Search Documents

By Alexander L. Field

In the light of the experimental data on equilibrium for the reaction C + FeO = Fe + CO in molten steel recently obtained by Kinzel and Egan,l it is necessary to revise current theories regarding the nature of equilibrium between carbon and FeO in the basic open-hearth furnace. According to the measurements of these investigators the equilibrium constant m for the above reaction for a pressure of dissolved CO equal to 1 atm. is equal to 0.0005 at 1550" C., when concentrations of carbon and FeO are expressed in percentages by weight. Their work also shows that, with the pressure of CO fixed at 1 atm., not only is the product of carbon and FeO constant, but carbon and FeO are each independently constant—a circumstance which might have been predicted from theoretical considerations. At 1550" C., carbon is constant at about 0.025 per cent. and FeO at about 0.020 per cent., with the pressure of dissolved CO equal to 1 atm., the product of these two constants being equal to the originally mentioned constant of 0.0005. Available data on the dissolved FeO content of samples taken from the metal bath at practical slag-metal equilibrium prove that this FeO content is determined solely by temperature and the effective FeO content of the slag. The distribution constant r at 1550" C., as determined by Herty, Gaines, Larsen, Simkins, Geruso and Watkins2 is equal to 0.0086. A slag would have to contain 0.020 = 2.3 per cent. effective 0.0086 FeO or less in order to prevent the metal from containing more dissolved FeO than that required for equilibrium with CO at 1 atm. pressure. Such low percentages of FeO are never found in basic open-hearth slags at the completion of a heat when rate of carbon drop has become practi-

Jan 1, 1930

By J. S. Kasper, R. M. Waterstrat, B. F. Decker

THE large difference in the X-ray scattering factors for molybdenum and manganese makes the o- phase in the Mn-Mo system an interesting one to study with respect to ordering of the atoms. Such a study has been carried out using data obtained from a powder sample, and the resulting evidence for ordering in this compound is presented here. It is not possible, of course, to obtain all the details of structure for a u phase from powder data only. Most difficult of all would be the determination of precise atomic parameters. There is reason to believe, however, that the atomic parameters do not vary greatly in the different s'S and that the precise values obtained from one s structure would then allow decisions as to the ordering of atoms to be made when there is a large difference in scattering factors. In particular, the powder intensities for Mn-Mo s are for the most part in good agreement with those observed for Co-Cr, for which single crystal studies have been made by the authors.' There are a few marked discrepancies in the intensity comparison of the two s's, and these cannot be removed by adjustment of the parameters. They are interpreted as resulting from a more pronounced effect of ordering of the atoms. Accordingly, the parameters of Co-Cr s' have been used for the calculations of the Mn-Mo intensities. For Co-Cr, the space group is D4h14-P4/mnm with atoms in the following positions: 1—2 in (b); 11—4 in (f), with x=0.1031; 111—8 in (i), with x= 0.3713 and y=0.0370; IV—8 in (i), with x=0.5662 and y=0.2396; and V—8 in (j), with x=0.3160Y and y — -0.250. The unit cell is tetragonal, with an==9.10A and cn=4.74A for the Mn-Mo u phase studied here.

Jan 1, 1955

By D. M. Boulin, E. S. Greiner

Single crystals of vanadium were bent at 293" and 77°K to a maximum fiber strain of about 1 pct. Analysis of slip line and etch markings of- crystals deformed at either temperature show the slip planes are {112}. The slip directions at 298° and 77°K, deterwined from the asterism axes of rotation of crystals compressed in a {110} direclion, were (111). Etch pits, associated with dislocations, were observed in the plastically deformed vanadium. There was no evidence of mechanical twinning. THIS paper presents results on single crystals of vanadium plastically deformed by bending and compressing at 298° and 77°K. Bcc metals have been observed to slip on {110}, (1121, and (123) planes while the slip direction has invariably been found to be ( 111) 1 Lindley and smallman2 have studied the deformation intension of polycrystalline vanadium between 298° and 20°K and reported that at and above 77°K the deformation is predominantly by slip, but at 20°K the deformation is associated with twinning. Later, Edington and smallman3 found that single crystals of vanadium compressed in a (111) direction at 77°K deformed by twinning on { 112}( 111) systems. Clough and pavlovic4 have reported that mechanical twins were observed in vanadium loaded by impact at 77°, 173°, and 195°K, respectively. PREPARATION OF SINGLE CRYSTALS The vanadium single crystals were made from commercial vanadium reported to contain 0.03 pct C, 0.03 pct 0, 0.02 pct N, 0.0X* pct Ca, 0.0X pct Si, proximately 0.8 cm diam, 4 cm long and were grown in (100) and (110) directions. A crystal for studies of etch pits was gound to have a face parallel to a {l00} plane by the Bond crystal-orienting technique.7 In order to avoid straining, the crystals were placed on the steel mount with a low-melting organic compound (glycol phthalate) before grinding. Crystals for the bending experiments were ground to have the four side faces parallel to ( 100) planes. The crystals were electropolished8 in 10 pct H2So4 using a current density of about 3 amp per sq cm to remove the strained surface material. The crystals were bent slowly by three-point loading in a stainless-steel jig designed by Sylwestrowicz.9 The end rollers of the jig were 3.8 cm apart. DEFORMATION AT 298°K The bent vanadium crystal, after removal from the jig, had a radius of curvature of 20.4 cm over the 2-cm length close to the center loading roller, where the maximum bending moment occurred. This radius of curvature corresponded to a maximum fiber strain of 0.9 pet. The side faces contained slip bands as shown in Fig. 1. These bands are straight where the strain is high, top and bottom of micrograph, but are curved on either side of the neutral axis in the center. This curvature of the slip bands in the low-stress area may be due to cross slip. The plastically deformed crystal was subsequently electropolished and then electroetched in 10 pct H2SO4 solution, using a current density of 0.25 amp per sq cm. The structure is shown in Fig. 2. The directions of the traces on two adjoining faces were plotted stereo graphically, Fig. 3.* Since there were two sets of

