Search Documents

By W. J. West, T. D. Mueller, J. E. Warren

The authors have presented valuable information on the influence of the interfacial tension and the contact angle on the recovery efficiency of the waterdrive process. It is considered, however, that the following points deserve a closer examination. 1. As pointed out by Wyllie and Spangler1 the displacement pressure PD i.e. the pressure required to initiate the displacement of the wetting phase from the core, is a measure of the maximum pore diameter dmax. If the capillary pressure Pe as a function of the wetting

Jan 1, 1956

PRESIDENT Truman's economic report to Congress calls for an increase of 40 billion dollars in the value of goods and services produced in the United States by 1955; this is an increase of 16 percent over our 1949 production. If such an increase is to be realized, it will be possible only by a comparable increase in the production of steel-the keystone of our economy. Going one step further, since the raw materials of steel are iron ore, limestone, and coal, the President's goal can be reached only through the efforts of the mining industry. Coal and limestone reserves are not critical at this time, but the abundance of iron ore reserves has been subject to controversy. In this issue we proudly present "Cerro Bolivar--Saga of a Crisis in Iron Ore Averted" (a story which has been seven years in the making and three years in the getting).

Jan 2, 1950

By J. A. Reeves

The unit-train for moving mineral raw materials is considered by many railroad men as the most significant contribution toward reducing rail freight costs since the introduction of the diesel locomotive. The idea, which involves assigning railroad equipment to only one haul and keeping the equipment rolling, results in the maximum utilization of equipment. For example, before the unit train was placed in service on coal hauled to one of Mid-Continent Coal and Coke Company's customers, about 900 cars and 9 locomotives were needed to move its coal requirements, compared with 250 cars and 6 locomotives currently used. If unit-train economics are to be achieved, coal companies cannot use railroad cars as small storage bins on wheels to accumulate their coal in train-load shipments, instead, these companies must build large bins which incorporate facilities for the rapid loading of railroad cars in a minimum length of time.

Jan 1, 1970

There are no data available of shipments until 1858, and then estimated, when railroad service became available. By reason of the iron made in the county, and the large amounts of salt, the tonnage used locally was quite large, and until 1860 these are estimated from the probable salt and iron production. After 1859 the tonnages shipped by rail are partly estimated from the total shipments of the Allegheny Valley Railroad from four counties. It is believed that the totals are below, rather than above, what the actual production was. While considerably larger for the same years than figures given by the Secretary of Internal Affairs and census reports, these data were always too low in those days, partly because of lack of facilities for gathering them, but more largely because of the strong prejudice existing in those days against furnishing such data to any governmental agencies.

Jan 1, 1942

THREE-QUARTERS of the amount needed to defray the cost of the Louvain memorial clock and carillon has been subscribed by one-thirtieth of the total number of mem- bers of the engineering societies that are indorsing this memorial to the engineers who gave their lives in the Great War. Gifts of materials and services have been made, but about $20,000 is still needed to meet the total expense involved. Small contributions from the twenty-nine-thir- tieths of the total membership who have not yet subscribed should promptly provide this sum. The accompanying illus-tration shows the 48 gold stars made by the American Brass Co. for the four faces of the clock, being boxed for shipment at the works of the Dwight & Lloyd Co. at Netcong, N. J. The actual material of the stars is, of course, an aluminum bronze, which retains its gold color without tarnishing.

Jan 5, 1928

Considerable discussion took place at the June 18th Board of Directors Meeting concerning ways the Petroleum Branch office in Dallas could better serve its members and the essentially Petroleum Local Sections, namely the Delta, East Texas, Gulf Coast, Kansas, Mid-Continent, North Texas, Oklahoma City, Permian Basin, and Southwest Texas. The question of whether decentralization strengthens or weakens the Institute was debated, particularly as to what services could be advantageously decentralized and how both offices could keep informed on their mutual problems. Among other things, it was decided that an Auxiliary Admissions Committee could screen applications from Petroleum members before final action by the National Admissions Committee in New York. Finally it was voted, "That all administrative matters that can be properly delegated to a Branch organization may be so delegated". Final details were approved at the July 16th meeting of the Executive and Finance Committees.

