur and indirectly increases the effective sulfur-combining power of any manganese which may be present. IN A previous paper,1 the experimental methods used and some of the results obtained in an extensive investigation of steels containing zirconium were described. The present paper considers in greater detail one of the most interesting of these effects, namely, the elimination of "red shortness" and the occurrence in steel of a compound of zirconium and sulfur. A consideration of the actual percentages of zirconium, manganese, and sulfur in numerous steels in the light of behavior during rolling has led to new conclusions of the most practical import regarding the reciprocal relationships of these elements. The microscopic examination of high-sulfur steels containing zirconium has also been productive of interesting results. Before discussing the experimental data in question, it may be stated, briefly, that the reaction between zirconium and sulfur in molten steel may he represented by the simple equation, Zr + 2S = ZrS2, and that the zirconium sulfide thus formed occurs in the finished steel in the form of gray-colored inclusions, closely resembling manganese sulfide and, like the latter, exhibiting plasticity at rolling temperatures. Molten steel containing zirconium retains such a negligibly small amount of oxygen in solution that the foregoing reaction goes to completion.

Jan 2, 1924

By Tim Avery, Steve Klein, Mark Schmoll

Tunnel boring machine (TBM) performance in hard rock is highly dependent on the geologic conditions, including the type of rock and hysical properties like the rock strength, hardness, and the spacing of the fractures. This paper examines TBM performance relative to the geologic conditions and rock mass properties at four recent TBM-bored tunnels in California.

Jan 1, 1995

By Lawrence L. J

The Australian Broken Hill Consols Mine, situated some 600 yd east of the main Broken Hill line of lode, is noted for its rich ores of silver. In contrast to the vast conformable orebodies of the Broken Hill field, the Consols lode occupies a narrow fissure dipping to the south west at angles increasing from 240 through to vertical and transgressing the strike of the metamorphosed country rock at an oblique angle. This feature, together with the abundance of calcite and siderite and the virtual absence of silicate minerals in the gangue, has led to its classification as an orebody of the Thackeringa type (King, 1953). Recorded production during the period 1890 to 1903 is given as 845,000 oz of silver and 20 tons of lead.The unusually rich silver values of the Consols lode were concentrated at the intersection of the fissure with beds of amphibolite, whereas in the adjacent schists and gneisses the lode became markedly impoverished. From the surface to a depth of some 120 ft extensive surface oxidation had occurred, resulting in the breakdown of siderite and its replacement by limonite and associated manganese oxides.Silver halides, dyscrasite, acanthite and partly oxidised tetrahedrite were the main silver minerals in this zone. With increasing depth the lode material gradually reverted to minerals representative of the hypogene zone.The only previous work specifically on the mineralogy of the Consols lode is that by Smith (1922), one time manager of the mine. His zeal as a mineral collector resulted in much valuable information being available on the distribution of the minerals. More recently, Garretty (1943) noted the...

Jan 1, 1962

By A J. Falconer

Two magnetic parameters are proposed as a basis for the assessment of ironsands beneficiation. The parameters are determined for raw sand prior to dredging and for magnetic separator head feed over a production period of five months. The relationships between these parameters and the performance of the magnetic separators are examined to establish the value of magnetic assessment compared with the traditional soluble iron assay method. The results illustrate that the first parameter, true magnetic fraction (TMF). Has a value superior to that of soluble iron when relating raw sand grade calculated by triangulation to magnet performance. In terms of the relationship between magnet head feed grade and magnet performance, TMF and soluble iron perform equally as assessment parameters. For the ironsands mined during the five month period, the second magnetic assessment parameter, composite fraction (CF), is shown to merely reflect TMF and offers no additional information for assessment. Conclusions are that true magnetic fraction has many advantages over soluble iron in terms of time and cost of determination and that it is a meaningful and reliable parameter upon which to base all calculations relating to the mining and beneficiation of ironsands.