Jan 1, 1968

By C. A. Siebert, S. H. Bush

Isothermal temper-embrittlement studies were conducted on a 5140 steel at various temperatures for times as long as 3000 hr. Specimens from the embrittled steel were subjected to impact tests, metallographic examination, microhardness, and lattice-parameter measurements. SEVERAL of the steels in the low alloy group are subject to a pronounced decrease in impact energy if held within, or cooled slowly through, a range of temperatures below the lower critical. This phenomenon, known as temper embrittlement, is quite pronounced in the chromium steels of which AISI 5140 is typical. This study considered the response of one heat of 5140 steel when embrittled isothermally at various temperatures for times as long as 3000 hr. Excellent reviews of the work done in the field of temper embrittlement have been written by Hollomonl and Woodfine.' Both authors list the various theories which have been advanced to explain temper embrittlement. Some of the mechanisms considered were: 1—a transformation below 700°C; 2—an allotropic modification of iron; 3—precipitation from the ferrite of such compounds as carbides, nitrides, phosphides, or chromium oxides; 4—decomposition of retained austenite; 5—modification of special carbides; 6—grain-boundary segregation; and 7—selective distribution of carbides. The present study investigated the changes in hardness, Meyer's number, impact properties, micro-structure, and lattice parameter which occurred on embrittlement. Previous studies considered the influence of microstructure and of prior austenitic grain size3 on the response of 5140 steel to temper embrittlement. Equipment and Procedure All samples were taken from one heat of 5140 steel; the chemical composition of this steel was: 0.43 pct C, 0.86 pct Mn, 0.020 pct P, 0.019 pct S, 0.27 pct Si, 0.84 pct Cr, 0.10 pct Ni, 0.06 pct Mo, 0.10 pct Cu, and the remainder Fe. The material was received as % in. rounds. This stock was cut down to blanks measuring approximately 0.425~0.425~2.196 in. Heat Treatment: The rough blanks were normalized at 1600°F (870°C) for 1 hr, then austenitized at 1600°F (870°C) for 1 1/2 hr, and quenched into an agitated oil bath. The specimens were tempered at 1275°F (690°C) for 5 hr and water quenched. These tempered specimens were designated as the toughened state. Embrittling Treatments: The tempered bars were divided into sets and subjected to the various embrittling treatments listed in Table I. Temperatures from 750" to 1050°F were investigated for times of 1 to 3000 hr. Special tests to determine the effect of heating a short time at a higher temperature after long-time embrittlement at some lower temperature were also conducted. All specimens were water quenched at the end of the embrittling cycle, then ground and notched to obtain standard Charpy V-notch specimens. Impact Tests: The bars were fractured in a 260 ft-lb Charpy impact unit; specimens were fractured at temperatures ranging from —315°F to room temperature. Fixed temperatures used consisted of —315°F with liquid nitrogen, —115°F with dry ice and acetone, and 32°F with ice and water. Intermediate temperatures were obtained by suspending the bars in a jig over the liquid nitrogen, dry ice and acetone, or ice and water.

Jan 1, 1955

By Leonard R. Weisberg

HE procedure of directional freezing by the Bridgman technique1 is frequently used in crystal preparation. On those occasions where the crystal is regrown, it can be advantageous to Crop part of the ingot before regrowth to achieve purification. This note describes some simple, yet interesting, observations concerning the effects of cropping an ingot between successive freezes. First, it is not effective to Crop the front end of an ingot, whether or not the distribution coefficient, k , of the impurities is greater or less than unity. This can be shown as follows. The concentration C, of an impurity in a directionally frozen ingot of length d with a uniform cross section is given by where x is the distance along the ingot, and C0 is the initial concentration per unit length. It is assumed in deriving this equation that diffusion is negligible in the solid, is complete in the melt, and that k is constant. Consider that a section of the ingot Ad is removed from the front end. Then the average impurity concentration in the remaining (d- Ad) section of the ingot can be shown by integration to be given by When the ingot is remelted and refrozen, the new impurity distribution is given by where xl is the distance along the refrozen ingot. Substituting the value of c into Eq. [3], one finds This is identical to Eq. [11 when x = (x, Ad), which represents the original impurity distribution in the (d - Ad) section of the ingot after the first directional freeze. Therefore, the cropping and re-freezing accomplished nothing. This can also be seen physically by realizing that the average impurity content in the melt after the first Ad section is frozen, is identical to that after the resulting ingot has been cropped and remelted. Hence, it is assumed in the following sections that only the tail end of the ingot is cropped. However, it must be realized that for impurities with k greater than one, the pieces cropped from the tail end are purer, and are therefore saved. After cropping an amount Ad from the tail end of an ingot, the average impurity concentration of impurities in the remaining portion of the ingot is given by wheref= d/d. For the case of k < 1, the purification is defined as c,/c. It is obvious from Eq. [5] that the purification increases asf increases, but the increase in purification is not large. For example, iff is doubled from 0.1 to 0.2, the purification increases by only 10 pct for k = 0.5, by only 24 pct for k = 0.1, and by 32 pct for k =0.01. Much smaller values off than 0.1 are not desirable since insufficient purification is achieved. These figures indicate that much larger values off do not lead to substantial improvement, especially considering that much of the original ingot is lost. Therefore, it is generally useful to Crop about 1/10 of the ingot to achieve purification. As compared to doubling the value off, it is much more helpful to remelt, refreeze, and crop the ingot twice. Using Eq. [51 reiteratively, and assuming f= 0.1, it is found that the purification after this process is found to be increased over the purification after a single freeze and cropping by 33 pct for k= 0.5, 450 pct for k = 0.1, and 4100 pct for k = 0.01. This indicates that considerable purification can be obtained by this procedure. However, if purification is the main goal, one should resort to zone refining,3

