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By T. P. Clendenin

THE northerly two thirds of Mexico falls into five main physiographic divisions, illustrated on the accompanying map. In form, these divisions are a series of strips, paralleling the northwest-southeast axis of the country.

Jan 10, 1951

By A. D. Wilkinson

A CROSS-SECTION of the converter aisle through one of the converters and reverberatories is shown in Fig. 5. The aisle is 280 ft. long by 60, ft. wide by 681 ft. to the roof trusse, which have a 63-ft. span and are us )ported by steel columns spaced at 2b-ft. centers. Two 80-ton electric trails, supplied by the Welman Smith .Owen Engineering Co., with 20-ton auxiliary lifts, serve this building. Matte shells and converter-slag shells are dumped into heavily con¬structed flat-bottom bins located on the south side of the converter aisle and 1.0 ft. above the floor. The material is broken by ball and by hand, shoveled off into ladles for unloading on to the reverberatory charge floor, and charged into the furnace as previously mentioned.

Jan 1, 1934

1. What Effect Has Sulfur Or Vanadium (In The Oil) On The Steel With Your Burner? 2. Also, what is the decibel rating on the floor when your burner is on? AUTHORS' REPLY 1. There is no effect. 2. The decibel rating is 98-99 decibels.

Jan 1, 1972

By R. S. Shoemaker, F. W. McQuiston

CAMPBELL RED LAKE MINES Balmertown, Ontario 1974 Operating Data MINE LOCATION: Balmertown, in Red Lake mining area of Ontario TYPE OF MINE: Underground mine developed by vertical shaft to 4300 feet. Mining active above 3000 ft depth. ORE DESCRIPTION: Gold and minor silver.. Sulfur content about 1.3%. Ar senopyrite , pyrite, pyrrhotite, and stibnite. CAPACITY IN TONS124 HRS: 825 ASSAY: 0.66 oz Au per ton heads MILL PROCESS: Amalgamation, flotation, roasting of concentrate and separate treatment of calcines and flotation tails by cyanide. PLANT BUILDING: Mine mill and service facilities all housed in insulated and heated buildings POWER: Total consumption, mine and mill - 100 Kwh/T WASTE DISPOSAL: Impoundment of tailings. Arsenic to sealed underground storage EMPLOYEES: Total of 300 men on payroll. Housing in Balmertown and nearby communities.

Jan 1, 1975

The resolution drafted by J. W. Richards, J. V. N. Dorr, and Allen H. Rogers on the death of J. E. Johnson, Jr., and adopted by the Board of Directors, is as follows: "The Boards of Directors of the American Institute of Mining and Metallurgical Engineers wishes to place on record its great personal loss in the sudden death of Mr. J. E. Johnson, Jr., our fellow Director of the activities of the Institute, a member our Executive Committee, Chairman of the Institute's Committee on Admissions, and Vice-chairman of its Iron and Steel Committee. "A mere recital of these positions of trust and responsibility, which he filled with conscientious efficiency and marked ability, shows how greatly the Institute has lost by his death. No one else of the Institute's officers could have been so illy spared. We, his colleagues, take up his tasks with a sense of our inability to discharge them as well as he, and this with a doubled sense of our loss. "Others have written and spoken of the blow which his death has been to the furtherance of the metallurgy of iron and steel. His pre-eminence in this line is one of the facts of which the Institute is justly proud. Here his personality, originality, courageousness in advocating new principles, clearness of writing and forcible presentation of facts, are irreplaceable. His two great treatises on the blast furnace are his literary and scientific memorial.

Jan 7, 1919

By F. B. Plummer

PERHAPS the greatest progress made in the technical methods of oil production during the last year has been in handling gas from the new fields that yield light distillate fractions. At least sixteen recycling plants have been perfected and installed in South Texas fields alone during 1939 having a daily capacity of more than one billion -2 cubic feet of gas and capable of producing more than a million gallons of distillate daily. The process consists of running the gas under pres- sure through especially designed plants, separating out the condensate, then compressing the gas to 3000 lb. or more, depending on the subsurface pressure in the formation, and injecting gas back into the reservoir to be produced again later, along with more of the liquid hydrocarbons, and again recycled. Hence production in these distillate fields in sense has changed from that of producing a constantly diminishing and much-wasted product to a more or less continuous manufacturing process, in which practically all the gas is conserved-a real triumph in engineering practice.

