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By Ivor Jenkins

PROCESSES employing controlled atmospheres in the heat-treatment of metals and alloys are now well established on an industrial scale, and the general principles involved and the advantages to be gained in the use of the technique have received considerable publicity over a period of years. During this time the greatest emphasis has been on the establishment of the process in industry, the main effort being devoted to development work on various types of atmospheres, their useful fields of application and the design of suitable heat-treatment furnaces in which they are to be used. The various types of controlled atmospheres are fairly well standardized, but there still remains a considerable field for the investigation of related problems, in connection with both the gas-generating equipment and the surface chemistry of the heat-treatment of metals, especially in complex controlled atmospheres. This paper describes certain investigations of this nature that were carried out in England up to 1939. The development of processes employing controlled atmospheres has been associated to a very large extent with the heat-treatment of steels, both because of the major importance of steel in industry and the many diverse and difficult problems of surface chemistry involved when steels of such a wide range of composition are heated in the presence of active gases Controlled atmospheres such as dissociated and burnt ammonia or charcoal gas are used in the heat-treatment of low-carbon and high-carbon steels, but from certain points of view a suitable atmosphere generated by the partial combustion of city gas is to be preferred. Both the ammonia derivatives are comparatively expensive, and even if the burnt ammonia is regenerated, thereby reducing operating costs, the capital expenditure of the gas plant may make it prohibitive for the smaller type of furnace installation. Charcoal-gas generators are not without their operating difficulties: especially those associated with the quality of the charcoal, clinker formation and the removal of carbon dust from the generated gas. City gas has the advantage of being comparatively cheap and "on tap" in most if not all industrial centers. The use of raw city gas as a protective atmosphere in the heat-treatment of steels has been described,1 but it presents certain difficulties because of its complex composition and its explosive nature when mixed with air. These factors, together with the tendency toward sooting at elevated temperatures, arising mainly from the hydrocarbon gases present, all militate against its use as a protective atmosphere in industrial furnaces. The following analysis, based on the analyses of city gas in different localities in Great Britain, indicates the wide limits existing

Jan 1, 1947

The First Conference of the Powder Metallurgy Committee convened in the East Foyer of the Hotel Waldorf-Astoria, New York City, at 9:45 a.m., on Feb. 21, 1944, Mr. John Wulff, General Chairman, presiding. THE CHAIRMAN.-In behalf of the American Institute of Mining and Metallurgical Engineers I welcome all members and guests to this conference on Powder Metallurgy. We hope that this meeting will give expert and novice in the field a chance for discussion. Unfortunately, the subject has been overemphasized by some, and, of late, severely criticized by others. We have here today powder producers, fabricators, and engineers of different viewpoints, who can make the meeting a success. Such success depends not only on the caliber of the papers presented but more so on the discussion. To give you time for a free exchange of views, the papers have been shortened purposely. With the hope that you will all benefit by this conference, I shall turn the meeting over to the Chairmen of the morning session, Mr. Roland P. Koehring, of Moraine Products Division of General Motors, and Dr. R. K. Waring, of the New Jersey Zinc Company. SESSION ON DESIGN FACTORS IN POWDER METALLURGY R. P. Koehring and R. K. Waring presiding The opening paper of the session was presented by Mr. Fred P. Peters, as follows:

Jan 1, 1945

By Robert B. Hoy

If the reader finds that the basic information in a commodity chapter is insufficient, he can consult the appropriate sources in this chapter to find more detailed or more up-to-date information. In these days, technology develops so rapidly that this 5th edition will be somewhat out of date even by the time it is distributed. A comparison of this edition with the 4th edition (1975) of Industrial Minerals and Rocks will clearly demonstate how rapidly the scene changes. One of the best sources of new information, of course, is attendance at technical meetings. For example, the papers presented at the national and sectional meetings of AIME usually discuss new developments in the respective divisions of the society. Frequently this information is available in Preprints. In addition some are printed in Mining Engineering and/or the Transactions of the Society of Mining Engineers of AIME. Furthermore, other professional and trade journals contain articles pertinent to the field. A journal introduced in 1967, Industrial Minerals, published by the Metal Bulletin, Ltd., London, is an excellent source of information. The Mining Journal, Ltd., also in London, publishes a weekly journal, a Mining Magazine (monthly), and a Mining Annual Review. The latter covers the field from three aspects: (1) by commodities, (2) through technical developments, and (3) geographically. The Industrial Minerals Directory 1977, 1st ed., Metal Bulletin Books, Ltd., London, provides addresses of organizations in the field. Other useful magazines and periodicals include Engineering and Mining Journal, Pit and Quarry, Rock Products, and World Mining, all published in the United States. In addition many new books related to industrial minerals have been published since the 4th edition of Industrial Minerals and Rocks. Most of these are included in the bibliography of each chapter in this volume. Another excellent information source is the proceedings of the Forum on Geology of Industrial Minerals. This group, which held its 18th annual meeting in 1982, is sponsored by a state geological survey or another mineral agency on a rotational basis. The proceedings have been published by the various sponsors and are available as indicated in Table 1. Two major sources of basic industrial mineral and rock data in the United States, and also a good source for many foreign countries, are the US Geological Survey and the US Bureau of Mines. The two agencies publish many reports and maps on a variety of geological and mining subjects. In addition, each agency has an indexed list of all their publications with a free service announcing new publications: New Publications of the Geological Survey, US Geological Survey, 329 National Center, Reston, VA 22092 and New Publications-Bureau of Mines, Publications Distribution Branch, US Bureau of Mines, 4800 Forbes Ave., Pittsburgh, PA 15213. The US Bureau of Mines (USBM) publishes annually Minerals Yearbooks which provide statistical data on mineral products including production, consumption, imports and exports, as well as information on new developments. Another very useful USBM series is called Mineral Facts and Problems. Editions were published in 1960, 1965, 1970, and 1975. Four major series of publications by the Bureau are Information Circulars, Reports of Investigations, Mineral Trade Notes, and Minerals and Materials. The last two are particularly good for news of foreign developments. The Bureau of Mines Employee Directory, available at all USBM offices, lists addresses and telephone numbers for all offices as well as same for all commodity and area specialists.

