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By J. E. Pavlick, W. W. Mullins, H. W. Paxton

The growth of nitrogen-austenite during nitriding of large-gvained ferrite between 650" and 800°C has been studied as a functimz oJ time and nitrogen potential of the atmosphere for a variety of alloying elements dissolved in the ferrite. Whereas no preferential grain boundary penetration by aistenite takes place in zone-refined iron, the addition of aboit I zot pct oj' V, Ti, Cr. Si, or A1 produces significant protrusion of austenite down former 0-0 boundaries. This group of elernents also produces ragged y-0 interfaces in the a grains which advance more slozuly than those in zone-refined iron. 1 zut pct of Ni, Co, Mn, or Mo dissolved in ferrite leads to essentially smooth 7-a interfaces, which advance at rates very sinzilar to those in zone-refined iron. The reasons for this effect are not clear. Two possible limiting hypotheses, not necessarily exclusive, are discussed. One involves p.referentia1 grain bozindary diffusion of nitrogen. the other the production of a zone of ferrite, stpersatcirated with respect to nitrogen, from which austenite precipitates helerogeneozisly on the a-a gyain boundaries. In many phase transformations which occur by nu-cleation and diffusion-controlled growth, information on the parameters which control the rates of nuclea-tion and of growth is frequently not quantititative. The present work describes a continuation of efforts to obtain quantitative data on growth rates in systems where thermodynamic and kinetic factors are known independently, and thus where comparison with models of the growth process is possible. The work has been conducted on iron-base systems for two reasons. Firstly, there are several interesting transformations in this system, many of which are of practical importance. Secondly, the information on phase diagrams, activities, and diffusion coefficients is more complete in this system than in any other. These data are still inadequate to check all the effects of alloying elements, but at worst it is possible to make estimates and thus examine order-of-magni-tude agreement with proposed models. It will be necessary to do this in the present work. The problem studied was the growth of nitrogen-austenite in from the surface of large-grained columnar crystals of alloyed ferrite exposed to an NHs/Hz atmosphere. Earlier work by Grozier et al.' had suggested that growth of austenite may occur preferentially along grain boundaries of alloyed ferrite, whereas zone-refined (ZR) iron shows no such effect, Fig. 1. Growth of nitrogen-austenite into single crystals of zone-refined ferrite is planar provided sufficient nu-cleation sites for austenite are present, and is controlled by volume diffusion of nitrogen through the

Jan 1, 1967

By R. A., D. L. Sponseller, Flinn

Using specially del'eloped titanium nitride crucibles and a pressurized syslem, it has been possible to determine the solzibilitv of liquid calcium in liquid iron and iron-base alloys. At 2925°F the solubility is 0.032 wt pet Ca in pure iron. The solubility is increased by aluminum, carbon, nickel, and silicon additions, and lowered by additions of gold. An inflection in the calcium-solubility curve occurs as carbon is added to iron. At approximately 0.87 Wt pet Ca the CaC, phase replaces liquid calcium, and the calcium concentration de- creases as more carbon is added to the iron. The maximum solubility, 0.36 wt pet Ca, was obtained in iron containing 10.5 wt pet Si. The data have important implications regarding the use of calcium in process metallurgy, as well as providing an interesting test of theories of metallic solutions. Reasonably good agreement is found with theories of Alcock and Richardson and of Wagner, and criteria are suggested which permit these theories to be applied more readily to systems of this type. AT the present time relatively little is known about the factors influencing solubility in liquid metals. Information of this type is important for such matters as the control of impurity levels in liquid metals, the use of magnesium in ductile-iron production, and the use of liquid-metal alloys as fuels and coolants in nuclear power plants. One important example of restricted solubility concerns the extent to which liquid calcium will dissolve in liquid iron. This is a matter of considerable interest in view of the strong potential of calcium for removing certain impurities in steel,. as well as the ability of calcium to desulfurize, inoculate, and produce spheroidal graphite in cast irons.' Since ferrous materials normally contain other elements in addition to iron, the interactions of third elements with the Fe-Ca system are of interest. In view of the foregoing, this investigation was conducted to determine the solubility of liquid calcium in liquid iron and the effects of various third elements upon the solubility. For reasons of theoretical and engineering importance, the elements investigated were aluminum, carbon, gold, nickel, and silicon. Numerous attempts were made in the early part of the present century to determine the solubility of calcium in both liquid iron and steel, employing a variety of open-melt and closed bomb-type systems.2-4 From the results of these tests Wever concluded that calcium is insoluble in liquid and solid iron.5 These investigations were unsatisfactory in that they failed to insure the presence of a liquid layer

