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By George Krauss, M. Cohen

The reverse martensitic transfomzation (i.e., the conversion of martensite to austenite on heating) was investigated in Fe-Ni alloys containing 30.5 to 33.5 wt pct Ni. The reversed austenite was found to be sufficiently distorted to exhibit marked differences in mechanical properties and to undergo recovery and re crystallization on further heating. In particular, the yield strength of the reversed austenite was as much as 2.5 times higher than that of the virgin austenite: with five cycles of the direct and reverse martensitic transformation, the yield strength was 2.6 times higher. There was an accompanying decrease in strain-hardening capacity and in stable ductility or uniform elongation. The recrystallization was observed to follow sigmoidal kinetics, but was characterized by an abnormal1y large temperature dependence which was evidently due to carbon segregation at the migrating grain boundaries. Upon recrystallization, the strength Properties reverted to those of the virgin austenite, but the ductility did not fully recover until the annealing temperature was further raised to dissipate the carbon segregation at the grain boundaries. The transformation of reversed austenite to produce second-generation martensite resulted in an unusually imperfect structure, thereby leaditg to additional strengthening. Horlleuer, the martensitic phase was much less responsive in this respect than was the austenite. MOST martensitic transformations are capable of undergoing a reverse transformation back to the austenitic phase on heating.&apos; This reaction, like the direct transformation to martensite on cooling, is usually athermal. In analogy with the Ms andMf temperatures for the martensitic transformation (where M, > Mf), the reverse transformation is characterized by the As andAf temperatures (where As<Af). It is well-known that the finish (Af) of the martensite-to-austenite reaction on heating may occur at a temperature where austenite is not stable relative to other phases in the equilibrium diagram.&apos; Reverse martensitic transformations have been found to influence the properties of the parent austenitic phase in a number of ferrous alloys. The austenite thus produced after one or more reversals is significantly altered in strength, microstruc-ture, diffusivity, and annealing characteristics compared to well-annealed, virgin austenite. The first detailed observations of such phenomena were made by Wasserman3 on an Fe-30 wt pct alloy. He found that the reversed austenite (i.e., austenite formed by the reverse martensitic transformation) was much stronger than the original austenite, and the second-generation martensite (i.e., martensite produced from the reversed austenite) was somewhat stronger than the first-generation martensite. On heating the reversed austenite, recrystallization occurred in a manner similar to that of a cold-worked metal; the Laue spots sharpened and the strength decreased.4 In recent years, Russian workers have shown considerable interest in these reverse martensitic transformations. Most of such investigations5-10 have been concerned with the stabilization of reversed austenite relative to subsequent martensitic transformation, and because of its unusual nature, this phenomenon will be discussed in detail elsewhere." On the other hand, the annealing behavior of reversed austenite and the attendant variation in properties have received little attention beyond the experiments of Wasserman.3,4 Gridnev eta1.,8 in one of the few such studies. followed the hardness change of reversed austenite as a function of time at three annealing temperatures. The marked strengthening of austenite achieved by the reverse martensitic transformation has been referred to as "transformation strengthening" by Wasserman3,4 and as "phase hardening" by Malyshev et a1.7,9,10 to differentiate it from hardening produced by cold working. Both groups of investigators noted that further strengthening of the austenite could be attained by repeated or cyclic transformations, but the first cycle resulted in the most pronounced effect. Evidence of the altered microstructure of reversed austenite has been reported by Maximova and Nikonorova6 and by Edmonson and KO.12 The former found that reversed austenite was much more sensitive to etching than the original austenite, and the latter authors observed a (&apos;ghost" structure resembling martensite in certain areas of the reversed austenite. Enhancement of the self-diffusion rate in reversed

Jan 1, 1962

By C. J. Bechtoldt, H. C. Vacher

Quenched alloys, prepared by powder metallurgical techniques, were examined by microscopic and X-ray diffraction methods. The compositions and heat treatments were chosen so that the chromium and nickel solvuses could be determined and a range of composition and temperature, in which a eutectoid had been reported, could be explored in small intervals. The results showed no evidence of eutectoid reactions having taken place. ALLOYS containing iron, chromium, molybdenum, and nickel are extensively used in high-temperature applications. In order to provide basic information on the solid-state reactions that occur in such alloys, the National Bureau of Standards is engaged in an extensive study of the equilibrium phases in the binary, ternary, and quaternary systems involving these four metals. Attention was directed to the chromium-nickel system because a review of the literature showed conflicting data. A recent compendium1 of the constitution of binary alloys gives two diagrams for the chromium-nickel system, one a simple eutectic and the second a diagram showing a eutectoid and a eutectic. The eutectoid was the result of an allotropic transformation in a high-temperature solid-solution form of a chromium-rich phase called 0. The approximate temperature and composition of the eutectoid was 1200°C and 30 at. pct Ni. In the preliminary study, at the Bureau, no transformation was indicated in the chromium-rich phase of ternary and quaternary alloys in which chromium and nickel were major components. Similar results have been reported from time to time in the literature,2-8 In consequence of this situation, a systematic study was made of the constitution of heat-treated chromium-nickel alloys using metallographic and X-ray diffraction methods. The compositions of the alloys were selected so as to determine the boundaries of the chromium-rich and the nickel-rich phases and to explore in small intervals the ranges in composition and temperature in which the eutectoid had been reported. The results of this study are reported and discussed in the present paper. EXPERIMENTAL PROCEDURES Materials, Alloys, and Heat Treatments—The alloys were prepared by a powder metallurgy technique similar to that used in earlier work.9 Analyses of the materials used are given in Table I. Powders were mixed using a vibrator in 30-g batches of predetermined composition; 2-g pellets were made from the mixture by compacting at room temperature in a 1/2-in. diam mold under 60,000 lb per sq in. pressure. The pellets were sintered in dry hydrogen for 10 days at 1300°C. At the end of the sintering treatment the specimens were quenched in water, which caused a pale green film to form on the chromium-rich alloys and thin black scale to form on the nickel-rich alloys. The pellets after sintering were approximately 1/2 in. diam by 3/32 in. thick. The purification train9 was modified by inserting a tube of titanium turnings, heated at 700°C to increase the efficiency of the removal of oxgen and nitrogen. It was found in the earlier work that the sintering treatment lowered the carbon, oxygen, and nitrogen contents of chromium-rich alloys to 0.01, 0.01, and 0.004 wt pct, respectively, and that there was a loss of chromium. In order to ascertain the extent of this loss, the chromium contents of certain alloys were determined chemically. They included those alloys used to determine the parameter-composition curves and those of critical composition, used to determine the chromium-solvus microscopically; these analyses were made on samples after the final heat treatments. The mixed powder values for the chromium content of those alloys that were not analyzed were adjusted to conform to a smooth curve based on the chemically analyzed values for

