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By F. E. Block

The metallic reduction of vanadium chlorides was investigated by the Federal Bureau of Mines as a possible new route for preparing vanadium metal in an effort to develop a production process that would be adaptable to large-scale plant production and would yield metal of uniformly high quality. Vanadium tetrachloride was usually prepared by chlorinating vanadium pentoxide in the presence of carbon. Although oxygen-?free tetrachloride was difficult to prepare this way, it could be prepared by the direct chlorination of vanadium carbide. Lower valent vanadium trichloride was prepared by the thermal decomposition of vanadium tetrachloride. Vanadium dichloride was also prepared by the thermal disproportionation of vanadium trichloride.

Jan 1, 1961

By V. M. Benson

A simplified, routine method for determining lithium in lithium-bearing rock is presented. The sample is decomposed by repeated treatments with nitric, hydrofluoric, and perchloric acids. Since this procedure does not appreciably dissolve beryl, interference by beryllium (the principal interfering cation) is minimized for most samples. The salts are brought into solution with water and enough citric acid-ammonium citrate buffer is added to make the final volumetric dilution 0.20 M with respect to citrate. The addition of citrate greatly reduces anion interference in the hydrogen-oxygen flame, slightly increases the intensity of the lithium 671 millimicron emission line, and reduces the effect of most of the interfering cations to the extent that analytical separations are not necessary. The accuracy of results of single determinations of lithium in a pegmatite containing spodumene, lithium-bearing mica, and beryl are approximately equal to that obtained by other flame methods, INTRODUCTION This investigation was undertaken in Bureau of Mines laboratories to develop a reliable, rapid, routine analytical method for determining lithium in lithium-bearing minerals. The requirements of the procedure were that the method should be applicable to the analysis of a variety of lithium-bearing ores and test products, and the results would be reasonably accurate for materials containing 0.05 to 8 percent Li20.

Jan 1, 1961

By M. F. Koehler

[THE LITERATURE contains relatively few thermodynamic values for interoxidic compounds, and these often are unreliable. This is especially true of data for ferrites and aluminates for which heat of formation determinations may involve extreme experimental difficulties. This report contains the results of new experimental work for obtaining the heats of formation of five ferrites (Ca2Fe2O5, CaFe2O4, MgFe2O4,, NaFeO2, and LiFeO2) and one aluminate (CaAl4O7), and a review and revision of previous similar work of this laboratory on five aluminates (Ca3A12O6,, 12/7 CaO-Al2O3, CaAl2O4, NaA1O2, and LiAlO2), The results for the 11 compounds are combined with entropy and high-temperature heat content data to derive tables of heats and free energies of formation (both from the oxides and from the elements) for the temperature range 298° 1,800° K, The relative stabilities of the compounds are discussed. The presented data all have application to ceramic reactions, and those for the calcium and sodium aluminates are applicable in considering soda-lime sintering processes for extracting alumina from silicate minerals such as day and labradorite.]

Jan 1, 1961

By Louis J. Czel

Although lithium was first discovered by Arfwedson in Sweden in 1817, it did not reach any significant status in commercial application until 1908 when Thomas A. Edison received a patent covering the use of lithium hydroxide in alkaline' storage batteries. Edison's achievement can be regarded as a major breakthrough in the development of the lithium industry. In the years prior to 1908 lithium salts had found only modest applications in the pharmaceutical and pyrotechnic fields. The next important milestone in the growth of this net industry occurred in Germany in 1918 when Metallgesellschaft at its metallurgical laboratory at Frankfort-on-Main discovered that the addition of a few hundredths percent of lithium metal to aluminum and its alloys increased-the hardness. This brought into being a new commercial use of lithium in the manufacture of bearing metals. The new material, called "Bahnmetall" (railroad, metal), was widely used for, many years in the manufacture of bearings for railroad and automotive purposes. Its use continued until the early 1930's and there was a short-lived renewal of its production during World War II. Subsequent use of-the alloy was soon outmoded.

