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NEW YORK LOCAL SECTION Executive Committee Louis D. HUNTOON, Chairman ARTHUR S. DWIGHT, Vice-Chairman THOMAS T. READ, Secretary, Woolworth Bldg., New York, N. Y. E. MALTBY SHIPP, Treasurer GEORGE F. KUNZ W. DE L. BENEDICT Meeting, Jan. 16, .1914 A meeting of the New York Local Section of the American Institute of Mining Engineers was held at the Engineering Societies Building, 29 West 39th Street, New York City, Jan 16 1914 the Chairman, -L. D. Huntoon, presiding. Forty members weld present. In the absence of the Secretary, C. A. Bohn was appointed Secretary pro teen. N. H. Darton, Geologist of the U. S. Geological Survey, delivered an address on. The Occurrence of Gas in Coal, illustrated by lantern slides of charts, curves, and tables showing various features of gas occurrences. J. W. Richards, J. T. Beard, W. L. Saunders, L. D. Huntoon, and Mr. Darton participated in the discussion which followed the address. THOMAS T. READ; Secretary.

Jan 3, 1914

B. F. TILLSON,* Franklin Furnace, N. J.-I would like to ask Major Yerkes if he will not give us more examples of the tests than are contained in the printed pamphlet. It would be of great interest to study them more carefully. ROBERT M. YERKES, Washington, D. C.-The reason for not reproducing the methods in any public print is that it lessens their value and necessitates the preparation of new test materials. BRADLEY STOUGHTON, New York, N. Y.-I hope that this matter will be of so much interest to the members of the Institute that the Directors will decide to appoint a committee which can bring further results of this practice before us. I understand that Columbia University, at least in some departments, has already adopted the B and A tests and is using them. I understand that some industries have considered seriously the question of grading their employees in accordance with

Jan 4, 1919

Executive Committee, Board of Directors Grover J Holt, Chairman, C E Reistle, Jr , Vice-Chairman, A W Thornton, A B Kinzel, J L Gillson Finance Committee, Board of Directors Andrew Fletcher, Chairman, R B Caples, Gail F Moulton Investments Erle Daveler, '60, Chairman, Henry Krumb, '59, John Warren, '60, C R Dod¬son, ex off as Treasurer, Andrew Fletcher, ex off as Chairman, Finance Committee Endowment Andrew Fletcher, Chairman, N G Alford, E V Daveler, W J Coulter, J V N Dorr, R B Gilmore, J B Haffner, 0 H Johnson, D H McLaughlin, J R McMillan, L F Reinartz, C E Weed, Wilfred Sykes, J R Suman Honorary Memberships L F Reinartz, Chairman, C E Reistle, Jr , H DeWitt Smith, ex off as Past Presidents of AIMS, Grover J Holt, ex off as President AIMS, P D Merica, '59, Henry Krumb, '58, M L Haider, '60, D H McLaughlin, '61

Jan 1, 1957

By Norman P. Goss

The Chairman.—Thank YOU, Mr. Goss Gentlemen, I believe we have heard one of the finest papers, especially since Mr. Goss has been very generous in his frank discussion of continuous casting. One point he has brought out which 1 think some of us have not thought through to the same extent that he has—that the continuous casting process offers the small producer an opportunity to compete with the larger, more conventional and presumably better established industries. The meeting is now open for discussion. Are there any questions concerning the first two papers? J. A. Malone.*—I should like to ask Mr. Goss whether there is any special problem involved in the first part, the upper part of the mold before he gets to the first graphite lubricant area. N. P. Goss.—You mean in the forming chamber where chilling first takes place? J. A. Malone.—Yes. N. P. Goss.—So far I have not had any trouble in this part of the setup. My only

Jan 1, 1945

DISCUSSION, A. Y. Bethune presiding M. E. Wadsworth and W. M. Fassell (University of Utah, Salt Lake City)—The authors of this paper should be complimented on the experimental techniques they have employed to investigate the rate of solution of galena in sodium hydroxide solution. Studies of this type are important not only as a practical means of leaching normally non-leachable substances, but also to determine the mechanism of solution at the solid-aqueous solution interface. There is some question, however, as to the conclusions which have been drawn by these authors concerning their proposed mechanism. Unfortunately, the contribution of OH- was not definitely established in their work, and concentrations less than 0.5 N NaOH evidently were not investigated. The pressure data at 123°C and 0.5 N NaOH were used to determine pressure dependency and the subsequent model proposed was taken as correct on the basis of the three points presented in Fig. 5 of the paper. In developing the

