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By R. O. Williams

It is shown that Ni3Al precipitates homogeneously from nickel-rich alwminum alloys as plates on the (100) planes. Prior to actual precipitation a process occurs which is believed to be one of increasing short-range order. After precipitating the Ni3Al plates enlarge through competitive growth. Discontinuous precipitation can occur simultaneously with the above processes. Recent ideas of the origin of precipitation strengthening appear adequate to explain the hardness changes. REMARKABLY little appears to be known about the precipitation process in Ni-Al alloys in spite of their technical importance. This investigation originated to supply additional information about precipitation in general, this system in particular. Information on the structures and kinetics have been obtained through the use of hardness, X-rays, microscopy, calorimetry, and resistivity on high-purity alloys. PROCEDURES Six alloys, Table I, were prepared by melting carbonyl nickel and high-purity aluminum in alumina crucibles in vacuum and casting into 1-in. graphite molds. All rods were homogenized at least once at 1300°C for 24 hr prior to swaging and this was repeated on the first three alloys after 75 pct reduction. Alloy 4 could be reduced only 10 pct at 1000°C (probably in two-phase field) prior to fracture but 1/4-in. samples quenched from 1100°C were readily reduced cold. Alloy 5 was reduced 15 pct cold but failed on the next pass while alloy 6 of essentially the same aluminum content failed inter-granularly without apparent flow up to 1000°C. The alloys were heated in hydrogen at the elevated temperatures and formed thin, coherent aluminum oxide coatings which provided excellent oxidation resistance at lower temperatures. However, freshly prepared surfaces showed considerably less resistance at 500"to 700°C in air and apparently resulted in internal oxidation. As a consequence, low-temperature agings were carried out in evacuated tubes. RESULTS The isothermal hardening behavior of these alloys at 500"and 565C is given in Figs. 1 and 2. These results were obtained from samples cold worked 75 pct, recrystallized at 1000°C (1100°C for the 7.8 pct Al) and quenched in water. This recrystallization was used to give smaller grain sizes so as to obtain more uniform hardness values and the points represent an average of five readings. The electrical resistivity was measured on 1/16-in. wires quenched from 1000°C during aging at 495°C to give Fig. 3. The energy release and its rate are given in Fig. 4 for the 6.9 pct Al alloy during aging around 500°C. Inasmuch as this was a single run, its accuracy is not known but certainly the general shape and magnitudes are correct. The method used to obtain these results is described elsewhere.' Data for the aging at 600°, 700°, and 800°C of these alloys cold worked 50 pct are given in Fig. 5. Supplementary information from microscopy and X-ray diffraction have been included to indicate recrystallization, discontinuous precipitation and the appearance of superlattice lines from the Ni3Al. The hardness of these alloys as annealed, aged, cold worked, and cold worked and aged is given vs composition in Fig. 6. Those samples which were isothermally aged, Figs. 1 and 2, were reaged at 532°C and at successively higher temperatures for the indicated times to give the data of Fig. 7. These results as well as certain others, support the idea that the level of hardness reached for temperatures above 600°C are equilibrium values more or less independent of path. This being the case, the breaks in the curves would be the complete solution of the Ni,Al. The electrical resistivity versus temperatures for some of these alloys, both aged and unaged, is given in Fig. 8 along with those data from heating slowly (10 deg per day) to high temperatures. Interesting points include the lowering of the Curie temperature (the change in slope), the lack of any indications of a solubility limit and the large temperature coefficient for the Ni3Al. A slight break for Ni3Al around 100C shows up but this is not a Curie temperature as Ni3Al is not ferromagnetic down to -190°C. Metallographically both the nickel-rich solid solution and the Ni3Al appear very much like pure nickel. Profuse twin boundaries are present both

Jan 1, 1960

By A. Gatti

Studies were made on the system iron plus alumina. Various methods of dispersing and various amounts of alumina were used. Powder metallurgy techniques were used to produce the final product. Microstructures and some mechanical properties are presented. Alloys containing up to 16 pct alumina by weight are ductile at all temperatures tested. The ivon-alumina materials have a higher yield stress and improved creep resistance over that of pure iron. SINCE the development of SAP' an A1- Al2O3 powder metallurgy product, great interest has been shown in the development of a SAP-like structure in metals and alloys other than aluminum. The outstanding properties of this class of materials are: 1) Good creep resistance at high temperature. 2) High yield strengths and high hardness at high temperatures. 3) High recrystallization temperature. However, the lack of ductility and formability has thus far limited the applications of SAP-like materials. The following report deals with methods of dispersing A12O3 in Fe, processing of powders into rod, structures produced after processing, and mechanical properties of the iron-alumina material produced. Methods of dispersing the alumina and also the volume fraction of alumina added were varied. MATERIAL Powder Processing— Four methods of obtaining dispersions of alumina in iron were studied. 1) Oxidation-reduction of a Fe + 8 pct Al alloy. .2) Coprecipitation of Fe(OH)3 + Al(OH)3 from aqueous solution. 3) Colloidal mixing of Fe,O3 and Al2O3. 4) Colloidal mixing of Fe powder and A1,O3. Fig. 1 is a processing flowsheet which outlines the processing steps taken to produce a final extruded bar 1/4 in. in diameter and about 30 in. long. The - 100 mesh iron-aluminum alloy was oxidized by placing a thin layer of powder on an alumina plaque. The reduction step was modified to include 1/2 hr at 1000°C since the powders tended to become pyro-phoric unless sintered slightly after low-temperature reduction. Compacting was done in a 1-1/8-in.-diam pressing die. The slugs produced averaged 1 in. in length. The billets were encased in low-carbon steel cans shown schematically in Fig. 2. The blank is included for structure and property comparison purposes. TESTING PROCEDURE All tests were made on as-extruded material.