Jan 1, 1952

The Institute offers two distinct relationships to. students: one is an individual relationship as a Student Associate; and the other is a relationship with local organizations of students, known as Student Chapters of the AIME This individual relationship is set forth in Section 8 of Article I of the AIME Bylaws, as follows "A student in good standing in an approved school, who has been nominated by at least three instructors of the nominee (one of whom must be an Institute member), may affiliate with the Institute as a Student Associate by payment of $4.50 annual fee, for which he shall receive one monthly journal and be privileged to attend meetings of the Institute and to use the Engineering Societies Library and the Personnel Service A student may remain such until December 31 of the year in which he ceases to be in university residence as a student "

Jan 1, 1952

The income of the Institute is derived from dues, subscriptions to MINING AND METALLURGY and sale of publications. These sources are fortunately supplemented by the interest from invested funds now amounting to over $500,000, a considerable portion constituting endowments for especial purposes. Aside from the medal funds the principal endowments are the James Douglas Fund for support of the Library, the Rocky Mountain Fund and the Seeley W. Mudd Memorial Fund. The income from the two last named is available for the support of research and a variety of other purposes. It is allocated by the Board of Directors upon recommendation of standing committees in each case. An active effort is being made to increase the endowments of the Institute, it being felt that unusual opportunities exist for research and public and professional service through the organization and at a minimum of expense.

Jan 1, 1932

By GEORGE H. DERN

IF THE engineer is to go into politics, as I think he should, I believe the curriculum of every engineering school should be amended to include a good stiff course in public speaking. My observation has been that the engineer in private conversation can scintillate as brightly as a life insurance agent or an oil stock salesman, but before an audience, with rare exceptions, he is a total loss. He will not get up and talk. He hides his light under a bushel, and sits on the bushel as dumb as an oyster. I have seen meetings of the Utah Section at which some topic of general interest to the members was up for discussion, and where an animated debate was the logical thing to expect. After the chairman states the subject and invites discussion, there is dense silence. Finally a member, bolder than the rest, gets up and with trembling voice and knees makes a motion. The motion carries, the meeting adjourns, and then the members gather into groups and begin to discuss the question seriously -and intelligently, giving cogent arguments on either side and embellishing their remarks with appropriate or inappropriate epithets illustrations and figures of speech. Now, I am not pleading for more speechmaking. The good Lord knows we have too much of this great American indoor sport already. But I think every man ought to be able and ready to express his opinions at the proper time. Some men have a reputation for wisdom because they do not talk much. We speak of the wise old owl because she never speaks, but in my opinion the owl's reputation for wisdom is vastly overrated. silence is more apt to be a cloak for stupidity than for wisdom. The person who has ideas can- not exert any influence by keeping them locked up in his own mind. The great motive force of the world is not muscle, but ideas, and ideas in order to get in their work must be released.

Jan 1, 1925

By T. D. Yensen, N. A. Ziegler

The elements aluminum,' arsenic,2 silicon,3 tin2 and vanadium,~.~ when used in relatively small amounts as alloying elements, seem to have a beneficial effect on the magnetic properties of iron—i. e., they increase the maximum permeability and decrease the coercive force—whereas there are definite indications that boron,5 carbon,6 nitrogen: oxygen," phosphorus16 sulfur6 and titaninum,~ as well as the metals of and adjacent to the ferromagnetic group, nickel,~ cobalt,1° copper," and manganese,% have a detrimental effect on these properties. The effects of calcium4 and magnesium4 are small, if any, while the effect of chromium12 in small amounts is unknown and in large amounts is generally detrimental. WeveR's Classification13 All chemical elements may be divided into three classes based on their effect on the allotropic transformation points of iron. Class 1 contains the nonmetallic elements (except phosphorus) and these lower the A3 point and raise the A4 point. Class 2 contains the common metals and