Jan 1, 1962

By M. J. Ginsberg, N. A. Gokcen

THE preliminary study of electrochemical desul-furization performed by Ohtani and Gokcen1 left a number of points concerning the process to be investigated. Two of these were i) the determination of the effect of greater current and voltage on the desulfurizing Flower of acid slags (% CaO/% SiO2- 1) and ii) the possibility of the loss of silica in slag by the reactions 2C (in metal) + SiO2 (slag) = Si (in metal) + 2CO(g) and C + SiO2 (in slag) = SiO(g) + cO(g) proceeding to a point at which the composition of the slag was sufficiently altered toward the basic side so a1.s to noticeably affect the rate of de-sulfurization. The apparatus and the procedure used in the present investigation were the same as those used by Ohtani and Gokcen, except the control circuit was connected to 120 v dc instead of 24 v dc and thereby allowed greater freedom in choosing the values of both current and voltage. The graphite crucible containing the melt and serving as the cathode was 3-in. high, and was of 1 1/2-in. ID with a graphite bar of 3/8-in. diam and 8-in. length threaded into the bottom for electrical connection. This was placed into a magnesja outer crucible with a hole in the bottom and alumina insulation was packed between the two crucibles. A charge consisting of 180 g of

Jan 1, 1962

By H. P. Stüwe

HE recent papers of Aust and Rutter112 have again brought to mind the importance of certain "special" orientation relationships between the lattices of two fcc crystals on the mobility of the grain boundary separating them. No theoretical treatment of this problem has been offered till now. The only principle published so far that has given an indication why certain orientation relationships should be "special" is the counting of "coincidence sites" according to the suggestions by Kronberg and Wilson.3 The "coincidence plots" published by these authors show, for instance, that two fcc lattices rotated by 38 deg around a common (111)-axis have 1/7 of their lattice sites in common. Such an orientation relationship is also characteristic for high boundary mobility. The accuracy of the orientation relationship needed for high mobility is not too rigid. Deviations up to 10 deg from the ideal orientation seem to be tolerable as can be gathered from the experimental data.&apos;j4 The auestion arises, then. how the density of coincidence sites will be affected by a deviatioi from mathematical accuracy. This can be checked by a simple model. Two sieves are prepared, the arrangement of the holes corresponding to lattice sites on a (111)-plane in a fcc crystal. They are placed upon each other, Fig. 1. One is kept fixed, the other is rotated around an axis pushed through one hole in common to both. The light falling through holes of both sieves is then a measure for the density of coincidence sites. If the diameter of the holes is very small, light intensity is contributed only by holes the centers of which coincide "exactly." If the diameter of the holes is rather large, some intensity will be contributed by

Jan 1, 1962

By Michael Hoch, Walter C. Wyder

The isothermul section of the Nb-Ti-Zr-O system at 1500°C was investigated using X-ray dzffraction and metallographic techniques. UP to 66.7 at. pct 0, the system contains nine four-phase regions. Tsopleths at 10, 20, 30, 40, 50, and 55 at. pct 0 weye constructed. The purpose of this investigation was to determine the general shape of the quaternary equilibrium phase diagram of niobium, titanium, zirconium, and oxygen at 1500°C. The system was truncated at 66.7 at. pct. O., PREVIOUS INVESTIGATIONS The Ti-Zr-O system was investigated in this laboratory.&apos; The binary systems of interest have been compiled and discussed by anssen2 and Levin, McMurdie, and Ha11. Elliott4 has determined the Nb-O system by metallographic and X-ray diffraction techniques. He shows the existence of three oxides, namely NbO, NbO2, and Nb2O5. At 1500°C the solubility of oxygen in niobium is about 4 at. pct. No solid solubility region is shown for either NbO or NbO2. EQUIPMENT The same equipment as that for the study of the Ti-Zr-O system was used. The X-ray diffraction patterns were analyzed with the help of the ASTM card set5 and NBS circulars.6 MATERIALS The niobium powder (99 pct pure), the titanium powder (99.6 pct pure), the niobium pentoxide, and the zirconium dioxide used in this study were purchased from the Fairmount Chemical Co., Newark, N.J. The zirconium powder (99.4 pct pure) was obtained from the Charles Hardy Co., Inc., N.Y. Reagent-grade titanium dioxide was purchased from the Matheson Co., Inc., Norwood, Ohio. The oxides were dried in air at 700°C for 24 hr before use. Though the materials used were not "hyper-pure," the impurities present do not affect the results (lattice parameters, phase boundaries), within the experimental accuracy. PROCEDURE Samples of the desired compositions were made up, in mole pct, from the materials listed above. In some cases the intermediate binary compounds, such as NbO and TiZrO4 were prepared beforehand and used in the preparation of the samples. This technique enabled equilibrium to be reached from two sides. The components of each sample were mechanically mixed in a mortar and pestle and pressed into 3/16-in. diam pellets. The pressures used in compacting were of the order of 50 to 100 x 103 psi. Sintering was accomplished by heating the samples in a tungsten crucible (3/4-in. high, %-in. diam, 1/8-in. wall, lid with XB-in. hole). The pellets were separated from each other and from the crucible by means of small spiral coils of tungsten wire placed between the stacked pellets and on the bottom of the crucible. The sintering time was from 4 to 12 hr at 1500°C under a vacuum of 6 x 101-5 to 1 x 10-6 mm of Hg. All samples were reground after the first or second heating repressed, and reheated. In most cases: equilibrium was obtained after the first heating, as the X-ray diffraction pictures after each heating remained unchanged. Quenching of the samples from 1500°C was at first only possible by allowing the crucible and its contents to lose heat by radiation. The temperature dropped from 1500° to 900°c in approximately 1 1/2 min, which was considered adequate when compared to the times used by other investigators to reach equilibrium in the temperature range of 1000°c and lower. Later, a new technique for faster quenching of the samples was cleveloped. This technique involved the removal of the samples from the crucible, whereupon they were quenched by coming in contact with the water-cooled copper base of the furnace. This manipulation was performed without breaking the vacuum. The sample pellets were placed on a tungsten wire rack inside the crucible. The wire rack passed through the hole in the crucible lid, where it was connected to a small nonmagnetic chain. The chain was fed to the side of the furnace by means of a brass rack which fitted between the body and lid of the furnace. Suspended at the end of the chain, near the furnace wall, were three magnetic washers. With the use of a strong