Jan 1, 1964

By E. N. Silverman

Mixtures of' MnS, ZFeO-SiO,, ZMnO.SiO, FeO, and MnO were prepared synthetically and used to study the planes ZFeO. Si0,-ZMnO.SiO,-MnS, FeO-MnO-MnS, and Fe0-MnO.Si0,-MnS in the quaternary system. Because the oxides and silicates studied flux MnS, inclusions in this system are partly liquid during rolling. Also, oxygen can modify subsurface inclusions through the reaction MnS + FeO—FeS + MnO during the soaking of ingots and the reheating of blooms and billets. NONMETALLIC inclusions in steel have long been a subject of study and conjecture because the properties of many steels are known to be affected by the the kind and amount of inclusions present. In free-machining steels, the type of inclusion present has a direct bearing on their machinability; in other steels, cleanliness is important and metallurgists direct their efforts at reducing the amount of non-metallic inclusions. Thus, the accumulation of knowledge about the formation and behavior of inclusions during all stages of steelmaking and processing should aid in improving the quality of steels and decreasing the production costs resulting from rejections. Previous studies of inclusions have contributed greatly to our understanding. The investigators have generally examined inclusions in finished steel. Boulger, Moorehead, and Garvey1 found that in Bessemer steels, low silicon contents results in globular sulfide inclusions with attendant high machin- ability ratings. Van vlack2 also found that low silicon contents favor inclusion morphology that contributes to high machinability ratings. Boquist and Stoll* found that silicon content affected sulfide inclusions and machinability of blooms, billets and bars more than did the finishing temperature in the range between 1775° and 2075°F. Carney and Rudolphy3 studied the distribution of sulfur, manganese, silicon, and carbon in a commercial ingot of resulfur-ized steel and found that silicon was concentrated near the bottom. This helped to explain why bottom cuts had poorer machinability. Klinger and Koch4 developed techniques for extracting inclusions from steel, and the technique devised by Gurry, Chris-takos, and stricker5 for extracting carbides can also be adapted to the study of inclusions. A different approach to the study of inclusions in steel consists of synthesizing the constituents that form inclusions and determining the phase eauilibria in the system that contains the constituents. The resulting phase diagrams can then be used to determine the effect of the various constituents upon each other. In this way, it becomes possible to under-

Jan 1, 1962

By Alexander Coucoulas

FABRICATION of thin-film circuits deposited on glass substrates requires the formation of permanent electrical contacts. Since thin films are in the order of a few thousand angstroms thick and are deposited on nonconductive surfaces such as glass, new methods of lead attachment are being pursued in the microelectronics industry. Ultrasonic welding is being considered in thin-film technology since joining can be accomplished between a wide variety of dissimilar materials.l,' Ultrasonic welding is accomplished by a transducer-coupling-tip system which converts high-frequency electrical energy into mechanical vibrations and delivers it into the weld region. During the process the tip oscillates in a direction parallel to the surface of the weldments, inducing shear stresses in the work pieces which are clamped between the tip and anvil. Though the basic bonding mechanism is not clearly understood, it has been described as closely akin to friction welding. In the course of an investigation concerned with ultrasonic we!ding of aluminum wires to tantalum thin films (1400A) deposited on glass, low weld strengths were related to glass failure. Upon investigating this condition, an improved method of bonding was developed where the aluminum was held at a temperature where a minimum amount of strain hardening occurred during the introduction of ultrasonic energy. Experimental Procedure. Aluminum wires (0.015 in,) were bonded to tantalum thin films with an optimized set of welding parameters (power, time, clamping force) employing a commercial 100-w 60-kc ultrasonic welder. Forty-five degree shear-peel tests, where the lead is pulled at a 45-deg angle with respect to the substrate at 0.2 in. per min, produced a large variation from zero to the strength of the wire, Table I. Inspection of the weld region generally revealed: glass cracking before and after testing; the removal of glass nuggets from the substrate by the lead during testing, Table I; thin-film penetration. In an effort to improve the shear-peel strength, the aluminum between the tip and substrate was heated above ambient temperature through an argon gas media prior to and during welding with the same parameters employed above. With the addition of heat: wire deformation was increased; shear-peel tests all failed at the weld-wire junction, leaving the bonded portion undisturbed; no evidence of glass cracking or film penetration prior to or after testing was observed. In order to prevent failure at the weld-wire junction due to excessive wire deformation, 0.035-in. aluminum wires were welded to tantalum thin films with an optimized set of welding and heating parameters. As

Jan 1, 1967

By N. A. D. Parlee

THE gas-liquid metal diffusion cell technique1-3 has been used to study the diffusion of nitrogen in Fe-C alloys. The actual apparatus and technique were the same as employed by the authors to study the diffusion of hydrogen in liquid iron.' The diffusion cell' was formed by immersing an alumina tube in a stagnant melt contained in an alumina crucible. The tube (hereafter called absorption tube) contained nitrogen gas at 1 atm and was connected to a sensitive gas-measuring system. The change in the average concentration of nitrogen in the melt in the absorption tube was determined by measuring the rate of absorption of nitrogen in the diffusion cell. Eq. [I], 1-3 derived from the appropriate solution of Fick's second law, was used to examine the data and to calculate chemical diffusion coefficients (D) in situations where the absorption appeared to be controlled by diffusion in the liquid: where V is the stp volume in cu cm, d is the diffusion cell diameter in cm, p, is the density of the melt in g per cu cm, pg is the stp density of nitrogen in g per cu cm, C, is expressed in wt pct, D is in sq cm per sec, and t is in min. According to Eq. [I], a plot of v vs vt should yield a straight line passing through the origin if absorption is controlled by diffusion in the liquid. The slope of this line could be used to determine the value of D under appropriate conditions. As discussed in earlier reports,1,2 the initial thermal expansion of the gas upon immersing the absorption tube distorts the line in the initial stages of a diffusion experiment. However, this is not a serious problem since the slope of V vs 6 plots can be determined from the data points obtained after the initial expansion ceases. The volumes reported on the data plot presented here represent absorption after this thermal expansion ceased. Several preliminary diffusion experiments were attempted with melts of pure iron and with Fe-C alloys containing up to 0.6 pct C. In these cases, no or very little absorption was observed. The only data obtained were for an Fe-C melt which was in addition thoroughly deoxidized by successive hydrogen and vacuum-degassing treatments. These treatments introduced an appreciable amount of aluminum into the melt and reduced its omgen content. The original charge material for this melt contained 0.23 pct s and approximately 0.001 pct &. After repeated hydrogen and vacuum-degassing treatments two diffusion experiments were performed. The analysis of the melt