Jan 1, 1961

By T. T. Campbell

This report traces the development of techniques for the preparation of high-purity rare-earth metals. Rare-earth metals, excepting samarium, europium, and ytterbium, were prepared by converting their oxides to anhydrous chlorides or fluorides and reducing the rare-earth halides with active metals such as lithium or calcium. High-purity, anhydrous rare-earth chlorides were prepared by dissolving the rare-earth oxides in hydrochloric acid to form hydrated chlorides and by subsequently dehydrating the hydrated salts in the presence of ammonium chloride at temperatures ranging from 70° to 360° C. while under reduced pressure (50 microns to 1 inch Hg). The chlorides were also prepared by direct chlorination of rare-earth oxide-carbon mixtures. Reaction efficiencies in excess of 95 percent were obtained by either method; however, purer chlorides were prepared by the aqueous ammonium chloride conversion method. Purification of yttrium chloride by high-temperature vacuum distillation proved to be an effective method of separating, oxygen-bearing compounds from the chloride. Yttrium metal prepared from purified chloride contained significantly smaller amounts of oxygen (990 p.p.m. oxygen in yttrium metal prepared from raw chloride and 200 p.p.m. in that prepared from distilled chloride).

Jan 1, 1961

By Richard Havens

A flotation procedure was devised by the Federal Bureau of Mines for beneficiating Mount Wheeler, Nev., beryllium ores that contain the beryllium minerals bertrandite and phenacite in a complex association with calcite, fluorspar, mica, quartz, and other accessory minerals, The method also has proven to be effective in trials on ore from the Lake George, Colo., area. Samples used in most of the research ranged from 0.49 to 0.73 percent BeO. Beryllium mineralization varied from two-thirds bertrandite to all phenacite. An unusually high grade sample containing 5 percent BeO as phenacite was floated on a batch basis to prepare concentrate for utilization studies. The beryllium minerals were floated from undeslimed pulps at natural pH using sodium fluoride and sodium hexametaphosphate (HMP), as modifiers, and a fatty acid-fuel oil combination as the collector. Key factors were the use of a minimum of about 4 pounds of sodium fluoride and between 2 and 4 pounds of HMP per ton of ore. Efficacy of the HMP was related to the grind, mineralogical composition, corollary reagents, and type and time of conditioning. Addition of the fluoride, HMP, and collector in that order, followed by appropriate conditioning after each addition, was essential for satisfactory flotation.

Jan 1, 1961

By N. Melnyk, H W. Habgood

The conventional low temperature process for extracting' helium from natural gas involves liquefying the whole gas stream in order to remove the relatively small fraction of helium. A process based on the selective diffusion of helium through a semi-permeable barrier is, in principle, more economical and flexible, particularly for the treatment of small re-serves and low concentrations. The well-known permeability of glass to helium offers the possibility of such a diffusion process and McAfee of the Bell telephone Laboratories showed in 1958 that practical separations could be achieved by passing natural gas over bundles of fine capillary glass tubing. Developmental studies have been carried out involving larger units and more extended field tests than those of McAfee. Fine capillary tubing of Pyrex glass 0.0035 in. diameter was prepared by drawing ordinary 6 mm. laboratory tubing in a furnace. Extraction units were pre-pared containing about 10,000 such tubes, 4 ft. long and cemented inside

Jan 1, 1961

By K. C. Dean

The combination of flotation and chemical processing methods presented in this report of the Bureau of Mines enabled treatment of typical low-grade ferberite ores from the Boulder County, Colo. area, to produce specification-grade synthetic scheelite. The overall recovery from ore to synthetic scheelite was 87 percent, based on a flotation recovery of 93 percent and a similar recovery in chemical processing. Preliminary mineral dressing studies revealed that the physical and mineralogical nature of typical ferberite ores precluded high recovery of tungsten in plus 60-percent-W03-grade products by these methods. Therefore, the flotation research was focused on attaining plus 90-percent recovery in a concentrate containing 10 percent W03. Detailed studies were made (1) to establish optimum grinding conditions for obtaining adequate mineral liberation, (2) to develop collecting and modifying reagent combinations that would enable controllable selective flotation, and (3) to define the influence of different pulp solids, temperature, pH, and time for conditioning and for the rougher and cleaner flotation stages.