Jan 1, 1962

By J. E. Hilliard, J. W. Cahn

calculation has been made of the standard deviations to be expected in the measurement of volume fractions by areal analysis, lineal analysis and four point-counting Procedures. The effect of experimetztal errors is not included. Our conclusion is that a point count using a two-dimensional grid will be the most efficient method of volume fraction analvsis providing the grid spacing IS coarse enough. The predicted standard deviation for such an analysis is shown to he in good agreement with that determined experimentally. A metallurgist wishing to estimate a structural property by means of quantitative metallography is often faced with a choice between several different procedures. In such a case, he will naturally wish to know: a) Which procedure is the most efficient in the sense of requiring the least effort for a given precision? b) For a given procedure, what are the conditions for maximum efficiency? c) Under these conditions, how many measurements are required to attain a given precision? It is our aim in this paper to provide at least partial answers to these queries as they relate to the estimation of volume fractions from measurements on a random two-dimensional section of an opaque specimen. The commonly used techniques1,2 for volume-fraction analyses are based on one or more of the following principles: i) For an areal or Delesse3 analysis: That the areal fraction of a three-dimensional feature intercepted by a random plane provides an unbiased estimate of the volume fraction of that feature. ii) For a lineal or Rosiwal4 analysis: That the fractional intercept on a line passing at random through a two-or three-dimensional feature provides an unbiased estimate of, respectively, the areal or volume fraction of that feature. iii) For a point-count analysis: That the fractional number of randomly or regularly dispersed points falling within the boundaries of a two-dimensional feature on a plane, or within the boundaries of a three-dimensional feature in a volume, provides an unbiased estimate of, respectively, the areal or volume fraction of that feature. The absence of bias referred to in these principles does not, of course, imply that the results of an analysis will be free of error, but only that the expected result is equal to the true one. Application of the foregoing principles provide the following six possible experimental procedures: a) An Areal Analysis—This involves the measurement with a planimeter (or other means) of the area of a constitutent intercepted by the plane of polish b) A Two-Dimensional Random Point Count—Apos-sible experimental procedure for this analysis is to superimpose a sheet of transparent graph paper on a micrograph, and then use a table of random numbers to select coordinates for the points. c) A Two-Dimensiotuzl Systematic Point Count-Similar to b) except that the points are distributed in a prescribed manner, usually at the corners of a lattice superimposed on a micrograph or the screen of a projection microscope. d)A Lineal Analysis—A measurement of the fractional line length intercepted. It is usually performed by traversing the specimen under the cross hairs of a microscope and recording the distance travelled in each constituent. e) 4 One-Dimensional Random-Point Count— This could be performed by traversing the specimen with stops at random intervals to identify the constituent then present under the cross hairs. f) A One-Dimensionul Systematic Point Count— Similar to e) except that the traverse is stopped at prescribed (usually equal) intervals. It will be noted that the point-counting procedures b) and c) can be regarded as methods of estimating the areal fraction. Similarly, e) and f) are indirect methods of making a lineal analysis. All of the six procedures described above involve at least one stage of sampling. Thus, quite apart from any experimental errors, there will always be a statistical uncertainty associated with the final results. It is with the calculation of this uncertainty that we will be concerned. To avoid unnecessary repetition, the statistical relationships that will be used in the calculations are collected together in the appendix. For a fuller discussion reference should be made to one of the many textbooks5,6 on statistics. For symbols relating to the specimen structure we will follow as far as possible the terminology used by Smith and Guttman.7

Jan 1, 1962

By C. Feng, P. Levesque

HE addition of rhenium to molybdenum is known to produce alloys with good workability.&apos; Lawley and Maddin found that the critical stress for twinning in this system was lowered by the addition of 35 pct Re, which suggests that twinning may re- place the usual slip operation as the major element of deformation. The twinning elements in bcc Mo-Re alloys have been reported as the (112) planes and the <111> directions.3 This note represents the continuation of this investigation, in which the authors found that the occurrence of twinning promotes the formation of a bcc tetragonal phase, previously identified as u by Greenfield and Beck.4 Specimens of Mo-35 pct Re alloy, prepared as described previusly, were solution annealed at 2400o, cooled to room temperature, and plastically deformed by compression to induce twinning. After subsequent aging for 8 hr at 1300°C, traces of a were observed along the grain boundaries and at the interfaces between the twins and the matrix, Fig. 1. With increased aging time the cr phase grew into larger clusters and finally occupied the entire twinned area, Fig. 2. Experiments also indicated that if twinning did not precede aging, there was no visible evidence of a in the microstructure.

Jan 1, 1962

By R. J. Grace

Primarily, this report presents the results of direct efficiency tests which were conducted on the 200-hp Coal-Pak, hot water generator, No. 3 unit, at the Otterbein College heating plant in Westerville, Ohio. Also included is a comparison of fuel consumption of the old plant with that of the new plant, a comparison of efficiencies obtained by the indirect method on a 300-hp Coal-Pak, and the cost of gas vs coal to show the savings effected by the latter. Tests were conducted with ten different bituminous coals selected by Mr. S. A. Frye, business manager at Otterbein College. The coals, of ten different suppliers, from four different states and eight different seams, represented competitive products economically available to the heating plant. The tests were conducted by the usual plant personnel which consisted of the plant superintendent and two assistants. No outside supervision of any kind was given during the tests. The tests were made from Dec. 13, 1960, through Mar. 4, 1961. During this period, 300.03 tons of coal were burned in the No. 3 unit. This tonnage represented 25.5 pct of the total coal requirements for the 1960-61 season. Operation during the period was typical for the comfort heat load which the plant supplies. Of the 78.12 operating days, the boiler was on bank or holdfire 14.31 days, or 18.32 pct of the time. The length of individual bank periods varied from 2 hr to three days. Run periods varied from about 2 hr to 7.26 days. DESCRIPTION OF PLANT AND HEATING EQUIPMENT The new Otterbein College heating plant, completed in the summer of 1957, is located in a 50x50 ft boiler room on the lower level of a combination maintenance building and heating plant. The building is situated away from the main college complex on a hillside, which allows for on-grade delivery of coal to the three bunkers. The bunkers are located directly above and connected with the individual stoker hoppers. Fig. 1 shows an in-plant view of the Coal-Pak installations. The No. 3, hot water, unit is at the extreme right. The heating plant consists of three 200-hp Coal-Paks. Unit No. 1 is operated at 4 psi and carries the steam heating load of 14,000 sq ft EDR (steam) installed in two buildings. Provision has been made to convert these buildings to hot water heating at some future date. Since the unit under maximum load conditions operates only at about 50 pct steaming capacity, a heat exchanger was installed to convert steam to hot water. Thus, during light loads in mild weather the unit can be employed more efficiently to supply both steam and hot water and eliminate the need for operating either of the two hot water units. Units No. 2 and No. 3 serve a hot water heating circuit for a large group of 21 buildings of the College. These boilers deliver hot water at temperatures up to 200°F to the various buildings through distribution lines in tunnels. The present calculated maximum heat loss for the College is 15.195 million Btu per hr. The Coal-Paks have individual design capacities of 6.700 million Btu per hr. Table I lists the design date for the Coal-Paks. The No. 3 unit was chosen as the test unit, primarily because of its bunker location at the far end of the delivery ramp. Because of this location any excess coal above bunker capacity could be conveniently stored and isolated from the adjoining bunkers. Each bunker has a capacity of 30 to 35 tons of coal. The No. 2 and No. 3 hot water generators are equipped with automatic controls which maintain the