Jan 1, 1960

Established as a Division March 13, 1935 R H Feierabend, Chairman T E Gillingham, Jr, Northeast Vice-Chairman W A Riggs, Southeast Vice-Chairman C F Clausen, Mid-Continent Vice-Chairman R H Wilpolt, Rocky Mountain Vice-Chairman J K Brooke, Pacific Southwest Vice-Chairman Leslie C Richards, Pacific Northwest Chairman V A Haw, Canadian Vice-Chairman J S Holland, Sec'y -Treas National Lead Company Mining Department 111 Broadway New York 6, New York

Jan 1, 1960

By I. Cadoff, E. Miller, K. Komarek

Jan 1, 1960

By P. K. Koh, H. A. Lewis, H. F. Graff

New data on the distribution of silicon between slag and carbon-saturated iron at 1600Oand 1700OC are presented which, in combination with previously published data, permit the determination of silica activities over a broad range of compositions in the CaO-Al2O3-SiO2 system. The distribution of silicon between graphite-saturated Fe-Si-C alloys and blast furnace-type slags in equilibrium with CO has been described in previous publications.1"3 In this past work the silica-silicon relation was established at temperatures of 1425" to 1'700°C for slags containing up to 20 pct A12O3. This paper presents the results of additional studies at 1600" and 1700° C which extend the silicon distribution data at these temperatures for CaO-A12O3-SiO, slags over a range from zero pct Al2O3 to saturation with Al2O3, or CaO.2Al2O3. The upper limit of SiO2 is set by the occurrence of Sic as a stable phase when the metal contains 23.0 or 23.7 pct Si at 1600" or 1700°C, respectively. The activity of silica over the expanded range is determined directly from the distribution data.3 Recently4-7 other investigators have studied the activities of SiO, and CaO, principally in the binary system, using different methods and obtaining somewhat different results. EXPERIMENTAL STUDY The experimental apparatus and procedure have been fully described in previous publications.1, 3 Six new series of experimental heats have been made, four at 1600° and two at 1700°C. Master slags of several fixed CaO/Al203 ratios were pre-melted in graphite crucibles, and these were used with additions of silica to prepare the initial slag for each experiment. Slag and metal were stirred at 100 rpm and CO was passed through the furnace at 150 cc per min. The initial sample was taken 1 hr after addition of slag at 1600°C or 1/2 hr after addition at 1700°C. The run was normally continued for 8 hr at 1600°C or 7 hr at 1700°C, and the final sample was taken at the end of this period. Changes in Si and SiO2 content indicate the direction of approach to equilibrium, and in a series of runs where the approach is from both sides this permits approximate location of the equilibrium line. Fig. 1 shows the results of such a series of 15 runs at 1600°C for slags of CaO/Al,O3 = 1.50 by weight. Figs. 2 and 3 record other series at 1600°C and Fig. 5 a series at 1700°C with fixed CaO/Al0 ratios. The results of the experiments at 162003°C have been reported in part in a preliminary note.3 In the experiments recorded in Figs. 4 and 6, the slags were saturated with A12O3 (or with CaO.2A12O3 within its field of stability) by suspending a pure alumina tube in the melt during the course of the run. The final slag analyses were used to establish the liquidus boundaries8 in the stability fields of CaO.2Al2O3 and of Al20,. ACTIVITY OF SILICA The free-energy change in the reaction has been calculated by Fulton and chipman2 from recent and trustworthy data including heats of formation, entropies, and heat capacities. The more recent determination by Olette of the high-temperature enthalpy of liquid silicon is in satisfactory agreement with the values used and therefore requires no revision of the result which is expressed in the equation: SiO2 (crist) + 2C (graph) = Si + 2CO(g.) [1] &F° = + 161,500 - 87.4T The standard state for silica is taken as pure cristobalite and that of Si as the pure liquid metal. Since the melts were made under 1 atm of CO and were graphite-saturated, the equilibrium constant for Eq. [I] reduces to K1 = asi /asio2. The value of this constant is 1.77 at 1600°C and 16.2 at 1700°C. Through K1, the activity of silica in the slag is directly related to the activity of silicon in the equilibrium metal.