Jan 1, 1983

By Thomas Brownfield

Development and production activity in Oklahoma during the year 1940 was of routine nature. Production, according to the Corporation Commission's figures, averaged 409,100 bbl. daily as compared with 421,000 bbl. for the year 1939. Discoveries were of minor importance except for the Cumberland pool in Marshall and Bryan Counties, in the southern part of the state. Maintenance of a relatively stable producing rate is attributable to the drilling of new wells and the recompletion of many old wells in the previously established producing areas. During the year 1785 new wells were drilled, a decline of approximately 10 per cent as compared with the previous year. Of the wells drilled, 962 were oil wells with a combined initial production of 241,000 bbl. daily, 172 were gas wells having aggregate capacities of 1205 million cu. ft., and 651 were dry holes. Wildcat activity increased 20 per cent over 1939 and 227 such wells were completed during the year; that isl 43 oil wells, 16 gas wells, and 168 dry holes. In addition to the new work completed, 603 wells were recorded as having been drilled deeper or plugged back to test new horizons; included were 334 producing wells with total initial production of 65,000 bbl. daily, 37 gas wells with initial aggregating 305 million cu. ft., and 232 abandonments. Footage drilled amounted to 4,730,000 ft., an average of 2650 ft. per well as com-pared with an average depth of 2600 ft. recorded the previous year. The principal new pools discovered as a result of the exploratory drilling were Cumberland; East Cromwell, in Okfuskee County, and Prague, in Lincoln County. At the end of the year Cumberland had 13 completed wells, which averaged 700 bbl. initial through tubing from the Simpson Bromide formation (Ordovician) at 4750 ft. East Cromwell had 10 wells with average initial of 435 bbl. in the Cromwell sand (Pennsylvanian) at 3460 ft. Prague had II wells with an initial average of 220 bbl. from the Senora sand (Pennsylvanian) at 3260 ft. There were notable extensions to the Dill pool, Okfuskee County, and to the Hewitt pool, Carter County. At the end of the year, 19 producing wells had been drilled in the former, with initials averaging 1000 bbl., and 63 wells averaging 150 bbl. daily in the latter. There were no notable changes in the policy of State conservation authorities with respect to proration. The Bureau of Mines recommendations for the year averaged 413,000 bbl. daily; the State author-ities fixed allowables at an average of 406,000 bbl. daily, while, as noted above, production averaged 409,100 barrels. The most important development in the older areas occurred in the following pools: Billings.—Seven oil wells with an average initial production of 2500 bbl. and two dry holes were completed during the year. Production from the Simpson horizon averaged 6025 bbl. daily as compared with 5950 the previous year. Production from this field has been almost steady since reaching its peak early in 1937. The major portion of the pool is efficiently operated as