Jan 1, 1940

By Gilbert P. Moore

Bolivia does not yet have any production which is being marketed. It does have a potential production, however, from wells which have been completed by the Standard Oil Co. of Bolivia, a subsidiary of the Standard Oil Co. of New Jersey. No other company is active in drilling and development work to date. The total potential production from wells now completed is about 6000 bbl, daily. Wells Completed Completions during 1928 and their initial daily productions. if any, were as follows: Camatindi No. 1, 350 to 1000 bbl.: Camiri No. 1, 500 bbl.; Sanandita No. 3, 100 bbl.; Tatarenda No. 1, dry hole, and Bermejo No. 2, deepened 50 ft. made 1000 barrels. The most striking development of the year was the Camiri No. 1 well which, after just entering the sand, made 500 bbl. per day of 52" B. oil. This well is the northernmost good producer which the Standard has brought in to date. Oil from this well is used without refining in the tractors and trucks of the company. A small topping plant has been installed from which high-grade gasoline is obtained for use in motor cars and some is being produced for the use of air plants stationed at Villa Montes. The results for Sanandita No. 13 were somewhat disappointing since Sanandita No. 2 was rated at about 3000 bbl. Tatarenda NO. 1, located on a large unbroken structure, was drilled to 4000 ft. and abandoned as a dry hole. Bermejo No. 2 was deepened 50 ft. to 2085 ft.. and on a 10-day test averaged 1000 bbl. per day. This well is on the border between Bolivia and the Argentine. Wells Drilling The wells drilling are Camiri No. 2, Sanandita No. 5, Machareti No. I and Bermejo No. 5. This is the smallest number of drilling wells which the Standard has had for several years but is principally due to

Jan 1, 1929

By Matti J. Saarivirta

Two new precipitation hardening copper-base alloys, Cu-1.5pct Ti-2.5 pct Sn and Cu-1.5 pct Ti-2.5 pct Sn-0.4 pct Cr were developed. High strength and medium conductivity are obtained by solution annealing and subsequent heat treatment. Combination of solution annealing, cold working, and heat treatment increases the strength further. Good elevated temperature strength and ductility makes these alloys superior to copper-beryllium-cobalt alloys. A considerable amount of research work is being done throughout the world to develop new and improved copper-base alloys. In many cases, the object is to develop alloys having a combination of high electrical and thermal conductivities, and high strength. The problem is complicated by the fact that any alloying element added to increase strength, invariably decreases conductivity. Among the few commercial precipitation hardening type copper-base alloys, the Cu-Be-Co alloys are best known. These alloys are used in many applications that require good spring characteristics cornbined with high strength and moderately high electrical conductivity. They can be formed readily after solution annealing, then heat treated to obtain high strength and conductivity. Because of the relatively high cost of the Cu-Be-Co alloys, considerable research has been aimed at developing new lower cost alloys having similar properties. As far as is known today, the binary Cu-Ti alloy is the only one whose properties are

Jan 1, 1962

By F. L. Grammer

In these day, when anthracite is less extensively used as a blastifurnace fuel than it was a generation ago, and managers endeavor to maintain regular and known ore-mixtures, the " freezing " of tuyeres, cinder-notch or iron-notch is infrequeut; and, consequently, the oil-burner or " kerosene blowpipe "* is seldom employed; and furnace-foremen have, to a considerable degree, forgotten their former cunning and persistency in the use of the drill and sledge. Still, in starting new or abandoned plants with untrained labor, and in running some of our large 100-ft. furnaces, slips, resulting in very cold furnaces, may occur, even under experienced managers. During my superintendence of the Cleveland, O., blast-furnaces, such a misfortune, owing to a dearth of trustworthy foremen, was experienced; and our electrician, Mr. Thomas Martin, proposed to open the tuyeres and cinder-notch by means of the heat of the electric arc. We have heard that the surface-cracks or marks developed in rolling heavy plates have been closed by electric welding, as by a soldering-iron, and also that an electric burner has been employed at some German blast-furnaces; but the experiment was quite novel to us; and I think it constituted one of the first, if not the very first, successful application of this device, for the purpose named, in the United States. †