Jan 1, 1931

By E. Buehler

THE floating zone refining technique'-4 has provided a new experimental approach to the purification of many reactive materials especially those with high melting points. The method avoids the use of a crucible and at the same time it provides a favorable environment at the freezing interface for the growth of single crystals. The physical properties of refractory metals such as molybdenum and tungsten have long been of interest from a fundamental point of view and because of their widespread use in vacuum electronics. Single crystals are often desirable for study. Prior to the introduction of zone melting, single crystals of these metals were usually grown in the solid state at temperatures slightly below the melting point by strain annealing3 or by the application of a moving temperature gradient. Such techniques were mostly successful on wires, ribbons, or rods having small cross-sectional areas. Recently, larger samples of tungsten, molydbenum, tantalum, columbium, and rhenium were melted by a floating zone process which employed electron bombardment heating.10 Single crystals were obtained in many instances

Jan 1, 1959

By F. Habashi

Conclusive evidence is given showing that the dissolution of gold in cyanide solution follows mainly the over-all equation A similar equation can also be written for the dissolution of silver. Theoretical derivation of the velocity equation for this reaction has been obtained, which describes quantitatively the experimental facts. The equation is as follows: where [CN-] and [O2] = the concentrations (in moles/ml) of cyanide and dissolved oxygen, respectively. DcN- and Do2 = the diffusion coefficients of cyanide and dissolved oxygen; 1.83 x 10-5 and 2.76 x 10-5 cm2 sec-1, respectively. A = the surface area of the metal in contact with the aqueous phase, in cm S = the thickness of the boundary layer; varies between 2 and 9 x 10-3 cm, depending on the speed and method of agitation. Rate being expressed in g. equiv. sec-1. INTRODUCTION During recent years a number of papers have been published on the kinetics of dissolution of gold and silver in cyanide solution.1,6 The authors agree that the rate of dissolution is diffusion-controlled, but disagree regarding the mechanism of the reaction. Some authors'-3 support the Bodlander equations: The apparently conflicting results, when critically reviewed, are concordant and lead to the conclusion that the proper equation for the dissolution reaction should be only Eq. 1. This conclusion is based on the following facts: 1) For every 2.2 equivalents of metal dissolved one mole O2 was consumed. 2) For every 1 equivalent of metal dissolved, 2 moles of cyanide were consumed.' 3) Hydrogen peroxide is formed during the dissolution of gold or silver, and for every 2.2 equivalents of metal dissolved, one mole H2O2 was produced.1,2 The fact that Kudryk and Kellogg4 did not detect H2O2 during the dissolution of gold should not throw doubt on the many affirmative reports of other investigators. Lund2 has shown that depending on the crystalline nature of the silver surface, (e.g. method of etching the sample) H2O2 may undergo catalytic decomposition heterogeneously according to: Further Kudryk and Kellogg4 carried out their experiments in the presence of 0.5% KC1 to achieve a greater electrolytic conductivity, and Matsudaira7 has shown that H2O2 is catalytically decomposed (homogeneously) in the presence of C1- ion in alkaline solution. 4) Experiments carried out by Boonstra8 and Lund2 showed that the dissolution of gold and silver respectively in KCN + H2O2 in the absence of oxygen was a slow process. Thus the reaction takes place to a minor extent only. Further kinetic studies showed that: 1) The rate of dissolution depends on the surface area of the metal in contact with the liquid phase, thus indicating that the process of dissolution is a heterogeneous process. 2) The rate of dissolution depends on the speed of stirring,5,6 thus indicating that the process is controlled by a physical phenomenon.