Jan 1, 1941

By Thomas Brownfield

Development and production activity in Oklahoma during the year 1940 was of routine nature. Production, according to the Corporation Commission's figures, averaged 409,100 bbl. daily as compared with 421,000 bbl. for the year 1939. Discoveries were of minor importance except for the Cumberland pool in Marshall and Bryan Counties, in the southern part of the state. Maintenance of a relatively stable producing rate is attributable to the drilling of new wells and the recompletion of many old wells in the previously established producing areas. During the year 1785 new wells were drilled, a decline of approximately 10 per cent as compared with the previous year. Of the wells drilled, 962 were oil wells with a combined initial production of 241,000 bbl. daily, 172 were gas wells having aggregate capacities of 1205 million cu. ft., and 651 were dry holes. Wildcat activity increased 20 per cent over 1939 and 227 such wells were completed during the year; that isl 43 oil wells, 16 gas wells, and 168 dry holes. In addition to the new work completed, 603 wells were recorded as having been drilled deeper or plugged back to test new horizons; included were 334 producing wells with total initial production of 65,000 bbl. daily, 37 gas wells with initial aggregating 305 million cu. ft., and 232 abandonments. Footage drilled amounted to 4,730,000 ft., an average of 2650 ft. per well as com-pared with an average depth of 2600 ft. recorded the previous year. The principal new pools discovered as a result of the exploratory drilling were Cumberland; East Cromwell, in Okfuskee County, and Prague, in Lincoln County. At the end of the year Cumberland had 13 completed wells, which averaged 700 bbl. initial through tubing from the Simpson Bromide formation (Ordovician) at 4750 ft. East Cromwell had 10 wells with average initial of 435 bbl. in the Cromwell sand (Pennsylvanian) at 3460 ft. Prague had II wells with an initial average of 220 bbl. from the Senora sand (Pennsylvanian) at 3260 ft. There were notable extensions to the Dill pool, Okfuskee County, and to the Hewitt pool, Carter County. At the end of the year, 19 producing wells had been drilled in the former, with initials averaging 1000 bbl., and 63 wells averaging 150 bbl. daily in the latter. There were no notable changes in the policy of State conservation authorities with respect to proration. The Bureau of Mines recommendations for the year averaged 413,000 bbl. daily; the State author-ities fixed allowables at an average of 406,000 bbl. daily, while, as noted above, production averaged 409,100 barrels. The most important development in the older areas occurred in the following pools: Billings.—Seven oil wells with an average initial production of 2500 bbl. and two dry holes were completed during the year. Production from the Simpson horizon averaged 6025 bbl. daily as compared with 5950 the previous year. Production from this field has been almost steady since reaching its peak early in 1937. The major portion of the pool is efficiently operated as

Jan 1, 1941

NEW MEMBERS The following list comprises the names of those persons who became members during the period Mar. 10, 1916 to Apr. 10, 1916. ALLEN, P. R., Pres., McAlester Coal & Coke Co., Knight Templar Bldg., McAlester, Okla. BERNARD, CLINTON PERCIVAL, Min. Engr., Care Forminiere Mission Kasai, Tschikapa, Congo Belge, W. Africa. CARPENTER, GEORGE 0., Vice-Pres National Lead Co. St. Louis Mo. CLARK, WILLIAM ANDREWS, JR., Min. Engr., Pres., Elm Orlu Mining Co., Butte, Mont. CLAYTON, CHARLES YANCEY, Asst. PrOf. of Metallurgy and Ore Dressing, Missouri School of Mines, Rolla, Mo. COHEN, JULIUS MILTON, Mgr. Croesus Gold Mines, Ltd., Matheson, Ont., Canada. CRAMER, WILLIAM BRONSON, Met. at Concentrator, Old Dominion Copper Min. & Smelt. Co., Globe, Ariz. DAHL, SIMEON H., Mill Supt., Messina Transvaal Dev. Co., Messina, Transvaal S. Africa.

Jan 5, 1916

By Jerry G. Rose, Robert C. Howell

This paper addresses a process by which both the disposal and utilization of preparation plant coal refuse can be simultaneously accomplished with an attendant benefit of significantly increasing the percentage of extractable coal. A laboratory study is described in which coal refuse was successfully utilized as an aggregate in low cost concrete (coal-crete) mixes under simulated mine environments. Coal-crete specimens with compressive strengths of 14 000 kPa (2000 psd were consistently produced. A construction sequence and mining plans are offered for placing the low-cost coal-crete pillars in accessible areas in room and-pillar mines so that a substantial portion of the remaining coal pillars could be extracted. The method could be applicable in areas where mining procedures do not permit pillar extraction because of possible surface subsidence, roof problems, or other conditions. Possible structural difficulties with the coal-crete pillar support system are discussed. Using a discounted cash flow analysis, the economic feasibility of mining with the coal-crete pillar system is investigated. The cost of the system is compared to the cost of a mining system which would have less coal recovery. The analysis indicates that although at higher coal selling prices the coal-crete mining system may yield an acceptable rate of return, the alternative of leaving the coal pillars is more attractive at the present time.

Jan 1, 1980

By Robert E. Thurmond

DISCOVERY of a commercial ore deposit has resulted from a program emphasizing geophysical techniques and concentrating upon exploration of alluvial-covered areas. United Geophysical Co. selected these areas as offering the best possibility of success, for here the surface evidence of ore deposits has been hidden from the eyes of prospector and geologist alike. Pima mining district, Pima County, Arizona, was selected for initial exploration. The project was successful in that a commercial ore deposit was discovered and proved through drilling and extensive underground development. A limited region of activity was chosen and library research was begun on available economic and regional geological publications relating to the mining districts. Field reconnaissance of those districts which seemed to hold exploration possibilities provided a general picture and ascertained the existence of alluvial-covered areas of interest. At the conclusion of the reconnaissance trips all data obtained were compiled, and the district which seemed to present the best exploration possibilities was selected by statistical methods. The statistical summary was based on the following considerations: Geological Factors: 1—type of intrusive, P—presence of favorable host rocks, 3—apparent intensity of mineralization, and 4—presence of favorable structure in covered or unexplored areas. Economic Factors: 1—past production from district or mine; 2—size, shape, grade, and type of ore deposit in the district; 3—ease of acquiring mineral rights; and 4—general development facility. Exploration Favorability Factors: 1—results to be anticipated from geological methods alone; 2—application of geophysical methods, namely, topographic conditions, surface interference, depth-size relation, physical property contrasts as related to ores or controlling structural features; and 3—drilling factors. Admittedly, many of these, factors do not lend themselves to absolute evaluation, but relative evaluation, subject to inaccuracies of personal judgment, is always possible. A relative scale from 1 to 10 was established for every factor, representing varying degrees of favorability. For each district a numerical evaluation of each factor was established and a numerical total determined. The obvious advantage of this scheme is that a more concise summation can be presented by numerical means than can be achieved by descriptive means. After a district had been selected as favorable, the first step was to carry out more detailed geological and economic studies to narrow down the areas of interest. The second step was to compile all available geological data from publications and add to these data by mapping where necessary. Geological interpretation and projection of structural or other control into covered or unexplored areas was made whenever logical. To determine the possibilities of geophysical application and to select a geophysical method, physical property contrasts were related to mineral assemblages and/or structural control. If geophysics seemed applicable, trial profiles were run crossing the area normal to the strike and spaced

