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By Robert E. Green, P. W. Kingman

Application of a constant geometry compression test to single crystals of aluminum of selected diameters from 1/4 to 1/64 in. showed the presence of a diameter-dependmt size effect. The most pronounced effects were found in those crystals oriented for single slip, while for specimens possessing orientations in the comers of the standard stereographic triangle virtually no size effect was exhibited. The yield stress of the crystals oriented for single slip was found to increase with decrease in specimen diameter, while the strain-hardening rate was found to be lower for the smaller specimens. The experimental results are in general agreement with those of other investigators obtained from lensile tests on copper and aluminum crystals. THE earliest systematic investigation of a possible size effect on the plasticity of metals was that of no,' who in 1926 performed tensile tests on cylindrical aluminum single crystals with diameters of 3 to 8 mm. Ono concluded that the gross stress-strain curve did not show a diameter dependence, but that the resistance to slip for strains of 0.1 pet and less appeared higher for 3-mm-diam crystals than for larger sizes. Later studies of aluminum by Maddin et al2 tentatively concluded that a size effect exists, but the conclusions were again open to question because of inconsistencies in the experimental data. Wu and Smoluchowski3 had previously shown that the slip system activated in a single-crystal sheet specimen of aluminum is a function of the specimen cross section in the slip direction, but no stress-strain data were obtained. Subsequently Fleischer and Chalmers4 studied the effect of the length of the slip direction of the primary-slip system on the stress-strain curve by testing aluminum crystals with geometrically dissimilar cross sections. In the course of this investigation a size effect was indicated in rather large crystals; however, the number of these tests was small. Other investigators have indicated that a size effect in aluminum is appreciable only for diameters of 0.5 mm or less.5, 6 Size-effect studies have also been carried out on copper crystals, the most detailed being that of Suzuki et a1.7 who performed tensile tests on specimens of many diameters ranging from 2 to 0.12 mm. Suzuki found a strong size dependence in the easy-glide region, both the extent of the easy glide and the hardening rate in easy glide were size-dependent, and the size effect was found to be orientation-dependent. Suzuki's results are in agreement with the less extensive observations of Pater-sonB and those of Garstone et al.9 A size effect was found by Rebstock using tubular copper crystals.'0 Size effects have also been noted in a brass,6, 11 in cadmium,12'19 and in hexagonal crystals.14 All the previously cited works have been entirely concerned with the variation of specimen cross section. The effects of specimen length and the change of specimen geometry which results from using progressively thinner specimens while maintaining the same specimen length have been largely ignored. A theoretical discussion of the effects of specimen length and geometry has been given by Hauser and Jackson,15 who predict a grip effect on easy glide as a function of specimen geometry provided that the specimen dimensions are large compared with the spacing between the slip bands, and by Fleischer and Chalmers,18 whose analysis of grip effects resulting from lattice rotation predicts an increase in easy glide with an increase in specimen length. A study of size and geometry effects in aluminum crystals by Kitajima and shimba17 indicated increasing amounts of easy glide in specimens of increasing length and identical cross section, and nearly identical stress-strain curves for specimens of different sizes having constant length-to-diameter ratios. Since the present study is primarily concerned with diameter dependence, the following factors were taken into account: specimen material, specimen geometry, testing method, range of sizes to be tested, and possible influence of surface and volume effects. Aluminum was chosen because of the present lack of conclusive results and the seeming possibility of size effects at relatively large diameters, the

Jan 1, 1964

By G. H. Kesler, J. E. Oberele, C. E. Dryden, J. H. Oxley

Heat-transfer rates were measured in a model of a multifilament vapor-deposition bulb fo the preparation of high-purzty metals. Local transfer coefficients for heat transfer frow the filaments to the circuates process stream were determined as a functiol of gas flow rates and bulb, inlet, and filament, geowzetvies. These results a-e then convertted to n mass-t7,ansfer basis to provide a method of correlating vapor-deposition rates and to predict the performance of commercial urzits. The firm1 cor?,elating equation for mass transfer was found to be- wheve k, is the mass-transfer coefficient; D, is bze gas difficsivity : P is the system pressure; R is the gas constant; T is the gas temperature; Df, DB, and Di ave tlze diameters of the filament, bulb, and inlet, respectively; k is the gas conductivity; C, is the specific heat of the gas, M is the wzolecular zleight of the gas; Npr . N,,, NRe a7'e the Prandtl, Schmidt, and Reynolds numbem of the system, respectively; LB is the height of the bulb; and SB and Sf are the total suyiace area of the bulb and filaments, respectively. ONE of the more conventional methods of preparing very high-purity metals is the vapor deposition of the metal upon heated filaments. The reactions which can be employed in such a process generally fall into two classes: 1) Pyrolysis of a volatile metal compound. Generally because of their instabilities, metal iodides are used; however, other metal halides and hydrides have been employed. These processes are frequently carried out under vacuum conditions, and the filaments are maintained at high temperatures. 2) Hydrogen reduction of a volatile metal compound. A metal chloride is normally the preferred feed for these processes, but other halides are sometimes used under special conditions. These hydro- gen-reduction processes are usually operated at atmospheric pressure. Many of the current processes for the production of semiconductor materials are actually vapor-deposition processes. However, the vapor-deposition process itself is relatively old, and almost all metals can be prepared in a state of very high purity by the use of vapor-deposition techniques. Loonam has recently given an excellent review of the iodide process for metal deposition,' and Owen has started some detailed studies with a carbonyl system.' A more general treatment of all vapor-deposition processes has been outlined by Powell, Campbell, and Gonser.3 Despite the fact that vapor-deposition techniques have been employed since 1890, there is a surprising lack of fundamental information regarding the transport characteristics of even the simplest deposition system, the heated filament. The purpose of the investigation described in this paper was to extend some of the earlier data obtained at Battelle to predict deposition rates and the uniformity of deposition in large-diameter, multifilament deposition bulbs under forced convection conditions.4'5 A number of other investigators have already presented a simplified treatment of the deposition process under non-flow conditions, i.e., pure diffusion.6"9 To obtain information on the transport characteristics of a deposition bulb, a model of a typical plant deposition unit was constructed, and local heat-transfer coefficients from the filaments to a circulating air stream were determined under various conditions of air-flow rates and bulb, inlet, and filament geometries. These results were then converted to a mass-transfer basis, and consequently provided a method to correlate experimental vapor-deposition rates and to design commercial deposition units. EXPERIMENTAL WORK Description of Model. The apparatus which was used in this work was a scaled model of one type of deposition bulb. It was constructed of Lucite and was easily altered to give several combinations of diameter of bulb liner, inlet size and location, number of filaments, and outlet geometry. The model is shown in Figs. 1 and 2. The bulb shell was made octagonal for convenience in construction and observation, and the bulb liners were cylindrical. Air, introduced through one of several different jet inlets, was used as the test fluid in these model studies. Filaments for deposition of metal were simulated by metal rods 1/4-in. in diam. Two of the rods could be heated by passing electrical current through them ¦ while the remaining rods could not be heated. This procedure minimized the amount of heat which was