Jan 1, 1967

By D. C. Hilty

C. E. SIMS*—This is a most interesting and important paper. It is important from two standpoints. First, it has as-spects of being highly accurate and therefore extremely useful to the operating man in showing how far he can go in oxidizing carbon from a steel bath while retaining chromium and the effect of temperature on this limit. Fig 5 is undoubtedly the highlight of the paper, and in checking it against available data, it seems capable of predicting actual results. The other important aspect is the apparently significant fact that reactions within a steel bath, such as between carbon and an oxide, are homogeneous reactions which do not require equilibrium with an external phase. In this case, it seems obvious that the reaction and the equilibrium established were between dissolved carbon (or carbide) and dissolved CrO. The classic reaction which requires equilibrium with solid Cr2O3, did not fit the data. It was recognition of this principle that made Fig 5 possible. G. R. FITTERER*—It might be in assuming the CrO is dissolved in the metal that you are actually approaching the correct factor for activity. If that is true and if the percentages that were used represent an equilibrium constant, this would mean, in effect, that the minimum temperature at which chromium would be reduced by an equivalent percentage of carbon would be about 2400°F from your equation. I believe that is in line with my experience particularly if you deal only with low percentages. J. CHIPMAN†—The author in discussing the equilibrium of the reaction offers two choices of explanation. One postulates an effect of chromium on the activity coefficient of carbon; it would require perhaps more data than are available to us at the present time to test this thoroughly. The other postulate which he offers is a reaction with CrO. This explanation is consistent with physical and chemical principles provided that a solid phase CrO is present, and that is essentially what he is postulating. If that oxide were present one would expect and, I think, almost require the kind of results that he obtained. The weakness of that postulate lies in the lack of confirmatory evidence regarding the presence of solid CrO as such. This should offer an interesting subject for further study. It seems a pity that the theoretical arguments revolving around CrO should have obscured for a moment the very real excellence of this paper. E. CARTER*—I think there is a problem that presents itself in practical application where the metal temperature is from 3200 to 3300 and the temperature desired in pouring is considerably less. B. M. LARSEN†—I get the impression from some of the work that was done earlier that there is probably a localized zone of high temperature at the slag metal interface which effects the removal of the carbon. Without that I wonder if the effect is possible to have a localized superheat and an equilibrium there favorable to low carbon content and

Jan 1, 1950

Reports on process control computer projects at the Kamioka Plant are summarized from the Japanese technical literature (see references). Fluidized Bed Roaster and Sulfuric Acid plant1 A small process control computer (Yokogawa CCS-200 with an OKITAC 5090P 8K central processor) was installed in the Kamioka smelter in the summer of 1964. A year-and-one-half installation project followed, which successfully brought the roaster and acid converters under computer control. The process plant consisted of two 130 RPD fluosolids roasters and two Monsan to acid units. The roasters are charged with lead-zinc concentrates with SO2 from the roaster processed to sulfuric acid. The computer system provides the following functions: 1) log data from the plant--the input is taken from 50 analog signals, 130 high-low digital alarm points, and 50 analog high- low alarm points; 2) set-point control on 18 control loops; 3) direct digital control (DDC) on eight control loops for which conventional controllers were difficult to adapt due to abnormal loop characteristics or delay times; 4) execution of a safe shut-down procedure

Jan 1, 1969

By Paul L. Burkhart

THOUGH at an earlier period brief studies had been made by the Lehigh Navigation Coal Company Inc., it was not until 1924 that J. B. Warriner, then general manager, called for a comprehensive study of timber treatment, treating solutions, and related operations. Because of the impossibility of procuring accurate costs and other pertinent treating data, the American Wood Preserving Co. agreed to treat a car of mine timber at the Port Reading plant of the Reading Railroad. Fig. I shows the treating data collected at the treating plant on this timber, which was installed in two of the Lehigh mines in 1925. [ ] In the latter part of 1925, a survey of the tunnels and gangways of the company's Panther Valley mines was made to determine the proportion of gangways or tunnels timbered, cause of timber failures, approximate life of the average wood set and the approximate percentage of treated timber that it would be profitable for the company to use. Results of this survey appear in Table I. Because of the high percentage of timber that gave evidence of failure by rot, as noted in Table I, and a further study of the life of the sections where timbering was necessary, it was deemed advisable to fill 25 per cent of the yearly gangway timber requirement with treated timber. QUANTITIES AND TREATMENTS OF TREATED TIMBER PURCHASED In the early days of the program, none of the large treating companies would accept orders for small quantities of treated timber and the company was compelled to state the quantity of timber it would require at each operation in each month of the year. Table 2 is an example of the tabulation given to the various treating companies to assist them in making a yearly bid on the minimum quantity of timber required by the company during the year 1931. A bill of timber was calculated for each car, the weight of which would be between the minimum and maximum weight permitted for railroad-car loading. The treating company was paid for timber upon delivery at the operation specified. As extra cars of timber were required, they were ordered from the treating company, and payment was required on their receipt, on the basis of the piece or tonnage