Jan 1, 1902

By George B. Lee

DURING The Two Years In Which The New Reduction-Works Of The Copper Queen Consolidated Mining Co. Have Been In Operation At Douglas, Ariz., There Has Developed A Remarkable Condition In Regard To The Corrosive Action Of The Water Used To Cool The Jackets Of The Blast-Furnaces. Were It Not For The Many Contradictory Features, It Might Pass As One Of The Unavoidable Troubles Due To The Composition Of The Water. This Water, Obtained From Wells 600 Ft. Deep, Is Also Used In The Steam-Boilers, And Its Composition, As Shown By The Following Analysis, Does Not Indicate The Presence Of Any Ingredient Which Would Explain The Corrosion Grains Per U. S. Gal. Silica, 0.861 Iron Oxide And Alumina, 0.223 Calcium Carbonate, 0.2111 Calcium Sulphate, Magnesium Carbonate, Sodium And Potassium Sulphates, . 14.850 Sodium And Potassium Chlorides, 9.732 Sodium And Potassium Carbonate, 6.452 32.409 The Jackets Are Made Of Inner Plates 0.5 In. Thick And An Outer Plate I In. Thick, With 3-In. Stiffeners Between The Inner And Outer Plates. In From 10 To 12 Months The Inner Plates Have Been Reduced By Corrosion To A Thickness Of From 1/8 To 1/16 In., While The Outer Plate In The Same Time Is Reduced By Less Than 1/16 In., And The Stiffeners Show Very Little Corrosion. The Plates Are Pitted And Eaten Away In Some Places More Than In Others. There Is Practically No Scale Found On The Jackets, But When Cleaned Considerable Iron Oxide Is Found In The Bottoms. With An Action So Marked, Serious Trouble Would Be Expected In The Boilers, But, On The Contrary, A Recent Inspection By a

Mar 1, 1908

By R. E. Crater

Brown, Gaudin, and Loeb in their study of intergranular comminution by heating attempt to find one explanation for all types of rock in terms of the properties of the phases present. The only necessary condition for intergranular cracking by heating is the setting up of high stresses at the grain boundaries. Such stresses may be set up in multiphase isotropic mixtures if the thermal expansions of the phases are different, in non-cubic single phases because of the anisotropy of thermal expansion in the various crystallographic directions, and in materials containing quartz because of the a-ß transformation at 575°C. In addition, for intergranular comminution by heating, the cooling and not the heating is most important.

Jan 3, 1959

By Richard W. Lodge

Ix the crucible-method of assaying ores for silver a certain amount of litharge is essential to supply sufficient lead to collect the precious metals. The object of this paper is to point out that the use of a .large excess of litharge in the assay of some ores will give results for silver that are uneven as well as low. So far as I know, however, an excess of litharge does not affect the results obtained in the crucible-assay of ores for gold. The main reasons for using, in the crucible-assay, much more litharge than is required to give the necessary lead button are : 1, its action as a flux; 2, its action as a desulphurizer; and 3, its action as an oxidizer, especially on metals like copper and nickel, whereby they are forced into the slag as oxides and thus prevented from passing into the lead button. Hence, by the use of much litharge in the crucible-assay more-ore can often be taken than in the scorification-process, and a lead button obtained which can possibly be cupelled at once or after a single scorification. The method is specially advantageous with an ore carrying much copper or similar impurity and poor in silver, when the assayer does not wish to resort to a wet-analysis for the determination of the silver. It is well known that some ores give better results when assayed by the scorification-method, while others give better results by the crucible-method. For several years I have noticed that, when much litharge was used with certain sulphide and arsenical ores, the results were considerably lower than when the scorification-method was used. This fact was more forcibly brought out in connection with certain work carried on this year by Messrs. H. A. Frame and