Jan 1, 1954

By B. Yarar, J. Kaoma

[Introduction The critical surface tension of wetting of hydrophobic materials has been investigated extensively by Zisman et al. (1973) and relates the spreading of a liquid on a solid to the surface tension of this liquid. Thus, the Zisman ap¬proach shows that a plot of Cos 0 versus ?LV where, 0 is the contact angle and ?LV is the surface tension of that liquid in contact with its own vapor at equilibrium, produces a straight line which can be extrapolated to Cos 0 = 1. The intercept corresponds to a given ?LV, termed the critical surface tension of wetting. In instances, however, Cos 0 - ?LV plots show deviations from linearity. Alternative approaches have also included the plotting of adhesion tension (YLV COs 0) versus ?LV that can be interpreted in terms of critical surface tension data (Lucassen-Reynders, 1963). It has, on the other hand, been customary to correlate contact angle (0) with flotation data, although it is recognized that surface inhomogeneities and related contact angle hysteresis limit the interpretations pertaining to solid surface structures purely based on contact angle measurements. It is nonetheless true that 0 = 0, when the liquid is water, corresponds to a hydrophilic solid. Determination of ?c by contact angle measurements in conformity with the Zisman approach can encounter experimental difficulties, especially when solids are in a powder form. Following the reasoning that 0 = 0 corresponds to the hydrophilic state of a solid, froth flotation experiments can be expected to produce critical surface tension of wetting values for powders. The technique that consists of plotting recovery (% R) versus YLV data and extrapolating the linear part of the curve to % R = 0, has been described elsewhere (Yarar and Kaoma, 1984). This paper describes some of the results obtained by the extrapolation technique mentioned above, using various sulfide minerals. Experimental Materials Molybdenite (MoS2), sphalerite (ZnS), chalcopyrite (CuFeS2), chalcocite (Cu2S), and galena (PbS) were handsorted from massive samples and ground by mortar and pestle, and the -147 Fan fraction used in experiments; sulfur (S) was a C.P. Fisher Scientific Co. product. Method One gram powder samples were conditioned for three minutes in methanol-water solutions of predetermined surface tension values and the percents recovered by flotation using a Partridge-Smith Cell (Partridge and Smith, 1972), were plotted against each ?LV value. Results and Discussion The percent recovery versus ?LV for two naturally hydrophobic solids, i.e., natural molybdenite, MoS2 and sulfur are given in Fig. 1 where it is seen that ?c for sulfur is obtained as 31.5 mNm-1 whereas for MoS2, it is 26 mNm-1. Figure 1 also shows that the new flotation technique described, for estimating ?c is in good agreement with the Zisman method. Curves obtained by the same method for the minerals Cu2S, PbS, and ZnS are given in Fig. 2, where it is seen that for Cu2S, ZnS, and PbS, the extrapolation to % R = 0 produces ?c values of 36, 39, and 49 mNm-1, respectively. CuFeS2, on the other hand, gives a curve that does not permit such an extrapolation to obtain a ?c value with certainty. Nonetheless, treatment of the powder with 8.95 X 10-5 molar Na2S solution followed by washing with distilled water prior to flotation effects the curves as shown in the insert of Fig. 2. The type of curves given in Fig. 1 appear to be typical of hydrophobic solids as can also be observed in Fig. 3. The composition of solid and minute quantities of inclusions seem to play an important role as regards the surface properties of solids as reflected by the slope of the linear part of the % R - ?LV plot and thus the value of ?c obtained by this technique. For example, MoS2 of three different stoichiometric compositions produced the data given below. [MoS2MoS2.14Mo1.002S2 ?c mNm-126.029.031.0 dR/d?8.95.23.0]]

Jan 1, 1985

By A. W. Ashbrook

There are essentially three main classifications for extractants: acidic, basic, and neutral. The acidic and basic are also referred to as cationic and anionic, respectively. Some extractants are shown in Table 11-1. Acidic Extractants Acidic extractants which are of use, because of cost and/or insolubility in water, are alkylphosphoric, sulphonic, aliphatic monocarboxylic acids and naphthalene derivatives.