Jan 1, 1960

Univ of Alabama-University, Alabama-Mining and Metallurgical Society William L Mason, Faculty Sponsor, E C Wright, Dept Head Univ of Alaska-College, Alaska-Mining Society of the Univ of Alaska Douglas W Huber, Faculty Sponsor, E H Beistline, Mining & Metallurgy Dept Head, Troy L Pewe, Geology Dept Head, James Crawford, Chapter Counselor Univ of Arizona-Tucson, Arizona-Miners Society Willard C. Lacy, Faculty Sponsor, J D Forrester, Mining & Metallurgy Dept Head, F. W Galbraith, Geology Dept Head Univ of California-Berkeley, California-Mineral Technology Association H E Hawkes, Faculty Sponsor, Joseph A Pask, Dept Head Carnegie Inst. of Technology-Pittsburgh, Pa -The Metals Club William R Bitler, Faculty Sponsor, Robert F Mehl, Dept Head

Jan 1, 1960

By D. D. Donald

C. J. Barber (U. S. Smelting Refining & Mining Co., Salt Lake City)—In his paper Donald describes how New Jersey Zinc Co. made surveys for a connection between the Ivanhoe and Van Mater shafts at Austin-ville, Va. Except to say that the two faces had to meet "accurately" on line and grade, Donald does not indicate the required precision. Assuming that there were 24 angles in the 11/2-mile traverse and 15 in the one-mile traverse, it can be shown that if the average error in plumbing each shaft was 230" and the average error in measuring each traverse angle was 210". then the average error at the point of -connection would have been about ±1.9 ft normal to the line between the shafts. This calculation assumes that any errors in the triangulation would be negligible compared with the errors in the plumbings and traverses, and it also neglects taping errors. With no constant errors or blunders, the latter would be important only in lines normal to the line between the shafts. To make the average error at the connection less than 1.9 ft would, therefore, require either reducing the error in the plumbings to less than ±30", or that in the traverse angles to less than ±l0", or fewer stations, or a combination of these. Referring briefly to the triangulation, because of the problem of fitting a new triangulation into older surveys of the district the orientation deserved some mention, even though the connection could have been made with an assumed bearing. It would be interesting to know how many triangles were required and what the average summation error was before making any adjustments and without considering the algebraic signs. Perhaps this is referred to indirectly in the statement that the maximum angular error distributed was 2". Turning to the shaft plumbings, it would be helpful to know how many men were employed and how long each shaft was in use. Donald says that the surface positions of W-2 and W-3 were carefully surveyed from the collar position of W-1, without indicating how this was done. The length of the backsight would be particularly important. There must have been some error in setting W-1 vertically below the stations in the headframes. How immovable were the headframes, especially the Van Mater, which appears higher than the Ivanhoe and subject to more vibration because of skip hoisting? Donald does not say whether the plumbing wires had been previously restraightened to minimize spinning (otherwise they behave like weak helical springs). The use of light steel weights is most surprising because there seem to be excellent reasons for using heavier, nonmagnetic weights. Did the shafts contain no steel sets, pipes, power cables, etc., which might attract steel? The plumbing method described by Donald was designed for deep shafts in South Africa but differed from the South African practice in two important respects. As described by Browne,6 in South Africa the line between the wires was made parallel to the long axis of the shaft, whereas in the Ivanhoe shaft the lines between the wires were diagonally across the shaft. The main reason given for the South African practice is to insure that the gravitational attraction between the wires and the rock walls is the same on both wires, and therefore does not affect the bearing of the line between them. It seems probable, however, that the effect of air currents might be minimized in the South African procedure, and might be serious with the wires in the diagonal position at the Ivanhoe shaft. In the South African case cited by Donald the wires were swinging freely (although the plumb bobs were sheltered from air currents) but in the Ivanhoe case they were dampened with the plumb bobs set in water. In the discussion of Browne's paper R. St. J. Rowland said:' It has been the practice for a long time to damp the oscillations by immersing the bobs in oil or water. The time per oscillation is thus increased, thereby extending the time taken to complete the work. The longer the suspended wire the less there is to recommend the practice . . . The theoretical time for one swing of a simple pendulum 1050 ft long is approximately 36 sec, which would be increased by dampening the plumb bob in water. Hence very few complete swings would be observed in the 5 min intervals used at the Ivanhoe shaft. In the two South African cases described by Browne, the length of plumb line in one shaft was 5425 ft, the calculated period of swing was 81.6 sec, the average actual period was 76.6 sec, and 94 complete swings were observed in 2 hr. In the other case the length of plumb line was 3116 ft, the calculated period of swing was 61.8 sec, the average period was 63.5 sec, and 86 complete swings were observed in 1 hr 31 min. Browne concluded that observations of more than 30 swings are not likely to result in sufficient gain in accuracy to be justified. Returning to the Ivanhoe and Van Mater plumbings, an objection to the method used is that all four azimuths were taken from fixed points instead of swinging wires, and that each pair of observations would— barring blunders— check closely, and so perhaps give a false feeling of security. In fact, it seems that only two azimuths were obtained from one plumbing, and not four as stated by Donald. Nevertheless, the tying in of each pair of wires from both sides of the shaft has much to commend it. Donald's description leaves the impression that if each shaft was plumbed only once, the engineers were fortunate indeed if the average error in the underground orientation was as little as 30". Because the survey was done over a period of three years, it seems likely that the plumbings were repeated, perhaps more than once. The underground traverse angles were measured by conventional methods, but because the number of angles in the overlapping traverses was not given, the angular closure given by Donald does not indicate the accuracy with which this was done. Donald's description of a method of taping lines of irregular length is welcome. The literature on taping is usually confined to lines of about one tape length, generally 100 ft. Such lines are rare in metal mining because the time, trouble, and cost of setting points at 100-ft distances underground are not warranted. (Nevertheless civil engineers may go to this expense

