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By H. Reinhardt, P. Haglund, J. Rydberg, B. Lunden

As legislation to minimize pollution in effluent streams becomes stricter, it is important to treat used acid pickling baths before discharge. This is usually achieved by neutralization of the acids and precipitation of the dissolved metals in such a way that neither acids nor metals can be re-used. A process has been designed and tested on a pilot plant scale to recover both acids and metals from a stainless steel pickling bath leaving only Na2SOs in the effluent. In this process, H2SOr is added to the spent pickling liquor and the recovery of the pickling acids HN03 and HF is achieved by solvent extraction, using TBP in kerosene as the organic solvent. The extracted acids are stripped with water, giving an acid concentration high enough for direct use in the pickling bath. Molybdenum is also extracted by TBP and is recovered in a separate step. The other metals, Fe, Cr and Ni, are precipitated from the raffinate as hydroxides, dried and recycled to the metal process. In evaluating this process, comparative experiments with mixer-settler and pulsed column have been performed. The process described is being considered for use by a Swedish company pickling 70,000 tons per annum of stainless steel.

Jan 1, 1973

By P. Ramakrishnan, Ramjilal

Fine powders of lead zirconate titanate have been prepared by three different methods such as ball milling, conventional coprecipitation and spray drying. Different powders have also been prepared by changing the process variables in each method. These powders were analysed for particle size chemical composition and reactivity. DTA, TGA and x-ray analysis have been carried out to study the lead zirconate titanate formation with reference to calcination temperatures. The calcined powders were then consolidated by compaction and sintering. An attempt has bean made to explain the consolidation behaviour of these powders on the basis of powder characteristics.

Jan 1, 1980

By Earl S. Greiner, Eric R. Jette

The literalure on the binary alloys of iron and silicon has been reviewed by Stoughton and Greiner.1 Another even more extensive and detailed survey of the present knowledge has been prepared under the auspices of the Alloys of Iron Research Committee by Greiner, Marsh and Stoughton. Since the latter surrey has already been issued in its preliminary form, it will be unnecessary to review the literature in the present article. However, in this connection there should be noted the important work on the crystal structures of the iron-silicon alloys by Phragmén,2 who investigated the entire system, identified the various phases and determined the homogeneity ranges of these phases. It was evident in the surveys cited above that in the range from 0 to 15 per cent silicon, which includes the commercially most important, alloys, the results obtained by thermal analysis, microscopic examination and the determination of electrical, magnetic and mechanical properties were extremely confusing. From time to time various compounds between iron and silicon have been postulated to account for the results yielded by the classical methods, and much argument has ensued. It was presumed that if compounds occurred which are sufficiently diverse in their properties to account for the characteristics of the alloys, they should be recognizable as separate phases but satisfactory proof of this sort has not been found by thermal or microscopic methods. Contributing to the confusion is the fact that the electrical, the magnetic and some of the mechanical properties are "structure sensit'ive"; i. e., they are influenced to a marked degree by the presence of minute amounts of impurities, the specific characters of these impurities, the grain size, the character of the grain boundaries, small general or local strains, etc. Thus interpretations of the discontinuities in the various property versus composition curves that identified these discontinuities with phase changes or compound formation have always been open to question.