Jan 1, 1961

By Bee R. Waples

The Alimak Raise Method, using the Alimak Climber, has proven to be a new, fast, economical method of driving raises at the Iron King Branch of Shat-tuck Denn Mining Corporation, Humboldt, Arizona. In order to fully understand the advantages of the Alimak Raise Climber, it is necessary first to describe the basic machine; second, a complete cycle of a raise round; and third, the comparative speed and economy afforded the Iron King operation by using this new method of raise driving: The raise climber consists of a drilling platform that is raised and lowered by two 6.2 HP compressed air motors that drive, through roller chains and sprockets, three worm gears connected in series. These worm gears drive pinions which grip the guide rail rack. The worm gems are fitted with spring-loaded couplings so that a small rock or grit in the rack is passed over without disturbing the mesh between the rack and the other pinions.

Jan 1, 1961

By Edward J. Murphy

A comparative study has been made by the Bureau of Mines of several analytical methods for determining carbon monoxide and nitrogen oxides in toxic gases produced by the detonation of explosives. Laboratory and field methods and detector-tube devices are described. Analytical results are compared, and reliability of the various methods is discussed. INTRODUCTION In all underground mining there is ever-present danger to persons from possible overexposure to carbon monoxide and nitrogen oxides created by explosives or blasting agents. These health hazards, recognized for many years, led to the early establishment by the Bureau of Mines of specific requirements regarding fumes generated by explosives authorized for use in underground coal mines in the United States.3

Jan 1, 1961

By R. F. Shurtz

R. Duval (Mining Engineer, Ancien eleve de PEcole Polytechnique, Paris, France) I do not agree with the Eq. 3, reading: m =1/100- [(0.214x30.4) + (0.7B6 x0.00)] =6.5pct CaO If 0.214 and0.786 were proportions by weight, the equation would represent the well known mixtures law of the conventional arithmetics and 6. 5 pct CaO would be the correct average content. But it is not the case as the author states: "In samples consisting of single grains of mineral, those grains must, as already mentioned, be either of dolomite or magnesite. Since 78.6 pct of the deposit consists of magnesite and 21.4 pct of dolomite (excluding for present purpose the presence of other minerals), for any single grains picked at random the probability will be 0.214 that is it dolomite and0.786 that is it magnesite. In 1000 such samples the expected numbers of dolomite and mapesite grains will be 214 and 786 respectively." 0.214 and 0.786 would be proportions by weigbt under the necessary condition that all grains of dole mite and magnesite should have an identical weight. Obviously it is not the case, as the specific gravities are not the same for mapesite and dolomite and the volumes of the grains are different. Furthermore, because of these differences the conditions for a random sampling are not fulfilled and we are not authorized to state that the probabilities are, respectively, 0.214 and 0.786. The author however makes a simple application of Eq. 1: M = 1/n— ? fi x i . n Should we deduce that this relation is wrohg? Not at all, but when applying Eq. 1 you must not overlook what it actually. means. Eq. 1 gives a definition of the arithmetic mean of a total of n observed values Xi and nothing else. But the average conteht of a deposit has not the same significance. It is the ratio between the weight of concerned mineral in the deposit and the total weight of the deposit. As from 1000 particles the 214 of dolomite and the 786 of magnesite have not the same weight, the two definitions do not concur, and when applying Eq. 1 the result is an arithmetic mean of figures which has no connection with what is named average contentof a deposit. The situation is similar to the calculation of an average velocity. If a car travels a first mile over at 30 miles per hr and a second mile over at 60 miles per hr, when applying formula 1 you find as average velocity for the 2 miles: 30+60 ------- - 45 miles per hour. Many people calculate in this way and they do not realize that a mistake is involved. In fact the definition of he average velocity for the 2 miles is the quotient of the distance of 2 miles by the time (in hours) necessary for 2 miles travel, i.e.: 2 ---------- = 40 miles per hr. 1 + 1 30 60 In other words, the average volocity wanted is not the arithmetic but the harmonic average of the two velocities. The above mentioned bias in the calculation of the average contents of deposits is frequent, even in the assessments made by experienced engineers and is independant of what is named the sampling error. In order to supress the bias and to be able to use Eq. 1, you must apply a correction. An example on the subject can be found in an article by Duval et al. in the January 1955 issue of the ''Annales des Mines" (French), page 19. R. F. Schurtz (Author's Reply) Mr. Duval's position is quite correct. The proportions shown for dolomite and magnesite., respectively, of 0.214 and 0.786 are, in fact, proportions by weight uncorrected for specific gravity. In our day to day operation of producing magnesite from these mines at a very substantial rate, we do not normally make corrections for the difference between the specific gravity of dolomite and that of magnesite. If these corrections are made in Eq. 3 as shown in my article, then the numbers of grains turn out to be in proportions of 0.226 dolomite and 0.774 mapesite instead of the values actually shown in the equation. For the purposes of our work, and in view of the inherently low accuracy of the data, this correction was not deemed worthwhile making.