Jan 1, 1968

JESSE L. JONES,* Pittsburgh, Pa. (written discussion?).-The most important criterion on which judgment of the quality of manganese bronze can be based is its freedom from lead. Not over 0.03 per cent. of lead should be present in a good grade of manganese bronze. While it is not questioned that manganese bronze with a high tensile strength and considerable ductility can be made .from materials that will give a lead content of possibly 2 to 3 per cent., there is no doubt that such material, while it may machine readily, will be found to withstand the impact test very poorly, and hence be unsuited for high-grade engineering work. When lead is present in considerable amounts, it forms in small pools in the alloy and the material has little strength at these points; in fact, such spots in the metal are equivalent to nicks in a test bar as far as their effect on tensile strength is concerned. A further objection to a high lead content is the ease with which it oxidizes and its consequent tendency to produce dross. A second characteristic of a high-grade manganese bronze is a low content of manganese. This should not exceed 0.05 per cent.; in fact, very many of the best grades of manganese bronze show, on analysis, only a trace of manganese or no manganese whatever. Manganese is a deoxidizer and its ready oxidation protects the other metals of the alloy; but if it is present in large amounts it will produce considerable manganese dioxide, which does not separate readily from the molten alloy and may produce black specks or drossy spots and render the obtaining of clean castings difficult. Aluminum should be present in a good grade of manganese bronze in only very small amounts. A content of 0.10 per cent. aluminum is ample. Larger amounts have a tendency to increase the shrinkage of the alloy, to give the ingots and castings a white, scruffy appearance, and to prevent the beautiful, golden, oxidization color characteristic of high-grade manganese bronze and a most excellent indication of quality. The work that the author of the paper has done is valuable from a con- servation standpoint, and it will supplement, in a marked degree, the advances that have been made by a number of manufacturers of manganese bronze in utilizing the turnings from this material. A number of firms have succeeded in making a very good grade of ingot metal from turnings and other light scrap, obtaining a tensile strength and elongation

Jan 4, 1919

By Michael B. Bever, Carl F. Floe

he possibility that carbon may be soluble in copper to a limited extent has bten recognized for over a century. The quantitative investigation of this problem, however, requires more sensitive techniques than have formerly been available. Three recent developments have made possible more accurate determinations: the vacuum-fusion method of analysis, the production of copper of high purity and the availability of high-purity refractories, particularly graphite. In addition to its obvious theoretical interest, the problem of carbon solubility in copper is of practical importance. In the production of copper and of high-copper alloys, carbonaceous covers are freauerltlv used. If even minute amounts of carbon are dissolved, insoluble carbon oxide gases will be formed when such metals are poured under oxidizing conditions. A mechanism of this kind could well be one of the principal causes of gas porosity in casting copper-base products. Review of Literature In 1823 Vivian1 raised the question as to whether copper by overpoling becomes "combined with a minute portion of carbon." Karsten2 asserted, in 1832, that carbon reduces the high-temperature strength of pure copper, so that when the carbon content has reached 0.2 per cent the metal will be brittle at a dark red heat. According to Karsten, carbon contents of 0.05 per cent make it difficult to hot-work copper. He also reported that the specific gravity of copper is 8.8969 and that it increases to 8.9258 if the copper is cemented with carbon and then melted. He emphasized the difficulty of determining analytically the small amounts of carbon present in copper. The metal was removed by wet methods and the residue considered as carbon. At Percy's request, Dick,3 in 1856, carried out various working tests on copper that had been ill prolonged contact with carbon, and found that the working properties of the metal had not been affected. He also attempted to determine the presence of carbon analytically. In one experiment the copper was dissolved and the residue was fused with litharge, and in another essentially a combustion analysis was made on a copper sample. In a final experiment, a sample was dissolved and the residue subsequently subjected to a combustion analysis. Indications of as much as 0.005 per cent carbon were found, but Dick considered his work inconclusive largely because of the possible interference of sulphur. Percy4 concluded, from Dick's experiments and from some experimental work of his own, that the solubility of carbon in copper had not been established with

Jan 1, 1946

By Carl F. Floe, Michael B. Bever

he possibility that carbon may be soluble in copper to a limited extent has bten recognized for over a century. The quantitative investigation of this problem, however, requires more sensitive techniques than have formerly been available. Three recent developments have made possible more accurate determinations: the vacuum-fusion method of analysis, the production of copper of high purity and the availability of high-purity refractories, particularly graphite. In addition to its obvious theoretical interest, the problem of carbon solubility in copper is of practical importance. In the production of copper and of high-copper alloys, carbonaceous covers are freauerltlv used. If even minute amounts of carbon are dissolved, insoluble carbon oxide gases will be formed when such metals are poured under oxidizing conditions. A mechanism of this kind could well be one of the principal causes of gas porosity in casting copper-base products. Review of Literature In 1823 Vivian1 raised the question as to whether copper by overpoling becomes "combined with a minute portion of carbon." Karsten2 asserted, in 1832, that carbon reduces the high-temperature strength of pure copper, so that when the carbon content has reached 0.2 per cent the metal will be brittle at a dark red heat. According to Karsten, carbon contents of 0.05 per cent make it difficult to hot-work copper. He also reported that the specific gravity of copper is 8.8969 and that it increases to 8.9258 if the copper is cemented with carbon and then melted. He emphasized the difficulty of determining analytically the small amounts of carbon present in copper. The metal was removed by wet methods and the residue considered as carbon. At Percy's request, Dick,3 in 1856, carried out various working tests on copper that had been ill prolonged contact with carbon, and found that the working properties of the metal had not been affected. He also attempted to determine the presence of carbon analytically. In one experiment the copper was dissolved and the residue was fused with litharge, and in another essentially a combustion analysis was made on a copper sample. In a final experiment, a sample was dissolved and the residue subsequently subjected to a combustion analysis. Indications of as much as 0.005 per cent carbon were found, but Dick considered his work inconclusive largely because of the possible interference of sulphur. Percy4 concluded, from Dick's experiments and from some experimental work of his own, that the solubility of carbon in copper had not been established with