Jan 1, 1978

By Robert Glass Cleland

[PHELPS DODGE COPPER PRODUCTS CORPORATION OFFICE, 40 WALL STREET, NEW YORK 5, N. Y. OFFICERS Whipple Jacobs President Howard T. Brinton Vice-President Edgar P. Dunlaevy Vice-President Weightman Edwards Vice-President S. Allan Jacobs Vice-President]

Jan 1, 1952

By T. Rosenqvist

From the chemical, metallurgical, and mineralogical points of view, the importance of thermodynamic data for metal-sulphides and sulphur dissolved in molten metal has long been realized. Such data will give a basis for thermo-dynamic calculations of processes such as roasting and the distribution of sulphur between molten metal and slags. Furthermore, it will help us understand the chemical forces which tie sulphur to the metal and to the melt. Thermodynamic studies of solid sulphides and the equilibria between solid sulphides and metals have been carried out in a rather large number of cases by several investigators. An excellent review of this work is given by Kelley.1 On the other hand, very little is known about the thermodynamic properties of molten sulphides and of sulphur dissolved in molten metal. The only system which previously has been investigated in this respect is the iron/sulphur system. The purpose of the present investigation was primarily to obtain further data for metalisulphur melts and the system silver/sulphur was chosen, not because this system was expected to be of special interest in itself, but because the silver/sulphur system is a typical example of a metal/sulphur system. Because of the low melting temperatures, the work could be carried out without appreciable furnace and refractory difficulties. The sulphur in this system possesses a rather high escaping tendency compared to most other metal/sulphur systems. By the method employed (reaction with hydrogen to form hydrogen sulphide) this gives ratios Ph2s/Ph2 up to 0.30, which may be determined accurately. 'rhermodynamic investigations of the heterogeneous reaction Ag2S +H2 —+ 2Ag + H2S have previously been carried out by Pelabon,2 Keyes and Felsing,3 Jellineb and Zakowski,4 Wat-anabe,6 and Britzke and Kapustinsky.6 Their results are in rather poor agreement. Experimental Part PRINCIPLE In the present invehgation the escaping tendency of sulphur from the condensed phase was determined by the reaction: S + H2 = H2S The ratio Ph2s/Ph2 is at constant temperature, directly proportional to the escaping tendency of sulphur and to its chemical activity in the condensed phase. (This ratio will subsequently be denoted by H2S/H2.) From this ratio and its variation with temperature and with change in the com- position of the condensed phase, thermodyrlamic quantities such as free energy and heat of reaction can be derived. The apparatus used is shown in Fig 1. The silver/sulphur alloy was placed in a crucible inside a refractory tube and mounted inside the furnace to the left. The tube was a part of a closed, gas-tight system in which the gas mixture could circulate until equilibrium was established. Circulation was maintained by the glass propeller to the right, driven by an external magnet, and promoted by the chimney action of the furnace. The gas passed up through the furnace, down into the crucible where it came in contact with the alloy, passed rapidly up through a narrow tube and out of the hot zone. After equilibrium was established between the gas and the condensed phase, the composition of the gas mixture was determined from its density. In its circulation, the gas mixture passed through a chamber (lower right on Fig 1) containing a buoyancy-balance, where the density of the gas was determined by magnetic balancing. From the measured density,

Jan 1, 1950

[E. E. SCHUMACHER, Chairman ARTHUR PHILLIPS, Past-Chairman L W. KEMPF, Senior Vice-Chairman E. A. ANDERSON, Vice-Chairman H. A. MALONEY, Treasurer FRANK T..SISCO. Secretary 29 West 39th Street, New York 18, N. Y.]

Jan 1, 1946

By AIME AIME

A REQUEST for information as to the details of activities of the Engineering Council was made by the Joint Conference Committee for the benefit of the new American Engineering Council. , This request was complied with, and the scheduled reply so succinctly sets forth the activities of the old Council as well as the scope of possible activities of ,the new Council, about whose efforts there has been much discussion, .that it' is given herewith in full, except the 'budget which is summarized.

Jan 1, 1920

By Russell B. Cornell, William B. Plank

AT the close of the academic year 1940-'41 the largest number of students ever recorded received their first or bachelor degree in the mineral technology schools of the United States. The total of men thus prepared to enter their professional careers in the mineral industries was 1601, a number nearly 12 per cent larger than two years ago and nearly 75 per cent larger than four years ago. Notwithstanding this increase in the number of graduates and as had been predicted in the preliminary report in February, there was a slight decrease in the total student population of the schools in both the United States and Canada. During the college year 1940-'41, 9133 students were enrolled in the 54 schools of the United States and 764 in six of the seven schools of Canada.