Jan 1, 1933

By E. A. von Hahn, T. R. lngraham

Cementation rates ulere studied by rotating an elec-tropolished or etched copper strip in aqueous solutions, of either perchloric acid or alkaline cyanide, containing silver ions. The rates of cementation were more rapid in acidic media than in cyanide media. In both, the rates varied with the rate of rotation of the copper strip. The deposits formed in the acidic solutions were finely divided, loosely adhering powders. Those formed in the cyanide solutions were dense and adherent. The presence of the deposits influenced the cementation rates. In the acidic solutions the rate was enhanced, possibly because of the increased cathodic area. In the alkaline solutions the rates were decreased in the presence of the deposits. This has been attributed to restricting the diffusion of the copper ion from the rnetal outward into the bulk of the solution. In an earlier paper1 the authors described a kinetic study of the cementation of palladium on copper in perchloric acid solutions. That work indicated that there were two stages in the palladium cementation process. The first, more rapid stage was consistent with rate control by the diffusion of Pd11 ions to the copper surface and/or by chemical reaction at the surface. The second stage was consistent with rate control by the diffusion of copper ions from the copper surface, through the deposit, out into the main body of solution. The effect of the type of deposit on the rate of cementation is of particular interest because it may be one of the primary features involved when large quantities of metal are to be cemented from solution. No substantial investigations of the effect seem to have been made. Accordingly, an extension of the previous work was arranged to study the cementation of silver on copper. This system was selected because of the convenience of the analytical methods, the previously established technology with copper, and the fact that the system could be studied in both acidic and alkaline media. By selecting perchloric acid and alkaline cyanide solutions as the media, it was hoped that some assessment might be made of the effects, on cementation, of having the silver ion present in a virtually uncomplexed state and in a highly complexed state. EXPERIMENTAL The cementation rates were studied, as previously described,' by rotating a copper strip (1.0 by 23.2 cm) clamped to the peripheral surface of a lucite cylinder. The solutions were kept at constant temperatures (±0.05°C) under an atmosphere of purified nitrogen, and samples were taken periodically for analysis. The initial solution volume was 1000 ml and the sample volume 5 ml. The initial silver(1) ion concentrations were made low (0.5 to 1.0 x 10-4 moles per liter) to minimize the influence of the cemented deposit on rates. The solutions were prepared by dilution of suitable aliquots of silver perchlorate and silver cyanide stock solutions. Both stock solutions were prepared from purified silver powder (Johnson, Matthey, and Mallory Ltd.) with redistilled deoxygenated water, and they were kept under an atmosphere of purified nitrogen. To prepare the stock solutions, weighed amounts of silver powder were dissolved with nitric acid. For the AgC104 stock solution the silver nitrate solution was evaporated twice to near dryness with perchloric acid and then made up to volume: For the NaAg(cN)2 stock solution, the silver ions were precipitated with sodium hydroxide solution. The precipitate was filtered, washed thoroughly with redistilled water, dissolved with 1.1 times the required stoichiometric amount of sodium cyanide solution, and made up to volume. The small amounts of free perchloric acid and sodium cyanide present in the stock solutions were disregarded in the preparation of the solutions. The copper strips were cut accurately from 0.025-in. sheet (American Metal Climax OFHC brand) and annealed for 1.5 hr at 470°C in a stream of nitrogen. Analyses of the solution samples for silver and copper were done with a Techtron Model AA-3 atomic absorption spectrophotometer. Calibration standards of the same composition as the experimental solutions were prepared and analyzed simultaneously with the samples. No difficulty was experienced in the analyses, and the reproducibility was within 1 to 2 pct in both alkaline cyanide and perchloric acid solutions.

Jan 1, 1968

By R. A. Swalin, B. W. Roberts

ONSIDERABLE controversy has centered about the existence of an order-disorder transformation in alloys in the composition vicinity of 75 atomic pct Ni and 25 atomic pct Cr. All the evidence to date for such a transformation is of a rather indirect nature, since direct X-ray confirmation is difficult to obtain as a result of the small difference in X-ray scattering factors between nickel and chromium. As a result, superlattice lines would be very faint if present. Several investigators1-5 have observed anomalies in the electrical resistivity vs temperature curves of alloys in the vicinity of 25 atomic pct Cr. The observed change is characterized by a rather broad resistivity peak at about 540°C. A discontinuous drop in resistivity is normally associated with ordering. However, Taylor and Hin-ton4 have rationalized that the discrepancy could conceivably be caused by changes in the Brillouin zones upon ordering. The same investigators measured the specific heat as a function of temperature and have also observed anomalies in the vicinity of 540°C. Nordheim and Grant5 have proposed, because of the absence of superlattice lines and the absence of a discontinuity in the resistivity vs temperature curve, that long-range order is improbable and that the results could be better explained by short-range ordering. To date, however, the question has not been resolved satisfactorily. Neutron diffraction techniques provide a method for partially resolving the question since nickel and chromium have considerably different atomic scattering factors in the case of neutrons and, therefore, superlattice peaks, if ordering occurs, should be readily discernable. The results of a neutron diffraction investigation* coupled with a dilatometric in- vestigation are reported here. An alloy containing 28.0 atomic pct Cr was prepared from carbonyl nickel and electrolytic chromium in the form of a 1-in. diam x 10-in. ingot. Melting was done in an alumina crucible and casting in a graphite mold. The ingot was homogenized at 1250°C for seven days, after which a 5-in. long piece was cut into shavings in order to obtain a suitable neutron diffraction sample. Hardness samples and samples suitable for dilatometric analysis (% in. diam x 2 in.) were prepared from the remainlng piece. The neutron diffraction sample, along with a hardness sample, was annealed at 501°C for seven days, at which time the temperature was lowered to 479°C and held at this temperature for twenty-four more days. The hardness was observed to increase from 133 to 147 Vhn during the course of the annealing treatment, in qualitative agreement with Nordheim and Grant." Neutron diffraction traces taken at room temperature and at 42 °K are shown in Fig. 1. The insert shows the trace taken at room temperature with short counting times and thus only fair statistical accuracy. No evidence for superstructure reflections of Cu3Au-type ordering is observed. The statistical accuracy of the 4.2°K trace was improved by using longer counting periods. Several weak intensities are observed at small angles, including an aluminum reflection from the cryostat assembly and a very