Jan 1, 1962

By W. D. Robertson, R. E. Reed-Hill

DEFORMATION of magnesium crystals in a direction parallel to the basal plane has a special significance as a result of the preferred orientation characteristic of cold worked and recrystallized polycrystalline magnesium sheet and extruded rod in which the basal plane tends to lie in or near the plane of the sheet or the axis of a rod. The principal objective of the present study is a determination of the modes of plastic deformation in magnesium single crystals in this orientation. Evidence for nonbasal slip in magnesium has been presented by a number of authors. Schmid and Was-serman&apos; indicated that pyramidal slip on {1011} < 1120> or {1012} <1120> could occur above 225°C. Bakarian and Mathewson2 stablished that the slip system {1011} <1120> operates at high temperatures and that 225°C was a lower limit for pyramidal slip. The latter authors also showed that the critical resolved shear stress for {1011} slip was 400 g per sq mm at 330°C, while that for basal slip was 66 g per sq mm at the same temperature. Thus, at 330°C basal slip should be expected for all orientations except those in which the stress axis lies almost in the basal plane. More recently Burke and Hibbard3 oserved pyramidal slip at 25°C, when the stress axis was 6" to the basal plane and 14" to a <1120> slip direction. The critical resolved shear stress for pyramidal slip was 52 g per sq mm, which is only slightly greater than their value for basal slip (46 g per sq mm). Chadhuri, Chang, and Grant4 have observed non-basal slip in creep tests with polycrystalline specimens in the temperature range 250" to 350°C. The observed slip bands, which were extremely irregular in appearance, can be explained in terms of cooperative slip on {1011} and (1010) planes which have a common slip direction. Prismatic (1070) slip in polycrystalline magnesium was observed by Hauser, Landon, and Dorn.5 It was found to occur at low temperatures (78" and 195°K) and it was accompanied by cross slip in which the cooperating plane was the basal plane. Since prismatic slip occurred only at regions of high stress concentrations, the critical resolved shear stress could not be determined. Experimental Procedure The present work was performed on crystal specimens which were all cut from the same large single crystal. The original cylindrical crystal, 0.5 x 7 in., was grown in a Bridgman type furnace in which the temperature gradient was moved past the stationary crystal in the manner described by Jillson6 and Burke.&apos; High purity magnesium was furnished by the Dow Chemical Co. with the following spectro-graphic analysis in weight percent: 0.003 pct Al, <0.01 pct Ca, 0,002 pct Cu, <0.001 pct Fe, 0.008 pct Mn, <0.001 pct Ni, <0.002 pct Pb, <0.01 pct Si, <0.001 pct Sn, and <0.01 pct Zn. The large crystal was cut into four cylindrical pieces about 1.5 in. long. A flat surface parallel to the basal plane was made by hand grinding with lubricated metallographic paper on one side of each cylinder. In order to prevent bending in subsequent cutting operations, the crystals were supported by

Jan 1, 1958

By H. H. Rachford, W. P. Schultz

The use of computing machines to solve physical problems has made it imperative to represent physical data in a form computing machines can use. Although curve-fitting is an old and well-practiced art, there still seems to be some interest in questions regarding what methods can be used and why. Even though there are many good references on this subject, it may be of some value to discuss a particular method which has been found to be useful, and to make available the associated tables for its use in the hope that there can be saved a few of the tedious hours necessary to reduce many of the suggested methods to practice. Although a very brief discussion of the mathematical background of the tables is included immediately below, those interested only in their use can skip directly to the section on Use of the Tables. Direct Fit of a Set of Points A frequently encountered problem is: Given data which can be represented by a smooth curve +(x), to find an easy-to-evaluate function F(x), with only a few coefficients, which is a good approximation of +(x) on the interval 0 5 x 5 x,,. Consider F(x) as a linear combination of m + 1 arbitrary, single-valued, continuous, linearly independent functions, f,(x), Ff.r) = a,f,,(x) + a,f,(x) + . . . -+ aifi(x) + If the value of Q(x) is known or can be read from the curve at the points xj: +(x,), +(x,), . . . +(xj) . . . +(x.), and if n = m, then all the coefficients of F(x) can be determined, and F(x,) — +(x,) = 0 for j =. 0, 1, . . . n. This follows from the solution of the set of linear simultaneous equations. +(x<.) = aofu(x,) + aJI(x0) + . . . + a,,f,,(x,) =a, = f,,(x,) + a,f,(x,) + . . . + a,f,,(x,) +(x,,) = a,,f,(x,,) + a,f,(x,) + ... + a,,f.,(x,,) ...........(2) for the coefficients ai. Although the set a, from the solutions of the set of Equations 2 yields an fix) which gives an exact value of $(x,) for the n + 1 points, there is no restraint on ~(xj in the interval xi < x < xj+,. Indeed, if the points +(x,) are not sufficiently smooth, very serious differences may arise between F(x) in the interval and the smooth curve +(x). Least-Squares Fit It has been suggested&apos; that if n is made to exceed m, and the set a, is found to minimize the function the function F(x) is much less sensitive to small errors in +(xi), and usually provides a much better fit to the smooth function +(x). This is known as the best fit in the sense of the least-squares error. To minimize $, set £ = 0,i = 0,1,... iTi,.....(3) The m + 1 equations from Equation 3 are k—n k=n a.^p /,,(a) f,(xt) + a, X A: = 0 k=O k = n k = n k=0 k=0 +(x.) f,(x,),............(4) one equation being obtained for each i = 0, 1, . . . m. Inasmuch as the arbitrary functions f(x) may be evaluated for x,, k = 0, 1, . . . n, and the +(x,) are known values of the curve to be fitted, the simultaneous Equations 4 may be solved for the set a,. Particular Functions Given the functions fi(x) and the set +(xj), the solutions for require evaluating a number of sums of products as well as the solution of an m + 1 order set

Jan 1, 1956

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,&apos; there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells&apos; and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported&apos; in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F&apos; (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 &apos;/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By Eric R. Morgan, J. C. Shyne