Jan 1, 1960

By Oliver Bowles

Dimension stone is a term applied to stone sold in blocks or slabs of specified shapes and usually of specified sizes, contrasted with crushed, broken and pulverized stone covered in another chapter. Dimension stone includes cut stone, rough building stone, ashlar,* rubble, monumental stone, paving blocks, curbing, flagging, and many types of ornaments and novelties carved from stone. Riprap-large, irregular blocks used for shore protection-is classed with crushed and broken stone. Composition, Varieties, and Properties Dimension stones are of many kinds. The principal varieties are granites, trap rock (diabase, basalt, and gabbro), sandstone, limestone, and marble. Slate is covered in a separate chapter. Granite is a visibly granular crystalline rock consisting essentially of feldspar, quartz, and mica or hornblende. The basaltic rocks are darker in color than the granites. They contain little or no quartz and consist largely of plagioclase feldspar, augite, pyroxene, and hornblende. They are classed commercially as black granites. Limestone consists essentially of calcium carbonate. Dolomites and magnesian limestones used as dimension stone are classed with the high-calcium limestones. Marble is a crystalline form of limestone, but in the trade, any carbonate rock which will take a polish is called a marble. Many limestones which are fossiliferous but which will take a polish are sold as a decorative stone for lobbies of hotels and office buildings. Sandstone consists essentially of silica in the form of sand grains cemented into a coherent mass. Although rock occurrences are numerous and widespread, the exacting requirements of use condemn all but a small fraction of them for commercial use as dimension stone. No deposit that has closely spaced joints or planes of weakness can be used because sound blocks of moderate to large size are demanded. Uniform texture and grain size, constant and attractive colors or color pattern, and freedom from impurities that may cause stains or deterioration usually are demanded. Hardness is a variable property. Granites and diabases are as hard as or harder than steel, while limestones and marbles may be scratched with a knife. The hardness of sandstone depends upon the degree of cohesion of the grains. Workability depends to a considerable extent on hardness, but the degree of hardness has little influence on use except where stones are subjected to abrasion as on steps or floors. "Texture" as applied to stone relates to the arrangement, uniformity, and size of the constituent grains. Stones are of many colors and thus can satisfy a variety of tastes. For monumental stone, a marked contrast between polished and tooled surfaces is preferred in order that inscriptions may be read easily. Strength requirements usually may be disregarded because any sound structural stone suitable in other respects is almost invariably many times as strong as would be required for any ordinary use. The pressure on the base course of the Washington Monument, Washington, D. C., is less than 700 psi, and highgrade granites, limestones, sandstones, and marbles will sustain a crushing load of 10,000 to 25,000 psi. A structure made of stone with a crushing strength of 15,000 psi would have to be nearly 21h miles high before crushing of the lower courses would occur. However, stone disintegrates more readily under severe

Jan 1, 1960

By P. Gordon, A. S. Iyer

IN a paper on the mechanical behavior of heat-treated steel, N. H. Polakowski' put forward arguments to the effect that the stored energy resulting from the deformation of metals should be reduced during the inital stages of subsequent deformation carried out under conditions which produce work softening. At the time (1957) the only energy measurements available as indirect evidence on this point were the results of M. M. Degtyarev,2 some of which Polakowski reproduced in his Fig. 6, and which are again reproduced here in Fig. 1. The solid lines in the upper part of Fig. 1 are Degtyarev's, the dashed Lines Polakowski's prediction of the true trend of the stored energy in copper samples pre-strained in tension and then given various amounts of subsequent compression. The accuracy of this prediction has been borne out by some experiments carried out on American Smelting and Refining Co. copper (99.999' percent Cu) by the present authors. Bars of this copper about 0.4 in. in diam and 12 in. long were prepared by vacuum melting and casting, followed by cold forging and swaging in several stages of about 40 pct reduction in area with intermediate recrystallization anneals. After the final anneal one bar was deformed in tension to 30 pct elongation; the gage length was then cut into several samples which were given axial compressions of various amounts. The hardness of

Jan 1, 1960

MAJOR AWARDS JAMES DOUGLAS GOLD MEDAL 1960-Augustus B Kinzel "For outstanding contributions and inspiring leadership in the field of electrolytic and electrothermic winning of nonferrous metals and for his notable administrative ability " BENJAMIN F FAIRLESS AWARD 1960-Charles McElroy White "His ability, energy and determination in starting the top-pressure blast furnace and foresight in providing it with prepared burdens have created the world's dominant metal producer " HAL WILLIAMS HARDINGE AWARD 1960-Samuel H Dolbear "Eminent mineral consultant and engineer-first chairman, Industrial Minerals Division of AIME-first editor, 'Industrial Minerals and Rocks'-for the improvement and increase of industrial mineral knowledge "