Jan 1, 1941

By K. G. Davis, P. Fryzuk

A study has been made of the effect of undercooling on the grain structure and solute distribution in small ingots of pure bismuth and of a 100 ppm Ag in bismuth alloy. Autoradiographic evidence shows that in undercooled melts a network of dendrites is formed throughout the melt immediately after nu-cleation. At large undercoolings the dendrites are very thin and closely spaced. The origin of the observed grain morphology can be explained on the basis of information about the mode of solidification revealed by the impurity substructure. WHILE a great number of studies of nucleation in undercooled molten metals have been made, comparatively little attention has been given to the mode of solidification from melts with large undercool- ings. Colligan and Bayles1 and Walker2 have measured the rate of advance of the solid-liquid interface in undercooled nickel melts, but the morphology of the solidifying material remained a matter of speculation. Fehling and Scheil3 have described the grain structure in ingots formed from undercooled melts of nickel, palladium, and copper, and a series of Ni-Cu and Ni-Pd alloys. At small undercoolings, equiaxed structures are observed, the grain diameter tending to increase as the temperature of nucleation is lowered. At greater undercoolings, a columnar structure is developed, while with still further undercooling there is a smaller grain size incorporating rather coarse subgrains. All-bright and Colligan4 examined the grain structure shown by ingots solidified from melts of nickel and of Ni-Ag alloy at an undercooling of 105°C, and concluded that considerable grain growth had taken place after solidification. The object of the present work is to correlate the mode of solidification from undercooled melts with both the grain structure and impurity segregation, using tracers to examine the latter.

Jan 1, 1965

By G. L. Tufford, R. L. Bleifuss

Low-grade manganiferous iron ores of Minnesota's Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite with subsequent magnetic separation and flotation have not given satisfactory results because, in many instances, concentrate grade and manganese recovery are low. Metallization of iron and concurrent reduction of higher manganese oxides to MnO, as in the R-N process, followed by recovery of iron by magnetic separation and manganese by leaching, seems to be a technically feasible process. High-temperature x-ray diffraction studies show that solid-state reactions between iron and manganese, with the formation of intermediate iron-manganese oxides, occur during reduction and affect recovery of both iron and manganese from the final product. Solid state reactions also occur between FeO, MnO, and SiO, at temperatures as low as 900°C. The kinetics of these reactions are such that they become an important factor in the treatment of ores by the R-N process. These investigations suggest a temperature and gas composition cycle that would maximize both iron and manganese recovery. During the past ten years, iron ore shipments from the Cuyuna Range of Minnesota have decreased sharp1y. Because of adverse grade, structure, and cost, many Cuyuna ores are no longer competitive with high-grade foreign ores and domestic pellets. The low-grade manganiferous iron ores from the Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite for subsequent magnetic separation and flotation has not given satisfactory results because concentrate grade and manganese recovery are often low. However, a technically feasible process appears to be metallization of the iron and concurrent reduction of manganese oxides to MnO with recovery of metallic iron by magnetic separation and extraction of manganese from the tailings by leaching. In 1962 the R-N Corp., with a grant from the Area Redevelopment Administration, conducted an amenability study of the metallization of manganiferous iron ore from the Cuyuna Range. The results of this preliminary investigation were sufficient to interest the Economic Development Administration in sponsoring further studies of the process with emphasis on secondary recovery of manganese from the nonmagnetic tailings. Inasmuch as the metallization process has considerable influence on the final form of the manganese - its texture and distribution between the magnetic concentrate and nonmagnetic tailings-the investigation included a study of metallization of the ore as well. Therefore, the investigation conducted at the Mines Experiment Station covered three interrelated phases: (1) laboratory R-N roasting studies and magnetic separation tests, (2) laboratory chemical extraction experiments of the nonmagnetic tailings, and (3) a mineralogical study of the crude ores and their various roast products. High-temperature x-ray diffraction investigation of the Fe-Mn-Si0,-0, system is the main topic of this paper and an extension of the mineralogical work. GENERAL GEOLOGY The Cuyuna Range is known for its complicated geologic structure, complex orebodies, and generally indifferent response to attempts at conventional beneficiation. Several geologists have made intensive studies of the Cuyuna Range, including Leithl (1907), ~darns' (1910), Zapffe3 (1925), Grout and Wolff4 (1955), and schmidt5 (1963), whose study was the most comprehensive of all. The Range is covered with glacial deposits - till, out-wash, and lake sediments -up to 250 ft thick. Bedrock stratigraphic units of the Cuyuna Range consist of three tightly folded Precambrian sedimentary formations. The lower unit is the Mahnomen formation, composed of 2000 or more feet of argillite, slate, siltstone, and quartzite. The middle unit is the Trommald formation, which varies from 45 to 500 ft in thickness and comprises the major iron-bearing formation. The upper unit is the Rabbit Lake formation, consisting of over 2000 it of argillite, slate, and interbedded lenses of lean iron formation. In the central part of the Cuyuna Range, the units have been folded into a series of