STRAIN aging is the name given to time-dependent changes which occur in the properties of cold-worked metals and alloys during storage. These changes are best observed through a study of mechanical properties, as illustrated in Fig. I for low-carbon steel. The effects of strain aging are usually regarded as being detrimental, particularly in deep-drawing steels. For example, an increase in yield strength and loss in ductility lead to buckling and tearing during drawing. At the same time the return of the yield point results in the formation of Luders bands or stretcher strains during the pressing operation. As a result of these effects many attempts have been made to eliminate strain aging from low-carbon steel. The problem still remains, however, because all known methods of preventing strain aging result in a more costly steel. The present work is an assessment of the situation in terms of theoretical, practical, and economic factors and suggests a new solution to the problem. Previous Work According to the Cottrell theory,&apos; strain aging in a-iron may be regarded as the migration of interstitial atoms to free dislocations and the anchoring of dislocations by the resulting atmospheres. It may be concluded that the important factors which will govern the degree of strain aging are the diffusivity, the effective amount of interstitial element in solution, and the time of aging. The diffusivities and effective amounts of carbon and nitrogen in solution in low-carbon rimming steel are such that significant aging occurs in a few hours&apos; storage at room temperature. Strain aging in deep-drawing steels cannot be controlled by controlling the time of aging because in commercial practice this is determined by economic factors concerned with inventories and may be several weeks. The diffusivity of nitrogen is twice that of carbon at room temperature but the diffusivities can be controlled by controlling the storage temperature. The retardation produced by only a 25 °C drop in temperature is significant but the cold storage of large steel inventories is an impractical solution to Table I. Analysis of Base Materials Alloy Pet C Yet 0 Pet N Vac 0.0037 0.052 0.0003 H 0.0044 0.013 0.0008 C 0.06 0.0014 0.0001 the problem. By far the most simple and effective ways to control strain aging are through control of the amount of carbon and nitrogen in solution. This may be effected through alloying, controlled precipitation, or by eliminating the carbon and nitrogen. Consider first the control of the amount of carbon in solution. The simplest approach would be alloy -ing in which strong carbide-forming elements are added. Examples of this approach are the additions of titanium&apos; and niobium9 0 steel. These elements also combine with nitrogen and oxygen and when added in sufficient quantity result in a completely killed and non-aging steel. They are, however, impractical additions because they result in a costly steel. Carbon and nitrogen are often removed from iron on a laboratory scale by annealing in wet hydrogen, but because of cost this process has never been adopted on a commercial scale. In practice the amount of carbon in solution is controlled by the rate of cooling from the annealing temperature (710°C or 1310°F). In commercial box

Jan 1, 1958

By D. H. Desy, L. C. Fincher

The magnesium-rich end of the Mg-Ti phase diagram was investigated. The liquidus, solidus, and solvus boundaries to 1 pct Ti were established. All alloys were prepared by saturating molten magnesium with titanium in a consumable titanium crucible under inert gas maintained at 230 psig. The liquidus of the Mg- Ti system was determined by analysis of dip samples taken from 700° to 1300°C under equilibrium conditions in a pressurized inert atmosphere furnace and by analysis of small ingots rapidly poured and quenched from 1400° to 1500°C. The solubility of titanium in magnesium ranged from 0.018 wt pet Ti at 700°C (0.012 wt pet at 650°C by extrapolation) to 1.035 wt pet Ti at 1500°C. The solidus for compositions ranging from 0.03 to 1.00 wt pet Ti was determined to be 650° ± 1°C by thermal analysis. The titanium solid solubility values ranged from 0.08 wt pet at 350°C to 0.19 wt pet by extrapolation to 650°C. The freezing reaction is peritectic. No intermetallic compounds were found in the system; the phase in equilibrium with molten magnesium saturated with titanium was found to be titanium with magnesium in solid solution. Solid titanium will dissolve at least 1.32 wt pct Mg. PREVIOUS investigations of the Mg-Ti system have shown considerable disagreement on the solubility of titanium in liquid magnesium. Furthermore, the solid solubility of titanium in magnesium has not been well established. Liquidus curves for previous work and for the present investigation are shown in Fig. 1. Aust and Pidgeon1 used a dip-sampling method on molten magnesium held in equilibrium with solid titanium under a protective atmosphere to determine the solubility and found that it ranged from 0.0025 wt pet Ti at 651°C to 0.015 wt pet Ti at 850°C. Eisenreich2 introduced titanium into molten magnesium by means of TiCL4 adsorbed on BaCl2. Ingots were then cast at various temperatures. Making the assumption that only the titanium dissolved in magnesium at the time of casting was soluble in H2SO4, Eisenreich determined the solubility of titanium in molten magnesium to range from 0.003 wt pet at 655°C to 0.115 wt pet at 800°C. Eisenreich also determined the solid solubility of titanium in magnesium to be 0.015 wt pet at room temperature and 0.045 wt pet at 500°C. Since the solid solubility just below the freezing temperature for the bulk of the alloy was much larger than the liquid solubility just above the freezing temperature, Eisenreich concluded that the freezing reaction was peritectic. Obinata et al.3 equilibrated molten magnesium with titanium in hermetically sealed titanium containers which were then furnace-cooled. The titanium content of the magnesium was then determined and found to range from 0.170 wt pet at 700°C to 0.85 wt pet at 1200°C. No intermetallic compound was found in the system. The Armour Research Foundation4 determined two points on the solvus by electrical resistivity methods: 0.00057 wt pet at 200°C and 0.0008 wt pet at 300°C. At higher temperatures, data were meaningless with no trends observable. The authors of this report believed that the lack of significant data at the higher temperatures was due to variations in specimen geometry, although there was no positive evidence to verify this supposition. The present investigation was undertaken to clarify the uncertainty in both the liquidus and solvus of the magnesium-rich end of the Mg-Ti system. EQUIPMENT AND MATERIALS The equipment used in this investigation, with some modifications, was essentially that used by Crosby and Fowler5 in their determination of part of the Mg-Zr phase diagram. The equipment, as modified for this work, is shown in Fig. 2. It consists of a sealed furnace chamber which can be pressurized with inert gas so that melts can be made above the boiling point of magnesium at atmospheric pressure. Melts are made by induction heating in a titanium crucible which, after diffusion of sufficient magnesium into the walls of the crucible to saturate the titanium at the sampling temperature, comprises the solid phase in equilibrium with the molten magnesium. Dip samples may be taken with the sampling tube, or the entire furnace may be tilted so that ingots may be poured into a mold in the side chamber. The principal difference from the earlier apparatus is in the thermocouple, which in the present equipment is enclosed in a protection tube and immersed directly in the melt. The tips of both the thermocouple protection tube and the sampling tube, which dip into the melt, are made of high-purity titanium. The 4 1/2-in.-long titanium tip of the sampling tube is threaded into a steel tube, O in Fig. 2, which extends through the top of the furnace. To determine whether the temperature at the tip of