Jan 1, 1955

By E. L. Bruce

The district of Patricia, in the province of Ontario, lies northwest of the Albany River and extends northward to Hudson Bay. Formerly this was the unorganized district of Keewatin, the southern part of which was divided in 1912 between the provinces of Manitoba and Ontario. The interprovincial boundary now runs north from Lake of the Woods for 275 miles and thence northeast 375 miles to Hudson Bay. This district is comparable in size to all the older part of Ontario south of the Canadian Pacific Railway east of Lake Huron—thus it is roughly one-third of the whole of the present provincial area. The central part of this great triangle is one of the least accessible parts of Canada. From it streams flow southward to the English River, southeastward to the Albany, northward to Hudson Bay and the Hayes River, and westward to Lake Winnipeg. None of the streams is large and canoe travel is not easy. The only industry it has ever had is the trade in furs. Until the development of the airplane on a commercial basis, the only means of travel was by canoe or dog-train. There is not a mile of railway in the whole district. The two areas to be dealt with lie in the southwestern part of Patricia. Red Lake is 50 miles east of the Manitoba boundary and 75 miles north of the transcontinental railway from Cochrane to Winnipeg. Woman Lake is 50 miles farther east and slightly farther north. The late Dr. D. B. Dowling, of the Geological Survey of Canada, visited Red Lake and spent some time there during his exploration survey from Lac Seul to Berens River in 1893. He also visited the Woman Lake basin during the same journey, but his examination of it was much less detailed, the great area covered by him during the one field season making it impossible to make more than a hurried reconnaissance. Some prospecting in the Red Lake district followed Dowling's exploration, but the distance from railway was too great for any systematic work to be done. In 1922, following the usual plan, the Ontario Department of Mines made a geological reconnaissance of the English River, following :in instrumental survey of that river and its lakes by the Department of Lands. A side trip was taken to examine the rocks of Red Lake described

Jan 1, 1928

By P. H. Wendland

Calculations are presented for the design of a silicon photodiode in which the incident light beam makes multiple passes between the detector surfaces. Total internal reflection is used for this "light-trapping" effect. By this means, the optical path length can be extended to several millimeters, while the electrode separation remains less than 102 cm, as required for nanosecond response time. Data are presented for a Schottky barrier photodiode constructed on a multiply reflecting silicon base wafer. It is shown that the long-wavelength response is considerably extended in such structures without a corresponding sacrifice in high-speed response. The development of efficient and powerful lasers at 1.06 p has stimulated interest in detectors which operate at this wavelength. In typical silicon photodiodes, for detecting 1.06 p radiation, the requirements for high speed and high sensitivity are mutually exclusive. Since the absorption coefficient is only 25 cm-', a lo-'-cm path length is required to absorb 92 pct of the incident 1.06 p radiation. If the electrode separation is greater than 10 cm, however, the carrier transit time will be greater than 1 nsec. This problem can be solved by allowing the incident light beam to make multiple passes between the electrodes. The optical path length can then be extended to several millimeters, as required for complete absorption, while the electrode separation remains less than 10' cm, as required for nanosecond response time. In a typical photodiode geometry, one ohmic contact and one rectifying contact are formed on the two opposite surfaces of a base wafer, and the wafer thickness determines the electrode separation. The objective of the multiple reflection design is to allow all 1.06 p radiation to enter the detector front surface and to form the back detector surface so that no 1.06 radiation can exit. Total internal reflection at the back detector surface is well-suited for light trapping of 1.06 p radiation because the relatively large dielectric constant of silicon leads to a critical angle of 16.5 deg for total internal reflection. LIGHT TRAPPING It is well-known that, as light passes from one medium such as air into another medium such as glass or silicon, the angle of refraction is always less than the angle of incidence. In the limiting case, where the incident rays approach an angle of 90 deg with the normal, the refracted rays approach a fixed angle +, beyond which no refraction is possible: this is called the critical angle. It follows from Snell's law that where = critical angle, n - index of refraction of air, n' - index of refraction of the medium. Applying the principle of reversibility of light rays, all internal angles of incidence greater than +, will produce total internal reflection and "light trapping". The index of refraction of silicon at 1.06 p is 3.5,' and the critical angle is thus 16.5 deg. Fig. 1 shows these relationships for silicon. This very small critical angle in silicon is significant because all incident angles between 16.5 and 90 deg will produce total internal reflection and "light trapping". This effect can be implemented with a "prismlike" geometry, so that incident light can be introduced into the sample without loss and "trapped". PHOTOSIGNALS A precise knowledge of the absorption coefficient at 1.06 in silicon is of critical importance to the design of fast and efficient silicon photodiodes for 1.06 radiation. Dash and newman2 show a value of 25 cm-l, and our measurements have corroborated this value. Assuming that the collection of photoinduced minority carriers is perfect, the quantum efficiency of a photodiode is dependent only on the absorption coefficient. It then follows from Lambert's law that where QE is the quantum efficiency in pct, a is the absorption coefficient, d is the optical path length, and the reflectivity at the surface is assumed to be completely suppressed by an optical interference layer. Fig. 2 gives the maximum quantum efficiency for 1.06p radiation of a silicon photodiode with optical path length d, using Eq. [2]. The ultimate response time of a fully depleted photodiode to an incident light pulse can be considered to be the arrival times of all photoinduced carriers at the contacts, i.e., the minority carriers at the junction interface and the majority carriers at the oppo-