Jan 1, 1969

Henry Louis, Newcastle-upon-Tyne, England (communication to the Secretary): I think very highly of the novel and ingenious device of Prof. Richards for analyzing the movement of the various elements of the jig; it is a method that certainly seems to promise valuable results, if we could only make certain that these various indicator-appliances have no effect upon the action of the jig. I would like, however, to suggest that in future experiments the connection between the plunger indicator-rod and the pencil should be made by means of parallel motions, so as better to reproduce the rectilinear motion of the piston. I should expect, if this were done, that the " curve " of the plunger in the Harz jig, at any rate, would be represented either by straight lines or else by quite regular curves, according to the method by which the plunger is set in motion; the apparent combinatioil of straight line and curve seems difficult to explain. With respect to the water-curve, I am afraid I am completely at fault, but no doubt Prof. Richards can explain my difficulty. In Fig. 2, the areas of the screen-side and the plunger-side of the jig are equal. If the piston be a fair fit and the bottom of

Jan 1, 1897

By C. S. Brooks

Several of the commonly used methods for deter-mination of effective grain densities of minerals have been evaluated for accuracy and precision, and their applicability to various types of petroleum reservoir minerals tested. Consideration was given to the effect of consolidation, swelling clay, and wettability on these grain-density determinations. Procedures with helium displacement, a modified low-pressure Boyle's law porosimeter, and liquid displacement (water, n-decane, and n-octanol) were tested. The helium-displacement procedure was used primarily as an independent reference for which the effects of fluid-solid interaction, e.g., adsorption and wettability, were negligible. The procedures with the Boyle's law porosimeter and with liquid displacement are the methods in common use. Minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The number of samples tested, while not large, was adequate to permit application of statistical methods. Grain-density measurements on calcite (Iceland spar) provided a basis of comparison for the accuracy and precision of the procedures under investigation for a material with a high degree of chemical and physical homogeneity and for which fluid-solid interactions were at a minimum. Liquid-displacement procedures (water or n-decane) provided the greatest reliability and precision for measurement of the grain densities of the limestone tested. Gas-displacement procedures (helium or Boyle's law porosimeter) provided the greatest reliability and experimental convenience, if not the greatest precision, for the measurement of the grain densities of the swell- ing clay, Wyoming bentonite, and the shah sandstones which -contained appreciable amounts of swelling, in-terstitial clays. These experiments were designed to evaluate the applicability of the grain-density procedures in common we to some of the less tractable minerals—tight limestones, shaly sandstones, and swelling clays. The results should provide a useful basis for a selection of the method most suitable for application to the various petroleum reservoir minerals encountered and especially for use in the estimation of formation porosity. INTRODUCTION These experiments were undertaken to evaluate the accuracy and precision of several commonly used methods for determination of effective grain densities of minerals, and to test their applicability to various types of petroleum reservoir minerals. Consideration was also given to the effect of consolidation, clay, and wettability on these grain-density determinations. Procedures used included measurements with helium displacement, with a modified low-pressure Boyle's law porosimeter, and with liquid displacement (water, n-decane, and n-octanol). The minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The accurate determination of the porosity of petroleum reservoir formations, in particular those of low porosity, has received much attention. Both bulk-volume and grain-volume measurements necessary in the evaluation of porosity have been examined by many investigators with the objectives of improving both the accuracy and the precision of these determinations. In this investigation statistical criteria for selection of the most reliable and suitable procedure for use with a given type of mineral are demonstrated. The grain-volume measurement procedures appear to be the most susceptible to improvement.