Jan 1, 1942

Organization Place Date 1918 American Chemical Society Cleveland, O. Sept. American Society of Sanitary Engineers Chicago, 111. Sept. National Petroleum Association Atlantic City, N. J. Sept. American Institute of Mining Engineers Colorado Sept. 2-7 National Association of Stationary Engineers.... Cincinnati, O. Sept. 9-13 Association Iron, Steel, Electrical, Engineers Baltimore, Md. Sept. 9-14 British Iron and Steel Institute, Autumn Meeting London, Eng. Sept. 12-13 National Exposition of Chemical Industries New York, N. Y. Sept. 23-28 American Electrochemical Society Princeton, N.J. Sept 30-Oct. 2

Jan 7, 1918

Organization Place Date 1918 American Chemical Society Cleveland, O. Sept. 9-12 American Society of Sanitary En Engineers Chicago, Ill. Sept. 3-5 National Petroleum Association Atlantic City, N.J. -Sept. American Institute of Mining Engineers Colorado Sept. 2-7 National Association of Stationary Engineers.... Cincinnati, O. Sept. 9-13 Association Iron, Steel, Electrical, Engineers Baltimore, Md. Sept. 9-14 British Iron and Steel Institute, Autumn Meeting London, Eng. Sept. 12-13 National Exposition of Chemical Industries New York, N. Y. Sept. 23-28 American Electrochemical Society Princeton, N. J. Sept. 30- Oct. 2