Jan 1, 1962

By D. E. Swets, R. C. Frank

It is well known that hydrogen is introduced into iron or steel as a result of many chemical processes (acid pickling, electrolytic cleaning, plating, etc.). One of the reactions that has been of recent interest1 is the reaction between an iron surface and water vapor. It was shown a few years ago2-4 that hydrogen can be introduced into steel at an accelerated rate during abrasion as a result of this reaction. Grun-berg and Scott have also observed that water in mineral oil lubricants increases pitting failure in ball bearings5 and they have suggested that hydrogen from the water is the primary cause of this effect.&apos; In this laboratory, the question was raised as to whether or not hydrogen is also introduced into the metal surface of a bearing as a result of the decomposition of the hydrocarbon lubricant itself, and an experiment was performed to try to find a satisfactory answer. All steel parts contain some residual hydrogen. Therefore, it appeared that the best way to carry out this experiment without the need for highly accurate quantitative analyses was to use deuterium as a tracer. The natural abundance of deuterium in H2 is only 0.015 pct. The tracer was obtained in the form of deuteroparaffin (CD,(CDJ, CD,) and 0.25 g were dissolved in 20 cc of mineral oil to form the lubricant to be used in the tests. The bearings used were New Departure Type QOLOO ball bearings with a ball diam of 0.187 in. Prior to adding the mineral oil-deuteroparaffin lubricant, the bearings were cleaned in warm trichloroethylene to remove the packing grease. After packing with the new deuterated lubricant, the bearings were operated in a bearing fatigue test machine under a radial load of 190 lb and a thrust load of 190 lb at a speed of 3800 rpm. The expected life under these conditions is about 500 hr. Two tests were made; one for a period of 27 hr and the other for a period of 102 hr. The bearings achieved a temperature of 120o F during the tests. When the tests were stopped the balls were mechanically removed from the bearings and were immediately placed in liquid nitrogen to reduce degassing until the analysis for deuterium could be made. Before analyzing, the balls were warmed to room temperature and scrubbed with several degreasing agents to remove all traces of the deuteroparaffin mixture. This cleaning procedure was shown to be satisfactory by running a control test in which one ball bearing was subjected to all parts of the test except running in the fatigue machine. The hydrogen and deuterium were removed from the balls using a hot extraction apparatus attached to a mass spectrometer. Four balls from each bearing were analyzed. Each one was analyzed separately by removing it from a cold storage volume of the hot extraction apparatus and transferring it to the oven tube with a magnet. As the gases were evolved they were analyzed with the mass spectrometer. Since the hydrogen and deuterium pass through steel in the atomic form and since there are many more hydrogen atoms than deuterium atoms in the sample, the probability of forming an HD molecule is greater than forming a D2 molecule. For this reason the evolution of HD and H was followed as each ball was placed in the oven. The results showed that as each ball from the test bearing was dropped into the oven, the mass spectrometer recording of the HD evolution increased by about ten divisions. When balls from the control test bearing were dropped into the oven, the increase was about one division or less. The hydrocarbon background in the mass spectrometer was also monitored to see if hydrocarbons or deuterocarbons were given off when the balls were dropped into the oven, but no change in the hydrocarbon peaks was observed. Since the balls contained a fair amount of residual hydrogen, isotope ratio measurements were made on the gas obtained from each ball. The D/H value found for those balls which had been operated in the fatigue testing machine was consistently about 0.3

Jan 1, 1962

By H. F. Ramstad, F. D. Richardson

The equilibria (a) SiOz +Hz =SiO +H20 and (b) Si + SiO, = 2Si0 have beet1 studied at temperatures of 1425"to 1600°C ad 1310°to 1485°C respectively. The stattdard free energy changes for the tzrro reactions are given by the equatiotts Combination of the results for both equilibria leads to tiotz removes certain anomalies in existing high-terlzperature data for equilibria involving silica and silicon in iron. In many metallurgical processes and in many laboratory investigations silicon monoxide undoubtedly plays an important role. It is unfortunate therefore that wide differences exist between the results obtained by different investigators1-7 in their studies of such equilibria as In an attempt to put our knowledge of SiO on a surer basis, an exhaustive study has been made of equilibria [I] and [2] at temperatures ranging from 1300" to 1600°C. Reaction [I] was studied by measuring the amounts of silica which could be condensed from streams of Hz or Hz + HzO which had previously been brought into equilibrium with silica at temperatures ranging from 1425" to 1600°C. Reaction [2] was studied by measuring the material that could be condensed from streams of Hz or argon which had been brought into equilibrium with mixtures of silicon and silica at temperatures ranging from 1310" to 1485°C. EXPERIMENTAL Materials. The silicon was "superpure" grade and contained less than 0.1 pct impurities. The silica was prepared from pure mineral quartz; this was crushed and treated with concentrated hydrochloric acid to remove particles of iron, washed with water, and finally dried at 120°C. For the hydrogen + silica reaction, the silica was sized to —20+100 mesh. For the silicon + silica reaction, the two materials were ground to a fine powder in an agate mortar. The hydrogen and argon were commercial oxygen-free gases. The gas streams were controlled with capillary flow meters and the volumes were measured by wet gas meters. After passing through the meters, the gases were partially dried by silica gel. The hydrogen for the HZ + SiOz reaction was then passed through palladised asbestos at 300°C and dried with magnesium perchlorate. The efficiency of oxygen removal was checked throughout the experiments by passing the gas over an electrically heated strip of nichrome, used as an indicator as described by Rathman and de itt.&apos; When mixtures of HZ + Hz0 were required, the partial pressures of water vapor (1.8 to 22 mm) were obtained by passing the hydrogen through oxalic acid dihydrateg&apos; lo held at various controlled temperatures, O.l°C, by means of a water bath. The hydrogen for the Si + Si02 reaction was purified by passing it over a mixture of 3 parts of magnesium to 5 of lime heated to 600°."l1 u The argon for this reaction was passed through titanium powder (-3/16 in. + 100 mesh) heated to 900°C. The nitrogen used to prevent the reaction products escaping from the condenser (see later), was deoxidized by copper or iron at 600°C. All these gases were finally dried with magnesium perchlorate. Furnace, Temperature Contr01, and Measurement A molybdenum resistance furnace was used for both sets of experiments. The reactions were conducted inside a high-grade alumina tube, 36 in. long and 1 in. in diam as indicated in Fig. 1. With this arrangement an even temperature zone (2"C) 4 cm long was satisfactorily obtained. The temperatures were kept constant by means of a proportional controller actuated by a Pt-Pt 13 pct Rh thermocouple. This was placed between the two alumina tubes, so that the temperature at the junction was 1400" to 1450°C. Up to 1485"C, the temperatures were measured with Pt-Pt 13 pct Rh thermocouples. For higher temperatures an optical pyrometer was used, this being sighted (through the glass window 1 in Fig. 1) on the end of the alumina tube, that held the SiOz or Si +SiOz mixture, 10 in Fig. 1. The optical pyrometer was recalibrated whenever a change was made in any part of the apparatus situated in the hot zone. Successive readings with the optical pyrometer were reproducible to within 1"C. Equilibrium Apparatus and Procedure. Hydvogen and Silica Reaction. The apparatus is shown in Fig.