Jan 1, 1960

By G. S. Ansell, J. Weertman

The creep behavior of an aluminum alloy hardened with a finely dispersed phase of aluminum oxide was investigated. The as-extruded alloy shows an approximate steady-state creep in which the creed rate depends exponentially on the applied stress. The activation energy of creeb is abbroximately 150,000 cal per mole. The recrystallized alloy shows no steady-state creep. ONE method of improving the creep resistance of a metal is to introduce a finely dispersed second phase into the metal matrix. The improvement of the creep resistance has been qualitatively explained by assuming that the dispersed second-phase particles act as obstacles to dislocation motion. If the main effect of second-phase particles is simply to hinder dislocation motion then it is possible to derive a high-temperature creep equation for a dispersion-hardened alloy in a straightforward manner. In the Appendix of this paper such an equation is derived from a creep model which works very well for pure metals. Recently, F. V. Lenel has fabricated, for the first time, powder extrusions of aluminum-aluminum oxide in a large-grained recrystallized form. This alloy, designated as MD 2100, consists of a fine dispersion of aluminum oxide plates in a matrix of commercial purity aluminum. A considerable amount of investigation has been carried out concerning the microstructure and physical properties of this alloy.&apos; ) The aluminum oxide is present in the form of flakes 130A units thick and 0.3 u on edge. They are dispersed in the aluminum matrix with an average spacing of approximately 0.5 jx. The spacing varies in the range of 0.05 to 1.5 µ. The alloy structure is extremely stable at high temperatures. For this reason the alloy offers a unique opportunity for a fundamental study of creep of a very finely dispersed two-phase alloy. Lenel supplied specimens in both the unrecrystallized and recrystallized condition. This paper reports high-temperature creep experiments carried out on these specimens. The results obtained were rather unexpected. No steady-state creep was observed in the recrys-tallized material. In fact, after some transient creep which takes place upon loading, the creep rate is essentially zero ( < 10-8per min). If the second-phase particles acted solely as obstacles to the motion of dislocations, measurable steady-state creep would be expected. Since none is observed it appears that the main effect of the fine dispersion in the recrystallized material is to inactivate the dislocation sources themselves, rather than hinder the motion of dislocation loops created at these sources. EXPERIMENTAL DETAILS Specimens were tested in wire form, 0.087 in. in diam for the as-extruded alloy, and 0.035 in. in diam for the recrystallized alloy. These samples were held in friction-type wire grips; a gage length of 2.5 cm was used for all the creep tests. The specimens were held at 600°C in the test apparatus for at least 15 hr prior to each test. The tests were run under the condition of constant loading and, since the creep strains were small, can be considered as constant stress tests. The temperature of testing was held constant within 3°C. Elongations were measured with an optical cathetometer which was capable of measuring strains as smaIl as 0.00012. This allowed the measurement of strain rates as low as l0-8&apos;per rnin. In addition to the creep tests optical micrographs were made in order to determine both the grain size and microstructure of these materials. RESULTS Fig. 1 shows a few typical creep curves obtained from the as-extruded material. The elongations were somewhat erratic, but each curve shows a region of quasi-steady-state creep from which an approximate steady-state creep rate can be obtained. In general the higher the stress at a given temperature, the greater the total elongation before fracture. The lower the applied stress, the longer is the region where the creep rate is almost constant. Summary data from the creep tests of the as-extruded material are listed in Table I. The steady-state creep data of the as-extruded material for a range of stresses at a constant temperature follow a creep equation of the type creep rate = K&apos; = A exp (&) [11 where A and B are constants, k is Boltzmann&apos;s constant, T is the absolute temperature, and a the stress. The standard error of estimate of the data received is less than one order of magnitude. As shown in Fig. 2, if one compensates the creep-rate data for the effect of temperature over the range of test temperature, the steady-state creep data roughly follow a creep equation of the type Temperature compensated creep rate = K* = A exp

Jan 1, 1960

By Julien F. Phillips, Donald E. Garrett

The production of soda ash from natural sources is one of the United States&apos; oldest industries. The London Company, which financed the settlement of Jamestown, in the fall of 1608 exported in its first cargo from Virginia " . . . trials of pitch, tar, glass, frankincense, and soap-ashes."1 This last product, a crude mixture of sodium and potassium carbonates obtained by the burning of wood in iron pots, was the commercial soda ash of its day, used in the infant soap, glass, and bleaching industries. Besides having a good cash value, its production helped to clear the land, and it was a compact, easily shipped commodity. The extra high potassium content of these American "pot-ashes" gave them an added market as a fertilizer, a field that they dominated until the opening of the Strassfurt deposits in 1860. This form of natural soda ash disappeared forever from commercial importance with the introduction of the Le Blanc process (1791), and later the Solvay process for manufacturing soda ash. The Solvay process was rapidly accepted in the United States, and has accounted for most of the country&apos;s soda ash production since 1884. It was not until the western part of the country began to be developed that natural soda ash was again produced. A number of lakes, playas, and springs west of the Rocky Mountains were found to be rich in this mineral, and climatic conditions were ideal for its easy recovery by solar evaporation. The production of natural soda ash from these deposits has become a steadily growing industry in the United States. Production A summary of the production and value of natural sodium carbonates in the United States is presented in Table 1. Prior to 1927 the principal output came from several different companies at Owens Lake, California. Then production at Searles Lake, California, began to [ ] increase until it became the most important source. In 1948 the sale of crude trona from Green River, Wyoming, commenced and since that time production from these latter two areas has been about equal. Table 2 lists the four