Jan 1, 1961

By R. G. Dressler

The Federal Bureau of Mines designed, constructed, and operated a demonstration plant at Louisiana, Mo., to produce gasoline, liquid fuels, and organic compounds from coal by a modified Fischer-Tropsch gas-synthesis process. Satisfactory equipment was developed to produce and purify synthesis gas and convert it into the desired products. Coal or coke was gasified with oxygen and steam to make a gas consisting essentially of carbon monoxide, hydrogen, and carbon dioxide. Dust in the raw gas was removed by cyclone separation, water scrubbing, and electrostatic precipitation. Carbon dioxide, hydrogen sulfide, and organic sulfur were removed with diethanolamine, iron oxide, and activated carbon. The gas was passed over iron catalyst and was converted into synthetic liquids, which were then separated and fractionated into gasoline, diesel oil, other liquid fuels, and oxygenated organic compounds. A 39-day continuous run demonstrated the feasibility of the process. Addition of 3 milliliters of tetraethylead per gallon of upgraded (or finished) gasoline gave a product with an octane rating up to 90 by the research method. After a caustic wash, the diesel oil was of a superior quality; its cetane number was 60 or above.

Jan 1, 1961

By F. P. Haver

The Federal Bureau of Mines developed a 10,000-ampere cell to determine the economic feasibility of producing high-purity electrolytic titanium from mill scrap or offgrade sponge. Operating variables were investigated, matetial handling procedures were established, and the cost of electrorefining titanium was determined. The prototype cell produced premium-grade metal (<100 Brinell hardness number (B.h.n.)) from very impure Kroll sponge at a processing cost of less than $0.60 per pound. Refined metal was deposited at the cathode in the form of coarse (85 percent plus 34-mesh), hexagonal crystals of a titanium when the cell was operated an 850° C. A cathode current density of 1,000 amperes per square foot and a molten sodium chloride electrolyte containing approximately 5 percent by weight of soluble titanium were used. In continuous operation, at the optimum number of ampere-hours, (40,000), the current efficiency averaged slightly less than 60 percent. It was possible to supply large enough amounts of electric current for electrolysis to maintain the temperature of the bath, thus reducing overall power consumption to less than 5 kilowatt-hours per pound of metal refined.