Jan 1, 1962

By B. Chalmers, L. Bäckerud

The growth temperature of dendrite tips has been measured in a binary alloy system, Al-Cu, as a function of rate of formation of solid phase. Metallographic examination has rerealed the dendritic structure dereloped during different stages of the freezing process and factors influencing the undercooling, such as solute buildup, surface tension, and kinetic effects, have been estimated. Practical implications of the results are discussed. THE development of a dendritic growth pattern during the solidification of metals and alloys has an influence at least equal to that of grain size on the properties of the casting or ingot being produced. and consequently much interest has been devoted to the study of this phenomenon. A review of the knowledge gathered up to 1964 has been given by Chalmers.' Among recent publications in the area the works of Jackson et al 2 and Flemings and his coworkers3,4 are of special interest. This work is an experimental study of the factors which influence the development of a dendritic pattern during the solidification of a typical binary alloy system, A1-Cu, when there is no heat source in the liquid. This means that the temperature and the temperature gradient are controlled by the heat extraction from and latent heat evolved by the growing crystals. EXPERIMENTAL PROCEDURE Samples were prepared from a master alloy made up of aluminum, 99.995 pct, and copper. 99.99 pct, of the concentrations given below and of sufficient size to fill cylindrical graphite molds of 35 mm ID and 35 mm height. Bottom. wall. and lid of the graphite molds were all of 6 mm thickness, Fig. 1. Thin ceramic thermocouple shields could be introduced at different positions in the sample through holes in the lid. The assembly was heated in a small vertical resistance furnace to a suitable temperature. 700° to 720°C. which is well above the melting point of the sample. It was thereafter taken out of the furnace and chilled at selected rates, and the temperature changes in the sample were recorded. For high sensitivity in the temperature recordings, a reference thermocouple was held in a solidifying pure aluminum melt. which was very well insulated and therefore was at a constant temperature. 660°C, for nearly half an hour. The thermocouples were connected so that the difference voltage was fed into the recorder of which the most sensitive range was 1 mV. Temperature variations could be read to within 0.l°C. The thermocouples used were of the Chromel-Alumel type (28- or 38-gage wires) and the recorder a two-pen Moseley strip chart recorder. The different rates of chilling were obtained in the following way. a) The graphite crucible was wrapped in one or two layers of an insulating. feltlike material (Fiberfrax paper from the Carborundum Co.). The drop in temperature per unit time after complete solidification could thereby be varied from 8" to 18°C per min. This corresponds to a rate of heat extraction in the given samples from 0.08 to 0.17 cal cm-' sec-I. 6) The bare graphite mold was placed free on a piece of firebrick. The measured temperature drop was around 50°C per min (-0.5 cal cm-" ' sec- I). c) By blowing compressed air through a tube with many holes surrounding the mold in a ring shape. the rate of heat transfer could be raised to 150' to 200°C per min (-1.7 cal cm-3 sec- I). d) Cooling rates around 1000 C per mill (-9.4 cal cm-3 sec-l) were obtained by substituting the air in the device used in c by water. The range of cooling rates used in these experiments correspond to technical casting processes from slow solidification as obtained in sand molds to very rapid freezing which occurs in some continuous casting and welding processes. EXPERIMENTAL RESULTS The A1-Cu system was chosen for the experiments: the relevant part of the phase diagram is reproduced in Fig. 2. Observation of the Center Temperature. When a thermocouple is inserted in the center of the melt. the type of cooling curves obtained at slow solidification rates differs little from numerous published curves from similar systems. and the solidification pattern

Jan 1, 1970

By W. F. Domis, F. von Gemmingen, R. W. Whitmore, F. Garofalo

Constant-load creep-rupture tests at 1100°, 1300° and 1500°F were made on a Type-316, 18 Cr-8 Ni-ZMo, austenitic stainless steel to determine the relationship between ruptzire life and other aspects of creep behavior, The test program was designed on a statistical basis to check the variability of various creep properties and to determine emprically the dependence of minimutn creep rate and ruptzire life on initial stress, The dependence of the rupture life, tn, on the initial stress, a,, is found to be related to the stress dependence of the wrinimum creep rate, i,, and secondary creep strain, The instabilities or breaks found in the conventionual log - logt, plots can be traced to either a change in the linear dependence of log i, on log a, or to a change in secondary creep strain. In the alloy tested, rupture is found to be predowmanantly of the inter crystalline type, For this material, the secondary creep strain is -found to depend on the nature of the grain boundary precipitate, which affects grain boundary migration. It has been shown for a variety of metals and al tested at elevated temperatures under creep conditions that the empirical relationship exists between rupture life, tr, and minimum creep rate, i,. This relationship, in which C and a are in some cases independent of stress or temperature, shows in a general way that creep rupture depends on creep behavior prior to tertiary creep stage. To determine more fully the factors which control creep rupture requires, therefore, more knowledge of the relationship between rupture and creep behavior. To obtain such information, constant-load creep-rupture tests have been made on a Type-316, 18 Cr-8 Ni-2 Mo, austenitic stainless steel at 11000, 1300°, and 1500°F. These tests were designed on a statistical basis to determine the variability of the various creep properties measured and to determine empirically the stress dependence of minimum creep rate and rupture life. As a result of this work, various empirical relations have been established defining more closely the factor, C, in the relation between rupture life and minimum creep rate. This factor is found to be proportional to the amount of strain during secondary creep. The variation of secondary creep strain with rupture life and temperature is determined and its effect on rupture behavior discussed. The variability in minimum creep rate and rupture life is also dis- cussed and the dependence of these quantities on initial stress is interpreted. TEST MATERIAL AND TEST PROCEDURES The material tested is an austenitic stainless steel, AISI Type 316, of the following composition: C, 0.07 pct; Mn, 1.94 pct; P, 0.01 pct; S, 0.021 pct; Si, 0.38 pct; Cr, 18 pct; Ni, 11.4 pct; Mo, 2.15 pct; All 0.003 pct and N, 0.043 pct. The material was received as a hot-rolled 0.5-in. diam bar which was sectioned into 3.25 in. long blanks. Each blank was heat treated by holding 1/2 hr at 2000° F followed by water quenching. A 3/8-in. coupon was removed from each heat-treated blank and the microstructure was examined, the grain size determined, and the hardness measured. The microstructure was found to be uniform from blank to blank and the grain size was found to range from 4 to 6 ASTM numbers. Hardness, measured using a 20-kg load, varied between 127 and 148 Vpn. Tensile creep-rupture specimens having a 0.25 in. diam within a 1.5-in. reduced section were machined from the heat-treated blanks. Constant-load tests were made on these specimens at 1100°, 1300°, and 1500 F. Six specimens were tested at each stress level. Three creep-rupture machines were employed for tests at each temperature, two specimens being tested in each machine for each stress level. To minimize any effect due to local inhomogeneities along the length of the as-received bar the specimens were randomized before test. Each specimen was tested to rupture and in most cases an autographic extension-time curve was obtained. For very low stress levels at 1500°F no auto-

Jan 1, 1962

By J. L. Walter, W. R. Hibbard

A GREAT deal of work has been done on the rolling of single crystals of iron. Barrett and evensoon studied end orientations of heavily cold-rolled iron crystals and found that some crystals maintained a sharp single orientation during rolling. Others rotated into two or more orientations, and some fragmented and approached the entire polycrystalline texture depending on the original orientation of both the normal and rolling directions. Barrett, Ansel, and Mehl2 studied iron-silicon alloys and found that the addition of silicon to the iron had little effect on heavily rolled polycrystalline material. Dunn3 has extensively studied the cold-rolling and recrystallization of silicon-iron single crystals. Dunn found that for single crystals having initial orientation between (110) [001] and (111) [112], the principalcomponent of the cold-rolled texture is (111) [112]. Koh and Dunn4 studied the cold-rolled textures of single crystals having initial orientations in the range (001) [110] to (111) [IT01 and found that these are stable end orientations. They also found that all orientations having a [110] direction parallel to the transverse direction rotate to either the (001) [110] or the (111) [112] stable end orientation except for orientations near (112) [11], which divide and produce a final texture consisting of (001) [110]and (111) [112] components. Crystals having a (111) <112>-type texture re-crystallized to a (120) [001] or (110) [001]-type texture. Crystals having orientations with a range of (001) to (335) in the rolling plane and [110] in the rolling direction recrystallized5 to a wide spread of the initial orientations resulting from a multiplicity of 30-deg rotations about several (110) poles. The present study was undertaken to relate other orientations of crystals of silicon-iron to their cold-rolling and recrystallization textures, so that one might rationalize polycrystalline recrystallization data on the basis of the known deformation texture and the behavior of single crystals in these orientations. PROCEDURE Samples were obtained from a cylindrical ingot of 3 pct silicon iron prepared as follows: Armco iron was melted with high-purity silicon flakes under an atmosphere of argon to minimize oxidation. The alloy was poured into a special mold to form an ingot which consisted partially of large columnar crystals. Plates were cut from the columnar portions of the ingot with the longitudinal direction parallel to the columnar axes and ground to 0.040 in. thick. The plates were heavily etched to a thickness of 0.032 in. to remove the cold-worked surface. Orientations of seventeen crystals were determined by Laue back-reflection techniques keeping the mean columnar axis as the reference direction. The plate was then cut in two, parallel to the columnar axis. One portion of the plate was rolled at room temperature parallel to the columnar axis to a reduction in thickness of 84 pct. The remaining portion of the plate was rolled also at room temperature across the columnar axis to a reduction of 66 pct, at which point the crystals began to separate at the boundaries. After rolling, nine individual crystals were removed from the strip by cutting along the crystal boundaries with a jeweler&apos;s saw. Fig. 1 shows the original orientations of the six crystals that were straight-rolled and of the three crystals (4, 7, and 8) that were cross-rolled. Each rolled crystal was carefully etched to approximately 0.002 in. thick. Textures of the cold-rolled crystals were determined by use of the diffractometer with a non-integrating sample holder. The pole figures were made for the (200) poles using molybdenum Ka radiation and were plotted by an automatic stereographic projection recorder.&apos; Spurious poles were determined by rerunning portions of the pole figures using strontium oxide to filter out the Ka radiation. The central portions of the pole figures have not been determined. The pole figures were completed to about 55 deg from the periphery at which point the sample holder interfered with passage of the beam. Following the determination of the cold-rolled