Jan 1, 1958

By E. A. Gulbransen, J. W. Hickman

INTRODUCTION DURING the past two decades considerable progress has been made in the art of manufacturing heater alloys. The conventional iron-chromium-nickel alloys have been improved by the addition of small quantities of other elements. Up to the present time, to our knowledge, there has not appeared a systematic study of these alloys where the newer tools of investigation have been brought to bear on the problem. It is not yet clear what roles the additional elements play in increasing life time in usage. As a first approximation one might guess that elements such as manganese, silicon, zirconium, calcium and aluminum would aid in the formation of a protective film on the alloy surface, thus retarding the oxidation rate and increasing lifetime. If these additional elements do form protective oxides in the outer surface of the oxide film, it may be possible to identify them by means of reflection electron diffraction. It is also possible that the additional elements may not diffuse to the surface but may remain at the interface between the oxide and the metal. Then, too, the major elements in the alloys undoubtedly form oxides which are stratified on the surface. If the minor elements concentrate in a layer in contact with the substrate where they undergo oxidation and if this oxide film offers resistance to the diffusion of iron, chromium and nickel ions, then the lifetime of the heater element might be expected to increase. It is also possible that preferential reduction in the diffusion rates of the several ions may occur to such a degree that oxides may form in the body of the film and on the outer surface which are different from those that would normally form if the additional elements were not present. The use of transmisson electron diffraction may aid us in interpreting these phenomena. Up to the present time all of the factors which influence the lifetime of a given heater element are not definitely known. Among these are: (I) The rate of oxidation of the alloy. This may be dependent upon the composition and the physical state of the alloy. (2) The stability of the structure of the coating which forms. Transitions from one structure to another or solid phase reactions resulting in a change of composition may occur. The tendency of the film to adhere to the substrate when heated and cooled successively will be important. (3) The evaporation of various constituents from the alloy such as the removal of carbon by oxygen in a decarburization reaction. With these possibilities in view, an electron diffraction study of the oxides occurring on six different nickel-chromium alloys was undertaken with the hope that the results of this study could be correlated with oxidation rate studies as determined by means of the vacuum microbalance method1 and with

Jan 1, 1948

By B. H. Sage, R. T. Carter, W. N. Lacey

The phase behavior of a number of binary systems consisting of parafin hydro-carbons has been determined in recent years. In addition, the composition of the coexisting phases of mixtures of crude oil and natural gas has been investigated.~ However, the latter study did not include information concerning the influence of the concentration of a component upon its distribution between two coexisting phases. Owing to the paucity of such information it was considered desirable to investigate in some detail the composition of the coexisting phases in the methane-propane-n-pentane system throughout the greater part of the two-phase region at a tempera-ture of 100°F. Information of this nature also permits the establishment of the critical behavior of this ternary system. Method The compositions of the coexisting phases in this ternary system at 100°F. were deter-mined by withdrawing samples from a pres-sure vessel containing a heterogeneous mixture of the three components that had been brought 10 equilibrium by mechanical agitation at the desired pressure and tem-perature. The samples were withdrawn under such conditions that the equilibrium was not disturbed and the composition of each of the phases was ascertained by means of the conventional low-temperature fractionation procedure. The apparatus employed in this investi-gation was nearly the same as that utilized in an earlier study of the methane-pentane system.~ Several minor modifica-tions in the arrangement of the apparatus were made in the interest of simplifying the procedure and avoiding the possibility of condensation in the tubing connecting the equilibrium apparatus with the analyti-cal equipment. The pressures were meas-ured by means of a pressure balance with a precision of 0.5 lb. per sq. in. It is believed that the equilibrium pressure was ascer-tained with an uncertainty of not more than 2 lb. per sq. in., even though small varia-tions in pressure obtained during the withdrawal of the samples. The tempera-ture of the equilibrium equipment was maintained by use of an automatically controlled oil bath. The bath temperature was determined by means of a copper-constantan thermocouple, the electromo-tive force being determined by means of a potentiometric circuit of such a nature as to reduce the uncertainty of the tempera ture to less than O.I f. The fractionating column employed in the determination of the composition of the gas phase had a diameter of 0.12 in. and was approximately 4 ft. long, while the column employed in the analysis of the liquid phase was 0.18 in. in diameter and about 5 ft. long. Each column was equipped with the conventional constant-volume receivers, which were maintained at a constant temperature by means of an automatically controlled oil bath. In nearly every case the distillation in thr neighborhood of the transition between