Jan 1, 1961

By R. W. Smith

Many industries such as the cement industry handle large quantities of limestone and clay slurries. However, at present very little is known about the flow properties, such as friction loss due to flow of slurries in pipelines. This lack of knowledge has made it often very difficult to calculate the total dynamic head of a proposed slurry handling system, and therefore has often made the selection of correct size slurry handling equipment difficult. Because of lack of knowledge about slurry flow a study of slurry flow theory has been made at the Portland Cement Association&apos;s Research and Development Laboratory with the idea of developing a method whereby friction losses due to slurry flow may be predicted for any size pipeline. The flow equations developed have been checked by pilot plant size equipment. DERIVATION OF FLOW EQUATIONS It has been known for some time that limestone and clay slurries handled in cement plants do not flow in the same manner as a Newtonian fluid such as water. When a Newtonian fluid flows the shear stress at any flow velocity is proportional to the rate of shear. This phenomenon can be illustrated by a line (Figure 1). The viscosity of the fluid is the slope of the curve. Thus, the flow properties of the material may be characterized by a single materials constant: viscosity. When a non-Newtonian fluid with the type of characteristics exhibited by limestone and clay slurr-ries flow, a similar curve can be constructed (Figure 2). This graph is a shear diagram of a Bingham plastic non-Newtonian fluid. It should be noted that with the Bingham(1) plastic type of flow viscosity, the slope of the curve, is still an important materials constant. In addition, however, there is another materials constant, namely the yield stress of the material. One way to visualize this constant is to consider it as the amount of energy that must be put into a Bingham plastic material to start it flowing.

Jan 1, 1961

Comparative tests of four coals used industrially for coke production have been made by three laboratories of the Federal Bureau of Mines, each using its standard equipment and procedures for evaluating coal for coking. Two of the coals were blends used in the western and eastern sections of the United States, the third was a strongly coking coal widely used for producing coke in Alabama, and the fourth was a blend typical of those used for producing foundry coke in the Birmingham district. The coals used and the cokes produced from them covered a wide range of chemical and physical properties. The tests used at all three laboratories for determining the physical properties of the cokes were made according to ASTM (American Society for Testing Materials) methods. The excellent agreement found for the physical properties of the cokes indicated that, for the coals tested, the BM-AGA (Bureau of Mines-American Gas Association) 18-inch circular retort used at Pittsburgh, Pa" the 14-inch slot-type oven used at Denver, Colo., and the 17-inch slot-type oven used at Tuscaloosa, Ala., were substantially equivalent for evaluating coals for production of coke. Thus, added value is given to data obtained previously and independently at these three Bureau laboratories. INTRODUCTION Laboratory equipment to produce coke for evaluation has not been standardized by the industry. The results obtained with anyone design of equipment have been regarded as showing only the relative values of coal to produce coke of the requisite quality. Few systematic studies have been made to correlate results obtained in different types of equipment. Results of one, in which the Bureau of Mines participated, were published recently.2/ This