Sep 1, 1907

Through the generosity of Sir Robert Hadfield, Honorary Member, the Directors of the American Institute of Mining Engineers are enabled to announce the Hadfield Research Prize of $1,000 for the best contribution to the publications of the Institute upon the general subject of The Different Forms and Combinations of Carbon with Iron, including those in Iron Alloys. The prize will be awarded at the Annual Meeting of the Institute in February, 1916, to the best paper upon this subject which is presented to the Institute before Nov. 1, 1915, provided such paper is deemed worthy by the Institute's Iron and Steel Committee. The following suggestions are also added for the guidance of those who may take part in this research. While it is not desired to define closely the exact lines or scope of the proposed research, as it is advisable to make these as broad as possible, the object in mind may be said to be generally as follows: To elaborate and find out the best methods of determining the forms of carbon in steel or iron, including those in iron alloys. A portion of the work would probably be a continuation of the researches which have in the past been carried out by Jullien, Abel, Muller, Ledebur, T. Sterry Hunt, Akerman, Arnold, Stead, E. D. Campbell, Hogg, Parry, Upton, and others.Through the generosity of Sir Robert Hadfield, Honorary Member, the Directors of the American Institute of Mining Engineers are enabled to announce the Hadfield Research Prize of $1,000 for the best contribu¬tion to the publications of the Institute upon the general subject of The Different Forms and Combinations of Carbon with Iron, including those in Iron Alloys. The prize will be awarded at the Annual Meeting of the Institute in February, 1916, to the best paper upon this subject which is presented to the Institute before Nov. 1, 1915, provided such paper is deemed worthy by the Institute's Iron and Steel Committee. The following suggestions are also added for the guidance of those who may take part in this research. While it is not desired to define closely the exact lines or scope of the proposed research, as it is advisable to make these as broad as possible, the object in mind may be said to be generally as follows: To elaborate and find out the best methods of determining the forms of carbon in steel or iron, including those in iron alloys. A portion of the work would probably be a continuation of the researches which have in the past been carried out by Jullien, Abel, Muller, Ledebur, T. Sterry Hunt, Akerman, Arnold, Stead, E. D. Campbell, Hogg, Parry, Upton, and others.

Jan 1, 1917

By Marius R. Campbell

VARIOUS classes of coals are recognized in this country at the present time. These classes depend largely upon physical characteristics rather than upon chemical composition, and consequently they cannot be accurately defined. The divisions into anthracite, semi-anthracite and semi-bituminous are fairly satisfactory; but the term bituminous embraces so large a variety of coal that it is of little value, and the term lignite is so loosely applied that it has little or no place in a scientific classification. At present there is no way of accurately defining the vari¬ous classes of coal, because no adequate scheme of classification, which applies to lignites as well as bituminous coal and anthracite bas been proposed. The object of this paper is to present such a scheme, which is based upon data obtained dur¬ing the past year by Prof. N. W. Lord,1 in charge of the chemical laboratory of the United States Geological Survey coal-testing plant at the Louisiana Purchase Exposition, St. Louis. All the classifications of coals proposed prior to 1877 were based either on physical characteristics or on proximate analyses, including all of the impurities. These schemes were illogical and highly unsatisfactory, for the physical properties of a coal give little indication of its true composition; and impurities, such as ash and sulphur, are largely the results of acci-

Sep 1, 1905

(Members are urged to send in for this column any notes of interest concerning themselves or their fellow-members.) Members and guests who called at Institute headquarters during the period July 10, 1916 to August 1, 1916: W. A. Barnes, San Francisco, Cal. W. J. Mead, Madison, Wis. W. L. Bell, Davenport, Fla. Charles Mentzel, San Pedro, N. M. James P. Clarke, Jr., Little Rock, Ark. H. H. Miller, New York, N. Y. R. A. Carhart, Mitchell, S. D. W. E. Pomeroy, El Paso, Tex. G. M. Colvocoresses, Humboldt, Ariz. M. K. Rodgers, Los Angeles, Cal W. E. Defty, Phoenix, Ariz. S. C. Rodgers, Guanajuato, Mex. Carl F. Dietz, Worcester, Mass. John M. Baker and Hamilton W. Baker have resigned as general manager and mine superintendent respectively of the Baker Mines Co., of Oregon. After Aug. 1, their address will be 43 Emerson St., Denver, Colo.