Jan 1, 1958

The following is an incomplete list of members and guests who called at Institute headquarters during the period June 10, 1918 to July 10, 1918. F. C. Alsdorf, Tucson, Ariz. Emory M. Marshall, Camp Raritan, N. J. Juan F. Brandes, Santa Barbara, Cal. Jacques S. Negru, Camp Niagara, Ont. .H. Smith Clark, Kansas City, Mo. Arvid E. Nissen, High Bridge, N. J. J. S. Cunningham, Charleston, W. Va. Richard G. Place, So. Strafford, Vt. W. G. Eberhardt, Tucson, Ariz. Frank H. Probert, Berkeley, Cal. M. Eldredge, Bombay,. India. Martin A. Roudabush, Osterburg, Pa. A. D. R. Galloway, Accra, W. Africa;. P. H. Royster, Minneapolis, Minn. F. Hanst, Harrisburg, Pa. J. L. Schueler, Peoria, Ill. B. B. Hood, Chrome, N.. J. Henry B. Smith, New Britain, Conn. Paul S. King, Wilmington, Del. W. G. Sommer, Peoria, Ill. E. D. Kinney, Anaconda, Mont. A. L. Toenges, Roanoke, Va. E. W. Kohl, Jr., Philadelphia, Pa. G. D. B. Turner, Butte, Mont. James W. Love, Knoxville, Tenn. A. T. Ward, Bellefonte, Pa. Edwin A. Austin, formerly with the Yukon Gold Co., is superintendent of the Elkoro mine at Jarbidge, Nev. John W. Beard is now with the Cia Minera de Penoles, Ojuela, Dgo., Mexico, via Mapimi. R. S. Bonsib has accepted a position with the United States Emergency Fleet Corporation as District Safety Engineer, San Francisco, Cal. Albert Burch has been appointed by the Bureau of Mines to encourage the mining of chrome. F. B. Caldwell is working for the U. S. Bureau of Mines, under Albert Burch, in the investigation of chromite deposits. W. A. Carlyle has taken over the duties (in addition to his own) formerly assigned to E. P. Mathewson with the British America Nickel Corporation, at Sudbury, Canada. R. M. Catlin received the honorary degree of Doctor of Science at the recent commencement of Rutgers College, New Brunswick, N. J. S. K. Dahl is giving up his position as mill superintendent with the Messina Mines, which have been suspended, and is returning to this country. Algernon Del Mar has become manager of the Techatticup mines, El Dorado Canyon, Nev. Robert Dye has succeeded D. L. Forbes as manager of the Teck-Hughes at Kirkland Lake, Ont., Canada. J. O. Elton, superintendent of the Anaconda company's electrolytic zinc plant at Great Falls, Mont., is doing special work with the U. S. Bureau of Mines. R. B. Caples takes charge of the plant in his absence. George H. Gibbs has resigned his position as engineer at Messrs. T. & 1. Bradley & Sons, Ltd., Darlaston blast furnaces, Darlaston, and is now located at "Belmont." Litchfield Road, Rushall, Walsall, England. William D. Gordon, for the past 7 years manager of The Mine & Smelter Supply Co. at El Paso, has been elected president of Camphuis, Rives & Gordon,. Inc., and has opened American headquarters for the company at 81 New Street, New York, N. Y. E. Harms, for the past 16 years inn charge of metallurgical operations of the Torreon, Mexico; lead and copper smelter, has resigned and is now located at El Paso, Tex.