Jan 1, 1941

By W. N. Lacey, R. T. Carter, B. H. Sage

The phase behavior of a number of binary systems consisting of parafin hydro-carbons has been determined in recent years. In addition, the composition of the coexisting phases of mixtures of crude oil and natural gas has been investigated.~ However, the latter study did not include information concerning the influence of the concentration of a component upon its distribution between two coexisting phases. Owing to the paucity of such information it was considered desirable to investigate in some detail the composition of the coexisting phases in the methane-propane-n-pentane system throughout the greater part of the two-phase region at a tempera-ture of 100°F. Information of this nature also permits the establishment of the critical behavior of this ternary system. Method The compositions of the coexisting phases in this ternary system at 100°F. were deter-mined by withdrawing samples from a pres-sure vessel containing a heterogeneous mixture of the three components that had been brought 10 equilibrium by mechanical agitation at the desired pressure and tem-perature. The samples were withdrawn under such conditions that the equilibrium was not disturbed and the composition of each of the phases was ascertained by means of the conventional low-temperature fractionation procedure. The apparatus employed in this investi-gation was nearly the same as that utilized in an earlier study of the methane-pentane system.~ Several minor modifica-tions in the arrangement of the apparatus were made in the interest of simplifying the procedure and avoiding the possibility of condensation in the tubing connecting the equilibrium apparatus with the analyti-cal equipment. The pressures were meas-ured by means of a pressure balance with a precision of 0.5 lb. per sq. in. It is believed that the equilibrium pressure was ascer-tained with an uncertainty of not more than 2 lb. per sq. in., even though small varia-tions in pressure obtained during the withdrawal of the samples. The tempera-ture of the equilibrium equipment was maintained by use of an automatically controlled oil bath. The bath temperature was determined by means of a copper-constantan thermocouple, the electromo-tive force being determined by means of a potentiometric circuit of such a nature as to reduce the uncertainty of the tempera ture to less than O.I f. The fractionating column employed in the determination of the composition of the gas phase had a diameter of 0.12 in. and was approximately 4 ft. long, while the column employed in the analysis of the liquid phase was 0.18 in. in diameter and about 5 ft. long. Each column was equipped with the conventional constant-volume receivers, which were maintained at a constant temperature by means of an automatically controlled oil bath. In nearly every case the distillation in thr neighborhood of the transition between

Jan 1, 1941

By Petri Bryk, John Ryselin, Rolf Malmstrom, Jorma Honkasalo

THE theoretical possibilities for the realization of flash smelting have been known for a long time. Calculations concerning the same can be found in previously published literature,1 and suggestions for its accomplishment in practice are described in patents on the subject. Likewise a smaller number of practical test results are known. Autogenous smelting is closely connected with flash smelting, since in flash smelting techniques it is possible to use the heat evolved by oxidation of the sulfides for the smelting process to such an extent that under certain conditions smelting can proceed without additional fuel. However, in the event that insufficient heat is available from the oxidation of the sulfide concentrates, then additional heat may be supplied by preheating the air, using oxygen enriched air, on burning additional fuel with the concentrate.