Jan 1, 1968

By R. Bakish, M. A. Badiali, N. W. Kirshenbaum

One pound of ultra pul-e molybdenum has been produced containing both metallic and nonmetallic impuvities close to or less than the limits of detection. various purification methods were investigated; althouglz the use of move than one purification step was consideved, it was found that a single, caefully-controlled sublimation of MoCl5 yielded a highly puvified product without prior treatment or recourse to repeated sublimation. Hydrogen reduction of MoC1, to metal was attempted at atmospheric pressure; however, reduced pressure was necessary to obtain substantial yields. The tubular deposits of metal were consolidated into bulk fovm by electron beam melting undev high vacuum yielding a very low gas content. Boblems involved in monitoring the puvity of these materials and analytical results obtained are also presented. THE pronounced effect of even trace amounts of impurities upon fundamental properties of materials is well known to metallurgists and solid-state physicists. Consequently, groups interested in basic studies of metals have in recent years immensely stimulated the preparation and production of numerous ultra-pure metals. Increased demand by scientists for these high purity materials has necessitated development of facilities to prepare them in significant quantities; the procedures reported here were devised to produce significant quantities of ultra-pure molybdenum. Previous work performed in the field of vapor phase purification and hydrogen reduction of several other refractory metal chlorides had demonstrated valuable techniques applicable to molybdenum.' Various purification and reduction steps were individually investigated. Those procedures which showed the most favorable results with respect both to attainment of high purity and to ease of operation were then incorporated in the process utilized to produce the metal.' STARTING MATERIALS It is well known that because of differences in volatility, chlorides may be separated by fractional distillation. It was presumed that distillation of molybdenum pentachloride offered a simple and straightforward method of purification due to its relatively low boiling point. Alternatively, sublimation of the solid chloride also appeared feasible since MoC15 has both a reasonably narrow temperature range in which it exists as a liquid (a property typical of refractory metal chlorides) and a low enthalpy of sublimation. Pertinent thermochemical data of MoC15 are given in Table I. It should be noted that this compound must be handled with care as it is extremely hygroscopic. Anhydrous MoC15 was obtained from the A Metal Climax Co. METHODS OF PURIFYING MOLYBDENUM PENTACHLORIDE Distillation. It was expected that distillation methods, while affording an efficient purification, would prove simple to control and would have a higher production rate than sublimation processes. Also considered was the possibility of effecting a high degree of purification by using both these volatilization methods in conjunction—possibly a distillation followed by sublimation of the solidified condensate. Distillation of MoC15 was investigated using a single stage distillation column packed with chemically resistant glass beads. Heating coils were wound around the column and collection tube (condenser). As-received MoCl5 was charged into a flask connected with the column using a side loading arm under an argon flow. After the column and condenser were brought to about 270" and 210°C, respectively, the apparatus was lowered until the flask was fully immersed in a constant temperature fused salt bath maintained at about 285 °C. Distillation was continued for about 10 or 15 min until 50 to 70 g of distillate had been collected. Analyses of these distillations indicated that several elements, e.g., Cu, Fe, Ni, Cr, and Mg, were lowered in quantity although not all were removed to the same extent. The occurrence of Na, B, Si, and A1 in the distillates appeared to be due to contamination, possibly from corrosion of the pyrex glass. An improved distillation system of larger capacity and longer distilling column was built. Improvements were effected in lowering the amounts of such impurities as B, Mn, Ni, Na, Mg, Cr, Cu, and Fe. These studies were pursued concomitantly with efforts to purify by sublimation; it was subsequently found that although improvements in purity were obtained by distillation, sublimation processes were simpler to control and effected a high degree of purity.