Jan 1, 1959

By G. L. Schroeder

Investigations were conducted at two underground locations, foreman&apos;s room and 5702 area, of the Kermac Nuclear Fuels Corp. uranium mining installation, Ambrosia Lake, New Mexico. The rock environment is stratified sandstone. Pressures were varied from minus 0.4 an Hg to plus 3.8 cm Hg with respect to barometric pressure, and were maintained for periods ranging from several hours to 21 days. One cm Hg overpressure (-1.5% of normal barometric pressure) produced a 20-fold decrease in Rn flux into the foreman&apos;s room as compared to the Rn flux observed during dilution ventilation. The 5702 area experienced a 5-fold decrease in Rn flux for a similar overpressure. During 21 days of continuous 1 cm Hg overpressure in the 5702 area this reduced Rn flux was maintained. The smaller reduction in flux for the 5702 area results in part from the proximity of the foreman&apos;s room to a non-pressured area and the presence of an impermeable shale lens overlying the ceiling of the 5702 area. A 0.4 cm Hg underpressure of the 5702 area increased the Rn flux into the area by 3-fold over the non-pressured value. A barometric pressure influence on Rn flux into the mine and on air Rn concentrations in non-pressurd areas of the mine was measured. A falling barometric pressure causes an increase in the flux of interstitial gas into the mine; a rising barometric pressure decreases this flux. These effects are not seen in overpressured mine areas. Radon concentrations in rock interstices show, during overpressure, decreases of all locations monitored except in the immediate vicinity of the shale lens above the 5702 area ceiling. These reductions are the result of air flowing from the mine into the rock interstices under the influence of the pressure gradient induced by the overpressure. The relative humidity of the 5702 area was reduced after 2 days of 1 cm Hg overpressure from a pre-overpressure value of 96% to 81%. The control of harmful or noisesome gases which emanate into underground mining areas from surrounding rocks is often a costly necessity. In uranium (U) mines this problem is presented by the high interstitial concentrations of radon-222 (Rn), a radioactive noble gas of 3.82-day half-period, formed in the decay scheme of U238, and the relative ease with which this noble gas diffuses from its parent rock into the interstices of the rock and then to a working area. Long-term exposure to moderate concentrations of Rn (3000 µµc per 1) and its short-lived alpha-ray emitting daughter products, RaA (Po218) and RaC (po214), has been found to result in an increased incidence of bronchial carcinomaa2 The acceptable limit of Rn daughter products in a mine atmosphere is presently set at a concentration of short-lived radon daughters which would be in equilibrium with 100 ppc of Rn per 1 of air. Ventilation of mines is conventionally accomplished by continuously diluting the mine air with fresh air brought in by fan or natural convection from above ground surface. The diluted air is allowed to vent freely to the atmosphere. This process does nothing to retard the rate at which gases (including Rn) diffuse into the mine from surrounding rock. It merely reduces the concentrations of these gases within the mine. It is suggested that in a sufficiently permeable rock environment a slight pressurization of the mine air may induce air flow from the mine into the interstices of rock surrounding the mine. The convective flow of comparatively fresh air will reduce the concentration and the concentration gradient of undesirable gases in the rock interstices adjacent to the mine. Radon will diffuse counter-current to this convective flow at a rate proportional to its concentration gradient. In time, a steady state of convection and counter diffusion will be established. The Rn flux into the mine will never be reduced to zero, and will only asymptotically approach zero as the overpressure (and hence the convective velocity of purging air) approaches infinity. During 1963 and 1964, an investigation into the effect which such applied pressures have upon the Rn characteristics of a mine atmosphere was conducted at the Kermac Nuclear Fuels Corp. uranium mines, Ambrosia Lake (near Grants), New Mexico.

Jan 1, 1967

By W. A. Backofen, D. H. Avery, G. A. Miller

An evaluation has been made of the relative importance of yield strength (?) and stacking-fault energy (y) to the rate of fatigue-crack growth in materials of fcc structure. Pure copper and its solid-solution al-loys with aluminum and nickel were chosen for the study because they provided sufficient range in both quantities of interest that either could be varied independently of the other. Experiments involved alternating tension and compression of flat specimens which were prepared with sharpened internal notches so that most, if not all, of the crack-nucleation interval could be eliminated. Growth rate (dC/dN) was concluded to be proportional to the square of the plastic-strain amplitude (€,,) over a strain range of approximately 6x 10-4 to 6 x 10-3. The factor, k, linking dC/dN and ep in dC/dN = kEp2 increased and decreased with corresponding variations in y, but it did not respond syste?>/atically to change in ay, indicating that y is the significant variable in crack growth at constant plastic-strain amplitude. In polycrystalline material, k varied by a factor of 5 over the available range of y. In a few single-crystal experiments on Cu-A1 alloys the growth rate responded less strongly to change in y. It has been suggested that single crystals behave somewhat differently than poly crystalline material because there is more extetnsive substructure near the grain boundaries in the latter, and this facilitates crack advance by separation along subgrain boundaries. A point of some controversy in current work on fatigue relates to the effects of strength and stacking-fault energy on crack growth. In recent experiments a separation was made between the cycling intervals for crack nucleation and the subsequent growth that eventually ends a specimen&apos;s fatigue life.&apos; The study was carried out on Cu-A1 alloys primarily, fatigued in alternating four-point bending to constant deflection. A nucleation interval of about 10&apos; cycles (at a total strain amplitude = 0.2 pct) was found to be insensitive to aluminum content in the range 0 to 7.5 wt pct, while the growth period was increased approximately forty fold over the same compositional range. The increase was not in any sense linear, however. Rather, most of the change occurred below 4 pct A1 or a stacking-fault energy, ?, of about 15 ergs per sq cm. It was argued that the plastic-strain amplitude was approximately constant, and therefore the effect of composition must have grown out of the reduction in stacking-fault energy. Several studies have shown that, with high ?, cross slip is encouraged, subgrain structure is introduced during fatigue, and cracking is aided through propagation along subgrain boundaries.1-5 Therefore, lowering ? sufficiently to interfere with substructure formation would be expected to retard growth rate. On the other hand, it is a general rule that resistance to fatigue cracking increases as strength is raised. Accordingly, there might still have been some doubt that Y was the controlling variable, since strength would be increased as y was lowered by the aluminum additions. To help in dispelling that doubt, an experiment was made on a polycrystalline Cu-Ni alloy similar in strength to the Cu-A1 alloys but of higher ?; the crack-growth interval was found to be essentially that of pure copper.&apos; Further support for this position on stacking-fault energy as it relates to crack growth is derived from work by Boettner and McEvily,6 in which the actual crack-growth rate was measured on samples previously notched so as to minimize the nucleation period. Unfortunately, it was necessary in isolating strength level to compare different alloy systems and grain sizes. Recognizing the complication, it was still concluded that growth may be retarded by a reduction in y, per se. A related study has also been made by Roberson and Grosskreutz.7 The zinc content of a brass was systematically changed to alter strength and stack-ing-fault energy, although not below the 15 ergs per sq cm at which pronounced change in growth interval was found in the earlier work. The results were limited to more or less conventional S-N diagrams so that nucleation and growth events could not be separated. No definite conclusions were drawn, but