Jan 1, 1946

The Pinson Mining Co., which will start production in very early 1981, is the fourth Carbon-In-Pulp plant to be put into operation in the United States. The property is located in Humbolt County, Nevada, 38 km (24 miles) northeast of the town of Golconda. The famous Getchell Mine was also near Golconda and was the site of one of the early Carbon-In-Pulp plants in the 1940s. The deposit was discovered in 1971 by Reno based Cordilleran Explorations, which is founded by a consortium of Canadian mining companies. Cordilleran is a partnership consisting of John Livermore and Peter Galli. In 1972 a second but smaller deposit, called "Preble", was discovered at a location 15 miles south of Pinson. During 1980, a decision was made to place the Pinson deposit into production and Pinson Mining Company was formed. Ownership of Pinson is vested in Lacana Mining Inc. , Rayrock Mines, Inc. , Siscoe Metals, Inc., John S. Livermore, Peter E. Galli and Donald M. Duncan. Three distinct but connected ore zones occur at Pinson. Combined reserves of milling ore total 3, 200, 000 tons at an average (undiluted) grade of 4. 12 g per mt (0. 12 oz per st) Au. Initial mining will be from "A" zone which contains 1, 500, 000 tons with an average (undiluted) grade of 5. 8 g per mt (0. 17 oz per st) Au. An additional 5, 500, 000 tons of low grade ore will be mined from the Pinson deposit and processed by heap leaching. Mining reserves at Preble total at least 1, 500, 000 tons grading 2. 7 g per mt (0. 08 oz per st) Au. Production plans for the Preble deposit have not been formulated at the date of writing. Gold mineralization at both deposits is finely disseminated as sub micron sized particles. The ore at Pinson is structurally controlled and occurs in an Ordovician limestone-siltstone unit. Much of the ore has been silicified to a jasperoid. The ore zones have been entirely oxidized. Preble ore occurs in the Cambrian formation in a carbonaceous, limey shale. Only the upper part of the Preble is oxidized and amenable to conventional cyanide leaching. The Pinson ore body is adjacent to the mouth of Granite Creek in the Osgood Mountains at an elevation of 1, 615 m (5, 300 ft) with the mill being 1. 2 km (3/4 mile) from the mine at an elevation of 1, 495 m (4, 900 ft). Mine development work began in May of 1980 with ore being stockpiled for later processing. Pertinent factors affecting

Jan 1, 1981

By George Fancher, R. L. Whitting

A typical drilling mud from the Hastings oil field, Brazoria County, Texas, containing only 8 per cent (dry basis) of material of colloidal dimensions, which is largely illite, was concentrated to a density of 10.2 lb. per gal. and used in this study. The effects of water dilution, treatment with complex polyphos-phates, temperature and the time of heating upon the rheological properties of the mud were investigated. It was found that water plays an important part in chemical treatment and that sodium acid pyrophosphate and sodium tripolyphosphate were more efficient than other complex polyphosphates for chemical treatment. Muds treated with either of these chemicals manifested maximum reduction in viscosity and minimum filtration rates at low concentrations. Furthermore, .mud treated to minimum viscosity with either of these two chemicals was virtually unaffected by heat-treatment. Introduction The drilling of deep wells is dependent upon the use of drilling mud, and problems frequently arise concerning the effects on mud of temperature, prolonged heating and aging. The use of chemicals to control the rheological properties of mud is a well-established practice. Salts of weak organic acids such as sodium tannate or gallate were used at first until the complex phosphates of sodium were found to be more efficient. Consequently, it seemed important to investigate the reaction of a mud to chemical treatment with phosphates, temperature, heat-treatment and aging, particularly since previous work in the laboratory at the University of Texas had provided the particle-size distribution and mineral composition of Hastings mud. Properties or Mud Used in Experiments A large sample of the mud from a drilling well in the Hastings field, Brazoria County, Texas, was obtained directly from the circulatory system. Some of the general physical characteristics of the mud and other data are presented in Table I. Table i.—General Properties of Hustings Drilling Mud Alex- Cur-ander keet Well Well Depth when sample was taken, It.. 5720 5700 Weight. lb. per gal............... 9.5 0.8 Viscosity, sec. A.P.I.............. 47 60 Viscosity, Stormer, grams......... 80 Viscosity, centipoises............. 13 Filtration rate, c.c. per 30 min.a. . . 19.6 22.8 Salt content (chlorides), per cent... 0.13 0.12 pH............................. 8.9 8.9 The Alexander mud was used for the experimental work. Comparison with Curkeet mud indicates a considerably greater dilution but otherwise suggests similarity. The mineral composition and particle-size distribution of Curkeet mud (Table 2) are available (Fancher and Oliphant6). It is suggested that Alexander mud would have a similar composition.