Jan 1, 1961

By M. J. Saarivirta

A high-purity copper-zirconium alloy system was imesti-gated. The zirconium content of the alloys studied varied from 0.003 to 0.23 pet. The solid solubility of zirconium in copper and some physical and mechanical properties of the alloys have been determined. By proper heat treatment, Cu-Zr alloy can develop a high electrical conductivity and resistance to softening at temperatures up to 500°C (930°F). This combination of desirable properties makes this alloy superior, to other com-merzcrrl copper base alloys for- use in the electrical conductor field. DEMAND for high conductivity copper alloys that retain their mechanical properties at elevated temperatures is growing rapidly. At present, copper-base alloys such as copper-silver and copper-chromium are used where these characteristics are required. As an example, commutators in electric motors are often made of these alloys. However, the life at elevated temperature of commutators made of copper-silver alloys is much shorter than the life of the same part made of copper-chromium and copper-zirconium alloys. Copper-silver alloys are subject to creep and subsequent failure when the service temperature exceeds several hundred degrees centigrade. Use of copper-chromium alloys has been known for the past several years, but little information is available in the literature concerning the properties of alloys in the copper-zirconium alloy system. Some work had been directed toward determining the solubility of zirconium in copper as well as determining properties of the Cu-Zr alloys. These investigations have revealed the superior high-temperature and electrical conductivity properties of copper-zirconium alloys over copper-chromium alloys. The United States Metals Refining Co., Carteret, N. J. has recently produced OFHC R copper-zirconium alloys for experimentation and evaluation. Because OFHC R copper contains no appreciable oxygen, no harmful oxides are formed and the full benefit of Zr as an alloying addition is obtained. This paper describes the results of this work. It contains room-temperature and some high-temperature data which have been obtained after various processing techniaues. Actual elevated temperature properties are being determined and will be reported in a separate paper. Preliminary results obtained at elevated temperatures suggest that the Cu-Zr alloy is superior to other high conductivity copper-base alloys. WORK PROCEDURE The high-purity oxygen free (OFHC R) copper-zirconium alloys with zirconium content ranging from 0.003 to 0.23 pct were cast into 4-by 4-in. wirebars by both continuous casting and conventional casting methods. Zr was added in the form of a master alloy containing 30 pct Zr and 70 pct Cu. Castings were analyzed for zirconium and nine bars containing various amounts of zirconium were selected for this study. The results of analyses and the sample numbers are given in Table I. Typical analyses of OFHC R copper are also shown. The following properties were studied: A) Solid solubility of zirconium in copper. B) Effect of zirconium on properties of copper. C) Effect of combined working and heat treating on properties of Cu-Zr alloys. The solid solubility of zirconium in copper was determined by metallographic techniques. Specimens for this phase of the investigation were hot rolled at 900oC (1650oF) to 0.250-in. rod. The rolled rods were cut into 2/3-in. long specimens and solution annealed at 950 °C (1740°F), 980°C (1795 °F). and 1020 °C (1870 °F) for 6 hr and quenched in water. In order to find the solid solubility limits at lower temperatures, the homogenized specimens were reheated at various temperatures for 1 hr and quenched. The physical and mechanical properties were determined on 0.250 in. rod, 0.132- and 0.081-in. wires. The wires were cold drawn from the 0.250-in. rods after they were solution annealed at 980 °C (1795°F) and quenched in cold water. Mechanical and electrical properties were determined on cold drawn and

Jan 1, 1961

By Leland A. Yerkes

Refining aluminum from crude aluminum alloys by the subhalide reaction was investigated to develop a method of producing aluminum by means other than electrolysis of its oxide. The best materials and design for the apparatus and also optimum operating conditions, including temperature, pressure, vapor flow rate, and composition of alloy charge were studied. In the subhalide process, aluminum-trihalide vapor reacts with aluminum in the alloy under high temperature and low pressure, forming volatile aluminum monohalide which reverts to aluminum metal and aluminum trihalide on cooling. The only halide used in this investigation was aluminum trichloride. The crude aluminum-silicon alloys used as the principal raw material contained from 21.9 to 36 percent aluminum, and significant quantities of iron and titanium. These alloys were produced by direct electric smelting of clays. Graphite tubing that was heated by an induction coil proved to be satisfactory material for the laboratory reactor chamber, Enclosed in an insulated glass or quartz pipe, the reactor was used in both vertical and horizontal positions with various baffle and tray arrangements for directing the trihalide vapor both over and through the alloy. Aluminum trichloride vapor was generated in the sublimer at one end of the glass pipe, passed into the reactor where contact was made with the crude alloy, and aluminum monochloride gas was formed. When the gaseous mixture of aluminum monochloride and unreacted tri-chloride passed out of the reactor and entered the condenser, the gases were cooled to 900° C. or less, causing the monochloride to disproportionate into aluminum and aluminum trichloride vapor. The aluminum was deposited on the condenser walls while the aluminum trichloride vapor was carried out of the condenser and into the opposite end of the glass pipe where it solidified on the cooled copper coils.

Jan 1, 1961

By Miles B. Royer

The experimental blast furnace has attracted increasing interest during the past decade as a practical means for investigating a broad range of blast-furnace smelting problems. Under experimental-furnace conditions, information can be obtained with less expenditure of time and raw materials and, therefore, at lower cost than comparable information could be obtained under industrial operating conditions. Furthermore, the experimental furnace may be operated beyond the range of smooth operation, even to failure, to delineate the limits of operability. Such deviation from normal operating practice would be economically intolerable in industrial operations where production and operating stability might be disrupted. The Federal Bureau of Mines experimental blast furnace at Bruceton, Pa., near Pittsburgh, has been operated and under development since 1951. However, the usefulness of this experimental data to industrial practice was somewhat nebulous in early experiments, and the correlation of the experimental blast furnace with the industrial blast furnace was not known.