Jan 9, 1916

By C. BARING HORIVOOD

(Chattanooga Meeting, October, 1908.) THIS paper is intended, in the light of recent investigations, to call attention to some of the essential features of good practice in sampling and mine-valuation. Mine-sampling may be divided broadly into two classes : (1) development-sampling and computation of ore-reserves; and, (2) stope-sampling and estimation of stope-values. DEVELOPMENT-SAMPLING. It is with development-sampling only that this paper deals-the term development being taken to mean the opening-up of a mine by cross-cuts, drives, connections, etc., preparatory to actual extraction of the ore for milling. In development-sampling the work of the sampler and the consequent estimation of the probable value of the mine or portions of the mine, as the case may be, cannot be verified until a later period, when the ground thus sampled has been exploited; hence, extreme care and accuracy are essential. Moreover, the development-sampler has to foresee and allow for contingencies which may arise when stoping is started. It follows that the sampling, in development-work, demands familiarity with the conditions likely to be encountered later in actual mining. In stopes, on the other hand, sampling is clone under actual working-conditions, and the sampler's valuations are immediately checked by the gold-output, or in some cases by a second sampling of the broken ore. A stope-sampler therefore need not be an experienced miner, though he should possess sound technical training and work accurately. Should he be somewhat inexperienced, be soon has his errors discovered for him, and learns to avoid them. Taking these facts into account, it is obvious that a mining company employing two or more samplers should

Jan 1, 1909

By P. M. Robinson, M. B. Bever

The heats oj formation at 273°K of the compounds CdTe, I)z2Te, InTe, In2Te3. In2Te5, SrzTe, and PbTe have been rleasrred in a liquid metal solutiotz caloritrete? 1.t1itlz bismuth as solvent. The?, are iterpretecl in yelation to tlze stability and bonding of the cott/pozltzds. Tile heats of fusion atzd the melting- points of tlze cotlzpounds InTe and Itzz,Te3 1lcti.e been measured in a cotrslant-temperature gradient calorimeter. The entropies of fusion are disc,ztssecl in YIIIS 01. the degree of order in the solid at the melting point. THE heats of formation of the tellurides of cadmium, indium, tin, and lead have been measured as a continuation of research on the thermodynamic properties of compounds of tellurim.' The tellurides of these metals were selected with a view to examining the relation between the heat of formation and the position of the metal in the periodic system. The elements cadmium, indium, and tin are in the same period and tin and lead are in the same group of the periodic system. The tellurides of indium are of special interest because four compounds, In2Te, InTe, In2Te3, and InzTe5, occur in this system. The available information on the heats of formation of the compounds investigated consists of values for CdTe, SnTe, and PbTe derived from electromotive-force measurements,J a value for CdTe obtained by tin solution alorimetr, and values for InTe and In2Te3 determined by combustion calorimetry.5 These values, however, refer to various temperatures ranging from 273' to 673°K and some of the reported error limits are large. Liquid metal solution calorime-try may be expected to yield more accurate values for the heats of formation than electromotive-force measurements or combustion calorimetry. The heats of fusion and the melting points of the compounds InTe and In,Te3 were determined in a constant-temperature gradient calorimeter. No published information appears to be available on the heat of fusion of these compounds. The results reported here give an indication of the degree of order in the solid compounds at the melting point. 1) MATERIALS AND EXPERIMENTAL PROCEDURE Materials. Samples of the compounds SnTe and PbTe were obtained from the Westinghouse Research Laboratories and samples of the compound InTe from Lincoln Laboratory, Massachusetts Institute of Tech- nology. Additional samples of the compounds InTe, SnTe, and PbTe and samples of CdTe, In2Te, In2Te3, and In,Tes were prepared from 99.995 pct Cd (Baker Chemical CO.), 99.999+ pct In (American Smelting and Refining Co.), 99.99 pct Sn (Baker Chemical Co.), 99.999+ pct Pb (Fisher Scientific Co.), and 99.999+ pct Te (American Smelting and Refining Co.). Stoichiometric amounts of the component elements were melted in sealed, evacuated Vycor tubes. The melts were held at approximately 100°C above the liquidus for about 16 hr and shaken repeatedly. The melts of the compounds In2Te and InzTe5, which form by peritectic reactions, were quenched into iced water. The melts of the other compounds, which have congruent melting points, were slowly cooled to room temperature. The samples were then annealed for 5 days at approximately 50°C below their respective solidus temperatures. Metallographic examination did not reveal any evidence of second phases or segregation. At least two batches of each compound were prepared. Samples from each batch were used in determining the heats of formation and, in the cases of InTe and In,Te3, the heats of fusion. The Heats of Formation. The heats of formation at 273°K of the compounds were measured by metal solution calorimetry with liquid bismuth at 623" as solvent. In this technique, the heat of formation is determined from the measured heat effects on dissolution of the compound and of a mechanical mixture of the component elements. The difference between these heat effects adjusted for changes in the composition of the bath gives the heat of formation at the temperature from which the samples are added to the bath (273°K). The experimental technique and method of calculation have been described in detail elsewhere.= It should be emphasized that the reported heats of formation depend on the thermodynamic data used in calculating the heat effects for the calibration additions. In the present investigation, the calorimeter was calibrated by adding pure bismuth at 273°K to the bismuth bath at 623°K. The reported heats of formation are based on a value of 4.96 kcal per g-atom for the difference in the heat contents of bismuth at 623" and 273". If a new value for this quantity becomes available, the reported results may be adjusted in direct proportion. The concentration of solute in the bath at the end of a calorimetric run did not exceed 1.7 at. pct and was usually less. In this range, the heat effect on dissolution of the solute was a linear function of the concentration of solute. In determining the heats of formation of the compounds in the system In-Te, a few runs were carried out in which two neighboring compounds such as InTe and In,Te3 and the corresponding mechanical mixtures of the components were added to the calorimeter. The