Jan 1, 1962

By J. W. Borough

THE electrical conductivity of pure copper is markedly decreased by small amounts of impurity in solution. The magnitude of this effect has been very carefully determined by numerous investigators who studied a wide variety of impurity elements. Much of this work is summarized in an excellent review by Pawlek and Reichel.&apos; The case of zinc impurity in copper is an exception to the above in that there has been no well-documented study of the effect using high-purity starting materials. The values for the effect of zinc on conductivity, which are usually taken from unpublished work by Skowronki, indicate that zinc in low concentration has no effect whatever in lowering the conductivity of pure copper. This effect, if true, is unusual since it is generally known that even in lowest concentration, impurities exert an effect on conductivity which is proportional to the amount dissolved. It is more reasonable to suspect that in the original work on the effect of zinc some of the zinc was oxidized out of solution during specimen preparation. The following experi- and calculated d-spacings based on the unit cell dimensions of Baenziger et al. Since the single crystal studies of Baenziger et al. were limited to (hk0) and (hk 1) data, it was not possible to Compare all the intensities of the powder and single crystal patterns. However, the strongest reflections of both studies, the (321) reflection, agree very well when the appropriate multiplicity factor is used. Good agreement was also found in a number of other reflections of lesser intensity. Despite the precautions taken in annealing the U6Fe powder, an appreciable amount of UO, was detected in the powder pattern after heat treatment. The powder pattern reported by Groganoand Clews is given in Table I. Except for the 3.15A line, which is the strongest line of UO,, their pattern, as far as it goes, compares favoEably with the data from this study. Gordon and Kaufmann have reported a diffraction powder pattern purported to be U, Fe but it bears very little resemblance to the patterns of Table I. ments were carried out to redetermine the effect of zinc on conductivity using high-purity starting materials and processing conditions capable of producing oxygen-free alloys. Materials used in the experiment were ASR 99.999 pct Cu and Cumingo 99.999 pct Zn. Four 1 lb melts were prepared with identical procedure in argon atmosphere with crucibles made from Speer No. 580 graphite. The compositions were 0.0, 0.1, 0.3 and 1.0 pct Zn. Standard No. 14 wire (0.064 in. diam) was made from these melts as follows. The 1 pct Zn sample was first reduced 94 pct by cold swaging with five annealing treatments of 800o for 10 min in hydrogen between swagings, and then reduced 94 pct to the

Jan 1, 1962

By R. W. Kraft, F. D. George, F. D. Lemkey

From a conszderation of the geometrically possible ways in which an array of lines or linear features in three-dimensional space can depart from a statistically random arrangement, a system was developed to describe and measure different types of anisotrypic arrangements of lines in opaque solids. The technique was applied to a specimen of unidirectionally solidified Al-Cwll, eutectic which contained microstructural imperfections termed lamellar faults. Experimental data obtained from photomicrographs of different facets of a grain of this alloy were then analyzed using this system. It was deduced that the defects, which are essentially linear in natuve, were predominantly parallel to one another but not parallel to the nominal growth direction probably because of some lateral heat flow during solidification. InGOTS of lamellar eutectic alloys which have been unidirectionally solidified under growth conditions which prevent colony formation consist of large elongated grains in which the lamellae are approximately parallel to one another. Deviations from a parallel lamellar structure within a grain are caused by extra lamellae which form occasionally during the solidification process. Three-dimensional analyses of such specimens have revealed that one extra platelet produces two defects, termed 1amellar faults, which can and do grow more or less independently of one another.&apos; The faults are analogous in many ways to edge dislocations in crystals. If a lamella of one phase is considered to be basically two-dimensional, e.g., a surface, then a fault can be defined as the locus of points which delineates an edge (or half the periphery) of one extra lamella as it grows and forms bridges and saddles in an otherwise parallel arrangement oi lamellae, Fig. 1. Were it not for the fact that bridges and saddles occur in the structure, the extra platelet could be defined as the unit defect and the concept of linear faults of positive and negative character around the periphery of the extra platelet would be unnecessary. If an extra platelet is merely inserted (actually it is grown in) between other parallel platelets, the fault line around the periphery of the extra platelet would circumscribe one and only one platelet, namely the extra one, and the faults would lie in a plane parallel to the lamellae. But when an extra platelet merges with adjacent ones and each side grows independently of the other, it is no longer topologically possible to delineate "the extra plate." A fault circuit which either closes on itself or passes out of the specimen still occurs although it no longer will be coplanar with the lamellae. In fact, it is usually not even Planar even if the lamellae are. Under these conditions a concept that a specimen contains N extra platelets of a given size per unit volume would be very artificial and consequently meaningless. Therefore, because of the topological complexity of the alloys, it was deemed necessary to define one-dimensional

Jan 1, 1962

By W. A. Tiller

The unidirectional freezing of a semiinfinite liquid from one end has been treated by calculating the solute and temperature distributions in the liquid and solid phases with time, when the solid-liquid interface advances at a rate proportional to (time)lt2. The nucleation probability for new grain formation is calculated as a function of the constitutional and thermal properties of the alloy, the pouring conditions and the catalytic efficiency of the nucleating agents. The transition from columnar crystal formation to equiaxed crystal formation is assumed to occur at a critical nucleation frequency for a particular alloy and the quantitative dependence of the ratio (columnar zone length/equiaxed zone length) upon the freezing conditions has been predicted. The effects of (i) fluid flow in the liquid, (ii) heat transfer through a mold wall, and (iii) a finite ingot length, have been explicitly tveated as departures from ideality. These departures from ideality are found to have very important consequences on the ingot stmcture. In Part I&apos; of this series, a qualitative description of the general ingot structure was developed. The factors that determine i) the ratio of the equiaxed zone length to columnar zone length and ii) the grain sizes in these zones, were discussed. In the present paper, topic (i) will be treated quantitatively, and it is intended that topic (ii) will be treated quantitatively in Part 111. The complete treatment has been split in this manner for ease of development and coherency of presentation. The treatments are quite mathematical in nature and, although some of the conclusions to Part 11 depend upon the treatment presented in Part 111, it was felt that the intended audience would find the material more readable and more useful in its present form. To this same end, it seems worthwhile to reiterate some of the qualitative aspects of grain nucleation during ingot solidification before embarking on the mathematical description. QUALITATIVE ANALYSIS In the conventional method of casting, a liquid alloy with a certain degree of superheat is poured into a mold. The outer rim of liquid metal cools rapidly to the liquidus temperature of the alloy and begins to undercool. As the degree of undercooling increases, nuclei of solid begin to form in this chill layer, this nucleation being catalyzed by certain heterogeneous particles in the liquid. The grains in the chill layer which are generally of random orientation, begin to grow inwards because of heat conduction through the mold. The grains usually develop a columnar shape since the frequency of nucleation of new grains in the liquid ahead of the advancing interface is generally insufficient to seriously impede the growth of the original grains. Due to the slow diffusion rate of solute in the liquid, a solute distribution is formed in the liquid adjacent to the interface which is either an excess or a depletion if the partition coefficient, ko, of the solute is < 1 or > 1, respectively. Thus, the liquidus temperature of the liquid adjacent to the interface is a function of position. The actual temperature in the liquid is also a function of position and the temperature gradient at the interface decreases as the interface moves away from the mold wall. Since the rate of advance of the interface decreases with time, the equilibrium temperature distributions and the actual temperature distributions as a function of interface position, X, can be illustrated as in Fig. 1. Thus, a region of liquid may exist in which the actual temperature is below the liquidus temperature. This liquid is contitutionally supercooled and therefore unstable with respect to the nucleation of new grains. Now, since the supercooling in Fig. 1 increases as the interface moves further away from the mold wall, the nucleation rate of new grains will increase. When the nuclea-