Jan 6, 1958

By H. A. J. Wilkens, H. B. C. Nitze

At the Atlanta meeting of the Institute in October,' 1895, some brief remarks were made by Mr. Wilkens on the above subject. It is the object of this paper to set forth the substance of these previous statements, embodying therewith additional information gained since that time, and a brief illustrated description of the method and means of the separation.* Lack of time will unfortunately not allow as complete a resume of the subject in all its phases, especially those relating to the scientific side of the question, as its novelty and importance would warrant, so that even this paper must be considered a preliminary one. It is hoped that at some future meeting of the Institute we may find an opportunity of presenting supplementary data of interest. The paradoxical title above used requires some explanation. The term " non-magnetic material " is applied to such substances as have heretofore been considered non-magnetic in the arts, more especially in the practice of ore-concentration. Scientifically, it has been shown by Faraday, Plucker, Wiedemann and other physicists that magnetism is an inherent property common to all substances, solid, liquid and gaseous, i.e., all suhstances are either attracted or repelled by the poles of a magnet, although ill the great majority of cases the manifestation of this

Jan 1, 1897

By W. L. DeMoulin

A rather detailed description of the entire plant and leaching process was given in a paper recently presented to the Institute,I so this paper will cover briefly only the crushing practice of the New Cornelia Copper Co. for the year 1918. The ore, which is mined by steam shovels and loaded in side-dump cars, passes through two crushing plants. These crushing plants were constructed to crush the ore required by a leaching plant of 5000 tons daily capacity, during a crushing period of 16 hours. The primary plant reduces to less than 3 in. (76 mm.) and the secondary plant, to 1/4 in. (6.35 mm.), which is sufficiently fine for satisfactory percolation of solution through the ore in the leaching tanks, and to give-good extraction. The ore is then conveyed to the leaching tanks by a system of 28-in. (71-cm.) belt conveyors. On the way to the leaching tanks, it passes through an automatic sampling plant, where a 1-per cent. sample is taken. From the primary crushing plant, the ore is conveyed by two 36-in. (91-cm.) belt conveyors to a 10,000-ton steel storage bin, with a reinforced-concrete flat bottom. The ore discharges from the bottom of this' bin onto four 20-in. belt conveyors, which deliver it to the four units of crushers in the secondary crushing plant. There is no storage bin between the mine and the primary crushing plant. The ore breaks very coarse, is very hard, and contains a great many boulders, some as large as 4 1/2 by 4 1/2 by 10 ft. (1.3 by 1.3 by 3 m.). Jams form in the bowl of the coarse crusher in the primary crushing plant, as a consequence, and are freed by means of an immense steel hook operated from a 40-ton electric traveling crane. Primary Crushing Plant The primary plant consists of one No. 24 Gates, style K, gyratory crusher, followed by four Gates No. 8, style K, gyratory crushers. All

Jan 1, 1920

By R. P. E. Hermsdorf

THE electrolytic refining of metals for the removal of undesirable impurities has become a recognized necessity in the nonferrous field. Copper, lead, zinc, nickel, silver and gold have been produced in this manner for years. The United States Metals Refining Co., realizing that considerable quantities of lead and tin could be made available to the trade if a satisfactory method of purification of these metals could be established, decided to investigate the possibilities of electrolytic solder. In cooperation with Dr. Edward F. Kern, of the School of Mines at Columbia University, the company developed a process of electrolytic refining of lead-tin alloys using a tin-lead fluosilicate electrolyte. A pilot plant was installed in November, 1927, and the commercial unit was put in October, 1929. Since that time thousands of tons of electrolytic solder have been produced in this plant and consumed by all branches of industry that use solder.