Jan 1, 1967

By H. E. Swanson

A description of the field apparatus has been published by D. G. Brubaker. Data from laboratory model studies of the in-line and broadside methods of operation are detailed. The conductor models include a single sheet conductor at several strike and dip angles and a schistose-type conductor. In addition, data on the effects of the strike length and of the depth of the conductor are presented for the broadside method of operation. All of the data show that the inclintion reverses direction over the top edge of dipping single sheet conductors. Differences between anomalies over conductors dipping between 90" and 30" are subtle,but flat-lying sheets can be readily distinguished from steeply dipping sheets. Schistose conductors are easily distinguished from single sheet conductors, and a procedure is given for determing the direction of schistosity. The depth of penetration under ideal conditions is 0.7 of the coil separation. In 1950, The New Jersey Zinc Co. (of Pa.) developed a lightweight apparatus for electromagnetic prospecting. A description of this apparatus has been published by D. G. Brubaker.1 It consists of a small, battery-powered vertical source coil and a direction-finding receiving coil. Source and receiver are kept a fixed distance apart and move as a unit along the survey lines. At each receiver station the inclination of the magnetic field created by the source is measured. Two methods of operation are used, in each of which measurements are taken with a constant source-to-receiver distance and with the plane of the source oriented to pass through the receiver station. In one procedure, called the in-line method, source and receiver travel in tandem along the same line. In the other procedure, called the broadside method, source and receiver move along adjacent lines, with the source-to-receiver direction oriented parallel to the assumed strike direction. The data recorded in either case are the inclinations, measured in degrees from the horizontal, of the magnetic field created by the source. These data are plotted at the receiver stations on a map. Scale-model studies of both methods of operation have been conducted in the laboratory and are reported in this paper. APPARATUS Small source and receiving coils wound with many turns of fine copper wire were used to produce and measure an alternating magnetic field in the same manner as the field apparatus. The model source coil was mounted in a vertical position and oriented so that the receiving coil was in the plane of the source. The receiving coil was mounted in a frame so it could be rotated to obtain the inclination measurements. The source coil was excited by a 100-kc signal generator. A tuned amplifier and a voltmeter were used to detect the null position of the receiving coil. The coils used in the field apparatus are usually spaced about 400 ft. The coils used in the model work were spaced from 4 in. to 4 ft apart. Thus the scale of the model work ranges between 1/1200 to 1/100 natural size. The model conductors were aluminum-coated building paper supported on wooden frames. The conductivity-thickness product was measured using a four-electrode system and was found to be about 300 ohms-&apos;. CONDUCTIVITY CONSIDERATIONS The electromagnetic response from a thin sheet conductor is a function of the product of the conductivity of the sheet times the thickness of the sheet times the frequency of the alternating electromagnetic field times some linear dimension of the system such as the coil separation which indicates scale. The secondary electromagnetic field produced by the conductor increases in amplitude from zero at zero conductivity to a maximum value for infinite conductivity, while the phase of the secondary field with respect to the primary field shifts from 90" at zero conductivity to 0" at infinite conductivity. Several authors2-&apos; have shown that most of both the increase in amplitude and the change in phase of the secondary field takes place over a three-decade range of the conductivity-thickness-frequency product. Only small changes in the amplitude and

Jan 1, 1961

By W. L. Phillips

Stress-train curves were obtained for single crystals of silver, Ag-5 pct Zn, Ag-10 pct Zn, and Ag-20 pct Zn tested in tension and shear at 78°, 195°, and 297°K. At room temperature the critical resolced shear stress gC increased, the length of&apos; the easy-glide region increased, and the rate of&apos; work hardening dwving easy glide decreased with increasixg zinc concentration. The change in the ratio of uc at room temperature to that at lower temperatures was significantly greater for the alloys than for pure silver. It was found that an increment in stress was necessary to continue slip when the slip direction was rotated 60 deg. The magnitude of this increment increased with strain for all alloys, increased with zinc concentration for a given strain, and for a given strain increased with decreasing -temperature. DESPITE its practical importance in improving the mechanical properties, alloying is not fully understood. Except for copper alloys few sets of systematic data are available. Von Goler and Sachs&apos; studied the deformation of Cu-Zn alloys of increasing zinc content and found that, for dilute alloys, the critical resolved shear stress increases linearly with concentration. The range of easy glide was found to increase with increasing zinc content. Schmid and seliger,2 Sachs and Weerts,3 and Osswald4 have shown that with Mg-A1, Au-Ag, and Cu-Ni crystals, respectively, the critical resolved shear stress also varies linearly with concentration. More recently, Linde and his coworkers have investigated the variation of the critical shear stress of copper alloyed with tin , antimony, indium, germanium, silicon, nickel, and gold. They found that the slope of the critical resolved shear stress is related to the change of lattice parameter with composition, and also to the difference in Goldschmidt&apos;s atomic diameter between solvent and solute atoms. Garstone, Honey-combe, and creetham6 have shown that similar relationships can be found for small additions of silver, gold, and germanium to pure copper. They found that, with increasing silver or gold concentration, the critical shear stress for glide is increased by alloying, and so is the range of easy glide, which reaches as much as 60 pct for 0.50 pct Ag alloy and 0.62 pct Au alloy, as compared to 6 pct for pure copper of similar initial orientation. They also found that the alloying additions had little effect on the rate of hardening during easy glide, the slope scarcely changing with increasing alloy content. General secondary slip was detected only when the crystals began to harden rapidly. Although the slip appeared to be very fine in the early stages of deformation, coarser slip bands were formed towards the end of the extensive easy-glide range. The present investigation describes the deformation characteristics of single crystals of Ag-Zn containing different concentrations of zinc. Tension and shear testing were used for this study. EXPERIMENTAL PROCEDURE The method of growing the single crystals, sample preparation, and method of testing have been described in detail previously.&apos; EXPERIMENTAL RESULTS A) Tension-Room Temperature. The initial orientations and stress-strain curves of single crystals of silver, Ag-10.0 pct Zn, and Ag-20.0 pct Zn are shown in Fig. 1. It is evident that there is considerable change in the stress-strain characteristics as a function of zinc concentration. The effects of zinc concentration on the critical resolved shear stress for both CU-zn8 and Ag-Zn alloys are summarized in Fig. 2. At all concentrations the resolved shear stress of the Cu-Zn alloys is higher than that of the Ag-Zn alloys. The resolved shear stress increases parabolically as a function of composition for both alloy systems. The length of easy-glide region increased with increasing zinc concentration, Fig. 3b). As the length increased the slope (do/de) decreased slightly, Fig. 3(b). Metallographic investigations demonstrated two significant effects of increasing zinc concentration. First, the amount of clustering increased, compare Figs. 4(a) and (b). The slip lines changed from uniform in pure silver to clustered in the Ag-20 pct Zn and Ag-30 pct Zn alloys. Second, the amount of cross slip decreased as the amount of clustering decreased.

Jan 1, 1968

By E. A. Farrell

A comprehensive survey is made of the status of the asbestos industry as it relates to marketing the product. Included are descriptions of the various types of asbestos and the grading and classification systems used. The uses of asbestos, distribution practices, and types of ore bodies are all related to marketing. World production, the producers and their capacities and world consumption for 1966-67 are summarized and statistical data are included. Asbestos is a general term describing a family of fibrous minerals of the serpentine and amphibole mineral groups. Asbestos has a long history going back to the time of the Egyptians, when it was used as a lamp wick. The commercial mining of asbestos started in Canada, Russia, and Africa in the 1800&apos;s, and the first asbestos products were made in Italy and Russia. The five main types of asbestos are: chrysotile, accounting for 95% of the total mined, amosite, crocido-lite, anthophyllite, and tremolite. Canada, Russia, and Africa are the major producers of asbestos. The commercial utility of asbestos was at first based on the heat resistance of the fibrous mineral in the form of packing, at the start of the industrial revolution. Its current utility is based more on its ability to reinforce binders such as portland cement, rubber, and plastics. Its inertness to the chemical nature of most binders is unique. Most important is its ability to maintain its reinforcing utility when the product is exposed to weather and soil conditions as in asbestos cement boards and pipe, and heat, pressure, and chemical exposure as in brake linings and gaskets and packings. The mineral asbestos is also unique because its fibrous form permits it to be spun and woven to cloth or formed into paper. Many asbestos applications are critical to national defense and at the present time, there are no satisfactory substitutes. Grading and Classification Canadian chrysotile asbestos fiber is graded and priced by length since basically the longer the fiber the higher the utility. The Canadian asbestos industry does not, however, classify the fiber by direct length measurement, but by a dry screening test. The method is called the Quebec Standard Screen (QS) test. One pound of fiber is mechanically shaken in four vertically stacked sieve boxes. The relative proportions remaining on the sieves defines the grade. The longer the fiber, the larger is the amount that stays on the top coarse screens and the less on the lower, finer mesh screens. Other tests can be used to further define the length distribution of fiber such as the wet screen Bauer McNett and the Suter Webb Comb (3 group only). The Canadian grading system divides the milled fibers into 5 main groups: group 3, 4, 5, 6, and 7, with 3 group being the longest, and 7 the shortest. Each group is further divided to subgrades, identified in each group by the letters A to Z, with "A" the longest and "Z" the shortest. See Appendix 1 for the Canadian QS classification system. The Russians also use the QS test on chrysotile. The Africans classify their chrysotile into grades similar to Canadian. The African crocidolite and amosite, however, are classified into actual length groups such as l to 2 in. and 2 to 3 in. Amosite and crocidolite are generally longer than chrysotile but also more brittle. Milled asbestos is not composed of staple length fibers like fiber glass or cotton, but of a mixture or blend of fibers ranging from long to short. Milled asbestos has a fiber length distribution similar to the particle size distribution of a powder. For example, the longest group 3 chrysotile grades have a high percentage of the longest fibers (1/2 to 3/4 in.) and low percentage of short fibers (0.003 in.). The figures in Table 1 give the approximate length distribution of the longest, middle, and shortest groups. A second and further method of classifying fiber is the degree to which the fiber bundles are separated to form a larger number of smaller diameter bundles. This property is normally described as the degree of fiberization, openness or surface area. Air permeability tests are used to measure surface area. Asbestos pro-