Jan 1, 1960

By A. Gatti, R. L. Fullman

A very fine dispersion of aluminum oxide is produced by internal oxidation of solid-solution alloy of 0.14 pet A1 in Ag. The particle size of the aluminum oxide is approximntely 50 to 100A in radius. The yield strength of the alloy is increased markedly by internal oxidation. A further increase in strength is produced by cold working the internally oxidized alloy. Recrystallization is retarded by the finely dispessed aluminum oxide particles, so that the strength increase resulting from cold work is retained on annealing at temperatures 14 to about 700°C. MANY workers&apos;-3 in the past have studied various aspects of the internal oxidation of aluminum-silver alloys. This paper is an extension of these studies with emphasis placed on the effect of time and temperature of annealing on the strength of these alloys after oxidation and subsequent cold working. Two general conditions are necessary to internally oxidize an alloy. First, oxygen must diffuse through the base material more rapidly than does the addition; otherwise oxidation will take place as a surface layer. Secondly, the affinity of oxygen for the addition must be greater than for the base material. After internal oxidation of certain alloys takes place, a marked increase in hardness accompanied by higher yield stress and improved creep properties is noted, presumably as a result of the highly dispersed oxide within the base material. Meijering and Druyvesteyn1 also noted that the internally oxidized portion of a partly oxidized alloy failed to recrys-tallize under annealing conditions that led to coinplete recrystallization of the unoxidized part. EXPERIMENTAL-METHODS AND PROCEDURES Few alloys can be made to contain a second phase that is extremely stable at high temperatures. Silver plus aluminum in solid solution was chosen for these internal oxidation studies because of the high rate of oxygen diffusion through silver and the very stable nature of aluminum oxide. Two alloys were vacuum cast. The nominal compositions were: Alloy A—1 pct Al, balance Ag; Alloy B—0.1 pct Al, balance Ag. Chemical analysis, which does not distinguish between aluminum and aluminum oxide, showed the conlposition to be: Alloy A—1.6 pct Al, and Alloy B—0.14 pct Al. The ingots were machined for surface cleaning, swaged and drawn to 0.020-in. diam wire. A sample 20 ft long of the 0.020-in. dianl wire of each composition was annealed 24 hr at 800°C in pure dry hydrogen. Each wire was then cut into two equal pieces. Photomicrographs of the 0.14 pct A1 alloy are shown in Fig. 1, the annealed 0.020-in. wire at the left and the oxidized wire to the right. The oxidation treatment for the first set of data was 1000 hr at 800°C in air. After this treatment the 1 pct A1 proved to be brittle. It is assumed that high alunlinum oxide concentration at the grain boundaries was responsible. The 0.14 pct Al wire remained ductile and all further data were derived using this alloy. One-half of this wire, about 5 ft, plus 5 ft of as-homogenized wire, was then drawn cold to 0.005 in. diam. All tensile tests were conducted with an Instron Engineering Corp. tensile-testing machine, Model TT-B. Unless otherwise indicated, the tests were made at room temperature with a strain rate of 0.1 per min. All metallographic samples were etched with an aqueous solution of 2 pct each of CrO3 and H2SO4 . EXPERIMENTAL RESULTS AND DISCUSSION PARTICLE SIZE DETERMINATION A study was made of the particle size of the aluminum oxide produced in the samples of Ag + 0.14 pct Al, oxidized 1000 hr at 800°C. A cross section of the as-oxidized wire was mounted in bakelite, polished, and etched with an aqueous solution of 2 pct each of CrO3 and H2SO4. The specimen was then thoroughly cleaned by stripping successive coatings made by applying 10 pct nitrocellulose in amyl acetate. The final replica of the cross section was made by applying 2 pct nitrocellulose in amyl acetate. The replica was stripped, transferred to a copper screen, shadow cast with chromium at 10 deg and photographs taken using a Phillips Metallix electron microscope at an accelerating potential of 100 kv. A photograph of an etched sample of the as-oxidized material is shown in Fig. 2. We believe the pits in the photograph are places were A12O3 inclusions were sitting in the matrix. By inspection, it appears that the volume fraction ob-