Jan 1, 1969

PRESIDENT ARTHUR DWIGHT District 0 NEW YORK, N Y PAST PRESIDENTS EDWIN LUDLOW District 0 MINNEAPOLIS, MINN HERBERT HOOVER, District 4 WASHINGTON, D C FIRST VICE-PRESIDENT JVC REYNOLDS NEW YORK, N Y

Jan 1, 1923

By A. H. Geisler, J. H. Keeler

Preferred orientations in rolled and annealed titanium sheets were determined by the Geiger counter spectrometer X-ray diffraction technique. Five annealing textures dependent upon the temperature range of annealing were found, and in order of increasing annealing temperature pendent upon the temperature range are: 1—a deformation like texture, 2—a rotated inorder a-recrystallization temperature texture, 3-a retained u-recrysraIlization texture, on annealing at lower temperatures of the ß-region, 4—a transformation texture based on recrystallized a and predicted by the Burgers&apos; relationship, and 5—a ,ß-cube texture. These results are examined in terms of current theories of recrystallization textures. UMEROUS investigators have described the tex- ture obtained by cold rolling the hexagonal metals, titanium, zirconium, and beryllium, which have c/a ratios less than that of ideal packing, 1.633. The basal planes are rotated out of the rolling plane, about the rolling direction, so that the basal poles are tilted toward the transverse direction as shown schematically in Fig. la. In all instances but one,&apos; it was also reported that the [1010] direction was parallel to the rolling direction (see Fig. lb). Hot rolling has been reported as causing a similar tilt of the basal poles in the transverse direction (see Fig. la) and causing the [1010] direction also to be parallel to the rolling direction as shown schematically in Fig. lb. Annealing after deformation does not appreciably change the tilt of the basal poles in the transverse direction." Beryllium2-7 continues to have the [1010] direction in the rolling direction after annealing, and similar observations for titanium and zirconium&apos; . have been reported for annealing at fairly low temperatures, again as in Fig. lb. At higher annealing temperatures, however, the recrystallized grains of titanium" and zirconium have an orientation such that the [1120] direction is approximately in the rolling direction, although the basal poles are still inclined in the transverse direction. Figs. la and lc show the resulting orientations schematically. This change in orientation has been described as a nominally ±30° rotation of the hexagonal crystallites about the basal poles of the cold rolled texture and is apparent from the results which are summarized in Table I for investigations with the X-ray diffraction technique employing film. The angles y, , and ß are indicated in Fig. 2 which represents the stereographic projection of (1070) poles for the mean orientation of a pole figure. Texture determinations for titanium using the Geiger counter spectrometer have provided similar results except that in some instances additional components of the texture were proposed, as shown by the summary of data in the upper half of Table 11. On the other hand, the spectrometer technique, when applied to zirconium,* has revealed a splitting Recently completed studies of the textures of annealed zirconium", show zirconium to possess textures very similar to those reported here for titanium. Therefore, much of this discussion will include zirconium by virtue of its close similarity to titanium in pref erred orientations. of the intense areas of the pole figure for samples annealed at 600°C. This splitting could be described by a 7" rotation of the tilt axis about the normal to the rolling plane. Such a splitting for the annealed texture relative to the cold rolled texture was not observed in other determinations for either zirconium or titanium using the less sensitive film X-ray methoe and makes the relationship between the two types of texture more complex than the simple rotation about the (0001) pole based on film work. The more precise investigations on zirconium permit the descriptions in the lower part of Table 11, which show that the texture depends quantitatively on the temperature of annealing. When zirconium is annealed at temperatures up to 400°C, the texture is similar to the cold rolled texture, while annealing in the range 500" to 900°C produces a texture which is only approximately described as [11%] in the rolling direction. More precisely described results for zirconium show that the two types of splitting ( 1—about an axis in the rolling plane through an angle given in the second column in Table II and 2—about the normal to the rolling plane through an angle given in the third column of Table 11) depend on annealing temperature. The [1120 is the rolling direction only when the annealing temperature is in the vicinity of 900°C