Jan 1, 1971

By Peter Tegart

The discovery of gold in the Toodoggone River area is credited to Charles McClair who mined placer deposits in 1925, reportedly valued at $17,500. After he and his partner went missing in 1927, efforts to relocate their workings resulted in the formation of Two Brothers Valley Gold Mines Ltd. in 1933, in which the legendary Grant McConachie (first president of CP Air) played an active role. This was the age when the prospector first utilized the airplane to reconnoitre remote areas. What greeted the observer from the air was an area rich in orange and yellow colours characteristic of gossans formed by the oxidation of sulphides. However, Samuel Black, a Hudson Bay Company fur trader, had also noted in his diary as early as 1824, the unusual and many gossanous colours in the headwaters of the Finlay River. These gossans, coupled with white limestone bluffs and the presence of placer gold, attracted the first reconnaissance of the area by Cominco in 1929. Cominco was ever active in remote areas at this time. They staked and worked several base-metal showings hosted by limestone at the margins of intrusive stocks. These early workers also obtained erratic high gold assays from chalcedony float samples found in creeks draining into the Toodoggone River. However, because the samples gave inconsistent assays, no concerted effort was made to locate their source. Except for the occasional horse-supported prospecting party of the late 1940s and early 1950s, the area did not receive much attention until 1968. Work until this time focused on the base metal lead-zinc showings which contained attractive silver credits. Gold was not an attraction because of the set price established by the US government. The late 1960s saw the northward expansion of porphyry copper exploration into the Toodoggone. A program of gossan soil sampling (gossans which had attracted the early workers) was carried out by Kennco Explorations (Western) Ltd. in 1966-1967. They analysed for base metals in the field, using a cold extraction method. The Kemess copper- gold prospect was staked as a result of anomalous copper values from this early geochemical program. In 1968, Kennco continued the program of silt traversing and field geochemical testing. The samples were further subjected to multielement analysis consisting of copper, molybdenum, lead, zinc, cobalt, nickel, and silver at Kennco&apos;s North Vancouver laboratory. Several anomalous creeks, high in combinations of copper, molybdenum, and silver, were outlined. Some initial soil grids were also established. The fall of 1969 saw the return of Kennco prospector Gordon Davies and geologist Bob Stevenson to check out a well-defined molybdenum, scattered copper and silver anomaly in soils from a grid on the Chappelle claims. The subsequent analysis of several selected quartz felsenmeer floats yielded one assay which ran in the order of 0.25 kg/t (8 oz per st) gold and 2.2 kg/t (70 oz per st) silver. Subsequent trenching on the Chappelle claims exposed the source of float in a 4- m (134) wide vein of high grade gold-silver mineralization. These results led quickly to the realization that the district had precious metal potential. Subsequent exploration in the period 1969-1974 by Kennco resulted in the discovery of most of the gold and silver occurrences on the Chappelle and Lawyers properties. Several other gold and silver occurrences were found in this district by Cordilleran, Cominco, and Sumitomo, working the district during this period. Conwest optioned the Chappelle in 1973 and explored underground by adit entry as part of a one-year program. In 1974, Du Pont of Canada Exploration Ltd. optioned the Chappelle claims and in March 1980, using reserves developed on the A vein, placed the Baker mine into production at a rate of 90.7 Vd (100 stpd). The Amethyst zone on the Lawyers property, 8 km (5 miles) north of Chappelle, was found in 1973 by Kennco using continued, persistent followup prospecting of silver silt geochemical anomalies. A silt anomaly in the order of 3.4 ppm silver occurred in a stream flowing 300 m (984 ft)

Jan 1, 1985

By Horace Pops

Martensitic transformation has been studied during cooling and heating in ß-phase Cu-Zn alloys to which small additions have been made of Ni, Ag, Au, Cd, Ga, In, Si, Ge, Sn, and Sb. The start and finish of the martensitic reaction and the variation of transformation temperature with third-element content were determined by electrical-resistivity measurements from alloys which had either constant zinc contents or constant values of electron concentration. All of the third elements, except nickel, lowered the transformation temperature if the results were plotted along the lines of constant zinc contents in each ternary system. A significant difference in the rate of lowering of the transformation temperature per atomic percent of the third element was observed for elements which had the same nominal valence. No systematic variation of transformation temperature with the valence of the third element was observed. It is suggested that the observed increase in transformation temperature for nickel-bearing alloys is due to the transfer of electrons from the conduction band of the alloy to virtual bound states. However, electron concentration is not the most important factor controlling the instability of the 0 phase. The transformation temperatures of the ternary alloys can be predicted from the following approxilnate expression: Ms (°K) = +3280 - 80 Zn + 8 Ni - 30 Ag - 12 Au - 140 Cd -90 Ga- 145 In - 80 Ge -175 Sn - 120 Si - 150 Sb MOST binary ß -phase alloys based upon the noble metals copper, silver, and gold are unstable at low temperatures and transform spontaneously by a martensitic reaction. This transformation has been studied recently in the ordered bcc ß&apos;-phase Cu-Zn binary al1oys1,2 where the transformation temperature is below the room temperature and decreases with an increase in zinc content. It has been reported that the transformation temperatures can be raised above room temperature by small additions of a third element such as silicon3,5 or gallium,4,5 but no quantitative study has been made. The transformation temperature of different binary alloys can be altered by third-element additions. For example, it was shown that nickel and copper may have a large effect on the Ms temperature of CU-Al6 and Au-cd7 alloys. The present investigation was made to determine systematically the influence of various third elements on the martensite-transformation temperature of Cu-Zn ß-phase alloys. Since these alloys have an electronic origin,&apos; alloy compositions were chosen so that the transformation temperatures could be determined at constant zinc contents or at constant values of electron concentration. I) EXPERIMENTAL PROCEDURE Ten ternary alloy systems were obtained by adding nickel, the noble metals silver and gold, and some B-subgroup elements to a Cu-Zn matrix. These are arranged according to their rows and columns in the Period Table as follows: Each ternary alloy was prepared by melting and casting weighed quantities of high-purity metals (99.99+ pct) in sealed quartz tubes under a partial pressure of helium to make a 4-g ingot. The molten alloys were shaken vigorously and then quenched in water. Since the weight loss was negligible, the compositions of the ingots after casting and annealing were assumed to be the same as the nominal compositions. The ingots were homogenized after casting in helium-filled Vycor tubes for 24 hr at temperatures between 750" and 810 C and quenched into brine. Metallographic examination revealed that all alloys were homogeneous, poly crystalline ß-phase alloys, and that the grain size was in the range 1 to 5 mm. Electrical-resistivity measurements were made to determine transformation temperatures of the ternary alloys during continuous cooling or heating. Transformation temperatures of the ternary alloys can be determined by electrical-resistivity measurements since the resistance of the martensitic phase is much higher than that of the 0&apos; phase. The technique has been described previously in connection with a study of Au-Zn alloys.9 The reproducibility of transformation temperature was approximately ±6°C. II)RESULTS A hysteresis was always observed in electrical-resistivity curves and was usually less than about 12°C.

Jan 1, 1967

By R. W. Kraft

A back- reflection precession-type X-yay camera for determining the crystallographic orientation of the crystallites of both phases in small areas of thick specimens of polyphase alloys is described ad the geometry, advantages, and limitations of the apparatus are discussed. Metallographic obseg-vations of interfacial angles (or habit planes or growth direction are made on the same specimen so that the crystallographic and metallographzc orientation data call be directly correlated. An example of the application of tile technique to a unidi-~~ectionally solidified CuA12-A1 eutectic specimen is presented. The interfacial planes ad growth directions of each phase were established, and the orientation relationship between the phases was observed and found to be approximately intermediate between two previously reported relationships. The crystallographic interfacial relationship between two solid phases is an important parameter in a variety of metallurgical phenomena because of the energy associated with the interface and because this energy is at least partly associated with the way in which the two space lattices are in contact along the interface. In order to describe the interfacial planes in the crystallites of both phases it is necessary to determine the crystallographic orientation of each phase in a specimen relative to each other, and to directly correlate these data with met-allographic measurements from which the interfacial planes can be determined on the same specimen. The back-reflection Laue technique is the easiest way to determine the orientation of thick single crystals or large grains and the method can be combined with metallographic techniques to provide the necessary data, provided the reflections from each phase can be distinguished from one another. However, if the crystallites are small or of varying orientation or if one or both phases has a unit cell with less than the maximum symmetry, many overlapping and complex Laue patterns are recorded simultaneously and it becomes impractical if not impossible to interpret the photographs. All of these complexities were present in a unidirectionally so- lidified A1-CuA12 eutectic alloy1 for which a crystallographic analysis was desired. Consequently the method described here was developed since no known X-ray or electron diffraction technique had all of the following attributes which were required. 1) Method should yield data from which the crys-tallographic orientation of every crystallite or diffracting unit in the irradiated area can be determined. 2) Method should be adaptable to the study of small areas. Depending upon the degree of preferred orientation in the specimens, it should be possible to obtain reliable data in a reasonable length of time on irradiated areas as small as 1.0 or even 0.1 mm in diam. 3) Method should permit direct correlation of crystallographic data with microscopic orientation data pertaining to crystallite axes, habit, morphology, and growth directions as determined by optical microscopy. 4) method should be such that selected areas of large specimens can be easily studied. Trepanning of a small specimen (such as an electron microscope specimen) from larger specimens was undesirable since it would greatly increase the problem of correlating the crystallographic and microscopic directional data. Requirements 3 and 4 dictated that an X-ray back-reflection pinhole technique should be used on large samples, such as metallographic specimens which had previously been examined and analyzed for their microscopic characteristics. Similarly, requirement 2 could be satisfied by choosing a collimator of appropriately small diameter. Exposure times would not be excessive provided the detector were close enough to the specimen. Because of space limitations film was chosen in preference to a Geiger counter. Requirement 1 was fulfilled by using monochromatic radiation and providing enough additional degrees of freedom in specimen rotation to compensate for Bragg law restrictions on diffracted beams. DESCRIPTION OF APPARATUS The apparatus shown in Fig. 1 consists of a pin-hole collimator, (a), projecting through a rotatable circular film in a holder, (b), which records X-ray reflections in the back-reflection region. The specimen, (c), is mounted on the end of a shaft, (d), which is provided with an adjustment, (e), so that the specimen surface can be placed accurately on