Jan 8, 1918

By Raynor Linzey, Karl M. Busen

The formation of thin films of silicon oxide by anodic oxidation of silicon and the subsequent removal of these films by an etch is a process often used for the evaluation of concentration distributions Profiles) in silicon layers by the differential sheet conductance method. The accuracy of the resulting profile is very strongly influenced by the uniformity of the thickness of the reacted silicon. Normally, it would be expected that for a constant number of coulombs passed the thickness would be the same from oxidation to oxidation. Investigations show that in certain electrolytes, for a given number of coulombs passed through an n-type silicon sample, the thickness of the reacted silicon increased with increasing resistivity. Even for the same resistivity the thickness varied sometimes by a factor of 1.5. When an electrolyte was used which consisted of 10 pct water by volume in ethylene glycol with 4.0 g KNO per 1000 ml of solution, anodiza-tion at 5 ma per sq cm led to satisfying results. Short-time anodizations gave oxide layers of a higher apparent density than those experienced from thermally gown silicon oxides. THE functioning and the electrical characteristics of semiconductor devices are based upon the incorporation of "impurities" into a single-crystalline body of suitable material and on the concentration distribution (profile) of this impurity. The incorporation can be achieved by well-known processes as, for example, by diffusion, epitaxial growth, alloying, or ion implantation. Often the profile resulting from these processes is not known. A powerful tool to learn about a concentration distribution is given by the method of differential sheet conductance which employs successive four-probe measurements on a layer subjected to stepwise removal of thin sublayers. Differential sheet conductance vs position (or penetration depth) of a sublayer is plotted and a smooth curve is drawn through the data. From this curve the profile is then calculated. When the semiconductor material is silicon, the sublayers are removed suitably by anodic oxidation of the silicon and subsequent dissolving of the formed silicon oxide by an etch. The accuracy of the resulting profile is very strongly influenced by the uniformity of the sublayer thickness. Normally, it would be expected that, for a constant number of coulombs passed, the thickness would be constant from oxidation to oxidation. Investigations showed that for sublayers several hundred angstroms thick the reproducibility can be rather poor. Therefore, efforts were made to obtain a reliable technique for uniform removal. The present paper describes such a technique and certain phenomena which were encountered during the investigations. APPARATUS AND TECHNIQUE The first report on the investigation of concentration distributions, where for differential sheet conductance measurements thin silicon sublayers were removed from a diffused layer by anodic oxidation, was given by Tannenbaum. The author reports the removal of sublayers which for the most part were 400 thick. More advanced device designs now require much narrower layers. When it was tried in these laboratories to determine profiles within such layers, difficulties were encountered with respect to sublayers which by necessity had to be thinner than the ones reported by Tannenbaum. The apparatus used for the investigations is sketched in Fig. 1. Two cylindrical containers connected by a wide tube are filled with an electrolyte. The left container receives the cathode whereas the right container is closed at the bottom end by a sample support consisting of a Teflon base and a copper pedestal. The silicon sample (1 by 1 cm) is mounted to the pedestal embedded flush in the Teflon base using silver paint (Degussa) for electrical contact. Pyseal is applied to the edges of the sample to protect the copper pedestal from the electrolyte. The base is mounted to the container using a water-tight silicon rubber gasket. Fig. 2 gives a view of the sample support. The copper pedestal is connected to the positive side of a power supply operating at a constant current output (Kepco Model ABC 425M). The electrolyte which has been reported by Duffek et al. consisted of either 2 or 10 pct water by volume in ethylene glycol and 4.0 g KNO3 in 1000-ml solution. The electrolyte is best prepared