Jan 1, 1962

By A. S. Nowick, C. Y. Li

It is deMonstrated that quenching from an elevated temperataupe accelerates the grain boundary relaxation in two solid solutions (aAg-Zn and a Cu-Al). This result is consistent with the proposal that, in solid solutions, grain boundary relaxation occurs by a mechanism of&apos; self diffusion. Nevertheless, an alternative possibilitg, that quenching introduces vacancies into the boundary itself, must also be considered. THE phcnomenon of grain boundary relaxation has been well known for many years,1,2 yet the mechanism of this process is very poorly understood. One of the most interesting suggestions which relates to the mechanism of grain boundary relaxation was that of Ke,3 who claimed that the activation energy for grain boundary relaxation and for lattice self diffusion were essentially the same. The implication is therefore that the elementary step in the two processes is the same. This suggestion is particularly startling in view of the fact that activation energy for self diffusion along a grain boundary is very significantly lower than that for volume self-diffusion. Later evidence5-7 showed that there really are two grain boundary peaks, one which appears in high-purity metals, and the other (which develops at a higher temperature than the first) which appears in solid solutions beginning at solute concentrations in the range of 0.1 pct. Data for silver6 show that Kg&apos;s hypothesis is surely incorrect for the grain boundary peak in the high-purity metal, since it has an activation energy of only 22 kcal per mole, but that the hypothesis may still be correct for the grain boundary peak in various silver solid solutions, for which activation energies in the range 40 to 50 kcal per mole are observed. If the elementary step in the grain boundary relaxation process were the same as that for self-diffusion, it would be expected that the relaxation process could be hastened by quenching, 2.c. by introducing a non-equilibrium excess of lattice vacancies. Such a quenching effect has already been demonstrated in the case of another anelastic relaxation process, viz., the Zener relaxation effect. The Zener effect, which occurs in essentially all solid solutions, may be attributed to the reorientation of pairs of solute atoms in the presence of an applied shear stress,&apos; and therefore must take place by means of a volume diffusion mechanism. The hastening of this process through quenching9 has been one way of demonstrating that atom movements in the lattice take place through a defect mechanism, presumably single vacancies. In order to see if the grain boundary relaxation is affected by quenching, it is particularly convenient to compare the grain boundary relaxation with the Zener effect, by choosing a specimen for which both relaxation effects appear. Specifically, a fine-grained sample of a solid solution shows in the curve of internal friction vs temperature, first a peak due to the Zener effect, then a second rise (and eventually a peak at substantially higher temperatures) due to the grain boundary relaxation. The same phenomena are also observable in static anelastic measurements, such as creep at very low stress levels. Thus, for the same fine-grained solid solution, the creepstrain, when plotted against log time, falls on a sigmodial curve with a sharp inflection point, due to the Zener effect, which is followed by a second rise and inflection resulting from the grain boundary relaxation. To look for a quenching effect, static measurements are preferable to the dynamic internal friction measurements, due to the fact that quenching effects tend to anneal out too rapidly at the temperatures at which the internal friction is measured.9 RESULTS AND DISCUSSION Creep experiments in torsion were carried out in an apparatus similar to that described by Ke1, whereby a wire is held under constant torque and its angular displacement is observed as a function of time. The alloy Ag-30 at. pct Znwas selected because of the large Zener relaxation that it displays. The two samples used were a "coarse grained" wire with a mean grain size about twice the diameter of the wire (diam = 0.032 in.), and a "fine-grained" wire which had several grains across the diameter. In Fig. 1 a comparison is made of the creep curves at 160°C of these two samples after they had been cooled slowly from 400°C. Curve A, which represents the coarsegrained sample, shows a unique relaxation process due to the Zener relaxation, with a relaxation time, T , in the vicinity of 100 sec. Curve B, which represents the behavior of the fine-grained sample, on the other hand, shows first the same relaxation process as that in A, followed by a turning up of the curve which corresponds to the onset of a second overlap-

Jan 1, 1962

By Charles Law McCabe, Lyndon H. Everett, Edna A. Dancy

It has been found that the carbide phase present at equilibrium in the system M-H2-CH4, at about 600°C, is MC for the rare-earth metals Ce and Pr. X-ray diffraction analysis showed that the monocarbides have fcc structures with lattice constants of 5.036 + 0.009Å and 5.131 + 0.001Å for CeC and PrC respectively. Gaseous equilibrium measurements were used to calculate the standard free energy of formation of the monocarbides from the elements. for the formation of (+ 1300) for the formation of PrC. THE rare-earthdicarbides, and their crystal structures, have been known for some years,l but only more recently were the carbides CeC,2,3 Ce2C3 2 and CeCS3 reported. In 1958 to 1959, Spedding et al. published work on the lanthanum-carbon system4 and other rare-earth metal-carbon systems,5 proving the existence of M2C3 and MC2, and measuring the lattice constants. They also demonstrated that tri-rare earth carbides, M3C, exist for the rare-earth metals samarium through ytterbium. However, they concluded that the cerium monocarbide reported by Brewer and Krikorian2 and by Warf,3 and given a fcc structure with a lattice constant of 5.130Å bythe former workers, was, in fact, cerium metal with carbon dissolved in it. They were also unable to find any evidence for the existence of Warf&apos;s CeC3, for which no structural details had been given. Even more recently, Palenik22 reported the existence of only M2C3 and MC2, having been unable to find any evidence for the existence of any other rare-earth carbides. There are no published experimentally derived thermodynamic data for the formation of any of these carbides, although Brewer and Krikorian6 have estimated values of for CeC, Ce2C3 and CeC2. The objective of the present investigation was; to determine experimentally the free energy of formation of any of the reported carbides of cerium and praseodymium, through a study of the rare-earth metal-hydrogen equilibrium. EXPERIMENTAL A methane-hydrogen mixture was circulated, in a closed system over previously prepared cerium or praseodymium hydride, and when equilibrium had been attained, the gas mixture was analyzed by selectively oxidizing the hydrogen and condensing out the water formed. The metal hydrides were used as starting material for convenience because, otherwise, the hydrogen in the gas mixture would immediately dissolve in the metals; in addition, the metals would not react with methane alone at the experimental temperature (around 600°C). The circulating system was based on that used by Browning, DeWitt, and Emmett7 for similar studies on iron carbides. It consisted of a quartz reaction vessel, all-glass circulating pump, analysis tube containing copper oxide that could be heated to 300" C by means of a small furnace, a solid CO2-methanol trap, and a double limb absolute manometer, Fig. 1. A cathetometer, capable of reading to 0.005 cm, was used to measure the difference in height between the two columns of mercury. In its final form, the reaction vessel was enclosed in an outer jacket, containing approximately the same pressure of hydrogen as that within, to reduce errors due to diffusion of hydrogen out through the fused silica of the reaction vessel., The circulating system was supplied with