Jan 1, 1943

By R. L. Whitting, George Fancher

A typical drilling mud from the Hastings oil field, Brazoria County, Texas, containing only 8 per cent (dry basis) of material of colloidal dimensions, which is largely illite, was concentrated to a density of 10.2 lb. per gal. and used in this study. The effects of water dilution, treatment with complex polyphos-phates, temperature and the time of heating upon the rheological properties of the mud were investigated. It was found that water plays an important part in chemical treatment and that sodium acid pyrophosphate and sodium tripolyphosphate were more efficient than other complex polyphosphates for chemical treatment. Muds treated with either of these chemicals manifested maximum reduction in viscosity and minimum filtration rates at low concentrations. Furthermore, .mud treated to minimum viscosity with either of these two chemicals was virtually unaffected by heat-treatment. Introduction The drilling of deep wells is dependent upon the use of drilling mud, and problems frequently arise concerning the effects on mud of temperature, prolonged heating and aging. The use of chemicals to control the rheological properties of mud is a well-established practice. Salts of weak organic acids such as sodium tannate or gallate were used at first until the complex phosphates of sodium were found to be more efficient. Consequently, it seemed important to investigate the reaction of a mud to chemical treatment with phosphates, temperature, heat-treatment and aging, particularly since previous work in the laboratory at the University of Texas had provided the particle-size distribution and mineral composition of Hastings mud. Properties or Mud Used in Experiments A large sample of the mud from a drilling well in the Hastings field, Brazoria County, Texas, was obtained directly from the circulatory system. Some of the general physical characteristics of the mud and other data are presented in Table I. Table i.—General Properties of Hustings Drilling Mud Alex- Cur-ander keet Well Well Depth when sample was taken, It.. 5720 5700 Weight. lb. per gal............... 9.5 0.8 Viscosity, sec. A.P.I.............. 47 60 Viscosity, Stormer, grams......... 80 Viscosity, centipoises............. 13 Filtration rate, c.c. per 30 min.a. . . 19.6 22.8 Salt content (chlorides), per cent... 0.13 0.12 pH............................. 8.9 8.9 The Alexander mud was used for the experimental work. Comparison with Curkeet mud indicates a considerably greater dilution but otherwise suggests similarity. The mineral composition and particle-size distribution of Curkeet mud (Table 2) are available (Fancher and Oliphant6). It is suggested that Alexander mud would have a similar composition.

Jan 1, 1943

By S. Y. Ogawa

The effects of sulfur (up to 0.1 pet) on the deformation and fracture characteristics of iron, in cast form, were studied at strain rates up to 100 pct pcr sec and at temperatures of 1600o to -3300 oF. The effects of oxygen and manganese additions on the behavior of Fe-S alloys were studied under comparable test conditions. Brittle fracture characteristics, evident at all strain rates, resulted from the presence of the liquid iron sulfide phase at grain boundaries. Ductility could be restored in three ways: solution of the sulfide in solid y iron at higher temperatures, spheroid-zzation of the liquid sulfide, and increase. in the melting point ot the sulfide. THE literature shows that most previous studies of deformation and fracture at hot working temperatures have been based on measurements of energy absorption, reduction of height in forging upset tests, torsion tests of bar or wire samples, and so forth,' but that relatively few tension tests have been used at high temperatures and strain rates. The present work was initiated to study the ef- fects of temperature, strain rate, composition, and structure on the deformation and fracture characteristics of iron, utilizing cast specimens tested in tension. As in a previous study,' strain rates up to 100 pct per sec were chosen for the temperature range 1600° to 2400° to provide data which might be useful in the interpretation of the deformation and fracture behavior of steels under hot working conditions. The previous work was with Fe-P solid solution al10ys;2 this work is concerned with Fe-S alloys, and with the effects of oxygen and manganese additions. MATERIALS AND PROCEDURE Cast tes! specimens were employed throughout, since most of the difficulty during hot working occurs in the initial breakdown of the ingot. Alloy Systems. Ten 25 lb. heats containing sulphur were prepared. Of these, three had manganese additions, and two had oxygen additions. The sulfur content varied from 0.023 to 0.10 pct. Manganese contents were intended to be ten to twenty times the sulfur content of the particular alloy. Oxygen, being more difficult to control in small melts, was varied by the amount of solid deoxidizer added, but poor control of the oxygen content was experienced in most instances. Table I shows the chemical analyses of the heats. Melting and Casting. Electrolytic-iron chips were melted by high frequency induction in a prefired, clay-graphite crucible lined with rammed magnesite.