Jan 1, 1967

By T. Cantwell, N. C. Rasmussen, H. E. Hawkes

Beryl is a mineral that may be difficult to distinguish from quartz by casual field inspection. The easily recognized green color and hexagonal crystal form of coarse-grained beryl are by no means universal, even in beryl from pegmatitic deposits. If it occurred as a fine-grained accessory mineral in an igneous rock, it would almost certainly escape detection unless samples were submitted for petrographic or chemical analysis. There may be substantial deposits of some beryllium mineral, other than beryl, that has been overlooked because that mineral also closely resembles the common rock-forming minerals. A reliable and simple method of identifying beryllium minerals and determining the beryllium content of a rock would be helpful in exploration. This article describes preliminary experiments in applying nuclear reaction to the qualitative identification of beryl and to the semiquantitative determination of the beryllium content of rock samples.

Jan 9, 1959

By J. A. Fellows, Earnshaw Cook, Howard S. Avery

HEAT-RESISTANT alloys of the higher nickel and chromium ranges have been empirically developed through the practical experience of the past two decades to a position of significant industrial importance. Few quantitative metallurgical data have been published, however, that could be related directly to engineering specifications and design. Inadequate information led to the inauguration, in 1934, of a research directed toward a better understanding of the properties and performance of these steels at temperatures between 1400° and 2000°F. Investigation was concentrated upon the 26 per cent Cr:12 per cent Ni type, which owes its extensive application to an excellent combination of economy, strength and surface stability at elevated temperatures. The requirements of the oil-refining industry have been prominent in influencing the scope and evolution of the program. Creep strength at the maximum allowable deformation ranges has been employed to evaluate the merits of these alloys. Permissible elongation rates vary from 1.0 per cent in one million hours for turbine blades to 1.o per cent in ten thousand hours for tube supports and heating-furnace equipment. Throughout this paper, the limiting creep stress (L.C.S.) for a given temperature has been defined as the stress that will produce a uniform elongation rate (stage II) of one per cent in ten thousand hours as extrapolated from rates per hour or tests of less than two thousand hours duration. Certain current specifications require a minimum L.C.S. of 1600 lb. per sq. in. at 1800°F., of 3600 lb. per sq. in. at 1400°F., and include a tensile acceptance test at room temperature, after aging for 24 hr. at 1400°F., as a measure of embrittlement in service. An elongation of 4 per cent is considered satisfactory for general use, while a minimum of 9 per cent is prescribed on occasion. Many differences of opinion concerning the properties and performance of these alloys appear to result from their sensitivity to unappreciated variations of chemical analyses which, for example, may change their L.C.S. from 3500 to 350 lb. per sq. in. at 1800°F. Within broad chemical limits, it is possible to balance the six or more important elements present to attain desirable properties with a number of different combinations. One method for adjusting the composition has been described under the sponsorship of the Alloy Casting Institute,1 in which, by maintaining a substantially austenitic* alloy, optimum creep strength and minimum tendency to embrittle after aging are expected. Unless, however, the limits are undesirably dose, it has not been possible to ensure a moderate range of strength and of ductility by any chemical specification alone. There is a definite need