Jan 1, 1936

By James Terry Duce

The symposium on production for the year 1940 contains few papers on the foreign situation. It is probable that the foreign part of next year's symposium will be even shorter. This is due to rigid censorship in various countries, as the question of the volume of petroleum supplies has become one of great strategic importance. This is even more true than in the last war, owing to greater mechanization of armies. 'It has always been the policy of officers in charge of the symposium to refrain from publishing information that might possibly injure national or private interests. At the close of the war we hope again to publish full and accurate records of production abroad. Excerpts from Circular to Authors In order to facilitate interpretation of the data in this chapter, we print the following excerpts from the Circular to Authors. The field is the unit in this tabulation. In cases of fields extending across State boundaries, such as Rodessa, it is suggested that each State author treat the section of the field in his State as a unit, and by a footnote indicate that the field extends into an adjacent State. Each space in Table I may represent one of four possibilities; either it is not applicable to the particular field, or the proper entry is not determinable, or the proper entry may be determinable but is not determinable from data available to the author, or the proper entry is determinable. When spaces are not applicable, leave blank; in spaces where the proper entries are determinable but not de-terminable frod data available to the author, please inserty; in spaces where the proper entries are determinable by the author, make such entries. y implies a hope that in some future year a definite figure will be available. The entry of a zero is a positive declaration, and an important declaration where it is in order. Inability to determine precisely the correct entry for a particular space should not lead the author to insert merely y. Contributions of great value may be made by the author in many cases where entries are not subject to precise determination. In sucli cases the author should use his good judgment and make the best entry possible under the circumstances. For many spaces the correct entries represent the opinion of the author (for example, "Area Proved') and in such cases the entry need not be hedged to such extent as when the quantities are definite yet can be ascertained only approximately by the author. In cases under definite headings but where figures are only approximate, the author may use x. It is thought that the nearest whole numbers are sufficiently accurate for our purposes except as to percentage of sulphur in oil. If an author desires to report any other figures to tenths, he may do so. The quantity of gas produced should include, where possible, gas sold or otherwise marketed, and gas blown into the air, burned as flares or otherwise wasted. Segregation of these figures would be interesting if the authors can make such segregation. In any event, the figures should represent as nearly as possible the total quantity of gas removed from the reservoir. Under the columns on "Depth," the average depth to the top of the productive zones and to the bottom of the productive wells, when

Jan 1, 1941

Secondary minerals are the result of a process of concentration and enrichment and are commonly richer than the primary minerals of the same deposit. Secondary ores that contain abundant sulphides are commonly distinguishable in the field from primary ores; this distinction is more difficult with ores that carry a small quantity only of sulphide minerals, and microscopical examination of the ore in thin section is advisable in all doubtful cases. It is frequently difficult, and in some cases impossible, to determine the primary or secondary character of quartzose gold ores. The safest guide is the presence or absence of gaseous or fluid inclusions in association with the ore minerals; such primary association coupled with a lack of traces of oxidation is indicative of primary origin. Any ore that carries traces of oxidation, such as iron stains, endritic oxides of manganese, kaolin and so forth must be considered to have been acted upon by surface agencies, and secondary enrichment must be suspected. Further examination, however, may indicate that the contained value is primary, and, therefore, persistent in its vertical distribution. The manner of occurrence of secondary minerals is frequently characteristic; secondary minerals, being due to the action of surface waters, are commonly found in cracks through earlier minerals, or as crusts lining vugs or surrounding nucleal masses, or in general, in some distribution later than and not conforming to the arrangement of the primary minerals. Secondary sulphides are often found as soft black pulverulent masses or coatings, although they frequently occur well crystallized or as

Jan 1, 1932

Jan 1, 1924

Jan 1, 1933

By Richard P. Rothwell

The anthracite coals of Pennsylvania are all mined from large veins. A seam less than four feet. in thickness is generally considered as unworkable, those from which most of the coal now comes being from 8 'to 30 feet thick. The system of mining employed is, almost without exception, that known as " chamber and pillar work;" that is, the coal is taken out of chambers of from 18 to 30 feet in width, and pillars of from 12 to 20 feet are left between these to support the roof. In general, the entire thickness of the seam, even

By E. R. Parker, C. F. Riisness

That grain size has a great effect on the mechanical properties of metals has been recognized for a long time. Bassett and Davis1 in 1919 did excellent work in determining the effect of grain size on the hardness of brass. About the same time Jeffries2 and Sykes3 ascertained the effect of grain size on the strength and ductility of several metals at temperatures ranging from 80°K. to their melting points. When creep was recognized as an important property of metals, those engaged in the study of this property tried to determine the effect of grain size4-9 on creep rates. Unfortunately, most of the investigations were conducted on only two grain sizes, often designated simply as "fine" and "coarse." It is well known that at high temperatures coarse-grained test bars creep less than fine-grained bars. The relation between grain size and size of test bar, however, has been frequently overlooked. In his early work, Jeffries2 showed that the number of grains in the cross section has a more important influence on the properties of the material than the actual grain size. More recently Hanson and Sandfordl0 and Pell-Walpole,ll in their measurements of the creep and tensile properties of tin, tested a wide range of grain sizes and correlated the grain size with the strength. Hanson9 later established the relation between the number of grains in the cross section and the creep rate. At high temperatures, generally a coarsegrained structure is considered superior in creep to a fine-grained structure, but it is evident that for a given bar size continuously increasing the grain size will