Jan 1, 1962

By D. R. Miller

Internal friction and elastic modulus variations in electrorefined titanium, iodide refined titanium, and alloys of the latter material with oxygen, nitrogen, aluminum, and zirconium were investigated. No oxygen peak was detected with electrorefined titanium but, provided precautions were taken to prevent increases in background damping, an oxygen peak at about 410°C could be resolved with each of the other materials. An additional partially resolved peak was observed at 500°C in a Ti-N alloy. An anomaly in the variation of rigidity modulus with temperature was observed. Possible mechanisms for the formation of any oxygen peak have been discussed. PRATT, Bratina, and Chalmersl investigated the internal friction of commercial purity titanium and alloys of this material containing 1.5, 3.5, and 4.5 at. pct O. With commercial titanium the internal friction curve consisted of two components, a background which increased steadily with temperature and a peak at about 600" C which was due to grain boundary relaxation. In the Ti-O alloys, however, an additional internal friction peak was observed at 430" to 450°C and, since this peak increased in height as the oxygen content was increased, it was thought to be associated with the presence of oxygen. The diffusion of oxygen in titanium at temperatures between 300" and 500° C is believed to have marked effects in its tensile properties2'3 and the present internal friction measurements were undertaken to obtain further information on this diffusion, using material of higher purity than that of Pratt et d. and an apparatus of very much greater sensitivity. In the course of the investigation a number of important limitations on the work of Pratt et al. were revealed and results have been obtained which emphasize the need for ensuring that in this type of experiment, internal friction is independent of strain amplitude and that the values obtained are reproducible. 1) MATERIALS AND APPARATUS The basis material from which the majority of the specimens was prepared was iodide-refined titanium, the major impurities in which were oxygen and nitrogen—the metallic impurities being present at concentrations less than 0.001 at. pct. The hardness of this material after arc melting, forging, and swaging to rods 1/4 in. diameter was Dph = 110. Specimens 10 in. long and 0.020 in. (0.51 mm) diameter were prepared from these rods by further swaging and wire drawing and were finally annealed in vacuo (5 x 10-6 mmHg) for 24 hr at 800°C. The oxygen alloys were prepared from iodide-

Jan 1, 1962

By K. L. Clark, Nicholas Kowall

MAXIMUM furnace efficiency and close control of final steel composition demand that the steel melter be able to follow closely the variations in the carbon content of the bath. For many years, the fracture test has been used by melters for estimating carbon, because it requires only a very short time to pour a sample into a chill mold, cool it in water, break it with a sledge hammer, and observe the fracture. After long experience gained from the observation of such fractures, most melters are able to estimate the carbon content of steel with amazing accuracy, particularly in the lower carbon ranges. Notwithstanding the utility of the fracture test, there has been widespread interest in other methods for rapid carbon determination to supplement it and to ensure against possible errors in human judgment. Several methods, based upon measurement of magnetic properties as functions of carbon content, have been described in the literature1-6 and have been found to give reasonably reliable results in plant practice when scrap composition is known and controlled. A difficulty encountered in the use of analyzers of the magnetic type is that alloying elements do change the relationship between carbon content and magnetic properties and it becomes necessary to establish calibration curves for all the expected combinations of alloy residuals that are not oxidized in the bath. The work reported here is of an investigation of a method that is independent of alloying elements normally present in constructional steels, being based upon the relatively well-known fact that in plain carbon and low-alloy steels martensitic hardness is a function of carbon content alone. WORK OF OTHER INVESTIGATORS In 1938, Burns, Moore and Archer published a curve7 that showed that the hardness of martensite is a function of carbon from 0.10 to 0.50 per cent and is independent of grain size or alloy content, at least within the range found in constructional S.A.E. compositions. Some of the deeper hardening types investigated, however, contained carbon to a maximum of only 0.20 per cent. Using this principle, Kern8 developed a method of rapid carbon determination for S.A.E. 43xx steels. His procedure consisted of chill-casting a test bar that was large enough to give a surface that could be prepared for Brinell indentations. The test piece was quenched immediately after solidification was complete and hardness readings were taken, so that the carbon content could be read from an experimentally determined curve giving the relationship between as-quenched hardness and carbon. EXPERIMENTAL WORK Although Kern's work had been done with a relatively deep-hardening steel, it

Jan 1, 1944

By A. A. Smith

THE application of indium to bearings was first advocated by C. F. Smart1 in 1938, for the purpose of inhibiting corrosion of certain bearing alloys. He found that a thin layer of indium plated on the bearing surface and subsequently diffused at elevated temperatures markedly decreased the rate of corrosion in lubricating oils containing organic acids. Most of his work was done on cadmium-base alloys, although he showed that the treatment was also effective for copper-lead and other alloys. Since their introduction, indium-treated bearings have found considerable use, particularly in connection with airplane motors.2 Undoubtedly the effectiveness of the indium plate in resisting corrosion depends upon its relative concentration on the bearing surface after the diffusion treatment and after prolonged use at operating temperatures. Some diffusion experiments were made on a number of base metals that had been indium plated, to determine the depth of penetration after heating for reasonably long periods of time. As only the practical aspects were desired, no attempt was made to determine actual diffusion constants. METHOD Two different series of experiments were carried out to study the diffusion of indium into several base metals. Cast cylinders about one-inch diameter were machined to 0.750-in. diameter, so as to remove all surface imperfections, and final finishing was done with oo sandpaper. The original diameters were very carefully measured with micrometers and then a layer of indium was electrolytically deposited on the cylinders from a sulphate bath.3 In the first series of experiments, about 0.002 in. of indium was deposited and diffusion was carried out at 150°C. for a period of 500 hr. in a thermostatically con- trolled electric oven. After the diffusion period, successive layers were machined from the specimens and analyzed spectro- graphically and chemically-the spectro- graphic examination serving as a guide to determine which layers should be chemically analyzed. Apparently there was some surface oxidation of the indium plate due to the long heat-treatment, which may have had some effect on the diffusion. Also, the cadmium alloy showed some incipient melting, which probably was caused by the formation of a low-melting eutectic. To eliminate these factors, another series of experiments was carried out by heating in an electrically heated, automatically controlled, oil bath at lower temperature. The preparation of the specimens was the same as before except that a layer of indium 0.0001 in. thick, an amount commonly used commercially on bearings, was deposited on each of the cylinders. Diffusion was carried out at l20°C. for a period of 200 hours.