Jan 1, 1963

By J. L. Lamon, W. Crafts

Study with the electron microscope of the carbides in vanadium-chromium-molybdenum steels after tempering up to 1000 hr at 600 teelsto 1400°F confirmed that alloy carbides are formed at the secondary hardening temperature by decomposition of the plate-like iron carbides. It was also demonstrated that vanadium carbide persists as much smaller particles than do chromium- or molybdenum-bearing carbides. Conditions conducive to the formation of fine vanadium carbides are indicated to be favorable for high temperature strength. IN order to determine the effects of long exposure at high temperatures on vanadium-bearing steels, a survey has been made of their hardness and carbide structure. The behavior of carbides in the tempering of martensite was studied by X ray diffraction and electron microscope examination of electrolytically extracted residues in greater detail than in an earlier investigation.' A group of steels with about 0.25 pct carbon and containing chromium up to 5 pct, molybdenum up to 1 pct, and vanadium up to 1 pct was either quenched or annealed and then tempered for peri- ods of up to 1000 hr at 600° to 1400°F. Their hardness after tempering agreed with the Hollomon and Jaffe2 relation of equivalency of time and temperature, and with the degree of secondary hardening predicted from composition. Further, the appearance of the carbides indicated that the time and temperature equivalency relation was also applicable to the degree of carbide development. The mechanism of the tempering of martensite was demonstrated more clearly than in the earlier study. It was confirmed that carbides develop from martensite as poorly defined plates of the Fe2C type carbide followed by thickening of the plates with a transition to Fe,C. Finally the plate structure deteriorates into a lacy mass from which alloy carbides emerge as chunky particles that grow slowly with further increase of tempering temperature. Vanadium carbide derived from tempered martensite was found in characteristically small particles that tended to grow very slowly. The addition of chromium or molybdenum to a steel with predominant vanadium carbide tended to introduce carbides of a chromium- or molybdenum-bearing type having a somewhat larger particle size. The Cr,C, type carbide particles were larger than those of the V,C, type and somewhat smaller than the carbides in steel containing both Cr,C and M,C. Similar observations were made of the carbides in the pear lite of annealed steels. It appeared that high temperature properties would be benefited by the retention of the fine carbide particles that result from a balance of composition and heat-treatment designed to produce a maximum amount of vanadium carbide. Procedure: The steels used in the investigation were made with a base of Armco iron in a high-frequency furnace at the Union Carbide and Carbon Research Labs., Inc. The steels were deoxidized

Jan 1, 1951

By T. R. Graham, R. G. Feustel, J. R. Long, R. S. Dean

The comprehensive study of the copper-manganese-zinc alloy system in the Bureau of Mines Laboratories has so far been principally concerned with alloys that lie within the alpha solid solution field of the system. Two regions, one centering about 65 per cent copper, 10 manganese and 25 zinc, and the other centering about 70 per cent copper, 20 manganese, 10 zinc, have been carefully examined. These have indicated that when the alloys are made with electrolytic manganese considerable amounts may be readily introduced and that the strength and hardness are increased without excessive losses in ductility. In the course of the work of establishing the limits of the alpha solid solution range,3 enough of certain of the alloys was prepared to permit determination of their- physical properties at a future date. The 60 per cent copper alloys concerned here are part of that series. They cross through the alpha field and into the adjacent alpha plus beta and alpha plus X fields, and are of interest because they offer some information on the effects of manganese on alloys lying in these fields. Composition and Fabrication of Alloys The chemical composition of the alloys involved is given in Table I. They were intended to contain 60 per cent copper with manganese increasing from 5 to 25 per cent in 5 per cent steps and zinc decreasing from 35 to 15 per cent. The analyses are so close to the intended composition that the alloys mill be referred to hereafter by their norninal compositions. They were finished into sheet by cold-rolling and intermediate annealing procedurzs calculated to produce sheet $i6 in. thick, cold-reduced by 20, qo, 60, and 80 per cent in thickness. Physical properties were determined on standard flat tensile specimens with 4-in. gauge length, although the test gauge section used was 2 in. The properties were obtained on cold-worked material and on material annealed at temperatures ranging from 700' to r500°F. after 60 per cent cold reduction. Since an annealing temperature of 1200°F.