Jan 1, 1967

By M. B. Kasen

eralized strain equation appear quite different they are really identical. This identity can be shown in a simple mathematical rearrangement. Referring to Eq. [I], the substitution of ln(1 +?E) for ? (where ?E is the engineering strain) yields: a =s8- (s8?so)e?1/?c) ln(1 +s8??E) [4] or s =s8?(s8?so)(l +?E)-1 [5] Replacing (1 + cE) with its equivalent, (l/lo): s=s8?(s8?so)l/€c [6] Adding and subtracting the quantity (s8 - so) yields: s=s8?(s8?so)+ (s8-so) l-(^)l/£c [7] = s0+(s8?so)ri-(^0)1/^l [8] Letting n = 1/?c it follows that: This equation will be seen to be identical to the generalized strain expression in Eq. [3], the coefficients a and b being equal to so and (s8?so)/?c or n(s8?so), respectively. Confirmation of the relationship noted above was provided by fitting experimental stress-strain data5 for 304 stainless steel (total strain from 0.072 to 1.15) at room temperature at a true total strain rate of 4 x 10-3 sec-1 to Eqs. [I] and [3]. In this study nonlinear regression analyses were used to evaluate the equation constants. The results of this evaluation are presented in Table I. When these constants are used in Eqs. [I] and [3] the curves obtained are coincident. It will also be noted that the value of n is equal to YE,, the value of a is equal to so, and the value of b is equal to (s8 - so)/Ec. These equalities are illustrated in Table I where the Voce constants in parentheses were calculated from a, b, and n values. Excellent agreement is seen to exist. It is concluded, therefore, that the Voce equation is, indeed, identical to the linear expression involving generalized strain. In applying the generalized strain concept to stress-strain data, it has been noted3 that data within what was termed the transition region (first few points in the plastic flow region) must be excluded from the analysis in order to obtain the linearity in Eq. [3]. A similar exclusion applies in the use of the Voce equation since an expression which would describe the strain-hardening region would usually be found to be not too effective in the elastic-plastic fillet2 which connects the elastic line to the strain-hardening region. These considerations further substantiate that Eqs. [I] and [3] do indeed describe identical behavior. Note added in proof. Since this manuscript was submitted for publication, correspondence with Professor S. R. Davies, University of Edinburgh, (of Ref. 3) indicated that his associates have also confirmed the identity between the Voce equation and the generalized strain concept. It is sometimes desirable to obtain a small grain size in super-purity metals. Unfortunately, the absence of impurities, the low recrystallization temperatures, and the low activation energies for boundary motion result in rapid growth of relatively few grains when conventional recrystallization practices are used. For example, Arajs et al.1 were unable to obtain a mean grain diameter less than about 0.4 mm in iron containing 38 at. ppm of impurity. The <1 at. ppm purity range in many modern superpurity metals results in yet larger limiting grain sizes. It is the purpose of this communication to describe a technique by which mean grain diameters as small as 30 µ have been produced in aluminum having an impurity content < 0.5 at. ppm. The technique should be applicable to superpurity metals other than aluminum and has potential applications to grain refinement of commercial alloys. The necessary and sufficient requirements for production of a small grain size are as follows: a) a large number of potential nucleating sites must be created randomly within the cold worked material, b) sufficient thermal energy must be provided at a rate that will simultaneously activate a large fraction of the potential nuclei, and c) the grain growth must be stopped shortly after grain impingement.&apos; A high density of potential grain nuclei may be cre-

Jan 1, 1970

By B. A. Cheadle, K. P. Steward

Axial tensile, ring tensile, closed end burst, and free end burst tests were done at room tempe.vature and 300°C on three batches of Zircaloy-2 sheathing zuith different textures. Knoop hardness tests were also done on all batches. The mechanical properties of the tubes were largely dependent on the percentages of cold work, but were also markedly affected by the textures, particularly with respect to deformation behavio&apos;r. The deformation behavior observed confirmed Picklesimer&apos;s predictions, zuhereas Knoop hardness results could be correlated with texture and yield strength anisotropy after the ,method of Wheeler and Ireland. From the mechanical properties, and from efjectiue strain values deterrlzined at the fractures using a photoqid technique, it zuas concluded that tubing witlz a single preferred orientation of radial basal poles best combines strength and ductility for any given deqee of cold work. THE mechanical properties required in collapsible Zircaloy-2 fuel sheathing for water-cooled power reactors are strength to resist wrinkling deformation by coolant pressure and ductility to accommodate a small amount of deformation in service without rupturing. Zircaloy-2 tubing during fabrication develops pre- ferred orientations of the a Zr grains due to aniso-tropic deformation behavior, and these textures markedly affect mechanical properties. Picklesimer&apos; had predicted the deformation behavior of tubes with various textures, but the texture required to provide the optimum strength and ductility for a given degree of cold work has not been reported. To investigate this problem, tests at three transverse to axial stress ratios were done at room temperature and 300°C on three batches of Zircaloy-2 tubing covering a wide range of textures and percentages of residual cold work. Knoop hardness values were also measured to correlate with preferred orientation and yield strength anisotropy after the method of Wheeler and relland.&apos; 1) MATERIAL For this investigation, three batches of tube-reduced tubing were chosen from the Zircaloy-2 sheathing produced for the Douglas Point Reactor. Individual tubes were 191/2 in. long, 0.600 in. OD, and 0.0165 in. nominal wall thickness. The identities of the batches, together with their textures, are shown in Table I. The tubes had the normal Zircaloy-2 composition3 of 1.5 wt pct Sn, 0.3 wt pct Fe, Ni, Cr combined with the following oxygen concentrations: Batch VII 1140 to 1390 ppm 0 Batch VIII 1400 to 1750 ppm 0 Batch IX 880 to 1320 ppm 0

Jan 1, 1968