Jan 9, 1918

By S. R. Goodman, Hsun Hu

The formation of secondary - recrystallization tex-tlires in cube-textured 18-8 stain less steel (Type 304) Ilas been studied at three temperatures. Prolonged annealing at 100°'C protluces a PredoninanGly (520) [OOZJ-type texture, which is related to the cube te.ture of the primary lnatrix by a rotation of approxivzately 22 deg around the [001] axis in the rolling direction. Annealing at 1200 or 1300°C facers the formation of the (123)[272/-type texture, which is related to the matrix texture by a [111] rotation of app.voxiniately 40 deg. These observations suggest that in the secondary recrystallization of cube-texlut-ed stainless steel an apparent actilation energy for growth is higher for grains related to the tncrtuix Og [111] rotations thun those reloted by [100] rotations. THE formation of secondary-recrystallization textures in cube-textured primary matrices of fcc metals has been studied widely by various investigators. For Fe-40 pct Ni alloys, Pawlek' and wassermann2 reported that the orientations of secondary grains were related to the cube texture by rotations of 30 and 38 deg around [001] in the rolling direction. However, Rathenau and custers3 found that, while in one Fe-48 pct Ni alloy, most of the secondary grains were oriented with respect to the cube-textured matrix by rotations around [001] of 26.5 deg, in another alloy of a different origin, the orientations of secondary grains were related to the cube texture by rotations of approximately 35 deg around a [lll] axis. Similar orientation relationships were also observed between the secondary grains and the cube-textured primary matrices of copper.4"a No attempt was made to differentiate these two types of orientation relationships; reorientation by either a [111] or a [100] rotation was considered to be equally favored. The present investigation consisted of a study of the secondary recrystallization textures in cube-textured stainless steel. It was noted that the secondary grains formed in stainless steel were considerably smaller than those of Fe-Ni alloys or copper. This offered the advantage that the secondary recrystallization texture could be determined by the texture-goniometer technique, and a more detailed study of the textural development during the course of secondary recrystallization could be made. The effect of annealing temperature on the formation of secondary-recrystallization textures was also investigated. MATERLAL AND METHOD It was shown earlier"-" that a strong cube texture can be obtained in 18-8 stainless steels by rolling at 800°C to produce the copper-type deformation texture, followed by annealing at 800" to 1000°C for recrystallization. To improve the cube texture for the present study, a commercial-grade 18-8 stainless steel (Type 304) was rolled at 800°C first to 5 mm (0.2 in.) thick plates. Three of these plates were then stacked and welded together along the edges into a sandwich assembly. After annealing at 900°C for 20 min: the assembly was finally rolled at 800'C to 90 pct reduction in thickness with reheats and end-for-end reversals after each pass. Only the central strip, which was reduced from 5.0 to 0.50 mm (0.7 in. to 0.020 in.) thick, was used. The chemical composition of the steel in weight percent was as follows: C, 0.06; Mn, 0.38: Cr, 18.71; Ni, 9.56: P, 0.011; S, 0.009; and Si, 0.39. The purpose of rolling the strip in a sandwich assembly was to prevent direct contact between the central strip and the rolls. It was observed earlier" that, when the strip was rolled at 800°C without being enclosed in a sandwich assembly, the cube texture obtained by subsequent annealing at 900" or 1000° C for recrystallization was largely confined to the central section of the strip, while most of the recrystallized grains formed in the surface section of the strip were not cube-textured. This was obviously due to the fact that the actual temperature at the strip surface during rolling, as a result of direct contact between the strip and the cold and massive rolls, was considerably lower than 800°C. By using a sandwich assembly for hot rolling, the cube texture obtained upon subsequent annealing for recrystallization was found to extend through the entire thickness of the strip. After rolling, the central strip was taken from the sandwich assembly. and cut into specimens. Prior to annealing. the specimens were etched to 0.25 mm (0.010 in.) thick. A tube furnace provided with a purified, dry argon atmosphere was used for annealing. Textures were determined by the reflection technique. using a Siemens automatic texture-goniometer and ZrOz-filtered MoKa radiation. With a time constant of 4 sec. the preferred orientation of the secondary grains could be measured satisfactorily by the integrated intensities. Both (111) and (200) reflections were measured, and corresponding pole figures were constructed according to the techniques described previously.10 The agreement between results deduced from these two reflections was excellent. RESULTS AND DISCUSSION Secondary-Recrystallization Texture due to Prolonged Annealing at 1000°C. Fig. 1 shows the primary-recrystallization texture of a specimen annealed at 1000°C for 30 min. A substantial improvement in both sharpness and intensity of the cube texture, owing to the present processing method, can be noted readily by comparing Fig. 1 with similar pole figures shown earlier in Refs. 9 and 11. Secondary recrystallization