Jan 1, 1944

By C. F. Riisness, E. R. Parker

That grain size has a great effect on the mechanical properties of metals has been recognized for a long time. Bassett and Davis1 in 1919 did excellent work in determining the effect of grain size on the hardness of brass. About the same time Jeffries2 and Sykes3 ascertained the effect of grain size on the strength and ductility of several metals at temperatures ranging from 80°K. to their melting points. When creep was recognized as an important property of metals, those engaged in the study of this property tried to determine the effect of grain size4-9 on creep rates. Unfortunately, most of the investigations were conducted on only two grain sizes, often designated simply as "fine" and "coarse." It is well known that at high temperatures coarse-grained test bars creep less than fine-grained bars. The relation between grain size and size of test bar, however, has been frequently overlooked. In his early work, Jeffries2 showed that the number of grains in the cross section has a more important influence on the properties of the material than the actual grain size. More recently Hanson and Sandfordl0 and Pell-Walpole,ll in their measurements of the creep and tensile properties of tin, tested a wide range of grain sizes and correlated the grain size with the strength. Hanson9 later established the relation between the number of grains in the cross section and the creep rate. At high temperatures, generally a coarsegrained structure is considered superior in creep to a fine-grained structure, but it is evident that for a given bar size continuously increasing the grain size will

Jan 1, 1944

By C. C. Clark, J. S. Iwanski

The purpose of this investigation was to study mi-crostructural changes that take place in a commercial nickel-chromium-iron alloy, such as Incoloy "901," over long periods of time at temperatures up to 13 50°F and to correlate such changes with creep-rupture properties. of the alloy. In the course of the investigation, some microstructural changes were observed which correspond to microstructural alterations found in previous studies of Inconel "X." Microstructural phases have been identified in both alloys with the aid of electron and X-ray diffraction and an electron probe microanalyzer. The materials used in this investigation were from commercial heats of the following chemical composition: Pct Cr Pct Ni Pct Mo Pct Fe Pct Cb Incoloy "901" 12.51 43.67 5.72 Bal. -Inconel "X" 14.61 73.44 - 6.61 1.02 Pct A1 Pct Ti Pct Mn Pct Si Pct C Incoloy "901" 0.10 2.46 0.46 0.24 0.05 Inconel "X" 0.70 2.43 0.51 0.36 0.04 Long-term creep-rupture tests were conducted on Incoloy "901" at temperatures of 1000°, 1200°1 and 1350°F. A summary of these results is shown in Table I along with the results of a long-term creep-rupture test conducted on Inconel "X" at 1500°F. The heat treatments given the specimens are also shown in Table I. When the creep-rupture results on Incoloy "901" are compared with shorter-tertn data, there is no evidence of any undue deterioration of the creep-rupture strength with time, nor is the elongation decreased more than would be expected from the influence of time alone. INCOLOY "901" PHASE IDENTIFICATION Microscopic examination of the Incoloy "901" specimens reveals a dark etching grain boundary constituent in the specimen which was under test for about 11,500 hr at 1000°F. This grain boundary constituent was seen to increase in size as the test temperature was increased to 1200" and 1350°F, Figs. 1, 2, and 3. Simultaneously, an acicular structure of definite crystallographic orientation appears within the grains of the 1350°F specimen, Fig. 3. Under examination with the electron microscope, a fine precipitate is observed in the 1200 °F specimen. Fig. 4. It becomes considerably larger in the 2850-hr 1350°F specimen, Fig. 5. In a few areas the precipitated particles have been replaced by, or transformed to, small needles or platelets. After 7380 hr at 1350°F, Figs. 3 and 6, the needles are much larger and have replaced nearly all of the fine precipitate. X-ray diffraction studies detected the presence of hexagonal Laves phase and hexagonal n phase (Ni,Ti) in the 1350°F specimens, Table 11. Only the Laves phase was detected by X-ray diffraction in the 1200°F specimen and none was detected in the 1000°F specimen. In this latter specimen, however, the small quantity of precipitate in the grain boundaries (presumed to be Laves phase) precludes its detection by X-ray diffraction. Composition of the hexagonal Laves phase is not yet known, although its diffraction

Jan 1, 1960