Jan 1, 1942

By N. E. Rogen, N. J. Grant

WHILE direct measurements of the growth of precipitate particles during aging is of fundamental value, few such measurements have been made. Direct measurements by means of optical or electron-microscopy and X-ray techniques are preferred, however, many of the aging studies have been based on indirect methods such as electrical resistivity and hardness. Because of the minute size of most precipitate particles (less than 1000A) the light microscope is of limited use while electron microscopy is subject to slowness, etching problems and consequent resolution problems. It is fortunate that alloys of the Nimonic type, based on Ni-Cr-Ti-Al, lend themselves to accurate and relatively easy particle size measurements. With proper balance of titanium and aluminum, the only aging precipitate is the gamma prime (r') Ni3,(Al, Ti)2 phase and this phase is the basis of the high-temperature strength of these allos.3-6 The Ni3(Al, Ti) phase is a face-centered-cubic, ordered structure with nickel atoms occupying the cube faces. Titanium atoms can replace three out of every five aluminum atoms and when substituting do so preferentially.2 Electron microscopy has shown that during aging of most of the commercial alloys of this type, precipitate particles are unusually uniform in size and distribution, and that the volume of (r') phase is large (20 pct).4,7 The aim of this investigation was to measure the growth of (y') phase during aging. In so doing, it was hoped that a clearer understanding of the aging process would be attained. X-ray line broadening was used as the measure of precipitate particle size. This technique was selected because it can measure and average the diameter of thousands of particles in one operation. The variations in hardness and matrix lattice parameter with aging were also studied and related to the particle size. EXPERIMENTAL PROCEDURE An alloy of the following composition was studied: Cr Ti A1 C Ni Wt pct 20.71 2.98 1.43 0.04 bal. At. pct 22.06 3.47 2.95 0.18 bal. The alloy, a 15- lb vacuum melt, was forged to 1/2-in. diam at a temperature of 1900" to 2200°F; was solution heat treated for 4 hr at 2000°F and water quenched; and was then aged in various ways. The ASTM grain size was 4 to 5. No (7') phase could be detected by X-ray analysis after solution treatment and electrolytic extraction. Aging was performed on 2-in. long specimens at 1400°, 1500°, and 1600°F for increasing times. One-half inch sections were removed after each time increment and were then electropolished in a solution of H3P04 saturated with chromium trioxide at a potential of 30 v and rectified with a tantalum electrode. Rockwell hardness measurements were taken using one side of the polished specimen. Matrix lattice parameter determinations were made on the other side using filtered chromium radiation references with the position of the (220) line of a silicon standard. To enable the precipitate particles of the (y') phase to be measured using X-ray line broadening techniques, it is first necessary to separate and concentrate this phase by electrolytic extraction. Extraction is necessary because the difference between matrix and precipitate lattice parameters is only approximately 0.5 pct and intensities of.the (y') phase lines are very weak relative to those of the matrix. The extraction techniques employed have been described before and found to produce a reasonably quantitative separation.398 A water solution of 15 pct H3Po4 is used at a current density of 0.5 amp per sq in. at 6 v. The precipitate particles are separated from the liquor by centrifuging and decanting and are then washed, dried and repowdered. A plot of the X-ray intensity vs diffraction angle for the (111) line of the precipitate particles was used as a measure of particle size. The intensity curve approximated the shape of Gaussian distribution function and its breadth was measured at the half height. The (220) line of a silicon standard was used to correct the measured line breadth for instrumental and other broadening errors. The Scherrer formula was used to calculate particle

Jan 1, 1961