Jan 1, 1960

By E. P. Pfleider, O. Rellensmann

For many years mine surveyors and exploration engineers have sought an accurate means of transferring meridian underground by using the gyro-compass. These efforts have generally failed, either because they were inaccurate or because the size and cost of the unit were prohibitive. During the past ten years, however, great strides have been made. Autonetics in California has developed a comparatively light-weight (100-lb) gyro-theodolite, and the Institute for Mine Surveying at Clausthal Mining Academy in Germany has developed an instrument that is accurate to within 20" to 30" of arc. Concurrently, Minneapolis-Honeywell has produced an astounding gyro, the size of a salt shaker, that weighs less than 0.5 lb and compares favorably in performance with the 50-lb gyros of conventional design. This unit, designed for missile guidance, should be adaptable for surveying small boreholes. Given the proper interest and approach from the engineering fraternity, excellent gyrocompasses could probably be available for accurate underground survey work at nominal cost within the next three years. Principles of the Gyro-Compass: The gyrocompass, used for 50 years as a navigational instrument in ships and aircraft, senses the turning axis of the earth and points out true polar north. It does this by employing the earth&apos;s rotation, the force of gravity, and the precession characteristics of a gyro. For further details the reader is referred to several excellent publications&apos;"3 covering the principles and application of the gyroscope. The heart of the gyro-compass is the gyroscope, or rapidly spinning wheel, which rigidly maintains its angular orientation in inertial space. Free gyros employ universal joints to allow the wheel axle to maintain its rigid spatial orientation independent of base motion disturbances. Free gyros are independent of the earth&apos;s turning and are not north-seeking. Only as they might be initially oriented parallel to the earth&apos;s turning axis could any north indication be obtained. In practice, the free gyro tends to drift off its set position and lose its accuracy. The Sperry-Sun Well Surveying Co. instrument (5M in O. D.) is of this free gyro type. It is counterbalanced, however, against the rotational effects of the earth, so that orientation of the spinning axis will be maintained throughout the survey.

Jan 1, 1960

By E. C. van Reuth

FIFTY-three alloys have been examined in the Fe-W and Co-W alloy systems in an attempt to verify the finding of o phases in these systems as reported by Goldschmidt.&apos; The alloys were examined metallographically and by X-ray diffraction. The 10-g specimens were made by powder metallurgy techniques. Very fine, high-purity powders were compressed in a double-acting die at 120,000 psi after hydrogen reduction. All compacts were then sintered for 200 hr at 950°C in a helium atmosphere. Metallographic investigation and X-ray diffraction proved this time to be sufficient to allow complete homogenization before the subsequent high-temperature anneal. Each specimen was then sealed into an evacuated silica capsule and annealed at 1400"or 1500 C (except two) for 25 hr. (The 60 pct Fe and 55 pct Co alloys taken to 1610"and 1680°C respectively were held at these temperatures for 1hr. However, since these structures were at equilibrium before the anneal, and in view of their resultant structures, it is assumed that they reached equilib-

Jan 1, 1960

Ferrous and Nonferrous Physical Metallurgy Established as a Division April 26, 1918 T A Read, Chairman O T Marzke, Past Chairman J H Jackson, Senior Vice-Chairman David Swan, Vice-Chairman D C Johnston, Secretary-Treasurer AIME, 29 West 39th Street New York 18, New York

Jan 1, 1960

By M. F. McCarty, R. S. Olson

New organic flocculants of high-molecular weight are replacing lime, glue, and starch in liquid-solid separation. Of these synthetic materials, poly-acrylamides are outstanding. Polyacrylamides form a class of compounds varying widely in composition and activity. Separan 2610, one of the first of these flocculants&apos; released to the mining industry in 1954, is described&apos; as a high-molecular weight polymer of acrylamide with or without a copolymer material and with some replacement of amide by carboxylic groups. MECHANISM OF FLOCCULATION In practice, flocculation makes solids settle faster and filter better. But two opposing factors control it. The random motion that causes particles to collide favors Van der Waals&apos; forces, which hold the particles together. The effect of zeta potential opposes this contact, and particles are mutually repelled. Flocculation can be achieved by reducing the magnitude of the zeta potential; this is the mechanism of flocculation by lime addition. The way in which polyacrylamides accomplish flocculation is not fully understood, but the action is undoubtedly comp1ex and probably varies considerably depending on the system. To begin with, the active groups of these compounds have an extremely high affinity for solid surfaces, probably by hydrogen bonding." Initially some active groups of the molecule attach themselves to the solids with a large portion of the molecule extending into the solution. Two particles can become tied together by long flocculant molecules in the following ways—by bonding between the active groups of two flocculant molecules on different particles, or by an extended molecule from one particle attaching itself directly to the surface of the other particles." These flocculant bridges prevent the particles from moving apart through random motion, but when such motion moves them together other active groups on the flocculant bridge bond to the solids, holding them in the closer position. This process is repeated until the particles are close together. Although bridging is probably a major flocculation mechanism, it is not the only phenomenon involved. Relatively neutral acrylamide flocculants reduce the magnitude of the zeta potential by increasing the viscosity of solution in the immediate vicinity of the solid surface which contains the mobile counter ions of the double layer. In other words, it moves the shear surface which bounds the zeta potential out into the solution containing counter ions which tend to neutralize the zeta potential. This effect is probably more pronounced during the initial adsorption period, before the flocculant molecules are pulled close to the solid. In some cases the slight charge of the polyacry-lamide molecule tends to neutralize a zeta potential. However, this is not a primary flocculation mechanism, as evidenced by the fact that the polyacrylamides will flocculate solids with either positive or negative zeta potential. Adsorption of polyacrylamide flocculants by a solid is substantially an irreversible reaction. Since the flocculant molecule is attached to the particle surface by many active groups of high bonding strength, desorption would require the simultaneous breaking of many bonds—an unlikely occurrence. UNIQUE PROPERTIES The irreversible adsorption of certain polyacrylamides, the flocculant&apos;s high affinity for solid surfaces and its rapid adsorption make it effective, but these unique properties require special techniques to achieve maximum flocculation. If flocculants of this type are added to a pulp as a relatively concentrated solution, the solids in the