Jan 1, 1944

By George Mah, Charles Wert

Internal-friction peaks caused by diffusion of oxygen and nitrogen have been observed in ytterbium. They are thought to be caused by the redistribution, under stress, of strain dipoles around an interstitial oxygen or nitrogen and a neighboring substitutional impurity. With the use of a simple geometrical model, diffusion coefficients for oxygen and nitrogen between special interstitial sites have been calculated. a) APPLICATION OF INTERNAL FRICTION TO MEASUREMENT OF DIFFUSION RATES IN DISSOLVED INTERSTITIAL ATOMS In bcc metals, the interstitial atoms occupy the centers of cube faces (0, 1/2, 1/2), or their equivalents, the center of the cube edges (0, 0, 1/2). An interstitial atom in this position causes an aniso-tropic distortion in the lattice. When stress is applied, mechanical relaxation can take place by the movements of the interstitial atoms. This relaxation has been used to obtain information concerning the movements of the interstitial atoms in the bcc metals. Data for these alloys have been compiled by Stanley and Wert. Other researchers have extended the investigation of interstitial diffusion to the close-packed metals. Gupta and weinig2 found an oxygen peak in a titanium, the height of which is linearly dependent on the oxygen concentration. They assumed, therefore, that they were dealing with movement of atomic ally dispersed oxygen in titanium. KG and wang3 determined that the diffusion coefficients of carbon in fcc steels and in nickel obtained by internal-friction methods were consistent with those obtained by macrodiffusion methods at much higher temperatures. Bisogni found oxygen and nitrogen peaks in hafnium by use of which he deduced the diffusion coefficient of these gases in hafnium. He observed further that the half-widths of these peaks corresponded almost exactly with those of a single-relaxation process; he assumed it to be caused by movement of atomically dispersed oxygen and nitrogen. From these studies, the deduction can be drawn that, in general, diffusion data can also be obtained for the interstitial diffusion in close-packed metals (or more precisely, in slightly impure close-packed metals). One group of such metals for which little data exist for the diffusion of dissolved oxygen and nitrogen is the rare earths. They have great affinity for gases, which enter solution interstitially. In this investigation results were obtained for the Yb-O and Yb-N interstitial solid solutions with traces of substitutional impurities; these solid solutions are of fcc structure. b) MECHANISM OF THE RELAXATION IN FCC CRYSTALS In the fcc structure, an interstitial gas atom is usually situated in the octahedral position (1/2, 1/2,

Jan 1, 1964

By Joseph M. Jacisin

Fatigue tests were conducted on 2017-T4 alumium in alloy in an u1lrcthig.h vacuum of 2 x 10-lo Torr and in air. The vatio of vacuum-to-air faligue life for this ~malerial varied Jrom 3.5:1 at a strain of 2.5 X 1O-3 ill. pegr in. to 8:l at a strum of 3.3 x X ill. per 171. Sotlze pvelivtlinary data were also obtained on the faligue life of the alumirnum alloy in a dvy-nitrogen atmosphere. A dark deposit observed on the fracture surfaces of the aiv-tested specimens was identified as oxides of tr~angarzese and magnesium This observalion, and the close correlalion betaveen results obtained in vaCuum and dry-nitrogen environtments, tend to confirm that air stvongly influences the fatigue mechanism by a covrosion process. THE fatigue life of certain metals is known to increase when the atmospheric pressure is reduced. Gough and Sopwith1-2 postulated that this is due to a joint chemical and mechanical process operating in air at the surface of the metal with oxygen and water vapor playing significant roles. Wadsworth and Hutchings3 observed that aluminum is mainly affected by the presence of water vapor. Very little information is available on the fatigue properties of structural aluminum alloys in a vacuum environment. This report describes work performed on 2017-T4 aluminum alloy in an ultrahigh vacuum (2 x 10-loTorr) and in air. Some preliminary data are also presented on the fatigue life of the alloy in a dry-nitrogen environment. 1) EXPERIMENT 1.1) Test Material. The material tested was commerciaT 2017-T4 aluminum alloy which, in addition to aluminum, has an approximate composition of 4 pct Cu, 1 pct Fe, 0.8 pct Si, 0.5 pct Mg, 0.5 pct Mn, plus smaller amounts of other elements.* Some typical naturally age to a substantially stable condition. Specimens were then machined from these rods and ground to a No. 8 microfinish. In order to minimize variation in material characteristics, specimens were made from rods procured from the same lot. 1.2) Apparatus. The apparatus and test specimen used in the fatigue tests are shown in Fig. 1. The device utilized a single-cantilever beam with rotating-bending loading. Bending stress was applied to the fatigue test specimen by placing a spacer beneath the bearing support, thereby providing a constant deflec-