Jan 1, 1962

By Charles Smeal, Robert J. Schafer, Max Quantinetz

Normally metal powders cannot be ground to sub-micron sizes because of welding and agglomeration phenomena. Through the use of selected grinding aids and grinding fluids, nickel and other metal powders have been ball-milled as fine as 0.1 It was found that certain inorganic salts are more effective grinding aids for metal powders than conventionally used surfactants. METAL and alloy powders are used to produce reagents, pigments, coatings, solders, brazes, and parts for industry by powder metallurgy techniques. They are also combined with refractory compounds to produce cermets and dispersion-hardened products. One of the interests at the Lewis Research Center has been to explore the potentialities of the dispersion strengthening process. Since the work of Ir-mann, many investigators have shown that the strength of dispersion-hardened products may increase with decreasing interparticle spacing.24 One approach to achieving small interparticle spacing is to combine fine refractory compounds and metal powders, preferably below 1 in size. In attempting to obtain fine metal powders, it was found that until very recently the best that could be obtained from commercial suppliers, particularly of ductile metals, was about 1.0 . Interest was therefore developed in providing finer metal powders for dispersion-hardening studies. Information obtained from the literature, from others working in the field, and from prior experimental work performed at NASA, led to a consideration of ball-milling as a technique to produce the desired materials. Some of the variables associated with ball-milling are the size, material, and nature of construction of the grinding container; the nature and amount of the grinding material and material to be ground; and the nature and amount of the grinding liquid and grinding aid, if employed, and the grinding time. In all ball-milling, welding and agglomeration can oc- cur as well as grinding. Because of the tendency of ductile metals to weld together, they are difficult to grind.5 The ultimate particle size obtained on grinding is generally the one at which the rate of grinding becomes equal to the rate of welding. To help delay welding and thus obtain smaller particle sizes, grinding aids are often employed. The principal objective of this investigation was to produce submicron metal powders by ball-milling the powders with selected grinding aids and grinding fluids. A secondary objective has been to attempt to explain the variations observed in grinding behavior by considering possible grinding mechanisms and correlating various parameters with grinding effectiveness. Three groups of ball-milling experiments were run; one in which the grinding aid was varied, a second in which the grinding fluid was varied, and a third in which the material being ground was varied MATERIALS, APPARATUS, AND PROCEDURE In the first group of experiments in which the grinding aid was varied Inco Carbonyl Grade B nickel powder initially 2.5 (all sizes refer to average particle size as measured by Fisher Sub -sieve Sizer) was used as the material being ground and 200-proof ethyl-alcohol as the grinding fluid. Surfactants, representative of typical organic structures, were selected as grinding aids. Inorganic salts used as grinding aids were chosen on the basis of the size and valence of their ions. Water soluble salts were used in order to facilitate their removal from the slurry after grinding. In the second set of experiments, grinding of the 2.5- Ni powder was tried in four different grinding liquids; water, cyclohexane, n -heptane, and methy-lene chloride. In this study seven grinding aids selected from those tried in the first group of experiments were employed. In the third group of experiments 200-proof ethyl alcohol was again used as the grinding fluid to mill Cu, Cr, Fe, Ag, and Ni powders of various initial particle sizes&apos; All mill charges contained 300 ml of grinding liquid and 3000 g of 1/2 in. stainless steel balls. When inorganic salts were used as the grinding aid, 70 g of salt and 210 g of metal powder were employed, and with surfactants 6 g of grinding aid and 300 g of

Jan 1, 1962

By S. E. Haszko

SEVERAL new XGa2 intermetallic compounds, Table 1, where X is a rare earth, having the AlB, structure were prepared as part of a continuing study of the magnetic and structural properties of rare-earth alloys.&apos; In this note, the crystallographic results of these compounds are presented. Chart, Eq. 121 for the data in Fig. 1 can be adequately represented by The corresponding standard free-energy change is AF; = -4.576 T log K = -20,900 + 10.20T [5I At low nitrogen concentrations the ratio of mole fraction to weight percentage is a constant so that the mole fraction X of nitrogen is given by X = 0.0392 [%NJ. At low values of X, the activity and the concearation approach each other, hence K, = 0.0392 K,, where K, is expressed in terms of the mole fraction of nitrogen. Hence Eqs. [4]. and [5] become