Jan 1, 1946

By J. R. Long, T. R. Graham, R. G. Feustel, R. S. Dean

The comprehensive study of the copper-manganese-zinc alloy system in the Bureau of Mines Laboratories has so far been principally concerned with alloys that lie within the alpha solid solution field of the system. Two regions, one centering about 65 per cent copper, 10 manganese and 25 zinc, and the other centering about 70 per cent copper, 20 manganese, 10 zinc, have been carefully examined. These have indicated that when the alloys are made with electrolytic manganese considerable amounts may be readily introduced and that the strength and hardness are increased without excessive losses in ductility. In the course of the work of establishing the limits of the alpha solid solution range,3 enough of certain of the alloys was prepared to permit determination of their- physical properties at a future date. The 60 per cent copper alloys concerned here are part of that series. They cross through the alpha field and into the adjacent alpha plus beta and alpha plus X fields, and are of interest because they offer some information on the effects of manganese on alloys lying in these fields. Composition and Fabrication of Alloys The chemical composition of the alloys involved is given in Table I. They were intended to contain 60 per cent copper with manganese increasing from 5 to 25 per cent in 5 per cent steps and zinc decreasing from 35 to 15 per cent. The analyses are so close to the intended composition that the alloys mill be referred to hereafter by their norninal compositions. They were finished into sheet by cold-rolling and intermediate annealing procedurzs calculated to produce sheet $i6 in. thick, cold-reduced by 20, qo, 60, and 80 per cent in thickness. Physical properties were determined on standard flat tensile specimens with 4-in. gauge length, although the test gauge section used was 2 in. The properties were obtained on cold-worked material and on material annealed at temperatures ranging from 700' to r500°F. after 60 per cent cold reduction. Since an annealing temperature of 1200°F.

Jan 1, 1946

PRECEDING chapters on thermochemistry, and the reactions in and between metal and slag phases in the bath of the furnace tend to emphasize the equilibrium or "static" conditions in the furnace and process, such as the total amounts of heat from fuel combustion or from certain bath reactions, the concentration relationships between slag and metal at the steady state for certain reactions, and the like. Such data are obtained essentially by means of the logic of thermo- dynamics, which helps to determine the energy change between initial and final states in a process as well as to define its equilibrium or steady-state condition, but which is not concerned with the rate of change in the process or with the mechanisms or path followed between initial and final states. These questions of just "how it works" and "how fast" belong to the kinetic aspect of any process; their answers are helpful in speeding up or slowing down and thus controlling intelligently its operation, and also to understand certain natural limitations which are especially important in many high-temperature processes. The kinetic aspects of interest here comprise mainly (1) the flow of gases through the furnace system, (2) the flow of heat in the system, and (3) the mechanisms and rate factors in the various chemical reactions. A really adequate discussion of the first two subjects would require at least three or four times the space available here; it has been tried, therefore, in this and the next chapter to outline but a few fundamentals necessary to an intelligent approach and to indicate some of the conditions of heat and gas flow more or less peculiar to the open hearth, since several good general discussions on these subjects may be found in the literature.(1) For the designer of open-hearth furnaces, the principles of gas flow are of paramount importance.(2,3,4,5) They are also important to the operation of the process, however, at least to the extent of a general qualitative picture of the movement of gases in the system, which is all that is attempted here.

Jan 1, 1944

By Keith Leonard Sutherland

This paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate-free.14 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. Purity of Reagents The xanthates were purified in the usual manner.' Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes, This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. Results The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the "absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1943

By Keith Leonard Sutherland

This paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate-free.14 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. Purity of Reagents The xanthates were purified in the usual manner.' Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes, This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. Results The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the "absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1943

By J. R. Cooper, A. Bruynesteyn

The final results of the operation of the Cananea test dumps are discussed. Scale-up factors between shake-flask tests, column tests and the large test dumps are established for the Cananea ore. The formation of clay layers, which formed inside the dumps and markedly affected extraction, as well as secondary enrichment, are discussed.