Jan 1, 1968

By R. I. Jaffee, H. R. Ogden, D. J. Maykuth, W. L. Finlay

Titanium with up to 7.5 pct Al forms single-phase a alloys that are work hardening, not heat treatable, and ductile as welded. The high aluminum Y phase alloys are not usefully ductile, despite their low hardness, but they have excellent oxidation resistance and hot hardness. LITTLE has been published on the effect of aluminum on the mechanical properties of titanium, despite the fact that two of the first four commercial alloys released by titanium alloy producers contained aluminum as an important alloying ingredient. These were both a-ß type alloys, one containing 4 pct A1 and 4 pct Mn and the other containing 3 pct A1 and 5 pct Cr. However, neither of these alloys reflects the true alloying nature of aluminum, since each contains important amounts of the ß-stabilizing addition, manganese or chromium. In a previous publication on the constitution of Ti-A1 alloys,' the authors showed that aluminum had a high solubility in a titanium and was strongly a stabilizing in nature. About 25 wt pct A1 is soluble in a titanium at room temperature. With as little as 5 pct added aluminum, the a transus temperature is increased from 882" to 970°C, and the correspond- ing ß transus to 995°C. The first intermediate phase in the Ti-A1 system is the ordered face-centered tetragonal TiAl phase, which extends from 34 to 46 wt pct Al. The present paper presents hardness data over the entire titanium-rich region of the system, through the TiAl phase, and mechanical property data on the alloy range capable of being fabricated. Methods of Investigation The materials used and general preparation of alloys, as well as experimental techniques used in the investigation of Ti-A1 alloys, have been adequately described.' Briefly, the preparation consisted of arc-melting the desired amount of high purity aluminum (99.99 pct purity) and iodide titanium (maximum hardness 100 Vickers, as deposited) together on a water-cooled copper hearth under a partial pressure of argon. The resulting button ingot was of such form that it could be fabricated without further treatment. All work was done using ingots weighing 10 to 15 g, which were hot-rolled to strip form whenever possible. Tensile samples were 3.25 in. long, 0.5 in. wide, and 0.040 in. thick, with a reduced section 1.25 in. long by 0.250 in. wide. The gage length used was 1 in. Electrical strain gages mounted on the

Jan 1, 1954

By P. C. Claspy, P. H. Smakula

The electro-optic coefficients of LiNbO, and KTao.,5Nboe3,O3 (KTN) have been experimentally determined at the HeNe laser wavelengths of 0.6328, 1.15, and 3.39 µ. The coefficients were calculated fronz the retardation induced by an applied electric field. The retardations were measured by observing one or move transmission maxima and minima as a function of the applied field, and by measuring the retardation directly with a Babinet-Soleil compensator. The values obtained agree quite well with those previo~lsly reported by others. Extinction ratios as high as 3000:l have been observed. Resistivities and Curie temperatures have also been measured. Light-induced optical inhornogeneities in LiNbO, repovted by others have been observed. CONSIDERABLE interest has recently been shown in the electro-optic properties of LiNb03 (Refs. 1 and 2) and KTN.3, 4 These crystals have a number of advantages over such well-known materials as KDP. These advantages include: 1) the infrared transmission of KTN and LiNb03 extends to 5 p whereas that of KDP cuts off at 1.5 p ; 2) driving voltages required for modulators using these materials are considerably lower than those required for KDP. After first discussing some theoretical considerations of the electro-optic effect, we will report the results of measurements of the dc electro-optic coefficients of these materials at wavelengths of 0.6328, 1.15, and 3.39 p. THEORY The generalized equation for the electro-optic effect can be written: Although lattice polarization is the fundamental variable, rather than the applied electric field, we follow the convention of expressing the linear electro-optic effect in terms of the applied field. For LiNbO the quadratic terms are negligible. Since KTN has a center of symmetry the rijk tensor is 0. After applying the usual symmetry considerations and index contractions,* the rijk and gijkl tensors can be expressed as follows: LiNbOaT If field directions are now chosen, the change in refractive index and the angle between the induced optic axes and the crystallographic axes can be found. The induced rotations of the principal axes of the index ellipsoid for fields in principal crystallographic directions are given in Table I. Since KTN is initially isotropic, the principal axes in the zero-field condition are parallel to the crystallographic axes. The induced retardations are given in Table 11. EXPERIMENTAL We obtained the various electro-optic coefficients by measuring the induced retardation as a function of

Jan 1, 1968

By W. McA. Johnson

The work of J. E. Johnson, Jr., on the effect of small amounts of oxygen in cast iron in increasing its strength and resistance to shock, is of interest from the technical and scientific standpoints. The following exposition of the theory carries Mr. Johnson's explanation further and, in my opinion, will disclose certain related phenomena and perhaps shed further light on the subject. Some facts, so novel in character as to excite incredulity, have been accepted finally by many metallurgical authorities. One of these is that oxygen to the amount of 0.060 per cent. in cast iron gives it a breaking strength of 3,500 Ib. per square inch, compared with a breaking strength of 2,500 lb. per square inch in cast iron of the same composition with respect to elements other than oxygen, but having only 0.010 per cent, oxygen. The "oxygenated" cast iron, even if made in a coke furnace, has properties equivalent to the best charcoal pig iron. Mr. Johnson has also established the fact that the variations in combined carbon cannot account for the results. By microphotographic evidence he has shown that in oxygenated cast iron the graphite particles are dense and spherical, while in well-deoxidized cast iron the graphite particles are flaky and leaf-like. It is just a matter of common sense that iron of the latter structure is much weaker than the former. The analytical and microscopical work has been done with care and there is no doubt in my mind about the accuracy of the experimental results. In this paper then, we shall consider it as accepted that small amounts (0.060 per cent.) of oxygen increase the strength of cast iron by producing a structure in which the round and solid particles of graphite are surrounded firmly by a principal matrix of ferrite. The purpose of this paper is to show that the reason why the graphite particles are round is founded on the fact that the particles of any precipitate are made denser and harder by the presence of a reagent having a solvent action on the precipitate. This can be stated as a law, although I have never seen it so given in any textbook. Let us then, for purposes of illustration, give a concrete example and develop the theory of such mechanical and chemical actions as occur: It is well known that, by a soluble sulphate, a barium salt in solution is precipitated in a dense and easily filtered body when the solution is

Jan 1, 1916