Jan 1, 1962

By B. D. Cullity, K. S. Sree Harsha

When a copper or aluminum single crystal is swaged into wire, the resulting deformation texture depends on the original orientation of the crystal. The<100> and <111>orientations me essentially stable, while <110> is unstable. The greater the <100> content of the deformation texture, the stronger the wire is in torsion. the greater the<111>content, the stvonger it is in tenszotz. The preferred orientation (texture) of fcc wires, either after deformation or recrystallization, is usually a double fiber texture in which some grains have <100> parallel to the wire axis and others have <111>. The relative amounts of these two texture components, as reported by different investigators for the same metal, vary considerably. Previous work in this laboratory&apos; has shown that the starting texture of a wire, i.e., the texture which it has before deformation, can have a decided influence on the texture produced by deformation. In particular, it was found that the deformation texture of copper wire is essentially a single <100> texture, if the wire before deformation contains only a <100> component. This is true even when the deformation is carried to more than 98 pct reduction in area. This paper reports on further studies of the role played by the starting texture. Copper and aluminum single crystals of various orientations have been cold swaged into wire, and quantitative measurements of the resulting deformation textures have been made. The tensile and torsional properties of the deformed wires have also been measured, and the relation between these properties has been correlated with the texture of the wire. These measurements were made in order to demonstrate that a cold-worked wire can be made relatively strong in torsion and weak in tension, or vice versa, by proper selection of the texture before deformation. MATERIALS The copper was of the tough-pitch variety, containing, by weight, 99.962 pct Cu, 0.003 pct Fe, 0.025 pct 0, and 0.0021 pct Si. The aluminum contained more than 99.99 pct .&apos;41; the only reported impurities were 0.001 pct Fe, 0.001 pct Si, and 0.003 pct Zn, by weight. Large single crystals of these metals were grown by the Bridgman method in graphite crucibles and a helium atmospliere. Cylindrical specimens of predetermined orientation, about 1.5 in. long and 0.36 in. in diameter, were machined from the as-grown crystals and then etched to 0.25 in. to remove the effects of machining. Their orientations were checked by back-reflection Laue photographs, and they were then swaged to a diameter of 0.050 in. (96 pct reduction in area). 111 order to study the "inside texture" of the deformed wires, they were etched, after swaging, to a diameter of 0.040 in. before the texture measurements were made. TEXTURE MEASUREMENTS The fiber texture which exists in wire or rod can be represented by a curve showing the relation between the pole density I, for some selected crystal-lographic plane, and the angle $ between the pole of that plane and the wire axis (fiber axis). Such a curve will show maxima at particular values of , and these values disclose the texture components which are present. The relative amounts of these components can be determined2&apos;3 from the areas under the maxima on a curve of I sin F vs F. It is seldom necesszlry to measure I over the whole range of F from 0 to 90 deg, since the existence of maxima in the low-F relgion can be inferred from measurements confined to the high-F region. The X-ray measurements were made with a General Electric XRD-5 diffractometer and filtered copper radiation, according to one or the other of the following procedures: 1) A method developed in this laboratory,4 involving diffraction from a single piece of wire. 2) A modification of the Field and Merchant method.5 This method was originally devised for the examination of sheet specimens, but it can easily be adapted to the measurement of fiber texture. Three or four short lengths of wire are held in grooves machined in the flat face of a special lucite specimen holder. The axes of the wires are parallel to the plane defined by the incident and diffracted X-ray beams, and the holder to which the wires are attached can be rotated step-wise about the diffractometer axis for measurements at various angles 9.

Jan 1, 1962

By N. M. Parikh, T. J. Koppenaal

The strengthening mechanism of fiber-reinforced silver has been investigated as a function of fiber density and fiber material. Stress-strain curves were determined in the range 2 x 10-6 to 2 x 10-3 plastic styain and slip lines were examined. The yield strength at 0.2 pct permanent strain is markedly dependent upon fiber density but the stress necessary to initiate plastic deformation is independent of fiber density. The strengthening mechanism of the fibers is shown to be malogous to grain boundary strengthening in poly crystalline metals. The variation in strengthening with different types of fibers is also noted and discussed. In recent years, considerable progress has been made in the understanding of the mechanical properties of two-phase systems, particularly in the classical dispersed-phase alloys where the separation between the dispersed phases is 0.01-0.1µ. However, little work has been done on fiber-reinforced metals where the dispersed-phase separation is considerably larger than this. Parikh1 investigated the mechanical properties of many fiber-reinforced metals and found that two general relationships are always observed, as follows: 1) A fibrous network incorporated into a second weaker metal strengthens the latter, and the amount of strengthening increases with fiber concentration. 2) At a corrstant fiber concentration, the amount of strengthening in a given matrix can vary considerably, depending upon the type of fiber employed. The object of the present investigation was to examine the fuiidamental factors controlling these two observations. procedure: Fig. 1 shows the initial step in the fabrication of the specimens. The sieve is shaken so that the fibers fall into a mold with the longitudinal axes of most fibers in the X-Z plane. The fibers are then compressed to a predetermined density, thus forming a "felt", and the necessary amount of matrix metal is added to the top of the felt. The mold is heated, in vacuum or hydrogen, to above the melting point of the matrix metal; the molten metal flows into the felt, and the entire assembly is cooled. This produces a "composite" that is essentially free of voids. A number of composites were prepared in this manner using 1/4-in. kinked lengths of mild steel

Jan 1, 1962

By Robin O. Williams

The increase in internal energy as the result of deformation has been measured for lead, aluminum, silver, nickel, iron, and zirconium by using rapid, adiabatic compression. The stored energy increase is roughly Proportional to the strain; the propor-tionality constant increases rapidly with increasing melting point. The fraction of the mechanical energy which is stored increases more slowly, since the strength of the metals also increases with melting point. The values of the stored energy are considered accurate to about 10 pet. The present values appear about 50 pet larger than the more reliable published results where comparisons are possible. It is possible that this difference is due to the high strain rate used in this investigation. Immediately after deformation all these metals release energy at a rate roughly proportional to (time)-&apos;. This release is considered to be associated with dislocation motion but in aluminum (and copper) some additional process seems to be present. This release can represent 20 pet or more of the stored energy. WHEN pure metals are plastically deformed, most of the mechanical energy is converted into heat. The energy remaining within the metal is significant in that it is the energy of the disorder produced and thus detailed knowledge of this energy is a powerful tool in understanding the nature of deformational disorder. While much effort has been expended on this problem, the amount of information available is limited. The situation as of 1958 has been carefully reviewed by Titchener and ever.&apos; The present results have been obtained by a new experimental approach to this problem. The method necessitates high-strain rates which make comparisons with published results less certain, but a high-strain rate is an advantage in that the energy release immediately after deformation can be followed. EXPERIMENTAL PROCEDURE In the experimental method used, the internal (stored) energy is given as the difference between the mechanical work used in deforming the sample and the heat which is released (the first law of thermodynamics). The work is supplied by two identical hammers swinging freely from a fixed height, the available energy being the product of the mass, the gravitational constant, and the distance through which the center of gravity moves. The initial temperature rise of the sample represents the heat produced by the deformation. The sample temperature is determined by a small thermocouple embedded in and supporting the sample. This process can be repeated over and over to produce increased strains. Most samples are run through about five cycles to a total strain of around 0.7. Further details are covered elsewhere. The determination of the heat is dependent upon the sample weight, its specific heat, the rise in temperature, and any gains or losses to the surroundings. One is dependent on published results for specific heals (the values were taken from a collection).3 The values must be accurate to about 0.1 pet in order that they not affect the results. The best values thus do not contribute to the uncertainty, but this is probably not always the case. The accuracy of the temperature rise is limited primarily by knowledge of the thermocouple characteristics over short temperature intervals, but careful calibration eliminates this as an important factor. One can calculate readily the heat flow between the sample and hammers if the time of contact and the sample temperature are known and if there were no oil at the interface. Assuming the maximum temperature difference, upper values for this interchange have been calculated (the time of contact is determined from the decrease in sample length) and it may or may not be significant. However, no correction is colnsidered necessary because of the presence of a thin oil film which has a thermal conductivity much less than the metals. Except for the possible uncertainty in specific heat, the heat is considered to be adequately known. The mechitnical losses which are recognized as important are: 1) friction between the sample and the hammer:;, 2) the kinetic energy in the hammer suspension system which may not be entirely usable, 3) the rebound energy of the hammers, and 4) the vibration of the hammer heads. All these have been covered in detail elsewhere2 and only the more significant points are made here. The friction turns out to be small except for soft materials (lead)

Jan 1, 1962