Jan 1, 1957

By R. Gibala

Internal-friction measurements on hydrogen-charged iron over the temperature range 4° to 300°K are reported. Two relaxation peaks, the hydrogen Snoek peak at 48 °K and the hydrogen cold-work peak in the range 145" to 2200K, are observed at 80 kc per sec. The effects of hydrogen-charging, aging, and deformation on the internal-friction results are determined and are used to show evidence of partitioning of hydrogen between solid solution and dislocations. The hydrogen-dislocation binding energy is estimated from the behaviors of the relaxation tiwzes and relaxation strengths of the Snoek peak and the cold-work peak. Its value is approxi,mately 6400 cal per mole. MANY investigators have demonstrated the usefulness of internal-friction measurements in determining the manner in which interstitial impurities interact with dislocations in bcc metals. Part of this success has resulted from the existence in bcc interstitial alloys of two anelastic relaxation peaks—the Snoek peak&apos; and the cold-work or Koster peak2 (designated hereafter by SP and CWP, respectively). The SP has its origin in the redistribution of interstitials in solid solution among sites made energetically nonequivalent by an applied stress. The rate at which the redistribution occurs, measured by the relaxation time for the process, is related in a simple way to the diffusion rate of the interstitial in the free solution. The relaxation strength is proportional to the concentration of interstitial in solid solution. The CWP appears to have its origin in the relaxation of an interstitial-dislocation complex for which the relaxation time at a given temperature is much longer than that for the SP. The relaxation strength depends strongly on the concentration of interstitial and the amount of deformation at relatively low concentrations and deformations.2-8 From the dependence of the relaxation strength on interstitial concentration, the SP and CWP may serve as measures of the concentrations of interstitials in free solution and bound at dislocations, respectively. Thus their behaviors have been used to investigate interstitial-dislocation interactions in Fe-C, Fe-N, and several refractory metal systems.&apos;-&apos; However, the Fe-H system has not been studied extensively,? even though disputes in recent years over the mechanism of hydrogen embrittlement in steels involve argument over the extent to which lattice hydrogen and hydrogen-dislocation interactions play an important role.?-&apos;&apos; Previous work on Fe-H indicates the internal-friction behavior to be qualitatively consistent with that for other systems. Apparently, both a SP and a CWP are observed in the temperature ranges 30" to 50°K and 100°to 140°K, respectively (at 1 cps). However, there is neither sufficient nor accurate enough information to identify convincingly these peaks with their supposed counterparts in other systems. Nor have there been any attempts to make quantitative use of these peaks to study hydrogen diffusion, aging, or interaction processes. In this paper, an attempt is made to obtain more complete information on internal friction of hydrogen in iron than presently available. Internal-friction measurements in the range 4° to 300°K on hydrogen-charged iron show that the two peaks discussed above are in fact the hydrogen SP and CWP. Several effects of hydrogen charging, aging, and deformation on these peaks are observed and are used to determine the partitioning of hydrogen between solid solution and dislocation sites in iron. EXPERIMENTAL Materials. The starting material for this investigation was a high-purity iron supplied by National Research Corp. as a 1-in.-diam rod. The following analysis was given (inwt pct): C, 0.004; N, 0.0003; 0, 0.007; P, 0.002; S, 0.005; Si, 0.006; Mn, 0.001; Cu, 0.002; Ni, 0.005; Cr, 0.001; Mo, 0.001. After an initial vacuum anneal (-5 XTorr) at 700°C, the rod was cold-

Jan 1, 1968

By J. O. Brittain, E. Lautenschlager

Yield point measurements were made on polycrys-talline specimens of a iron deformed various amounts at 770, 1950, or 273°K, aged, and redeformed at 77: 195°, or 273°K. When the prestrain temperature is lower than that subsequent to aging, the yield point return is suppressed relative to specimens deformed at the same temperature both before and after aging. The degree of suppression is a function of both the magnitude of prestrain at the lower temperature and the difference between the deformation temperatures before and after aging. It is proposed that the suppression is caused by the formation of dislocation barriers during the initial low-temperature deformation. The aging kinetics of polycrystalline a-iron wires deformed at 77o or 303oK were studied at 44 " and 64 "C using internal friction measurements. No change was noted as a result of the difference in prestrain temperature. IN an earlier investigation1 it was observed that the return of the yield point was suppressed when a poly-crystalline specimen of a iron was plastically deformed at 77oK, aged at room temperature, and subsequently tested at room temperature. In order to investigate this observation, a research program was undertaken to measure the effect of prestrain temperature on the strain aging of a iron.&apos; According to Thomas and Leak,3 return of the yield point and internal friction are similar measures of strain aging since both are dependent on solute atoms leaving the solid solution. The decrease in internal friction as a function of aging time is indicative of the removal of solute atoms from the solution, while the return of the yield point as a function of aging time gives the rate of arrival of solute atoms at the dislocations. According to Cottrell and Bilby,4 the solute atoms create an "atmosphere" which locks the dislocations and causes a return of the yield point upon restraining. In this experiment, both methods of measuring strain aging were employed in order to have two independent measurements of the strain aging phenomenon. In a previous study,5 the strain aging kinetics of a similar lot of a iron were measured for specimens which were prestrained and tested at the same temperature over the range of 77" to 273°K. Although some differences were found in the correlation of the two methods employed for measuring strain aging, the kinetics of strain aging were unaffected by the change of prestrain and test temperature. In another study,6 dislocation line tension and the density of the solute atmosphere were found to contribute to the return of the yield point when ingot iron specimens were prestrained at 303°K and tested at a lower temperature, namely 77°K. This paper is concerned with changes in strain aging kinetics produced by pre-straining at 77" to 303°K and testing at either the prestrain temperature or at higher temperatures up to 273°K. EXPERIMENTAL PROCEDURE The polycrystalline a iron specimens used in both the tensile and internal friction tests were 0.033-in. diam ingot iron wires, wet hydrogen treated and re-carburized. A more detailed procedure for processing a 3/16 in. ingot iron rod (nominal wt. pet composition: Fe - 0.013; C - 0.0125; Mn - 0.023; Si -0.005; P - 0.0023; S - 0.11; Cu - 0.004 N) to 0.033 in. diam specimens containing approximately 0.020 wt pet C and no detectable nitrogen with a grain diameter of 0.033 to 0.040 mm is given elsewhere.5 Immediately prior to testing, specimens were solution treated for 15 min at 700o ± 2°C in a static vacuum of less than 50 ?. of Hg and rapidly quenched into an ice-water bath while still enclosed in a 3 mm quartz vial. The internal friction specimens had 8-in. gage lengths and the tensile specimens had 2-in. gage lengths. The wires used as tensile specimens were first run as internal

Jan 1, 1962

By Robert Gorham Morse

This paper presents the results of an investigation made in the metallurgical laboratory of Columbia University, New York City. The object of the investigation was to determine how the tensile strength, the elastic limit, and the size of the grain, of a pure medium-carbon steel are affected by heating to successive temperatures between 500° and 1300° C., with slow cooling therefrom. Since Dr. Sorby&apos;s first investigations into the microstructure of steel, the study of the subject has been continued by Professor Martens, Mr. F. Osmond, Professor Arnold, Professor Howe, Mr. A. Sauveur, Mr. J. E. Stead, and many others. Among many valuable and interesting papers I mention the following as having a special bearing upon this investigation.* " Microstructure of Steel," by Albert Sauveur, Trans., xxii., 546 (1893); Microscopic Metallography," by F. Osmond, Trans., xxii., 243 (1893); "The Microstructure of Steel and the Current Theories of Hardening," by Albert Sauveur, Trans., xxvi., 863 (1896); "The Crystalline Structure of Iron and Steel," by John Edward Stead, J. Iron and Steel Inst., 1898. II.—Statement of Experiments. Through the kindness of Mr. N. Lilienberg, New York City, round rods 3/4 of an inch in diameter were obtained, which had been rolled from one ingot. The analysis of the steel was as follows : C, 0.343; Si, 0.027; Mn, 0.221; I?, 0.0266; S, 0.0037 per cent.