Jan 1, 1961

By Charles W. Huggins

Electron diffraction and electron microscopy were used to determine the unit cell parameters of garnierite [(Ni,Mg)3 Si2O5 (OH)4] and to examine its crystal habit. Bundles of ribbons, many less than 200 A. in cross section, make up the bulk specimen of the garnierite Electron diffraction revealed the unit cell to be monoclinic. Unit cell parameters were: a, 5.33 A,; b, 9.23 A.; c, 14.96 A.; and ß, 94°441.

Jan 1, 1961

By Nicholas J. Grant, Rolf Nordheim, Thomas B. King

Constant-load creep-rupture tests were conducted in an argon atmosphere at temperatures of 1600 to 2200°F on two heats of iron containing about 0.06 and 0.09 pct P in solid solution. The tests were conducted in the as-cast condition. Stresses were selected to give strain rates approaching those encountered in the hot working of steel, and within the limits of the creep-rupture test apparatus, namely. from about 0.001 to 50 pct per sec. FOR generations, rolling and forging practices have been developed largely by empirical methods, based on prior experience. While largely successful, difficulties are frequently encountered when new or different alloy compositions are tried for the first time. There is need to know the relationships which exist among temperature, strain rate, composition, and other variables on the deformation and fracture characteristics of steels. It has been shown for aluminum and several high-temperature alloys that the deformation and fracture characteristics follow rather well-defined laws and patterns which are closely related to the effects of strain rate, temperature, and composition.1"3 As the melting temperature of aluminum or its alloys was approached, it was possible to study the interplay of work-hardening factors and recovery or recrystal-lization, the latter resulting in improved ductility and increased resistance to intercrystalline fracture. In particular, the effects of composition are very poorly known. Within the meaning of "composition" should be included impurity elements, such as sulfur, phosphorous, lead, copper, and many others, as well as those elements which are added for alloying purposes in iron. The role of multiphase structures, in contrast to solid solutions, should also be studied in much greater detail. high strain rate creep-rupture tests would provide information regarding the deformation and fracture characteristics of metals at hot-working temperatures. It was also desired to establish the stresses which are necessary to accomplish the desired deformation, and to relate these to the strain rate and temperature. Secondly, it was the purpose of this particular study to determine the effects of phosphorus, within solid solution limits, on the deformation and fracture characteristics of iron at hot-working temperatures. EXPERIMENTAL PROCEDURE Two phosphorus levels were selected, one corresponding to the upper limit normally found for commercial steels, and one substantially higher than this, but within the region of solid solubility at the test temperatures chosen for this investigation. Twenty-pound heats were prepared by induction melting electrolytic iron in air in a magnesia lined furnace. After deoxidation with about 0.2 pct Al, ferro-phosphorus was added, and the heats were then poured into prefired silica molds. The purpose of using silica molds was to obtain a slow cooling rate during solidification to produce a relatively coarse grain size, producing a structure subject to some segregation and therefore more nearly characteristic of ingot structures. The major part of the casting assembly provided a large shrinkage head in order to produce sound castings and to promote slow cooling of the specimens. The primary austenitic grain size varied from ASTM No. 2 to No. 00. The composition of the heats, including a low phorphorus melt, used for comparison purposes, is shown in Table I. It will be noted that the oxygen content of the phosphorus containing heats is relatively high, in spite of the deoxidation practice, a condition which is difficult to control in small melts. Creep-rupture tests were nevertheless undertaken when it was noted that this quantity of oxygen did not appear to give results any different from those from a heat containing 0.01 pct 0, low phosphorus and comparable carbon Content;4 see Table 11.

Jan 1, 1961