Jan 1, 1980

By R. H. Colquhoun

"INTRODUCTION The Holt-McDermott Mine is wholly-owned gold mining operation of American Barrick Resources Corp. that begun operations in June 1988.The property is located 0.5 km. south of Highway 101 East in the Harker-Holloway Townships of Northeastern Ontario, 7 miles south of Lake Abitibi and 15 miles west of the Quebec-Ontario border.Employees of the operation travel daily from various communities in the area, predominantly from Kirkland Lake, Ont., which is located 65 km. to the southwest.The significance of the operation is that it is the first full scale operation associated to the Oestor-Porcupine Fault to go into full production in recent history as well as the first Carbon-in-Leach (CIL) operation in the province owing to the natural occurring carbonaceous ores that are associated to the ore body and the geological fault systems.GEOLOGYThe Holt-McDermott deposit is located in the Abitibi Greenstone Belt, a short distance west of the Ontario-Quebec border. Ore grade material follows the footwall contact of a fault zone known locally as the McKenna Fault, which is thought to be a splay off of the Oestor-Porcupine Fault, itself a major feature in the Abitibi belt.The McKenna Fault strikes approximately east-west (as does the Oestor-Porcupine) and dips to the south at sixty-five to seventy degrees. The fault lies within a package of mafic volcanic rocks (basalts). These rocks have been strongly altered and mineralized adjacent to the McKenna Fault, and the resulting lens-like ore bodies constitute the mining targets."

Jan 1, 1989

An intensely sheared and mineralized zone occurs in the quartz dolerite greenstone (or younger greenstone) mass on the western limb of the Kalgoorlie syncline. This zone comprises the western part of the Golden Mile and has produced the greater part of the 33,000,000 oz of gold produced to date from the main mining belts. A study of the general geological and structural features suggests that the lode shear system will continue southward on a pitch similar to that of the main syncline. Although payable ore has been found recently further to the south, the expectation of large quantities extending southward from the present mining areas is problematical.INTRODUCTIONUntil the late 1930's the principal mining activities in the western lode system were centred on three major ore-shoots formed on the No. 4, No. 3 and to a lesser extent on the No. 2 lode shears (Fig. 1). With the gradual reduction of grade in depth on these main ore shoots, increasing attention was paid to the "Minor Lode" system of lode shears known to exist in the same area. A large quantity of payable ore was found on these "Minor Lodes" particularly in the central part of the mining area. In recent years more attention has been given to exploration in a southerly direction.ROCK TYPES AND STRUCTURESThe western system occurs on the western flank of a dragfolded, south pitching syncline. The rock succession consists of Black Flag sediments overlying the younger greenstone horizon which overlies the fine grained older greenstone horizon. The axis of the syncline is regarded as a tight infold of the overlying Black Flag sediments. This infold has been faulted and intruded by albite porphyry resulting in the formation of a composite body of slates...

Jan 1, 1964

By Gordon E. Agar, Brian Lyons, Gregory H. Styles, William B. Kipkie

"Rock rejection during the flotation of a copper-nickel ore was improved by adding carboxymethyl cellulose to both a rougher and cleaner flotation stage. The selection of the rock depressant was based on laboratory rates studies. Plant operating results are presented which confirm the laboratory selection of two particular brands of carboxymethyl cellulose.The rock assay of the concentrate was reduced from more than 40% to less than 15%.IntroductionThe traditional method of selecting flotation reagents relied upon batch bench scale tests, conducted under arbitrary conditions, to identify the effect of the reagent under examination. Too often these were ""one-off"" tests with little or no regard paid to the reproducibility of the results. Sophisticated researchers used statistical methods to design and evaluate the experiments but they were still obliged to rely on the arbitrary and often unreliable batch tests to generate the numbers that were analyzed statistically. An interesting side-effect of the enhanced sophistication of the statistical analysis was often that no significant effects would be uncovered in a series of experiments that would have generated many positive conclusions and much further experimentation if the same results had been evaluated by the traditional method.In the recent past, at least two groups of researchers a have directed their attention to the reliability of the batch experiments with a view toward improving the reproducibility of the test data. In this work the best of the improvements advocated by both of these groups have been adopted in order to generate kinetic data from batch tests that are as reproducible as possible.The objective of the work was to reduce the rock content of a bulk sulphide concentrate produced at Inco's Shebandowan mill. During 1982 the Shebandowan concentrate analyzed 3.5% Cu, 7.4010 Ni, 25% pyrrhotite and more than 40% rock, which resulted in an MgO content of 10.4%. Besides the expense of shipping all of this rock to Sudbury, the rock also contributed to the poor filterability of the concentrate. On favourable occasions the moisture content of the filter cake was slightly over 20% by weight. The magnesia content of the concentrate was deleterious to the reverberatory furnaces used by Inco for smelting nickel concentrate because the slag viscosity increased as the magnesia content increased, and the nickel lost in the slag went up."