Jan 1, 1900

By Geo Ashley

THE following paper is intended to be suggestive only, and to open the way for discussion and further observation. Its preparation was requested only two days before the time limit set for the submission of the papers comprising this symposium. Thus no time existed for detailed studies so it is largely a memorandum of such facts as have come incidentally to the notice of the writer in the study of coal in the field. The field study of sulfur in coal has received very little special attention or description from coal students. The presence of sulfur concretions is noted in hundreds of descriptions, and certain benches of a coal bed may be described as "sulfury" or the presence and position of sulfur bands may be noted in coal sections in connection with sampling. It may be accepted that some sulfur is present in all coal. The amount varies greatly in different regions, in different beds, and in the same bed in different areas. The anthracite of Rhode Island comes the nearest of any coal known to the writer of being free from sulfur, several analyses of that coal showing less than 0.1 per cent. Subbituminous coals in Colorado in a few places have close to 0.2 per cent. of sulfur on the dry-coal basis and in other states subbituminous coals approach this lower limit. Bituminous coals seldom run under 0.4 per cent. of sulfur on the dry basis, though in a few places dry bituminous coals in Colorado and Washington have between 0.3 and 0.4 per cent. The better known bituminous coals have almost everywhere over 0.4 per cent. The best of the Pocahontas and New River coals run close to 0.4 per cent., but there is very little commercial coal in Pennsylvania, Ohio, Indiana, Illinois, Kentucky, or the other states that runs under 0.5 per cent. on the dry basis. From these minimum figures, the amount will range up to 5 or 6 per cent. or higher if visible sulfur is not excluded. It must be remembered that the usual -analysis of a coal bed is not intended to give the total proportion of sulfur in the bed but the amount in the coal after the removal of the more obvious and larger sulfur masses.

Jan 9, 1919

By R. B. G. Yeo

The effects of alloy additions on the M, and A, temperatures of an Fe-22.5 pct Ni alloy have been determined. Increasing amounts of titanium, colum-bium, vanadium, and silicon raise and then lower M,while raising A, cmtinuously. Cobalt raises both M, and A,. Aluminum has little effect on Ms but raises A,. Chromium md nickel lower M, and A,. It is proposed that elements raise M, in accordance with their effect on the Ae3 temperature of iron until the lattice becomes stiffened against the shear transformation so that M, is then lowered. An anomaly, first pointed out by Zener,1 arises in steels when the addition of elements, such as molybdenum and tungsten, which raise the Ae3 temperature, also lower the M, temperature.2&apos;3 During the development of a series of martensitic precipitation-hardening (maraging) steels, the effect of several elements on the transformation of austenite to martensite was studied. The results show that under suitable conditions several elements which raise Ae3 also raise the M, and A, temperatures. PREPARATION OF MATERIALS STUDIED A series of alloys was made in which cobalt, titanium, columbium, vanadium, silicon, aluminum, molybdenum, chromium, and nickel were added to an iron base containing 22.5 pct Ni. The compositions of the alloys prepared are given in Table I. The residual manganese contents of the heats were in the range of 0.030 to 0.35 pct, silicon 0.05 to 0.1 pct, carbon 0.0008 to 0.009 pct, and nitrogen from 0 to 0.004 uct. The allois were made as 50-lb induction heats starting with electro-iron and electro-nickel, melted in air to oxidize impurities. Additions of silico-manganese and ferro-silicon were made after which the power was turned off to allow the products of deoxidation to rise and be skimmed from the surface of the melt. The furnace chamber was pumped down to a pressure of 5 p and the charge was heated to 2900°F for the addition of other alloying elements. The heats were poured into five 10-lb ingots, making successive alloy additions to each. The ingots were soaked for 2 hr at 2300°F and hot-worked to 3/4-in.-diam bars. This stock was heated to 1500°F for 1

Jan 1, 1963

By R. P. Carreker

ONE of a series, this report is concerned with the experimental documentation of the deformation behavior of pure metals over a wide range of temperature. Previous reports in the series describe the creep behavior of platinum1 and aluminum2 and the tensile behavior of copper,&apos; silver,& and molybdenum.5 Subsequent reports will describe the creep behavior of copper and silver and the tensile behavior of platinum, thus providing extensive creep and tensile data on four face-centered-cubic metals tested under comparable conditions. Material Two lots of high-purity aluminum were used in this investigation. One lot, designated AC, was obtained direct from the Aluminum Co. of America as high-purity aluminum in notch-bar form. A typical analysis of this type of aluminum is 0.006 pct Si, 0.015 pct Cu, 0.006 pct Fe, and 99.975 pct Al. Lot BS was obtained from J. I. Hoffman of the Bureau of Standards as a portion of the Aluminum A described in his report of the redetermination of the atomic weight of aluminum.6 Lot BS originated with the Aluminum Co. of America also, and was received in the standard notch-bar form. A detailed chemical and spectroscopic analysis of lot BS has been published.6 Principa1 impurities were 0.006 pct Si, 0.003 pct Fe, 0.002 pct Cu, and >99.987 pct Al. Samples were processed identically by room-temperature swaging and drawing to 0.030 in. diam wires from approximately ½ in. diam rods that were machined from the notch-bar pigs. Samples were cut from the cold-drawn wire, placed in a grooved graphite block in groups of thirteen, and annealed in air for 1 hr at each of several temperatures, with the results shown in Table I. The two lots of aluminum responded quite differently to annealing, the behavior of aluminum AC suggesting that its grain growth was controlled by impurities. The recrystallization texture of aluminum of similar purity comparably treated has been reported as predominantly <111> fiber with some <100> fiber present.7 Testing Procedure The testing procedure and method of analyzing the data have been described previously.2,3 Annealed specimens of 5 in. gage length were tested in an Instron tensile testing machine at a constant head motion corresponding to a strain rate of 0.04 min-&apos; at a number of temperatures. Instantaneous tenfold rate changes were employed in some tests to deter-