Jan 1, 1962

By Pradeep K. Rohatgi, Clyde M. Adams

An analysis of heal conduction in the freezing of a solution has been performed. The case considered is the semi-infinite mass of solution, bounded by a con-stant-temperature plane with one-dimensional heat flow, Numerical cooling rate and freezing rate distributions hare been calcutated for the particular case of unidirectional freezing of aqueous solutions against. a cold copper chill. The solution at each level parallel to the chill surface is subjected to a spectra of frcezing rates; the freezing rate is inilially lour., passes through a maximum, and then decreases until solidification is camplete. Arange and maximum freeeing rates are inversely proportional to the square of distance from the chill surface. The temperature of the chill surface in contact with the solution remains constant during solidification. Experimentally, it is observed that deudrite sparing increases linearly with distance from the chill surface; in the light of heat -flow analysis this means that the dendrile spacing is imersely proportional to the square root of the maximum freezing rate. SOLIDIFICATION of liquids is accompanied by rejection of latent heat at the solid-liquid interface. The over-all rate of liquid to solid transformation is governed by the rate of heat extraction. Analysis of the heat transfer in the liquid during freezing is important since it determines the freezing rate and resulting structure. A considerable amount of work has been done on metallic systems since solidification is frequently a major step in processing metals. Unidirectional freezing from heat sinks has been treated by several investigators.1-4 Much of the work has been limited to the simpler case of substances such as pure metals which freeze isothermally at a unique transformation temperature. In this case the thickness of the solid zone y, next to a chill surface. is a parabolic function of the time. 8. where a and b are constants. Eq. |1| is a close approximation giving the progress of solidification for the case in which there is a small but finite thermal contact resistance at the interface between the freezing liquid and the chill.&apos; It has been used with some success in connection with large steel ingots4 when the therma1 contact resistance is negligibly small (as is the case when water is brought into contact with the metal chill). The constant, b. becomes zero and Eq. [l] is then exact. even when the thermal properties of the chill and the freezing liquid depend on temperature. Analysis of unidirectional solidification of solutions is more complicated since the latent heat is evolved over a range of temperatures. Next to the all-solid zone in contact with the chill surface there is a solid plus liquid zone in which solidification takes place. Although the equations presented are considered quite general the numerical and experimental results are for freezing of aqueous solutions from a copper chill. I) EXPERIMENTAL PROCEDURE Solutions of potassium chloride, sodium chloride. and lithium chloride have been used. These solutions form a eutectic: a typical phase diagram is shown in Fig. 1. A solution at its liquid us temperature is poured into a tygon tube mounted on a relatively large copper chill. The chill is immersed in a freezing mixture of dry ice and acetone at -70°C. A thermocouple connected to a high-speed recorder was mounted near the top of the chill to measure the fluctuation in the temperature of chill surface in contact with the solution. In this system the progress of solidification can be visually observed through the tygon tube. After the specimens freeze to a desired height they are removed from the copper chill and stripped from the tygon tube. Longitudinal and transverse sections are cut from the specimen for micrographic examination. Specimens in the form of a thin slice are mounted on a transparent glass slide by freezing small drops of water around the periphery. They are then polished on a series of emery papers; the final finishing is done on a soft tissue paper. A Leitz Biological microscope was used for structural observations; photography was

Jan 1, 1968

By G. S. Cole, G. F. Bolling

A series of Al-Cu alloys has been cast from constant superheat to solidify either with a hot top or with a free liquid/air interface. All the other variables which affect relative fluid motions were kept constant except the imposition of slow rotations m oscillations of the mold. Depending upon the exact circumstances, evi-dence could be found for the nucleation of equiaxed grains from dendrite bits detached from the columnar zone, or from the free surface, or from solid bits induced at pouring; a special experiment showed the solute buildup during ingot solidification and by inference the reality of constitutional supercooling. All methods of grain nucleation are thus supported. When solidification is arranged in a static mold the columnar- to-equiaxed transition occurs by one of these nucleation paths, subject to the natural decay of temperature gradients which promotes nucleation or the survival of nuclei. But when solidification is forced under special fluid flows it may display odd transitions. In one of these the equiaxed zone is synihesized from. dendrite bits detached from the solid/liquid interface. These survive under the concurrent lowering of temperature gradients and eventually cause transition by impeding columnar growth. GRAIN structure control is desired because real experience shows that specific properties are associated with specific cast grain structures. But since control is thus a matter of need and does not require understanding, much of casting remains art. For example, the manipulation of relative fluid motions in simple ingots provides a control of grain structure development,1-4 but theoretical insight is not required in order to broaden its potential applicability. Fortunately, however, once a variable like fluid flow is recognized it can also provide paths toward new insight. New observations using this variable have provided an insight which is curious. All the theories or descriptions of the columnar-to-equiaxed transition (CET) seem to be supported as long as the appropriate experiment is carried out. In order to develop this idea, let us ignore segregation, the chill zone (until a later section of this paper), and the origin and development of the columnar zone.= The details of questioning how equiaxed material forms in a casting may be divided in two. The first part is simply a questioning of the origin for equi-axed grains: are there fresh nuclei from heterogeneous nucleation, or dendrite bits broken off or melted from the columnar zone or elsewhere,6 or other solid bits surviving from the outset of freezing? The second is more complex, a questioning of the CET: does columnar growth slow down and allow the dominance of equiaxed grains, however they are formed, or do equi-axed grains take over and force columnar growth to stop? This "chicken-or-the-egg" second question can be quite useful, especially because it allows us to delineate the ordinary or NATURAL EQUIAXED ZONE and the induced or SYNTHETIC EQUIAXED ZONE. A natural equiaxed zone occurs if solidification proceeds in the absence of disturbances or extraneous forces such as ultrasonics, stirrings, and so forth. Both the CET theory proposed by Winegard and Chal-mers, 7requiring constitutional supercooling, and the CET theory suggested by Chalmers,8 requiring nuclea-tion only on pouring, pertain to the natural equiaxed zone. The best collating evidence to date for both these theories is contained in the work by Biloni and Chal-mers;9,10 the former theory7 is supported by special versions of the unidirectional growth experiment performed by Plaskett and winegardl1 and the latter theory&apos; is supported in detail for the solidification of small ingots. An equiaxed zone can be synthesized when disturbances caused by forced fluid flows2-4 or other artificial means9,10 break off or melt off dendrite tips from an advancing solid/liquid interface,* if (and only if) temperature gradients in the melt are (forcibly) reduced enough to ensure the survival of these bits of dendrites, 2&apos;3 Willful disturbances even so trivial as those produced by rapping a mold might be included here; as will be shown for example, this follows Southin&apos;s suggestion that the free liquid/air interface