Jan 1, 1960

By R. A. Vandermeer, P. Gordon

The study of recrystallization in cold-worked metals is complicated by the impossibility of making direct three-dimensional optical measurements. Metallo-graphically, theinternal three-dimensional features of samples must be inferred from their intersections with the two-dimensional plane of polish. The inherent difficulties involved in this procedure have led— particularly during the last few years—to some instances of rather doubtful interpretations of experimental data in terms of nucleation and growth rates in recrystallization. In the present paper an analysis ; is given of the recrystallization characteristics in a polycrystalline alloy containing 0.008 wt pct copper in ZONE-refined aluminum *and an effort is madf to reemphasize the necessity in such studies for attention to the proper statistical relationships between one- two- and three-dimensional features of opaque samples. It is shown that, in common with several recently described cases for other types of transformations,1-5 recrystallization in this alloy can best be rationalized on the basis that all nucleation took place essentially at time zero—i.e., there is no significant time-dependent nucleation during annealing—and that the kinetics are controlled exclusively by the growth-rate parameters. This is true despite the fact that the number of

Jan 1, 1960

By A. Cochardt, D. H. Feisel

HE success of the sintered aluminum powder material (SAP)&apos; in raising the maximum useful temperature of aluminum alloys has stimulated effort in investigating similar systems in which the metallic matrixes have higher melting points. Examples of such systems which have been studied are nickel-alumina,2, 3copper-silica,4 copper-alumina,4 titanium-cerium oxide,5 and 80/20 nickel-chromium,8 cobalt,= and molybdenum7 matrixes with various hardeners. Conventional precipitation-hardened high-temperature alloys are often thermally unstable in service. The original fine particles that are responsible for good strength properties grow in size at elevated operating temperatures, a process termed "over-aging." This growth of precipitated particles causes a gradual loss in strength properties. A previous paperb describes the factors that govern the process of overaging, and estimates the time required for overaging of a nickel-alloy matrix dispersion-hardened by various precipitates such as are found in current high-temperature alloys, and by alumina. These calculations indicate that nickel-base alloys hardened with Ni3Al, Tic, or TiN are quite unstable at 1340" F (727°F). Such alloys should overage within a few hours at that temperature. A nickel-base alloy hardened with alumina, on the other hand, should behave differently. It should not overage appreciably within a thousand years. It was further shown8 that the thermal stability of the oxide-hardened alloy is mainly due to the low solubility of oxygen in equilibrium with alumina in the nickel-base matrix. Since the oxygen solubility is small, little oxygen can diffuse, and structural changes require very long times. This paper illustrates the effects of time and temperature on the structural stability of nickel alloy matrixes hardened by dispersions of Ni3A1, Ni3Ti, Tic, and alumina, and of nickel-chromium matrixes hardened by alumina. Hardness measurements and metallography have been used as a measure of structural stability. EXPERIMENTAL PROCEDURE Using the best information from published phase diagrams,&apos;-l4 compositions of the Ni-Al, Ni-Ti, and Ni-Ti-C alloys were determined so as to have 5 vol pct of precipitate at 1350° F(732°C), the temperature selected to illustrate the effect of time on structural stability. Table I lists the chemical compositions of these alloys. Standard laboratory melting and alloying techniques were used in preparing ingots of the F-Series of alloys. The cast ingots, 1 3/4 in. in diam, were forged to 3/8-in. diam rods.

Jan 1, 1960

Executive Joseph L Gillson, Chairman, J W Woomer, Vice-Chatrman, John S Bell, Walter R Hibbard, Jr. R R McNaughton Finance John P Hammond, Chairman, James C Gray, J S Smart, Jr Investments Gall F Moulton, &apos;63, Chairman, Andrew Fletcher, &apos;62, John M Lovejoy, &apos;61, George I Brigden, ex off as AIME Treasurer, John P Hammond, ex off as Chairman, AIME Finance Committee Award Committees Grouped together at end of list Cooperation with the Canadian Institute of Mining and Metallurgy and the Mining Society of Nova Scotia R R McNaughton, Chairman, C Gerow, Sherwin Kelly

Jan 1, 1960