Jan 1, 1958

By W. T. Hicks

Visual observation of the oxidation of columbium shows that the protective behavior noted previously in gravimetric work in the early stages of the reaction below 600°C and throughout the reaction at 640°C is associated with an adherent oxide. The fact that the oxide is seen to move outward from the metal at temperatures from 550° to 935°C implies that the reaction takes place at the oxide-metal interface throughout this temperature range. THE work described in this paper further clarifies the complex oxidation kinetics of Cb revealed, for example, by the continuous gravimetric studies of T. L. Kolski.1 Time-lapse motion picture studies reveal details of the reaction not provided by a study of the combustion products. EXPERIMENTAL PROCEDURE Cb specimens were prepared from material with the following typical analysis: 0, 0.03 pct; N, 0.002 pct; C, 0.006 pct; Ta, 0.04 pct; Fe, 0.01 pct; Ni <0.003 pct; and Cr <0.003 pct. Arc-cast ingots were swaged and cold rolled into slabs. These slabs were machined into blocks 7/16 by 7/16 by 7/16 in; 1/16-in. holes were drilled through the large face of the blocks for suspension. The samples were then de-greased and annealed 1 hr at 1200°C in vacuum. The sample was suspended by a platinum and Pt 10 pct Rh thermocouple inside a 1-in. quartz tube in a Kanthal wound furnace (2 in. OD by 4 in. long) equipped with windows 1/2 in. sq. A Cine-Kodak Special II 16 mm motion picture camera was trained on the sample through a Spencer microscope adjusted so that a magnification of X1.5 resulted on the film. Super Anscochrome film was used to record the events in color. Argon was flushed through the furnace while the sample came to temperature. The argon was then replaced by a stream of dry oxygen at 1 atm. Pictures were taken at the rate of eight per second for about 20 sec during the change of atmosphere. Then by use of a Stevens time-lapse device pictures were taken at the rate of four per minute starting within 1 min of the initial oxygen flow. In this manner continuous visual records of the oxidation of pure Cb

Jan 1, 1962

By K. Tangri, M. Chaturvedi

On water-quenching from within the (a + ß) phase region Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys can undergo w transfirmation. This transformation has been attributed to the enrichment of ß Zr phase, at the solution-treatment temperature, by the solute atoms. The ß—w transformation is accompanied by a hardening 01 the alloys and in the optimum condition w-bearing specimens of the ternary alloy are about 14 pct harder than those bearing only a&apos; phase. On aging crl reverls thermally to more stable phases, which results in a considerable softening of the specirnens, as follows: w quenched -waged + ß Zr (enriched) waged - a + ß Nb The high-temperature bcc ß Zr in certain zirconium alloys can transform to a metastable w phase which has a primitive hexagonal structure. In the Zr-Nb alloy system w phase has been observed in the composition range of 7 to 15 wt pct Nb by a number of investigators.&apos;-&apos; In this composition range w can form by water-quenching ß Zr or by aging. known as athermal and thermal w, respectively. Hatt and Roberts&apos; have found that thermal w has a constant c/a ratio of 0.622 +0.002 regardless of the composition and tha: the lattice parameters are of the order of a = 5.02A and c = 3.0 ?. The actual lattice parameters depend upon composition and the temperature of aging. The lattice constants of athermal w. however, depend upon alloy composition.3 The presence of w phase in zirconium alloys can cause substantial strengthening which has been attributed as probably due to the coherency between w and parent ß Zr phase. Robinson et al.&apos; found that the presence of w can raise the strength of Zr-5.0 Nb-2.0 Sn and Zr-5.0 Mo-2.0 Sn alloys to about 170.000 psi: however. the ductility is considerably reduced. With the growing use of Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys in the nuclear reactors, and the significant effect of w transformation on the mechanical properties of zirconium alloys studies were undertaken to study the w transformation in Zr-2.5 Nb and Zr-2.5 Nb-0.5 Cu alloys. This paper is concerned with the formation and reversion of w phase in these alloys. 1) MATERIALS AND EXPERIMENTAL TECHNIQUES The following two alloys were studied: 1) Zr-2.5 Nb-0.5 Cu (referred to as the ternary alloy): 2) Zr-2.5 Nb (referred to as the binary alloy). The chemical analysis of the alloys is given in Table I. The alloys, in the form of 3/8-in.-diam rods and 1/8-in.-thick sheets, were supplied by the Chalk River Nuclear Laboratories of the A.E.C.L. Initial fabrication for preparation of various specimens was carried out by cold rolling and swaging with intermediate anneals at 1000°C. All the heat treatments were carried out after the specimens were wrapped in zirconium foils and encapsulated in silica tubes under a vacuum of 5 x 10-% m of Hg. For optical metallography and hardness measurements disc specimens + in. diam by + in. thick were used. After the required heat treatments the specimens were mechanically and then chemically polished in a 45 pct HNO3, 45 pct H20. and 10 pct HF solution. The hardness measurements on the chemically polished specimens were carried out on a Vickers hardness tester using a 10-kg load. For each specimen at least fifteen indentations were made in order to obtain a representative hardness value. The phase identification and structural analysis were carried out using X-rays and electron diffraction techniques. Wires of 1.5 mm diam reduced to 0.12 mm diam by chemical etching were used for making Debye-Scherrer powder patterns using copper K-a radiations in 114.6-mm-diam camera. Thin films for transmission electron microscopy were prepared by electropolishing heat-treated a by 7 by 0.005-in.-thick strips using a modified Bollmann-Window technique. The 10 pct perchloric acid-90 pct methyl alcohol electropolishing bath was kepl at -5OCC and polishing was done at 5 to 10 v. The thinned specimens were washed in ethyl alcohol at -30" to -40°C and dried between filter papers. The thin films

Jan 1, 1970