Jan 1, 1970

By J. C. Shyne, T. D. Gulden

The steady-state creep behavior, in compression, of indium containing a dispersion of atomized glass particles was studzed over a range of temperature, stress, and composition. The observed behavior was not consistent with a simple model of dislocation climb over dispersed particles. From room temperature to about 100°C the temperature dependence could be described by an activation energy about one and a half times that of self-dijfusion in indium while at higher temperatures a much higher ternperature dependence was observed. THE value of dispersion-hardened and precipitation-hardened alloys has long been recognized. The mechanism of hardening, however, is not completely understood, especially at elevated temperatures where dispersed particles increase creep resistance. Following the suggestion of Schoeck1 that the rate of creep in dispersion-hardened materials is controlled by dislocation climb over second-phase particles, Ansel and weertman2 derived steady-state creep equations for dispersion-hardened materials. Their derivation was based on dislocation climb over non-deformable spherical particles in a metallic matrix. For low stresses they predicted a linear relation between applied stress and steady-state creep rate. For stresses large enough to cause dislocations to pinch off around the precipitate particles, the theoretical creep rate was shown to be proportional to the fourth power of stress. For very high stresses an exponential stress dependence was predicted. In all cases the theoretical creep rate is linearly proportional to the diffusion coefficient. This provided the primary temperature-dependent factor. Subsequently, Ansel and Lenel3 reported some experimental data on SAP, a composite of aluminum and aluminum oxide, that was in good qualitative agreement with the above theories. Their experimental creep rates, however, were four orders of magnitude less than the theory predicts. This was attributed to a low density of active dislocation sources in the material; somehow the dispersed particles inactivated the dislocation sources instead of merely interferring with dislocation motion. Meyers and sherby4 have recently reported on the creep behavior of SAP. Their results were inconsistent with a simple dispersion-strengthening model and led them to conclude that a continuous network of oxide controls the high-temperature mechanical characteristics of SAP. Because of the rather complex mechanical behavior of SAP and the lack of agreement about the morphology of its oxide phase, it appeared desirable to study the creep of a dispersion-strengthened material of controlled morphology. For the present work a dispersion of spherical glass particles imbedded in a matrix of indium was chosen. The microstructure of this material was similar to the idealized uniform dispersion of hard spheres in a deforming matrix assumed by Ansel and Weertman in their theoretical treatment. SPECIMEN PREPARATION For experimental convenience, it was decided to use a low melting-point metal in this investigation. It was necessary that the metal not be oxidized readily up to its melting temperature and that it wet the second-phase particles. It was desired that the material chosen for the dispersed phase be available as a fine powder with closely controlled size and shape. The material chosen to satisfy these requirements consisted of a matrix of indium metal containing a dispersion of atomized particles of a soft soda-lime-silica glass ranging from 5 to 30 µ in diam. The glass particles had a highly regular spherical shape. The composite was made by stirring the glass powder into liquid indium maintained at a temperature just above the melting point of indium, 156°C. The creep specimens were prepared by a hot pressing operation. Five to ten g of the mixture were placed in a steel die and pressed at 125°C for 5 min under a pressure of 30,000 psi. The resulting specimens were cylinders about 3/8 in. in diam and ranged from 0.4 to 0.7 in. high. By following this procedure a uniform dispersion was obtained in the creep specimens. Typical microstructures of specimens containing twenty and forty volume percent glass powder are shown in Figs. 1 and 2. Unfortunately, grain size could not be determined by the metallo-graphic techniques used. CREEP TESTING PROCEDURE Creep tests were performed in compression under constant stress. The specimens were placed in

Jan 1, 1963

By S. R. Balajee, I. Iwasaki

The adsorption mechanism of corn starch and its derivatives at mineral-solution interfaces was investigated by the adsorption of cationic starch, unmodified corn starch, British Gum 9084, and anionic starch on quartz and hematite. The adsorption of these starches, which decreases in the order mentioned, is dependent on the balance between the magnitude of the electrostatic interaction and the magnitude of the hydrogen bonding. There exists a critical starch concentration for both optimum flotation and flocculation conditions of iron ores, which corresponds to a point where the starch adsorption reaches a saturation coverage. Flocculation occurs due to the adsorption of starch via electrostatic and hydrogen-bonding forces and by interparticle bridging as a result of the conformation of starch molecules at the interface. The depressant property of starches and starch derivatives in flotation&apos; and their flocculation char: acteristics in clarification and filtration2.3 have long been recognized on a wide variety of ores. The effectiveness of a starch as a depressant for iron minerals has been the subject of much investigation in recent years both in the amine flotation of siliceous gangue and in the anionic flotation of activated silica from iron ores. It has been reported that the depressant activity of starches and dextrins in the cationic flotation of quartz from hematite increases with molecular weight, branching, and number of hydroxyl groups, 1 and that the selectivity is affected by changing the configuration of starch molecules and the composition of its polar groups.4 ,5 The manner in which starches are solubilized was shown to exert a significant influence as a depressant in the anionic silica flotation, and a series of articles covering the practical aspects of flotation and flocculation have already been reported.618 Chemical modification of the starch structure, the pulp pH, the calcium ion, and the residual starch concentration were identified as some of the more important variables affecting the flotation behavior. In the flocculation of iron ores, it was noted that most starches flocculated suspensions of hematite in water but did not flocculate similar suspensions of quartz,9 and that an excessive use of starch restabilized the suspensions due presumably to protective action. 6 An admirable application of such an observation to practice may be cited in the selective flocculation and desliming in the anionic silica flotation of iron ores, which resulted in superior metallurgy and lower reagent cost. 10 From detailed adsorption measurements, Schulz&apos;and Cooke4 established that the adsorption of starches and their derivatives depended on the types of minerals and of starches, pH, and electrolytes present. Their adsorption data and the foregoing flotation and flocculation observations suggested that an electrical interaction between starches and charged mineral surfaces might be playing a role in their adsorption process. Adsorption of organic polymers, particularly of synthetic origin, at solid-liquid interfaces has been extensively studied in recent years,&apos; and it is realized that their adsorption mechanism is considerably more complex than that of simple ions or molecules. A polymer molecule possesses a number of functional groups, and the adsorption at a point may restrict the adsorbability of adjacent groups. The mechanism may be further complicated by the conformation of the polymer molecules which may exist as coiled spheres, helices, or extended chains as a result of intramolecular interactions among functional groups as well as intermolecular interactions with solvent molecules. The object of the present investigation was to examine the effect of the chemical modification on the adsorption characteristics of starches and starch products on quartz and hematite at several pH values, so that by correlating this information with flocculation and flotation results, adsorption mechanism of starches on mineral-solution interface may be elucidated. EXPERIMENTAL MATERIALS Quartz: St. Peter sand was screened at 35 mesh and the undersize was scrubbed and deslimed at a Fagergren cell. The deslimed sand was cleaned with 0.1 N hot hydrochloric acid and washed repeatedly with distilled water, For anuscript, measurementsl the -200-mesh fraction of the sand was ground dry in a porcelain mill for 3 hr. The specific surface of the finely ground quartz was

Jan 1, 1970

By Carl F. Lutz, Robert F. Mehl

A layer of brass was formed on 0 brass using a vapor-solid reaction technique. The variation in composition with distance within the phase layer and across the a -ß interface was determined by an electron probe. The diffusivities were calculated as a function of concentration; the diffusion coefficient in brass was found to change by a factor of twenty-five over a compositional range of 8 at. pct. An explanation is proposed to account for the large change in the diffusivity, based on possible stresses in the diffusion zone; it is suggested that the concentration dependence of the thermodynamic factor might decrease the activation energy with increasing zinc content. ALTHOUGH the body of data on diffusion coefficients (D- values) in terminal solid solutions and in isomorphous systems is quite large, there is but little quantitative information for intermediate alloy phases. This paper recounts measurements of D-values for the ? phase in the Cu-Zn system. The experimental method employed consists in the forming of alloy layers and determining and analyzing the concentration-distance (c-x) curve. The experimental method employed could have been applied to several systems; the Cu-Zn system was chosen because the D-values in the a and ß phases are well known, and can thus be used for purposes of comparison. The rates of growth, of intermediate alloy layers are known for a number of systems. In nearly all cases the thickness varies parabolically with time, as to be expected if the rate of growth is controlled by the D-values. In a few cases, nonparabolic behavior has been noted.1 Nonparabolic growth may be the result of a) a variation of the composition at the phase interface with time, b) interface-controlled kinetics, c) short diffusion times coupled with long vacancy lifetimes (in vacancy diffusion),2 and d) crystal reorientation during diffusion in anisotropic systems.3 In the Al-Ni system4 and in the Al-u5 system parabolic growth kinetics are slowly approached after an initial transient period. In general those phases stable at a given temperature in a system A-B appear as separate phase layers when A and B are put in contact and given a diffusion he at-treatment. In most cases the compositions at the interface of adjacent phase layers are those read from the phase diagrams for the termini of the respective phases. This discontinuity in concentration is taken as independent of time, and the growth of one phase at the expense of another is assumed to be independent of interface kinetics, i.e., the rate of interface movement is controlled by volume diffusion in the phases concerned. wagner6 has given many solutions for multi-phase diffusion processes, assuming that the chemical diffusion coefficient, D, is independent of concentration, as have others. Jost7 has pointed out that the familiar Boltzmann-Matano solution is as valid for a (c-x) curve exhibiting concentration discontinuities at phase boundaries as for the usual single-phase case. Heumann and associates8,9 have applied this solution to the multi-phase case, but lacking concentration data within the several layers were forced to assume linear concentration gradients, thus calculating only average D-values. The purposes of the present study were: 1) to determine the dependence of D on concentration, 2) to calculate the intrinsic diffusion coefficients D?Cu and D?Zn, 3) to establish the time-law for the movement of the interface, 4) to determine the concentration limits at the ß-? interface, and, 5) to attempt to clarify the mechanism of diffusion. EXPERIMENTAL PROCEDURE The ? phase is exceedingly brittle; conventional solid couples and conventional sectioning methods were thus inapplicable. Vapor-solid couples were accordingly employed. Unfortunately the equilibrium vapor pressures of Zn for the ? phase are unknown; to escape this awkwardness, samples were enclosed in a capsule containing powder of an alloy of known composition, sufficiently large in quantity as to be effectively an infinite source, maintaining the concentration of Zn at the sample surface constant with time. The sources of Zn-vapor which can be employed in reaction with Cu, or a brass, or ß brass, to form a layer of ? brass satisfactorily wide in concentration range, are alloys of the phases ?, or ? + E or ? + d (depending on the temperature).