Jan 1, 1987

By Robert S. Sanford

In April 1948, the Bureau of Mines was requested to evaluate the graphite deposit' known as the Benjamin Franklin and Just mines in Chester County, Pa. After preliminary investigation, it was recommended that the Bureau core-drill, trench, and sample the deposit and make beneficiation tests on the ore. During the first and second World Wars, flake graphite was in short supply, and a number of deposits in the United States were exploited. In 1942, the Defense Plant Corporation, through its lessee, the Benjamin Franklin Graphite Co., purchased 70.263 acres of graphite-bearing land and built a complete mining and milling plant with a capacity of 300 tons of crude ore per 24-hour day at a cost of $426,250 (Plancor No. 1254).

Jan 1, 1949

By Abdellah Chlk, Driss Msatef

Sedimentary phosphate ores are known for their relatively high specific surface area and porosity, which have a positive influence on their reactivity when used as fertilizer in acidic soils or in the manufacture of wet phosphoric acid and phosphatic fertilizers. However, these physical properties could have a negative effect on the behavior of these ores if dried. This effect has been studied on several phosphate ores samples by: the determination of mineralogical and textural properties of these samples, the determination of vapor water sorption isotherms, at different temperatures, from which the sorption heat has been calculated, carrying out several drying tests using a laboratory fluidized bed reactor under constant conditions, which showed important differences in drying rates and residual moistures.

Jan 1, 1999

Executive Committee, Board of Directors H D Smith, Chairman, C E Reistle, Jr, Vice-Chairman, T B Counselman, J S Smart, Jr, L F Remartz Finance Committee, Board of Directors A B Kinzel, Chairman, Philip Kraft, P D Wilson Investments Erle V Daveler, '57, Chairman, Henry Krumb, '56, Andrew Fletcher, '58, G F Moulton, ex officio as Treasurer, A B KInzel, ex officio as chairman of the Finance Committee Endowment W W Mein, Jr, Chairman, D H McLaughlin, J V N Dorr, J B Haffner, J R Suman, Henry Krumb, E V Daveler, D C Jackling, Wilfred Sykes, N G Alford, W J Coulter, C E Weed, 0 H Johnson, L F Reinartz, J B Morrow, R McMillan Endowment Fund "X" G F Moulton, Chairman (RIME Treasurer), Erle V Daveler, '58, G I Brigden, '57, Philip Kraft, '56

Jan 1, 1955

By H. S. Gibson

A PROCESS that has come to be known locally as "multistage stabiliza-tion" has been developed in the Haft Kel field of the Anglo-Iranian Oil Co. in southwest Iran, for the recovery of casinghead gasoline. It con-sists in releasing the dissolved gases from the crude by stages, a practice common in many fields, but which, so far as is known, has nowhere been carried to the extent to which it is employed in Iran. It has been in use there for nearly nine years, during which time some 200 million barrels of crude have been handled by the process. This process of gasoline retention consists in preventing the greater part of the casinghead gasoline hydrocarbons (the butanes and pentanes) from ever leaving the crude, instead of allowing them to be vaporized and then recovered from the lighter gases by the usual compression or absorption processes. Its efficiency is fully equal to that obtained by the absorption process; its disadvantage is that it increases the quantities of ethane and propane in the crude sent to the refinery, but with the growing demand for propane this drawback is vanishing. When casinghead gasoline is recovered as a separate liquid in the Iranian fields, it is blended with the crude, as the only outlet is through the refinery, and the crude-oil pipe line offers the cheapest means of transportation. It is under these conditions that the retention of the butanes and pentanes in the crude by multistage stabilization is a most attractive process, possessing as it does the following advantages: (1) extreme simplicity, (2) low first cost, (3) easy installation, (4) practically 100 per cent operating-time efficiency, (5) no operators required, (6) no water or other services required, (7) negligible maintenance, (8) once established, very little routine testing is necessary. The one essential for reasonably efficient multistage stabilization is that the flowing pressures of the wells should be relatively high; i.e., they should not be less than about one-third the saturation pressure of the crude in the reservoir. This is a very general statement, of course, and much depends on the type of crude and its temperature.