Jan 1, 1974

By M. Kitada, U. Kawabe, F. Ishida, T. Doi

The relations between micros tructures and critical current density in transverse magnetic field were experimentally investigated due to each transformation of the 0 to 0' + P" phases at 700' C for superconductmainly examined using replication electron microscopy. The ß' or a precipitates were found to pin down magnetic flux lines in these alloys. The effects of precipitation upon the critical current density were discussed in relation with the size, spacing, and characler of these precipitates. HIGH magnetic field superconductors, such as Nb-Zr, Nb-Ti, and Nb-Zr-Ti alloys, have been recently put to extensive practical use as winding materials for superconducting magnets.13 The critical current density of these hard superconductors under an applied magnetic field is an important characteristic for magnet materials and is very sensitive to metallurgical structure. It is generally known that the critical current density is increased by introducing dislocations and precipitates into a superconductor; that is, dislocations and precipitates are presumed to be barriers that hinder quantized flux lines from moving.4'5 Theoretical6'7 and experimental analyses of the motion of flux lines and the interaction between flux lines and various defects have already been reported by many authors. Metallographic analysis of high magnetic field superconductors such as Nb-Zr and Nb-Ti is difficult, so that no quantitative relationship between microstruc-ture and critical current density has been established yet. In this paper, the effect of precipitation on the critical current density in magnetic field was investigated for two superconducting alloys, Nb-40Zr-10Ti and Nb-5Zr-60Ti. In these alloys the resistive critical field H, at 4.2oK was about 100 kG and the critical current density Jc at 80 kG was of the order of 104 amp per sq cm.13-l5 The superconducting properties were examined in relation to the microstructural changes due to transformation of i) the ß to ß' + ß" phases at 700°C for Nb-40Zr-10Ti alloy and ii) the ß to a + ß phases at 500°C for Nb-5Zr-6OTi alloy. The effect of size, spacing, and character of precipitates on flux line pinning was in particular examined. The microstructures were studied by means of residual resistivity, microhardness, and tensile strength measurements as well as by X-ray diffraction, optical, and replication electron microscopies. I) EXPERIMENTAL PROCEDURE Pure niobium, zirconium, and titanium, in the form of rods 0.8 cm in diam, served as raw materials. Results of chemical analyses of these rods are given in Table I. Ingots of the alloys, 0.4 cm in diam and 3 cm in length, were prepared by means of levitation melting, utilizing a copper mold in an argon-gas atmosphere. Samples from the ingot then were cold-worked by grooved mill to 0.2 cm in diam, heat-treated homogeneously (in the ß phase region) for 5 hr at 1100° in a vacuum of 1 x 106 Torr, and finally cold-drawn to 0.025 cm in diam. For heat treatments, samples were wrapped in niobium foil and sealed in an argon-gas atmosphere in fused quartz capsules. Water quenching was done after each heat treatment. Subsequently H-J, were performed at 4.2° by slowly transporting the current through the samples 4 cm long, under transverse magnetic field, until the least detectable resistive terminal voltage was observed. The resistive critical field H, was taken as the field at which 100 pv appeared at 4.2°K across a sample 3 cm in length, with a current of 5 ma. The critical temperature T, was measured by means of a conventional four-probe resistivity technique and taken as the temperature at which the sample resistance reached one-half of full restoration of the normal-state resistance with a current l ma flowing through a sample 2 cm in length. Precipitates were observed by means of optical microscopy and carbon replication electron microscopy. The etching solution consisted of 5 ml HF, 10 ml H2SO4 10 ml H2O2, and 50 ml H2O, and shadowed carbon replicas were examined in a itachi HU-11 electron microscope operated at 50 kv. X-ray diffraction photographs were taken by a 11.46-cm-diam Debye-Scher-rer camera using copper Ka radiation. The micro-hardness was measured under a load of 200 g using

Jan 1, 1969

By F. D. Hoyt, H. L. Hartman

The development of new processes and methods by The Pennsylvania State University to improve slate quarrying technology has centered in recent years on cutting and sawing stone in the quarry to eliminate a second cutting process in the mill. Two machines exhibit promise for this work: 1) a circular saw mounting diamonds or hard inserts to produce smaller sizes of stone and 2) a chain saw with insert cutting teeth to produce stone in the larger dimensions. Prototype machines have been constructed and tested in several Pennsylvania slate quarries, and one commercial installation has been operated for several months with a circular diamond saw. Other kinds of dimension stones may be cut by these saws. Research at Penn State has begun to study the fundamental cutting action of rotary tools or saws in slate and other dimension stones. A laboratory drill press is being instrumented to permit thrust-torque-rotational speed us penetration rate studies of single tooth cutting surfaces on stone. Machinability studies of slate conducted with tungsten-carbide inserts have been performed. The dimension stone industry generally accepts the rather basic premise that the larger the block removed from the quarry, the more practical and economical the operation. Thus, the concept of cutting to size any dimension stone while it remains in place in the parent bed would receive little consideration from the majority of members of the industry. However, the slate industry, which is usually considered a separate member of the dimension stone family, is pioneering in the development of an in-place sawing method. Before any final decision can be reached concerning a proposed new system, it is essential to take a long, hard look at the present method of operation in order to determine if the new system is indeed an improvement or even desirable. In the following section is a brief description of present quarry practice in the slate quarries of eastern Pennsylvania. PRESENT METHOD OF QUARRYING SLATE In the numerous slate quarries of Lehigh and Northampton Counties of Pennsylvania, the grain and cleavage of the slate are most often at right angles to each other; if a third surface is broken at right angles to these two natural planes of weakness, blocks of more or less rectangular shape can be separated.' In conventional quarrying a large calyx core drill prepares holes of 36-in. diam in which wire-saw standards are positioned. By wire sawing between strategically located core-drill holes, large sinks or benches of virgin slate are opened up. The sides freed by wire sawing will vary from quarry to quarry but generally are rectangular in shape with dimensions averaging 20 ft in length and about 15 ft in depth. Some quarries are fortunate in having a joint or natural parting to work to, which of course diminishes the amount of core drilling and wire sawing required. Once the various benches have been developed either through wire sawing alone or through a combination of wire sawing and natural jointing planes, the block removal proceeds in the following manner. A plug hole is drilled in the block with a compressed-air hammer and a feathering chisel is inserted in the hole to cause a fracture of the rock either with or against the grain as indicated by the positioning of the so-called feathers. This operation is referred to as sculping. After a block has been freed with and against the grain by means of wedging from the cross fracture with long bars or levers, the block is further freed along the cleavage plane by shimming it up with small wooden pieces in an operation known as styling. A large steel loading chain is wrapped around a block thus freed and the chain is attached to the wheel of an overhead cable. The block is then hoisted vertically to the cableway and moved along this cableway laterally to the lip or edge of the quarry. From here it is unloaded onto a rail car or truck for transportation to the processing mill. Except for occasional blasting to free stubborn blocks,

Jan 1, 1961