Jan 1, 1967

By G. A. Beske, P. Hilsch, J. Wulff

The effects of the growth precipitates on the su-perconduching properties of an Al- 15 al. pel Zu alloy have been studied using magneization, transition lem-perature, and residual resistivity measurements. Aging at 230C for 1/2 to 11 he produces an increase in Hfp, Ike field of first penetration, and tut increase in trapped flux. The upper critical field, Hc2 remains constant for such aging tunes. Aging at 200°C produces a decrease in Hfp and an increase in trapped flux. The transition temperature remains constant at Tc - 1.227° ± 0.02°K for aging at 220°C for tims of from 1/2 to 10 hr, and for aging at 200°C it remains constant at Tc. = 1.18° i 0.02°K for times from 1/2 hv to 26 hr. The observed behavior indicates that the superconducting matrix when aged at 220°C behaves tike a type U su-perconducior, but when aged at 200°C behares like a type I superconductor. The magnetization changes after aging can be attributed to the growth and clutnge in distribution of the precipitate in a matrix of fixed composition. IT has been realized for some time that the superconducting properties of alloys are highly structure-sensitive. This is evident in the work of Mould and Mapother1 who examined the properties of an aluminum alloy. Precipitation effects have also been briefly mentioned in other studies.2-4 Bonnin and coworkers5 have observed a sharp inc rease in trapped flux in an A1-Mg alloy when the residual resistivity reaches a value that indicates it is a type II superconductor. Recently Blanc, Goodman, and Nemoz5p have reported on precipitation effects in A1-Ag alloys. Detailed studies of precipitation in Pb-Sn and Pb-Cd alloys made by Livingston6 serve to show that the upper critical fields are enhanced by quenched-in solute. Furthermore. at various stages in the precipitation process? the upper critical field is determined largely by the remanent solute. The observed magnetic hysteresis and trapped flux in such alloys result from the interaction between precipitate and the flux filaments in the mixed state. The flux trapping appears to depend largely on the precipitate distribution and is greater if the superconductor is type II than if it is type I. To examine the effect of precipitation in another alloy system, particularly one in which the composition of the superconducting phase does not change significantly during the course of precipitation, the Al-Zn system seems interesting, especially in view of the transition temperature and resistivity studies of Chiou and seraphim.' Furthermore, the recent detailed electron-microscope studies of an Al-Zn alloy by Richards and Garwood8 provide a guide for relating superconducting properties to changes in structure. For these reasons, magnetization, transition temperature, and residual resistivity measurements for varying times of heat treatment at two temperatures were made with a -15 at. pct Al-Zn alloy. The results are reported in this paper. I) EXPERIMENTAL The alloy used was prepared by Cominco Products Inc. from 99.9999 A1 and 99.999 Zn. It was chill-cast, swaged, and drawn to 0.125-in.-diam rod. The analyzed composition was 15.6 at. pct Zn (31.1 wt pct). A jeweler's saw was used to cut the 0.125-in.-diam rod into the 0.875-in. lengths needed for magnetization measurements. The ends of the cylinders were slightly beveled to remove the sharp edges. A portion of the original 0.125-in.-diam rod was drawn into 0.010-in.-diam wire and used for transition temperature measurements. Specimens were suspended from wires within a vertical furnace during heat treatment. All were homogenized at 500°C for a minimum of 3 days and subsequently solutionized for times in excess of 6 hr. The solutionizing temperature was held constant to +3°C. Individual specimens were homogenized, quenched, and aged several times and no effects indicating loss of zinc were noted. The suspended specimens were quenched by cutting the wires and allowing the specimens to fall into a silicone oil bath held at the aging temperature. They were then isothermally transforked by aging in the same bath used for quenching. After aging for the required time (approximately 10 min aging was necessary before the upper critical field reached a fixed value), they were briefly (1 to 2 sec) dipped into an acetone bath at room temperature to remove adherent oil and then immediately transferred to liquid nitrogen where they remained until inserted into the helium bath (usually within an hour). The temperature of the aging bath was held constant to +3°C for longer aging times. The cryostat used for the measurement of superconducting properties consisted of outer and inner dewars for liquid nitrogen and liquid helium, Stokes 6-in. booster diffusion pump and Stokes Model 212 mechanical pump, temperature controller to measure and control the temperature of the helium bath, and a superconducting solenoid with inserted search coils to provide the magnetic field and measure the magnetic moment of the specimens. A schematic diagram of the cryostat is shown in Fig. 1. An ultimate temperature of 0.85°K was reached with this apparatus. The temperature controller used is similar to the one described by Blake and chase.' A 0.5 pct Allen-Bradley carbon resistor and a nichronle heater (200