Jan 1, 1939

By Edward J. Felten

Binary Cr-A1 alloys containing from 2.5 to 30 wt pct Al and 0.7 wt pct Y were heated in oxygen, air, and nitrogen between 1000" and 1200°C. The reacLivity of the alloys was found to be dependent both on the alloy composition nnd the nature of t he atmosphere. In oxygen, nllojs containing up to 15 to 20 wt pct A1 reacted to produce an external scale of Crz03 and a subscale consisting Predominently of Al203. Alloys contazning 20 to 30 wt pct A1 react in oxygen to produce an A1203 external scale and little m no subscale. The latter alloys were markedly more oxidation resistant than those of low alurninum content. In air, the alloys on which an external Crz03 scale was formed were found to be permeable to nitrogen ns evidenced by the copious amomts of chromium and aluminum nilrides observed ns part of the subscale. The reactizities in nir (or nitrogen) of these alloys increase <m their aluminurn contents increase. However, alloys on which Al,O, us an external scale is formed were nol culnerable to nccelerated attack in air, and no eltldence of nitvide subscnles were observed. For all alloys, yttrium serwed pYimarily to improve oxide adhrence. THE role of chromium in the oxidation resistance of Fe-Cr alloys &apos;-&apos; and that of aluminum in Fe-Cr-A1 al10s&apos; has received considerable attention in recent years. This is understandable since many of these alloys have excellent oxidation resistance due to the formation of either a Cr203 or a-Ala03 film between the metal and the oxidizing atmosphere. Small additions of yttrium or other rare earth metals are effective in preventing spalling of the protective oxide from the metal substrate."" In contrast, little is known regarding the oxidation resistance of Cr-A1 alloys, although some work has been done by Tumarov et a1.&apos; The poor niechanical properties exhibited by Cr-A1 alloys make them undesirable for use as structural components, but their use as coatings cannot be disregarded. The use of chromium-rich aluminide coatings for refractory metal alloys is an example of the potential use of this type of sytem. The purpose of this work is to examine the oxidation behavior of Cr-A1 alloys containing 2.5 to 30 wt pct A1 and 0.7 wt pct Y. The effects of temperature, atmosphere, and thermal cycling have been determined. EXPERIMENTAL PROCEDURE The alloys used in this investigation can be divided into two groups. Those containing 2.5, 5, 7.5, and 10 wt pct A1 and 0.7 wt pct Y were extensively evaluated in the temperature range from 1000" to 1200°C. Alloys containing 15, 20, 25, and 30 wt pct A1 and 0.7 wt pct Y were tested only at 1200°C. All of the alloys were prepared by standard arc-melting techniques in the form of cylinders approximately 4 in. long and 19 in. in diam. Wafers were cut from the cylinders and subsequently subdivided into rectangular coupons. The alloys were brittle and therefore some cracks were found in almost all specimens. The coupons were prepared for oxidation by mechanically polishing through 600 grit Sic paper, and were thoroughly degreased just prior to testing. Two types of oxidation experiments were conducted, namely; cyclic tests in which the specimens were examined and weighed after each 2 hr exposure, and continuous thermal balance tests run in a controlled atmosphere (oxygen, air, or nitrogen) for 20 hr. In the former test the spalled oxide was not included when the specimens were weighed. The physical condition of a specimen was noted visually after each cycle and testing was continued either to failure or until the performance of the specimen was well characterized. Both Micro and Semi-Micro Thermal Balances (Ains-worth) were used in the continuous tests. The oxidized specimens were sectioned and prepared for metal log raphic examination. The specimens were polished through 600 grit Sic paper. After polishing through 6 and l p diamond, a final mechanical polish with Linde B-Alz03 was used. Specimens containing 2.5 pct A1 were etched electrolytically using a 10 pct oxalic acid solution at 4 v for about 2 sec. Selected specimens were examined in the electron microprobe analyzer. Oxide specimens were examined by standard X-ray diffraction techniques. EXPERIMENTAL RESULTS For convenience, the test results have been broken down according to the exposure temperature, and further subdivided according to the type of test and atmosphere employed. Because of the poor quality of the specimens a larger than normal amount of scatter was observed in the measured rate constants. Also, the evaluation of the weight gain data was done on a somewhat arbitrary basis and may not be truly representative. However, the results obtained do show a significant trend in behavior regarding both alloy composition and the nature of the oxidizing atmosphere. I) Oxidation Behavior at 1000°C. A) Continuous Oxidation estsin Oxygen. This series of experiments was run in the Ainsworth Micro-Thermal Balance using pure oxygen at a pressure of 76 mm Hg. Under these conditions all specimens oxidized in accordance with the parabolic rate law over a major portion of the exposure time; the rate constants appear in Table I. The oxide formed externally on all specimens was predominantly Cr,O,, which was generally adherent. In some cases a slight amount of spalling in the form of a fine powder was noted. a-A1203 was observed as a subscale, along with Yz03 in all alloys. Alloys containing up to 7.5 wt pct A1 oxidize more rapidly than the Cr-0.7Y alloy.

Jan 1, 1970