Jan 1, 1962

By Ronald K. Linde

Metastable Ag-Cu solid solutions at two compositions beyond the maximum limits of solubility obtainable by quenching from the solid state were obtained by rapid quenching from the liquid state. The process of transformation of the metastable solid solutions into the equilibrium phases was studied by means of X-ray diffraction intensity measurements and electrical-resistance measurements; metallographic examination was also performed. Results are compared with those for an alloy quenched from the solid state at a composition which exists as a solid solution at elevated temperatures. Activation energies for the trans-formation were computed to be 33,600 * 2500 and 33,100 * 2000 cal per g mole for the 60.1 and 75.0 at. pct Ag;Cu compositions, respectively THE kinetics of precipitation in supersaturated solid solutions obtained by quenching from high temperature has been thoroughly studied in many alloys, and detailed investigations of the early stages of nucleation and subsequent growth of the equilibrium phases have been carried out. All of these studies have been made on alloys quenched from the solid state, however, and it is the purpose of this paper to present some of the results on the kinetics of transformation of metastable solid solutions in Ag-Cu binary alloys whose compositions lie outside of the solid-state limits of solubility. Limits of solubility in the solid state can be increased by rapid quenching from the liquid state. This was first demonstrated by Falkenhagen and Hofmann, who obtained appreciable increases in solubility limits of the elements of the first transition series in aluminum by rapid cooling of liquid alloys through contact with a copper mold maintained at liquid nitrogen temperature.&apos; The same basic idea of cooling a liquid alloy by conduction onto a substrate rather than by convection of a gas or liquid (conventional quenching) has been recently revived and extended to very high rates of cooling by Duwez and his collaborators. The new technique was first applied to Ag-Cu alloys because the existence of a eutectic in this system is not predicted by the Hume-Rothery rules of alloy phase formation. Rapid quenching from the liquid state resulted in metastable solid solutions at all concentrations. The kinetics of decomposition of these metastable solid solutions containing 60.1 at. pct Ag;Cu (eutectic composition) and 75.0 at. pct Ag;Cu is the subject of the present paper. EXPERIMENTAL TECHNIQUES Alloys were made in 10- to 20-g heats using silver of purity 99.99 pet and copper of purity >99.999 pct. Components were weighed accurately to 0.1 mg and melted by induction heating in an alumina crucible under an atmosphere of hydrogen. Weight losses amounted to less than 0.02 ~ct in all cases. Rapid cooling from the liquid state was achieved in an apparatus of the type described by Pietrokowsky. 3 In this technique a freely falling drop of molten alloy is caught between a stationary anvil and a fast moving piston, both anvil and piston being lined with copper. The resulting foils were approximately circular (about 2 cm in diam) and from about 50 to 150 u in thickness, depending on the pressure driving the piston. Metallographic samples were prepared for polishing by edge-mounting foils in Quickmount. The mostef-fective etching procedure was found to be: 10 parts NH4OH (concentrated), 1 part H2O2 (30 pct), 5 parts H2O, swab for 5 to 10 sec. The transformation of the metastable alloys to equilibrium was followed by X-ray diffraction and electrical-resistivity measurements. The peak intensity and the integrated intensity of suitable Bragg reflections of the metastable and stable solid solutions were studied with a Norelco dif-fractometer, using nickel-filtered copper KO radiation. The peaks were step-scanned at intervals of 0.05 deg. Using either a Kelvin bridge or a null circuit with a Leeds and Northrup K-2 potentiometer, the changes in electrical resistance due to phase transformation were measured for specimens cut into strips about 20 mm long and 4 mm wide. All resistivity measurements were carried out at liquid-nitrogen temperature. The isothermal heat treatment was accomplished by sealing the samples in argon-filled aluminum containers with stainless-steel O-rings. Containers were then suspended in wax baths with temperatures in the

Jan 1, 1967

By Y. Shimomura, M. Serizawa, Y. Takahashi, K. Miyagawa

The "semi-pellet" sintering method developed and currently being used at the Fuji Iron & Steel&apos;s Hirohata Works is discusssd. It is shown that the method makes fine-sized material easily sinterable and increases sinter production. The operation can be incorporated readily into conventional sintering plants. Sintering plant raw materials currently being used in the Hirohata Works consist of 40 pct pyrite cinder, 40 pct fines resulting from crushing and screening of imported ores, and 20 pct others, such as mill scale and iron sands. Pyrite cinder, a major component in the sinter feed, has been getting finer since 1952, due to the increased grinding required for the improvement of the results in the iron sulfide flotation and to the adoption of FluoSolid roasters in sul-furic acid plants; some fines pass 100-mesh sieve almost completely. Increased use of the fine-sized pyrite cinders in the sinter raw mix resulted in such difficulties as decreased bed permeability, uneven firing conditions, and low yield. In an attempt to study the cause and to find a remedy for this problem, a series of experiments were made, using an 80-kg experimental sintering pan. As a result it was established that, by rolling the fine-sized pyrite cinders into small balls of 10 to 3 mm diam (hereafter called semi-pellets) and mixing them into the sinter raw mix, the bed permeability was improved, the sintering time shortened, and the yield and production rate increased. It is proposed that this new method be called the semi-pellet sintem&apos;ng. In recent years the pelletizing process has taken the spotlight in the agglomeration field for treating fine-sized ores here in Japan as well as in the U.S. and Europe. This process produces pellets suitable for the blast furnace charge as such, and consists of three major operations: fine grinding, balling, and firing. With regard to the firing technique, some problems still appear unsolved. In the semi-pellet sintering, however, several ad- vantages can be claimed: the balling operation is relatively simple because only small-sized balls are shown to be acceptable and the operation can be readily incorporated into the conventional sintering plant, since only balling, not grinding or firing, equipment is needed. Basic test work on the process was initiated in 1954 and favorable results were obtained. Accordingly a pilot plant was built in 1955 and the test work was continued. The semi-pellets thus prepared in the pilot plant were tested further by USing them in the actual sintering pan and their beneficial effects ascertained. In late 1956 a drum-type balling machine (2.4X4 m) was installed and it went into operation in April 1957 in conjunction with the Greenawalt sintering plant (8 pans having dimensions of 7.2 m in length, 3 m in width, and 0.3 m in depth). In October 1958 a cone-type pelletizer, with a 2.2 m diam, and later a disk-type pelletizer were further added in the plant. In the DL sintering plant (2000 tpd), newly built in July, 1960, four disk-type pelletizers (3.2 m diam, 10 tph capacity) were installed. By mixing the semi-pellets thus prepared with the feed, the sintering operation was found to be greatly improved. The results of the basic test work, and the equipment and operation of the semi-pellet sintering operation at the Hirohata Works will be described. ON THE SINTERING CHARACTERISTICS OF FINE SIZED PYRITE CINDERS To ascertain the effect of addition of fine-sized pyrite cinders on the sintering characteristics, a series of measurements on bed permeability was carried out by varying the size distribution of pyrite cinders. The composition of the raw mix used in the tests was fixed at 50 pct pyrite cinder, 20 pct Larap magnetite fines, 30 pct sinter return, and 5 pct coke; only the size distribution of the pyrite cinder was varied. Also the moisture content was changed at each size distribution. The results are given in Fig. 1. For all pyrite cinders tested the bed

Jan 1, 1961