Jan 1, 1968

By I. J. Hegyi, J. J. Tietjen, H. Nelson, J. I. Pankove

The fabrication of p-n junctions in GaAsl-,P, alloys by a vapor-phase gowth technique has for the first tirne resulted in room-temperature injection lasers capable of operating over a broad range of wavelengths extending into the visible region of the spectrum. The shortest wavelength achieved to date is 6750A at room tetnperature. In addition, at 78°K the threshold current density values for these lasers are generally the lo~vest reported, and the emitted radiation extends to the lozc,est wavelength ever attained (6350A). With lasers fabricated from material containing 14 pct Gap, quanticm efficiencies of 26 pct and peak power outputs of 25 zu were obtained at room temperature. ALTHOUGH room-temperature operation of GaAs injection lasers has been well-documented,&apos;-5 the operation of GaAsl-,P, (x > 0) laser diodes has been restricted to relatively low temperatures.8-&apos;0 This has been previously attributed5, 7, 10-12 partially to the difficulty of preparing single-crystalline GaAsl-& alloys having a high degree of chemical homogeneity and purity. Also, with these materials it has been difficult to prepare high-quality, abrupt p-12 junctions by diffusion techniques; and, in turn, this has made it difficult to obtain optimum electrical properties for room-temperature operationL3 in the resulting laser diodes. As a result, GaAsl-,P, laser diodes have not been efficient enough to permit operation at room temperature. For example, using diffused structures, only a few diodes were obtained which could be operated even close to room temperature (255K)." Recently, a vapor-phase growth method of preparing epitaxial deposits of GaAsl - .P, alloys has been described,14 and the high-purity and homogeneity of these materials has been previously demonstrated. Of special significance, with this technique, n- or p -type doping can be initiated or discontinued at any time and at almost any rate during the crystal growth so that the donor and the acceptor concentrations can be easily controlled to obtain desired impurity profiles. This permits high-quality, abrupt p-TZ junctions to be vapor-phase grown entirely during the crystal growth process, so that diffusion or other p-n junction fabrication processes are unnecessary. After growth, the device does not have to be heated to elevated temperatures, which avoids the possible unwanted introduction and motion of both impurities and lattice defects. Using the vapor-phase growth method cited above, over 300 room-temperature injection lasers have been prepared from GaAsl-,P, alloys having compositions in the range of 0 5 x 5 0.41. These lasers have emitted cohe~ent radiation in the spectral range of 8350 to 6350A at 78°K or from 9000 to 6750A at room temperature. The threshold current densities of the best lasers are independent of the alloy composition over the range 0 < x < 0.2 and compare favorably with values for good GaAs lasers.&apos; MATERIAL PREPARATION Multilayer, epitaxial deposits of GaAsl-,P, alloys are prepared by a vapor-growth technique described elsewhere.14 With this technique, the individual layers which comprise the multilayer structure are prepared sequentially in the deposition apparatus without interrupting the crystal growth. The epitaxial layers are deposited on GaAs substrate surfaces oriented normal to the ( 100) direction. The substrate wafers employed in this study were usually doped with tellurium to an electron concentration of approximately 2 x 10" per cu cm. To avoid strains, the first 10 to 15 p of the deposited material is uniformly graded from pure GaAs to the specific GaAsl- ,P, alloy composition of interest. The GaAsl - ,P, alloy growth is then continued to form a layer of constant composition having a thickness in the range of 25 to 75 p. Both the graded region and the layer of constant composition are doped with selenium to an electron concentration of about 2 x 10" per cu cm. The p region of the diode is then incorporated in the crystal by abruptly changing the dopant concentrations in the vapor phase to facilitate doping with zinc. This layer has a hole concentration of approximately 3 X 1019 per cu cm and typically is 50 p thick. DEVICE FABRICATION In general, the GaAs substrate and the region of graded composition are removed. Ohmic contacts are made to the n-type side by tin evaporation and to the p-type side by an electrodeless nickel deposition. This is followed by an electrodeless deposition of gold on both sides. The crystal wafer is then cleaved along (110) planes and sawed into rectangular parallelepipeds. Typical dimensions are 100 by 300 for the junction area and 100 µ for the diode height. The diodes are either soldered to a copper stud or pressure-mounted in a copper clip. RESULTS AND DISCUSSION Approximately 400 laser diodes having compositions in the range of 0.41 have been prepared by the method described above. Each laser was routinely tested at liquid-nitrogen temperature. The lasers were operated with l-psec current pulses at a repetition rate of 60 pulses per sec. The parameters of greatest practical interest are the photon energy or wavelength of the laser output and the threshold current density. Fig. 1 shows the variation of photon energy with alloy composition at 78°K. The composition was determined from the lattice constant of the material obtained by X-ray back-reflection measurements. Although there

Jan 1, 1968